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Sample records for coupled plasma icp

  1. Inductively coupled plasma mass spectrometry (ICP-MS)

    International Nuclear Information System (INIS)

    Shimamura, Tadashi

    1997-01-01

    The period of investigation for the previous general remarks on the progress of ICP-MS was from January, 1991 to September, 1993. In the investigation of this time, for the object of the Chemical Abstracts from January, 1994 to September, 1996, retrieval was carried out by using the STN International. As the key words, ICP-MS, Inductively Coupled Plasma Mass Spectrometry or Inductively Coupled Plasma Mass Spectrometer was used. The number of hit was 373 in 1994, 462 in 1995, and 356 as of September, 1996, 1191 in total. The cumulative number of the papers from 1980 to 1996 is shown. It is known how rapidly the ICP-MS has pervaded as the means of analysis. In order to cope with the enormous number of papers, this time, it was decided to do the review by limiting to the papers which were published in the main journals deeply related to analytical chemistry. As to the tendency in the last three years, it is summarized as how to overcome the spectrum interference and matrix effect in the ICP-MS and the trend of using the ICP-MS as the high sensitivity detector for separation techniques. The technical basic research of the ICP-MS on spectrum interference, sample introduction method and others and the analysis of living body samples are reported. (K.I.)

  2. LLNL large-area inductively coupled plasma (ICP) source: Experiments

    International Nuclear Information System (INIS)

    Richardson, R.A.; Egan, P.O.; Benjamin, R.D.

    1995-05-01

    We describe initial experiments with a large (76-cm diameter) plasma source chamber to explore the problems associated with large-area inductively coupled plasma (ICP) sources to produce high density plasmas useful for processing 400-mm semiconductor wafers. Our experiments typically use a 640-nun diameter planar ICP coil driven at 13.56 MHz. Plasma and system data are taken in Ar and N 2 over the pressure range 3-50 mtorr. RF inductive power was run up to 2000W, but typically data were taken over the range 100-1000W. Diagnostics include optical emission spectroscopy, Langmuir probes, and B probes as well as electrical circuit measurements. The B and E-M measurements are compared with models based on commercial E-M codes. Initial indications are that uniform plasmas suitable for 400-mm processing are attainable

  3. Determination of hafnium with the inductively coupled plasma (ICP)

    International Nuclear Information System (INIS)

    Wuensch, G.; Pose, K.

    1985-01-01

    The relative intensities of 198 hafnium lines in the Ar-ICP are listed. Spectral interference tables are given for the 9 analytically best lines, covering the range of +-60 pm around the Hf-lines. They include measured (not calculated) data of the interferent equivalent concentrations (IEC) and the critical concentration ratios (CCR) for 115 lines of all 34 possibly interfering elements. In many cases, these IEC- or CCR-data differ by 1 or 2 orders of magnitude from those calculated from intensities observed in the NBS-copper arc. Since no intense Hf-line is free from spectral interferences, examples are given for the calculation of the most suitable line for a known matrix. (orig.) [de

  4. Impact of plasma tube wall thickness on power coupling in ICP sources

    International Nuclear Information System (INIS)

    Nawaz, Anuscheh; Herdrich, Georg

    2009-01-01

    The inductively heated plasma source at the Institute of Space Systems was investigated with respect to the wall thickness of the plasma tube using an air plasma. For this, the wall thickness of the quartz tube was reduced in steps from 2.5 to 1.25 mm. The significance of reducing the wall thickness was analyzed with respect to both the maximum allowable tube cooling power and the coupling efficiency. While the former results from thermal stresses in the tube's wall, the latter results from a minimization of magnetic field losses near the coil turns of the inductively coupled plasma (ICP) source. Analysis of the thermal stress could be validated by experimental data, i.e. the measurement of the tube cooling power when the respective tube structure failed. The coupling efficiency could be assessed qualitatively by simplified models, and the experimental data recorded show that coupling was improved far more than predicted.

  5. Plutonium bioassay by inductively coupled plasma mass spectrometry ICP/MS

    International Nuclear Information System (INIS)

    Wyse, E.J.; Fisher, D.R.

    1993-04-01

    The determination of plutonium in urine poses several analytical challenges, e.g., detectability, matrix, etc. We have investigated the feasibility of analyzing plutonium in processed urine by inductively coupled plasma mass spectrometry (ICP/MS). The urine samples are first spiked with 244 Pu as a tracer and internal standard, then processed by co-precipitation and column chromatography using TRU-Spec trademark, an extraction resin. By enhancing ICP/MS detection capabilities via improved sample introduction and data acquisition efficiencies, an instrumental detection limit of 5 to 50 fg (0.3 to 3 fCi for 239 pu) is typically obtained, depending on the desired degree of quantitation. A brief summary of the analytical method as well as the basis for measuring radionuclides by ICP/MS are submitted; the separation procedure, methods of sample introduction, and data acquisition techniques are then highlighted

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

    Energy Technology Data Exchange (ETDEWEB)

    Lewis, L.A.

    1998-05-01

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

  7. Complete chemical analysis of produced water by modern inductively coupled plasma spectroscopy (ICP)

    Energy Technology Data Exchange (ETDEWEB)

    Graham, G M; Sorbie, K S; Johnston, A; Boak, L S

    1997-12-31

    ICP (Inductively Coupled Plasma) spectroscopy is recognised as a very effective tool for monitoring ion compositions in many different waters. It has also been used by a number of laboratories to determine residual levels of phosphonate (PH) scale inhibitors in produced waters, based on phosphorus content. Until recently, it had not been used effectively to monitor phosphino-polycarboxylate (PPCA) returns. Large errors had frequently been observed where it had been applied. The poor detection limits and accuracy obtained for PPCA inhibitors relates to much lower amount of phosphorus present when compared with a typical phosphonate inhibitor. This paper demonstrates the effectiveness of IPC detection for PPCA and other phosphorus containing inhibitors by the use of modern instruments without the need of pre-treatment. 6 refs., 3 figs., 10 tabs.

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

    International Nuclear Information System (INIS)

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

    1989-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-06-30

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

  10. Multi-elemental analysis of aqueous geochemical samples by quadrupole inductively coupled plasma-mass spectrometry (ICP-MS)

    Science.gov (United States)

    Wolf, Ruth E.; Adams, Monique

    2015-01-01

    Typically, quadrupole inductively coupled plasma-mass spectrometry (ICP-MS) is used to determine as many as 57 major, minor, and trace elements in aqueous geochemical samples, including natural surface water and groundwater, acid mine drainage water, and extracts or leachates from geological samples. The sample solution is aspirated into the inductively coupled plasma (ICP) which is an electrodeless discharge of ionized argon gas at a temperature of approximately 6,000 degrees Celsius. The elements in the sample solution are subsequently volatilized, atomized, and ionized by the ICP. The ions generated are then focused and introduced into a quadrupole mass filter which only allows one mass to reach the detector at a given moment in time. As the settings of the mass analyzer change, subsequent masses are allowed to impact the detector. Although the typical quadrupole ICP-MS system is a sequential scanning instrument (determining each mass separately), the scan speed of modern instruments is on the order of several thousand masses per second. Consequently, typical total sample analysis times of 2–3 minutes are readily achievable for up to 57 elements.

  11. The effect of dielectric top lids on materials processing in a low frequency inductively coupled plasma (LF-ICP) reactor

    International Nuclear Information System (INIS)

    Lim, J.W.M.; Chan, C.S.; Xu, L.; Xu, S.

    2014-01-01

    The advent of the plasma revolution began in the 1970's with the exploitation of plasma sources for anisotropic etching and processing of materials. In recent years, plasma processing has gained popularity, with research institutions adopting projects in the field and industries implementing dry processing in their production lines. The advantages of utilizing plasma sources would be uniform processing over a large exposed surface area, and the reduction of toxic emissions. This leads to reduced costs borne by manufacturers which could be passed down as consumer savings, and a reduction in negative environmental impacts. Yet, one constraint that plagues the industry would be the control of contaminants in a plasma reactor which becomes evident when reactions are conducted in a clean vacuum environment. In this work, amorphous silicon (a-Si) thin films were grown on glass substrates in a low frequency inductively coupled plasma (LF-ICP) reactor with a top lid made of quartz. Even though the chamber was kept at high vacuum (~10 −4 Pa), it was evident through secondary ion mass spectroscopy (SIMS) and Fourier-transform infra-red spectroscopy (FTIR) that oxygen contaminants were present. With the aid of optical emission spectroscopy (OES) the contaminant species were identified. The design of the LF-ICP reactor was then modified to incorporate an Alumina (Al 2 O 3 ) lid. Results indicate that there were reduced amounts of contaminants present in the reactor, and that an added benefit of increased power transfer to the plasma, improving deposition rate of thin films was realized. The results of this study is conclusive in showing that Al 2 O 3 is a good alternative as a top-lid of an LF-ICP reactor, and offers industries a solution in improving quality and rate of growth of thin films. (author)

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

    Science.gov (United States)

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

    2018-04-15

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

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

    International Nuclear Information System (INIS)

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

    1998-01-01

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

  14. Zinc, lead and copper in human teeth measured by induced coupled argon plasma atomic emission spectroscopy (ICP-AES)

    Energy Technology Data Exchange (ETDEWEB)

    Chew, L.T.; Bradley, D.A. E-mail: D.A.Bradley@exeter.ac.uk; Mohd, Y.; Jamil, M

    2000-11-15

    Inductively Coupled Argon Plasma Atomic Emission Spectroscopy (ICP-AES) has been used to determine Pb, Zn and Cu levels in 47 exfoliated human teeth (all of which required extraction for orthodontic reasons). Lead concentrations for the group were 1.7 {mu}g (g tooth mass){sup -1} to 40.5 {mu}g (g tooth mass){sup -1}, with a median of 9.8 {mu}g (g tooth mass){sup -1}. A median lead level in excess of the group value was found for the teeth of six lorry drivers who were included in the study. A more significant enhancement was found for the seven subjects whose age was in excess of 60 years. The median values for Zn and Cu were 123.0 and 0.6 {mu}g (g tooth mass){sup -1} respectively. Present values for tooth-Zn are lower than published data for other ethnic groups.

  15. Comparison of standard and reaction cell inductively coupled plasma mass spectrometry in the determination of chromium and selenium species by HPLC-ICP-MS

    International Nuclear Information System (INIS)

    Bednar, A.J.; Kirgan, R.A.; Jones, W.T.

    2009-01-01

    Elemental speciation is becoming a common analytical procedure for geochemical investigations. The various redox species of environmentally relevant metals can have vastly different biogeochemical properties, including sorption, solubility, bioavailability, and toxicity. The use of high performance liquid chromatography (HPLC) coupled to elemental specific detectors, such as inductively coupled plasma mass spectrometry (ICP-MS), has become one of the most important speciation methods employed. This is due to the separation versatility of HPLC and the sensitive and selective detection capabilities of ICP-MS. The current study compares standard mode ICP-MS to recently developed reaction cell (RC) ICP-MS, which has the ability to remove or reduce many common polyatomic interferences that can limit the ability of ICP-MS to quantitate certain analytes in complex matrices. Determination of chromium and selenium redox species is achieved using ion-exchange chromatography with elemental detection by standard and RC-ICP-MS, using various chromium and selenium isotopes. In this study, method performance and detection limits for the various permutations of the method (isotope monitored or ICP-MS detection mode) were found to be comparable and generally less than 1 μg L -1 . The method was tested on synthetic laboratory samples, surface water, groundwater, and municipal tap water matrices

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

    NARCIS (Netherlands)

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

    2015-01-01

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

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

    NARCIS (Netherlands)

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

    2015-01-01

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

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

    Science.gov (United States)

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

    2015-03-17

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

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

    Science.gov (United States)

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

    2001-08-01

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

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

    Science.gov (United States)

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

    2018-01-01

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

  1. Determination of some inorganic metals in edible vegetable oils by inductively coupled plasma atomic emission spectroscopy (ICP-AES

    Directory of Open Access Journals (Sweden)

    Musa Özcan, M.

    2008-09-01

    Full Text Available Seventeen edible vegetable oils were analyzed spectrometrically for their metal (Cu, Fe, Mn, Co, Cr, Pb, Cd, Ni, and Zn contents. Toxic metals in edible vegetable oils were determined by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES. The highest metal concentrations were measured as 0.0850, 0.0352, 0.0220, 0.0040, 0.0010, 0.0074, 0.0045, 0.0254 and 0.2870 mg/kg for copper in almond oil, for iron in corn oil-(c, for manganese in soybean oil, for cobalt in sunflower oil-(b and almond oil, for chromium in almond oil, for lead in virgin olive oil, for cadmium in sunflower oil-(e, for nickel almond oil and for zinc in almond oil respectively. The method for determining toxic metals in edible vegetable oils by using ICP-AES is discussed. The metals were extracted from low quantities of oil (2-3 g with a 10% nitric acid solution. The extracted metal in acid solution can be injected into the ICPAES. The proposed method is simple and allows the metals to be determined in edible vegetable oils with a precision estimated below 10% relative standard deviation (RSD for Cu, 5% for Fe, 15% for Mn, 8% for Co, 10% for Cr, 20% for Pb, 5% for Cd, 16% for Ni and 11% for Zn.En este estudio se analizó espectrométricamente el contenido en metales (Cu, Fe, Mn, Co, Cr, Pb, Cd, Ni, and Zn de 17 aceites vegetales comestibles mediante ICP-AES. Las concentaciones más elevadas se encontraron para el cobre en el aceite de almendra (0.0850 mg/kg, para el hierro en el aceite de maiz(c,(0.0352 mg/kg, para el manganeso en el aceite de soja (0.0220 mg/kg, para el cobalto en el aceite de girasol (b (0.0040 mg/kg, para el cromo en el aceite de almendra (0.0010 mg/kg, para el plomo en el aceite de oliva virgen (0.0074 mg/kg, para el cadmio en el aceite de girasol (e (0.0045 mg/kg, para el niquel en el aceite de almendra (0.0254 mg/kg y para el zincen el aceite de almendra (0.2870 mg/kg. Los metales se extrajeron a partir de bajas cantidades de aceite (2-3 g, con

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

    International Nuclear Information System (INIS)

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

    2004-01-01

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

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

    DEFF Research Database (Denmark)

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

    2006-01-01

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

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

    OpenAIRE

    Ugarte Baztán, Ana

    2014-01-01

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

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

    Science.gov (United States)

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

    2015-06-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-10-01

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

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

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

    International Nuclear Information System (INIS)

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

    2011-01-01

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

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

    Science.gov (United States)

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

    2012-02-01

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

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

    International Nuclear Information System (INIS)

    Ozturk, Yildirim; Benderli, Cihan

    2010-01-01

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

  11. Vertically aligned Si nanocrystals embedded in amorphous Si matrix prepared by inductively coupled plasma chemical vapor deposition (ICP-CVD)

    Energy Technology Data Exchange (ETDEWEB)

    Nogay, G. [Department of Physics, Middle East Technical University (METU), Ankara 06800 (Turkey); Center of Solar Energy Research and Application (GÜNAM), Middle East Technical University (METU), Ankara 06800 (Turkey); Saleh, Z.M., E-mail: zaki.saleh@aauj.edu [Center of Solar Energy Research and Application (GÜNAM), Middle East Technical University (METU), Ankara 06800 (Turkey); Department of Physics, Arab American University–Jenin (AAUJ), Jenin, Palestine (Country Unknown); Özkol, E. [Center of Solar Energy Research and Application (GÜNAM), Middle East Technical University (METU), Ankara 06800 (Turkey); Department of Chemical Engineering, Middle East Technical University (METU), Ankara 06800 (Turkey); Turan, R. [Department of Physics, Middle East Technical University (METU), Ankara 06800 (Turkey); Center of Solar Energy Research and Application (GÜNAM), Middle East Technical University (METU), Ankara 06800 (Turkey)

    2015-06-15

    Highlights: • Inductively-coupled plasma is used for nanostructured silicon at room temperature. • Low temperature deposition allows device processing on various substrates. • Deposition pressure is the most effective parameter in controlling nanostructure. • Films consist of quantum dots in a-Si matrix and exhibit columnar vertical growth. • Films are porous to oxygen infusion along columnar grain boundaries. - Abstract: Vertically-aligned nanostructured silicon films are deposited at room temperature on p-type silicon wafers and glass substrates by inductively-coupled, plasma-enhanced chemical vapor deposition (ICPCVD). The nanocrystalline phase is achieved by reducing pressure and increasing RF power. The crystalline volume fraction (X{sub c}) and the size of the nanocrystals increase with decreasing pressure at constant power. Columnar growth of nc-Si:H films is observed by high resolution transmission electron microscopy (HRTEM) and scanning electron microscopy (SEM). The films exhibit cauliflower-like structures with high porosity that leads to slow but uniform oxidation after exposure to air at room temperature. Films deposited at low pressures exhibit photoluminescence (PL) signals that may be deconvoluted into three distinct Gaussian components: 760–810, 920–935, and 990–1000 nm attributable to the quantum confinement and interface defect states. Hydrogen dilution is manifested in significant enhancement of the PL, but it has little effect on the nanocrystal size and X{sub c}.

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

    Science.gov (United States)

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

    2013-10-01

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

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

    International Nuclear Information System (INIS)

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

    2009-01-01

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

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

    Science.gov (United States)

    Murphy, K E; Beary, E S; Rearick, M S; Vocke, R D

    2000-10-01

    Lead (Pb) and cadmium (Cd) have been determined in six new environmental standard reference materials (SRMs) using isotope dilution inductively coupled plasma mass spectrometry (ID ICP-MS). The SRMs are the following: SRM 1944, New York-New Jersey Waterway Sediment, SRMs 2583 and 2584, Trace Elements in Indoor Dust, Nominal 90 mg/kg and 10,000 mg/kg Lead, respectively, SRMs 2586 and 2587, Trace Elements in Soil Containing Lead from Paint, Nominal 500 mg/kg and 3,000 mg/kg Lead, respectively, and SRM 2782, Industrial Sludge. The capabilities of ID ICP-MS for the certification of Pb and Cd in these materials are assessed. Sample preparation and ratio measurement uncertainties have been evaluated. Reproducibility and accuracy of the established procedures are demonstrated by determination of gravimetrically prepared primary standard solutions and by comparison with isotope dilution thermal ionization mass spectrometry (ID TIMS). Material heterogeneity was readily demonstrated to be the dominant source of uncertainty in the certified values.

  15. Method validation for determination of metals in Vitis labrusca L. grapevine leaf extracts by inductively coupled plasma mass spectrometry (ICP-MS

    Directory of Open Access Journals (Sweden)

    LIANE V.V. BOKOWSKI

    Full Text Available ABSTRACT Vitis labrusca L. is the main species used for wine and juice production in Brazil. The grapevine leaves can be used both as functional foods and as cheapest sources for the extraction of phenolic compounds. Besides the antioxidant activity, grapevine leaves exhibited significant anti-inflammatory activity. Therefore, the aim of this study was to develop and validate an analytical methodology to determine the metals selenium (96Se, chromium (53Cr, nickel (62Ni, cadmium (111Cd and lead (206Pb in 30 samples of grapevine leaf extracts (Vitis labrusca, Bordo cultivar using inductively coupled plasma mass spectrometry (ICP-MS. To obtain the grapevine leaf extracts the samples were milled, weighed and digested in microwave oven with nitric acid. The method showed linearity, precision, accuracy and limits of quantification and detection acceptable for INMETRO protocol validation of analytical methods. Therefore, the method using ICP-MS was developed and validated to determine metals concentrations in grapevine leaves of Vitis labrusca L. and the proposed method could be applied in routine analytical laboratory.

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

    Science.gov (United States)

    Stanislawska, Magdalena; Janasik, Beata; Wasowicz, Wojciech

    2013-12-15

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

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

    International Nuclear Information System (INIS)

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

    1999-01-01

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

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

    Science.gov (United States)

    Brima, Eid Ibrahim

    2016-10-01

    Objective: The use of Shamma (smokeless tobacco) by certain groups is giving rise to health problems, including cancer, in parts of Saudi Arabia. Our objective was to determine metals levels in Shamma using inductively coupled plasma mass spectrometry (ICP-MS). Methods: Thirty-three samples of Shamma (smokeless tobacco) were collected, comprising four types: brown Shamma (n = 14.0), red Shamma (n = 9.0), white Shamma (n = 4.0), and yellow Shamma (n = 6.0). All samples were collected randomly from Shamma users in the city of Najran. Levels of 11 elements (Al, As, Cd, Co, Cr, Cu, Li, Mn, Ni, Pb, and Zn) were determined by ICP-MS. Results: A mixed standard (20 ppb) of all elements was used for quality control, and average recoveries ranged from 74.7% to 112.2%. The highest average concentrations were found in the following order: Al (598.8–812.2 μg/g), Mn (51.0–80.6 μg/g), and Ni (23.2–53.3 μg/g) in all four Shamma types. The lowest concentrations were for As (0.7–1.0 μg/g) and Cd (0.0–0.06 μg/g). Conclusions: The colour of each Shamma type reflects additives mixed into the tobacco. Cr and Cu were showed significant differences (P awareness about the safety and health effects of Shamma, which is clearly a source of oral exposure to metals. Creative Commons Attribution License

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

    International Nuclear Information System (INIS)

    Schlagenhaufen, C.

    1996-08-01

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

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

    International Nuclear Information System (INIS)

    Oliveira, Thiago Cesar de

    2014-01-01

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

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

    International Nuclear Information System (INIS)

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

    2004-01-01

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

  2. An inductively coupled plasma atomic emission spectrometric (ICP-AES) determination of boron and other trace impurities in aluminium metal

    International Nuclear Information System (INIS)

    Deshpande, S.S.; Patil, P.B.; Karanjikar, N.P.

    2002-01-01

    The optimisation and use of ICP-AES technique for the analysis of aluminium metal for B, Cr, Cu, Fe, Mg, Mn, Ni, Si, Ti, V and Zn in the concentration range 5.0 to 50.0 ppm is described. The method involves the dissolution of aluminium metal in acqua-regia. The matrix aluminium solution (2mg/ml) is mixed with composite impurity solution in proper proportions, for getting the required set of standards. JY 1 metre Czerny-Turner Scanning monochromator is used to measure peak intensities corresponding to each analyte wavelength selected. The mean relative standard deviation (RSD) of the method for various elements is found to be 4.0% -2.0% in the concentration range studied. (author)

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

    International Nuclear Information System (INIS)

    Dufailly, Vincent; Noel, Laurent; Guerin, Thierry

    2006-01-01

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

  4. Comparison of digestion procedures used for the determination of boron in biological tissues by ICP-AES [inductively-coupled, plasma-atomic emission spectroscopy

    International Nuclear Information System (INIS)

    Bauer, W.F.; Miller, D.L.; Steele, S.M.

    1988-01-01

    A study was designed to identify the most accurate and reliable procedures for the digestion of biological tissues prior to the determination of boron by inductively-coupled, plasma-atomic emission spectroscopy (ICP-AES). The four procedures used in this study were an acid bomb digestion and digestions performed in test tubes using perchloric acid and hydrogen peroxide, nitric acid and hydrogen peroxide, and nitric acid alone. Digestions using nitric acid and hydrogen peroxide and nitric acid alone were performed in a manner analogous to the perchloric acid/hydrogen peroxide procedure. The tissues used in the study were from dogs that had been administered a boron compound (Na 2 B 12 H 11 SH) and included two brain tissues, a liver and a tongue. These tissues were selected in order to eliminate results that may be due to surface spiking only. None of the test tube procedures were successful in completely dissolving the samples, as was evidenced by residual color and a coagulated precipitate. The amount of precipitate was much larger for the brain tissues in all cases. The acid bomb digestion and the perchloric acid/hydrogen peroxide procedures gave comparable boron concentrations for all of the tissues in this study. 2 refs., 1 tab

  5. Leaching of heavy metals from contaminated soils using inductively coupled plasma optical emission spectrometer (ICP-OES) and atomic absorption spectrometer (AAS)

    International Nuclear Information System (INIS)

    Hussain, Z.; Islam, M.

    2010-01-01

    The clean-up of soils contaminated with heavy metals is one of the most difficult tasks for environmental engineering. Heavy metals are highly persistent in soil and a number of techniques have been developed that aim to remove heavy metals from contaminated soil. A method has been adopted to evaluate dynamic leaching of metal contaminants from industrial soil samples obtained from textile industrial sites in Lahore, Pakistan. In the extraction procedures employed five different leaching liquors were used: 0.01 M CaCl/sub 2/, 1 M HNO/sub 3/, a 1:1 mixture of 0.1M HCl and 0.1M NaCl, 0.01 M EDTA and pH controlled 0.5 M acetic acid. The qualitative and quantitative analyses were carried out by Atomic Absorption Spectroscopy (AAS) and Inductively Coupled Plasma-Optical Emission Spectrometer (ICP-OES). The results indicate that Cu, Zn, Cd, Ni, Pb, Fe and As were extracted in the soil samples in varying concentration when using the different leach liquors. The predominant metals which were leached were As 78.7 ng/ml in 0.01 M EDTA; Zn 1.81 mu g/ml and Fe 898.96 macro g/ml in HNO/sub 3/. (author)

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

    Science.gov (United States)

    2012-01-01

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

  7. Determination of total strontium in uruguayan rice by inductively coupled plasma optical emission spectrometry (ICP-OES

    Directory of Open Access Journals (Sweden)

    Mario E. Rivero Huguet

    2011-04-01

    Full Text Available Strontium (Sr is found naturally as a non-radioactive element and has 16 known isotopes. Naturally occurring Sr is found as four stable isotopes: Sr-84, -86, -87, and -88. Twelve other isotopes are radioactive. Sr-90 is the most important radioactive isotope in the environment, discovered mostly after the nuclear experiments conducted in the 1950s and 1960s. In the present work, 86 rice samples (Oryza saliva L. and 7 rice husk samples were digested by dry ashing for the purpose of determining the total Sr levels by ICP-OES. The mean concentrations found were: 0.281 µg g-1 for milled, 0.287 µg g-1 for parboiled milled, 0.564 µg g-1 for brown, 0.73 µg g-1 for parboiled brown, and 1.16 µg g-1 for paddy rice, and 3.44 µg g-1 for the rice husks. Validation of the method was conducted with a certified reference material, NIST CAM 8418 Wheat Gluten, and the recovery obtained ranged from 89-98%. As the outer layers (aleurone, pericarp of the grain are removed, the Sr concentration decreases. It can then be assumed that most of the Sr is stored in these layers. Although no extensive data exist for Sr levels in rice, the values obtained are in good agreement with the results reported for Sr in brown rice from Japan (0.25-0.72 µg g-1 and with non-contaminated foodstuffs from other parts of the world. Thus, the Uruguayan rice has Sr levels that match non-contaminated samples and its consumption presents no health threat.Publicado en: Atomic Spectroscopy.-- 2006, 27(3:80-85

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2006-04-21

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

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

    Science.gov (United States)

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

    2005-08-15

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

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

    Directory of Open Access Journals (Sweden)

    Renata Brodzka

    2013-04-01

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

  11. Evaluation of analytical procedures for the determination of cadmium, boron and lithium in UALx samples by inductively coupled plasma optical emission spectrometry (ICP OES)

    International Nuclear Information System (INIS)

    Guilhen, Sabine Neusatz; Kakazu, Mauricio H.; Cotrim, Marycel Elena Barboza; Pires, Maria Aparecida Faustino; Souza, Alexandre Luiz de

    2013-01-01

    Used in over 80% of the worldwide diagnostic procedures, Technetium-99m ( 99m Tc), which is obtained from the decay of molybdenum-99 ( 99 Mo), is the most important radioisotope in nuclear medicine. IPEN/CNEN-SP has been developing technologies in order to produce Mo-99 by the irradiation of low-enriched uranium (LEU < 20% of 235U) targets in its research reactor IEA-R1 (IPEN, Sao Paulo/Brazil). These targets consist of low enriched uranium dispersed in a matrix of aluminum (UAlx-Al). Several impurities may be incorporated during the target's production process, such as boron, cadmium and lithium, which have a high capture cross section that may reduce the irradiation's efficiency. This study describes a simple and rapid inductively coupled plasma optical emission spectrometric method for the determination of cadmium, boron and lithium in uranium aluminum (UAlx) dispersion targets. The method involves a previous separation step, in which uranium gets removed from the matrix by chromatographic extraction with the use of a divinylbenzene resin Amberlite XAD - 4 doped with tri-n-butyl phosphate (TBP). TBP selectively separates the uranium, leaving behind the impurities in an aqueous medium for a further quantification by ICP OES. Possible spectroscopic interferences are also discussed in this article, because of the high amount of aluminum in the remaining solution. Experimental and instrumental conditions, such as initial mass, acid solution ratio and amount, resin mass, emission lines and interfering concentrations are carefully established. This method is to be applied for the determination of several others impurities in UAlx in the future, providing means to verify the UAlx targets' compliance to the current established specifications through routine laboratory analysis. (author)

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-09-24

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

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

  14. Determination of the mineral compositions of some selected oil-bearing seeds and kernels using Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES

    Directory of Open Access Journals (Sweden)

    Musa Özcan, M.

    2006-06-01

    Full Text Available The aim of this paper was to establish the mineral contents of oil-bearing seeds and kernels such as peanut, turpentine, walnut, hazelnut, sesame, corn, poppy, almond, sunflower etc., using Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES. Significant differences in mineral composition were observed among crops. All seeds and kernels contained high amounts of Al, Ca, Fe, K, Mg, Na, P and Zn. B, Cr, Cu, Li, Ni, Sr, Ti while V contents of the crops were found to be very low. The levels of K and P of all crops in this study were found to be higher than those of other seeds and kernels. The results obtained from analyses of the crops showed that the mean levels of potassiumcontent ranged from 1701.08 mg/kg (corn to 20895.8 mg/kg (soybean, the average content of phosphorus ranged from 3076.9 mg/kg (turpentine to 12006,5 mg/kg to 2617.4 mg/kg (cotton seed, and Ca from 68.4 mg/kg (corn to 13195.7 mg/kg (poppy seed. The results show that these values may  be useful for the evaluation of dietary information. Particularly the obtained results provide evidence that soybean, pinestone and poppy seed are a good source of K, P and Ca, respectively. Whereas pinestone is a good source of zinc.La finalidad del trabajo es establecer el contenido en elementos minerales de semillas oleaginosas tales como cacahuetes, trementina, avellana, sesamo, maiz, almendras, girasol, utilizando ICP-AES. Se han observado diferencias significativas en la composición de minerales entre cosechas. Todas las semillas contienen cantidades elevadas de Al, Ca, Fe, K, Mg, Na, P y Zn. Los contenidos de B, Cr, Cu, Li, Ni, Sr, Ti y V, sin embargo, fueron bajos. Los contenidos de K y P en todas las semillas estudiadas fueron superiores a las de otras semillas. El contenido medio de K osciló entre 1.701,1 mg/kg (maiz a 20.895,8 mg/kg (soja, el P entre 3.076.9 mg/kg (trementina a 12.006.5 mg/kg o 2.617,4 mg/kg (semilla de algodón, y Ca de 68,4 mg/kg (maiz a 13.195,7 mg

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

    Science.gov (United States)

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

    2003-02-01

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

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

    International Nuclear Information System (INIS)

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

    2003-01-01

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

  17. Study on spatial distribution of plasma parameters in a magnetized inductively coupled plasma

    Energy Technology Data Exchange (ETDEWEB)

    Cheong, Hee-Woon; Lee, Woohyun; Kim, Ji-Won; Whang, Ki-Woong, E-mail: kwhang@snu.ac.kr [Plasma Laboratory, Inter-University Semiconductor Research Center, Department of Electrical and Computer Engineering, Seoul National University, Seoul 151-742 (Korea, Republic of); Kim, Hyuk [Samsung Electronics Co., Banwol-dong, Hwaseong 445-701 (Korea, Republic of); Park, Wanjae [Tokyo Electron Miyagi Ltd., Taiwa-cho, Kurokawa-gun, Miyagi 981-3629 (Japan)

    2015-07-15

    Spatial distributions of various plasma parameters such as plasma density, electron temperature, and radical density in an inductively coupled plasma (ICP) and a magnetized inductively coupled plasma (M-ICP) were investigated and compared. Electron temperature in between the rf window and the substrate holder of M-ICP was higher than that of ICP, whereas the one just above the substrate holder of M-ICP was similar to that of ICP when a weak (<8 G) magnetic field was employed. As a result, radical densities in M-ICP were higher than those in ICP and the etch rate of oxide in M-ICP was faster than that in ICP without severe electron charging in 90 nm high aspect ratio contact hole etch.

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

    International Nuclear Information System (INIS)

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

    2009-01-01

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

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

    Science.gov (United States)

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

    2018-02-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1993-05-01

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

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

    International Nuclear Information System (INIS)

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

    2005-01-01

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

  2. Application of an argon-nitrogen inductively-coupled radiofrequency plasma (ICP) to the analysis of geological and related materials for their rare earth contents

    Science.gov (United States)

    Brenner, I. B.; Watson, A. E.; Steele, T. W.; Jones, E. A.; Goncalves, M.

