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Sample records for spectrometry techniques estudo

  1. Spectrometry techniques for radioactivity measurements

    International Nuclear Information System (INIS)

    Anilkumar, S.

    2016-01-01

    The energy of the radiation emission following the nuclear decay is unique and the characteristic of the radio nuclide which undergoes decay. Thus measurement of the energy of the radiation offers a method of identifying the radio nuclides. The prime requirement of the energy measurement is a suitable detector which shows response proportional to the energy of the radiation rather than the presence of the radiation. The response from such detectors are suitably processed and distributed with respect to the signal strength which is proportional to incident energy. This distribution is normally referred as energy spectrum and is recorded in the multichannel analyser. The measurement of energy and intensity of radiation from the spectrum is called radiation spectrometry. Thus the radiation spectrometry allows the identification and quantification of radioactive isotopes in variety of matrices. The radiation spectrometry has now become a popular radioanalytical technique in wide area of nuclear fuel cycle programs. The popular spectrometry techniques commonly used for the radioactivity measurement and analysis are Alpha spectrometry, Gamma ray spectrometry and Beta spectrometry

  2. Mass spectrometry. [review of techniques

    Science.gov (United States)

    Burlingame, A. L.; Kimble, B. J.; Derrick, P. J.

    1976-01-01

    Advances in mass spectrometry (MS) and its applications over the past decade are reviewed in depth, with annotated literature references. New instrumentation and techniques surveyed include: modulated-beam MS, chromatographic MS on-line computer techniques, digital computer-compatible quadrupole MS, selected ion monitoring (mass fragmentography), and computer-aided management of MS data and interpretation. Areas of application surveyed include: organic MS and electron impact MS, field ionization kinetics, appearance potentials, translational energy release, studies of metastable species, photoionization, calculations of molecular orbitals, chemical kinetics, field desorption MS, high pressure MS, ion cyclotron resonance, biochemistry, medical/clinical chemistry, pharmacology, and environmental chemistry and pollution studies.

  3. Liquid scintillation alpha spectrometry techniques

    International Nuclear Information System (INIS)

    McKlveen, J.W.; McDowell, W.J.

    1984-01-01

    Accurate, quantitative determinations of alpha emitting nuclides by conventional plate counting methods are difficult, because of sample self-absorption problems in counting and because of non-reproducible losses in conventional sample separation methods. Liquid scintillation alpha spectrometry offers an attractive alternative with no sample self-absorption or geometry problems and with 100% counting efficiency. Sample preparation may include extraction of the alpha emitter of interest by a specific organic phase-soluble compound directly into the liquid scintillation counting medium. Detection electronics use energy and pulse-shape discrimination, to yield alpha spectra without beta and gamma background interference. Specific procedures have been developed for gross alpha, uranium, plutonium, thorium and colonium assay. Possibilities for a large number of other applications exist. Accuracy and reproducibility are typically in the 1% range. Backgrounds of the order of 0.01 cpm are readily achievable. The paper will present an overview of liquid scintillation alpha counting techniques and some of the results achieved for specific applications. (orig.)

  4. Identification of bacteria using mass spectrometry techniques

    Czech Academy of Sciences Publication Activity Database

    Krásný, Lukáš; Hynek, R.; Hochel, I.

    2013-01-01

    Roč. 353, NOV 2013 (2013), s. 67-79 ISSN 1387-3806 R&D Projects: GA ČR GAP503/10/0664 Institutional support: RVO:61388971 Keywords : Mass spectrometry * Bacteria * Identification Subject RIV: EE - Microbiology, Virology Impact factor: 2.227, year: 2013

  5. Plutonium determination in urine by techniques of mass spectrometry

    International Nuclear Information System (INIS)

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

    2013-10-01

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

  6. Sample preparation techniques for (p, X) spectrometry

    International Nuclear Information System (INIS)

    Whitehead, N.E.

    1985-01-01

    Samples are ashed at low temperature, using oxygen plasma; a rotary evaporator, and freeze drying speeded up the ashing. The new design of apparatus manufactured was only 10 watt but was as efficient as a 200 watt commercial machine; a circuit diagram is included. Samples of hair and biopsy samples of skin were analysed by the technique. A wool standard was prepared for interlaboratory comparison exercises. It was based on New Zealand merino sheep wool and was 2.9 kg in weight. A washing protocol was developed, which preserves most of the trace element content. The wool was ground in liquid nitrogen using a plastic pestle and beaker, driven by a rotary drill press. (author)

  7. Emerging mass spectrometry techniques for the direct analysis of microbial colonies

    OpenAIRE

    Fang, Jinshu; Dorrestein, Pieter C.

    2014-01-01

    One of the emerging areas in microbiology is detecting specialized metabolites produced by microbial colonies and communities with mass spectrometry. In this review/perspective, we illustrate the emerging mass spectrometry methodologies that enable the interrogation of specialized metabolites directly from microbial colonies. Mass spectrometry techniques such as imaging mass spectrometry and real-time mass spectrometry allow two and three dimensional visualization of the distri...

  8. Water Vapor Remote Sensing Techniques: Radiometry and Solar Spectrometry

    Science.gov (United States)

    Somieski, A.; Buerki, B.; Cocard, M.; Geiger, A.; Kahle, H.-G.

    The high variability of atmospheric water vapor content plays an important role in space geodesy, climatology and meteorology. Water vapor has a strong influence on transatmospheric satellite signals, the Earth's climate and thus the weather forecasting. Several remote sensing techniques have been developed for the determination of inte- grated precipitable water vapor (IPWV). The Geodesy and Geodynamics Lab (GGL) utilizes the methods of Water Vapor Radiometry and Solar Spectrometry to quantify the amount of tropospheric water vapor and its temporal variations. The Water Vapor Radiometer (WVR) measures the radiation intensity of the atmosphere in a frequency band ranging from 20 to 32 GHz. The Solar Atmospheric MOnitoring Spectrome- ter (SAMOS) of GGL is designed for high-resolution measurements of water vapor absorption lines using solar radiation. In the framework of the ESCOMPTE (ExpÊrience sur Site pour COntraindre les Mod- Éles de Pollution atmosphÊrique et de Transport d'Emissions) field campaign these instruments have been operated near Marseille in 2001. They have aquired a long time series of integrated precipitable water vapor content (IPWV). The accuracy of IPWV measured by WVR and SAMOS is 1 kg/m2. Furthermore meteorological data from radiosondes were used to calculate the IPWV in order to provide comparisons with the results of WVR and SAMOS. The methods of Water Vapor Radiometry and So- lar Spectrometry will be discussed and first preliminary results retrieved from WVR, SAMOS and radiosondes during the ESCOMPTE field campaign will be presented.

  9. Surface Ionization and Soft Landing Techniques in Mass Spectrometry

    International Nuclear Information System (INIS)

    Futrell, Jean H.; Laskin, Julia

    2010-01-01

    The advent of soft ionization techniques, notably electrospray and laser desorption ionization methods, has extended mass spectrometric methods to large molecules and molecular complexes. This both greatly expands applications of mass spectrometry and makes the activation and dissociation of complex ions an integral part of large molecule mass spectrometry. A corollary of the much greater number of internal degrees of freedom and high density of states associated with molecular complexity is that internal energies much higher than the dissociation energies for competing fragmentation processes are required for observable fragmentation in time scales sampled by mass spectrometers. This article describes the kinetics of surface-induced dissociation (SID), a particularly efficient activation method for complex ions. Two very important characteristics of SID are very rapid, sub-picosecond activation and precise control of ion internal energy by varying ion collision energy. The nature of the surface plays an important role in SID, determining both efficiency and mechanism of ion activation. Surface composition and morphology strongly influence the relative importance of competing reactions of SID, ion capture (soft-landing), surface reaction and neutralization. The important features of SID and ion soft-landing are described briefly in this review and more fully in the recommended reading list.

  10. Ion beam analysis and spectrometry techniques for Cultural Heritage studies

    International Nuclear Information System (INIS)

    Beck, L.

    2013-01-01

    The implementation of experimental techniques for the characterisation of Cultural heritage materials has to take into account some requirements. The complexity of these past materials requires the development of new techniques of examination and analysis, or the transfer of technologies developed for the study of advanced materials. In addition, due to precious aspect of artwork it is also necessary to use the non-destructive methods, respecting the integrity of objects. It is for this reason that the methods using radiations and/or particles play a important role in the scientific study of art history and archaeology since their discovery. X-ray and γ-ray spectrometry as well as ion beam analysis (IBA) are analytical tools at the service of Cultural heritage. This report mainly presents experimental developments for IBA: PIXE, RBS/EBS and NRA. These developments were applied to the study of archaeological composite materials: layered materials or mixtures composed of organic and non-organic phases. Three examples are shown: evolution of silvering techniques for the production of counterfeit coinage during the Roman Empire and in the 16. century, the characterization of composites or mixed mineral/organic compounds such as bone and paint. In these last two cases, the combination of techniques gave original results on the proportion of both phases: apatite/collagen in bone, pigment/binder in paintings. Another part of this report is then dedicated to the non-invasive/non-destructive characterization of prehistoric pigments, in situ, for rock art studies in caves and in the laboratory. Finally, the perspectives of this work are presented. (author) [fr

  11. X-ray fluorescence spectrometry and related techniques an introduction

    CERN Document Server

    Margui, Eva

    2013-01-01

    X-ray fluorescence spectrometry (XRF) is a well-established analytical technique for qualitative and quantitative elemental analysis of a wide variety of routine quality control and research samples. Among its many desirable features, it delivers true multi-element character analysis, acceptable speed and economy, easy of automation, and the capacity to analyze solid samples. This remarkable contribution to this field provides a comprehensive and up-to-date account of basic principles, recent developments, instrumentation, sample preparation procedures, and applications of XRF analysis. If you are a professional in materials science, analytic chemistry, or physics, you will benefit from not only the review of basics, but also the newly developed technologies with XRF. Those recent technological advances, including the design of low-power micro- focus tubes and novel X-ray optics and detectors, have made it possible to extend XRF to the analysis of low-Z elements and to obtain 2D or 3D information on a microme...

  12. Accelerator mass spectrometry-current status in techniques and applications

    International Nuclear Information System (INIS)

    Imamura, Mineo; Nagai, Hisao; Kobayashi, Koichi.

    1991-01-01

    Accelerator mass spectrometry (AMS) is the mass spectrometry by incorporating an accelerator. After samples are ionized, they are accelerated to a certain energy, and mass, energy, nuclear charge (atomic number) are distinguished, and ion counting is made one by one with a heavy ion detector. For the measurement of long half-life radioisotopes, mass spectrometry has been used because of the high sensitivity, but in low energy mass spectrometry, there are the difficulties due to the mixing of the molecular ions having nearly same mass and the existence of isobars. One of the methods solving these difficulties is an accelerator which enables background-free measurement. The progress of AMS is briefly described, and at present, it is carried out in about 30 facilities in the world. In AMS, the analysis is carried out in the order of the ionization of samples, the acceleration of beam, the electron stripping with a thin film, the sorting of the momentum and energy of beam and the identification of particles. The efficiency, sensitivity and accuracy of detection and the application are reported. (K.I.)

  13. Structural analyses of sucrose laurate regioisomers by mass spectrometry techniques

    DEFF Research Database (Denmark)

    Lie, Aleksander; Stensballe, Allan; Pedersen, Lars Haastrup

    2015-01-01

    6- And 6′-O-lauroyl sucrose were isolated and analyzed by matrix-assisted laser desorption/ionisation (MALDI) time-of-flight (TOF) mass spectrometry (MS), Orbitrap high-resolution (HR) MS, and electrospray-ionization (ESI) tandem mass spectrometry (MS/MS). The analyses aimed to explore the physic......6- And 6′-O-lauroyl sucrose were isolated and analyzed by matrix-assisted laser desorption/ionisation (MALDI) time-of-flight (TOF) mass spectrometry (MS), Orbitrap high-resolution (HR) MS, and electrospray-ionization (ESI) tandem mass spectrometry (MS/MS). The analyses aimed to explore.......8, respectively, and Orbitrap HRMS confirmed the mass of [M+Na]+ (m/z 547.2712). ESI-MS/MS on the precursor ion [M+Na]+ resulted in product ion mass spectra showing two high-intensity signals for each sample. 6-O-Lauroyl sucrose produced signals located at m/z 547.27 and m/z 385.21, corresponding to the 6-O...

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

    OpenAIRE

    2011-01-01

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

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

    International Nuclear Information System (INIS)

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

    2003-01-01

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

  16. Measurements of uranium enrichment by four techniques of gamma-ray spectrometry

    International Nuclear Information System (INIS)

    Tojo, Takao

    1983-12-01

    Measurements of uranium enrichment with the uses of the LMRI (France) UO 2 standards have been made by four techniques of gamma-ray spectrometry, in order to examine measurement characteristics of each technique. The following results were obtained by the three techniques based on the direct determination of the peak area of the 186-keV gamma-rays from 235 U, when the standard sample of 6.297 a/o was used for measuring enrichments ranging from 1.4 a/o to 9.6 a/o ; (i) In a LEPS HP Ge gamma-ray spectrometry, standard deviation of the measured enrichments from the certified ones was 1.4 %, (ii) in a Ge(Li) gamma-ray spectrometry, the standard deviation was 2.0 %, (iii) in a NaI(Tl) gamma-ray spectrometry, the standard deviation was 1.2 %. In the fourth technique, the method of multiple single-channel analyzers, enrichments of 1.4 - 9.6 a/o were measured in the standard deviation of 0.51 %, when the most suitable pairs of standard samples were used for each sample. A part of sources of systematic errors which were caused by each technique adopted was revealed throughout the measurements. And also, it was recognized that the LMRI's values of enrichment were certified precisely, and the UO 2 standards were very useful for enrichment measurements in the four techniques of gamma-ray spectrometry used here. (author)

  17. Multivariate techniques of analysis for ToF-E recoil spectrometry data

    Energy Technology Data Exchange (ETDEWEB)

    Whitlow, H J; Bouanani, M E; Persson, L; Hult, M; Jonsson, P; Johnston, P N [Lund Institute of Technology, Solvegatan, (Sweden), Department of Nuclear Physics; Andersson, M [Uppsala Univ. (Sweden). Dept. of Organic Chemistry; Ostling, M; Zaring, C [Royal institute of Technology, Electrum, Kista, (Sweden), Department of Electronics; Johnston, P N; Bubb, I F; Walker, B R; Stannard, W B [Royal Melbourne Inst. of Tech., VIC (Australia); Cohen, D D; Dytlewski, N [Australian Nuclear Science and Technology Organisation, Lucas Heights, NSW (Australia)

    1997-12-31

    Multivariate statistical methods are being developed by the Australian -Swedish Recoil Spectrometry Collaboration for quantitative analysis of the wealth of information in Time of Flight (ToF) and energy dispersive Recoil Spectrometry. An overview is presented of progress made in the use of multivariate techniques for energy calibration, separation of mass-overlapped signals and simulation of ToF-E data. 6 refs., 5 figs.

  18. Multivariate techniques of analysis for ToF-E recoil spectrometry data

    Energy Technology Data Exchange (ETDEWEB)

    Whitlow, H.J.; Bouanani, M.E.; Persson, L.; Hult, M.; Jonsson, P.; Johnston, P.N. [Lund Institute of Technology, Solvegatan, (Sweden), Department of Nuclear Physics; Andersson, M. [Uppsala Univ. (Sweden). Dept. of Organic Chemistry; Ostling, M.; Zaring, C. [Royal institute of Technology, Electrum, Kista, (Sweden), Department of Electronics; Johnston, P.N.; Bubb, I.F.; Walker, B.R.; Stannard, W.B. [Royal Melbourne Inst. of Tech., VIC (Australia); Cohen, D.D.; Dytlewski, N. [Australian Nuclear Science and Technology Organisation, Lucas Heights, NSW (Australia)

    1996-12-31

    Multivariate statistical methods are being developed by the Australian -Swedish Recoil Spectrometry Collaboration for quantitative analysis of the wealth of information in Time of Flight (ToF) and energy dispersive Recoil Spectrometry. An overview is presented of progress made in the use of multivariate techniques for energy calibration, separation of mass-overlapped signals and simulation of ToF-E data. 6 refs., 5 figs.

  19. Current medical research with the application of coupled techniques with mass spectrometry

    OpenAIRE

    Ka?u?na-Czapli?ska, Joanna

    2011-01-01

    Summary The most effective methods of analysis of organic compounds in biological fluids are coupled chromatographic techniques. Capillary gas chromatography/mass spectrometry (GC-MS) allows the most efficient separation, identification and quantification of volatile metabolites in biological fluids. Liquid chromatography-mass spectrometry (LC-MS) is especially suitable for the analysis of non-volatile and/or thermally unstable compounds. A major drawback of liquid chromatography-mass spectro...

  20. Isotope correlation and mass spectrometry techniques for irradiated fuel assay

    International Nuclear Information System (INIS)

    Deron, S.

    1985-01-01

    This paper outlines the methods used to account for fissionable materials in irradiated nuclear fuel elements entering reprocessing plants. Verification is accomplished at three mass balance stations in the plant. Techniques employed fall into two categories: isotopic and isotope dilution analyses by mass spectometry and isotope correlation techniques. These methods are discussed in some detail

  1. Theory and technique of spark source mass spectrometry; Theorie et technique de la spectrometrie de masse a etincelles

    Energy Technology Data Exchange (ETDEWEB)

    Stefani, R [Commissariat a l' Energie Atomique, Grenoble (France). Centre d' Etudes Nucleaires

    1968-07-01

    Trace analysis in solids by spark source mass spectrometry involves complicated phenomena: element ionization in spark and blacking of sensitive emulsion by focused ion beam. However the principal risk of selectivity lies in analyser system, which realizes double focusing only for a part of the ions. Therefore, each analyst has to known ionic optics of his apparatus, for ensuring the transmission of mean energetic ions, which are representative of sample composition. By a careful photometry of mass spectrum, good reproducibility can be obtained. Thereafter accuracy depends on the knowledge of sensitivity coefficients proper to this apparatus. (author) [French] L'analyse de traces dans les solides par spectrometrie de masse a etincelles met en jeu des phenomenes complexes qui sont l'ionisation des elements dans l'etincelle, et le noircissement de l'emulsion sensible par les faisceaux ioniques focalises. Cependant, le risque majeur de selectivite provient de l'ensemble analyseur, qui realise la double focalisation sur une fraction seulement du faisceau d'ions. L'analyste doit donc connaitre en detail l'optique ionique de son appareil, pour assurer le passage de la bande d'energie moyenne des ions, qui seule caracterise quantitativement la composition chimique de l'echantillon. Une exploitation photometrique soignee du spectrogramme donne alors des resultats reproductibles, dont la justesse ne depend plus que des coefficients de sensibilite propres a ce type d'instrument. (auteur)

  2. An introduction to the technique of combined ion mobility spectrometry-mass spectrometry for the analysis of complex biological samples

    International Nuclear Information System (INIS)

    McDowall, Mark A.; Bateman, Robert H.; Bajic, Steve; Giles, Kevin; Langridge, Jim; McKenna, Therese; Pringle, Steven D.; Wildgoose, Jason L.

    2008-01-01

    Full Text: Ultra Performance Liquid Chromatography (UPLC) offers several advantages compared with conventional High Performance Liquid Chromatography (HPLC) as an 'inlet system' for mass spectrometry. UPLC provides improved chromatographic resolution, increased sensitivity and reduced analysis time. This is achieved through the use of sub 2μm particles (stationary phase) combined with high-pressure solvent delivery (up to 15,000 psi). When coupled with orthogonal acceleration time-of-flight (oa-TOF) mass spectrometry (MS), UPLC presents a means to achieve high sample throughput with reduced spectral overlap, increased sensitivity, and exact mass measurement capabilities with high mass spectral resolution (Ca 20,000 FWHM). Dispersive ion mobility spectrometry (IMS) implemented within a traveling-wave ion guide provides an orthogonal separation strategy for ions in the gas phase that can resolve isobaric ions formed by either Electrospray of MALDI ionization typically in Ca 20 mille seconds. All three techniques have the potential to be combined on-line (e.g. UPLC-IMS-MS/MS) in real time to maximize peak capacity and resolving power for the analysis of complex biological mixtures including; intact proteins, modified peptides and endogenous/exogenous metabolites

  3. Analysis of [U-13C6]glucose in human plasma using liquid chromatography/isotope ratio mass spectrometry compared with two other mass spectrometry techniques

    NARCIS (Netherlands)

    Schierbeek, H.; Moerdijk-Poortvliet, T.C.W.; van den Akker, C.H.P.; te Braake, F.W.J.; Boschker, H.T.S.; van Goudoever, J.B.

    2009-01-01

    The use of stable isotope labelled glucose provides insight into glucose metabolism. The 13C-isotopic enrichment of glucose is usually measured by gas chromatography/mass spectrometry (GC/MS) or gas chromatography/combustion/isotope ratio mass spectrometry (GC/C/IRMS). However, in both techniques

  4. Mass determination of U-233 and Pu-239 by gamma spectrometry technique

    International Nuclear Information System (INIS)

    Moraes, M.A.P.V. de; Pugliesi, R.

    1988-09-01

    The gamma spectrometry technique has been used for masses determinations of uranium-233 and plutonium-239, granted by AERE-HARWELL. A high purity Ge semicondutor detector was used and the total efficiency curve was obtained for the counting system in the energy range 13 KeV to 135 KeV. The calculated values for the masses compared with that obtained by means of gravimetry technique. (author) [pt

  5. Mass spectrometry techniques in the survey of steroid metabolites as potential disease biomarkers: a review.

    Science.gov (United States)

    Gouveia, Maria João; Brindley, Paul J; Santos, Lúcio Lara; Correia da Costa, José Manuel; Gomes, Paula; Vale, Nuno

    2013-09-01

    Mass spectrometric approaches have been fundamental to the identification of metabolites associated with steroid hormones, yet this topic has not been reviewed in depth in recent years. To this end, and given the increasing relevance of liquid chromatography-mass spectrometry (LC-MS) studies on steroid hormones and their metabolites, the present review addresses this subject. This review provides a timely summary of the use of various mass spectrometry-based analytical techniques during the evaluation of steroidal biomarkers in a range of human disease settings. The sensitivity and specificity of these technologies are clearly providing valuable new insights into breast cancer and cardiovascular disease. We aim to contribute to an enhanced understanding of steroid metabolism and how it can be profiled by LC-MS techniques. Crown Copyright © 2013. Published by Elsevier Inc. All rights reserved.

  6. Surface-assisted laser desorption ionization mass spectrometry techniques for application in forensics.

    Science.gov (United States)

    Guinan, Taryn; Kirkbride, Paul; Pigou, Paul E; Ronci, Maurizio; Kobus, Hilton; Voelcker, Nicolas H

    2015-01-01

    Matrix-assisted laser desorption ionization (MALDI) mass spectrometry (MS) is an excellent analytical technique for the rapid and sensitive analysis of macromolecules (>700 Da), such as peptides, proteins, nucleic acids, and synthetic polymers. However, the detection of smaller organic molecules with masses below 700 Da using MALDI-MS is challenging due to the appearance of matrix adducts and matrix fragment peaks in the same spectral range. Recently, nanostructured substrates have been developed that facilitate matrix-free laser desorption ionization (LDI), contributing to an emerging analytical paradigm referred to as surface-assisted laser desorption ionization (SALDI) MS. Since SALDI enables the detection of small organic molecules, it is rapidly growing in popularity, including in the field of forensics. At the same time, SALDI also holds significant potential as a high throughput analytical tool in roadside, work place and athlete drug testing. In this review, we discuss recent advances in SALDI techniques such as desorption ionization on porous silicon (DIOS), nano-initiator mass spectrometry (NIMS) and nano assisted laser desorption ionization (NALDI™) and compare their strengths and weaknesses with particular focus on forensic applications. These include the detection of illicit drug molecules and their metabolites in biological matrices and small molecule detection from forensic samples including banknotes and fingerprints. Finally, the review highlights recent advances in mass spectrometry imaging (MSI) using SALDI techniques. © 2014 Wiley Periodicals, Inc.

  7. Evaluation of three gas chromatography and two direct mass spectrometry techniques for aroma analysis of dried red bell peppers

    NARCIS (Netherlands)

    Ruth, van S.M.; Boscaini, E.; Mayr, D.; Pugh, J.; Posthumus, M.A.

    2003-01-01

    Three gas chromatography methods and two direct mass spectrometry techniques were compared for the analysis of the aroma of rehydrated diced red bell peppers. Gas chromatography methods included systems with olfactometry detection (GC-O), flame ionisation detection (GC-FID) and mass spectrometry

  8. Comparison of the sensitivity of mass spectrometry atmospheric pressure ionization techniques in the analysis of porphyrinoids.

    Science.gov (United States)

    Swider, Paweł; Lewtak, Jan P; Gryko, Daniel T; Danikiewicz, Witold

    2013-10-01

    The porphyrinoids chemistry is greatly dependent on the data obtained in mass spectrometry. For this reason, it is essential to determine the range of applicability of mass spectrometry ionization methods. In this study, the sensitivity of three different atmospheric pressure ionization techniques, electrospray ionization, atmospheric pressure chemical ionization and atmospheric pressure photoionization, was tested for several porphyrinods and their metallocomplexes. Electrospray ionization method was shown to be the best ionization technique because of its high sensitivity for derivatives of cyanocobalamin, free-base corroles and porphyrins. In the case of metallocorroles and metalloporphyrins, atmospheric pressure photoionization with dopant proved to be the most sensitive ionization method. It was also shown that for relatively acidic compounds, particularly for corroles, the negative ion mode provides better sensitivity than the positive ion mode. The results supply a lot of relevant information on the methodology of porphyrinoids analysis carried out by mass spectrometry. The information can be useful in designing future MS or liquid chromatography-MS experiments. Copyright © 2013 John Wiley & Sons, Ltd.

  9. Review of in situ derivatization techniques for enhanced bioanalysis using liquid chromatography with mass spectrometry.