    An account is given of the development of a procedure for the determination of the rare earth (RE) elements in a large variety of geological materials employing a medium power argon-nitrogen ICP coupled with a 3.4m Ebert spectrograph. The effects of the carrier and intermediate gas flow rates, height of observation and power on RE spectral line intensities have been studied. The line-to-background ratio of the RE analyte was found to increase with observation height and passed through a maximum at 12-14 mm above the top of the work coil. The method eventually developed allows the direct determination of the lanthanides and yttrium at the 50-200 μg g -1 levels using a single solution prepared by fusing 0.2-1 g samples with Na 2O 2 or LiBO 2 and dissolving the melt in 4-10% (v/v) HNO 3, or by treating the samples with HF-HClO 4-HNO 3 mixtures. For lower contents of the RE elements, they can be separated from matrix concomitants by ion exchange employing AG50W-X8 resin. A large variety of silicate and phosphate reference materials was analysed using scandium as the internal standard. The relative standard deviations vary from about 1.5-15%. No matrix effects were observed despite the large compositional variation of the samples analysed.

  3. Infinitely high etch selectivity during CH4/H2/Ar inductively coupled plasma (ICP) etching of indium tin oxide (ITO) with photoresist mask

    International Nuclear Information System (INIS)

    Kim, D.Y.; Ko, J.H.; Park, M.S.; Lee, N.-E.

    2008-01-01

    Under certain conditions during ITO etching using CH 4 /H 2 /Ar inductively coupled plasmas, the etch rate selectivity of ITO to photoresist (PR) was infinitely high because the ITO films continued to be etched, but a net deposition of the α-C:H layer occurred on the top of the PR. Analyses of plasmas and etched ITO surfaces suggested that the continued consumption of the carbon and hydrogen in the deposited α-C:H layer by their chemical reaction with In and Sn atoms in the ITO resulting in the generation of volatile metal-organic etch products and by the ion-enhanced removal of the α-C:H layer presumably play important roles in determining the ITO etch rate and selectivity

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

    Science.gov (United States)

    Jantzi, Sarah C; Almirall, José R

    2014-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, Thiago Cesar de

    2014-06-01

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

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

    International Nuclear Information System (INIS)

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

    2009-01-01

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

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

    International Nuclear Information System (INIS)

    Arslan, Zikri; Paulson, Anthony J.

    2003-01-01

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

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

    Science.gov (United States)

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

    2017-08-01

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

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

    Science.gov (United States)

    2015-04-01

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

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

    Czech Academy of Sciences Publication Activity Database

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

    2013-01-01

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

  11. Hydrodynamic chromatography coupled to single-particle ICP-MS for the simultaneous characterization of AgNPs and determination of dissolved Ag in plasma and blood of burn patients.

    Science.gov (United States)

    Roman, Marco; Rigo, Chiara; Castillo-Michel, Hiram; Munivrana, Ivan; Vindigni, Vincenzo; Mičetić, Ivan; Benetti, Federico; Manodori, Laura; Cairns, Warren R L

    2016-07-01

    Silver nanoparticles (AgNPs) are increasingly used in medical devices as innovative antibacterial agents, but no data are currently available on their chemical transformations and fate in vivo in the human body, particularly on their potential to reach the circulatory system. To study the processes involving AgNPs in human plasma and blood, we developed an analytical method based on hydrodynamic chromatography (HDC) coupled to inductively coupled plasma mass spectrometry (ICP-MS) in single-particle detection mode. An innovative algorithm was implemented to deconvolute the signals of dissolved Ag and AgNPs and to extrapolate a multiparametric characterization of the particles in the same chromatogram. From a single injection, the method provides the concentration of dissolved Ag and the distribution of AgNPs in terms of hydrodynamic diameter, mass-derived diameter, number and mass concentration. This analytical approach is robust and suitable to study quantitatively the dynamics and kinetics of AgNPs in complex biological fluids, including processes such as agglomeration, dissolution and formation of protein coronas. The method was applied to study the transformations of AgNP standards and an AgNP-coated dressing in human plasma, supported by micro X-ray fluorescence (μXRF) and micro X-ray absorption near-edge spectroscopy (μXANES) speciation analysis and imaging, and to investigate, for the first time, the possible presence of AgNPs in the blood of three burn patients treated with the same dressing. Together with our previous studies, the results strongly support the hypothesis that the systemic mobilization of the metal after topical administration of AgNPs is driven by their dissolution in situ. Graphical Abstract Simplified scheme of the combined analytical approach adopted for studying the chemical dynamics of AgNPs in human plasma/blood.

  12. Separation, preconcentration and estimation of rare earth and trace elements by inductively coupled plasma-atomic emission spectrometry (ICP-AES) in thorium matrices

    International Nuclear Information System (INIS)

    Chakraborty, Prithwish; Kumar Vijay; Durani, Smeer; Satyanarayana, K.

    2007-01-01

    A simple, sensitive and efficient method is developed for the separation of Rare earth elements (REEs) La-Lu, and Y and some trace elements Cd, Co, Cr, Cu, Ni,V, Zn from thorium matrix and their subsequent estimations by ICP-AES. In thorium-rich geological samples, the estimation of REE's by ICP-AES suffers from the spectral interferences due to the presence of excess of Th. In the proposed method, thorium is separated from the matrix by the solvent extraction. To optimize the separation, of REEs and trace elements from Th matrix, synthetic mixture solutions was prepared containing Th, REEs and trace elements maintaining different acidic conditions (1M, 2M, 4M, 6M, 8M and 10M HNO 3 and 2M, 4M, 6M and 8M HCl) and each solution was subjected to solvent extraction. The solvent extraction was carried out using a mixture of di-2-ethylhexyl phosphoric acid (in 30 % Toluene) and 1- pentanol in the ratio of 5:1. The aqueous phase containing the required elements was evaporated to dryness and an acidity of 5% HCl is maintained in final volume. Solutions were analysed by ICP-AES and the quantitative recovery of REEs and trace elements were obtained at 6M HNO 3 acidity. The developed method was applied to the certified standard reference material: IGS-36 and the values obtained were comparable with the certified values. The method was also applied to the real time monazite sample and the recovery was quantitative. Corrections have been applied for the REEs inter-elemental interferences in ICP-AES. (author)

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-02-01

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

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

    Science.gov (United States)

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

    2008-11-01

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

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

    International Nuclear Information System (INIS)

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

    2008-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2008-11-15

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-07-16

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

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

  19. Sequential determination of environmental levels of isotopic thorium, uranium and the light rare earth elements within the terrestrial food chain by induced coupled plasma (ICP) and alpha spectrometry

    International Nuclear Information System (INIS)

    Linsalata, P.; Morse, R.; Ford, H.

    1986-01-01

    A radioecological study designed to measure soil to plant and soil to animal (livestock) transfer of Th, U, Ra and the light rare earth elements (REE) in typical and naturally-enhanced radiation environments required the development of radiochemical methods suitable for low-level determinations in a broad suite of environmental matrices including soil, edible vegetables and vegetation, and the major organs and tissues of various livestock. Earlier work has demonstrate the reliability of the methods summarized here for measuring the isotopic thorium and REE content of human feces, and that in the edible portions of various vegetables grown under field conditions. The very high degree of biological discrimination against Th and REE uptake in plants as well as in animal soft tissues necessitated the analysis of typical sample masses of 1-4 kg (fresh weight) to insure reasonably precise (eg., 10-20%) concentration estimates for most of the elements and isotopes of interest. As a result of the ''bone-seeking'' nature and relatively long retention times for these elements in skeletal tissue, typical analytical masses required for analysis of bone range from 40 to 70 g (fresh weight) except for the REE's in which a larger aliquot is recommended when determination is by induced coupled plasma spectrometry

  20. Inductively coupled plasma source mass spectrometry

    International Nuclear Information System (INIS)

    Price Russ, G. III

    1993-01-01

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

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

    International Nuclear Information System (INIS)

    Pedreira Filho, Walter dos Reis

    2000-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2013-07-01

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

  3. Determination of lead by hydride generation inductively coupled plasma mass spectrometry (HG-ICP-MS): On-line generation of plumbane using potassium hexacyanomanganate(III)

    Energy Technology Data Exchange (ETDEWEB)

    Yilmaz, Vedat [Jackson State University, Department of Chemistry and Biochemistry, Jackson, MS 39217 (United States); Erciyes University, Faculty of Pharmacy, Department of Analytical Chemistry, 38039 Kayseri (Turkey); Arslan, Zikri, E-mail: zikri.arslan@jsums.edu [Jackson State University, Department of Chemistry and Biochemistry, Jackson, MS 39217 (United States); Rose, LaKeysha [Jackson State University, Department of Chemistry and Biochemistry, Jackson, MS 39217 (United States)

    2013-01-25

    Highlights: Black-Right-Pointing-Pointer Potassium hexacyanomanganate(III), (K{sub 3}Mn(CN){sub 6}, was utilized first time for hydride generation (HG). Black-Right-Pointing-Pointer Hexacyanomanganate(III) promoted generation of lead hydride (PbH{sub 4}) remarkably. Black-Right-Pointing-Pointer The HG method using K{sub 3}Mn(CN){sub 6} enhanced sensitivity by at least 40-fold. Black-Right-Pointing-Pointer The method detection limits for Pb were as low as 8 ng L{sup -1} by ICP-MS. Black-Right-Pointing-Pointer The method is highly suitable for quantitative determination of Pb in various samples and salt matrices by ICP-MS. - Abstract: A hydride generation (HG) procedure has been described for determination of Pb by ICP-MS using potassium hexacyanomanganate(III), K{sub 3}Mn(CN){sub 6}, as an additive to facilitate the generation of plumbane (PbH{sub 4}). Potassium hexacyanomanganate(III) was prepared in acidic medium as it was unstable in water. The stability of hexacyanomanganate(III) was examined in dilute solutions of HCl, HNO{sub 3} and H{sub 2}SO{sub 4}. The solutions prepared in 1% v/v H{sub 2}SO{sub 4} were found to be stable for over a period of 24 h. The least suitable medium was 1% v/v HNO{sub 3}. For generation of plumbane, acidic hexacyanomanganate(III) and sample solutions were mixed on-line along a 5-cm long tygon tubing (1.14 mm i.d.) and then reacted with 2% m/v sodium borohydride (NaBH{sub 4}). A concentration of 0.5% m/v K{sub 3}Mn(CN){sub 6} facilitated the generation of PbH{sub 4} remarkably. In comparison to H{sub 2}SO{sub 4}, HCl provided broader working range for which optimum concentration was 1% v/v. No significant interferences were noted from transition metals and hydride forming elements, up to 0.5 {mu}g mL{sup -1} levels, except Cu which depressed the signals severely. The depressive effects in the presence of 0.1 {mu}g mL{sup -1} Cu were alleviated by increasing the concentration of K{sub 3}Mn(CN){sub 6} to 2% m/v. Under these conditions

  4. Simultaneous measurement of 239Pu, 240Pu, 241Pu, and 242Pu by high resolution inductively coupled plasma mass spectrometer (HR ICP-MS) in marine sediments

    International Nuclear Information System (INIS)

    Bruneau, F.

    1999-01-01

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

  5. Monitoring and assessment of heavy metal/metalloid concentration by inductively coupled plasma mass spectroscopy (ICP-MS) method in Gonyeli Lake, Cyprus.

    Science.gov (United States)

    Alkas, Fehmi Burak; Shaban, Jehad Abdullah; Sukuroglu, Ayca Aktas; Kurt, Mehmet Ali; Battal, Dilek; Saygi, Sahan

    2017-09-22

    The presence of heavy metals/metalloids in the ecosystem has been an increasing ecological and global public health concern due to their potential to cause adverse health effects. For this reason, the accumulation of some heavy metals such as Cr, Mn, Ni, Cu, As, Cd, Pb was assessed by way of ICP-MS in water, sediment and fish (Cyprinus carpio) sampled from Gonyeli Lake, North Cyprus. The results showed that these metals/metalloids are found widespread throughout the study area. In water, most concentrated element was manganese with 92.1 ppb and least concentrated was lead with 0.914 ppb. In sediment, copper had the highest concentration with 613 ppm, and cadmium the lowest with 1.57 ppm. In fish tissues (muscle and gills), the most concentrated element was manganese with 12.5 ppm and the least concentrated cadmium with 0.017 ppm. These results indicate that future remediation efforts are indispensable for the rehabilitation of the lake.

  6. [Determination of ru, rh and Pd in 30% trialkyl phosphine oxide (TRPO)-kerosene by inductively coupled plasma-atomic emission spectrum (ICP-AES)].

    Science.gov (United States)

    Wang, Jian-Chen; Zhang, Lin

    2013-07-01

    The determination method of Ru, Rh and Pd in 30% TRPO-kerosene ICP-AES was studied by using aqueous calibration reference solution and choosing ethanol as diluent. The effects of the contents of 30% TRPO-kerosene and aqueous solution and the concentration of HNO3 in 30% TRPO-kerosene on the intensities of Ru, Rh and Pd were described. The optimized condition for preparing samples and calibration solutions was chosen as follows: The contents of 30% TRPO-kerosene and aqueous phase were 10% (V/V) and 5% (V/V) respectively and the concentration of HNO3 30% TRPO-kerosene was 0.20 mol x L(-1). The determination method of Au, Ru and Pd was set up according to the above condition. The detection limit, precision and recovery ratio of Ru, Rh and Pd are well. The method is not only used in determination of Au, Ru and Pd in 30% TRPO-kerosene, but also used in other organic phases.

  7. A Comparative Study of Selected Trace Element Content in Malay and Chinese Traditional Herbal Medicine (THM Using an Inductively Coupled Plasma-Mass Spectrometer (ICP-MS

    Directory of Open Access Journals (Sweden)

    Sharifah Mohamad

    2013-02-01

    Full Text Available A total of 60 products of traditional herbal medicine (THM in various dosage forms of herbal preparation were analyzed to determine selected trace elements (i.e., Zn, Mn, Cu, Cd, and Se using ICP-MS. Thirty types of both Chinese and Malay THMs were chosen to represent each population. The closed vessel acid microwave digestion method, using CEM MARS 5, was employed for the extraction of the selected trace elements. The digestion method applied was validated by using certified reference material from the Trace Element in Spinach Leaves (SRM1570a. The recoveries of all elements were found to be in the range of 85.3%–98.9%. The results indicated that Zn, Mn, Cu, Cd and Se have their own trends of concentrations in all samples studied. The daily intake concentrations of the elements were in the following order: Mn > Zn > Cu > Se > Cd. Concentrations of all five elements were found to be dominant in Chinese THMs. The essentiality of the selected trace elements was also assessed, based on the recommended daily allowance (RDA, adequate intake (AI and the United States Pharmacopeia (USP for trace elements as reference. The concentrations of all elements studied were below the RDA, AI and USP values, which fall within the essential concentration range, except for cadmium.

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

    International Nuclear Information System (INIS)

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

    2001-01-01

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

  9. Inductively coupled plasma- mass spectrometry. Chapter 13

    International Nuclear Information System (INIS)

    Mahalingam, T.R.

    1997-01-01

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

  10. Electrolytic dissolution of aluminium alloys (chip form) and mullet-element determination by inductively coupled plasma optical emission spectrometry (ICP-OES)

    International Nuclear Information System (INIS)

    Grigoletto, Tania

    2001-01-01

    Several aluminum alloys with different chip's size were dissolved using aqua regia (HCl:HN0 3 ,3:1). The residues of the dissolution procedure were either rejected or used in silicon volatilization with hydrofluoric acid before determination of Fe, Cu, Mn, Mg, Cr, Ni, Zn, Pb, Sn, Ti and Zr by ICP-OES. The influence caused by crescent amounts of aluminum in the determination of other elements and the probable spectral interference by Cu in determination of Zn (with or without electrolytic separation of Cu) was evaluated. The electrolytic dissolution of aluminum alloys was performed by pressing chips against a platinum electrode for the electrolysis to occur, so that way the chips behaved as the anode. A tube (body of syringe of 2.5 mL) with perforations around the open base was used to contain the sample and Pt electrode. The alloy was placed on synthetic wool (perlon) in this tube. An acrylic dowel with a platinum wire across its interior was fixed in the superior part a tube with Teflon film, with an orifice through which the electrolytic solution flowed (HNO 3 1 mol L -1 ; 4.5 mL min -1 ). A platinum dish was fixed at the inferior extremity of the platinum wire to press the sample. The solution came out through the inferior orifices of the tube to a flask, from where it was again captured (with a peristaltic pump) to go into the superior part of the tube. In this flask, a Pt wire cathode was also placed. A current of 0.6 A and ten minutes of electrolysis provided good results. Due to the partial dissolution, the knowledge of percentages of previous elements analyzed after total dissolution, or using certified reference material are necessary. The results were normalized by knowledge percentages. The calculations were made by the ratio between the concentration of the element determined, with the determined concentration of aluminum; the ratio between concentration of the element and the sum of the concentrations of the elements determined, including Al; the ratio

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

    International Nuclear Information System (INIS)

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

    2008-01-01

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

  12. Study on the RF power necessary to ignite plasma for the ICP test facility at HUST

    Energy Technology Data Exchange (ETDEWEB)

    Yue, Haikun [School of Electronic Information and Communications, Huazhong University of Science and Technology, Wuhan (China); State Key Laboratory of Advanced Electromagnetic Engineering and Technology, Huazhong University of Science and Technology, Wuhan (China); Li, Dong; Wang, Chenre; Li, Xiaofei; Chen, Dezhi; Liu, Kaifeng; Zhou, Chi; Pan, Ruimin [State Key Laboratory of Advanced Electromagnetic Engineering and Technology, Huazhong University of Science and Technology, Wuhan (China)

    2015-10-15

    An Radio-Frequency (RF) Inductively Coupled Plasma (ICP) ion source test facility has been successfully developed at Huazhong University of Science and Technology (HUST). As part of a study on hydrogen plasma, the influence of three main operation parameters on the RF power necessary to ignite plasma was investigated. At 6 Pa, the RF power necessary to ignite plasma influenced little by the filament heating current from 5 A to 9 A. The RF power necessary to ignite plasma increased rapidly with the operation pressure decreasing from 8 Pa to 4 Pa. The RF power necessary to ignite plasma decreased with the number of coil turns from 6 to 10. During the experiments, plasma was produced with the electron density of the order of 10{sup 16}m{sup -3} and the electron temperature of around 4 eV. (copyright 2015 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

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

    Directory of Open Access Journals (Sweden)

    Gardolinski Paulo C. F. C.

    2002-01-01

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

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

    Science.gov (United States)

    Arslan, Zikri; Oymak, Tulay; White, Jeremy

    2018-05-30

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

  15. Using laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) to explore geochemical taphonomy of vertebrate fossils in the upper cretaceous two medicine and Judith River formations of Montana

    Science.gov (United States)

    Rogers, R.R.; Fricke, H.C.; Addona, V.; Canavan, R.R.; Dwyer, C.N.; Harwood, C.L.; Koenig, A.E.; Murray, R.; Thole, J.T.; Williams, J.

    2010-01-01

    Laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) was used to determine rare earth element (REE) content of 76 fossil bones collected from the Upper Cretaceous (Campanian) Two Medicine (TMF) and Judith River (JRF) Formations of Montana. REE content is distinctive at the formation scale, with TMF samples exhibiting generally higher overall REE content and greater variability in REE enrichment than JRF samples. Moreover, JRF bones exhibit relative enrichment in heavy REE, whereas TMF bones span heavy and light enrichment fields in roughly equal proportions. TMF bones are also characterized by more negative Ce anomalies and greater U enrichment than JRF bones, which is consistent with more oxidizing diagenetic conditions in the TMF. Bonebeds in both formations show general consistency in REE content, with no indication of spatial or temporal mixing within sites. Previous studies, however, suggest that the bonebeds in question are attritional assemblages that accumulated over considerable time spans. The absence of geochemical evidence for mixing is consistent with diagenesis transpiring in settings that remained chemically and hydrologically stable during recrystallization. Lithology-related patterns in REE content were also compared, and TMF bones recovered from fluvial sandstones show relative enrichment in heavy REE when compared with bones recovered from fine-grained floodplain deposits. In contrast, JRF bones, regardless of lithologic context (sandstone versus mudstone), exhibit similar patterns of REE uptake. This result is consistent with previous reconstructions that suggest that channel-hosted microfossil bonebeds of the JRF developed via the reworking of preexisting concentrations embedded in the interfluve. Geochemical data further indicate that reworked elements were potentially delivered to channels in a recrystallized condition, which is consistent with rapid adsorption of REE postmortem. Copyright ?? 2010, SEPM (Society for

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

    International Nuclear Information System (INIS)

    Beuvier, Ludovic

    2015-01-01

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

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

    Science.gov (United States)

    2016-02-29

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

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

    International Nuclear Information System (INIS)

    Fabien Pointurier; Amelie Hubert; Anne-Claire Pottin

    2013-01-01

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

  19. Flow injection analysis in inductively coupled plasma spectrometry

    International Nuclear Information System (INIS)

    Rosias, Maria F.G.G.

    1995-10-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Bruneau, F

    1999-07-01

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

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

    Science.gov (United States)

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

    2017-05-22

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

  2. Characterisation of spent nuclear fuels by an on-line coupled HPLC-ICP-MS system

    International Nuclear Information System (INIS)

    Guenther-Leopold, I.; Gabler, F.; Wernli, B.; Kopajtic, Z.

    2000-01-01

    The determination of burn-up is one of the essential components of post-irradiation examination of nuclear fuel samples. In the framework of the ARIANE programme (Actinides Research in a Nuclear Element), at PSI the analysis of the isotopic vectors of uranium, plutonium, neodymium and some other fission and spallation products was carried out for the first time in the Hot Lab using high-performance liquid chromatography (HPLC), coupled on-line with an inductively coupled plasma mass spectrometer (ICP-MS). The results of these investigations, a comparison with the classical technique for burn-up determination, the advantages and limitations of the new method, the accuracy and precision of these types of analyses, the applicability of the technique to other samples and separation problems, and conclusions for further analyses of nuclear fuel samples, are here presented. (authors)

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

    Science.gov (United States)

    Farnsworth, Paul B.; Spencer, Ross L.

    2017-08-01

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

  4. Diagnostic studies of ion beam formation in inductively coupled plasma

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-01-01

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

  5. 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).

    Science.gov (United States)

    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.

  6. Ion deposition by inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Hu, K.; Houk, R.S.

    1996-01-01

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

  7. Training course on inductively coupled plasma spectrometry - Note

    Digital Repository Service at National Institute of Oceanography (India)

    Valsangkar, A.B.

    TRAINING COURSE ON INDUCTIVELY COUPLED PLASMA SPECTROMETRY In the present day geological, chemical, environmental and archaeological research activities, the Inductively Coupled Plasma (ICP) Spectrometry is established as a cost-effective multi... the knowledge and advances in the analytical tools and methodologies for the benefit of the research scholars as well as professionals. National Institute of Oceanography, A.B. VALSANGKAR Dona Paula - 403 004 slip tectonics playing a major role...

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

    DEFF Research Database (Denmark)

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

    2016-01-01

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

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

    DEFF Research Database (Denmark)

    Gammelgaard, B.; Larsen, Erik Huusfeldt

    1998-01-01

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

  10. Stirring Strongly Coupled Plasma

    CERN Document Server

    Fadafan, Kazem Bitaghsir; Rajagopal, Krishna; Wiedemann, Urs Achim

    2009-01-01

    We determine the energy it takes to move a test quark along a circle of radius L with angular frequency w through the strongly coupled plasma of N=4 supersymmetric Yang-Mills (SYM) theory. We find that for most values of L and w the energy deposited by stirring the plasma in this way is governed either by the drag force acting on a test quark moving through the plasma in a straight line with speed v=Lw or by the energy radiated by a quark in circular motion in the absence of any plasma, whichever is larger. There is a continuous crossover from the drag-dominated regime to the radiation-dominated regime. In the crossover regime we find evidence for significant destructive interference between energy loss due to drag and that due to radiation as if in vacuum. The rotating quark thus serves as a model system in which the relative strength of, and interplay between, two different mechanisms of parton energy loss is accessible via a controlled classical gravity calculation. We close by speculating on the implicati...

  11. Study on water-sediment interaction in samples from Rio das Velhas - Minas Gerais State - Brazil using instrumental neutron activation analysis, and argon plasma coupled mass spectroscopy; Estudo da interacao agua-sedimento em amostras do Rio das Velhas - MG utilizando os metodos: analise por ativacao neutronica instrumental (INAA) e espectrometria de massa acoplada a um plasma de argonio (ICP-MS)

    Energy Technology Data Exchange (ETDEWEB)

    Veado, Maria Adelaide R.V.; Oliveira, Arno H. de [Minas Gerais Univ., Belo Horizonte, MG (Brazil). Dept. de Engenharia Nuclear; Revel, G.; Pinte, G. [CEA Centre d`Etudes Nucleaires de Saclay, 91 - Gif-sur-Yvette (France). Lab. d`Analyse par Activation Pierre Sue; Toulhoat, P. [CEA Centre d`Etudes Nucleaires de Saclay, 91 - Gif-sur-Yvette (France). Unite Mixte de Recherche Analyse et Environnement

    1999-11-01

    Sorption of the metallic elements in aqueous solutions in surface of the hydroxides affects the transport of heavy elements in the freshwaters. Sorption and the chemistry of the hydroxides are important studies for knowledge in geology, waters and waste treatment, and environment studies. In the industrial mining region areas, the river surface waters are subject to modifications in its physical and chemistries properties: pH, DBO, conductivity and alkalinity. Instrumental neutron activation analysis and inductively coupled plasma-mass spectrometry (ICP-MS), have ben used for the determination of toxic heavy metals and others pollutants in the Das Velhas river in State of Minas Gerais, in south-east Brazil. Water samples were collected with acidification on site, which provoked a change of its natural pH. Consequently, metallic elements associated to hydroxides and to particles in suspension were liberated. The objective of this paper is to show the different behavior of any elements, in water of Das Velhas river, with relation of its chemical forms (cations or anions), the solubility degree, the pH and the presence of rare earth elements. (author) 11 refs., 10 figs.; e-mail: adelaide at nuclear.ufmg.br; heeren at nuclear.ufmg.br; grevel at drecam.cea.fr; pierre.toulhoat at cea.fr

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

    Science.gov (United States)

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

    2004-10-01

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

  13. Effect of antenna capacitance on the plasma characteristics of an internal linear inductively coupled plasma system

    International Nuclear Information System (INIS)

    Lim, Jong Hyeuk; Kim, Kyong Nam; Park, Jung Kyun; Yeom, Geun Young

    2008-01-01

    This study examined the effect of the antenna capacitance of an inductively coupled plasma (ICP) source, which was varied using an internal linear antenna, on the electrical and plasma characteristics of the ICP source. The inductive coupling at a given rf current increased with decreasing antenna capacitance. This was caused by a decrease in the inner copper diameter of the antenna made from coaxial copper/quartz tubing, which resulted in a higher plasma density and lower plasma potential. By decreasing the diameter of the copper tube from 25 to 10 mm, the plasma density of a plasma source size of 2750x2350 mm 2 was increased from approximately 8x10 10 /cm 3 to 1.5x10 11 /cm 3 at 15 mTorr Ar and 9 kW of rf power

  14. Method validation in plasma source optical emission spectroscopy (ICP-OES) - From samples to results

    International Nuclear Information System (INIS)

    Pilon, Fabien; Vielle, Karine; Birolleau, Jean-Claude; Vigneau, Olivier; Labet, Alexandre; Arnal, Nadege; Adam, Christelle; Camilleri, Virginie; Amiel, Jeanine; Granier, Guy; Faure, Joel; Arnaud, Regine; Beres, Andre; Blanchard, Jean-Marc; Boyer-Deslys, Valerie; Broudic, Veronique; Marques, Caroline; Augeray, Celine; Bellefleur, Alexandre; Bienvenu, Philippe; Delteil, Nicole; Boulet, Beatrice; Bourgarit, David; Brennetot, Rene; Fichet, Pascal; Celier, Magali; Chevillotte, Rene; Klelifa, Aline; Fuchs, Gilbert; Le Coq, Gilles; Mermet, Jean-Michel

    2017-01-01

    Even though ICP-OES (Inductively Coupled Plasma - Optical Emission Spectroscopy) is now a routine analysis technique, requirements for measuring processes impose a complete control and mastering of the operating process and of the associated quality management system. The aim of this (collective) book is to guide the analyst during all the measurement validation procedure and to help him to guarantee the mastering of its different steps: administrative and physical management of samples in the laboratory, preparation and treatment of the samples before measuring, qualification and monitoring of the apparatus, instrument setting and calibration strategy, exploitation of results in terms of accuracy, reliability, data covariance (with the practical determination of the accuracy profile). The most recent terminology is used in the book, and numerous examples and illustrations are given in order to a better understanding and to help the elaboration of method validation documents

  15. Atlas of atomic spectral lines of plutonium emitted by an inductively coupled plasma

    Energy Technology Data Exchange (ETDEWEB)

    Edelson, M.C.; DeKalb, E.L.; Winge, R.K.; Fassel, V.A.

    1986-09-01

    Optical emission spectra from high-purity Pu-242 were generated with a glovebox-enclosed inductively coupled plasma (ICP) source. Spectra covering the 2280 to 7008 Angstrom wavelength range are presented along with general commentary on ICP-Pu spectroscopy.

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

    Science.gov (United States)

    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.

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

    International Nuclear Information System (INIS)

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

    2016-09-01

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

  18. A comprehensive study of different gases in inductively coupled plasma torch operating at one atmosphere

    International Nuclear Information System (INIS)

    Punjabi, Sangeeta B.; Joshi, N. K.; Mangalvedekar, H. A.; Lande, B. K.; Das, A. K.; Kothari, D. C.

    2012-01-01

    A numerical study is done to understand the possible operating regimes of RF-ICP torch (3 MHz, 50 kW) using different gases for plasma formation at atmospheric pressure. A two dimensional numerical simulation of RF-ICP torch using argon, nitrogen, oxygen, and air as plasma gas has been investigated using computational fluid dynamic (CFD) software fluent (c) . The operating parameters varied here are central gas flow, sheath gas flow, RF-power dissipated in plasma, and plasma gas. The temperature contours, flow field, axial, and radial velocity profiles were investigated under different operating conditions. The plasma resistance, inductance of the torch, and the heat distribution for various plasma gases have also been investigated. The plasma impedance of ICP torch varies with different operating parameters and plays an important role for RF oscillator design and power coupling. These studies will be useful to decide the design criteria for ICP torches required for different material processing applications.

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

    International Nuclear Information System (INIS)

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

    1991-01-01

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

  20. Instabilities in strongly coupled plasmas

    CERN Document Server

    Kalman, G J

    2003-01-01

    The conventional Vlasov treatment of beam-plasma instabilities is inappropriate when the plasma is strongly coupled. In the strongly coupled liquid state, the strong correlations between the dust grains fundamentally affect the conditions for instability. In the crystalline state, the inherent anisotropy couples the longitudinal and transverse polarizations, and results in unstable excitations in both polarizations. We summarize analyses of resonant and non-resonant, as well as resistive instabilities. We consider both ion-dust streaming and dust beam-plasma instabilities. Strong coupling, in general, leads to an enhancement of the growth rates. In the crystalline phase, a resonant transverse instability can be excited.

  1. SU-8 etching in inductively coupled oxygen plasma

    DEFF Research Database (Denmark)

    Rasmussen, Kristian Hagsted; Keller, Stephan Sylvest; Jensen, Flemming

    2013-01-01

    Structuring or removal of the epoxy based, photo sensitive polymer SU-8 by inductively coupled plasma reactive ion etching (ICP-RIE) was investigated as a function of plasma chemistry, bias power, temperature, and pressure. In a pure oxygen plasma, surface accumulation of antimony from the photo......-initiator introduced severe roughness and reduced etch rate significantly. Addition of SF6 to the plasma chemistry reduced the antimony surface concentration with lower roughness and higher etch rate as an outcome. Furthermore the etch anisotropy could be tuned by controlling the bias power. Etch rates up to 800 nm...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-06-01

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

  3. Quantification of pharmaceutical peptides in human plasma by LC-ICP-MS sulfur detection

    DEFF Research Database (Denmark)

    Møller, Laura Hyrup; Macherius, André; Hansen, Thomas Hesselhøj

    2016-01-01

    A method for quantification of a pharmaceutical peptide in human plasma was developed using gradient elution LC-ICP-MS. A membrane desolvation (MD) system was applied to remove organic solvents from the eluent prior to the detection as SO+ in the dynamic reaction cell (DRC) of the ICP-DRC-MS inst......A method for quantification of a pharmaceutical peptide in human plasma was developed using gradient elution LC-ICP-MS. A membrane desolvation (MD) system was applied to remove organic solvents from the eluent prior to the detection as SO+ in the dynamic reaction cell (DRC) of the ICP......-DRC-MS instrument and subsequent quantification by post-column isotope dilution (IDA). Plasma proteins were precipitated prior to analysis. Analytical figures of merit including linearity, precision, LOD, LOQ and accuracy were considered satisfactory for analysis of plasma samples. The selectivity of the developed...... method was demonstrated for five pharmaceutically relevant peptides: desmopressin, penetratin, substance P, PTH (1-34) and insulin. Preliminary experiments on an ICP-MS/MS system using oxygen to reduce the effect of organic solvents were also performed to compare sensitivity. The results of the study...