    Science.gov (United States)

    Baghdady, Yehia Z; Schug, Kevin A

    2016-01-01

    Accurate and specific analysis of target molecules in complex biological matrices remains a significant challenge, especially when ultra-trace detection limits are required. Liquid chromatography with mass spectrometry is often the method of choice for bioanalysis. Conventional sample preparation and clean-up methods prior to the analysis of biological fluids such as liquid-liquid extraction, solid-phase extraction, or protein precipitation are time-consuming, tedious, and can negatively affect target recovery and detection sensitivity. An alternative or complementary strategy is the use of an off-line or on-line in situ derivatization technique. In situ derivatization can be incorporated to directly derivatize target analytes in their native biological matrices, without any prior sample clean-up methods, to substitute or even enhance the extraction and preconcentration efficiency of these traditional sample preparation methods. Designed appropriately, it can reduce the number of sample preparation steps necessary prior to analysis. Moreover, in situ derivatization can be used to enhance the performance of the developed liquid chromatography with mass spectrometry-based bioanalysis methods regarding stability, chromatographic separation, selectivity, and ionization efficiency. This review presents an overview of the commonly used in situ derivatization techniques coupled to liquid chromatography with mass spectrometry-based bioanalysis to guide and to stimulate future research. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. In Situ Analytical Characterization of Contaminated Sites Using Nuclear Spectrometry Techniques. Review of Methodologies and Measurements

    International Nuclear Information System (INIS)

    2017-01-01

    Past and current human activities can result in the contamination of sites by radionuclides and heavy metals. The sources of contamination are various. The most important sources for radionuclide release include global fallout from nuclear testing, nuclear and radiological accidents, waste production from nuclear facilities, and activities involving naturally occurring radioactive material (NORM). Contamination of the environment by heavy metals mainly originates from industrial applications and mineralogical background concentration. Contamination of sites by radionuclides and heavy metals can present a risk to people and the environment. Therefore, the estimation of the contamination level and the identification of the source constitute important information for the national authorities with the responsibility to protect people and the environment from adverse health effects. In situ analytical techniques based on nuclear spectrometry are important tools for the characterization of contaminated sites. Much progress has been made in the design and implementation of portable systems for efficient and effective monitoring of radioactivity and heavy metals in the environment directly on-site. Accordingly, the IAEA organized a Technical Meeting to review the current status and trends of various applications of in situ nuclear spectrometry techniques for analytical characterization of contaminated sites and to support Member States in their national environmental monitoring programmes applying portable instrumentation. This publication represents a comprehensive review of the in situ gamma ray spectrometry and field portable X ray fluorescence analysis techniques for the characterization of contaminated sites. It includes papers on the use of these techniques, which provide useful background information for conducting similar studies, in the following Member States: Argentina, Australia, Brazil, Czech Republic, Egypt, France, Greece, Hungary, Italy, Lithuania

  11. Atmospheric pressure surface sampling/ionization techniques for direct coupling of planar separations with mass spectrometry.

    Science.gov (United States)

    Pasilis, Sofie P; Van Berkel, Gary J

    2010-06-18

    Planar separations, which include thin layer chromatography and gel electrophoresis, are in widespread use as important and powerful tools for conducting separations of complex mixtures. To increase the utility of planar separations, new methods are needed that allow in situ characterization of the individual components of the separated mixtures. A large number of atmospheric pressure surface sampling and ionization techniques for use with mass spectrometry have emerged in the past several years, and several have been investigated as a means for mass spectrometric read-out of planar separations. In this article, we review the atmospheric pressure surface sampling and ionization techniques that have been used for the read-out of planar separation media. For each technique, we briefly explain the operational basics and discuss the analyte type for which it is appropriate and some specific applications from the literature. Copyright (c) 2010 Elsevier B.V. All rights reserved.

  12. Study of different filtering techniques applied to spectra from airborne gamma spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Wilhelm, Emilien; Gutierrez, Sebastien; Reboli, Anne; Menard, Stephanie; Nourreddine, Abdel-Mjid [Commissariat a l' Energie Atomique et aux energies alternatives - CEA, DAM, DIF F-91297 Arpajon (France); Arbor, Nicolas [Institut Pluridisciplinaire Hubert Curien, UMR 7178 Universite de Strasbourg-CNRS, 23 rue du Loess, BP 28, F-67037 Strasbourg Cedex 2 (France)

    2015-07-01

    One of the features of spectra obtained by airborne gamma spectrometry is low counting statistics due to the short acquisition time (1 s) and the large source-detector distance (40 m). It leads to considerable uncertainty in radionuclide identification and determination of their respective activities from the windows method recommended by the IAEA, especially for low-level radioactivity. The present work compares the results obtained with filters in terms of errors of the filtered spectra with the window method and over the whole gamma energy range. The results are used to determine which filtering technique is the most suitable in combination with some method for total stripping of the spectrum. (authors)

  13. An analysis of nuclear fuel burnup in the AGR-1 TRISO fuel experiment using gamma spectrometry, mass spectrometry, and computational simulation techniques

    International Nuclear Information System (INIS)

    Harp, Jason M.; Demkowicz, Paul A.; Winston, Philip L.; Sterbentz, James W.

    2014-01-01

    Highlights: • The burnup of irradiated AGR-1 TRISO fuel was analyzed using gamma spectrometry. • The burnup of irradiated AGR-1 TRISO fuel was also analyzed using mass spectrometry. • Agreement between experimental results and neutron physics simulations was excellent. - Abstract: AGR-1 was the first in a series of experiments designed to test US TRISO fuel under high temperature gas-cooled reactor irradiation conditions. This experiment was irradiated in the Advanced Test Reactor (ATR) at Idaho National Laboratory (INL) and is currently undergoing post-irradiation examination (PIE) at INL and Oak Ridge National Laboratory. One component of the AGR-1 PIE is the experimental evaluation of the burnup of the fuel by two separate techniques. Gamma spectrometry was used to non-destructively evaluate the burnup of all 72 of the TRISO fuel compacts that comprised the AGR-1 experiment. Two methods for evaluating burnup by gamma spectrometry were developed, one based on the Cs-137 activity and the other based on the ratio of Cs-134 and Cs-137 activities. Burnup values determined from both methods compared well with the values predicted from simulations. The highest measured burnup was 20.1% FIMA (fissions per initial heavy metal atom) for the direct method and 20.0% FIMA for the ratio method (compared to 19.56% FIMA from simulations). An advantage of the ratio method is that the burnup of the cylindrical fuel compacts can be determined in small (2.5 mm) axial increments and an axial burnup profile can be produced. Destructive chemical analysis by inductively coupled mass spectrometry (ICP-MS) was then performed on selected compacts that were representative of the expected range of fuel burnups in the experiment to compare with the burnup values determined by gamma spectrometry. The compacts analyzed by mass spectrometry had a burnup range of 19.3% FIMA to 10.7% FIMA. The mass spectrometry evaluation of burnup for the four compacts agreed well with the gamma

  14. Laser desorption ionization mass spectrometry: Recent progress in matrix-free and label-assisted techniques.

    Science.gov (United States)

    Mandal, Arundhoti; Singha, Monisha; Addy, Partha Sarathi; Basak, Amit

    2017-10-13

    The MALDI-based mass spectrometry, over the last three decades, has become an important analytical tool. It is a gentle ionization technique, usually applicable to detect and characterize analytes with high molecular weights like proteins and other macromolecules. The earlier difficulty of detection of analytes with low molecular weights like small organic molecules and metal ion complexes with this technique arose due to the cluster of peaks in the low molecular weight region generated from the matrix. To detect such molecules and metal ion complexes, a four-prong strategy has been developed. These include use of alternate matrix materials, employment of new surface materials that require no matrix, use of metabolites that directly absorb the laser light, and the laser-absorbing label-assisted LDI-MS (popularly known as LALDI-MS). This review will highlight the developments with all these strategies with a special emphasis on LALDI-MS. © 2017 Wiley Periodicals, Inc.

  15. Determination of total uranium by mass spectrometry utilizing the isotopic dilution technique

    International Nuclear Information System (INIS)

    Cretella, R.F.; Noutary, C.J.; Servant, R.E.

    1981-01-01

    The isotopic dilution associated to mass spectrometry is a high-sensitivity technique that allows to work with microquantities of the sample, making it possible to analize the content in highly radioactive solutions with excellent accuracy and minimum risk. The proposed technique is described and its results are discussed through the analysis of: 1) A synthetic sample that simulates dissolved spent fuel elements; 2) Uranium dioxide of nuclear purity and 3) Uranium concentrate. 233 U(ORNL) was employed as a tracer and a Nuclide 12-90-SU mass spectrometer of simple magnetic focus as measurement instrument. The accuracy reached in the analyses is better than 0.5% with a reliability of 95%. The analysis of the errors shows that their main contributing source are the errors in the measurement of the isotopic ratios. (M.E.L.) [es

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2013-10-15

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

  17. Liquid separation techniques coupled with mass spectrometry for chiral analysis of pharmaceuticals compounds and their metabolites in biological fluids.

    Science.gov (United States)

    Erny, G L; Cifuentes, A

    2006-02-24

    Determination of the chiral composition of drugs is nowadays a key step in order to determine purity, activity, bioavailability, biodegradation, etc., of pharmaceuticals. In this article, works published for the last 5 years on the analysis of chiral drugs by liquid separation techniques coupled with mass spectrometry are reviewed. Namely, chiral analysis of pharmaceuticals including, e.g., antiinflammatories, antihypertensives, relaxants, etc., by liquid chromatography-mass spectrometry and capillary electrophoresis-mass spectrometry are included. The importance and interest of the analysis of the enantiomers of the active compound and its metabolites in different biological fluids (plasma, urine, cerebrospinal fluid, etc.) are also discussed.

  18. Liquid separation techniques coupled with mass spectrometry for chiral analysis of pharmaceuticals compounds and their metabolites in biological fluids.

    OpenAIRE

    Erny, Guillaume L.; Cifuentes, Alejandro

    2006-01-01

    Determination of the chiral composition of drugs is nowadays a key step in order to determine purity, activity, bioavailability, biodegradation, etc, of pharmaceuticals. In this manuscript, works published for the last 5 years on the analysis of chiral drugs by liquid separation techniques coupled with mass spectrometry are reviewed. Namely, chiral analysis of pharmaceuticals including e.g., antiinflammatories, antihypertensives, relaxants, etc, by liquid chromatography-mass spectrometry and ...

  19. Recent mass spectrometry-based techniques and considerations for disulfide bond characterization in proteins.

    Science.gov (United States)

    Lakbub, Jude C; Shipman, Joshua T; Desaire, Heather

    2018-04-01

    Disulfide bonds are important structural moieties of proteins: they ensure proper folding, provide stability, and ensure proper function. With the increasing use of proteins for biotherapeutics, particularly monoclonal antibodies, which are highly disulfide bonded, it is now important to confirm the correct disulfide bond connectivity and to verify the presence, or absence, of disulfide bond variants in the protein therapeutics. These studies help to ensure safety and efficacy. Hence, disulfide bonds are among the critical quality attributes of proteins that have to be monitored closely during the development of biotherapeutics. However, disulfide bond analysis is challenging because of the complexity of the biomolecules. Mass spectrometry (MS) has been the go-to analytical tool for the characterization of such complex biomolecules, and several methods have been reported to meet the challenging task of mapping disulfide bonds in proteins. In this review, we describe the relevant, recent MS-based techniques and provide important considerations needed for efficient disulfide bond analysis in proteins. The review focuses on methods for proper sample preparation, fragmentation techniques for disulfide bond analysis, recent disulfide bond mapping methods based on the fragmentation techniques, and automated algorithms designed for rapid analysis of disulfide bonds from liquid chromatography-MS/MS data. Researchers involved in method development for protein characterization can use the information herein to facilitate development of new MS-based methods for protein disulfide bond analysis. In addition, individuals characterizing biotherapeutics, especially by disulfide bond mapping in antibodies, can use this review to choose the best strategies for disulfide bond assignment of their biologic products. Graphical Abstract This review, describing characterization methods for disulfide bonds in proteins, focuses on three critical components: sample preparation, mass

  20. Evaluation of the natural radioactivity using thermoluminescence, gamma spectrometry and neutron activation techniques

    International Nuclear Information System (INIS)

    Fausto, A.M.; Otsubo, S.M.; Paes, W.S.; Yoshimura, E.M.; Okuno, E.; Hiodo, F.; Marques, L.S.; Alcala, A.L.

    1996-01-01

    The evaluation of the radiation dose in the living species due to the natural radioactivity is the main objective of this paper. The region that had been monitored was Intrusive Suite of Itu near to Sao Paulo city. Lateral[and depth distributions of natural radioactivity of the soil were determined using the techniques of thermoluminescence gamma spectrometry and neutron[activation. From the concentration in the soil of K-40 and radioactive elements of U and Th series experimentally determined, the dose due to gamma rays in air at 1 m from the soil was evaluated and the results compared with the direct dose measured with the portable rate-meter. (authors). 11 refs., 3 figs

  1. The Diagnosis of Plasma Parameters in Surface Alloying Technique by Optical Emission Spectrometry

    International Nuclear Information System (INIS)

    Fu Yabo; Zhang Yuefei; Chen Qiang; Zhang Guangqiu; Gao Yuan; Wang Jianzhong; Kui Xiaoyun

    2006-01-01

    Electron density (Ne) in a glow discharge plasma for the surface alloying technique is diagnosed by optical emission spectrometry (OES). With CH 4 as the feeding gas, Ne is obtained by comparing the Hβ spectrum according to the Stark broadening effect. It is noticed that Ne varies with the working pressures (30 Pa to 70 Pa) and cathode voltages (500 V to 1000 V), respectively. Due to an abnormal glow discharge, Ne is between 1.71x10 15 /cm 3 to 6.64x10 15 /cm 3 and increases rapidly with working gas pressures and cathode voltages. The results show that OES is a useful method to measure the plasma parameters in a surface alloying glow discharge plasma

  2. Metal oxide collectors for storing matter technique applied in secondary ion mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Miśnik, Maciej [Institute of Tele and Radio Technology, ul. Ratuszowa 11, 03-450 Warszawa (Poland); Gdańsk University of Technology (Poland); Konarski, Piotr [Institute of Tele and Radio Technology, ul. Ratuszowa 11, 03-450 Warszawa (Poland); Zawada, Aleksander [Institute of Tele and Radio Technology, ul. Ratuszowa 11, 03-450 Warszawa (Poland); Military University of Technology, Warszawa (Poland)

    2016-03-15

    We present results of the use of metal and metal oxide substrates that serve as collectors in ‘storing matter’, the quantitative technique of secondary ion mass spectrometry (SIMS). This technique allows separating the two base processes of secondary ion formation in SIMS. Namely, the process of ion sputtering is separated from the process of ionisation. The technique allows sputtering of the analysed sample and storing the sputtered material, with sub-monolayer coverage, onto a collector surface. Such deposits can be then analysed by SIMS, and as a result, the so called ‘matrix effects’ are significantly reduced. We perform deposition of the sputtered material onto Ti and Cu substrates and also onto metal oxide substrates as molybdenum, titanium, tin and indium oxides. The process of sputtering is carried within the same vacuum chamber where the SIMS analysis of the collected material is performed. For sputtering and SIMS analysis of the deposited material we use 5 keV Ar{sup +} beam of 500 nA. The presented results are obtained with the use of stationary collectors. Here we present a case study of chromium. The obtained results show that the molybdenum and titanium oxide substrates used as collectors increase useful yield by two orders, with respect to such pure elemental collectors as Cu and Ti. Here we define useful yield as a ratio of the number of detected secondary ions during SIMS analysis and the number of atoms sputtered during the deposition process.

  3. Recent development in mass spectrometry and its hyphenated techniques for the analysis of medicinal plants.

    Science.gov (United States)

    Zhu, Ming-Zhi; Chen, Gui-Lin; Wu, Jian-Lin; Li, Na; Liu, Zhong-Hua; Guo, Ming-Quan

    2018-04-23

    Medicinal plants are gaining increasing attention worldwide due to their empirical therapeutic efficacy and being a huge natural compound pool for new drug discovery and development. The efficacy, safety and quality of medicinal plants are the main concerns, which are highly dependent on the comprehensive analysis of chemical components in the medicinal plants. With the advances in mass spectrometry (MS) techniques, comprehensive analysis and fast identification of complex phytochemical components have become feasible, and may meet the needs, for the analysis of medicinal plants. Our aim is to provide an overview on the latest developments in MS and its hyphenated technique and their applications for the comprehensive analysis of medicinal plants. Application of various MS and its hyphenated techniques for the analysis of medicinal plants, including but not limited to one-dimensional chromatography, multiple-dimensional chromatography coupled to MS, ambient ionisation MS, and mass spectral database, have been reviewed and compared in this work. Recent advancs in MS and its hyphenated techniques have made MS one of the most powerful tools for the analysis of complex extracts from medicinal plants due to its excellent separation and identification ability, high sensitivity and resolution, and wide detection dynamic range. To achieve high-throughput or multi-dimensional analysis of medicinal plants, the state-of-the-art MS and its hyphenated techniques have played, and will continue to play a great role in being the major platform for their further research in order to obtain insight into both their empirical therapeutic efficacy and quality control. Copyright © 2018 John Wiley & Sons, Ltd.

  4. Atmospheric pressure chemical ionization studies of non-polar isomeric hydrocarbons using ion mobility spectrometry and mass spectrometry with different ionization techniques

    Science.gov (United States)

    Borsdorf, H.; Nazarov, E. G.; Eiceman, G. A.

    2002-01-01

    The ionization pathways were determined for sets of isomeric non-polar hydrocarbons (structural isomers, cis/trans isomers) using ion mobility spectrometry and mass spectrometry with different techniques of atmospheric pressure chemical ionization to assess the influence of structural features on ion formation. Depending on the structural features, different ions were observed using mass spectrometry. Unsaturated hydrocarbons formed mostly [M - 1]+ and [(M - 1)2H]+ ions while mainly [M - 3]+ and [(M - 3)H2O]+ ions were found for saturated cis/trans isomers using photoionization and 63Ni ionization. These ionization methods and corona discharge ionization were used for ion mobility measurements of these compounds. Different ions were detected for compounds with different structural features. 63Ni ionization and photoionization provide comparable ions for every set of isomers. The product ions formed can be clearly attributed to the structures identified. However, differences in relative abundance of product ions were found. Although corona discharge ionization permits the most sensitive detection of non-polar hydrocarbons, the spectra detected are complex and differ from those obtained with 63Ni ionization and photoionization. c. 2002 American Society for Mass Spectrometry.

  5. Software tool for resolution of inverse problems using artificial intelligence techniques: an application in neutron spectrometry

    International Nuclear Information System (INIS)

    Castaneda M, V. H.; Martinez B, M. R.; Solis S, L. O.; Castaneda M, R.; Leon P, A. A.; Hernandez P, C. F.; Espinoza G, J. G.; Ortiz R, J. M.; Vega C, H. R.; Mendez, R.; Gallego, E.; Sousa L, M. A.

    2016-10-01

    The Taguchi methodology has proved to be highly efficient to solve inverse problems, in which the values of some parameters of the model must be obtained from the observed data. There are intrinsic mathematical characteristics that make a problem known as inverse. Inverse problems appear in many branches of science, engineering and mathematics. To solve this type of problem, researches have used different techniques. Recently, the use of techniques based on Artificial Intelligence technology is being explored by researches. This paper presents the use of a software tool based on artificial neural networks of generalized regression in the solution of inverse problems with application in high energy physics, specifically in the solution of the problem of neutron spectrometry. To solve this problem we use a software tool developed in the Mat Lab programming environment, which employs a friendly user interface, intuitive and easy to use for the user. This computational tool solves the inverse problem involved in the reconstruction of the neutron spectrum based on measurements made with a Bonner spheres spectrometric system. Introducing this information, the neural network is able to reconstruct the neutron spectrum with high performance and generalization capability. The tool allows that the end user does not require great training or technical knowledge in development and/or use of software, so it facilitates the use of the program for the resolution of inverse problems that are in several areas of knowledge. The techniques of Artificial Intelligence present singular veracity to solve inverse problems, given the characteristics of artificial neural networks and their network topology, therefore, the tool developed has been very useful, since the results generated by the Artificial Neural Network require few time in comparison to other techniques and are correct results comparing them with the actual data of the experiment. (Author)

  6. Assessment of calibration parameters for an aerial gamma spectrometry system using Monte-Carlo technique

    International Nuclear Information System (INIS)

    Srinivasan, P.; Raman, Anand; Sharma, D.N.

    2009-01-01

    Aerial gamma spectrometry is a very effective method for quickly surveying a large area, which might get contaminated following a nuclear accident, or due to nuclear weapon fallout. The technique not only helps in identifying the contaminating radionuclide but also in assessing the magnitude and the extent of contamination. These two factors are of importance for the authorities to quickly plan and execute effective counter measures and controls if required. The development of Airborne gamma ray spectrometry systems have been reported by different institutions. The application of these systems have been reported by different authors. Radiation Safety Systems Division of the Bhabha Atomic Research Centre has developed an Aerial Gamma Spectrometry System (AGSS) and the surveying methodology. For an online assessment of the contamination levels, it is essential to calibrate the system (AGSS) either flying it over a known contaminated area or over a simulated contaminated surface by deploying sealed sources on the ground. AGSS has been calibrated for different detectors in aerial exercises using such simulated contamination on the ground. The calibration methodology essentially needs net photo-peak counts in selected energy windows to finally arrive at the Air to Ground Correlation Factors at selected flight parameters such as altitude, speed of flight and the time interval at which each spectrum is acquired. This paper describes the methodology to predict all the necessary parameters like photon fluence at various altitudes, the photo-peak counts in different energy windows, Air to Ground Correlation Factors(AGCF), the dose rate at any height due to air scattered gamma ray photons etc. These parameters are predicted for a given source deployment matrix, detector and altitude of flying using the Monte-Carlo code MCNP (Monte Carlo Neutron and Photon Transport Code.CCC-200, RSIC, ORNL, Tennessee, USA). A methodology to generate the completely folded gamma ray count

  7. Electron-capture negative-ion mass spectrometry: a technique for environmental contaminant identification

    International Nuclear Information System (INIS)

    Stemmler, E.A.

    1986-01-01

    Electron capture negative ion mass spectrometry (ECNIMS) is a method used to generate negative ions in a mass spectrometer by electron-molecule reactions. This technique facilitates the sensitive and selective detection of many toxic contaminants in environmental samples. Applications of this technique have been hindered by the limited understanding of instrumental parameters, by the questionable reproducibility of negative ion mass spectra, and by the inability to interpret negative ion mass spectra. Instrumental parameters which were important to control include the ion source temperature, ion source pressure, sample concentration, and the focus lens potential. The ability to obtain reproducible spectra was demonstrated by measurement of the spectrum of decafluorotriphenylphosphine (DFTPP) over a period of one year. Negative ion fragmentation mechanisms were studied by measuring the spectra of structurally related classes of compounds and isotopically labelled compounds. These results were combined with data obtained by other researchers. Fragmentations characteristic of particular functional groups or molecular structures have been summarized. From this data set, guidelines for the interpretation of electron capture negative ion mass spectra have been developed

  8. [Novel Hyphenated Techniques of Atomic Spectrometry for Metal Species Interaction with Biomolecules].

    Science.gov (United States)

    Li, Yan; Yan, Xiu-ping

    2015-09-01

    Trace metals may be adopted by biological systems to assist in the syntheses and metabolic functions of genes (DNA and RNA) and proteins in the environment. These metals may be beneficial or may pose a risk to humans and other life forms. Novel hybrid techniques are required for studies on the interaction between different metal species and biomolecules, which is significant for biology, biochemistry, nutrition, agriculture, medicine, pharmacy, and environmental science. In recent years, our group dwells on new hyphenated techniques based on capillary electrophoresis (CE), electrothermal atomic absorption spectrometry (ETAAS), and inductively coupled plasma mass spectroscopy (ICP-MS), and their application for different metal species interaction with biomolecules such as DNA, HSA, and GSH. The CE-ETAAS assay and CE-ICP-MS assay allow sensitively probing the level of biomolecules such as DNA damage by different metal species and extracting the kinetic and thermodynamic information on the interactions of different metal species with biomolecules, provides direct evidences for the formation of different metal species--biomolecule adducts. In addition, the consequent structural information were extracted from circular dichroism (CD) and X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, and Fourier transform infrared (FTIR) spectroscopy. The present works represent the most complete and extensive study to date on the interactions between different metal species with biomolecules, and also provide new evidences for and insights into the interactions of different metal species with biomolecules for further understanding of the toxicological effects of metal species.

  9. The alkali halide disk technique in infra-red spectrometry : Anomalous behaviour of some samples dispersed in alkali halide disks

    NARCIS (Netherlands)

    Tolk, A.

    1961-01-01

    Some difficulties encountered in the application of the alkali halide disk technique in infra-red spectrometry are discussed. Complications due to interaction of the sample with the alkali halide have been studied experimentally. It was found that the anomalous behaviour of benzoic acid, succinic

  10. Gamma-ray spectrometry combined with acceptable knowledge (GSAK). A technique for characterization of certain remote-handled transuranic (RH-TRU) wastes. Part 1. Methodology and techniques

    International Nuclear Information System (INIS)

    Hartwell, J.K.; McIlwain, M.E.

    2005-01-01

    Gamma-ray spectrometry combined with acceptable knowledge (GSAK) is a technique for the characterization of certain remote-handled transuranic (RH-TRU) wastes. GSAK uses gamma-ray spectrometry to quantify a portion of the fission product inventory of RH-TRU wastes. These fission product results are then coupled with calculated inventories derived from acceptable process knowledge to characterize the radionuclide content of the assayed wastes. GSAK has been evaluated and tested through several test exercises. GSAK approach is described, while test results are presented in Part II. (author)

  11. Burn-up measurements of spent fuel using gamma spectrometry technique

    International Nuclear Information System (INIS)

    Pereda, C.; Henriquez, C.; Klein, J.; Medel, J.

    2005-01-01

    Burn-up results obtained for HEU (45% of 235 U) fuel assemblies of the RECH-1 Research Reactor using gamma spectrometry technique are presented. The spectra were got from an in-pool facility built in the reactor to be mainly used to measure the burnup of irradiated fuel assemblies with short cooling time, where 95 Zr is being evaluated as possible fission monitor. A program to measure all spent fuel assemblies of the RECH-1 reactor was initiated in the frame of the Regional Project RLA/4/018: 'Management of Spent Fuel from Research Reactors'. The results presented here were obtained from HEU spent fuel assemblies with cooling time greater than 100 days and 137 Cs was used as fission monitor. The efficiency of the in-pool system was determined using a slightly burnt experimental fuel assembly, which has one fuel plate (one of the outer plates) and the rest are dummy plates. An average burn-up of 2.8% of 235 U was previously measured for the experimental fuel assembly utilizing a facility installed in a hot cell and 137 Cs was used as monitor. (author)

  12. Comparison of derivatization/ionization techniques for liquid chromatography tandem mass spectrometry analysis of oxylipins.