  4. AETHER: A simulation platform for inductively coupled plasma

    Energy Technology Data Exchange (ETDEWEB)

    Turkoz, Emre, E-mail: emre.turkoz@boun.edu.tr; Celik, Murat

    2015-04-01

    An in-house code is developed to simulate the inductively coupled plasma (ICP). The model comprises the fluid, electromagnetic and transformer submodels. Fluid equations are solved to evaluate the plasma flow parameters, including the plasma and neutral densities, ion and neutral velocities, electron flux, electron temperature, and electric potential. The model relies on the ambipolar approximation and offers the evaluation of plasma parameters without solving the sheath region. The electromagnetic model handles the calculation of the electric and magnetic fields using the magnetic vector potential. The transformer model captures the effect of the matching circuit utilized in laboratory experiments for RF power deposition. The continuity and momentum equations are solved using finite volume method. The energy, electric potential, and magnetic vector potential equations are solved using finite difference method. The resulting linear systems of equations are solved with iterative solvers including Jacobi and GMRES. The code is written using the C++ programming language, it works in parallel and has graphical user interface. The model is applied to study ICP characteristics of a plasma confined within a cylindrical chamber with dielectric walls for two different power deposition cases. The results obtained from the developed model are verified using the plasma module of COMSOL Multiphysics. The model is also applied to a plasma source configuration, and it is demonstrated that there is an overall increase in the plasma potential when current is extracted from ICP with a biased wall electrode.

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

    International Nuclear Information System (INIS)

    Zahran, N. F.

    2004-01-01

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

  6. Matrix effects in inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Chen, Xiaoshan.

    1995-01-01

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

  7. High-performance liquid chromatography and inductively coupled plasma mass spectrometry (HPLC-ICP-MS) for the analysis of xenobiotic metabolites in rat urine: application to the metabolites of 4-bromoaniline.

    Science.gov (United States)

    Nicholson, J K; Lindon, J C; Scarfe, G; Wilson, I D; Abou-Shakra, F; Castro-Perez, J; Eaton, A; Preece, S

    2000-02-01

    The use of HPLC-ICP-MS for the profiling and quantification of the metabolites of 4-bromoaniline following reversed-phase gradient chromatography is demonstrated. In the 0-8 h post dose sample, which contained the highest concentrations of compound-related material, it was possible to detect at least 16 metabolites of the compound. The methodology described offers the possibility of obtaining metabolite profiles and quantification for drugs and other xenobiotics in biological fluids and excreta without the requirement for radiolabelled tracers.

  8. Analysis of biogenic carbonates by inductively coupled plasma-mass spectrometry (ICP-MS). Flow injection on-line solid-phase preconcentration for trace element determination in fish otoliths.

    Science.gov (United States)

    Arslan, Z; Paulson, A J

    2002-04-01

    The aragonite deposits within the ear bones (otoliths) of teleost fish retain a chemical signal reflecting the life history of fish (similar to rings of trees) and the nature of fish habitats. Otoliths dissolved in acid solutions contain high concentrations of calcium and a variety of proteins. Elimination of matrix salts and organic interferences during preconcentration is essential for accurate determination of trace elements in otolith solutions by inductively coupled plasma-quadrupole mass spectrometry. An iminodiacetate-based chelating resin (Toyopearl AF-Chelate 650 M) has been used for on-line preconcentration and matrix separation for the determination of 31 transition and rare elements. Successful preconcentration of the elements was achieved at pH 5 by on-line buffering, except Mn which required pH 8.8. Sample solutions were loaded on to the column for 1 min at 3.2 mL min(-1), and then eluted directly into the mass spectrometer with 4% v/v nitric acid. This procedure enabled up to 25-fold preconcentration with successful removal of the calcium matrix. The effect of heat-assisted oxidation with concentrated nitric acid was investigated to eliminate the organic matrix. It was found that heating to dryness after dissolution and further mineralization with the acid significantly improved the retention of the transition elements. The method was validated by analysis of a certified reference material produced from saggittal otoliths of emperor snapper ( Lutjanus sebae), and then applied to the determination of trace metal concentrations in juvenile bluefin tuna ( Thunnus thynnus) from the Western Pacific Ocean.

  9. Atomic fluorescence spectrometry with the inductively coupled plasma

    International Nuclear Information System (INIS)

    Omenetto, N.; Winefordner, J.D.

    1987-01-01

    Atomic fluorescence spectrometry (AFS) is based on the radiational activation of atoms and ions produced in a suitable atomizer (ionizer) and the subsequent measurement of the resulting radiational deactivation, called fluorescence. Atomic fluorescence spectrometry has been of considerable interest to researchers in atomic spectrometry because of its use for both analytical and diagnostic purposes. Unfortunately, the analytical applications of AFS have suffered from the lack of commercial instrumentation until the recent marketing of the Baird multiple-element, hollow cathode lamp-excited inductively coupled plasma system. This chapter is concerned strictly with the use of the inductively coupled plasma (ICP) as a cell and as a source for AFS. Many of the major references concerning the ICP in analytical AFS are categorized in Table 9.1, along with several reviews and diagnostical studies. For more detailed discussions of the fundamental aspects of AFS, the reader is referred to previous reviews

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

    International Nuclear Information System (INIS)

    Becker, Johanna Sabine

    2002-01-01

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

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

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2005-01-01

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

  12. Determination of methylmercury and estimation of total mercury in seafood using high performance liquid chromatography (HPLC) and inductively coupled plasma-mass spectrometry (ICP-MS): Method development and validation

    Energy Technology Data Exchange (ETDEWEB)

    Hight, Susan C. [Elemental Research Branch, Center for Food Safety and Applied Nutrition, US Food and Drug Administration, 5100 Paint Branch Parkway, College Park, MD 20740-3835 (United States)]. E-mail: susan.hight@fda.gov; Cheng, John [Elemental Research Branch, Center for Food Safety and Applied Nutrition, US Food and Drug Administration, 5100 Paint Branch Parkway, College Park, MD 20740-3835 (United States)]. E-mail: john.cheng@fda.gov

    2006-05-17

    A method was developed for determination of methylmercury and estimation of total mercury in seafood. Mercury (Hg) compounds were extracted from 0.5 g edible seafood or 0.2 g lyophilized reference material by adding 50 ml aqueous 1% w/v L-cysteine.HCl.H{sub 2}O and heating 120 min at 60 deg. C in glass vials. Hg compounds in 50 {mu}l of filtered extract were separated by reversed-phase high performance liquid chromatography using a C-18 column and aqueous 0.1% w/v L-cysteine.HCl.H{sub 2}O + 0.1% w/v L-cysteine mobile phase at room temperature and were detected by inductively coupled plasma-mass spectrometry at mass-to-charge ratio 202. Total Hg was calculated as the mathematical sum of methyl and inorganic Hg determined in extracts. For seafoods containing 0.055-2.78 mg kg{sup -1} methylmercury and 0.014-0.137 mg kg{sup -1} inorganic Hg, precision of analyses was {<=}5% relative standard deviation (R.S.D.) for methylmercury and {<=}9% R.S.D. for inorganic Hg. Recovery of added analyte was 94% for methylmercury and 98% for inorganic Hg. Methyl and total Hg results for reference materials agreed with certified values. Limits of quantitation were 0.007 mg kg{sup -1} methylmercury and 0.005 mg kg{sup -1} inorganic Hg in edible seafood and 0.017 mg kg{sup -1} methylmercury and 0.012 mg kg{sup -1} inorganic Hg in lyophilized reference materials. Evaluation of analyte stability demonstrated that L-cysteine both stabilized and de-alkylated methylmercury, depending on holding time and cysteine concentration. Polypropylene adversely affected methylmercury stability. Total Hg results determined by this method were equivalent to results determined independently by cold vapour-atomic absorption spectrometry. Methylmercury was the predominant form of Hg in finfish. Ratios of methylmercury/total Hg determined by this method were 93-98% for finfish and 38-48% for mollusks.

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

    CSIR Research Space (South Africa)

    Archer, M

    2003-12-01

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

  14. Efficient generation of volatile cadmium species using Ti(III) and Ti(IV) and application to determination of cadmium by cold vapor generation inductively coupled plasma mass spectrometry (CVG-ICP-MS)†

    Science.gov (United States)

    Arslan, Zikri; Yilmaz, Vedat; Rose, LaKeysha

    2015-01-01

    In this study, a highly efficient chemical vapor generation (CVG) approach is reported for determination of cadmium (Cd). Titanium (III) and titanium (IV) were investigated for the first time as catalytic additives along with thiourea, L-cysteine and potassium cyanide (KCN) for generation of volatile Cd species. Both Ti(III) and Ti(IV) provided the highest enhancement with KCN. The improvement with thiourea was marginal (ca. 2-fold), while L-cysteine enhanced signal slightly only with Ti(III) in H2SO4. Optimum CVG conditions were 4% (v/v) HCl + 0.03 M Ti(III) + 0.16 M KCN and 2% (v/v) HNO3 + 0.03 M Ti(IV) + 0.16 M KCN with a 3% (m/v) NaBH4 solution. The sensitivity was improved about 40-fold with Ti(III) and 35-fold with Ti(IV). A limit of detection (LOD) of 3.2 ng L−1 was achieved with Ti(III) by CVG-ICP-MS. The LOD with Ti(IV) was 6.4 ng L−1 which was limited by the blank signals in Ti(IV) solution. Experimental evidence indicated that Ti(III) and Ti(IV) enhanced Cd vapor generation catalytically; for best efficiency mixing prior to reaction with NaBH4 was critical. The method was highly robust against the effects of transition metal ions. No significant suppression was observed in the presence of Co(II), Cr(III), Cu(II), Fe(III), Mn(II), Ni(II) and Zn(II) up to 1.0 μg mL−1. Among the hydride forming elements, no interference was observed from As(III) and Se(IV) at 0.5 μg mL−1 level. The depressive effects from Pb(II) and Sb(III) were not significant at 0.1 μg mL−1 while those from Bi(III) and Sn(II) were marginal. The procedures were validated with determination of Cd by CVG-ICP-MS in a number certified reference materials, including Nearshore seawater (CASS-4), Bone ash (SRM 1400), Dogfish liver (DOLT-4), Mussel tissue (SRM 2976) and Domestic Sludge (SRM 2781). PMID:26251554

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

    DEFF Research Database (Denmark)

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

    2001-01-01

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

  16. Development of a low-cost inductively coupled argon plasma

    International Nuclear Information System (INIS)

    Ripson, P.A.M.

    1983-01-01

    The aim of this investigation is to drastically reduce running costs of an inductively coupled plasma. This is done by reducing the argon consumption from 20 l/min to about 1 l/min. First, a sample introduction system operating on 0.1 l/min of carrier argon is described. This system ensures a high ratio of plasma argon and carrier argon even at the low total argon consumptions intended. Next, the developed low consumption plasma is presented. In the proposed design, air is blown perpendicularly against the outside of the torch. A different coil has been developed to make air-cooling efficient. Preliminary data on coupling efficiency for the air-cooled plasma are presented. A similarly low argon consumption has been achieved with water as an external coolant medium. It is concluded that a cheaper alternative to the current ICP has become available. (Auth.)

  17. Speciation of the plutonium at trace levels by capillary electrophoresis-ICP-MS coupling

    International Nuclear Information System (INIS)

    Ambard, Ch.

    2007-01-01

    The CE-ICP-MS coupling allowed the development of new analytical methods for the study of plutonium (Pu) speciation at trace levels including complexation studies of this element by organic and inorganic ligands. First, a method, called dual detection, based on the simultaneous use of the UV-Visible spectrophotometer integrated in the capillary electrophoresis and the ICP-MS was developed and validated. It allows the unambiguous determination of electrophoretic mobilities for separated chemical species and gives a powerful tool for speciation studies. Then, the influence on Pu redox speciation of the buffer from the background electrolyte was evaluated. This study showed the implications of the electrolyte constituents' choice on Pu redox equilibrium in the sample. Furthermore, the CE-ICP-MS coupling was used for studying the Pu complexation at trace levels by some organic (NTA and DTPA) and inorganic ligands (carbonates). The behaviour of Pu valence +III, +IV and +VI was studied in the presence of buffer at near neutral pH. Different species of Pu were observed depending on the initial oxidation state of the plutonium. The study showed the potential of poly-amino-carboxylic acids, such as NTA and DTPA, for dissolving Pu precipitates, regardless its initial speciation. Finally, the carbonation of pentavalent neptunium, as an analogue of Pu(V), was achieved at very low concentration of Np (10 -8 mol.L -1 ). The formation of NpO 2 (CO 3 ) - at 25 C and 2,5*10 -2 mol.L -1 ionic strength was measured by CE-ICP-MS and found to consistent with literature data. (author)

  18. Study of hard diamond-like carbon films deposited in an inductively coupled plasma source

    International Nuclear Information System (INIS)

    Yu Shiji; Ma Tengcai

    2003-01-01

    Chemical vapor deposition of the hard diamond-like carbon (DLC) films was achieved using an inductively coupled plasma source (ICPS). The microscopy, microhardness, deposition rate and structure characteristic of the DLC films were analyzed. It is shown that the ICPS is suitable for the hard DLC film deposition at relatively low substrate negative bias voltage, and the substrate negative bias voltage greatly affects chemical vapor deposition of the DLC film and its quality

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

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Jin-Won; Lee, Yun-Seong, E-mail: leeeeys@kaist.ac.kr; Chang, Hong-Young [Low-temperature Plasma Laboratory, Department of Physics, Korea Advanced Institute of Science and Technology, Daejeon 305-701 (Korea, Republic of); An, Sang-Hyuk [Agency of Defense Development, Yuseong-gu, Daejeon 305-151 (Korea, Republic of)

    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 due 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.

  20. Inductively coupled plasma-atomic emission spectroscopy glovebox assembly system at the West Valley Demonstration Project

    International Nuclear Information System (INIS)

    Marlow, J.H.; McCarthy, K.M.; Tamul, N.R.

    1999-01-01

    The inductively coupled plasma/atomic emission spectroscopy [ICP/AES (ICP)] system for elemental analyses in support of vitrification processing was first installed in 1986. The initial instrument was a Jobin Yvon (JY) Model JY-70 ICP that consisted of sequential and simultaneous spectrometers for analysis of nonradioactive samples as radioactive surrogates. The JY-70 ICP continued supporting nonradioactive testing during the Functional and Checkout Testing of Systems (FACTS) using the full-scale melter with ''cold'' (nonradioactive) testing campaigns. As a result, the need for another system was identified to allow for the analysis of radioactive samples. The Mass Spec (Spectrometry) Lab was established for the installation of the modified ICP system for handling radioactive samples. The conceptual setup of another ICP was predicated on the use of a hood to allow ease of accessibility of the torch, nebulizer, and spray chamber, and the minimization of air flow paths. However, reconsideration of the radioactive sample dose rate and contamination levels led to the configuration of the glovebox system with a common transfer interface box for the ICP and the inductively coupled plasma-mass spectrometer (ICP-MS) glovebox assemblies. As a result, a simultaneous Model JY-50P ICP with glovebox was installed in 1990 as a first generation ICP glovebox system. This was one of the first ICP glovebox assemblies connected with an ICP-MS glovebox system. Since the economics of processing high-level radioactive waste (HLW) required the availability of an instrument to operate 24 hours a day throughout the year without any downtime, a second generation ICP glovebox assembly was designed, manufactured, and installed in 1995 using a Model JY-46P ICP. These two ICP glovebox systems continue to support vitrification of the HLW into canisters for storage. The ICP systems have been instrumental in monitoring vitrification batch processing. To date, remote sample preparation and

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

    International Nuclear Information System (INIS)

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

    2009-01-01

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

  2. Development of a simple extraction cell with bi-directional continuous flow coupled on-line to ICP-MS for assessment of elemental associations in solid samples

    DEFF Research Database (Denmark)

    Buanuam, Janya; Tiptanasup, Kasipa; Shiowatana, Juwadee

    2006-01-01

    A continuous-flow system comprising a novel, custom-built extraction module and hyphenated with inductively coupled plasma-mass spectrometric (ICP-MS) detection is proposed for assessing metal mobilities and geochemical associations in soil compartments as based on using the three step BCR (now...... the Measurements and Testing Programme of the European Commission) sequential extraction scheme. Employing a peristaltic pump as liquid driver, alternate directional flows of the extractants are used to overcome compression of the solid particles within the extraction unit to ensure a steady partitioning flow rate...... and thus to maintain constant operationally defined extraction conditions. The proposed flow set-up is proven to allow for trouble-free handling of soil samples up to 1 g and flow rates ≤ 10 mL min–1. The miniaturized extraction system was coupled to ICP-MS through a flow injection interface in order...

  3. Aerosol detection efficiency in inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Hubbard, Joshua A.; Zigmond, Joseph A.

    2016-05-01

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

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

    International Nuclear Information System (INIS)

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

    1993-06-01

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

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

    International Nuclear Information System (INIS)

    Wong, K.L.

    1981-01-01

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

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

    Science.gov (United States)

    Gäckle, M.; Merten, D.

    2010-12-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-09-15

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

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

    Science.gov (United States)

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

    1992-01-01

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

  9. Speciation of the plutonium at trace levels by capillary electrophoresis-ICP-MS coupling

    International Nuclear Information System (INIS)

    Ambard, Ch.

    2007-01-01

    The CE-ICP-MS coupling allowed the development of new analytical methods for the study of plutonium speciation at trace levels including complexation studies of this element by organic and inorganic ligands. First, a method, called dual detection, based on the simultaneous use of the UV-Visible spectrophotometer integrated in the capillary electrophoresis and the ICPMS was developed and validated. It allows the unambiguous determination of electrophoretic mobilities for separated chemical species and gives a powerful tool for speciation studies. Then, the influence on plutonium redox speciation of the buffer from the background electrolyte was evaluated. This study showed the implications of the electrolyte constituents' choice on plutonium redox equilibrium in the sample. Furthermore, the CE-ICP-MS coupling was used for studying the plutonium complexation at trace levels by some organic (NTA and DTPA) and inorganic ligands (carbonates). The behaviour of plutonium valence +III, +IV and +VI was studied in the presence of buffer at near neutral pH. Different species of plutonium were observed depending on the initial oxidation state of the plutonium. This study showed the potential of poly-amino-carboxylic acids, such as NTA and DTPA, for dissolving plutonium precipitates, regardless its initial speciation. Finally, the carbonation of pentavalent neptunium, as an analogue of Pu(V), was achieved at very low concentration of Np (10 -8 mol.L -1 ). The formation constant of NpO 2 (CO 3 )- at 25 deg. C and 2,5 x 10 -2 mol.L -1 ionic strength was measured by CE-ICP-MS and found to be consistent with literature data. (author)

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

    International Nuclear Information System (INIS)

    Kawaguchi, Hiroshi

    1996-01-01

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

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

    Science.gov (United States)

    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

  12. Inductively coupled plasma-atomic emission spectroscopy

    International Nuclear Information System (INIS)

    Winge, R.K.; Fassel, V.A.; Peterson, V.J.; Floyd, M.A.

    1985-01-01

    This atlas of inductively coupled plasma-atomic emission spectroscopy records the spectra of the elements in a way that would reveal the general nature of the spectra, in all their simplicity or complexity; and offers a definitive summary of the most prominent spectral lines of the elements, i.e., those most likely to be useful for the determination of trace and ultratrace concentrations; it provides reliable estimates, based on the recorded experimental spectra, of the powers of detection of the listed prominent lines; and assesses the very important problem of spectral interferences. The atlas is composed of three main sections. Part I is concerned with the historical aspects of compilations of spectral information. Part II is based on 232 wavelength scans of 70 elements. Each of the wavelength scans covers an 80 nm spectral region. These scans allow a rapid comparison of the background and spectral line intensities emitted in the ICP and provide a ready means for identification of the most prominent lines of each element and for estimation of the trace element analytical capabilities of these lines. A listing of 973 prominent lines with associated detection limits is also presented. Part III addresses the problem of spectral interferences. On this topic a detailed collection of coincidence profiles is presented for 281 of the most prominent lines, each with profiles of ten of the most prevalent concomitants superimposed. (Auth.)

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

    International Nuclear Information System (INIS)

    Bricker, T.

    1994-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-01-01

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

  15. Inductively coupled plasma emission spectroscopy. Part II: applications and fundamentals. Volume 2

    International Nuclear Information System (INIS)

    Boumans, P.W.J.M.

    1987-01-01

    This is the second part of the two-volume treatise by this well-known and respected author. This volume reviews applications of inductively coupled plasma atomic emission spectroscopy (ICP-AES), summarizes fundamental studies, and compares ICP-AES methods with other methods of analysis. The first six chapters are devoted to specific fields of application, including the following: metals and other industrial materials, geology, the environment, agriculture and food, biology and clinical analysis, and organic materials. The chapter on the analysis of organic materials also covers the special instrumental considerations required when organic solvents are introduced into an inductively coupled plasma. A chapter on the direct analysis of solids completes the first part of this volume. Each of the applications chapters begins with a summary of the types of samples that are encountered in that field, and the kinds of problems that an elemental analysis can help to solve. This is followed by a tutorial approach covering applicability, advantages, and limitations of the methods. The coverage is thorough, including sample handling, storage, and preparation, acid, and fusion dissolution, avoiding contamination, methods of preconcentration, the types of interferences that can be expected and ways to reduce them, and the types of ICP plasmas that are used. The second half of the volume covers fundamental studies of ICP-AES: basic processes of aerosol generation, plasma modeling and computer simulation, spectroscopic diagnostics, excitation mechanisms, and discharge characteristics. This section introduces the experimental and modeling methods that have been used to obtain fundamental information about ICPs

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

    Science.gov (United States)

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

    2016-01-01

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

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

    International Nuclear Information System (INIS)

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

    1991-01-01

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

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

    Czech Academy of Sciences Publication Activity Database

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

    2016-01-01

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

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

    DEFF Research Database (Denmark)

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

    2015-01-01

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

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

    International Nuclear Information System (INIS)

    Farnsworth, P.B.

    1993-01-01

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

  1. Coupling of Plasmas and Liquids

    Science.gov (United States)

    Lindsay, Alexander David

    Plasma-liquids have exciting applications to several important socioeconomic areas, including agriculture, water treatment, and medicine. To realize their application potential, the basic physical and chemical phenomena of plasma-liquid systems must be better understood. Additionally, system designs must be optimized in order to maximize fluxes of critical plasma species to the liquid phase. With objectives to increase understanding of these systems and optimize their applications, we have performed both comprehensive modeling and experimental work. To date, models of plasma-liquids have focused on configurations where diffusion is the dominant transport process in both gas and liquid phases. However, convection plays a key role in many popular plasma source designs, including jets, corona discharges, and torches. In this dissertation, we model momentum, heat, and neutral species mass transfer in a convection-dominated system based on a corona discharge. We show that evaporative cooling produced by gas-phase convection can lead to a significant difference between gas and liquid phase bulk temperatures. Additionally, convection induced in the liquid phase by the gas phase flow substantially increases interfacial mass transfer of hydrophobic species like NO and NO2. Finally, liquid kinetic modeling suggests that concentrations of highly reactive species like OH and ONOOH are several orders of magnitude higher at the interface than in the solution bulk. Subsequent modeling has focused on coupling discharge physics with species transport at and through the interface. An assumption commonly seen in the literature is that interfacial loss coefficients of charged species like electrons are equal to unity. However, there is no experimental evidence to either deny or support this assumption. Without knowing the true interfacial behavior of electrons, we have explored the effects on key plasma-liquid variables of varying interfacial parameters like the electron and energy

  2. A comparison of the M3/M4 metastable defect detected in hydrogen and ICP Ar plasma treated n-GaAs

    International Nuclear Information System (INIS)

    Nyamhere, C.; Venter, A.

    2012-01-01

    Defects created by a dc hydrogen plasma have been compared to those observed in n-GaAs exposed to an inductively coupled (ICP) Ar plasma. The reference sample (in the case of H-plasma treated material) contained two prominent native deep level electron traps, possibly M4 and E C −0.56 eV, which were both passivated by hydrogen. Plasma treatment also resulted in the formation of a defect observed at 0.58 eV (M3) below the conduction band. This defect transforms back into what is believed to be M4 when annealed at 350 K for 3 h under reverse bias. These two defects compare well with two similar defects observed in the Ar ICP treated samples also showing metastable behavior. Additionally, the electrical characterization of Schottky barrier diodes on n-GaAs, prior to and after hydrogen passivation shows that, depending on the plasma conditions, the plasma ions significantly damage the surface resulting in poor rectifying contacts. The damage is considerably reversed/repaired upon annealing between the room temperature and 573 K (300 °C).

  3. A comparison of the M3/M4 metastable defect detected in hydrogen and ICP Ar plasma treated n-GaAs

    Energy Technology Data Exchange (ETDEWEB)

    Nyamhere, C., E-mail: cloud.nyamhere@nmmu.ac.za [Department of Physics, Nelson Mandela Metropolitan University, P.O. Box 77000, Port Elizabeth 6031 (South Africa); Venter, A. [Department of Physics, Nelson Mandela Metropolitan University, P.O. Box 77000, Port Elizabeth 6031 (South Africa)

    2012-05-15

    Defects created by a dc hydrogen plasma have been compared to those observed in n-GaAs exposed to an inductively coupled (ICP) Ar plasma. The reference sample (in the case of H-plasma treated material) contained two prominent native deep level electron traps, possibly M4 and E{sub C}-0.56 eV, which were both passivated by hydrogen. Plasma treatment also resulted in the formation of a defect observed at 0.58 eV (M3) below the conduction band. This defect transforms back into what is believed to be M4 when annealed at 350 K for 3 h under reverse bias. These two defects compare well with two similar defects observed in the Ar ICP treated samples also showing metastable behavior. Additionally, the electrical characterization of Schottky barrier diodes on n-GaAs, prior to and after hydrogen passivation shows that, depending on the plasma conditions, the plasma ions significantly damage the surface resulting in poor rectifying contacts. The damage is considerably reversed/repaired upon annealing between the room temperature and 573 K (300 Degree-Sign C).

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

    International Nuclear Information System (INIS)

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

    1979-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2000-11-01

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

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

    International Nuclear Information System (INIS)

    Yoshida, K.; Haraguchi, H.

    1984-01-01

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

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

    International Nuclear Information System (INIS)

    Nathan Joe Saetveit

    2008-01-01

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

  8. Room temperature inductively coupled plasma etching of InAs/InSb in BCl 3/Cl 2/Ar

    KAUST Repository

    Sun, Jian; Kosel, Jü rgen

    2012-01-01

    Inductively coupled plasma (ICP) etching of InAs and InSb at room temperature has been investigated using BCl 3/Cl 2/Ar plasma. Specifically, the etch rate and post-etching surface morphology were investigated as functions of the gas composition

  9. Study of HPLC/ICP-MS coupling for the As speciation; Estudo de um acoplamento de HPLC/ICP-MS para a especiacao do As

    Energy Technology Data Exchange (ETDEWEB)

    Cortez, Bruna C.G.; Oliveira, Arno Heeren de [Minas Gerais Univ., Belo Horizonte, MG (Brazil). Dept. de Engenharia Nuclear]. E-mail: brunacortez2004@yahoo.com.br; heeren@nuclear.ufmg.br

    2005-07-01

    Trace metals in the environment may provide benefit or risk to humans, other life forms, and the environment. More robust and information-rich trace and ultra-trace analyses are needed to all adequate risk/benefit assessments. Further, it is no longer adequate to consider only the total trace metal or metalloid, because the impact of elements on ecological systems or biological organisms is not necessarily given by total element concentrations alone. It is necessary to determine the chemical form (species) of the element, primarily the oxidation state or the organometallic nature, because different species of the same metal can range from essential to innocuous to toxic. The actual toxicity levels from different arsenic compounds vary greatly. Inorganic arsenic is considered the most acutely toxic form; arsenite (As{sup III}) is more toxic than arsenate (As{sup V}). The chronic toxicity of arsenic compounds is currently not well understood and is actively being researched. In this study, the viability of the ICP-MS detector coupled with High Performance Liquid Chromatography (HPLC) was tested in 21 water samples from the Das Velhas River, Minas Gerais state, in Brazil. The results showed that the low detection limits and the ease coupling HPLC system - which offers a rugged and versatile separation technique - makes ICP-MS a successful detection method for arsenic speciation analysis. (author)

  10. FLOW INJECTION ANALYSIS SYSTEM COUPLED WITH ICP-EOS FOR DETERMINATION OF SOME METALLIC ELEMENTS IN DRINKING WATER

    Directory of Open Access Journals (Sweden)

    Cristina Dinu

    2009-06-01

    Full Text Available The European Drinking Water Directive (98/83/EC, transposed in Romanian Legislation as Low 458/2002, amended by Low 311/2004, imposes the limit of concentration for metallic elements in water intended for human consumption. The toxic metals arsenic and selenium are among these elements and the limit value is 10 μg/L. In the paper there are presented the working conditions for determination of As and Se from drinking water using modern techniques based on the fl ow injection-hydride generation with the inductively coupled plasma atomic emission spectrometry (FIAS-ICP-EOS. The analyses were performed on Optima 5300 DV Perkin Elmer equipment with FIAS 400 Flow Injection System, Perkin Elmer type. For the hydride generation two types of solution were used: 10% (v/v HCl as a carrier solution and 0.2 % NaBH4 in 0.05%NaOH solution as a reducing agent [1]. The treatment step of the samples and standard solutions consisted in reducing with mixed solutions of KI and ascorbic acid in acidic condition (HCl for As and only with HCl and high temperature for Se [2,3]. The paper contains the characteristic parameters of the methods, such as: low detection limit, quantifi cation limit, repeatability, precision, recovery, which were evaluated using Certifi ed Reference Materials for each element.

  11. Rapid actinide analysis method coupling liquid chromatography/ICP-MS and "9"0Sr gas proportional counter in post-accidental situation environmental samples

    International Nuclear Information System (INIS)

    Habibi, Azza

    2015-01-01

    The present study follows the Fukushima power plant accident and aimed to develop an analytical method to achieve, during an emergency situation, a rapid identification and quantification of alpha and beta emitters in environmental samples. The first step of this study allowed us to list the alpha and beta emitters which can be released in the environment in case of a nuclear accident. The second step aimed towards the development of a rapid analysis method to quantify 17 radionuclides of U, Th, Pu, Am, Np and Sr. The main objective was the automation of the radiochemical separation step and its coupling for the measurement. The separation is performed using columns containing extraction resins, namely TEVA, TRU and Sr. The measurement is performed using an ICP-MS (inductively coupled plasma mass spectrometry) and in some cases a gas proportional counter to quantify radiostrontium ("8"9Sr and "9"0Sr). Excellent figures of merit were obtained, off line, with water (tap, river and sea water) and solid matrices (soil and aerosol filters), after a micro-wave digestion or an alkaline fusion dissolution followed by a Ca_3(PO_4)_2 coprecipitation. The proposed analytical strategy showed yields between 70 % and 100 % and standard deviations between 5 % and 10 %. The newly developed separation method was then automated and coupled on-line to ICP-MS. The operating parameters were optimized using a design of experiments and the results were processed with Minitab. The optimized automated separation coupled on-line to the ICP-MS allows the rapid quantification, in 1.5 h per sample, of U, Th, Pu, Am, Np and Sr with detection limits gain as high as 20 times for artificial radionuclide. (author)

  12. Inductively Coupled Plasma-Induced Etch Damage of GaN p-n Junctions

    International Nuclear Information System (INIS)

    SHUL, RANDY J.; ZHANG, LEI; BACA, ALBERT G.; WILLISON, CHRISTI LEE; HAN, JUNG; PEARTON, S.J.; REN, F.