    Science.gov (United States)

    Meckelmann, Sven W; Hellhake, Stefan; Steuck, Maryvonne; Krohn, Michael; Schebb, Nils Helge

    2017-05-01

    The performance of two derivatization and ionization techniques for the quantitative reversed phase liquid chromatography (LC)- mass spectrometry (MS) analysis of hydroxy fatty acids (OH-PUFA) in plasma was evaluated: One used AMPP (N-(4-aminomethylphenyl)pyridinium chloride) leading to a positive charged amid-derivate which can be detected by electrospray ionization (ESI)-MS. Second yielded penta fluorobenzyl bromide (PFB) ester derivates allowing detection in electron capture atmospheric pressure chemical ionization (ecAPCI)-MS. The sensitivity of detection of a comprehensive set of hydroxy fatty acids of n6- and n3- poly unsaturated fatty acids was investigated. On the SCIEX3200 MS the applied PFB derivatization led to poor limits of detection (LOD) of 10-100nM (0.1-1pmol/0.03-0.3ng on column). By contrast, AMPP derivatization led to a similar sensitivity compared to the standard ESI(-) of non derivatized analytes (LOD about 1nM (10fmol/3pg on column)). For several analytes, including 9-HETE, 11-HETE and 17-HDHA the AMPP derivatization improved sensitivity enabling their detection in human plasma. However, precision was reduced by AMPP derivatization and variation in IS recovery indicated a strong matrix influence on the MS-signal. In sum, with the instrumentation used, neither of these derivatization methods improves in our hands the LC-MS based quantification of oxylipins. Copyright © 2017 Elsevier Inc. All rights reserved.

  13. Metabolomic Fingerprints of Individual Algal Cells Using the Single-Probe Mass Spectrometry Technique

    Directory of Open Access Journals (Sweden)

    Mei Sun

    2018-04-01

    Full Text Available Traditional approaches for the assessment of physiological responses of microbes in the environment rely on bulk filtration techniques that obscure differences among populations as well as among individual cells. Here, were report on the development on a novel micro-scale sampling device, referred to as the “Single-probe,” which allows direct extraction of metabolites from living, individual phytoplankton cells for mass spectrometry (MS analysis. The Single-probe is composed of dual-bore quartz tubing which is pulled using a laser pipette puller and fused to a silica capillary and a nano-ESI. For this study, we applied Single-probe MS technology to the marine dinoflagellate Scrippsiella trochoidea, assaying cells grown under different illumination levels and under nitrogen (N limiting conditions as a proof of concept for the technology. In both experiments, significant differences in the cellular metabolome of individual cells could readily be identified, though the vast majority of detected metabolites could not be assigned to KEGG pathways. Using the same approach, significant changes in cellular lipid complements were observed, with individual lipids being both up- and down-regulated under light vs. dark conditions. Conversely, lipid content increased across the board under N limitation, consistent with an adjustment of Redfield stoichiometry to reflect higher C:N and C:P ratios. Overall, these data suggest that the Single-probe MS technique has the potential to allow for near in situ metabolomic analysis of individual phytoplankton cells, opening the door to targeted analyses that minimize cell manipulation and sampling artifacts, while preserving metabolic variability at the cellular level.

  14. Determination of 36Cl/Cl ratio in ground water using the accelerator mass spectrometry technique

    International Nuclear Information System (INIS)

    Sharma, Suman; Deodhar, A.S.; Saravana Kumar, U.; Surendran, P.; Shrivastava, A.; Gupta, A.K.; Nair, J.P.; Yadav, M.L.; Hemalatha, M.; Sparrow, H.; Mahata, K.; Thomas, R.G.; Bhagwat, P.V.; Kailas, S.; Kale, R.M.

    2009-01-01

    The Accelerator Mass Spectrometry (AMS) programme using the 14 MV Pelletron Accelerator at Mumbai has been initiated with major emphasis on the determination of 36 Cl in water samples, of interest to hydrology and environment. In order to carry out the AMS measurement, a beam chopper to cut down beam intensity by a factor of 20 has been developed and commissioned. A multi-anode gas -si detector has been built to separate 36 Cl from the interfering 36 S. A new TPS system has been procured to operate the machine in the GVM mode. Standard and blank samples from Prime lab, Purdue have been employed in these measurements to standardise the technique for 36 Cl/Cl ratio determination. The detector was calibrated using the stable 35,37 Cl ions. The background 36 Cl in the system has been measured using the blank sample from Purdue and it was estimated that the ratio of 36 Cl/Cl was of the order of 10 -13 in the present setup. Ground water samples collected from South India were converted to AgCl and put in the SNICS ion source for the AMS measurements. These ground water samples, with 14 C content estimated to be in the range of 1 to 4 pMC indicate that the samples may be more than 35,000 years old. Using the AMS technique we have determined the 36 Cl/Cl ratio values for these ground water samples. They are found to range between 2 to 5 x 10 -12 . Additional measurements are planned to determine the age of the water samples and to understand the reasons for the observed high values of 36 Cl in these samples. (author)

  15. Emerging techniques in vegetable oil analysis using stable isotope ratio mass spectrometry

    Directory of Open Access Journals (Sweden)

    Rhodes, Christopher

    2002-03-01

    Full Text Available As the practice of vegetable oil adulteration becomes more sophisticated, the possibility to subvert detection using established techniques such as capillary gas chromatography is increasing. One of the most powerful techniques to be used in food authenticity studies is stable isotope ratio mass spectrometry (SIRMS which utilises differences in the natural abundance of the stable isotopes of the ‘light’ bio-elements hydrogen, nitrogen, carbon, oxygen and sulfur to detect food fraud. SIRMS has found application in the authentication of a wide range of foodstuffs, including fruit juices, wines, spirits, honey and to detect the adulteration of flavour compounds with synthetic analogues. This papers reviews the current state-of-the-art for the authentication of vegetable oils using SIRMS and highlights emergent techniques such as compound- and position specific-isotope mass spectrometry. These latter developments offer the potential to provide more rapid and improved detection of the economic adulteration of vegetable oils.A medida que la práctica de la adulteración de aceites vegetales se hace más sofisticada, las posibilidades de evitar la detección utilizando técnicas tradicionales como la cromatografía de gases en columna capilar aumentan. Una de las técnicas más poderosas que más se utilizan en los estudios de autentificación de alimentos es la espectrometría de masas de relaciones isotópicas, que utiliza diferencias en la abundancia natural de isótopos estables de elementos ligeros biológicos hidrógeno, nitrógeno, carbón, oxigeno y azufre para detectar fraude en los alimentos. La espectrometría de masas de relaciones isotópicas ha encontrado aplicación en la autentificación de una amplia gama de alimentos, incluyendo zumos de frutas, vinos, bebidas alcohólicas de alta graduación, miel, y en la detección de la adulteración de los compuestos aromáticos con sus análogos de origen sintético. Este trabajo

  16. Ionizing radiation effects in Acai oil analysed by gas chromatography coupled to mass spectrometry technique

    International Nuclear Information System (INIS)

    Valli, Felipe; Fernandes, Carlos Eduardo; Moura, Sergio; Machado, Ana Carolina; Furasawa, Helio Akira; Pires, Maria Aparecida Faustino; Bustillos, Oscar Vega

    2007-01-01

    The Acai fruit is a well know Brazilian seed plant used in large scale as a source of feed stock, specially in the Brazilian North-east region. The Acai oil is use in many purposes from fuel sources to medicine. The scope of this paper is to analyzed the chemical structures modification of the acai oil after the ionizing radiation. The radiation were set in the range of 10 to 25 kGy in the extracted Acai oil. The analyses were made by gas chromatography coupled to mass spectrometry techniques. A GC/MS Shimatzu QP-5000 equipped with 30 meters DB-5 capillary column with internal diameter of 0.25 mm and 0.25 μm film thickness was used. Helium was used as carried gas and gave a column head pressure of 12 p.s.i. (1 p.s.i. = 6894.76 Pa) and an average flux of 1 ml/min. The temperature program for the GC column consisted of a 4-minutes hold at 75 deg C, a 15 deg C /min ramp to 200 deg C, 8 minutes isothermal. 20 deg C/min ramp to 250 deg C, 2 minutes isothermal. The extraction of the fatty acids was based on liquid-liquid method using chloroform as solvent. The chromatograms resulted shows the presences of the oleic acid and others fatty acids identify by the mass spectra library (NIST-92). The ionization radiation deplete the fatty acids presents in the Acai oil. Details on the chemical qualitative analytical is present as well in this work. (author)

  17. Approaches for the analysis of low molecular weight compounds with laser desorption/ionization techniques and mass spectrometry.

    Science.gov (United States)

    Bergman, Nina; Shevchenko, Denys; Bergquist, Jonas

    2014-01-01

    This review summarizes various approaches for the analysis of low molecular weight (LMW) compounds by different laser desorption/ionization mass spectrometry techniques (LDI-MS). It is common to use an agent to assist the ionization, and small molecules are normally difficult to analyze by, e.g., matrix assisted laser desorption/ionization mass spectrometry (MALDI-MS) using the common matrices available today, because the latter are generally small organic compounds themselves. This often results in severe suppression of analyte peaks, or interference of the matrix and analyte signals in the low mass region. However, intrinsic properties of several LDI techniques such as high sensitivity, low sample consumption, high tolerance towards salts and solid particles, and rapid analysis have stimulated scientists to develop methods to circumvent matrix-related issues in the analysis of LMW molecules. Recent developments within this field as well as historical considerations and future prospects are presented in this review.

  18. Determination of Mercury in an Assortment of Dietary Supplements Using an Inexpensive Combustion Atomic Absorption Spectrometry Technique

    OpenAIRE

    Levine, Keith E.; Levine, Michael A.; Weber, Frank X.; Hu, Ye; Perlmutter, Jason; Grohse, Peter M.

    2005-01-01

    The concentrations of mercury in forty, commercially available dietary supplements, were determined using a new, inexpensive analysis technique. The method involves thermal decomposition, amalgamation, and detection of mercury by atomic absorption spectrometry with an analysis time of approximately six minutes per sample. The primary cost savings from this approach is that labor-intensive sample digestion is not required prior to analysis, further automating the analytical procedure. As a res...

  19. [Determination of acetanilide herbicide residues in tea by gas chromatography-mass spectrometry with two different ionization techniques].

    Science.gov (United States)

    Shen, Weijian; Xu, Jinzhong; Yang, Wenquan; Shen, Chongyu; Zhao, Zengyun; Ding, Tao; Wu, Bin

    2007-09-01

    An analytical method of solid phase extraction-gas chromatography-mass spectrometry with two different ionization techniques was established for simultaneous determination of 12 acetanilide herbicide residues in tea-leaves. Herbicides were extracted from tea-leaf samples with ethyl acetate. The extract was cleaned-up on an active carbon SPE column connected to a Florisil SPE column. Analytical screening was determined by the technique of gas chromatography (GC)-mass spectrometry (MS) in the selected ion monitoring (SIM) mode with either electron impact ionization (EI) or negative chemical ionization (NCI). It is reliable and stable that the recoveries of all herbicides were in the range from 50% to 110% at three spiked levels, 10 microg/kg, 20 microg/kg and 40 microg/kg, and the relative standard deviations (RSDs) were no more than 10.9%. The two different ionization techniques are complementary as more ion fragmentation information can be obtained from the EI mode while more molecular ion information from the NCI mode. By comparison of the two techniques, the selectivity of NCI-SIM was much better than that of EI-SIM method. The sensitivities of the both techniques were high, the limit of quantitative (LOQ) for each herbicide was no more than 2.0 microg/kg, and the limit of detection (LOD) with NCI-SIM technique was much lower than that of EI-SIM when analyzing herbicides with several halogen atoms in the molecule.

  20. Determination of Cu, Cr, and As in preserved wood (Eucalyptus sp.) using x-ray fluorescent spectrometry techniques

    International Nuclear Information System (INIS)

    Sergio Matias Pereira Junior; Vera Akiko Maihara; Edson Goncalves Moreira; Vera Lucia Ribeiro Salvador; Ivone Mulako Sato

    2016-01-01

    Energy dispersive (EDXRF) and Portable (PXRF) X-ray fluorescence techniques are proposed for wood treatment control process and wood waste assortment. In this study, different retentions of chromated copper arsenate preservative were applied to Eucalyptus sp. sapwood samples. Cu, Cr and As were determined by XRF techniques in treated sapwood massive blocks and treated sapwood sawdust samples were analyzed by FAAS spectrometry (Flame Atomic Absorption) and INAA (Instrumental Neutron Activation Analysis). Cu, Cr and As mean values, obtained by FAASS and INAA, showed to be statically equal; however, XRF analysis showed considerable deviations, presenting the absorption and the enhancement effects in analytical lines. (author)

  1. Mercury in Environmental and Biological Samples Using Online Combustion with Sequential Atomic Absorption and Fluorescence Measurements: A Direct Comparison of Two Fundamental Techniques in Spectrometry

    Science.gov (United States)

    Cizdziel, James V.

    2011-01-01

    In this laboratory experiment, students quantitatively determine the concentration of an element (mercury) in an environmental or biological sample while comparing and contrasting the fundamental techniques of atomic absorption spectrometry (AAS) and atomic fluorescence spectrometry (AFS). A mercury analyzer based on sample combustion,…

  2. Characterization of the occupational exposure and air transported particles using the techniques of PIXE 252Cf PMDS and alpha spectrometry

    International Nuclear Information System (INIS)

    Carneiro, Luana Gomes

    2008-01-01

    The risk for human health due to exposure to aerosols depends on the intake pattern, the mass concentration and the speciation of the elements present in airborne particles. In this work PDMS (Plasma Desorption Mass Spectrometry) was used as complementary technique to the PIXE (Particle Induced X ray Emission) technique to characterize aerosols samples collected in the environment. The PIXE technique allows the identification of the elements present in the sample and to determine their mass concentrations. The mass spectrometry (PDMS) was used to identify the speciation of these elements present in the samples. The aerosol samples were collected using a six stage cascade impactor in three sites. The Mass Median Aerodynamic Diameter (MMAD) measured indicated that the airborne particulate were in the fine fraction of the aerosols. The theoretical uranium concentration in urine samples using ICRP lung model parameters suggest that the elemental mass concentration in respirable fraction of aerosol and the chemical speciation are important factors to determine the uranium concentration in urine and that the determination of specific solubility parameters for each compound is the most important factor to calculate the uranium concentration in urine. PIXE allows to identify and quantify the elements heavier than Na (Z=11) while PDMS allows to identify the organic and inorganic compounds present in the samples. As these techniques are used as complementary techniques they provide important information about the aerosols characterization. (author)

  3. Introduction to Body Composition Assessment Using the Deuterium Dilution Technique with Analysis of Urine Samples by Isotope Ratio Mass Spectrometry

    International Nuclear Information System (INIS)

    2010-01-01

    The IAEA has fostered the more widespread use of a stable isotope technique to assess body composition in different population groups to address priority areas in public health nutrition in Member States. It has done this by supporting national and regional nutrition projects through its technical cooperation programme and coordinated research projects over many years. This publication was developed by an international group of experts to provide practical hands-on guidance in the use of this technique in settings where analysis of stable isotope ratios in biological samples is to be made by isotope ratio mass spectrometry. The publication is targeted at new users of this technique, for example nutritionists, analytical chemists and other professionals. More detailed information on the theoretical background and the practical applications of state of the art methodologies to monitor changes in body composition can be found in IAEA Human Health Series No. 3, Assessment of Body Composition and Total Energy Expenditure in Humans by Stable Isotope Techniques

  4. Electrospray ionization mass spectrometry: a technique to access the information beyond the molecular weight of the analyte.

    Science.gov (United States)

    Banerjee, Shibdas; Mazumdar, Shyamalava

    2012-01-01

    The Electrospray Ionization (ESI) is a soft ionization technique extensively used for production of gas phase ions (without fragmentation) of thermally labile large supramolecules. In the present review we have described the development of Electrospray Ionization mass spectrometry (ESI-MS) during the last 25 years in the study of various properties of different types of biological molecules. There have been extensive studies on the mechanism of formation of charged gaseous species by the ESI. Several groups have investigated the origin and implications of the multiple charge states of proteins observed in the ESI-mass spectra of the proteins. The charged analytes produced by ESI can be fragmented by activating them in the gas-phase, and thus tandem mass spectrometry has been developed, which provides very important insights on the structural properties of the molecule. The review will highlight recent developments and emerging directions in this fascinating area of research.

  5. Electrospray Ionization Mass Spectrometry: A Technique to Access the Information beyond the Molecular Weight of the Analyte

    Science.gov (United States)

    Banerjee, Shibdas; Mazumdar, Shyamalava

    2012-01-01

    The Electrospray Ionization (ESI) is a soft ionization technique extensively used for production of gas phase ions (without fragmentation) of thermally labile large supramolecules. In the present review we have described the development of Electrospray Ionization mass spectrometry (ESI-MS) during the last 25 years in the study of various properties of different types of biological molecules. There have been extensive studies on the mechanism of formation of charged gaseous species by the ESI. Several groups have investigated the origin and implications of the multiple charge states of proteins observed in the ESI-mass spectra of the proteins. The charged analytes produced by ESI can be fragmented by activating them in the gas-phase, and thus tandem mass spectrometry has been developed, which provides very important insights on the structural properties of the molecule. The review will highlight recent developments and emerging directions in this fascinating area of research. PMID:22611397

  6. New technique for determination of long-lived radioisotopes, Iodine-129, using multiparameter coincidence spectrometry

    International Nuclear Information System (INIS)

    Hatsukawa, Yuichi; Oshima, Masumi; Toh, Yosuke; Shinohara, Nobuo; Kushita, Kosuke; Ueno, Takashi

    2003-01-01

    Multiparameter coincidence γ-ray spectrometry based on g-g coincidence is widely used in the field of nuclear structure studies, and has produced many successful results. In this study, feasibility of the method for neutron activation analysis of long lived iodine isotope, 129 I, was investigated. (author)

  7. Heterogeneous chemical kinetics by modulated molecular beam mass spectrometry: limitations of technique

    International Nuclear Information System (INIS)

    Olander, D.R.

    1977-01-01

    The advantages and limitations of modulated molecular beam, mass spectrometry as applied to the study of heterogeneous chemical kinetics are reviewed. The process of deducing a model of the surface reaction from experimental data is illustrated by analysis of the hydrogen reduction of uranium dioxide

  8. Column liquid chromatography- mass spectrometry: selected techniques in environmental applications for polar pesticides and related compounds.

    NARCIS (Netherlands)

    Slobodnik, J.; van Baar, B.L.M.; Brinkman, U.A.T.

    1995-01-01

    A review covering the field of environmental applications of liquid chromatography-mass spectrometry (LC-MS) is presented. Recent developments and advances are discussed with emphasis on the presently popular thermospray, particle beam and atmospheric pressure ionisation interfaces. Each interface

  9. Spectroscopic techniques (Moessbauer spectrometry, NMR, ESR...) as tools to resolve doubtful NMR images: Study of the craniopharyngioma tumor

    International Nuclear Information System (INIS)

    Rimbert, J.N.; Dumas, F.; Lafargue, C.; Kellershohn, C.; Brunelle, F.; Lallemand, D.

    1990-01-01

    Craniopharyngioma, an intracranial tumor, exhibits hyperintensity in the Spin-Echo-T 2 -NMR image and a hyposignal in the SE-T 1 -image. However, in some cases (15-20% cases), hypersignals are seen in both SE-T 1 and T 2 -MRI. Using spectroscopic techniques, Moessbauer spectrometry in particular, we have demonstrated that the T 1 hypersignal is due to ferritin, dissolved in the cystic liquid, after tumor cell lysis, in the course of time. Other possible reasons inducing a shortening of the T 1 relaxation time (presence of lipids, intratumoral hemorrhage) have been rejected. (orig.)

  10. Cometary and interstellar dust grains - Analysis by ion microprobe mass spectrometry and other techniques

    Science.gov (United States)

    Zinner, Ernst

    1991-01-01

    A survey of microanalytical measurements on interplanetary dust particles (IDPs) and interstellar dust grains from primitive meteorites is presented. Ion-microprobe mass spectrometry with its capability to determine isotopic compositions of many elements on a micron spatial scale has played a special role. Examples are measurements of H, N, and O isotopes and refractory trace elements in IDPs; C, N, Mg, and Si isotopes in interstellar SiC grains; and C and N isotopes and H, N, Al, and Si concentrations in interstellar graphite grains.

  11. Use of the electrodeposition technique in the preparation of samples of 237Np and its determination by alpha spectrometry

    International Nuclear Information System (INIS)

    Mertzig, W.; Matsuda, H.T.; Araujo, B.F. de; Araujo, J.A. de.

    1981-05-01

    The electroplating technique to prepare 237 Np source and its determination by alpha spectrometry is presented. The samples were prepared using a lucite-eletrolitic cell manufactured at IPEN, specially to trace amounts of actinides. A polished brass disk coated with Ni film has been used as cathodo and a fixed Pt wire as anode. The electroplated samples were alpha counted using a surface barrier detector. The optimum conditions to obtain the quantitative deposition of 237 Np have been achieved by studying the effects of some parameters as current density, pH and concentration of eletrolitic solution and time of eletrodeposition, using a carrier technique. After preliminary purification, the method is applied to control trace amounts of 237 Np in the Purex process solutions. (Author) [pt

  12. Trace uranium analysis in geological sample by isotope dilution-alpha spectrometry and comparison with other techniques

    International Nuclear Information System (INIS)

    Shihomatsu, H.M.; Iyer, S.S.

    1988-12-01

    Establishment of uranium determination in geological samples by alpha spectrometric isotope dilution technique using 233 U tracer is described in the present work. The various steps involved in the method namely, preparation of the sample, electrodeposition, alpha spectrometry, isotope dilution, calculation of the concentration and error statistics are discussed in detail. The experimental parameters for the electrodeposition of uranium, like current density, pH concentration of the electrolyte solution, deposition time, electrode distance were all optimised based on the efficiency of the deposition. The total accuracy and precision of the IDAS using 233 U tracer in the determination of uranium in mineral and granite samples were of the order of 1 to 2% for the concentration range of 50-1500 ppm of U. Our results are compared with those obtained by others workers using similar and different techniques. (author) [pt

  13. Making Mass Spectrometry See the Light: The Promises and Challenges of Cryogenic Infrared Ion Spectroscopy as a Bioanalytical Technique.

    Science.gov (United States)

    Cismesia, Adam P; Bailey, Laura S; Bell, Matthew R; Tesler, Larry F; Polfer, Nicolas C

    2016-05-01

    The detailed chemical information contained in the vibrational spectrum of a cryogenically cooled analyte ion would, in principle, make infrared (IR) ion spectroscopy a gold standard technique for molecular identification in mass spectrometry. Despite this immense potential, there are considerable challenges in both instrumentation and methodology to overcome before the technique is analytically useful. Here, we discuss the promise of IR ion spectroscopy for small molecule analysis in the context of metabolite identification. Experimental strategies to address sensitivity constraints, poor overall duty cycle, and speed of the experiment are intimately tied to the development of a mass-selective cryogenic trap. Therefore, the most likely avenues for success, in the authors' opinion, are presented here, alongside alternative approaches and some thoughts on data interpretation.

  14. Introduction to body composition assessment using the deuterium dilution technique with analysis of saliva samples by fourier transform infrared spectrometry

    International Nuclear Information System (INIS)

    2010-01-01

    For many years, the IAEA has fostered the more widespread use of stable isotope techniques to assess body composition in different population groups to address priority areas in public health nutrition in Member States. The objective is to support national and regional nutrition projects through both the IAEA's technical cooperation programme and its coordinated research projects. In particular, during the last few years, the increased access to analyses of deuterium enrichment by Fourier transform infrared (FTIR) spectrometry has increased the application of this technique in Africa, Asia and Latin America. This publication was developed by an international group of experts to provide practical, hands-on guidance in the use of this technique in settings where the analysis of deuterium enrichment in saliva samples will be made by FTIR. It is targeted at new users of this technique, for example nutritionists, analytical chemists and other professionals. More detailed information on the theoretical background and the practical application of state of the art methodologies to monitor changes in body composition can be found in an IAEA publication entitled Assessment of Body Composition and Total Energy Expenditure in Humans by Stable Isotope Techniques (IAEA Human Health Series No. 3)

  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. Improved detection limit for {sup 59}Ni using the technique of accelerator mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Persson, Per; Erlandsson, Bengt; Hellborg, Ragnar; Kiisk, Madis; Larsson, Ragnar; Skog, Goeran; Stenstroem, Kristina [Lund Univ. (Sweden). Dept. of Nuclear Physics

    2002-11-01

    59 Ni is produced by neutron activation in the stainless steel close to the core of a nuclear reactor. To be able to classify the different parts of the reactor with respect to their content of long-lived radionuclides before final storage it is important to measure the 59 Ni level. Accelerator mass spectrometry is an ultra-sensitive method for counting atoms, suitable for 59 Ni measurements. Improvements in the reduction of the background and in the chemical reduction of cobalt, the interfering isobar, have been made. This chemical purification is essential when using small tandem accelerators, <3 MV, combined with the detection of characteristic projectile X-rays. These improvements have lowered the detection limit for 59 Ni by a factor of twenty compared with the first value reported for the Lund AMS facility. Material from the Swedish nuclear industry has been analysed and examples of the results are presented.

  17. The Application of Resonance-Enhanced Multiphoton Ionization Technique in Gas Chromatography Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Adan Li

    2014-01-01

    Full Text Available Gas chromatography resonance-enhanced multiphoton ionization time-of-flight mass spectrometry (GC/REMPI-TOFMS using a nanosecond laser has been applied to analyze the 16 polycyclic aromatic hydrocarbons (PAHs. The excited-state lifetime, absorption characters, and energy of electronic states of the 16 PAHs were investigated to optimize the ionization yield. A river water sample pretreated by means of solid phase extraction was analyzed to evaluate the performance of the analytical instrument. The results suggested that REMPI is superior to electron impact ionization method for soft ionization and suppresses the background signal due to aliphatic hydrocarbons. Thus, GC/REMPI-TOFMS is a more reliable method for the determination of PAHs present in the environment.