    1999-01-01

    Plasma-induced etch damage can degrade the electrical and optical performance of III-V nitride electronic and photonic devices. We have investigated the etch-induced damage of an Inductively Coupled Plasma (ICP) etch system on the electrical performance of mesa-isolated GaN pn-junction diodes. GaN p-i-n mesa diodes were formed by Cl 2 /BCl 3 /Ar ICP etching under different plasma conditions. The reverse leakage current in the mesa diodes showed a strong relationship to chamber pressure, ion energy, and plasma flux. Plasma induced damage was minimized at moderate flux conditions (≤ 500 W), pressures ≥2 mTorr, and at ion energies below approximately -275 V

  13. Analysis of twenty five impurities in uranium matrix by ICP-MS with iron measurement optimized by using reaction collision cell, cold plasma or medium resolution

    International Nuclear Information System (INIS)

    Quemet, Alexandre; Brennetot, Rene; Chevalier, Emilie; Prian, Edwina; Laridon, Anne-Laure; Fichet, Pascal; Goutelard, Florence; Mariet, Clarisse; Laszak, Ivan

    2012-01-01

    An analytical procedure was developed to determine the concentration of 25 impurities (Li, Be, Ti, V. Cr, Mn, Fe, Co, Ni, Cu, Zn, Zr, Mo, Ag, Cd, In, Sm, Eu, Gd, Dy, W, Pb, Bi and Th) in a uranium matrix using the quadrupole inductively coupled plasma mass spectrometry (Q-ICP-MS). The dissolution of U 3 O 8 powder was made with a mixture of hydrochloric acid and nitric acid. Then, a selective separation of uranium using the UTEVA column was used before measurement by Q-ICP-MS. The procedure developed was verified using the Certified Reference Material 'Morille'. The analytical results agree well except for 5 elements where values are underestimated (Li, Be, In, Pb and Bi). Among the list of impurities, iron was particularly investigated because it is well known that this element possesses a polyatomic interference that increases the detection limit. A comparison between iron detection limits obtained with different methods was performed. Iron polyatomic interference was at least reduced, or at best entirely resolved in some cases, by using the cold plasma or the collision/reaction cell with several gases (He, NH 3 and CH 4 ). High-resolution ICP-MS was used to compare the results obtained. A detection limit as low as 8 ng L -1 was achieved. (authors)

  14. Analysis of twenty five impurities in uranium matrix by ICP-MS with iron measurement optimized by using reaction collision cell, cold plasma or medium resolution.

    Science.gov (United States)

    Quemet, Alexandre; Brennetot, Rene; Chevalier, Emilie; Prian, Edwina; Laridon, Anne-Laure; Mariet, Clarisse; Fichet, Pascal; Laszak, Ivan; Goutelard, Florence

    2012-09-15

    An analytical procedure was developed to determine the concentration of 25 impurities (Li, Be, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Zr, Mo, Ag, Cd, In, Sm, Eu, Gd, Dy, W, Pb, Bi and Th) in a uranium matrix using the quadrupole inductively coupled plasma mass spectrometry (Q-ICP-MS). The dissolution of U(3)O(8) powder was made with a mixture of hydrochloric acid and nitric acid. Then, a selective separation of uranium using the UTEVA column was used before measurement by Q-ICP-MS. The procedure developed was verified using the Certified Reference Material "Morille". The analytical results agree well except for 5 elements where values are underestimated (Li, Be, In, Pb and Bi). Among the list of impurities, iron was particularly investigated because it is well known that this element possesses a polyatomic interference that increases the detection limit. A comparison between iron detection limits obtained with different methods was performed. Iron polyatomic interference was at least reduced, or at best entirely resolved in some cases, by using the cold plasma or the collision/reaction cell with several gases (He, NH(3) and CH(4)). High-resolution ICP-MS was used to compare the results obtained. A detection limit as low as 8 ng L(-1) was achieved. Copyright © 2012 Elsevier B.V. All rights reserved.

  15. Surface characterization of hydrophobic thin films deposited by inductively coupled and pulsed plasmas

    International Nuclear Information System (INIS)

    Kim, Youngsoo; Lee, Ji-Hye; Kim, Kang-Jin; Lee, Yeonhee

    2009-01-01

    Different fluorocarbon thin films were deposited on Si substrates using a plasma-polymerization method. Fluorine-containing hydrophobic thin films were obtained by inductively coupled plasma (ICP) and pulsed plasma (PP) with a mixture of fluorocarbon precursors C 2 F 6 , C 3 F 8 , and c-C 4 F 8 and the unsaturated hydrocarbons of C 2 H 2 . The influence on the fluorocarbon surfaces of the process parameters for plasma polymerization, including the gas ratio and the plasma power, were investigated under two plasma-polymerized techniques with different fluorocarbon gas precursors. The hydrophobic properties, surface morphologies, and chemical compositions were elucidated using water contact angle measurements, field emission-scanning electron microscope, x-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FT-IR), and time-of-flight secondary ion mass spectrometry (TOF-SIMS). In this study, the ICP technique provides coarser grained films and more hydrophobic surfaces as well as a higher deposition rate compared to the PP technique. XPS, FT-IR, and TOF-SIMS analyses indicated that the ICP technique produced more fluorine-related functional groups, including CF 2 and CF 3 , on the surface. From the curve-fitted XPS results, fluorocarbon films grown under ICP technique exhibited less degree of cross-linking and higher CF 2 concentrations than those grown under PP technique.

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

    Science.gov (United States)

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

    2016-05-30

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

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

    Science.gov (United States)

    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.

  18. Biomonitoring of selenoprotein P in human serum by fast affinity chromatography coupled to ICP-MS.

    Science.gov (United States)

    Heitland, Peter; Köster, Helmut D

    2018-04-01

    Most of the Se in human serum is bound to selenoprotein P (SEPP1) in which Se is present in form of selenocysteine. The SEPP1 is a new possible biomarker for the Se status and for this reason we developed a fast, simple and reliable method for the quantitative determination of SEPP1 in serum by affinity chromatography coupled to ICP-MS. It is possible to separate SEPP1 from other selenoproteins in serum in only 5 min, which allows high sample throughput in clinical laboratories. Measured and certified concentrations of total Se and Se(SEPP1) are in good agreement for the reference material SRM 1950. The SEPP1 concentration was stable in serum samples of 3 persons for a minimum of 2 weeks. Further results of method validation were described including internal and external quality assurance. The analytical method was applied for a biomonitoring study of the SEPP1 and total Se concentration in human serum of 50 occupationally non-exposed persons living in northern Germany. Concentration ranges and mean concentrations for Se(SEPP1) are 31.1-59.7 and 46.2 μg/L, respectively. The corresponding values for total Se are 62-120 and 83.5 μg/L. The mean percentage of total Se in serum present as SEPP1 is 58%. Copyright © 2018 Elsevier GmbH. All rights reserved.

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

    International Nuclear Information System (INIS)

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

    2014-01-01

    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. (author)

  20. Applications of inductively coupled plasma spectroscopy to geochemical reconnaissance for uranium exploration

    International Nuclear Information System (INIS)

    Cagle, G.W.; Butz, T.R.

    1980-01-01

    The analysis of large numbers of natural groundwater and stream sediment samples by Inductively Coupled Plasma (ICP) Spectroscopy has been applied to a geochemical reconnaissance program as part of the National Uranium Resource Evaluation Program. Approximately 25 elements have been determined in over 60,000 samples by ICP analysis. These data are combined with additional measurements obtained by atomic absorption, colorimetry, neutron activation, and fluorescence spectroscopy. Results are presented and interpreted in terms of the uranium favorability of areas in Texas where this survey has been completed

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

    International Nuclear Information System (INIS)

    Lee Yiling; Chang Chaochiang; Jiang Shiuhjen

    2003-01-01

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

  2. Application of a particle separation device to reduce inductively coupled plasma-enhanced elemental fractionation in laser ablation-inductively coupled plasma-mass spectrometry

    International Nuclear Information System (INIS)

    Guillong, Marcel; Kuhn, Hans-Rudolf; Guenther, Detlef

    2003-01-01

    The particle size distribution of laser ablation aerosols are a function of the wavelength, the energy density and the pulse duration of the laser, as well as the sample matrix and the gas environment. Further the size of the particles affects the vaporization and ionization efficiency in the inductively coupled plasma (ICP). Some matrices produce large particles, which are not completely vaporized and ionized in the ICP. The previous work has shown that analytical results such as matrix-independent calibration, accuracy and precision can be significantly influenced by the particle sizes of the particles. To minimize the particle size related incomplete conversion of the sample to ions in the ICP a particle separation device was developed, which allows effective particle separation using centrifugal forces in a thin coiled tube. In this device, the particle cut-off size is varied by changing the number of turns in the coil, as well as by changing the gas flow and the tube diameter. The interaction of the laser with the different samples leads to varying particle size distributions. When carrying out quantitative analysis with non-matrix matched calibration reference materials, it was shown that different particle cut-off sizes were required depending on the ICP conditions and the instrument used for analysis. Various sample materials were investigated in this study to demonstrate the applicability of the device. For silicate matrices, the capability of the ICP to produce ions was significantly reduced for particles larger than 0.5 μm, and was dependent on the element monitored. To reduce memory effects caused by the separated particles, a washout procedure was developed, which additionally allowed the analysis of the trapped particles. These results clearly demonstrate the very important particle size dependent ICP-MS signal response and the potential of the described particle size based separator for the reduction of ICP induced elemental fractionation

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    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.

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

    International Nuclear Information System (INIS)

    Muto, Toshio; Shimokawa, Toshinari

    1997-01-01

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

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

    Science.gov (United States)

    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.

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

    International Nuclear Information System (INIS)

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

    2013-01-01

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

  8. Similarity analysis for the high-pressure inductively coupled plasma source

    International Nuclear Information System (INIS)

    Vanden-Abeele, D; Degrez, G

    2004-01-01

    It is well known that the optimal operating parameters of an inductively coupled plasma (ICP) torch strongly depend upon its dimensions. To understand this relationship better, we derive a dimensionless form of the equations governing the behaviour of high-pressure ICPs. The requirement of similarity then naturally leads to expressions for the operating parameters as a function of the plasma radius. In addition to the well-known scaling law for frequency, surprising results appear for the dependence of the mass flow rate, dissipated power and operating pressure upon the plasma radius. While the obtained laws do not appear to be in good agreement with empirical results in the literature, their correctness is supported by detailed numerical calculations of ICP sources of varying diameters. The approximations of local thermodynamic equilibrium and negligible radiative losses restrict the validity of our results and can be responsible for the disagreement with empirical data. The derived scaling laws are useful for the design of new plasma torches and may provide explanations for the unsteadiness observed in certain existing ICP sources

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

    International Nuclear Information System (INIS)

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

    2000-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-07-01

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

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

    International Nuclear Information System (INIS)

    Braverman, D.S.

    1992-01-01

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

  12. Determination of Rare Earth Elements in Thai Monazite by Inductively Coupled Plasma and Nuclear Analytical techniques

    International Nuclear Information System (INIS)

    Busamongkol, Arporn; Ratanapra, Dusadee; Sukharn, Sumalee; Laoharojanaphand, Sirinart

    2003-10-01

    The inductively coupled plasma atomic emission spectroscopy (ICP-AES) for the determination of individual rare-earth elements (REE) was evaluated by comparison with instrumental neutron activation analysis (INAA) and x-ray fluorescence spectrometry (XRF). The accuracy and precision of INAA and ICP-AES were evaluated by using standard reference material IGS-36, a monazite concentrate. For INAA, the results were close to the certified value while ICP-AES were in good agreement except for some low concentration rare earth. The techniques were applied for the analysis of some rare earth elements in two Thai monazite samples preparing as the in-house reference material for the Rare Earth Research and Development Center, Chemistry Division, Office of Atoms for Peace. The analytical results obtained by these techniques were in good agreement with each other

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

    International Nuclear Information System (INIS)

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

    1994-01-01

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

  14. Phosphorus doped graphene by inductively coupled plasma and triphenylphosphine treatments

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-10-15

    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 very 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.

  15. Theory and simulation of laser plasma coupling

    International Nuclear Information System (INIS)

    Kruer, W.L.

    1979-01-01

    The theory and simulation of these coupling processes are considered. Particular emphasis is given to their nonlinear evolution. First a brief introduction to computer simulation of plasmas using particle codes is given. Then the absorption of light via the generation of plasma waves is considered, followed by a discussion of stimulated scattering of intense light. Finally these calculations are compared with experimental results

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

    International Nuclear Information System (INIS)

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

    2014-01-01

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

  17. Fluid model of inductively coupled plasma etcher based on COMSOL

    International Nuclear Information System (INIS)

    Cheng Jia; Ji Linhong; Zhu Yu; Shi Yixiang

    2010-01-01

    Fluid dynamic models are generally appropriate for the investigation of inductively coupled plasmas. A commercial ICP etcher filled with argon plasma is simulated in this study. The simulation is based on a multiphysical software, COMSOL(TM), which is a partial differential equation solver. Just as with other plasma fluid models, there are drift-diffusion approximations for ions, the quasi-neutrality assumption for electrons movements, reduced Maxwell equations for electromagnetic fields, electron energy equations for electron temperatures and the Navier-Stokes equation for neutral background gas. The two-dimensional distribution of plasma parameters are shown at 200 W of power and 1.33 Pa (10 mTorr) of pressure. Then the profile comparison of the electron number density and temperature with respect to power is illustrated. Finally we believe that there might be some disagreement between the predicted values and the real ones, and the reasons for this difference would be the Maxwellian eedf assumption and the lack of the cross sections of collisions and the reaction rates. (semiconductor physics)

  18. State-space modeling of the radio frequency inductively-coupled plasma generator

    International Nuclear Information System (INIS)

    Dewangan, Rakesh Kumar; Punjabi, Sangeeta B; Mangalvedekar, H A; Lande, B K; Joshi, N K; Barve, D N

    2010-01-01

    Computational fluid dynamics models of RF-ICP are useful in understanding the basic transport phenomenon in an ICP torch under a wide variety of operating conditions. However, these models lack the ability to evaluate the effects of the plasma condition on the RF generator. In this paper, simulation of an induction plasma generator has been done using state space modelling by considering inductively coupled plasma as a part of RF network .The time dependent response of the RF-ICP generator circuit to given input excitation has been computed by extracting the circuit's state-space variables and their constraint matrices. MATLAB 7.1 software has been used to solve the state equations. The values of RF coil current, frequency and plasma power has been measured experimentally also at different plate bias voltage. The simulated model is able to predict RF coil current, frequency, plasma power, overall efficiency of the generator. The simulated and measured values are in agreement with each other. This model can prove useful as a design tool for the Induction plasma generator.

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

    Science.gov (United States)

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

    2014-08-20

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

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

    NARCIS (Netherlands)

    Krystek, Petra; Ritsema, R.

    2002-01-01

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

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

    International Nuclear Information System (INIS)

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

    2005-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2005-03-15

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

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

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

    International Nuclear Information System (INIS)

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

    2013-01-01

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

  5. Determination of organic and inorganic mercury species in Sungai Kinta, Perak by reversed-phase high performance liquid chromatography (HPLC) on-line coupled with ICP-MS

    International Nuclear Information System (INIS)

    Norshidah Baharuddin; Norashikin Saim; Rozita Osman; Sharifuddin Mohd Zain

    2012-01-01

    This paper describes a simple method for mercury speciation in river water samples of Sungai Kinta, Perak. Separation and measurement were done by high-performance liquid chromatography on-line with inductively coupled plasma mass spectrometry (HPLC/ ICP-MS). Separation of mercury species was accomplished within 6 minutes on an AQ C18 4.6 mm i.d x 150 mm, 5 μm reversed phase column with 0.1 % (w/ v) L-cysteine as mobile phase. Under the optimum instrumental conditions, recoveries of 101-104 % for MeHg + and 96 - 104 % for Hg 2+ were obtained with experimental detection limits of 1ngL -1 for inorganic mercury and 1.5 μgL -1 for organic mercury. (author)

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

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

    2015-01-15

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

  8. Electron energy distributions and electron impact source functions in Ar/N{sub 2} inductively coupled plasmas using pulsed power

    Energy Technology Data Exchange (ETDEWEB)

    Logue, Michael D., E-mail: mdlogue@umich.edu; Kushner, Mark J., E-mail: mjkush@umich.edu [Department of Electrical Engineering and Computer Science, University of Michigan, 1301 Beal Ave., Ann Arbor, Michigan 48109-2122 (United States)

    2015-01-28

    In plasma materials processing, such as plasma etching, control of the time-averaged electron energy distributions (EEDs) in the plasma allows for control of the time-averaged electron impact source functions of reactive species in the plasma and their fluxes to surfaces. One potential method for refining the control of EEDs is through the use of pulsed power. Inductively coupled plasmas (ICPs) are attractive for using pulsed power in this manner because the EEDs are dominantly controlled by the ICP power as opposed to the bias power applied to the substrate. In this paper, we discuss results from a computational investigation of EEDs and electron impact source functions in low pressure (5–50 mTorr) ICPs sustained in Ar/N{sub 2} for various duty cycles. We find there is an ability to control EEDs, and thus source functions, by pulsing the ICP power, with the greatest variability of the EEDs located within the skin depth of the electromagnetic field. The transit time of hot electrons produced in the skin depth at the onset of pulse power produces a delay in the response of the EEDs as a function of distance from the coils. The choice of ICP pressure has a large impact on the dynamics of the EEDs, whereas duty cycle has a small influence on time-averaged EEDs and source functions.

  9. Inductively coupled plasma and ion sources: History and state-of-the-art

    International Nuclear Information System (INIS)

    Hopwood, J.

    1994-01-01

    Over 100 years ago Hittorf first generated an electrodeless ''ring'' discharge by electromagnetic induction and began a 40 year controversy as to the true physical origin of such a discharge. Even Tesla advocated that these plasmas were merely the result of large electrostatic potential differences rather than electric fields induced by high frequency currents. Through clever experiments using crude spark gaps and leyden jars, the inductive nature of the discharge was confirmed in the late 1920's by MacKinnon, thus supporting the theories and experiments of Sir J.J. Thomson, perhaps the most staunch advocate of the induction mechanism. Today the authors routinely exploit the intense plasmas which are generated by induction. In this talk, the characteristics of inductively coupled plasma (ICP) and ion sources will be reviewed and future applications of intense plasma sources will be discussed. The inductively coupled plasma is Joule heated at moderate gas pressures, but the electromagnetic field penetration of these dense plasmas is limited by the plasma skin depth, typically a few millimeters to a few centimeters. The induction plasma is thus edge heated, a fact that constrains uniformity over large areas if helical induction coils are used. Flat, spiral coils may be used to improve uniformity by driving the plasma using a planar geometry. Issues of dimensional and frequency scaling will be discussed as they apply to large diameter sources. Ion beams extracted from ICPs are used for many applications including space propulsion, high power neutral beams, and materials processing. Broad ion beam (∼10 cm) current densities in excess of 100 mA-cm 2 at 100 keV are obtained in pulsed mode operation. Recently, however, more consumer-oriented applications of less intense ICPs are emerging

  10. Feasibility of asymmetric flow field-flow fractionation coupled to ICP-MS for the characterization of wear metal particles and metalloproteins in biofluids from hip replacement patients

    DEFF Research Database (Denmark)

    Löschner, Katrin; Harrington, Chris F.; Kearney, Jacque-Lucca

    2015-01-01

    or other elements, but the current analytical methods used to investigate the processes involved do not provide sufficient information to understand the size or composition of the wear particles generated in vivo. In this qualitative feasibility study, asymmetric flow field-flow fractionation (AF4) coupled...... to ICP-MS was used to confirm the metal–protein associations in the serum samples. Off-line single particle ICP-MS (spICP-MS) analysis was used to confirm the approximate size distribution indicated by AF4 of the wear particles in hip aspirates. In the serum samples, AF4–ICP-MS suggested that Cr...... unidentified compounds; AEC analysis confirmed the Cr results and the association of Co with Alb and a second compound. Enzymatic digestion of the hip aspirate sample, followed by separation using AF4 with detection by UV absorption (280 nm), multi-angle light scattering and ICP-MS, suggested that the sizes...

  11. Spectroanalytical investigations on inductively coupled N2/Ar and Ar/Ar high frequency plasmas

    International Nuclear Information System (INIS)

    Malinowski, P.; Mazurkiewicz, M.; Nickel, H.

    1981-03-01

    In order to improve the detection limits of trace elements in corrosion products of metallic materials, the inductively coupled plasma excitation source (ICP) was applied for spectroscopic analysis. Besides optimizing the working conditions for the mentioned materials, the fundamental research clearing the excitation processes in ICP was carried out. Basicly, two plasma systems were investigated: the nitrogen cooled N 2 /Ar- and pure Ar/Ar-plasma. The computed detection limits for 8 chosen elements are between 0.1 and 50 μg ml -1 in both plasmas. The advantage of ion lines was clearly present; in N 2 /Ar-plasma it was larger than in Ar/Ar-plasma. The excitation temperatures measured with help of ArI, FeI and ZnI lines rise with increasing power and decreasing distance from the induction coil. The distribution of Zn excitation temperature in N 2 /Ar-plasma as well as the measured N + 2 rotational and CN vibrational temperatures indicate, that the toroidal structure of Ar/Ar-plasma is not analogue to the N 2 /Ar-plasma. The values of the various excitation temperatures (Ar, Fe, Zn) and the differences between the excitation, vibration, rotation and ionization temperatures (Tsub(i) > Tsub(n) = Tsub(vib) > Tsub(rot)) indicate an absence of thermal equilibrium in the concerned system. (orig.)

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

    Science.gov (United States)

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

    2010-08-03

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

  13. Inductively coupled plasma-induced defects in n-type GaN studied from Schottky diode characteristics

    International Nuclear Information System (INIS)

    Nakamura, W.; Tokuda, Y.; Ueda, H.; Kachi, T.

    2006-01-01

    Inductively coupled plasma-(ICP-)induced defects in n-type GaN have been studied from current-voltage (I-V) characteristics and deep-level transient spectroscopy (DLTS) for Schottky diodes fabricated on etched surfaces. The samples after ICP etching show the ohmic I-V characteristics. Schottky characteristics are obtained after annealing at 600 and 800 deg. C in N 2 , but are not restored to that of the control samples. DLTS shows that the effect of ICP etching is small on the region beyond 80 nm from the surface. These results suggest that there remain ICP-induced damage in the near-surface region after thermal annealing

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

    Directory of Open Access Journals (Sweden)

    Q. J. Guo

    2018-02-01

    Full Text Available 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.

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

    International Nuclear Information System (INIS)

    Sanz-Medel, A.

    1991-01-01

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

  16. Mass spectra and ionization temperatures in an argon-nitrogen inductively coupled plasma

    International Nuclear Information System (INIS)

    Houk, R.S.; Montaser, A.; Fassel, V.A.

    1983-01-01

    Positive ions were extracted from the axial channel of an inductively coupled plasma (ICP) in which the outer gas flow was Ar, N 2 , or a mixture of Ar and N 2 . Addition of N 2 to the outer gas decreases the electron number density (n/sub e/) in the axial channel. Ar +2 , O 2 + , and ArH + react with N-containing species in the plasma and/or during the ion extraction process. Ar + remains abundant even if there is no Ar in the outer gas, which indicates the probable occurrence of charge transfer reactions between N 2 + and Ar. The present work corroborates two general concepts upon which several theories of theorigin of suprathermal ionization in ICPs are based: (a) species are physically transported from the induction region to the axial channel; and (b) these species may react with a ionize neutral species in the axial channel. Ionization temperatures (T/sub ion/) measured from the ratio Cd + /I + were 5750 to 6700 K for a N 2 outer flow ICP a forward power of 1.2 kW. This T/sub ion/ range is significantly below that obtained for an Ar outer gas ICP under otherwise similar operating parameters

  17. Plasma edge modelling with ICRF coupling

    Directory of Open Access Journals (Sweden)

    Zhang Wei

    2017-01-01

    Full Text Available The physics of Radio-Frequency (RF wave heating in the Ion Cyclotron Range of Frequencies (ICRF in the core plasmas of fusion devices are relatively well understood while those in the Scrape-Off Layer (SOL remain still unresolved. This paper is dedicated to study the ICRF interactions with the plasma edge, mainly from the theoretical and numerical point of view, in particular with the 3D edge plasma fluid and neutral transport code EMC3-EIRENE and various wave codes. Here emphasis is given to the improvement of ICRF coupling with local gas puffing and to the ICRF induced density convection in the SOL.

  18. The determination of transition probabilities with an inductively-coupled plasma discharge

    International Nuclear Information System (INIS)

    Nieuwoudt, G.

    1984-03-01

    The 27 MHz inductively-coupled plasma discharge (ICP) is used for the determination of relative transition probabilities of the 451, 459 and 470 nm argon spectral lines. The temperature of the argon plasma is determined with hydrogen as thermometric specie, because of the accurate transition probabilities ( approximately 1% uncertainty) there of. The relative transition probabilities of the specific argon spectral lines were determined by substitution of the measured spectral radiances thereof, together with the hydrogen temperature, in the two-line equation of temperature measurement

  19. Coupling of laser energy into plasma channels

    International Nuclear Information System (INIS)

    Dimitrov, D. A.; Giacone, R. E.; Bruhwiler, D. L.; Busby, R.; Cary, J. R.; Geddes, C. G. R.; Esarey, E.; Leemans, W. P.

    2007-01-01

    Diffractive spreading of a laser pulse imposes severe limitations on the acceleration length and maximum electron energy in the laser wake field accelerator (LWFA). Optical guiding of a laser pulse via plasma channels can extend the laser-plasma interaction distance over many Rayleigh lengths. Energy efficient coupling of laser pulses into and through plasma channels is very important for optimal LWFA performance. Results from simulation parameter studies on channel guiding using the particle-in-cell (PIC) code VORPAL [C. Nieter and J. R. Cary, J. Comput. Phys. 196, 448 (2004)] are presented and discussed. The effects that density ramp length and the position of the laser pulse focus have on coupling into channels are considered. Moreover, the effect of laser energy leakage out of the channel domain and the effects of tunneling ionization of a neutral gas on the guided laser pulse are also investigated. Power spectral diagnostics were developed and used to separate pump depletion from energy leakage. The results of these simulations show that increasing the density ramp length decreases the efficiency of coupling a laser pulse to a channel and increases the energy loss when the pulse is vacuum focused at the channel entrance. Then, large spot size oscillations result in increased energy leakage. To further analyze the coupling, a differential equation is derived for the laser spot size evolution in the plasma density ramp and channel profiles are simulated. From the numerical solution of this equation, the optimal spot size and location for coupling into a plasma channel with a density ramp are determined. This result is confirmed by the PIC simulations. They show that specifying a vacuum focus location of the pulse in front of the top of the density ramp leads to an actual focus at the top of the ramp due to plasma focusing, resulting in reduced spot size oscillations. In this case, the leakage is significantly reduced and is negligibly affected by ramp length

  20. Trace element determination in seawater by ICP-SFMS coupled with a microflow nebulization/desolvation system

    International Nuclear Information System (INIS)

    Turetta, Clara; Cozzi, Giulio; Barbante, Carlo; Capodaglio, Gabriele; Cescon, Paolo

    2004-01-01

    Direct and simultaneous determination of Al, Ag, As, Cd, Co, Cr, Cu, Fe, Mn, Mo, Pb, Sb, U, V and Zn in diluted (1:10 v:v) seawater from the Antarctic Ocean and the Venice Lagoon at the ng mL -1 and pg mL -1 level has been performed by using an inductively coupled plasma sector field mass spectrometer (ICP-SFMS). Samples were analysed by using a PFA microflow nebulizer coupled with a desolvation system or a PFA microflow nebulizer coupled with a Teflon spray chamber, respectively. Measurements were carried out at low (LR, m/Δm=300), medium (MR, m/Δm=3,000) and high (HR, m/Δm=7,500) resolutions depending on the studied isotope. To avoid contamination, sample pre-treatment was carried out in a clean laboratory equipped with a Class 100 vertical laminar flow hood. Concentration ranges (minimum-maximum in ng mL -1 ) found in the Antarctic seawater samples (in depth profiles) were: Ag 0.0004-0.0018, As 0.69-1.32, Cd 0.031-0.096, Co 0.018-0.065, Cr 0.18-0.46, Cu 0.04-1.58, Fe 0.13-1.63, Mn 0.02-0.12, Mo 5.97-12.46, Pb 0.007-0.074, Sb 0.033-0.088, U 0.5-1.9, V 0.6-2.5 and Zn 0.16-0.80. Concentration ranges (min-max in ng mL -1 ) found in the Venice Lagoon water samples (temporal profile from a benthic chamber experiment) were: Al 0.24-0.61, Ag 0.007-0.031, As 1.42-2.27, Cd 0.050-0.182, Co 0.440-1.461, Cr 0.15-0.34, Cu 0.81-2.46, Fe 0.25-1.66, Mn 11.6-31.7, Mo 6.50-10.6, Pb 0.047-0.225, Sb 0.240-0.492, U 1.7-3.3, V 1.3-2.8 and Zn 5.20-21.5. The detection limits range between 0.06 pg mL -1 for Ag and U to 15 pg mL -1 for Fe. In order to check the accuracy of the analytical procedure, measurements of the trace elements in a certified reference material (coastal Atlantic seawater, CASS-4-NRCC) were compared with the certified values. In addition, the results from the Antarctic and Venice Lagoon samples were compared with those obtained by using different analytical techniques. (orig.)

  1. Wavelength scaling of laser plasma coupling

    International Nuclear Information System (INIS)

    Kruer, W.L.

    1983-01-01

    The use of shorter wavelength laser light both enhances collisional absorption and reduces deleterious collective plasma effects. Coupling processes which can be important in reactor-size targets are briefly reviewed. Simple estimates are presented for the intensity-wavelength regime in which collisional absorption is high and collective effects are minimized

  2. Energy coupling in the plasma focus

    International Nuclear Information System (INIS)

    Wainwright, T.E.; Pickles, W.L.; Sahlin, H.L.; Price, D.F.

    1979-01-01

    Experiments have been performed with a 125-kJ plasma focus to investigate mechanisms for rapid coupling of inductively-stored energy into plasmas. The coupling can take place through the formation of an electron or ion beam that deposits its energy in a target or directly by the penetration of the magnetic field into a resistive plasma. Some preliminary results from experiments of both types are described. The experiments use a replaceable conical anode tip that is intended to guide the focus to within a few millimeters of the axis, where it can suddenly deliver energy either to a small target or to particles that are accelerated. X-ray and fast-ion diagnostics have been used to study the effects

  3. Effect of single aerosol droplets on plasma impedance in the inductively coupled plasma

    Energy Technology Data Exchange (ETDEWEB)

    Chan, George C.-Y., E-mail: gcchan@indiana.edu; Zhu, Zhenli; Hieftje, Gary M.

    2012-10-15

    forward power, contribute to both the jitter and the reduced trigger efficiency. The noise components that increase sharply with plasma forward power are at audio-frequencies between 150 and 300 Hz, and are attributed to gas dynamics in the plasma. - Highlights: Black-Right-Pointing-Pointer Single water-droplet introduction on the plasma impedance of an ICP was monitored. Black-Right-Pointing-Pointer A single 10-pL droplet causes a readily measurable change in plasma impedance. Black-Right-Pointing-Pointer Change in plasma impedance is directly proportional to droplet volume. Black-Right-Pointing-Pointer Change in peak RF power and total energy coupled into the plasma was estimated. Black-Right-Pointing-Pointer Noise power spectra of RF-probe coil and phase detector signals were computed.

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

    International Nuclear Information System (INIS)

    Kretschy, Daniela; Koellensperger, Gunda; Hann, Stephan

    2012-01-01

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

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

    International Nuclear Information System (INIS)

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

    2003-01-01

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

  6. Experimental control of the solvent load of inductively coupled argon plasmas and effects of the chloroform plasma load on their analytical performance

    Science.gov (United States)

    Maessen, F. J. M. J.; Kreuning, G.; Balke, J.

    The solvent plasma load ( QSPL) of water, methanol and chloroform was established as a function of the liquid uptake rate ( QL) by using a continuous weighing method for recording the rate differences between the relevant liquid streams. The shape of the QL vs QSPL curves revealed that the liquid uptake rate is a parameter much too insensitive to serve as a criterion for assessing the stability of "organic" plasmas. The quantity "maximum tolerable solvent plasma load" is suggested as a more useful criterion. Effects of rf power, observation height and solvent plasma load on the properties of chloroform inductively coupled plasmas (ICPs) are reported. The measurement of the axial distribution of net line intensities of representative spectral lines showed that the behaviour of emission lines as to their "hardness" is essentially the same in ICPs loaded with chloroform or water. The chloroform plasma load was regulated by the use of a condenser of which the temperature was varied in a range between -50°C and +20°C. Analytical performance characteristics such as net line and background intensities, signal-to-background ratios, and relative standard deviations of the background signal are presented for ICPs with various chloroform loads. Two sets of experimental conditions were finally selected for simultaneous multielement analysis of chloroform solvent solutions, one with and one without aerosol cooling. In the case that aerosol cooling was applied, the detection limits were similar to those for aqueous plasmas. Without aerosol cooling the detection limits were up to an order of magnitude poorer. An attempt has been made to catagorize organic solvents on the basis of both volatility and their behaviour in ICP systems. For a better understanding of the consequences of solvent volatility in ICP-AES it is of importance to consider separately the properties that determine the volatility of liquids, viz. the evaporation rate and the saturation vapour pressure.