  18. Thermogravimetry/mass spectrometry study of woody residues and an herbaceous biomass crop using PCA techniques

    Energy Technology Data Exchange (ETDEWEB)

    Gomez, C.J.; Velo, E.; Puigjaner, L. [Department of Chemical Engineering, ETSEIB, Universitat Politecnica de Catalunya, Avinguda Diagonal 647, G2, E-08028 Barcelona (Spain); Meszaros, E.; Jakab, E. [Institute of Materials and Environmental Chemistry, Chemical Research Center, Hungarian Academy of Sciences, P.O. Box 17, Budapest 1525 (Hungary)

    2007-10-15

    The devolatilization behaviour of pine and beech wood from carpentry residuals and an herbaceous product from an energy plantation (artichoke thistle) was investigated by thermogravimetry/mass spectrometry (TG/MS). The effect of three pre-treatments, hot-water washing, ethanol extraction and their combination, was also studied. Principal component analysis (PCA) was employed to help in the evaluation of the large data set of results. The characteristics of the thermal decomposition of the herbaceous crop are considerably different from that of the woody biomass samples. The evolution profiles of some characteristic pyrolysis products revealed that the thermal behaviour of wood and thistle is still considerably different after the elimination of some of the inorganic ions and extractive compounds, although the macromolecular components of the samples decompose at similar temperatures. With the help of the PCA calculations, the effect of the different pre-treatments on the production of the main pyrolysis products was evidenced. (author)

  19. Stable Isotope Quantitative N-Glycan Analysis by Liquid Separation Techniques and Mass Spectrometry.

    Science.gov (United States)

    Mittermayr, Stefan; Albrecht, Simone; Váradi, Csaba; Millán-Martín, Silvia; Bones, Jonathan

    2017-01-01

    Liquid phase separation analysis and subsequent quantitation remains a challenging task for protein-derived oligosaccharides due to their inherent structural complexity and diversity. Incomplete resolution or co-detection of multiple glycan species complicates peak area-based quantitation and associated statistical analysis when optical detection methods are used. The approach outlined herein describes the utilization of stable isotope variants of commonly used fluorescent tags that allow for mass-based glycan identification and relative quantitation following separation by liquid chromatography (LC) or capillary electrophoresis (CE). Comparability assessment of glycoprotein-derived oligosaccharides is performed by derivatization with commercially available isotope variants of 2-aminobenzoic acid or aniline and analysis by LC- and CE-mass spectrometry. Quantitative information is attained from the extracted ion chromatogram/electropherogram ratios generated from the light and heavy isotope clusters.

  20. The application of computer technique in routine neutron activation analysis using high resolution gamma ray spectrometry

    International Nuclear Information System (INIS)

    Szopa, Z.; Plejewska, M.; Staszelis, J.

    1982-01-01

    A full system of four computer programs for routine - qualitative and quantitative - neutron activation analysis (NAA) using high resolution gamma ray-spectrometry had been elaborated. The structure and possibilities of the ''data flow'' programs i.e. programs DIDPDP and DIDCDC, dedicated for fast and reliable ''off line'' data transfer between the buffer memory of the spectrometric line (9-track magnetic tape) and the fast access memory (disc) of the used computers PDP-11/45 and CYBER-73 had been presented. The structure and organization of the ''data processing'' programs i.e. programs SAWAPS and MAZYG had been presented as well. The utility and reliability of these programs in the case of the large-scale, routine NAA, exampled by analysis of filters with air polutants, had been tested and discussed. Programs are written mainly in FORTRAN. (author)

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

    Science.gov (United States)

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

    2009-10-30

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

  2. Element selective detection of molecular species applying chromatographic techniques and diode laser atomic absorption spectrometry.

    Science.gov (United States)

    Kunze, K; Zybin, A; Koch, J; Franzke, J; Miclea, M; Niemax, K

    2004-12-01

    Tunable diode laser atomic absorption spectroscopy (DLAAS) combined with separation techniques and atomization in plasmas and flames is presented as a powerful method for analysis of molecular species. The analytical figures of merit of the technique are demonstrated by the measurement of Cr(VI) and Mn compounds, as well as molecular species including halogen atoms, hydrogen, carbon and sulfur.

  3. Study of a new glass matrix by the thermoluminescence technique; Estudo de uma nova matriz vitrea pela tecnica de termoluminescencia

    Energy Technology Data Exchange (ETDEWEB)

    Ferreira, Pamela Z.; Vedovato, Uly P.; Cunha, Diego M. da; Dantas, Noelio O.; Silva, Anielle C.A.; Neves, Lucio P.; Perini, Ana P., E-mail: anapaula.perini@ufu.br [Universidade Federal de Uberlandia (INFIS/UFU), MG (Brazil). Instituto de Fisica; Caldas, Linda V.E. [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil); Carrera, Betzabel N.S.; Watanabe, Shigueo [Universidade de Sao Paulo (IF/USP), Sao Paulo, SP (Brazil). Instituto de Fisica

    2015-07-01

    The thermoluminescence technique is widely used for both personal and for high-dose dosimetry. In this work, the thermoluminescence technique was utilized to study a new glass matrix, with nominal composition of 20Li{sub 2}CO{sub 3}.10Al{sub 2}O{sub 3}.20BaO.50B{sub 2}O{sub 3} (mol%), irradiated with different doses in a {sup 60}Co source. The glow curves and the dose-response curve were obtained for radiation doses between 50 Gy and 900 Gy. The results showed that this new glass matrix presents potential use in high-dose dosimetry. (author)

  4. Ionization techniques in capillary electrophoresis-mass spectrometry: principles, design, and application.

    Science.gov (United States)

    Hommerson, Paul; Khan, Amjad M; de Jong, Gerhardus J; Somsen, Govert W

    2011-01-01

    A major step forward in the development and application of capillary electrophoresis (CE) was its coupling to ESI-MS, first reported in 1987. More than two decades later, ESI has remained the principal ionization technique in CE-MS, but a number of other ionization techniques have also been implemented. In this review the state-of-the-art in the employment of soft ionization techniques for CE-MS is presented. First the fundamentals and general challenges of hyphenating conventional CE and microchip electrophoresis with MS are outlined. After elaborating on the characteristics and role of ESI, emphasis is put on alternative ionization techniques including sonic spray ionization (SSI), thermospray ionization (TSI), atmospheric pressure chemical ionization (APCI), atmospheric pressure photoionization (APPI), matrix-assisted laser desorption ionization (MALDI) and continuous-flow fast atom bombardment (CF-FAB). The principle of each ionization technique is outlined and the experimental set-ups of the CE-MS couplings are described. The strengths and limitations of each ionization technique with respect to CE-MS are discussed and the applicability of the various systems is illustrated by a number of typical examples. Copyright © 2011 Wiley Periodicals, Inc.

  5. Application of data mining and artificial intelligence techniques to mass spectrometry data for knowledge discovery

    Directory of Open Access Journals (Sweden)

    Hugo López-Fernández

    2016-05-01

    Full Text Available Mass spectrometry using matrix assisted laser desorption ionization coupled to time of flight analyzers (MALDI-TOF MS has become popular during the last decade due to its high speed, sensitivity and robustness for detecting proteins and peptides. This allows quickly analyzing large sets of samples are in one single batch and doing high-throughput proteomics. In this scenario, bioinformatics methods and computational tools play a key role in MALDI-TOF data analysis, as they are able handle the large amounts of raw data generated in order to extract new knowledge and useful conclusions. A typical MALDI-TOF MS data analysis workflow has three main stages: data acquisition, preprocessing and analysis. Although the most popular use of this technology is to identify proteins through their peptides, analyses that make use of artificial intelligence (AI, machine learning (ML, and statistical methods can be also carried out in order to perform biomarker discovery, automatic diagnosis, and knowledge discovery. In this research work, this workflow is deeply explored and new solutions based on the application of AI, ML, and statistical methods are proposed. In addition, an integrated software platform that supports the full MALDI-TOF MS data analysis workflow that facilitate the work of proteomics researchers without advanced bioinformatics skills has been developed and released to the scientific community.

  6. Development of realtime monitoring technology for laser photoreaction product - Development of glow discharge-mass spectrometry (GD-MS) hybrid techniques for trace analysis of refractory elements

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Sang Chun [Kyungnam University, Masan (Korea); Kim, Ha Suck [Seoul National University, Seoul (Korea); Kim, Hyo Jin [Dongduk Women' s University, Seoul (Korea)

    2000-04-01

    This research is focusing on development of hybrid techniques of glow discharge-mass spectrometry for the trace analysis of refractory elements. At first, we developed a glow discharge(GD) ionization cell and its characteristics was investigated. The new GD cell was designed based on direct current hollow cathode glow discharge and it is used for quadrupole mass analyzer and time-of-flight mass analyzer. Currently, GD-quadrupole mass spectrometry is working for the analysis of refractory elements. The experimental results show relatively good for trace analysis. In addition, ion mobile spectrometry using plasma and liquid discharge technique were investigated for the analysis of refractory elements and both techniques need more investigation to deduce the their usefulness. 30 refs., 67 figs., 4 tabs. (Author)

  7. Fecal Metabolomics of Type 2 Diabetic Rats and Treatment with Gardenia jasminoides Ellis Based on Mass Spectrometry Technique.

    Science.gov (United States)

    Zhou, Yuan; Men, Lihui; Pi, Zifeng; Wei, Mengying; Song, Fengrui; Zhao, Chunfang; Liu, Zhiqiang

    2018-02-14

    Modern studies have indicated Gardenia jasminoides Ellis (G. jasminoides) showed positive effect in treating type 2 diabetes mellitus (T2DM). In this study, 60 streptozotocin-induced T2DM rats were divided into four groups: type 2 diabetes control group, geniposide-treated group, total iridoid glycosides-treated group, and crude extraction of gardenlae fructus-treated group. The other ten healthy rats were the healthy control group. During 12 weeks of treatment, rat's feces samples were collected for the metabolomics study based on mass spectrometry technique. On the basis of the fecal metabolomics method, 19 potential biomarkers were screened and their relative intensities in each group were compared. The results revealed G. jasminoides mainly regulated dysfunctions in phenylalanine metabolism, tryptophan metabolism, and secondary bile acid biosynthesis pathways induced by diabetes. The current study provides new insight for metabonomics methodology toward T2DM, and the results show that feces can preferably reflect the liver and intestines disorders.

  8. Experimental study of laser ablation as sample introduction technique for inductively coupled plasma-mass spectrometry

    International Nuclear Information System (INIS)

    Van Winckel, S.

    2001-01-01

    The contribution consists of an abstract of a PhD thesis. In the PhD study, several complementary applications of laser-ablation were investigated in order to characterise experimentally laser ablation (LA) as a sample introduction technique for ICP-MS. Three applications of LA as a sample introduction technique are discussed: (1) the microchemical analysis of the patina of weathered marble; (2) the possibility to measure isotope ratios (in particular Pb isotope ratios in archaeological bronze artefacts); and (3) the determination of Si in Al as part of a dosimetric study of the BR2 reactor vessel

  9. 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)

  10. Gamma-ray spectrometry combined with acceptable knowledge (GSAK). A technique for characterization of certain remote-handled transuranic (RH-TRU) wastes. Part 2. Testing and results

    International Nuclear Information System (INIS)

    Hartwell, J.K.; McIlwain, M.E.

    2005-01-01

    Gamma-ray spectrometry combined with acceptable knowledge (GSAK) is a technique for the characterization of certain remote-handled transuranic (RH-TRU) wastes. GSAK uses gamma-ray spectrometry to quantify a portion of the fission product inventory of RH-TRU wastes. These fission product results are then coupled with calculated inventories derived from acceptable process knowledge to characterize the radionuclide content of the assayed wastes. GSAK has been evaluated and tested through several test exercises. These tests and their results are described; while the former paper in this issue presents the methodology, equipment and techniques. (author)

  11. Laser diagnodent: a comparative study with other diagnostic techniques; Laser diagnodent: estudo comparativo com outras tecnicas de diagnostico

    Energy Technology Data Exchange (ETDEWEB)

    Godinho, Reugma Rego

    2002-07-01

    An evaluation of the Diagnodent equipment (Kavo Company, Germany) for the occlusal caries detection was dane through the comparison with other conventional diagnostic techniques, such as visual inspection, intra-oral micro camera and digital X-ray. The effectiveness of the equipment in the detection of hidden caries and its viability as a diagnosis method for caries in their initial stage was also studied. Fifty eight permanent molars and premolars teeth from patients with age between 6 and 30 years were studied. The obtained results indicated that the conventional methods employed for the caries diagnosis are unable to detect the carious lesion in its initial stage. The Diagnodent equipment has this capability to detect caries presenting a flawless surface, specially the hidden caries, allowing the dentist to decide between a preventive ar a conservative procedure. The main advantage of the Diagnodent is to be an objective method, compared to the visual and radiographic ones, that are dependent on the professional interpretation. The Diagnodent is, therefore, a promising alternative as an objective and standardized diagnosis method for the final diagnostic. (author)

  12. Candida "Psilosis" - electromigration techniques and MALDI-TOF mass spectrometry for phenotypical discrimination

    Czech Academy of Sciences Publication Activity Database

    Kubesová, Anna; Šalplachta, Jiří; Horká, Marie; Růžička, F.; Šlais, Karel

    2012-01-01

    Roč. 137, č. 8 (2012), s. 1937-1943 ISSN 0003-2654 R&D Projects: GA AV ČR IAAX00310701 Institutional research plan: CEZ:AV0Z40310501 Keywords : Candida parapsilosis * electromigration techniques * MALDI-TOF MS Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.969, year: 2012

  13. The technique of negative ions in mass spectrometry. Application to aromatics

    International Nuclear Information System (INIS)

    George, G.

    1984-01-01

    The author examines the application of NCI (study of negative ions created by chemical ionization and particularly by a reacting negative ion) on a model popular at the present time: the passion fruit. The author stresses that this technique has its limitations and should be considered as auxiliary to electron impact. However, it seems destined for a promising future for the analysis of natural produce [fr

  14. A Comparative Analysis of Uranium Ore using Laser Fluorimetric and gamma Spectrometry Techniques

    International Nuclear Information System (INIS)

    Madbouly, M.; Nassef, M. H.; El-Mongy, S.A.; Diab, A.M.