  7. Enhanced laser beam coupling to a plasma

    International Nuclear Information System (INIS)

    Steiger, A.D.; Woods, C.H.

    1976-01-01

    Density perturbations are induced in a heated plasma by means of a pair of oppositely directed, polarized laser beams of the same frequency. The wavelength of the density perturbations is equal to one half the wavelength of the laser beams. A third laser beam is linearly polarized and directed at the perturbed plasma along a line that is perpendicular to the direction of the two opposed beams. The electric field of the third beam is oriented to lie in the plane containing the three beams. The frequency of the third beam is chosen to cause it to interact resonantly with the plasma density perturbations, thereby efficiently coupling the energy of the third beam to the plasma. 10 claims, 2 figures

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

    International Nuclear Information System (INIS)

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

    2008-01-01

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

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

    International Nuclear Information System (INIS)

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

    2008-01-01

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

  10. InAs0.45P0.55/InP strained multiple quantum wells intermixed by inductively coupled plasma etching

    International Nuclear Information System (INIS)

    Cao, Meng; Wu, Hui-Zhen; Lao, Yan-Feng; Cao, Chun-Fang; Liu, Cheng

    2009-01-01

    The intermixing effect on InAs 0.45 P 0.55 /InP strained multiple quantum wells (SMQWs) by inductively coupled plasma (ICP) etching and rapid thermal annealing (RTA) is investigated. Experiments show that the process of ICP etching followed RTA induces the blue shift of low temperature photoluminescence (PL) peaks of QWs. With increasing etching depth, the PL intensities are firstly enhanced and then diminished. This phenomenon is attributed to the variation of surface roughness and microstructure transformation inside the QW structure during ICP processing.

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

    DEFF Research Database (Denmark)

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

    2000-01-01

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

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

    International Nuclear Information System (INIS)

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

    2000-01-01

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

  13. The PERC trademark process: Existing and potential applications for induction coupled plasma technology in hazardous and radioactive waste treatment

    International Nuclear Information System (INIS)

    Blutke, A.S.; Vavruska, J.S.; Serino, J.F.

    1996-01-01

    Plasma Technology, Inc. (PTI), a Santa Fe, New Mexico corporation has developed the Plasma Energy Recycle and Conversion (PERC)trademark treatment process as a safe and environmentally clean alternative to conventional thermal destruction technologies. The PERC trademark treatment process uses as its heat source an advanced Induction Coupled Plasma (ICP) torch connected to a reaction chamber system with an additional emission control system. For example, organic-based gas, liquid, slurry, and/or solid waste streams can be converted into usable or even salable products while residual emissions are reduced to an absolute minimum. In applications for treatment of hazardous and radioactive waste streams, the PERC system could be used for destruction of the hazardous organic constituents and/or significant waste volume reduction while capturing the radioactive fraction in a non-leachable form. Like Direct Current (DC) and Alternating Current (AC) arc plasma systems, ICP torches offer sufficient energy to decompose, melt and/or vitrify any waste stream. The decision for an arc plasma or an IC plasma system has to be made on a case by case evaluation and is highly dependent on the specific waste stream's form and composition. Induction coupled plasma technology offers one simple, but significant difference compared to DC or AC arc plasma systems: the ICP torch is electrodeless. To date, enormous research effort has been spent to improve the lifetime of electrodes and the effectiveness of related cooling systems. Arc plasma systems are established in research laboratories worldwide and are approaching a broad use in commercial applications. ICP technology has been improved relatively recently, but nowadays offers complete new and beneficial approaches in the field of waste conversion and treatment

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

    Data.gov (United States)

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

  15. Improved documentation of spectral lines for inductively coupled plasma emission spectrometry

    Science.gov (United States)

    Doidge, Peter S.

    2018-05-01

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

  16. Mode coupling of electron plasma waves

    International Nuclear Information System (INIS)

    Harte, J.A.

    1975-01-01

    The driven coupled mode equations are derived for a two fluid, unequal temperature (T/sub e/ much greater than T/sub i/) plasma in the one-dimensional, electrostatic model and applied to the coupling of electron plasma waves. It is assumed that the electron to ion mass ratio identical with m/sub e/M/sub i// much less than 1 and eta 2 /sub ko/k lambda/sub De/ less than 1 where eta 2 /sub ko/ is the pump wave's power normalized to the plasma thermal energy, k the mode wave number and lambda/sub De/ the electron Debye length. Terms up to quadratic in pump power are retained. The equations describe the linear plasma modes oscillating at the wave number k and at ω/sub ek/, the Bohn Gross frequency, and at Ω/sub k/, the ion acoustic frequency, subject to the damping rates ν/sub ek/ and ν/sub ik/ for electrons and ions and their interactions due to intense high frequency waves E/sub k//sup l/. n/sub o/ is the background density, n/sub ik/ the fluctuating ion density, ω/sub pe/ the plasma frequency

  17. Effect of sample matrix on the fundamental properties of the inductively coupled plasma

    International Nuclear Information System (INIS)

    Lehn, Scott A.; Warner, Kelly A.; Huang Mao; Hieftje, Gary M.

    2003-01-01

    In the inductively coupled plasma (ICP), the emission intensities of atomic and ionic spectral lines are controlled by fundamental parameters such as electron temperature, electron number density, gas-kinetic temperature, analyte atom and ion number densities, and others. Accordingly, the effect of a sample matrix on the analyte emission intensity in an ICP might be attributable to changes in these fundamental parameters caused by the matrix elements. In the present study, a plasma imaging instrument that combines Thomson scattering, Rayleigh scattering, laser-induced fluorescence and computed tomography has been employed to measure the above-mentioned parameters in the presence and absence of matrix elements. The data thus obtained were all collected on a spatially resolved basis and without the need for Abel inversion. Calcium, strontium and barium served as analytes, while lithium, copper and zinc were introduced as matrix elements. Comparing the data with and without the matrix elements allows us to determine the extent to which each fundamental parameter changes in the presence of a matrix element, and to better understand the nature of the matrix effects that occur in the ICP. As has been seen in previous studies with different matrix elements, ion emission and ion number densities follow opposite trends when matrix interferents are introduced into the plasma: ion emission is enhanced by the presence of matrix interferents while ion concentrations are lowered. These changes are consistent with a shift from collisional deactivation to radiative decay of excited-state analyte species

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

    International Nuclear Information System (INIS)

    Niu, Hongsen.

    1995-01-01

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

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

    International Nuclear Information System (INIS)

    He Man; Hu, Bin; Jiang Zucheng

    2005-01-01

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

  20. Multielemental fractionation in human peripheral blood mononuclear cells by size exclusion liquid chromatography coupled to UV and ICP-MS detection.

    Science.gov (United States)

    Alvarado, Gladys; Murillo, Miguel

    2010-10-01

    An analytical methodology is presented in this work to determine metal-biomolecule complexes size distribution patterns of several elements, among different compounds present in human peripheral blood mononuclear cells (PBMC). A hyphenated technique based on size exclusion chromatography (SEC) coupled online to UV and inductively coupled plasma mass spectrometry (ICP-MS) detection is used. Two different SEC columns with separation ranges between 1,500-1,000,000 relative molecular mass (M(r)) (Nanofilm SEC-250) and 5,000 and 100,000 relative molecular mass (M(r)) (TSK-Gel G2000 SW) are used with 10 mmol/L tris-HCl at pH 7.3 as mobile phase. Retention behavior (retention time and peak-area ratios) remained unchanged for several successive separations. Metal-containing compounds are found to a wide range of M(r). Copper-zinc superoxide dismutase, copper and zinc metallothionein, and copper and zinc transferrin are identified in PBMC samples. A high M(r) (147,000) metal-binding protein containing copper and zinc and a high M(r) (107,000) manganese-binding protein were also found; however, these remained unknown.

  1. Rapid determination of 99Tc in environmental samples by high resolution ICP-MS coupled with on-line flow injection system

    International Nuclear Information System (INIS)

    Kim, C.K.; Kim, C.S.; Rho, B.H.; Lee, J.I.

    2002-01-01

    High resolution inductively coupled plasma mass spectrometry coupled with an on-line flow injection system (FI-HR-ICP-MS) was applied to determine the ultra-trace level 99 Tc in soil. The flow injection system (PrepLab TM ) was composed of two TEVA-Spec R resins, reduced remarkably the sample amounts and the analysis time, compared to the conventional analytical methods. In the flow injection system, Mo and Ru were sufficiently eliminated by using the flow injection system, with the decontamination factors of 1.6 x 10 4 and 9.9 x 10 5 , respectively. With the present method, it was possible to determine ultra-low level of 99 Tc in 3∼6 soil at 3-5 hours of analysis time per sample. The relative standard deviation for each sample was less than 4%. The detection limits for 99 Tc was 85 fg x ml -1 (0.05 mBq x ml -1 ), which was calculated from the three times standard deviation of the count rate of the blank. (author)

  2. Self-consistent simulation study on magnetized inductively coupled plasma for 450 mm semiconductor wafer processing

    International Nuclear Information System (INIS)

    Lee, Ho-Jun; Kim, Yun-Gi

    2012-01-01

    The characteristics of weakly magnetized inductively coupled plasma (MICP) are investigated using a self-consistent simulation based on the drift–diffusion approximation with anisotropic transport coefficients. MICP is a plasma source utilizing the cavity mode of the low-frequency branch of the right-hand circularly polarized wave. The model system is 700 mm in diameter and has a 250 mm gap between the radio-frequency window and wafer holder. The model chamber size is chosen to verify the applicability of this type of plasma source to the 450 mm wafer process. The effects of electron density distribution and external axial magnetic field on the propagation properties of the plasma wave, including the wavelength modulation and refraction toward the high-density region, are demonstrated. The restricted electron transport and thermal conductivity in the radial direction due to the magnetic field result in small temperature gradient along the field lines and off-axis peak density profile. The calculated impedance seen from the antenna terminal shows that MICP has a resistance component that is two to threefold higher than that of ICP. This property is practically important for large-size, low-pressure plasma sources because high resistance corresponds to high power-transfer efficiency and stable impedance matching characteristics. For the 0.665 Pa argon plasma, MICP shows a radial density uniformity of 6% within 450 mm diameter, which is much better than that of nonmagnetized ICP.

  3. Surface properties of indium tin oxide treated by Cl2 inductively coupled plasma

    International Nuclear Information System (INIS)

    He, Kongduo; Yang, Xilu; Yan, Hang; Gong, Junyi; Zhong, Shaofeng; Ou, Qiongrong; Liang, Rongqing

    2014-01-01

    Graphical abstract: - Highlights: • The work function of chlorinated ITO increases initially by up to 1 eV. • The chlorinated ITO keeps an increment of work function of 0.3 eV after 100 days. • The WF decrease curves can be fitted with double exponential functions. • The desorption of unstable Cl in the surface leads to the rapid decrease of WF. • The core levels of In 3d5 and Sn 3d5 and O 1s shift toward higher binding energies. - Abstract: The effects of Cl 2 inductively coupled plasma (ICP) treatment on the time dependence of work function (WF) and surface properties of indium tin oxide (ITO) were investigated. Kelvin probe (KP) measurements show that the WF after Cl 2 ICP treatment is close to 5.9 eV. The WF decrease curve of Cl 2 plasma treated ITO is fitted with double exponential functions with an adjusted R-square of 0.99. The mechanism under the decrease process is discussed by X-ray photoelectron spectroscopy (XPS). The ITO WF decrease after Cl 2 ICP treatment performs much better than that after O 2 ICP treatment and the chlorinated ITO keeps a WF increment of 0.3 eV compared with that without plasma treatment after 100 days. Other properties of chlorinated ITO surface such as morphology and transmittance change slightly. The results are significant for the understanding of degradation of Cl 2 plasma treated ITO and the fabrication of organic semiconductor devices

  4. Surface properties of indium tin oxide treated by Cl{sub 2} inductively coupled plasma

    Energy Technology Data Exchange (ETDEWEB)

    He, Kongduo; Yang, Xilu; Yan, Hang; Gong, Junyi; Zhong, Shaofeng [Department of Light Sources and Illuminating Engineering, Fudan University, Shanghai 200433 (China); Ou, Qiongrong, E-mail: qrou@fudan.edu.cn [Department of Light Sources and Illuminating Engineering, Fudan University, Shanghai 200433 (China); Engineering Research Center of Advanced Lighting Technology, Ministry of Education, Shanghai 200433 (China); Liang, Rongqing [Department of Light Sources and Illuminating Engineering, Fudan University, Shanghai 200433 (China); Engineering Research Center of Advanced Lighting Technology, Ministry of Education, Shanghai 200433 (China)

    2014-10-15

    Graphical abstract: - Highlights: • The work function of chlorinated ITO increases initially by up to 1 eV. • The chlorinated ITO keeps an increment of work function of 0.3 eV after 100 days. • The WF decrease curves can be fitted with double exponential functions. • The desorption of unstable Cl in the surface leads to the rapid decrease of WF. • The core levels of In 3d5 and Sn 3d5 and O 1s shift toward higher binding energies. - Abstract: The effects of Cl{sub 2} inductively coupled plasma (ICP) treatment on the time dependence of work function (WF) and surface properties of indium tin oxide (ITO) were investigated. Kelvin probe (KP) measurements show that the WF after Cl{sub 2} ICP treatment is close to 5.9 eV. The WF decrease curve of Cl{sub 2} plasma treated ITO is fitted with double exponential functions with an adjusted R-square of 0.99. The mechanism under the decrease process is discussed by X-ray photoelectron spectroscopy (XPS). The ITO WF decrease after Cl{sub 2} ICP treatment performs much better than that after O{sub 2} ICP treatment and the chlorinated ITO keeps a WF increment of 0.3 eV compared with that without plasma treatment after 100 days. Other properties of chlorinated ITO surface such as morphology and transmittance change slightly. The results are significant for the understanding of degradation of Cl{sub 2} plasma treated ITO and the fabrication of organic semiconductor devices.

  5. Bright branes for strongly coupled plasmas

    International Nuclear Information System (INIS)

    Mateos, David; Patino, Leonardo

    2007-01-01

    We use holographic techniques to study photon production in a class of finite temperature, strongly coupled, large-N c SU(N c ) quark-gluon plasmas with N f c quark flavours. Our results are valid to leading order in the electromagnetic coupling constant but non-perturbatively in the SU(N c ) interactions. The spectral function of electromagnetic currents and other related observables exhibit an interesting structure as a function of the photon frequency and the quark mass. We discuss possible implications for heavy ion collision experiments

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

    Directory of Open Access Journals (Sweden)

    R. Bazurto

    2018-04-01

    Full Text Available 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.

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

    International Nuclear Information System (INIS)

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

    2008-01-01

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

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

    International Nuclear Information System (INIS)

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

    1998-01-01

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

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    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.

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

  12. Design Considerations in Capacitively Coupled Plasmas

    Science.gov (United States)

    Song, Sang-Heon; Ventzek, Peter; Ranjan, Alok

    2015-11-01

    Microelectronics industry has driven transistor feature size scaling from 10-6 m to 10-9 m during the past 50 years, which is often referred to as Moore's law. It cannot be overstated that today's information technology would not have been so successful without plasma material processing. One of the major plasma sources for the microelectronics fabrication is capacitively coupled plasmas (CCPs). The CCP reactor has been intensively studied and developed for the deposition and etching of different films on the silicon wafer. As the feature size gets to around 10 nm, the requirement for the process uniformity is less than 1-2 nm across the wafer (300 mm). In order to achieve the desired uniformity, the hardware design should be as precise as possible before the fine tuning of process condition is applied to make it even better. In doing this procedure, the computer simulation can save a significant amount of resources such as time and money which are critical in the semiconductor business. In this presentation, we compare plasma properties using a 2-dimensional plasma hydrodynamics model for different kinds of design factors that can affect the plasma uniformity. The parameters studied in this presentation include chamber accessing port, pumping port, focus ring around wafer substrate, and the geometry of electrodes of CCP.

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

    International Nuclear Information System (INIS)

    Hall, G.S.

    1990-01-01

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

  14. Data on final calcium concentration in native gel reagents determined accurately through inductively coupled plasma measurements

    Directory of Open Access Journals (Sweden)

    Jeffrey Viviano

    2016-03-01

    Full Text Available In this article we present data on the concentration of calcium as determined by Inductively Coupled Plasma (ICP measurements. Calcium was estimated in the reagents used for native gel electrophoresis of Neuronal Calcium Sensor (NCS proteins. NCS proteins exhibit calcium-dependent mobility shift in native gels. The sensitivity of this shift to calcium necessitated a precise determination of calcium concentrations in all reagents used. We determined the calcium concentrations in different components used along with the samples in the native gel experiments. These were: 20 mM Tris pH 7.5, loading dye and running buffer, with distilled water as reference. Calcium determinations were through ICP measurements. It was found that the running buffer contained calcium (244 nM over the blank. Keywords: Neuronal calcium sensor proteins, Electrophoresis, Mobility shift, Calcium, Magnesium

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

    International Nuclear Information System (INIS)

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

    2017-01-01

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

  16. Analysis of bauxite by inductively coupled plasma-atomic emission spectroscopy

    Science.gov (United States)

    Barnes, Ramon M.; Mahanti, Himansu S.

    Methods are described for the analysis of bauxite by inductively coupled plasma (ICP) emission spectroscopy. Bauxite samples were dissolved either in HCl, HNO 3, and HF at 160°C in all-PTFE bomb or fused with NaOH. Spectral lines were selected after examination of experimental wavelength scans at each potential analyte wavelength. Limits of detection, background equivalent concentration, and analytical figures of merit were established. The accuracy of the method was confirmed by determining 17 elements in NBS-SRM bauxite samples. Silicon in HF solutions was analyzed using a modified ICP torch with a graphite injector tube, an inert nebulizer using PTFE capillary tubes, and a PTFE spray chamber.

  17. High-rate reduction of copper oxide using atmospheric-pressure inductively coupled plasma microjets

    International Nuclear Information System (INIS)

    Tajima, Satomi; Tsuchiya, Shouichi; Matsumori, Masashi; Nakatsuka, Shigeki; Ichiki, Takanori

    2011-01-01

    Reduction of copper oxide was performed using an atmospheric-pressure inductively coupled plasma (AP-ICP) microjet while varying the input power P between 15 and 50 W. Cuprous oxide (Cu 2 O) and cupric oxide (CuO) were formed on the sputtered Cu surface by thermal annealing. Dynamic behavior of the microplasma jet, optical emission from H atoms, the substrate temperature, chemical bonding states of the treated surface, and the thickness of the reduced Cu layer were measured to study the fundamental reduction process. Surface composition and the thickness of the reduced Cu layer changed significantly with P. Rapid reduction of CuO and Cu 2 O was achieved at a rate of 493 nm/min at P = 50 W since high-density H atoms were produced by the AP-ICP microjet.

  18. High-rate reduction of copper oxide using atmospheric-pressure inductively coupled plasma microjets

    Energy Technology Data Exchange (ETDEWEB)

    Tajima, Satomi; Tsuchiya, Shouichi [Department of Bioengineering, Graduate School of Engineering, University of Tokyo, 2-11-16 Yayoi, Bunkyo-ku, 113-8656 (Japan); Matsumori, Masashi; Nakatsuka, Shigeki [Panasonic Factory Solutions Co., Ltd., 2-7 Matsuba-cho, Kadoma-city, Osaka, 571-8502 (Japan); Ichiki, Takanori, E-mail: ichiki@sogo.t.u-tokyo.ac.jp [Department of Bioengineering, Graduate School of Engineering, University of Tokyo, 2-11-16 Yayoi, Bunkyo-ku, 113-8656 (Japan); Institute of Engineering Innovation, Graduate School of Engineering, University of Tokyo, 2-11-16 Yayoi, Bunkyo-ku, Tokyo, 113-8656 (Japan)

    2011-08-01

    Reduction of copper oxide was performed using an atmospheric-pressure inductively coupled plasma (AP-ICP) microjet while varying the input power P between 15 and 50 W. Cuprous oxide (Cu{sub 2}O) and cupric oxide (CuO) were formed on the sputtered Cu surface by thermal annealing. Dynamic behavior of the microplasma jet, optical emission from H atoms, the substrate temperature, chemical bonding states of the treated surface, and the thickness of the reduced Cu layer were measured to study the fundamental reduction process. Surface composition and the thickness of the reduced Cu layer changed significantly with P. Rapid reduction of CuO and Cu{sub 2}O was achieved at a rate of 493 nm/min at P = 50 W since high-density H atoms were produced by the AP-ICP microjet.

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

    Science.gov (United States)

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

    2014-01-01

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

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

    International Nuclear Information System (INIS)

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

    2009-01-01

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

  1. DC plasma ion implantation in an inductively coupled RF plasma

    International Nuclear Information System (INIS)

    Silawatshananai, C.; Matan, N.; Pakpum, C.; Pussadee, N.; Srisantitam, P.; Davynov, S.; Vilaithong, T.

    2004-01-01

    Various modes of plasma ion implantation have been investigated in a small inductively coupled 13.6 MHz RF plasma source. Plasma ion implantation with HVDC(up to -10 kV bias) has been investigated in order to incorporate with the conventional implantation of diamond like carbon. In this preliminary work, nitrogen ions are implanted into the stainless steel sample with a dose of 5.5 x 10 -2 cm for a short implanting time of 7 minutes without target cooling. Surface properties such as microhardness, wear rate and the friction coefficient have been improved. X-ray and SEM analyses show distinct structural changes on the surface. A combination of sheath assisted implantation and thermal diffusion may be responsible for improvement in surface properties. (orig.)

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

    International Nuclear Information System (INIS)

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

    2011-01-01

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

  3. Inductively coupled plasma--atomic emission spectroscopy: an evaluation of the use of nitrogen--argon admixtures as plasma discharge atmospheres

    International Nuclear Information System (INIS)

    Zalewski, J.C.

    1979-01-01

    The effects of the use of nitrogen in either the plasma coolant or aerosol carrier gas flows on the physical and spectrochemical properties of the inductively coupled plasma (ICP) were examined. While the plasma operated with nitrogen in the coolant flow exhibited a stability comparable to that of the argon plasma, the use of nitrogen in the aerosol carrier gas flow resulted in a plasma that was less stable. The detection limits obtained for the three plasmas exhibited a similar trend. In addition, the use of nitrogen--argon admixtures in the plasma coolant gas flow yielded an increase in both the net analyte and the background emission intensities when the corresponding argon and nitrogen--argon plasmas were operated under various conditions. Furthermore, the effect of aluminum on the Ca II (393.4 nm) spectral line was reported for the 1000/1 Al/Ca molar ratio. At an observation height of 15 mm, the signal depressions were 4 and 14% for the nitrogen--argon and the argon plasmas, respectively. The above experimental evidence suggested that the operation of the ICP with an Ar--N 2 coolant gas might be hotter than the argon plasma currently in use in this laboratory. The demountable plasma torch designed in collaboration with K. Olson yielded detection limits for 15 elements and 19 spectral lines that were approximately within a factor of two of those obtained with the torch of fused quartz design. The design also appeared to offer a more readily initiated plasma discharge. The experimental evidence presented supports the utilization of nitrogen--argon admixtures in the plasma coolant gas flow as alternate discharge atmospheres for inductively coupled plasma--atomic emission spectroscopy. In contrast, the experimental evidence shows that there is a deterioration in both physical and spectrochemical properties of plasmas operated with a nitrogen aerosol carrier gas

  4. Study of sterilization-treatment in pure and N- doped carbon thin films synthesized by inductively coupled plasma assisted pulsed-DC magnetron sputtering

    Energy Technology Data Exchange (ETDEWEB)

    Javid, Amjed [Center for Advanced Plasma Surface Technology (CAPST), NU-SKKU Joint Institute for Plasma Nano-Materials (IPNM), Advanced Materials Science and Engineering, Sungkyunkwan University, Suwon 440-746 (Korea, Republic of); Department of Textile Processing, National Textile University, Faisalabad 37610 (Pakistan); Kumar, Manish, E-mail: manishk@skku.edu [Center for Advanced Plasma Surface Technology (CAPST), NU-SKKU Joint Institute for Plasma Nano-Materials (IPNM), Advanced Materials Science and Engineering, Sungkyunkwan University, Suwon 440-746 (Korea, Republic of); Han, Jeon Geon, E-mail: hanjg@skku.edu [Center for Advanced Plasma Surface Technology (CAPST), NU-SKKU Joint Institute for Plasma Nano-Materials (IPNM), Advanced Materials Science and Engineering, Sungkyunkwan University, Suwon 440-746 (Korea, Republic of)

    2017-01-15

    Highlights: • Pure and N-doped nanocrystallie carbon films are synthesized by ICP assisted pulsed DC plasma process. • ICP power induces the increase in average graphitic crystallite size from 4.86 nm to 6.42 nm. • Beneficial role of ICP source assistance to achieve high sputtering throughput (deposition rate ∼55 nm/min). • Post-sterilization electron-transport study shows N-doped carbon films having promising stability. - Abstract: Electrically-conductive nanocrystalline carbon films, having non-toxic and non-immunogenic characteristics, are promising candidates for reusable medical devices. Here, the pure and N- doped nanocrystalline carbon films are deposited by the assistance of inductively coupled plasma (ICP) in an unbalanced facing target pulsed-DC magnetron sputtering process. Through the optical emission spectroscopy study, the role of ICP assistance and N-doping on the reactive components/radicals during the synthesis is presented. The N-doping enhances the three fold bonding configurations by increasing the ionization and energies of the plasma species. Whereas, the ICP addition increases the plasma density to control the deposition rate and film structure. As a result, sputtering-throughput (deposition rate: 31–55 nm/min), electrical resistivity (4–72 Ωcm) and water contact angle (45.12°–54°) are significantly tailored. Electric transport study across the surface microchannel confirms the superiority of N-doped carbon films for sterilization stability over the undoped carbon films.

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

    Energy Technology Data Exchange (ETDEWEB)

    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 atlas 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.

  6. Atlas of Atomic Spectral Lines of Neptunium Emitted by an Inductively Coupled Plasma

    International Nuclear Information System (INIS)

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

    1987-01-01

    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 atlas 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.

  7. Chemical characterization of materials by inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

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

    2009-11-01

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

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

    International Nuclear Information System (INIS)

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

    1994-01-01

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

  9. Environmental samples analysis by Atomic Absorption Spectrophotometry and Inductively Coupled Plasma-Optical Emission Spectroscopy

    International Nuclear Information System (INIS)

    Popescu, I.V.; Iordan, M.; Stihi, C.; Bancuta, A.; Busuioc, G.; Dima, G.; Ciupina, V.; Belc, M.; Vlaicu, Gh.; Marian, R.

    2002-01-01

    Biological samples are interesting from many aspects of environmental monitoring. By analyzing tree leaves conclusions can be drown regarding the metal loading in the growth medium. So that, starting from assumption that the pollution factors from environmental medium can modify the normal concentration of elements, we decided to control the presence of toxic elements and the deviation from normal state of elements in leaves of different trees from areas situated at different distances of pollution source. The aim of this work is to determine the elemental composition of tree leaves using Atomic Absorption Spectrophotometry (AAS) method and Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES) method. Using AAS spectrophotometer SHIMADZU we identified and determined the concentration of: Cd, Co, Cu, Zn, Mn, Cr, Fe, Se, Pb with an instrumental error less than 1% for most of the elements analyzed. The same samples were analyzed by ICP-OES spectrometer, BAIRD ICP2070-Sequential Plasma spectrometer. We identified and determined in leaves of different trees the concentration of Mg, Ca, and Sr with a precision less than 6%. (authors)

  10. Level population measurements on analyte atom and ion excited states in the inductively coupled plasma

    International Nuclear Information System (INIS)

    Walker, Z.H.; Blades, M.W.

    1986-01-01

    During the past decade a number of publications dealing with fundamental studies of the inductively coupled plasma (ICP) have appeared in the literature. The purpose of many of these investigations has been to understand the nature of the interaction between the plasma gas and the analyte. The general conclusion drawn from these studies has been that the ICP is very close to Local Thermodynamic Equilibrium (LTE), but that some deviations from LTE do occur. Recent studies by the authors' have been directed towards the measurement of analyte atom and ion excited state level populations with the objective of obtaining a better understanding of both ionization and excitation in the ICP discharge and the extent to which such processes contribute to a non-equilibrium state. Further discussion is drawn from similar measurements made on elements with low ionization potentials, such as Barium, as well as on elements such as Iron in the presence of Easily Ionizable Elements (EIE's). The spatial and power dependences of such measurements are also discussed

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

    International Nuclear Information System (INIS)

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

    2004-01-01

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

  12. Characterization of silicon isotropic etch by inductively coupled plasma etcher for microneedle array fabrication

    International Nuclear Information System (INIS)

    Ji, J; Tay, F E H; Miao Jianmin; Sun Jianbo

    2006-01-01

    This work investigates the isotropic etching properties in inductively coupled plasma (ICP) etcher for microneedle arrays fabrication. The effects of process variables including powers, gas and pressure on needle structure generation are characterized by factorial design of experiment (DOE). The experimental responses of vertical etching depth, lateral etching length, ratio of vertical etching depth to lateral etching length and photoresist etching rate are reported. The relevance of the etching variables is also presented. The obtained etching behaviours for microneedle structure generation will be applied to develop recipes to fabricate microneedles in designed dimensions

  13. Characterization of silicon isotropic etch by inductively coupled plasma etcher for microneedle array fabrication

    Energy Technology Data Exchange (ETDEWEB)

    Ji, J [Mechanical Engineering National University of Singapore, 119260, Singapore (Singapore); Tay, F E H [Mechanical Engineering National University of Singapore, 119260, Singapore (Singapore); Miao Jianmin [MicroMachines Center, School of Mechanical and Aerospace Engineering, Nanyang Technologica l University, 50 Nanyang Avenue, 639798 (Singapore); Sun Jianbo [MicroMachines Center, School of Mechanical and Aerospace Engineering, Nanyang Technologica l University, 50 Nanyang Avenue, 639798 (Singapore)

    2006-04-01

    This work investigates the isotropic etching properties in inductively coupled plasma (ICP) etcher for microneedle arrays fabrication. The effects of process variables including powers, gas and pressure on needle structure generation are characterized by factorial design of experiment (DOE). The experimental responses of vertical etching depth, lateral etching length, ratio of vertical etching depth to lateral etching length and photoresist etching rate are reported. The relevance of the etching variables is also presented. The obtained etching behaviours for microneedle structure generation will be applied to develop recipes to fabricate microneedles in designed dimensions.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-02-27

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

  15. Properties and etching rates of negative ions in inductively coupled plasmas and dc discharges produced in Ar/SF6

    International Nuclear Information System (INIS)

    Draghici, M.; Stamate, E.

    2010-01-01

    Negative ion production is investigated in a chamber with transversal magnetic filter operated in dc or inductively coupled plasma (ICP) modes in Ar/SF 6 gas mixtures. Plasma parameters are evaluated by mass spectrometry and Langmuir probe for different discharge conditions. The density ratio of negative ion to electron exceeded 300 in dc mode while it was below 100 in the ICP mode. The possibility to apply a large positive bias to an electrode without affecting the plasma potential and the transition from a negative sheath to anodic glow are also investigated. The etching rates by positive and negative ions are evaluated on silicon substrate for different Ar/SF 6 gas ratios. The etching rate by negative ions was with less than 5% smaller than that by positive ions.

  16. Properties and etching rates of negative ions in inductively coupled plasmas and dc discharges produced in Ar/SF6

    DEFF Research Database (Denmark)

    Draghici, Mihai; Stamate, Eugen

    2010-01-01

    of negative ion to electron exceeded 300 in dc mode while it was below 100 in the ICP mode. The possibility to apply a large positive bias to an electrode without affecting the plasma potential and the transition from a negative sheath to anodic glow are also investigated. The etching rates by positive...... and negative ions are evaluated on silicon substrate for different Ar/SF6 gas ratios. The etching rate by negative ions was with less than 5% smaller than that by positive ions.......Negative ion production is investigated in a chamber with transversal magnetic filter operated in dc or inductively coupled plasma (ICP) modes in Ar/SF6 gas mixtures. Plasma parameters are evaluated by mass spectrometry and Langmuir probe for different discharge conditions. The density ratio...

  17. Carbon-enhanced inductively coupled plasma mass spectrometric detection of arsenic and selenium and its application to arsenic speciation

    DEFF Research Database (Denmark)

    Larsen, Erik Huusfeldt; Sturup, Stefan

    1994-01-01

    Addition of carbon as methanol or ammonium carbonate to the aqueous analyte solutions in combination with increased plasma power input enhanced the inductively coupled plasma mass spectrometry (ICP-MS) signal intensities of arsenic and selenium. In the presence of the optimum 3% v/v methanol...... (noise) was not increased. Therefore, the observed increase in analyte sensitivity led to a similar increase in signal-to-noise ratio. The addition of carbon as ammonium carbonate enhanced the arsenic signal by a similar factor but caused severe contamination of the ICP-MS instrument by carbon. In the 3....../nebulization efficiency. It is proposed that an increased population of carbon ions or carbon-containing ions in the plasma facilitates a more complete ionization of analytes lower in ionization energy than carbon itself. The enhanced detection power for arsenic was applied to arsenic speciation by high...

  18. Double plasma system with inductively coupled source plasma and quasi-quiescent target plasma

    International Nuclear Information System (INIS)

    Massi, M.; Maciel, H.S.

    1995-01-01

    Cold plasmas have successfully been used in the plasma-assisted material processing industry. An understanding of the physicochemical mechanisms involved in the plasma-surface interaction is needed for a proper description of deposition and etching processes at material surfaces. Since these mechanisms are dependent on the plasma properties, the development of diagnostic techniques is strongly desirable for determination of the plasma parameters as well as the characterization of the electromagnetic behaviour of the discharge. In this work a dual discharge chamber, was specially designed to study the deposition of thin films via plasma polymerization process. In the Pyrex chamber an inductively coupled plasma can be excited either in the diffuse low density E-mode or in the high density H-mode. This plasma diffuses into the cylindrical stainless steel chamber which is covered with permanent magnets to produce a multidipole magnetic field configuration at the surface. By that means a double plasma is established consisting of a RF source plasma coupled to a quasi-quiescent target plasma. The preliminary results presented here refer to measurements of the profiles of plasma parameters along the central axis of the double plasma apparatus. Additionally a spectrum analysis performed by means of a Rogowski coil probe immersed into the source plasma is also presented. The discharge is made in argon with pressure varying from 10 -2 to 1 torr, and the rf from 10 to 150 W

  19. Improvement of NiMoNb to polyimide adhesion by inductively coupled nitrogen plasma treatment

    Energy Technology Data Exchange (ETDEWEB)

    Bang, S.-H., E-mail: zxclucy@snu.ac.kr

    2016-01-01

    Graphical abstract: - Highlights: • NiMoNb was introduced as the adhesion layer for flexible Cu-clad laminate structure. • The effect of sputtering and plasma power on the peel strength was studied. • Plasma pretreatment in inductively coupled plasma greatly affects the peel strength. • FCCL with NiMoNb adhesion layer show outstanding peel strength. - Abstract: In this study, the effect of sputtering power on the peel strength of the flexible copper clad laminate (FCCL) was evaluated before and after heat treatment using 180° peel test. An increase in the sputtering powers from 200 W to 600 W increased film density and improved peel strength. To enhance peel strength much more, an inductively coupled plasma (ICP) was treated on the PI surface using N{sub 2} gas with Ar as a function of RF power. A dramatic enhancement of the peel strength, 923 N/m was achieved, especially after heat treatment by changing ICP power from 200 W to 900 W. The reduction ratio of the peel strength for the 900 W plasma-treated FCCL was only 12%, whereas that for the 200 W plasma-treated FCCL was 43%. The root mean square (RMS) surface roughness with PIs exposed to both 200 W and 900 W plasma treatments was rarely changed, while X-ray photoelectron spectroscopy (XPS) showed the substantial increase of C–N functional groups. To obtain insight the film characteristics, the NiMoNb/PI interfaces were investigated by a high resolution transmission electron microscopy (HR-TEM).

  20. Trace determination of Pu by LIF in an inductively coupled plasma

    International Nuclear Information System (INIS)

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

    1989-01-01

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

  1. Titanium oxidation by rf inductively coupled plasma

    International Nuclear Information System (INIS)

    Valencia-Alvarado, R; López-Callejas, R; Barocio, S R; Mercado-Cabrera, A; Peña-Eguiluz, R; Muñoz-Castro, A E; Rodríguez-Méndez, B G; De la Piedad-Beneitez, A; De la Rosa-Vázquez, J M

    2014-01-01

    The development of titanium dioxide (TiO 2 ) films in the rutile and anatase phases is reported. The films have been obtained from an implantation/diffusion and sputtering process of commercially pure titanium targets, carried out in up to 500 W plasmas. The experimental outcome is of particular interest, in the case of anatase, for atmospheric pollution degradation by photocatalysis and, as to the rutile phase, for the production of biomaterials required by prosthesis and implants. The reactor employed consists in a cylindrical pyrex-like glass vessel inductively coupled to a 13.56 MHz RF source. The process takes place at a 5×10 −2 mbar pressure with the target samples being biased from 0 to -3000 V DC. The anatase phase films were obtained from sputtering the titanium targets over glass and silicon electrically floated substrates placed 2 cm away from the target. The rutile phase was obtained by implantation/diffusion on targets at about 700 °C. The plasma was developed from a 4:1 argon/oxygen mixture for ∼5 hour processing periods. The target temperature was controlled by means of the bias voltage and the plasma source power. The obtained anatase phases did not require annealing after the plasma oxidation process. The characterization of the film samples was conducted by means of x-ray diffraction, scanning electron microscopy, x-ray photoelectron spectroscopy and Raman spectroscopy

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

    DEFF Research Database (Denmark)

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

    2001-01-01

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

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

    Science.gov (United States)

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

    2016-01-01

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

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

    Science.gov (United States)

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

    1983-05-01

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

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

    Science.gov (United States)

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

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

    Science.gov (United States)

    Hoekstra, Robert J.; Kushner, Mark J.

    1996-03-01

    Inductively coupled plasma (ICP) reactors are being developed for low gas pressure (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.

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

    International Nuclear Information System (INIS)

    Provitina, O.

    1993-01-01

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

  8. Transfer coefficients in ultracold strongly coupled plasma

    Science.gov (United States)

    Bobrov, A. A.; Vorob'ev, V. S.; Zelener, B. V.

    2018-03-01

    We use both analytical and molecular dynamic methods for electron transfer coefficients in an ultracold plasma when its temperature is small and the coupling parameter characterizing the interaction of electrons and ions exceeds unity. For these conditions, we use the approach of nearest neighbor to determine the average electron (ion) diffusion coefficient and to calculate other electron transfer coefficients (viscosity and electrical and thermal conductivities). Molecular dynamics simulations produce electronic and ionic diffusion coefficients, confirming the reliability of these results. The results compare favorably with experimental and numerical data from earlier studies.

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

    International Nuclear Information System (INIS)

    Ohno, Takeshi; Muramatsu, Yasuyuki

    2015-01-01

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

  10. Construcción y caracterización de un nuevo nebulizador múltiple para técnicas analíticas basadas en plasma (ICP-OES, ICP-MS y MP-AES).

    OpenAIRE

    Lúñez Fernández, Claudia

    2016-01-01

    En la siguiente memoria, se presenta la metodología para la construcción de un nuevo nebulizador múltiple, resultado de una serie de nebulizadores anteriores, los cuales se han ido mejorando para optimizar las características del aerosol generado y con ello los parámetros analíticos de calidad en la espectrometría de emisión atómica con plasma de microondas (MP-AES) y espectrometría de emisión óptica con plasma de acoplamiento inductivo (ICP-OES). Este nuevo nebulizador multiconducto presenta...

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

    International Nuclear Information System (INIS)

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

    2002-01-01

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

  12. Radiation from nonlinear coupling of plasma waves

    International Nuclear Information System (INIS)

    Fung, S.F.

    1986-01-01

    The author examines the generation of electromagnetic radiation by nonlinear resonant interactions of plasma waves in a cold, uniformly magnetized plasma. In particular, he considers the up-conversion of two electrostatic wave packets colliding to produce high frequency electromagnetic radiation. Efficient conversion of electrostatic to electromagnetic wave energy occurs when the pump amplitudes approach and exceed the pump depletion threshold. Results from the inverse scattering transform analysis of the three-wave interaction equations are applied. When the wave packets are initially separated, the fully nonlinear set of coupling equations, which describe the evolution of the wave packets, can be reduced to three separate eigenvalue problems; each can be considered as a scattering problem, analogous to eh Schroedinger equation. In the scattering space, the wave packet profiles act as the scattering potentials. When the wavepacket areas approach (or exceed) π/2, the wave functions are localized (bound states) and the scattering potentials are said to contain solitons. Exchange of solitons occurs during the interaction. The transfer of solitons from the pump waves to the electromagnetic wave leads to pump depletion and the production of strong radiation. The emission of radio waves is considered by the coupling of two upper-hybrid branch wave packets, and an upper-hybrid and a lower hybrid branch wave packet

  13. Uranium spectra in the ICP

    Energy Technology Data Exchange (ETDEWEB)

    Ghazi, A.A.; Qamar, S.; Atta, M.A. (Khan (A.Q.) Research Labs., Rawalpindi (Pakistan))

    1994-05-01

    Uranium spectra have been studied by inductively coupled plasma atomic emission spectroscopy (ICP-AES). In total, 8361 uranium lines were observed in the wavelength range of 235-500 nm. This article is an electronic publication in Spectrochimica Acta Electronica (SAE), the electronic section of Spectrochimica Acta Part B (SAB). The hard copy text is accompanied by a disk with data files and test files for an IBM-compatible computer. The main article discusses the scientific aspects of the subject and explains the purpose of the data files. (Author).

  14. Uranium spectra in the ICP

    International Nuclear Information System (INIS)

    Ghazi, A.A.; Qamar, S.; Atta, M.A.

    1994-01-01

    Uranium spectra have been studied by inductively coupled plasma atomic emission spectroscopy (ICP-AES). In total, 8361 uranium lines were observed in the wavelength range of 235-500 nm. This article is an electronic publication in Spectrochimica Acta Electronica (SAE), the electronic section of Spectrochimica Acta Part B (SAB). The hard copy text is accompanied by a disk with data files and test files for an IBM-compatible computer. The main article discusses the scientific aspects of the subject and explains the purpose of the data files. (Author)

  15. Jets in a strongly coupled anisotropic plasma

    Energy Technology Data Exchange (ETDEWEB)

    Fadafan, Kazem Bitaghsir [Shahrood University of Technology, Faculty of Physics, Shahrood (Iran, Islamic Republic of); University of Southampton, STAG Research Centre Physics and Astronomy, Southampton (United Kingdom); Morad, Razieh [University of Cape Town, Department of Physics, Rondebosch (South Africa)

    2018-01-15

    In this paper, we study the dynamics of the light quark jet moving through the static, strongly coupled N = 4, anisotropic plasma with and without charge. The light quark is presented by a 2-parameters point-like initial condition falling string in the context of the AdS/CFT. We calculate the stopping distance of the light quark in the anisotropic medium and compare it with its isotropic value. We study the dependency of the stopping distance to the both string initial conditions and background parameters such as anisotropy parameter or chemical potential. Although the typical behavior of the string in the anisotropic medium is similar to the one in the isotropic AdS-Sch background, the string falls faster to the horizon depending on the direction of moving. Particularly, the enhancement of quenching is larger in the beam direction. We find that the suppression of stopping distance is more prominent when the anisotropic plasma have the same temperature as the isotropic plasma. (orig.)

  16. Effects of rf power on electron density and temperature, neutral temperature, and Te fluctuations in an inductively coupled plasma

    International Nuclear Information System (INIS)

    Camparo, James; Fathi, Gilda

    2009-01-01

    Atomic clocks that fly on global-navigation satellites such as global positioning system (GPS) and Galileo employ light from low-temperature, inductively coupled plasmas (ICPs) for atomic signal generation and detection (i.e., alkali/noble-gas rf-discharge lamps). In this application, the performance of the atomic clock and the capabilities of the navigation system depend sensitively on the stability of the ICP's optical emission. In order to better understand the mechanisms that might lead to instability in these rf-discharge lamps, and hence the satellite atomic clocks, we studied the optical emission from a Rb/Xe ICP as a function of the rf power driving the plasma. Surprisingly, we found that the electron density in the plasma was essentially independent of increases in rf power above its nominal value (i.e., 'rf-power gain') and that the electron temperature was only a slowly varying function of rf-power gain. The primary effect of rf power was to increase the temperature of the neutrals in the plasma, which was manifested by an increase in Rb vapor density. Interestingly, we also found evidence for electron temperature fluctuations (i.e., fluctuations in the plasma's high-energy electron content). The variance of these fluctuations scaled inversely with the plasma's mean electron temperature and was consistent with a simple model that assumed that the total electron density in the discharge was independent of rf power. Taken as a whole, our results indicate that the electrons in alkali/noble-gas ICPs are little affected by slight changes in rf power and that the primary effect of such changes is to heat the plasma's neutral species.

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

    Science.gov (United States)

    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.

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

    International Nuclear Information System (INIS)

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

    2008-01-01

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

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

    International Nuclear Information System (INIS)

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

    1999-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-01-01

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

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

    Science.gov (United States)

    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 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 the environment.

  2. Nonlinear wave coupling in a warm plasma in the fluid

    International Nuclear Information System (INIS)

    Malara, F.; Veltri, P.

    1984-01-01

    The general expression for nonlinear coupling between plasma modes is obtained. The nonlinear conductivity tensor is then calculated by means of the two-fluid plasma description taking into account the thermal pressure effects

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

    OpenAIRE

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

    2001-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2000-11-01

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

  5. Direct rare earth determination by inductively coupled plasma optical emission spectrometry

    International Nuclear Information System (INIS)

    Marin, Sergio; Cornejo, Silvia; Rojas, Jacqueline

    2003-01-01

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

  6. Organo-Functionalization of Silicon Nanocrystals Synthesized by Inductively Coupled Plasma Chemical Vapor Deposition

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Don-Sung; Choe, Dong-Hoe; Jeong, Hyun-Dam [Chonnam National University, Gwangju (Korea, Republic of); Yoo, Seung-Wan; Kim, Jung-Hyung [Korea Research Institute of Standards and Science, Daejeon (Korea, Republic of)

    2016-05-15

    Octadecyl-terminated silicon nanocrystals (ODE-Si NCs) are obtained via a surface-initiated thermal hydrosilylation reaction on hydride-terminated Si NCs (H-Si NCs). Pristine Si NCs were synthesized at the gram scale by using inductively coupled plasma chemical vapor deposition (ICP-CVD) . The H-Si NCs were produced through a chemical etching process with hydrofluoric acid (HF), ethanol (EtOH), and distilled water (d-H{sub 2}O). The results obtained from X-ray diffraction (XRD) and field emission scanning electron microscopy (FE-SEM) indicate that the synthesized Si NCs obtained via ICP-CVD have diamond cubic-structured silicon with a grain size of 10 nm and a densely packed Si NC array consisting of individual NCs. Organo-functionalized Si NCs, i.e., ODE-Si NCs, are well soluble in organic solvent whereas pristine Si NCs synthesized through ICP-CVD are not. The surface chemistry of the ODE-Si NCs was confirmed via Fourier transform infrared spectroscopy (FT-IR), proton nuclear magnetic resonance spectroscopy ({sup 1}H-NMR), and field emission transmission electron microscopy (FE-TEM). Thereby, these newly synthesized and scalable organo-functionalized Si NCs are applicable as raw materials for practical use in devices by tuning the surface chemistry with various capping molecules.

  7. Internal standardization in atomic-emission spectrometry using inductively coupled plasma

    International Nuclear Information System (INIS)

    Moore, G.L.

    1985-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1996-08-01

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

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

    International Nuclear Information System (INIS)

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

    2003-01-01

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

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

    International Nuclear Information System (INIS)

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

    1999-01-01

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

  11. Two-dimensional HPLC coupled to ICP-MS and electrospray ionisation (ESI)-MS/MS for investigating the bioavailability in vitro of arsenic species from edible seaweed

    Energy Technology Data Exchange (ETDEWEB)

    Garcia-Sartal, Cristina; Barciela-Alonso, Maria del Carmen; Bermejo-Barrera, Pilar [University of Santiago de Compostela, Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Chemistry, Santiago de Compostela (Spain); Taebunpakul, Sutthinun [LGC Limited, Teddington, Middlesex (United Kingdom); Imperial College of Science, Technology and Medicine, South Kensington, Department of Materials, London (United Kingdom); National Institute of Metrology (Thailand), Pathumthani (Thailand); Stokes, Emma; Goenaga-Infante, Heidi [LGC Limited, Teddington, Middlesex (United Kingdom)

    2012-04-15

    Edible seaweed consumption is a route of exposure to arsenic. However, little attention has been paid to estimate the bioaccessibility and/or bioavailability of arsenosugars in edible seaweed and their possible degradation products during gastrointestinal digestion. This work presents first use of combined inductively coupled plasma mass spectroscopy (ICP-MS) with electrospray ionization tandem mass spectrometry (ESI-MS/MS) with two-dimensional HPLC (size exclusion followed by anion exchange) to compare the qualitative and quantitative arsenosugars speciation of different edible seaweed with that of their bioavailable fraction as obtained using an in vitro gastrointestinal digestion procedure. Optimal extraction conditions for As species from four seaweed namely kombu, wakame, nori and sea lettuce were selected as a compromise between As extraction efficiency and preservation of compound identity. For most investigated samples, the use of ammonium acetate buffer as extractant and 1 h sonication in a water bath followed by HPLC-ICP-MS resulted in 40-61% of the total As to be found in the buffered aqueous extract, of which 86-110% was present as arsenosugars (glycerol sugar, phosphate sugar and sulfonate sugar for wakame and kombu and glycerol sugar and phosphate sugar for nori). The exception was sea lettuce, for which the arsenosugar fraction (glycerol sugar, phosphate sugar) only comprised 44% of the total extracted As. Interestingly, the ratio of arsenobetaine and dimethylarsinic acid to arsenosugars in sea lettuce extracts seemed higher than that for the rest of investigated samples. After in vitro gastrointestinal digestion, approximately 11-16% of the total As in the solid sample was found in the dialyzates with arsenosugars comprising 93-120% and 41% of the dialyzable As fraction for kombu, wakame, nori and sea lettuce, respectively. Moreover, the relative As species distribution in seaweed-buffered extracts and dialyzates was found to be very similar

  12. Gluon Bremsstrahlung in Weakly-Coupled Plasmas

    International Nuclear Information System (INIS)

    Arnold, Peter

    2009-01-01

    I report on some theoretical progress concerning the calculation of gluon bremsstrahlung for very high energy particles crossing a weakly-coupled quark-gluon plasma. (i) I advertise that two of the several formalisms used to study this problem, the BDMPS-Zakharov formalism and the AMY formalism (the latter used only for infinite, uniform media), can be made equivalent when appropriately formulated. (ii) A standard technique to simplify calculations is to expand in inverse powers of logarithms ln(E/T). I give an example where such expansions are found to work well for ω/T≥10 where ω is the bremsstrahlung gluon energy. (iii) Finally, I report on perturbative calculations of q.

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

    DEFF Research Database (Denmark)

    Qiao, Jixin; Lagerkvist, Petra; Rodushkin, Ilia

    2018-01-01

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

  14. Electromagnetic modes in cold magnetized strongly coupled plasmas

    OpenAIRE

    Tkachenko, I. M.; Ortner, J.; Rylyuk, V. M.

    1999-01-01

    The spectrum of electromagnetic waves propagating in a strongly coupled magnetized fully ionized hydrogen plasma is found. The ion motion and damping being neglected, the influence of the Coulomb coupling on the electromagnetic spectrum is analyzed.

  15. Room temperature inductively coupled plasma etching of InAs/InSb in BCl 3/Cl 2/Ar

    KAUST Repository

    Sun, Jian

    2012-10-01

    Inductively coupled plasma (ICP) etching of InAs and InSb at room temperature has been investigated using BCl 3/Cl 2/Ar plasma. Specifically, the etch rate and post-etching surface morphology were investigated as functions of the gas composition, ICP power, process pressure, and RF chuck power. An optimized process has been developed, yielding anisotropic etching and very smooth surfaces with roughnesses of 0.25 nm for InAs, and 0.57 nm for InSb, which is comparable with the surface of epi-ready polished wafers. The process provides moderate etching rates of 820 /min for InAs and 2800 /min for InSb, and the micro-masking effect is largely avoided. © 2012 Elsevier B.V. All rights reserved.

  16. Hydrogen atom kinetics in capacitively coupled plasmas

    Science.gov (United States)

    Nunomura, Shota; Katayama, Hirotaka; Yoshida, Isao

    2017-05-01

    Hydrogen (H) atom kinetics has been investigated in capacitively coupled very high frequency (VHF) discharges at powers of 16-780 mW cm-2 and H2 gas pressures of 0.1-2 Torr. The H atom density has been measured using vacuum ultra violet absorption spectroscopy (VUVAS) with a micro-discharge hollow cathode lamp as a VUV light source. The measurements have been performed in two different electrode configurations of discharges: conventional parallel-plate diode and triode with an intermediate mesh electrode. We find that in the triode configuration, the H atom density is strongly reduced across the mesh electrode. The H atom density varies from ˜1012 cm-3 to ˜1010 cm-3 by crossing the mesh with 0.2 mm in thickness and 36% in aperture ratio. The fluid model simulations for VHF discharge plasmas have been performed to study the H atom generation, diffusion and recombination kinetics. The simulations suggest that H atoms are generated in the bulk plasma, by the electron impact dissociation (e + H2 \\to e + 2H) and the ion-molecule reaction (H2 + + H2 \\to {{{H}}}3+ + H). The diffusion of H atoms is strongly limited by a mesh electrode, and thus the mesh geometry influences the spatial distribution of the H atoms. The loss of H atoms is dominated by the surface recombination.

  17. Precise and accurate isotope ratio measurements by ICP-MS.

    Science.gov (United States)

    Becker, J S; Dietze, H J

    2000-09-01

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

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

    International Nuclear Information System (INIS)

    Popp, Maximilian; Hann, Stephan; Koellensperger, Gunda

    2010-01-01

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

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-07-23

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

  1. Determination of platinum drug release and liposome stability in human plasma by CE-ICP-MS

    DEFF Research Database (Denmark)

    Nguyen, Trinh Thi Nhu Tam; Ostergaard, Jesper; Stürup, Stefan

    2013-01-01

    An in vitro method for simultaneous assessment of platinum release and liposome stability of liposomal formulations in human plasma is demonstrated. The development and assessment of the method was performed on a PEGylated liposomal formulation containing cisplatin. Complete separation of free ci...

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

    Science.gov (United States)

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

    2017-11-27

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-08-15

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

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

    Science.gov (United States)

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

    2017-05-15

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

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

    Science.gov (United States)

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

    2016-01-01

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

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

    International Nuclear Information System (INIS)

    Ochsenkuehn-Petropoulou, Maria; Luck, Joachim

    1991-01-01

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

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

    International Nuclear Information System (INIS)

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

    2003-01-01

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

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-09-28

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

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

    International Nuclear Information System (INIS)

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

    2016-01-01

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

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

    International Nuclear Information System (INIS)

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

    2017-10-01

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

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

    Science.gov (United States)

    Kretschy, Daniela; Koellensperger, Gunda; Hann, Stephan

    2012-01-01

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

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-03-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-10-01

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

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

    International Nuclear Information System (INIS)

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

    2014-01-01

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

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

    International Nuclear Information System (INIS)

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

    2013-01-01

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

  18. LASER ABLATION-INDUCTIVELY COUPLED PLASMA-ATOMIC EMISSION SPECTROSCOPY STUDY AT THE 222-S LABORATORY USING HOT-CELL GLOVE BOX PROTOTYPE SYSTEM

    International Nuclear Information System (INIS)

    Lockrem, L.L.; Owens, J.W.; Seidel, C.M.

    2009-01-01

    This report describes the installation, testing and acceptance of the Waste Treatment and Immobilization Plant procured laser ablation-inductively coupled plasma-atomic emission spectroscopy (LA-ICP-AES) system for remotely analyzing high-level waste samples in a hot cell environment. The 2005-003; ATS MP 1027, Management Plan for Waste Treatment Plant Project Work Performed by Analytical Technical Services. The APD group at the 222-S laboratory demonstrated acceptable turnaround time (TAT) and provide sufficient data to assess sensitivity, accuracy, and precision of the LA-ICP-AES method

  19. LASER ABLATION-INDUCTIVELY COUPLED PLASMA-ATOMIC EMISSION SPECTROSCOPY STUDY AT THE 222-S LABORATORY USING HOT-CELL GLOVE BOX PROTOTYPE SYSTEM

    International Nuclear Information System (INIS)

    Seidel, C.M.; Jain, J.; Owens, J.W.

    2009-01-01

    This report describes the installation, testing, and acceptance of the Waste Treatment and Immobilization Plant (WTP) procured laser ablation-inductively coupled plasma-atomic emission spectroscopy (LA-ICP-AES) system for remotely analyzing high-level waste (HLW) samples in a hot cell environment. The work was completed by the Analytical Process Development (APD) group in accordance with Task Order 2005-003; ATS MP 1027, Management Plan for Waste Treatment Plant Project Work Performed by Analytical Technical Services. The APD group at the 222-S Laboratory demonstrated acceptable turnaround time (TAT) and provide sufficient data to assess sensitivity, accuracy, and precision of the LA-ICP-AES method

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-01-15

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-04-17

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

  2. Surface roughening of ground fused silica processed by atmospheric inductively coupled plasma

    International Nuclear Information System (INIS)

    Xin, Qiang; Li, Na; Wang, Jun; Wang, Bo; Li, Guo; Ding, Fei; Jin, Huiliang

    2015-01-01

    Highlights: • The morphology evolution of ground fused silica, processed by atmospheric plasma, was investigated experimentally. • The roughness development results from opening and coalescing of the plasma-etched cracks. • The shapes of grain-like etched pits are the results of the adjacent cracks coalescing with one another. • The descent of the pits density is due to some smaller etched pits that are swallowed up by larger pits. • Leading role in surface smoothing is laterally etching away the side walls of the intersecting pits. - Abstract: Subsurface damage (SSD) is a defect that is inevitably induced during mechanical processes, such as grinding and polishing. This defect dramatically reduces the mechanical strength and the laser damage thresholds of optical elements. Compared with traditional mechanical machining, atmospheric pressure plasma processing (APPP) is a relatively novel technology that induces almost no SSD during the processing of silica-based optical materials. In this paper, a form of APPP, inductively coupled plasma (ICP), is used to process fused silica substrates with fluorocarbon precursor under atmospheric pressure. The surface morphology evolution of ICP-processed substrates was observed and characterized by confocal laser scanning microscope (CLSM), field emission scanning electron microscope (SEM), and atomic force microscopy (AFM). The results show that the roughness evolves with the etching depth, and the roughness evolution is a single-peaked curve. This curve results from the opening and the coalescing of surface cracks and fractures. The coalescence procedure of these microstructures was simulated with two common etched pits on a polished fused silica surface. Understanding the roughness evolution of plasma-processed surface might be helpful in optimizing the optical fabrication chain that contains APPP

  3. Surface roughening of ground fused silica processed by atmospheric inductively coupled plasma

    Energy Technology Data Exchange (ETDEWEB)

    Xin, Qiang; Li, Na; Wang, Jun; Wang, Bo, E-mail: bradywang@hit.edu.cn; Li, Guo; Ding, Fei; Jin, Huiliang

    2015-06-30

    Highlights: • The morphology evolution of ground fused silica, processed by atmospheric plasma, was investigated experimentally. • The roughness development results from opening and coalescing of the plasma-etched cracks. • The shapes of grain-like etched pits are the results of the adjacent cracks coalescing with one another. • The descent of the pits density is due to some smaller etched pits that are swallowed up by larger pits. • Leading role in surface smoothing is laterally etching away the side walls of the intersecting pits. - Abstract: Subsurface damage (SSD) is a defect that is inevitably induced during mechanical processes, such as grinding and polishing. This defect dramatically reduces the mechanical strength and the laser damage thresholds of optical elements. Compared with traditional mechanical machining, atmospheric pressure plasma processing (APPP) is a relatively novel technology that induces almost no SSD during the processing of silica-based optical materials. In this paper, a form of APPP, inductively coupled plasma (ICP), is used to process fused silica substrates with fluorocarbon precursor under atmospheric pressure. The surface morphology evolution of ICP-processed substrates was observed and characterized by confocal laser scanning microscope (CLSM), field emission scanning electron microscope (SEM), and atomic force microscopy (AFM). The results show that the roughness evolves with the etching depth, and the roughness evolution is a single-peaked curve. This curve results from the opening and the coalescing of surface cracks and fractures. The coalescence procedure of these microstructures was simulated with two common etched pits on a polished fused silica surface. Understanding the roughness evolution of plasma-processed surface might be helpful in optimizing the optical fabrication chain that contains APPP.

  4. Unexpected properties of the inductively coupled plasma induced defect in germanium

    Energy Technology Data Exchange (ETDEWEB)

    Coelho, S.M.M., E-mail: sergio@up.ac.za; Auret, F.D.; Janse van Rensburg, P.J.; Nel, J.M.

    2014-04-15

    Inductively coupled plasma (ICP) etching of germanium introduces a single defect, the E{sub 0.31} electron trap, for a large range of argon partial pressures from 4×10{sup –3} to 6.5×10{sup –4} mbar that correspond to ion energies of 8 to 60 eV. Ge of three crystallographic orientations, (1 0 0), (1 1 0) and (1 1 1), treated with 20 and 60 eV ICP had defect concentration profiles that were similar in appearance, with a maximum concentration of 10{sup 14} cm{sup −3} extending more than a µm into the material, approximately three orders of magnitude deeper than what TRIM simulations predicted. All profiles were measured using Laplace deep level transient spectroscopy (L-DLTS), a technique that is sensitive to defect concentrations as low as 10{sup 11} cm{sup −3}. Isochronal annealing of samples showed concentration curves broadening after a 400 K anneal and decreasing to the 10{sup 13} cm{sup −3} level after a 450 K anneal. Unannealed samples measured after a year exhibited similar decreases in defect concentration without broadening of their profiles. A 550 K anneal lowered the defect concentration to levels below the L-DLTS detection limit. Thereafter additional plasma treatment of the surface failed to reintroduce this defect indicating that the structure required for the formation of E{sub 0.31} was no longer present in the region under observation.

  5. Coupled Langmuir oscillations in 2-dimensional quantum plasmas

    International Nuclear Information System (INIS)

    Akbari-Moghanjoughi, M.

    2014-01-01

    In this work, we present a hydrodynamic model to study the coupled quantum electron plasma oscillations (QEPO) for two dimensional (2D) degenerate plasmas, which incorporates all the essential quantum ingredients such as the statistical degeneracy pressure, electron-exchange, and electron quantum diffraction effect. Effects of diverse physical aspects like the electronic band-dispersion effect, the electron exchange-correlations and the quantum Bohm-potential as well as other important plasma parameters such as the coupling parameter (plasma separation) and the plasma electron number-densities on the linear response of the coupled system are investigated. By studying three different 2D plasma coupling types, namely, graphene-graphene, graphene-metalfilm, and metalfilm-metalfilm coupling configurations, it is remarked that the collective quantum effects can influence the coupled modes quite differently, depending on the type of the plasma configuration. It is also found that the slow and fast QEPO frequency modes respond very differently to the change in plasma parameters. Current findings can help in understanding of the coupled density oscillations in multilayer graphene, graphene-based heterojunctions, or nanofabricated integrated circuits

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

    OpenAIRE

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

    1992-01-01

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

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

    International Nuclear Information System (INIS)

    Walder, A.J.; Furuta, Naoki.

    1993-01-01

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

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

    Science.gov (United States)

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

    2014-08-01

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

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

    International Nuclear Information System (INIS)

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

    2004-01-01

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

  10. Shear viscosities of photons in strongly coupled plasmas

    Directory of Open Access Journals (Sweden)

    Di-Lun Yang

    2016-09-01

    Full Text Available We investigate the shear viscosity of thermalized photons in the quark gluon plasma (QGP at weak coupling and N=4 super Yang–Mills plasma (SYMP at both strong and weak couplings. We find that the shear viscosity due to the photon–parton scattering up to the leading order of electromagnetic coupling is suppressed when the coupling of the QGP/SYMP is increased, which stems from the blue-shift of the thermal-photon spectrum at strong coupling. In addition, the shear viscosity rapidly increases near the deconfinement transition in a phenomenological model analogous to the QGP.

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

    International Nuclear Information System (INIS)

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

    2000-01-01

    As a result of the accident at the Chernobyl nuclear power plant (NPP) the environment was contaminated with spent nuclear fuel. The 236 U isotope was used in this study to monitor the spent uranium from nuclear fallout in soil samples collected in the vicinity of the Chernobyl NPP. A rapid and sensitive analytical procedure was developed for uranium isotopic ratio measurement in environmental samples based on inductively coupled plasma quadrupole mass spectrometry with a hexapole collision cell (HEX-ICP-QMS). The figures of merit of the HEX-ICP-QMS were studied with a plasma-shielded torch using different nebulizers (such as an ultrasonic nebulizer (USN) and Meinhard nebulizer) for solution introduction. A 238 U + ion intensity of up to 27000 MHz/ppm in HEX-ICP-QMS with USN was observed by introducing helium into the hexapole collision cell as the collision gas at a flow rate of 10 ml min -1 . The formation rate of uranium hydride ions UH + /U + of 2 x 10 -6 was obtained by using USN with a membrane desolvator. The limit of 236 U/ 238 U ratio determination in 10 μg 1 -1 uranium solution was 3 x 10 -7 corresponding to the detection limit for 236 U of 3 pg 1 -1 . The precision of uranium isotopic ratio measurements in 10 μg 1 -1 laboratory uranium isotopic standard solution was 0.13% ( 235 U/ 238 U) and 0.33% ( 236 U/ 238 U) using a Meinhard nebulizer and 0.45% ( 235 U/ 238 U) and 0.88% ( 236 U/ 238 U) using a USN. The isotopic composition of all investigated Chernobyl soil samples differed from those of natural uranium; i.e. in these samples the 236 U/ 238 U ratio ranged from 10 -5 to 10 -3 . (orig.)

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

    Science.gov (United States)

    Makonnen, Yoseif; Beauchemin, Diane

    2015-01-01

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

  13. Diamond deposition using a planar radio frequency inductively coupled plasma

    Science.gov (United States)

    Bozeman, S. P.; Tucker, D. A.; Stoner, B. R.; Glass, J. T.; Hooke, W. M.

    1995-06-01

    A planar radio frequency inductively coupled plasma has been used to deposit diamond onto scratched silicon. This plasma source has been developed recently for use in large area semiconductor processing and holds promise as a method for scale up of diamond growth reactors. Deposition occurs in an annulus which coincides with the area of most intense optical emission from the plasma. Well-faceted diamond particles are produced when the substrate is immersed in the plasma.

  14. Analytical applications of atomic spectroscopy, with particular reference to inductively coupled plasma emission analysis of coal and fly ash

    International Nuclear Information System (INIS)

    Pougnet, M.A.B.

    1983-08-01

    This thesis outlines the analytical applications of atomic emission and absorption spectroscopy to a variety of materials. Special attention was directed to the analysis of coal and coal ashes. A simple slurry sampling technique was developed and used to determine V, Ni, Co, Mo and Mn in the National Bureau of Standards Standard Reference Materials (NBS-SRM) coals 1632a and 1635 by furnace atomic absorption spectroscopy (FAAS). Coal and fly ash were analysed by inductively coupled plasma atomic emission spectroscopy (ICP-AES). The determination of B, Be, Li, C, K and other trace elements by ICP-AES was investigated. Analytical methods were developed for the analysis of coal, fly ash and water samples. Fusion with sodium carbonate and a digestion bomb dissolution method were compared for the determination of boron in a South African boron-rich mineral (Kornerupine). Eight elements were determined in 10 industrial water samples from a power plant. Ca, Mg, Si and B were determined by ICP-AES and V, Ni, Co and Mo by FAAS. Various problems encountered during the course of the work and interferences in ICP-AES analysis are discussed. Some recommendations concerning method development and routine analysis by this technique are suggested

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

    Science.gov (United States)

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

    2009-01-01

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

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

    International Nuclear Information System (INIS)

    Krata, A.; Bulska, E.

    2005-01-01

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

  17. A Method to Construct Plasma with Nonlinear Density Enhancement Effect in Multiple Internal Inductively Coupled Plasmas

    International Nuclear Information System (INIS)

    Chen Zhipeng; Li Hong; Liu Qiuyan; Luo Chen; Xie Jinlin; Liu Wandong

    2011-01-01

    A method is proposed to built up plasma based on a nonlinear enhancement phenomenon of plasma density with discharge by multiple internal antennas simultaneously. It turns out that the plasma density under multiple sources is higher than the linear summation of the density under each source. This effect is helpful to reduce the fast exponential decay of plasma density in single internal inductively coupled plasma source and generating a larger-area plasma with multiple internal inductively coupled plasma sources. After a careful study on the balance between the enhancement and the decay of plasma density in experiments, a plasma is built up by four sources, which proves the feasibility of this method. According to the method, more sources and more intensive enhancement effect can be employed to further build up a high-density, large-area plasma for different applications. (low temperature plasma)

  18. 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.

    Science.gov (United States)

    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.

  19. Assessment of high precision, high accuracy Inductively Coupled Plasma-Optical Emission Spectroscopy to obtain concentration uncertainties less than 0.2% with variable matrix concentrations

    International Nuclear Information System (INIS)

    Rabb, Savelas A.; Olesik, John W.

    2008-01-01

    The ability to obtain high precision, high accuracy measurements in samples with complex matrices using High Performance Inductively Coupled Plasma-Optical Emission Spectroscopy (HP-ICP-OES) was investigated. The Common Analyte Internal Standard (CAIS) procedure was incorporated into the High Performance Inductively Coupled Plasma-Optical Emission Spectroscopy method to correct for matrix-induced changes in emission intensity ratios. Matrix matching and standard addition approaches to minimize matrix-induced errors when using High Performance Inductively Coupled Plasma-Optical Emission Spectroscopy were also assessed. The High Performance Inductively Coupled Plasma-Optical Emission Spectroscopy method was tested with synthetic solutions in a variety of matrices, alloy standard reference materials and geological reference materials

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

    International Nuclear Information System (INIS)

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

    2002-01-01

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

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

    Directory of Open Access Journals (Sweden)

    J. Dilip Kumar

    2007-01-01

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

  2. Growth of crystallized Ge films from VHF inductively-coupled plasma of H2-diluted GeH4

    International Nuclear Information System (INIS)

    Sakata, T.; Makihara, K.; Murakami, H.; Higashi, S.; Miyazaki, S.

    2007-01-01

    We have studied the Ge crystalline nucleation and film growth on quartz substrate at 250 deg. C from inductively-coupled plasma (ICP) of GeH 4 diluted with H 2 . The ICP was generated by supplying 60 MHz power to an external single-turn antenna which was placed on a quartz plate window of a stainless steel reactor and parallel to the substrate. We have found that the growth rate is significantly increased when the preferential growth of the (110) plane becomes pronounced after the formation of randomly-oriented crystalline network. The (110) oriented Ge films, of which average crystallinity is as high as 70%. The integrated intensity ratio of TO phonons in crystalline phase to those in disordered phase, were grown at a rate of ∼ 4.0 nm/s after the formation of amorphous incubation layer with a thickness of ∼ 0.1 μm on quartz

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

    International Nuclear Information System (INIS)

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

    2005-01-01

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

  4. Determination of strontium and lead isotope ratios of grains using high resolution inductively coupled plasma mass spectrometer with single collector

    International Nuclear Information System (INIS)

    Shinozaki, Miyuki; Ariyama, Kaoru; Kawasaki, Akira; Hirata, Takafumi

    2010-01-01

    A method for determining strontium and lead isotope ratios of grains was developed. The samples investigated in this study were rice, barley and wheat. The samples were digested with nitric acid and hydrogen peroxide, and heated in a heating block. Strontium and lead were separated from the matrix by adding an acid digested solution into a column packed with Sr resin, which has selectivity for the absorption of strontium and lead. Strontium and lead isotope ratios were determined using a high-resolution inductively coupled plasma mass spectrometer (HR-ICP-MS) with a single collector. The intraday relative standard deviations of 87 Sr/ 86 Sr and lead isotope ratios ( 204 Pb/ 206 Pb, 207 Pb/ 206 Pb, 208 Pb/ 206 Pb) by HR-ICP-MS measurements were < 0.06% and around 0.1%, respectively. This method enabled us to determine strontium and lead isotope ratios in two days. (author)

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

    Science.gov (United States)

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

    2018-06-01

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

  6. Actinides analysis in emergency situation by on-line coupling between a calix[6]arene-based chromatography column and an Inductively Coupled Plasma-Mass Spectrometer

    International Nuclear Information System (INIS)

    Baghdadi, Sarah

    2015-01-01

    In the event of a nuclear crisis, involving actinides (U, Pu, Am) it is important to have fast analysis methods available in order to identify people that could be contaminated. Usually, they are performed in urine or faeces. Even though, analytical methods used with alpha detection are reliable they are lengthy and tedious to set up. This work consisted in developing an on-line coupling method between a calix[6]arene-based chromatography column and an inductively coupled plasma mass spectrometer (ICP-MS). To do so, a speciation study of actinides in mineralised urine was developed to understand the chemical equilibria happening during the actinides extraction. A protocol was elaborated to extract simultaneously all three actinides at pH = 5, then co-elute them with 0.25 mol.L -1 H 3 PO 4 . Recovery was 56 %, 74 % and 85 % for U, Pu and Am respectively. The column was then coupled to the ICP-MS. A parameter study helped defining mineralisation duration, extraction and elution flow-rates. It was then possible to propose an on-line coupling system allowing reaching detection limits lower than 0.5 mBq.L-1 for 238 U and 243 Am and lower than 5 mBq.L -1 for 239 Pu and 241 Am, for analysis duration lower than 6 hours. These analytical performances show the interest of this technique for a use in a nuclear crisis situation. (author)

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

  8. Comparison of inductively coupled plasma mass spectrometry and colorimetric determination of total and extractable phosphorus in soils

    International Nuclear Information System (INIS)

    Ivanov, Krasimir; Zaprjanova, Penka; Petkova, Milena; Stefanova, Violeta; Kmetov, Veselin; Georgieva, Deyana; Angelova, Violina

    2012-01-01

    The most widely used method for determination of total phosphorus in soils is perchloric acid digestion, followed by a colorimetric assay to measure the concentration of P in solution. The first part of this study compares an alternative digestion method, using aqua regia (ISO 11466 and EPA Method 3052), with perchloric acid digestion procedure, and also compares inductively coupled plasma mass spectroscopy (ICP-MS) with colorimetry for the measurement of P on the basis of five internationally certified standard soils and 20 real-life soils with widely different extractability of phosphorus. The phosphorus concentration was determined by means of the reduced phosphomolybdenum blue and ICP-MS. The relationship between methods has been examined statistically. Good agreement of the results from colorimetry and ICP-MS was established for all certified soils. The microwave-assisted digestion with aqua regia was comparable, both in precision and accuracy, with the hot plate aqua regia method. The phosphorus concentration found with the HF + HClO 4 digestion method was in good agreement with the certified mean values, while the superiority in extracting phosphorus, when compared to other methods, was obvious. Soil testing for plant-available phosphorus in Bulgaria and many European countries is most commonly conducted using acid Ca-lactate extraction (Egner–Riehm test) and alkaline sodium bicarbonate extraction (BDS ISO 11263:2002), based on Olsen test, followed by a colorimetric assay to measure the concentration of P in solution. The second part of this study reports the differences between Egner–Riehm test and BDS ISO 11263:2002 measured colorimetrically and by ICP-MS. Fifty soils were selected from South Bulgaria to represent a wide range of soil properties. It was established that ICP-MS consistently yielded significantly higher P concentrations than the colorimetric method in both extraction tests, and the relative differences were greatest in soils with lower P

  9. Comparison of inductively coupled plasma mass spectrometry and colorimetric determination of total and extractable phosphorus in soils

    Energy Technology Data Exchange (ETDEWEB)

    Ivanov, Krasimir, E-mail: kivanov1@abv.bg [Department of Chemistry, University of Agriculture, Plovdiv (Bulgaria); Zaprjanova, Penka [Tobacco and Tobacco Products Institute, Plovdiv (Bulgaria); Petkova, Milena [Department of Chemistry, University of Agriculture, Plovdiv (Bulgaria); Stefanova, Violeta; Kmetov, Veselin; Georgieva, Deyana [Department of Analytical Chemistry, Plovdiv University ' Paisii Hilendarski,' Plovdiv (Bulgaria); Angelova, Violina [Department of Chemistry, University of Agriculture, Plovdiv (Bulgaria)

    2012-05-15

    The most widely used method for determination of total phosphorus in soils is perchloric acid digestion, followed by a colorimetric assay to measure the concentration of P in solution. The first part of this study compares an alternative digestion method, using aqua regia (ISO 11466 and EPA Method 3052), with perchloric acid digestion procedure, and also compares inductively coupled plasma mass spectroscopy (ICP-MS) with colorimetry for the measurement of P on the basis of five internationally certified standard soils and 20 real-life soils with widely different extractability of phosphorus. The phosphorus concentration was determined by means of the reduced phosphomolybdenum blue and ICP-MS. The relationship between methods has been examined statistically. Good agreement of the results from colorimetry and ICP-MS was established for all certified soils. The microwave-assisted digestion with aqua regia was comparable, both in precision and accuracy, with the hot plate aqua regia method. The phosphorus concentration found with the HF + HClO{sub 4} digestion method was in good agreement with the certified mean values, while the superiority in extracting phosphorus, when compared to other methods, was obvious. Soil testing for plant-available phosphorus in Bulgaria and many European countries is most commonly conducted using acid Ca-lactate extraction (Egner-Riehm test) and alkaline sodium bicarbonate extraction (BDS ISO 11263:2002), based on Olsen test, followed by a colorimetric assay to measure the concentration of P in solution. The second part of this study reports the differences between Egner-Riehm test and BDS ISO 11263:2002 measured colorimetrically and by ICP-MS. Fifty soils were selected from South Bulgaria to represent a wide range of soil properties. It was established that ICP-MS consistently yielded significantly higher P concentrations than the colorimetric method in both extraction tests, and the relative differences were greatest in soils with lower

  10. Air pollution studies using PIXE and ICP methods

    International Nuclear Information System (INIS)

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

    2006-01-01

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

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

    International Nuclear Information System (INIS)

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

    1995-01-01

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

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

    International Nuclear Information System (INIS)

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

    2008-01-01

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

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

    Science.gov (United States)

    Nie, Xi-Du; Fu, Liang

    2013-07-01

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

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

    Science.gov (United States)

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

    2016-09-01

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

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

    DEFF Research Database (Denmark)

    Andersen, Jens Enevold Thaulov

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

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

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2004-01-01

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

  17. Ideal gas behavior of a strongly coupled complex (dusty) plasma.

    Science.gov (United States)

    Oxtoby, Neil P; Griffith, Elias J; Durniak, Céline; Ralph, Jason F; Samsonov, Dmitry

    2013-07-05

    In a laboratory, a two-dimensional complex (dusty) plasma consists of a low-density ionized gas containing a confined suspension of Yukawa-coupled plastic microspheres. For an initial crystal-like form, we report ideal gas behavior in this strongly coupled system during shock-wave experiments. This evidence supports the use of the ideal gas law as the equation of state for soft crystals such as those formed by dusty plasmas.

  18. Nonlinear charge reduction effect in strongly coupled plasmas

    International Nuclear Information System (INIS)

    Sarmah, D; Tessarotto, M; Salimullah, M

    2006-01-01

    The charge reduction effect, produced by the nonlinear Debye screening of high-Z charges occurring in strongly coupled plasmas, is investigated. An analytic asymptotic expression is obtained for the charge reduction factor (f c ) which determines the Debye-Hueckel potential generated by a charged test particle. Its relevant parametric dependencies are analysed and shown to predict a strong charge reduction effect in strongly coupled plasmas

  19. Collisional Thermalization in Strongly Coupled Ultracold Neutral Plasmas

    Science.gov (United States)

    2017-01-25

    calculated collisions rates in a strongly coupled plasma. From Bannasch et al., PRL 109, 185008 (2012). DISTRIBUTION A: Distribution approved for public...applicability to other plasmas.) We use a Green- Kubo relation to extract the diffusion constant from our measurements of the relaxation towards...strongly coupled systems. Our measurements (data symbols) agree with numerical calculations (solid lines) from J. Daligault, PRL 108, 225004 (2012

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

    International Nuclear Information System (INIS)

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

    2010-01-01

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

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

    International Nuclear Information System (INIS)

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

    1987-01-01

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

  2. A separation method to overcome the interference of aluminium on zinc determination by inductively coupled plasma atomic emission spectroscopy

    OpenAIRE

    Jesus, Djane S. de; Korn, Maria das Graças Andrade; Ferreira, Sergio Luis Costa; Carvalho, Marcelo Souza de

    2000-01-01

    Texto completo: acesso restrito. p.389–394 The use of polyurethane foam (PUF) to separate zinc from large amounts of aluminium and its determination by inductively coupled plasma atomic emission spectroscopy technique (ICP-AES) in aluminium matrices is described. The proposed method is based on the solid-phase extraction of the zinc(II) cation as a thiocyanate complex. Parameters such as effect of pH on zinc sorption, zinc desorption from the foam and analytical features of the procedure w...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2008-11-23

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

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

    International Nuclear Information System (INIS)

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

    2008-01-01

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

  5. PIXE analysis of human stones: comparison with data from ICP-AES

    International Nuclear Information System (INIS)

    Pougnet, M.A.B.; Peisach, M.; Pineda, C.A.; Rodgers, A.L.

    1987-01-01

    25 human stone samples previously analyzed by inductively coupled plasma atomic emission spectroscopy (ICP-AES) and the IAEA Animal Bone Standard Reference Material were used to evaluate trace element analysis by PIXE. Bombardment with 4 MeV protons was used for the determination of Mn, Fe, Cu, Pb, Br, Rb, Sr and Ca. PIXE and ICP-AES data gave correlation factors better than 0.97 for the elements Ca, Fe, Zn, Sr and Pb. (author) 9 refs.; 5 figs

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

    International Nuclear Information System (INIS)

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

    2009-01-01

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

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

    Science.gov (United States)

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

    2015-07-23

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

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

    Science.gov (United States)

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

    2016-04-01

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

  9. Dry etching of ITO by magnetic pole enhanced inductively coupled plasma for display and biosensing devices

    Energy Technology Data Exchange (ETDEWEB)

    Meziani, T. [European Commission, Joint Research Centre, Institute for Health and Consumer Protection, 21020 Ispra (Vatican City State, Holy See,) (Italy)]. E-mail: tarik.meziani@jrc.it; Colpo, P. [European Commission, Joint Research Centre, Institute for Health and Consumer Protection, 21020 Ispra (Va) (Italy)]. E-mail: pascal.colpo@jrc.it; Lambertini, V. [Centro Ricerche Fiat, Strada Torino 50, 10043 Orbassano (TO) (Italy); Ceccone, G. [European Commission, Joint Research Centre, Institute for Health and Consumer Protection, 21020 Ispra (Va) (Italy); Rossi, F. [European Commission, Joint Research Centre, Institute for Health and Consumer Protection, 21020 Ispra (Va) (Italy)

    2006-03-15

    The dry etching of indium tin oxide (ITO) layers deposited on glass substrates was investigated in a high density inductively coupled plasma (ICP) source. This innovative low pressure plasma source uses a magnetic core in order to concentrate the electromagnetic energy on the plasma and thus provides for higher plasma density and better uniformity. Different gas mixtures were tested containing mainly hydrogen, argon and methane. In Ar/H{sub 2} mixtures and at constant bias voltage (-100 V), the etch rate shows a linear dependence with input power varying the same way as the ion density, which confirms the hypothesis that the etching process is mainly physical. In CH{sub 4}/H{sub 2} mixtures, the etch rate goes through a maximum for 10% CH{sub 4} indicating a participation of the radicals to the etching process. However, the etch rate remains quite low with this type of gas mixture (around 10 nm/min) because the etching mechanism appears to be competing with a deposition process. With CH{sub 4}/Ar mixtures, a similar feature appeared but the etch rate was much higher, reaching 130 nm/min at 10% of CH{sub 4} in Ar. The increase in etch rate with the addition of a small quantity of methane indicates that the physical etching process is enhanced by a chemical mechanism. The etching process was monitored by optical emission spectroscopy that appeared to be a valuable tool for endpoint detection.

  10. Fluorescence imaging of ion distributions in an inductively coupled plasma with laser ablation sample introduction

    International Nuclear Information System (INIS)

    Moses, Lance M.; Ellis, Wade C.; Jones, Derick D.; Farnsworth, Paul B.

    2015-01-01

    High-resolution images of the spatial distributions of Sc II, Ca II, and Ba II ion densities in the 10 mm upstream from the sampling cone in a laser ablation-inductively coupled plasma-mass spectrometer (LA-ICP-MS) were obtained using planar laser induced fluorescence. Images were obtained for each analyte as a function of the carrier gas flow rate with laser ablation (LA) sample introduction and compared to images with solution nebulization (SN) over the same range of flow rates. Additionally, images were obtained using LA at varying fluences and with varying amounts of helium added to a constant flow of argon gas. Ion profiles in SN images followed a pattern consistent with previous work: increasing gas flow caused a downstream shift in the ion profiles. When compared to SN, LA led to ion profiles that were much narrower radially and reached a maximum near the sampling cone at higher flow rates. Increasing the fluence led to ions formed in the ICP over greater axial and radial distances. The addition of He to the carrier gas prior to the ablation cell led to an upstream shift in the position of ionization and lower overall fluorescence intensities. - Highlights: • We map distributions of analytes in the ICP using laser ablation sample introduction. • We compare images from laser ablation with those from a pneumatic nebulizer. • We document the effects of water added to the laser ablation aerosol. • We compare distributions from a metal to those from crystalline solids. • We document the effect of laser fluence on ion distributions

  11. Deposition of controllable preferred orientation silicon films on glass by inductively coupled plasma chemical vapor deposition

    International Nuclear Information System (INIS)

    Li Junshuai; Wang Jinxiao; Yin Min; Gao Pingqi; He Deyan; Chen Qiang; Li Yali; Shirai, Hajime

    2008-01-01

    An inductively coupled plasma (ICP) system with the adjustable distance between the inductance coil and substrates was designed to effectively utilize the spatial confinement of ICP discharge, and then control the gas-phase transport process. The effects of the gas phase processes on the crystallinity and preferred orientation of silicon films deposited on glass were systematically investigated. The investigation was conducted in the ICP-chemical vapor deposition process with the precursor gas of a SiH 4 /H 2 mixture at a substrate temperature of 350 deg. Highly crystallized silicon films with different preferred orientations, (111) or (220), could be selectively deposited by adjusting the SiH 4 dilution ratio [R=[SiH 4 ]/([SiH 4 ]+[H 2 ])] or total working pressure. When the total working pressure is 20 Pa, the crystallinity of the silicon films increases with the increase of the SiH 4 dilution ratio, while the preferred orientation was changed from (111) to (220). In the case of the fixed SiH 4 dilution (10%), the silicon film with I (220) /I (111) of about 3.5 and Raman crystalline fraction of about 89.6% has been deposited at 29.7 nm/min when the total working pressure was increased to 40 Pa. At the fixed SiH 4 partial pressure of 2 Pa, the film crystallinity decreases and the preferred orientation is always (111) with increasing the H 2 partial pressure from 18 to 58 Pa. Atomic force microscope reveals that the film deposited at a relatively high H 2 partial pressure has a very rough surface caused by the devastating etching of H atoms to the silicon network

  12. Copper Determination in Gunshot Residue by Cyclic Voltammetric and Inductive Coupled Plasma-Optical Emission Spectroscopy

    Directory of Open Access Journals (Sweden)

    Mohd Hashim Nurul’Afiqah Hashimah

    2016-01-01

    Full Text Available Analysis of gunshot residue (GSR is a crucial evidences for a forensic analyst in the fastest way. GSR analysis insists a suitable method provides a relatively simple, rapid and precise information on the spot at the crime scene. Therefore, the analysis of Cu(II in GSR using cyclic voltammetry (CV on screen printed carbon electrode (SPCE is a better choice compared to previous alternative methods such as Inductive Coupled Plasma-Optical Emission Spectroscopy (ICP-OES those required a long time for analysis. SPCE is specially designed to handle with microvolumes of sample such as GSR sample. It gives advantages for identification of copper in GSR on-site preliminary test to prevent the sample loss on the process to be analyzed in the laboratory. SPCE was swabbed directly on the shooter’s arm immediately after firing and acetate buffer was dropped on SPCE before CV analysis. For ICP-OES analysis, cotton that had been soaked in 0.5 M nitric acid was swabbed on the shooter’s arm immediately after firing and kept in a tightly closed sampling tube. Gold coated SPCE that had been through nanoparticles modification exhibits excellent performance on voltammograms. The calibration was linear from 1 to 50 ppm of copper, the limit of detection for copper was 0.3 ppm and a relative standard deviation was 6.1 %. The method was successfully applied to the determination of copper in GSR. The Cu determination on SPCE was compared and validated by ICP-OES method with 94 % accuracy.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-08-15

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-10-20

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

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

    International Nuclear Information System (INIS)

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

    2016-01-01

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

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

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

    2016-05-01

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

  18. 2D elemental mapping of sections of human kidney stones using laser ablation inductively-coupled plasma-mass spectrometry: Possibilities and limitations

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-10-01

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

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-08-01

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

  1. Energy coupling to the plasma in repetitive nanosecond pulse discharges

    International Nuclear Information System (INIS)

    Adamovich, Igor V.; Nishihara, Munetake; Choi, Inchul; Uddi, Mruthunjaya; Lempert, Walter R.

    2009-01-01

    A new analytic quasi-one-dimensional model of energy coupling to nanosecond pulse discharge plasmas in plane-to-plane geometry has been developed. The use of a one-dimensional approach is based on images of repetitively pulsed nanosecond discharge plasmas in dry air demonstrating that the plasma remains diffuse and uniform on a nanosecond time scale over a wide range of pressures. The model provides analytic expressions for the time-dependent electric field and electron density in the plasma, electric field in the sheath, sheath boundary location, and coupled pulse energy. The analytic model predictions are in very good agreement with numerical calculations. The model demonstrates that (i) the energy coupled to the plasma during an individual nanosecond discharge pulse is controlled primarily by the capacitance of the dielectric layers and by the breakdown voltage and (ii) the pulse energy coupled to the plasma during a burst of nanosecond pulses decreases as a function of the pulse number in the burst. This occurs primarily because of plasma temperature rise and resultant reduction in breakdown voltage, such that the coupled pulse energy varies approximately proportionally to the number density. Analytic expression for coupled pulse energy scaling has been incorporated into the air plasma chemistry model, validated previously by comparing with atomic oxygen number density measurements in nanosecond pulse discharges. The results of kinetic modeling using the modified air plasma chemistry model are compared with time-resolved temperature measurements in a repetitively pulsed nanosecond discharge in air, by emission spectroscopy, and purely rotational coherent anti-Stokes Raman spectroscopy showing good agreement.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-10-12

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

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

    Science.gov (United States)

    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. .

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

    International Nuclear Information System (INIS)

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

    2004-01-01

    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 Cl 2 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 Cl 2 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 deg. 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

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

    International Nuclear Information System (INIS)

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

    2009-01-01

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

  6. 'Age' Determination of Irradiated Materials Utilizing Inductively Coupled Plasma Mass Spectrometric (ICP-MS) Detection

    International Nuclear Information System (INIS)

    Sommers, James; Giglio, Jeffrey J.; Cummings, Daniel; Carney, Kevin P.

    2009-01-01

    A gas pressurized extraction chromatography (GPEC) system has been developed to perform elemental separations on radioactive samples to determine total and isotopic compositions of Cs and Ba from an irradiated salt sample, fuel sample and two sealed radiation sources. The separation is necessary to remove isobaric interferences in the determination of 137Cs, 135Cs, 137Ba, 135Ba, which are used to determine the age of a sample from radioactive decay or purification. The micro-column extraction chromatography system employs compressed nitrogen to move liquid through the system, compared to gravity or pumped liquids that are typically used for separations. The use of compressed gas allows for accurate and precise recovery of all liquids put into the chromatography system, enabling very accurate dilutions. The use of a small analytical column permits the use of very small amounts of liquids to be used. As a benefit, the amount of radiological waste that is generated in the separation process is minimized. For this work, a commercially available Sr-Resin(trademark) was used to perform the separation for the above mentioned analytes. The column consists of a 7 inch piece of 1/16 in. O.D. x 0.030 in I.D. Teflon(trademark) tubing having an internal volume of 81 (micro)L. To this column, 49 mg of resin was added. The columns are re-usable after regeneration with 3 M HNO3. All samples were separated using batch collection, although real time analysis is possible with the current experimental design. A 1 % acetic acid solution was determined to be the best extractant for Ba. A flow rate of 0.1 mL/min was determined to be optimal for the separation of Ba. Complete recovery of the Cs and Ba was achieved, within the systematic error of the experiments.

  7. 'Age' determination of irradiated materials utilizing inductively coupled plasma mass spectrometric (ICP-MS) detection

    International Nuclear Information System (INIS)

    Sommers, J.; Cummings, D.; Giglio, J.; Carney, K.

    2009-01-01

    A gas pressurized extraction chromatography (GPEC) system has been developed to perform elemental separations on radioactive samples to determine total and isotopic compositions of Cs and Ba from an irradiated salt sample, fuel sample and two sealed radiation sources. The GPEC system employs compressed nitrogen to move liquid through the system, compared to gravity or pumped liquids that are typically used for separations. A commercially available Sr-Resin TM was used to perform the separation for the above mentioned analytes. A 1% acetic acid solution was determined to be the best extractant for Ba. A flow rate of 0.1 mL/min was determined to be optimal for the separation of Ba. Complete recovery of the Cs and Ba was achieved, within the systematic uncertainties of the experiments. (author)

  8. Analysis of heavy metals in rice bran oil by inductively coupled plasma (ICP) spectrometry

    Science.gov (United States)

    Rice is one of the most important staple crops in the world. Nevertheless, health-conscious consumers have expressed concern regarding the presence of heavy metals, specifically arsenic, in rice. The United Nations Food and Agriculture Organization (UNFAO) limits the arsenic concentration at 0.2 mg/...

  9. Theoretical and experimental studies of a planar inductive coupled rf plasma source as the driver in simulator facility (ISTAPHM) of interactions of waves with the edge plasma on tokamaks

    Science.gov (United States)

    Ghanei, V.; Nasrabadi, M. N.; Chin, O.-H.; Jayapalan, K. K.

    2017-11-01

    This research aims to design and build a planar inductive coupled RF plasma source device which is the driver of the simulator project (ISTAPHM) of the interactions between ICRF Antenna and Plasma on tokamak by using the AMPICP model. For this purpose, a theoretical derivation of the distribution of the RF magnetic field in the plasma-filled reactor chamber is presented. An experimental investigation of the field distributions is described and Langmuir measurements are developed numerically. A comparison of theory and experiment provides an evaluation of plasma parameters in the planar ICP reactor. The objective of this study is to characterize the plasma produced by the source alone. We present the results of the first analysis of the plasma characteristics (plasma density, electron temperature, electron-ion collision frequency, particle fluxes and their velocities, stochastic frequency, skin depth and electron energy distribution functions) as function of the operating parameters (injected power, neutral pressure and magnetic field) as measured with fixed and movable Langmuir probes. The plasma is currently produced only by the planar ICP. The exact goal of these experiments is that the produced plasma by external source can exist as a plasma representative of the edge of tokamaks.

  10. Study on characteristics of coupled cavity chain filled with plasma

    International Nuclear Information System (INIS)

    Li Jianqing; Xiao Shu; Mo Yuanlong

    2003-01-01

    In this paper, by using rigorous field analysis, a coupled-cavity (CC) chain filled with plasma has been analyzed. How the hybrid wave between the cavity mode and plasma mode is formed has been studied. The periodical CC chain filled with plasma demonstrates periodical TG modes with a cutoff frequency of zero. When the plasma density increase to a large scale, the cavity mode of the CC chain overlaps the TG mode, these two modes couple with each other and form the hybrid modes. In the case of hybrid modes, the 'cold' bandwidth and the 'warm' bandwidth expand, and the coupled impedance increases about 5 times larger than that of the vacuum. As a whole, the slow wave characteristics are improved substantially due to the formation of the hybrid mode

  11. Solar terrestrial coupling through space plasma processes

    International Nuclear Information System (INIS)

    Birn, J.

    2000-01-01

    This is the final report of a three-year, Laboratory-Directed Research and Development (LDRD) project at the Los Alamos National Laboratory (LANL). The project investigates plasma processes that govern the interaction between the solar wind, charged particles ejected from the sun, and the earth's magnetosphere, the region above the ionosphere governed by the terrestrial magnetic field. Primary regions of interest are the regions where different plasma populations interact with each other. These are regions of particularly dynamic plasma behavior, associated with magnetic flux and energy transfer and dynamic energy release. The investigations concerned charged particle transport and energization, and microscopic and macroscopic instabilities in the magnetosphere and adjacent regions. The approaches combined space data analysis with theory and computer simulations

  12. Analytical applications of ICP-FTS

    International Nuclear Information System (INIS)

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

    1986-01-01

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

  13. Coupling of RF antennas to large volume helicon plasma

    Directory of Open Access Journals (Sweden)

    Lei Chang

    2018-04-01

    Full Text Available Large volume helicon plasma sources are of particular interest for large scale semiconductor processing, high power plasma propulsion and recently plasma-material interaction under fusion conditions. This work is devoted to studying the coupling of four typical RF antennas to helicon plasma with infinite length and diameter of 0.5 m, and exploring its frequency dependence in the range of 13.56-70 MHz for coupling optimization. It is found that loop antenna is more efficient than half helix, Boswell and Nagoya III antennas for power absorption; radially parabolic density profile overwhelms Gaussian density profile in terms of antenna coupling for low-density plasma, but the superiority reverses for high-density plasma. Increasing the driving frequency results in power absorption more near plasma edge, but the overall power absorption increases with frequency. Perpendicular stream plots of wave magnetic field, wave electric field and perturbed current are also presented. This work can serve as an important reference for the experimental design of large volume helicon plasma source with high RF power.

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

    Science.gov (United States)

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

    2015-07-23

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

  15. An argon–nitrogen–hydrogen mixed-gas plasma as a robust ionization source for inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Makonnen, Yoseif; Beauchemin, Diane, E-mail: diane.beauchemin@chem.queensu.ca

    2014-09-01

    Multivariate optimization of an argon–nitrogen–hydrogen mixed-gas plasma for minimum matrix effects, while maintaining analyte sensitivity as much as possible, was carried out in inductively coupled plasma mass spectrometry. In the presence of 0.1 M Na, the 33.9 ± 3.9% (n = 13 elements) analyte signal suppression on average observed in an all-argon plasma was alleviated with the optimized mixed-gas plasma, the average being − 4.0 ± 8.8%, with enhancement in several cases. An addition of 2.3% v/v N{sub 2} in the outer plasma gas, and 0.50% v/v H{sub 2} to the central channel, as a sheath around the nebulizer gas flow, was sufficient for this drastic increase in robustness. It also reduced the background from ArO{sup +} and Ar{sub 2}{sup +} as well as oxide levels by over an order of magnitude. On the other hand, the background from NO{sup +} and ArN{sup +} increased by up to an order of magnitude while the levels of doubly-charged ions increased to 7% (versus 2.7% in an argon plasma optimized for sensitivity). Furthermore, detection limits were generally degraded by 5 to 15 fold when using the mixed-gas plasma versus the argon plasma for matrix-free solution (although they were better for several elements in 0.1 M Na). Nonetheless, the drastically increased robustness allowed the direct quantitative multielement analysis of certified ore reference materials, as well as the determination of Mo and Cd in seawater, without using any matrix-matching or internal standardization. - Highlights: • Addition of N{sub 2} to the plasma gas and H{sub 2} as a sheath gas results in a very robust ICP. • ArO{sup +} and Ar{sub 2}{sup +} background and oxide levels are reduced by over an order of magnitude. • Multielement analysis of rock digests is possible with a simple external calibration. • No internal standardization or matrix-matching is required for accurate analysis. • Cd and Mo were accurately determined in undiluted seawater.

  16. Some remarks on coherent nonlinear coupling of waves in plasmas

    International Nuclear Information System (INIS)

    Wilhelmsson, H.

    1976-01-01

    The analysis of nonlinear processes in plasma physics has given rise to a basic set of coupled equations. These equations describe the coherent nonlinear evolution of plasma waves. In this paper various possibilities of analysing these equations are discussed and inherent difficulties in the description of nonlinear interactions between different types of waves are pointed out. Specific examples of stimulated excitation of waves are considered. These are the parametric excitation of hybrid resonances in hot magnetized multi-ion component plasma and laser-plasma interactions. (B.D.)

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

    Science.gov (United States)

    Yoshida, Satoshi

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

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

    International Nuclear Information System (INIS)

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

    2011-01-01

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

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

    Science.gov (United States)

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

    2011-02-01

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

  20. On coupling fluid plasma and kinetic neutral physics models

    Directory of Open Access Journals (Sweden)

    I. Joseph

    2017-08-01

    Full Text Available The coupled fluid plasma and kinetic neutral physics equations are analyzed through theory and simulation of benchmark cases. It is shown that coupling methods that do not treat the coupling rates implicitly are restricted to short time steps for stability. Fast charge exchange, ionization and recombination coupling rates exist, even after constraining the solution by requiring that the neutrals are at equilibrium. For explicit coupling, the present implementation of Monte Carlo correlated sampling techniques does not allow for complete convergence in slab geometry. For the benchmark case, residuals decay with particle number and increase with grid size, indicating that they scale in a manner that is similar to the theoretical prediction for nonlinear bias error. Progress is reported on implementation of a fully implicit Jacobian-free Newton–Krylov coupling scheme. The present block Jacobi preconditioning method is still sensitive to time step and methods that better precondition the coupled system are under investigation.

  1. Combination of the ionic-to-atomic line intensity ratios from two test elements for the diagnostic of plasma temperature and electron number density in Inductively Coupled Plasma Atomic Emission Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Tognoni, E. [Istituto per i Processi Chimico-Fisici, Area della Ricerca del Consiglio Nazionale delle Ricerche Via Moruzzi 1, 56124 Pisa (Italy)], E-mail: tognoni@ipcf.cnr.it; Hidalgo, M.; Canals, A. [Departamento de Quimica Analitica, Nutricion y Bromatologia. Universidad de Alicante. Apdo. 99, 03080, Alicante (Spain); Cristoforetti, G.; Legnaioli, S.; Salvetti, A.; Palleschi, V. [Istituto per i Processi Chimico-Fisici, Area della Ricerca del Consiglio Nazionale delle Ricerche Via Moruzzi 1, 56124 Pisa (Italy)

    2007-05-15

    In Inductively Coupled Plasma-Atomic Emission Spectroscopy (ICP-AES) spectrochemical analysis, the MgII(280.270 nm)/MgI(285.213 nm) ionic to atomic line intensity ratio is commonly used as a monitor of the robustness of operating conditions. This approach is based on the univocal relationship existing between intensity ratio and plasma temperature, for a pure argon atmospheric ICP in thermodynamic equilibrium. In a multi-elemental plasma in the lower temperature range, the measurement of the intensity ratio may not be sufficient to characterize temperature and electron density. In such a range, the correct relationship between intensity ratio and plasma temperature can be calculated only when the complete plasma composition is known. We propose the combination of the line intensity ratios of two test elements (double ratio) as an effective diagnostic tool for a multi-elemental low temperature LTE plasma of unknown composition. In particular, the variation of the double ratio allows us discriminating changes in the plasma temperature from changes in the electron density. Thus, the effects on plasma excitation and ionization possibly caused by introduction of different samples and matrices in non-robust conditions can be more accurately interpreted. The method is illustrated by the measurement of plasma temperature and electron density in a specific analytic case.

  2. Elemental speciation via high-performance liquid chromatography combined with inductively coupled plasma atomic emission spectroscopic detection: application of a direct injection nebulizer

    International Nuclear Information System (INIS)

    LaFreniere, K.E; Fassel, V.A.; Eckels, D.E.

    1987-01-01

    An evaluation is presented of a direct injection nebulizer (DIN) interfaced to a high-performance liquid chromatograph (HPLC) with inductively coupled plasma atomic emission spectroscopic (ICP-AES) detection for simultaneous multielement speciation. The limits of detection (LODs) obtained with the DIN interface in the HPLC mode were found to be comparable to those obtained by continuous-flow sample introduction into the ICP, or inferior by up to only a factor of 4. In addition, the DIN allowed for the direct injection into the ICP of a variety of common HPLC solvents (up to 100% methanol, acetonitrile, methyl isobutyl ketone, pyridine, and water). The HPLC-DIN-ICP-AES system was compared to other HPLC-atomic spectroscopic detection techniques and was found to offer substantial improvement over the alternative on-line, detection methods in terms of LODs. Representative applications of the HPLC-DIN-ICP-AES system to the elemental speciation of coal process streams, shale oil, solvent refined coal, and crude oil are presented

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

    International Nuclear Information System (INIS)

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

    1988-01-01

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

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

  5. On plasma coupling and turbulence effects in low velocity stopping

    Energy Technology Data Exchange (ETDEWEB)

    Kurilenkov, Yu K [Unified Institute for High Temperatures of Russian Academy of Sciences, 13/19 Izhorskaya Str., 125412 Moscow (Russian Federation); Maynard, G [Laboratoire de Physique des Gaz et des Plasmas, UMR-8578, Bat. 210, Universite Paris XI, F-91405 Orsay (France); Barriga-Carrasco, M D [Laboratoire de Physique des Gaz et des Plasmas, UMR-8578, Bat. 210, Universite Paris XI, F-91405 Orsay (France); Valuev, A A [Unified Institute for High Temperatures of Russian Academy of Sciences, 13/19 Izhorskaya Str., 125412 Moscow (Russian Federation)

    2006-04-28

    The problem of stopping power (SP) for projectile ions is analysed in terms of the dielectric function and effective collision frequency for moderately dense and strongly coupled plasmas (SCP). We consider several issues regarding the calculation of stopping power for correlated ensembles of particles and oscillators. In particular, effects of group (few particle) modes, transition from positive to negative dispersion and excitation of collective modes up to suprathermal level at plasma targets are addressed. Linear SP of dense suprathermal (nonlinear) plasma targets at different levels of target plasma turbulence is estimated. The force of suprathermal plasma oscillations on the projectile ions is mostly in the nature of increased frictional drag. The results obtained show the possibility of increasing low velocity stopping (up to 'turbulent' values) in comparison with losses in equilibrium dense plasma targets. Experimental conditions to create specific turbulent targets as well as some connection between stopping phenomena and SCP transport properties are discussed briefly.

  6. On plasma coupling and turbulence effects in low velocity stopping

    International Nuclear Information System (INIS)

    Kurilenkov, Yu K; Maynard, G; Barriga-Carrasco, M D; Valuev, A A

    2006-01-01

    The problem of stopping power (SP) for projectile ions is analysed in terms of the dielectric function and effective collision frequency for moderately dense and strongly coupled plasmas (SCP). We consider several issues regarding the calculation of stopping power for correlated ensembles of particles and oscillators. In particular, effects of group (few particle) modes, transition from positive to negative dispersion and excitation of collective modes up to suprathermal level at plasma targets are addressed. Linear SP of dense suprathermal (nonlinear) plasma targets at different levels of target plasma turbulence is estimated. The force of suprathermal plasma oscillations on the projectile ions is mostly in the nature of increased frictional drag. The results obtained show the possibility of increasing low velocity stopping (up to 'turbulent' values) in comparison with losses in equilibrium dense plasma targets. Experimental conditions to create specific turbulent targets as well as some connection between stopping phenomena and SCP transport properties are discussed briefly

  7. ICP analysis of zinc and zamak alloys

    International Nuclear Information System (INIS)

    Gomez Coedo, A.; Dorado Lopez, M.T.

    1987-01-01

    A study was carried out on the possibilities of inductively coupled plasma emission spectrometry (ICP) in the determination of Cu, Cd, Fe, Pb, Sn, Al and Mg in zinc-base materials using direct sample solutions. A selection of analytical lines is made, on account of both their sensitivity and the corresponding study of spectral interferences; measurable minimum contents and calibrated terms are also established, to conduce therefore to a complete methodology which allows determination of the mentioned elements within the contents established on the specifications of these materials. (author)

  8. Microfabricated hollow microneedle array using ICP etcher

    Science.gov (United States)

    Ji, Jing; Tay, Francis E. H.; Miao, Jianmin

    2006-04-01

    This paper presents a developed process for fabrication of hollow silicon microneedle arrays. The inner hollow hole and the fluidic reservoir are fabricated in deep reactive ion etching. The profile of outside needles is achieved by the developed fabrication process, which combined isotropic etching and anisotropic etching with inductively coupled plasma (ICP) etcher. Using the combination of SF6/O2 isotropic etching chemistry and Bosch process, the high aspect ratio 3D and high density microneedle arrays are fabricated. The generated needle external geometry can be controlled by etching variables in the isotropic and anisotropic cases.

  9. Microfabricated hollow microneedle array using ICP etcher

    International Nuclear Information System (INIS)

    Ji Jing; Tay, Francis E H; Miao Jianmin

    2006-01-01

    This paper presents a developed process for fabrication of hollow silicon microneedle arrays. The inner hollow hole and the fluidic reservoir are fabricated in deep reactive ion etching. The profile of outside needles is achieved by the developed fabrication process, which combined isotropic etching and anisotropic etching with inductively coupled plasma (ICP) etcher. Using the combination of SF 6 /O 2 isotropic etching chemistry and Bosch process, the high aspect ratio 3D and high density microneedle arrays are fabricated. The generated needle external geometry can be controlled by etching variables in the isotropic and anisotropic cases

  10. Microfabricated hollow microneedle array using ICP etcher

    Energy Technology Data Exchange (ETDEWEB)

    Ji Jing [Mechanical Engineering National University of Singapore, 119260, Singapore (Singapore); Tay, Francis E H [Mechanical Engineering National University of Singapore, 119260, Singapore (Singapore); Miao Jianmin [MicroMachines Center, School of Mechanical and Aerospace Engineering, Nanyang Technological University, 50 Nanyang Avenue, 639798 (Singapore)

    2006-04-01

    This paper presents a developed process for fabrication of hollow silicon microneedle arrays. The inner hollow hole and the fluidic reservoir are fabricated in deep reactive ion etching. The profile of outside needles is achieved by the developed fabrication process, which combined isotropic etching and anisotropic etching with inductively coupled plasma (ICP) etcher. Using the combination of SF{sub 6}/O{sub 2} isotropic etching chemistry and Bosch process, the high aspect ratio 3D and high density microneedle arrays are fabricated. The generated needle external geometry can be controlled by etching variables in the isotropic and anisotropic cases.

  11. Experimental evaluation of analyte excitation mechanisms in the inductively coupled plasma

    International Nuclear Information System (INIS)

    Lehn, Scott A.; Hieftje, Gary M.

    2003-01-01

    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

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

    International Nuclear Information System (INIS)

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

    2010-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2001-09-15

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

  14. Jeans instability of self-gravitating magnetized strongly coupled plasma

    International Nuclear Information System (INIS)

    Prajapati, R P; Sharma, P K; Sanghvi, R K; Chhajlani, R K

    2012-01-01

    We investigate the Jeans instability of self-gravitating magnetized strongly coupled plasma. The equations of the problem are formulated using the generalized hydrodynamic model and a general dispersion relation is obtained using the normal mode analysis. This dispersion relation is discussed for transverse and longitudinal mode of propagations. The modified condition of Jeans instability is obtained for magnetized strongly coupled plasma. We find that strong coupling of plasma particles modify the fundamental criterion of Jeans gravitational instability. In transverse mode it is found that Jeans instability criterion gets modified due to the presence of magnetic field, shear viscosity and fluid viscosity but in longitudinal mode it is unaffected due to the presence of magnetic field. From the curves we found that all these parameters have stabilizing influence on the growth rate of Jeans instability.

  15. High efficiency nebulization for helium inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Jorabchi, Kaveh; McCormick, Ryan; Levine, Jonathan A.; Liu Huiying; Nam, S.-H.; Montaser, Akbar

    2006-01-01

    A pneumatically-driven, high efficiency nebulizer is explored for helium inductively coupled plasma mass spectrometry. The aerosol characteristics and analyte transport efficiencies of the high efficiency nebulizer for nebulization with helium are measured and compared to the results obtained with argon. Analytical performance indices of the helium inductively coupled plasma mass spectrometry are evaluated in terms of detection limits and precision. The helium inductively coupled plasma mass spectrometry detection limits obtained with the high efficiency nebulizer at 200 μL/min are higher than those achieved with the ultrasonic nebulizer consuming 2 mL/min solution, however, precision is generally better with high efficiency nebulizer (1-4% vs. 3-8% with ultrasonic nebulizer). Detection limits with the high efficiency nebulizer at 200 μL/min solution uptake rate approach those using ultrasonic nebulizer upon efficient desolvation with a heated spray chamber followed by a Peltier-cooled multipass condenser

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

    Science.gov (United States)

    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.

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

    International Nuclear Information System (INIS)

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

    2009-01-01

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

  18. Helicon wave coupling to a chiral-plasma column

    International Nuclear Information System (INIS)

    Torres-Silva, H.; Reggiani, N.; Sakanaka, P.H.

    1995-01-01

    Inductive helicon wave coupling to a chiro-plasma column is studied numerically. In our theoretical model, the RF current distribution of the chiro-plasma is taken into account using the constitutive relations of a chiral-plasma. Computational results based on the data of present-day helicon devices are show. In particular, we discuss the role of magnetic-field-aligned electron landau damping for the helicon wave absorption. In many a see, the numerical findings can be understood reasonably in terms of the wavenumber spectra of the helicon wave dispersion relation for slow and fast wave of a chiral-plasma. In general however, the full electromagnetic treatment is necessary in order to describe and to understand the inductive coupling in the helicon wave regime. (author). 9 refs., 1 fig

  19. A new class of strongly coupled plasmas inspired by sonoluminescence

    Science.gov (United States)

    Bataller, Alexander; Plateau, Guillaume; Kappus, Brian; Putterman, Seth

    2014-10-01

    Sonoluminescence originates in a strongly coupled plasma with a near liquid density and a temperature of ~10,000 K. This plasma is in LTE and therefore, it should be a general thermodynamic state. To test the universality of sonoluminescence, similar plasma conditions were generated using femtosecond laser breakdown in high pressure gases. Calibrated streak spectroscopy reveals both transport and thermodynamic properties of a strongly coupled plasma. A blackbody spectrum, which persists long after the exciting laser has turned off, indicates the presence of a highly ionized LTE microplasma. In parallel with sonoluminescence, this thermodynamic state is achieved via a considerable reduction in the ionization potential. We gratefully acknowledge support from DARPA MTO for research on microplasmas. We thank Brian Naranjo, Keith Weninger, Carlos Camara, Gary Williams, and John Koulakis for valuable discussions.

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

    Digital Repository Service at National Institute of Oceanography (India)

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

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

  1. Inductively-coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Dale, L.

    1990-01-01

    The instrument in operation at the Lucas Heights Research Laboratories is a VG Plasma-quad PQ 2. A schematic diagram of the instrument components is presented along with its applicability to various fields of research and its perceived limitations. Apart from its high sensitivity the capability for rapid multi-element analysis in one of its major advantages over other instrumental method analysis. The necessity to present the sample in the form of a solution is probably its major drawback. 4 tabs, 7 figs

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

    Science.gov (United States)

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

    2011-05-01

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

  3. Standard practice for analysis of aqueous leachates from nuclear waste materials using inductively coupled plasma-atomic emission spectrometry

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2010-01-01

    1.1 This practice is applicable to the determination of low concentration and trace elements in aqueous leachate solutions produced by the leaching of nuclear waste materials, using inductively coupled plasma-atomic emission spectroscopy (ICP-AES). 1.2 The nuclear waste material may be a simulated (non-radioactive) solid waste form or an actual solid radioactive waste material. 1.3 The leachate may be deionized water or any natural or simulated leachate solution containing less than 1 % total dissolved solids. 1.4 This practice should be used by analysts experienced in the use of ICP-AES, the interpretation of spectral and non-spectral interferences, and procedures for their correction. 1.5 No detailed operating instructions are provided because of differences among various makes and models of suitable ICP-AES instruments. Instead, the analyst shall follow the instructions provided by the manufacturer of the particular instrument. This test method does not address comparative accuracy of different devices...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-02-17

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

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

    Science.gov (United States)

    Lin, Li; Chen, Guang; Chen, Yuhong

    2011-07-01

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

  6. Equation of state of strongly coupled plasma mixtures

    International Nuclear Information System (INIS)

    DeWitt, H.E.

    1984-01-01

    Thermodynamic properties of strongly coupled (high density) plasmas of mixtures of light elements have been obtained by Monte Carlo simulations. For an assumed uniform charge background the equation of state of ionic mixtures is a simple extension of the one-component plasma EOS. More realistic electron screening effects are treated in linear response theory and with an appropriate electron dielectric function. Results have been obtained for the ionic pair distribution functions, and for the electric microfield distribution

  7. Non-Equilibrium Modeling of Inductively Coupled RF Plasmas

    Science.gov (United States)

    2015-01-01

    wall can be approximated with the expression for an infinite solenoid , B(r = R) = µ0NIc, where quan- tities N and Ic are the number of turns per unit...Modeling of non-equilibrium plasmas in an induc- tively coupled plasma facility. AIAA Paper 2014– 2235, 2014. 45th AIAA Plasmadynamics and Lasers ...1993. 24th Plas- madynamics and Laser Conference, Orlando, FL. [22] M. Capitelli, I. Armenise, D. Bruno, M. Caccia- tore, R. Celiberto, G. Colonna, O

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

    International Nuclear Information System (INIS)

    Matsuura, Hirotaka; Hokura, Akiko; Haraguchi, Hiroki

    2000-01-01

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

  9. Study of optical emission spectroscopy with inductively coupled plasma torch

    International Nuclear Information System (INIS)

    Bauer, M.

    1982-01-01

    Inductively coupled plasma optical emission spectroscopy is an excellent tool for quantitative multielement trace analysis. This paper describes the performance of a computer-controlled sequential measurement system. Chemical and ionization interferences are shown to be negligible due to the characteristics of the inductively coupled plasma, spectral interferences are eliminated by using a high-resolution monochromator and computer data handling. Good accuracy is achieved for most of the interesting elements, as is shown from both an interlaboratory test and from comparison of the results of water samples from the rivers Elbe and Weser with those achieved with neutron activation and X-ray fluorescence analysis. (orig.) [de

  10. Modeling of Perpendicularly Driven Dual-Frequency Capacitively Coupled Plasma

    International Nuclear Information System (INIS)

    Wang Hongyu; Sun Peng; Zhao Shuangyun; Li Yang; Jiang Wei

    2016-01-01

    We analyzed perpendicularly configured dual-frequency (DF) capacitively coupled plasmas (CCP). In this configuration, two pairs of electrodes are arranged oppositely, and the discharging is perpendicularly driven by two radio frequency (RF) sources. Particle-in-cell/Monte Carlo (PIC/MC) simulation showed that the configuration had some advantages as this configuration eliminated some dual frequency coupling effects. Some variation and potential application of the discharging configuration is discussed briefly. (paper)

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-07-23

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

  13. Quality control of Al alloy by ICP-MS

    International Nuclear Information System (INIS)

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

    2000-01-01

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

  14. ICP-MS analysis for long-lived radionuclides

    International Nuclear Information System (INIS)

    Roos, P.

    2010-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2000-11-01

    As a result of the accident at the Chernobyl nuclear power plant (NPP) the environment was contaminated with spent nuclear fuel. The {sup 236}U isotope was used in this study to monitor the spent uranium from nuclear fallout in soil samples collected in the vicinity of the Chernobyl NPP. A rapid and sensitive analytical procedure was developed for uranium isotopic ratio measurement in environmental samples based on inductively coupled plasma quadrupole mass spectrometry with a hexapole collision cell (HEX-ICP-QMS). The figures of merit of the HEX-ICP-QMS were studied with a plasma-shielded torch using different nebulizers (such as an ultrasonic nebulizer (USN) and Meinhard nebulizer) for solution introduction. A {sup 238}U{sup +} ion intensity of up to 27000 MHz/ppm in HEX-ICP-QMS with USN was observed by introducing helium into the hexapole collision cell as the collision gas at a flow rate of 10 ml min{sup -1}. The formation rate of uranium hydride ions UH{sup +}/U{sup +} of 2 x 10{sup -6} was obtained by using USN with a membrane desolvator. The limit of {sup 236}U/{sup 238}U ratio determination in 10 {mu}g 1{sup -1} uranium solution was 3 x 10{sup -7} corresponding to the detection limit for {sup 236}U of 3 pg 1{sup -1}. The precision of uranium isotopic ratio measurements in 10 {mu}g 1{sup -1} laboratory uranium isotopic standard solution was 0.13% ({sup 235}U/{sup 238}U) and 0.33% ({sup 236}U/{sup 238}U) using a Meinhard nebulizer and 0.45% ({sup 235}U/{sup 238}U) and 0.88% ({sup 236}U/{sup 238}U) using a USN. The isotopic composition of all investigated Chernobyl soil samples differed from those of natural uranium; i.e. in these samples the {sup 236}U/{sup 238}U ratio ranged from 10{sup -5} to 10{sup -3}. (orig.)

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

    Science.gov (United States)

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

    2012-10-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-01-01

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

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

    Science.gov (United States)

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

  19. Redox speciation of final repository relevant elements using separation methods in combination with ICP mass spectrometry; Redoxspeziation von endlagerrelevanten Elementen mit Hilfe von Trennmethoden gekoppelt an ein Massenspektrometer mit induktiv gekoppeltem Plasma

    Energy Technology Data Exchange (ETDEWEB)

    Graser, Carl-Heinrich

    2015-12-18

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

  20. Antenna coupling study for ICWC plasma characterization in TEXTOR

    Indian Academy of Sciences (India)

    2015-11-27

    Home; Journals; Pramana – Journal of Physics; Volume 80; Issue 1. Antenna coupling study for ICWC plasma characterization in ... Proceedings of the International Workshop/Conference on Computational Condensed Matter Physics and Materials Science (IWCCMP-2015). Posted on November 27, 2015. Guest Editors: ...

  1. Radial Distribution Functions of Strongly Coupled Two-Temperature Plasmas

    Science.gov (United States)

    Shaffer, Nathaniel R.; Tiwari, Sanat Kumar; Baalrud, Scott D.

    2017-10-01

    We present tests of three theoretical models for the radial distribution functions (RDFs) in two-temperature strongly coupled plasmas. RDFs are useful in extending plasma thermodynamics and kinetic theory to strong coupling, but they are usually known only for thermal equilibrium or for approximate one-component model plasmas. Accurate two-component modeling is necessary to understand the impact of strong coupling on inter-species transport, e.g., ambipolar diffusion and electron-ion temperature relaxation. We demonstrate that the Seuferling-Vogel-Toeppfer (SVT) extension of the hypernetted chain equations not only gives accurate RDFs (as compared with classical molecular dynamics simulations), but also has a simple connection with the Yukawa OCP model. This connection gives a practical means to recover the structure of the electron background from knowledge of the ion-ion RDF alone. Using the model RDFs in Effective Potential Theory, we report the first predictions of inter-species transport coefficients of strongly coupled plasmas far from equilibrium. This work is supported by NSF Grant No. PHY-1453736, AFSOR Award No. FA9550-16-1-0221, and used XSEDE computational resources.

  2. Numerical experiments on 2D strongly coupled complex plasmas

    International Nuclear Information System (INIS)

    Hou Lujing; Ivlev, A V; Thomas, H M; Morfill, G E

    2010-01-01

    The Brownian Dynamics simulation method is briefly reviewed at first and then applied to study some non-equilibrium phenomena in strongly coupled complex plasmas, such as heat transfer processes, shock wave excitation/propagation and particle trapping, by directly mimicking the real experiments.

  3. Experimental measurements of Helicon wave coupling in KSTAR plasmas

    Energy Technology Data Exchange (ETDEWEB)

    Kim, H. J.; Wi, H. H.; Wang, S. J.; Park, S. Y.; Jeong, J. H.; Han, J. W.; Kwak, J. G.; Oh, Y. K. [National Fusion Research Institute, Daejeon (Korea, Republic of); Chun, M. H.; Yu, I. H. [Pohang Accelerator Laboratory, Pohang (Korea, Republic of)

    2016-05-15

    KSTAR tokamak can be a good platform to test this current drive concept because it has adequate machine parameters. Furthermore, KSTAR will have high electron beta plasmas in near future with additional ECH power. In 2015 KSTAR experiments, low-power traveling wave antenna has been designed, fabricated and installed for helicon wave coupling tests in KSTAT plasmas. In 2016 KSTAR campaign, 200 kW klystron power will be combined using three coaxial hybrid couplers and three dummy loads. High power RF will be fed into the traveling wave antenna with two coaxial feeders through two dual disk windows and 6 inch coaxial transmission line system. Current status and plan for high power helicon wave current drive system in KSTAR will be presented. Mock-up TWA antenna installed at the KSTAR reveals high couplings in both L- and H-mode plasmas. The coupling can be easily controlled by radial outer gap without degradation of plasma confinement or local gas puffing with slight decrease of plasma confinement.

  4. 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

    International Nuclear Information System (INIS)

    Punjabi, Sangeeta B.; Sahasrabudhe, S. N.; Das, A. K.; Joshi, N. K.; Mangalvedekar, H. A.; Kothari, D. C.

    2014-01-01

    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) variation in sheath gas flow rate, and (c) variation in plasma gas flow rate. These studies will be useful for different material processing applications

  5. Thinning of N-face GaN (0001) samples by inductively coupled plasma etching and chemomechanical polishing

    International Nuclear Information System (INIS)

    Rizzi, F.; Gu, E.; Dawson, M. D.; Watson, I. M.; Martin, R. W.; Kang, X. N.; Zhang, G. Y.

    2007-01-01

    The processing of N-polar GaN (0001) samples has been studied, motivated by applications in which extensive back side thinning of freestanding GaN (FS-GaN) substrates is required. Experiments were conducted on FS-GaN from two commercial sources, in addition to epitaxial GaN with the N-face exposed by a laser lift-off process. The different types of samples produced equivalent results. Surface morphologies were examined over relatively large areas, using scanning electron microscopy and stylus profiling. The main focus of this study was on inductively coupled plasma (ICP) etch processes, employing Cl 2 /Ar or Cl 2 /BCl 3 Ar gas mixtures. Application of a standard etch recipe, optimized for feature etching of Ga-polar GaN (0001) surfaces, caused severe roughening of N-polar samples and confirmed the necessity for specific optimization of etch conditions for N-face material. A series of recipes with a reduced physical (sputter-based) contribution to etching allowed average surface roughness values to be consistently reduced to below 3 nm. Maximum N-face etch rates of 370-390 nm/min have been obtained in recipes examined to date. These are typically faster than etch rates obtained on Ga-face samples under the same conditions and adequate for the process flows of interest. Mechanistic aspects of the ICP etch process and possible factors contributing to residual surface roughness are discussed. This study also included work on chemomechanical polishing (CMP). The optimized CMP process had stock removal rates of ∼500 nm/h on the GaN N face. This was much slower than the ICP etching but showed the important capability of recovering smooth surfaces on samples roughened in previous processing. In one example, a surface roughened by nonoptimized ICP etching was smoothed to give an average surface roughness of ∼2 nm

  6. The strongly coupled quark-gluon plasma created at RHIC

    CERN Document Server

    Heinz, Ulrich W

    2009-01-01

    The Relativistic Heavy Ion Collider (RHIC) was built to re-create and study in the laboratory the extremely hot and dense matter that filled our entire universe during its first few microseconds. Its operation since June 2000 has been extremely successful, and the four large RHIC experiments have produced an impressive body of data which indeed provide compelling evidence for the formation of thermally equilibrated matter at unprecedented temperatures and energy densities -- a "quark-gluon plasma (QGP)". A surprise has been the discovery that this plasma behaves like an almost perfect fluid, with extremely low viscosity. Theorists had expected a weakly interacting gas of quarks and gluons, but instead we seem to have created a strongly coupled plasma liquid. The experimental evidence strongly relies on a feature called "elliptic flow" in off-central collisions, with additional support from other observations. This article explains how we probe the strongly coupled QGP, describes the ideas and measurements whi...

  7. The effect of CF4 addition on Ru etching with inductively coupled plasma

    International Nuclear Information System (INIS)

    Lim, Kyu Tae; Kim, Dong Pyo; Kim, Kyoung Tae; Kim, Chang Il

    2003-01-01

    Ru thin films were etched in CF 4 /O 2 plasma using an ICP (inductively coupled plasma etching) system. The etch rate of Ru thin films was examined as a function of gas mixing ratio. The maximum etch rate of Ru thin films was 168 nm/min at a CF 4 /O 2 gas mixing ratio of 10 %. The selectivity of Ru over SiO 2 was 1.3. From the OES (optical emission spectroscopy), the optical emission intensity of the O radical had a maximum value at 10 % of CF 4 gas concentration and decrease with further addition of CF 4 gas. From XPS (x-ray photoelectron spectroscopy) analysis, Ru-F bonds by the chemical reaction of Ru and F appeared in the surface of the etched Ru thin film in CF 4 /O 2 chemistry. RuF 3-4 compounds were suggested as a surface passivation layer that reduces the chemical reactions between Ru and O radicals. In a FE-SEM (field emission scanning electron microscope) micrograph, we had an almost perpendicular taper angle of 89 .deg.

  8. Deposition of silicon oxynitride at room temperature by Inductively Coupled Plasma-CVD

    Energy Technology Data Exchange (ETDEWEB)

    Zambom, Luis da Silva [MPCE-Faculdade de Tecnologia de Sao Paulo - CEETEPS, Pca Coronel Fernando Prestes, 30, Sao Paulo - CEP 01124-060 (Brazil)]. E-mail: zambom@lsi.usp.br; Verdonck, Patrick [PSI-LSI-Escola Politecnica da Universidade de Sao Paulo (Brazil)]. E-mail: patrick@lsi.usp.br

    2006-10-25

    Oxynitride thin films are used in important optical applications and as gate dielectric for MOS devices.