    2009-01-01

    A developed chemical separation method was used for the analysis of uranium in a standard U-ore (IAEA-RGU-1) by LASER fluorimetric technique. The non-destructive gamma assay technique was also applied to verify and compare the uranium content analyzed using laser technique. The results of the uranium analysis obtained by laser fluorimetry were found to be in the range of 360 - 420 μg/g with an average value of 390 μg/g. The bias between the measured and the certified value does not exceed 9.9%. For gamma-ray spectrometric analysis, the results of the measured uranium content were found to be in the range of 393.8 - 399.4 μg/g with an average value of 396.3 μg/g. The % difference in the case of γ- assay was 1.6 %. In general, the methods of analysis used in this study are applicable for a precise determination of uranium. It can be concluded that, laser analysis is preferred for assay of uranium ore due to the required small sample weight, the low time of sample preparation and cost of analysis.

  15. Pu abundances, concentrations, and isotopics by x- and gamma-ray spectrometry assay techniques

    International Nuclear Information System (INIS)

    Camp, D.C.; Gunnink, R.; Ruhter, W.D.; Prindle, A.L.; Gomes, R.J.

    1986-01-01

    Two x- and gamma-ray systems were recently installed at-line in gloveboxes and will measure Pu solution concentrations from 5 to 105 g/L. These NDA technique, developed and refined over the past decade, are now used domestically and internationally for nuclear material process monitoring and accountability needs. In off- and at-line installations, they can measure solution concentrations to 0.2%. The K-XRFA systems use a transmission source to correct for solution density. The gamma-ray systems use peaks from 59- to 208-keV to determine solution concentrations and relative isotopics. A Pu check source monitors system stability. These two NDA techniques can be combined to form a new, NDA measurement methodology. With the instrument located outside of a glovebox, both relative Pu isotopics and absolute Pu abundances of a sample located inside a glovebox can be measured. The new technique works with either single or dual source excitation; the former for a detector 6 to 20 cm away with no geometric corrections needed; the latter requires geometric corrections or source movement if the sample cannot be measured at the calibration distance. 4 refs., 7 figs., 2 tabs

  16. Microextraction Techniques Coupled to Liquid Chromatography with Mass Spectrometry for the Determination of Organic Micropollutants in Environmental Water Samples

    Directory of Open Access Journals (Sweden)

    Mª Esther Torres Padrón

    2014-07-01

    Full Text Available Until recently, sample preparation was carried out using traditional techniques, such as liquid–liquid extraction (LLE, that use large volumes of organic solvents. Solid-phase extraction (SPE uses much less solvent than LLE, although the volume can still be significant. These preparation methods are expensive, time-consuming and environmentally unfriendly. Recently, a great effort has been made to develop new analytical methodologies able to perform direct analyses using miniaturised equipment, thereby achieving high enrichment factors, minimising solvent consumption and reducing waste. These microextraction techniques improve the performance during sample preparation, particularly in complex water environmental samples, such as wastewaters, surface and ground waters, tap waters, sea and river waters. Liquid chromatography coupled to tandem mass spectrometry (LC/MS/MS and time-of-flight mass spectrometric (TOF/MS techniques can be used when analysing a broad range of organic micropollutants. Before separating and detecting these compounds in environmental samples, the target analytes must be extracted and pre-concentrated to make them detectable. In this work, we review the most recent applications of microextraction preparation techniques in different water environmental matrices to determine organic micropollutants: solid-phase microextraction SPME, in-tube solid-phase microextraction (IT-SPME, stir bar sorptive extraction (SBSE and liquid-phase microextraction (LPME. Several groups of compounds are considered organic micropollutants because these are being released continuously into the environment. Many of these compounds are considered emerging contaminants. These analytes are generally compounds that are not covered by the existing regulations and are now detected more frequently in different environmental compartments. Pharmaceuticals, surfactants, personal care products and other chemicals are considered micropollutants. These

  17. Experimental determination of nuclear reaction rates (n,γ) by the gamma-rays capture spectrometry technique

    International Nuclear Information System (INIS)

    Lucatero, M.A.

    1976-01-01

    The technique of the gamma-rays capture spectrometry was used in the experimental determination of nuclear reaction rates of the type (n,γ). This technique consists in the incidence of a thermal neutrons collimated beam upon a sample, detecting the capture spectrum of gamma rays emitted at a solid fixed angle. In the determination of the efficiency curve intrinsic to the detection electronic system the reactions 199 Hg(n,γ) 200 Hg, 56 Fe(n,γ) 57 Fe and 63 Cu(n,γ) 64 Cu were used with the energy of the gamma rays capture of 5.976, 7.635 and 7.915 Mev respectively, through the irradiation of standard samples of Hg(175.3g), Fe(110.4g) and Cu(108.5g) of cylindrical geometry the two former and parallelepiped the latter. The problem concerning the corrections due to the thermal neutrons flux depression, the gammas auto-attenuation, and the geometric factor due to the cylindrical and parallelepiped geometry are involved in the data process. The experimental determination of the reaction 35 Cl(n,γ) 36 Cl rate was made through the observation of the gamma caputre of 6.111 Mev when a sample of CaCl 2 of cylindrical geometry was irradiated. This rate can be favorably compared with the reaction rate determined theoretically. (author)

  18. X-ray spectrometry and X-ray microtomography techniques for soil and geological samples analysis

    Energy Technology Data Exchange (ETDEWEB)

    Kubala-Kukuś, A.; Banaś, D.; Braziewicz, J. [Institute of Physics, Jan Kochanowski University, ul. Świetokrzyska 15, 25-406 Kielce (Poland); Holycross Cancer Center, ul. Artwińskiego 3, 25-734 Kielce (Poland); Dziadowicz, M.; Kopeć, E. [Institute of Physics, Jan Kochanowski University, ul. Świetokrzyska 15, 25-406 Kielce (Poland); Majewska, U. [Institute of Physics, Jan Kochanowski University, ul. Świetokrzyska 15, 25-406 Kielce (Poland); Holycross Cancer Center, ul. Artwińskiego 3, 25-734 Kielce (Poland); Mazurek, M.; Pajek, M.; Sobisz, M.; Stabrawa, I. [Institute of Physics, Jan Kochanowski University, ul. Świetokrzyska 15, 25-406 Kielce (Poland); Wudarczyk-Moćko, J. [Holycross Cancer Center, ul. Artwińskiego 3, 25-734 Kielce (Poland); Góźdź, S. [Holycross Cancer Center, ul. Artwińskiego 3, 25-734 Kielce (Poland); Institute of Public Health, Jan Kochanowski University, IX Wieków Kielc 19, 25-317 Kielce (Poland)

    2015-12-01

    A particular subject of X-ray fluorescence analysis is its application in studies of the multielemental sample of composition in a wide range of concentrations, samples with different matrices, also inhomogeneous ones and those characterized with different grain size. Typical examples of these kinds of samples are soil or geological samples for which XRF elemental analysis may be difficult due to XRF disturbing effects. In this paper the WDXRF technique was applied in elemental analysis concerning different soil and geological samples (therapeutic mud, floral soil, brown soil, sandy soil, calcium aluminum cement). The sample morphology was analyzed using X-ray microtomography technique. The paper discusses the differences between the composition of samples, the influence of procedures with respect to the preparation of samples as regards their morphology and, finally, a quantitative analysis. The results of the studies were statistically tested (one-way ANOVA and correlation coefficients). For lead concentration determination in samples of sandy soil and cement-like matrix, the WDXRF spectrometer calibration was performed. The elemental analysis of the samples was complemented with knowledge of chemical composition obtained by X-ray powder diffraction.

  19. X-ray spectrometry and X-ray microtomography techniques for soil and geological samples analysis

    International Nuclear Information System (INIS)

    Kubala-Kukuś, A.; Banaś, D.; Braziewicz, J.; Dziadowicz, M.; Kopeć, E.; Majewska, U.; Mazurek, M.; Pajek, M.; Sobisz, M.; Stabrawa, I.; Wudarczyk-Moćko, J.; Góźdź, S.

    2015-01-01

    A particular subject of X-ray fluorescence analysis is its application in studies of the multielemental sample of composition in a wide range of concentrations, samples with different matrices, also inhomogeneous ones and those characterized with different grain size. Typical examples of these kinds of samples are soil or geological samples for which XRF elemental analysis may be difficult due to XRF disturbing effects. In this paper the WDXRF technique was applied in elemental analysis concerning different soil and geological samples (therapeutic mud, floral soil, brown soil, sandy soil, calcium aluminum cement). The sample morphology was analyzed using X-ray microtomography technique. The paper discusses the differences between the composition of samples, the influence of procedures with respect to the preparation of samples as regards their morphology and, finally, a quantitative analysis. The results of the studies were statistically tested (one-way ANOVA and correlation coefficients). For lead concentration determination in samples of sandy soil and cement-like matrix, the WDXRF spectrometer calibration was performed. The elemental analysis of the samples was complemented with knowledge of chemical composition obtained by X-ray powder diffraction.

  20. Characterisation of lipid fraction of marine macroalgae by means of chromatography techniques coupled to mass spectrometry.

    Science.gov (United States)

    Ragonese, Carla; Tedone, Laura; Beccaria, Marco; Torre, Germana; Cichello, Filomena; Cacciola, Francesco; Dugo, Paola; Mondello, Luigi

    2014-02-15

    In this work the characterisation of the lipid fraction of several species of marine macro algae gathered along the eastern coast of Sicily is reported. Two species of green marine algae (Chloropyceae), two species of red marine algae (Rhodophyceae) and four species of brown marine algae (Pheophyceae) were evaluated in terms of fatty acids, triacylglycerols, pigments and phospholipids profile. Advanced analytical techniques were employed to fully characterise the lipid profile of these Mediterranean seaweeds, such as GC-MS coupled to a novel mass spectra database supported by the simultaneous use of linear retention index (LRI) for the identification of fatty acid profile; LC-MS was employed for the identification of triacylglycerols (TAGs), carotenoids and phospholipids; the determination of accurate mass was carried out on carotenoids and phospholipids. Quantitative data are reported on fatty acids and triacylglycerols as relative percentage of total fraction. Copyright © 2013 Elsevier Ltd. All rights reserved.

  1. Thorium: one of the analytical techniques in neutronic activation and alpha spectrometry of the CDTN (Brazilian Nuclear Technology Development Center) in the last three decades

    International Nuclear Information System (INIS)

    Menezes, M.A.B.C.; Sabino, C.V.S.

    1994-01-01

    For long years, the CDTN (Brazilian Nuclear Technology Development Center ) has applied several analytical techniques in the thorium determination. This work is about the evolution of the neutronic activation in the thorium 232 analysis from the 1960's to now. The importance of the analysis request and alpha spectrometry for the thorium 228 and thorium 232 determination is emphasized. (J.A.M.M.)

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

    NARCIS (Netherlands)

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

    2016-01-01

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

  3. estudo comparativo

    OpenAIRE

    Álvaro, Rocha

    2005-01-01

    O sítio web é um importante meio de comunicação e competitividade das universidades. Há diferentes razões para acreditar que os sítios possam variar entre universidades, mas contudo há certeza da existência de requisitos de qualidade comuns e transversais a todas. Este estudo visou avaliar, de forma quantitativa e objectiva, o cumprimento de requisitos de qualidade pelos sítios web das Universidades Portuguesas, com base nas características de alto nível da norma ISO 9126-1 que interessam aos...

  4. Quantitative analysis of occluded gases in uranium dioxide pellets by the mass spectrometry technique

    International Nuclear Information System (INIS)

    Vega Bustillos, J.O.W.; Rodrigues, C.; Iyer, S.S.

    1981-05-01

    A quantitative analysis of different components of occluded gases except water in uranium dioxide pellets is attempted here. A high temperature vacuum extration system is employed for the liberation and the determination of total volume of the occluded gases. A mass spectrometric technique is employed for the qualitative and quantitative analysis of these gases. The UO 2 pellets are placed in a graphite crucible and are subjected to varing temperatures (1000 0 C - 1700 0 C). The liberated gases are dehydrated and transferred to a measuring unit consisting essentially of a Toepler pump and a McLeod gauge. In this system the total volume of the gases liberated at N. T. P. is determined with a sensitivity of 0.002 cm 3 /g of UO 2 . An aliquot of the liberated gas is introduced into a quadrupole mass spectrometer (VGA-100 Varian Corp.) for the determination of the different components of the gas. On the basis of the analysis suggestions are made for the possible sources of these gas components. (Author) [pt

  5. A comparative study of 232Th and 238U activity estimation in soil samples by gamma spectrometry and Neutron Activation Analysis (NAA) technique

    International Nuclear Information System (INIS)

    Rekha, A.K.; Anilkumar, S.; Narayani, K.; Babu, D.A.R.

    2012-01-01

    Radioactivity in the environment is mainly due to the naturally occurring radionuclides like uranium, thorium with their daughter products and potassium. Even though Gamma spectrometry is the most commonly used non destructive method for the quantification of these naturally occurring radionuclides, Neutron Activation Analysis (NAA), a well established analytical technique, can also be used. But the NAA technique is a time consuming process and needs proper standards, proper sample preparation etc. In this paper, the 232 Th and 238 U activity estimated using gamma ray spectrometry and NAA technique are compared. In the case of direct gamma spectrometry method, the samples were analysed after sealing in a 250 ml container. Whereas for the NAA, about 300 mg of each sample, after irradiation were subjected to gamma spectrometry. The 238 U and 232 Th activities (in Bq/kg) in samples were estimated after the proper efficiency correction and were compared. The estimated activities by these two methods are in good agreement. The variation in 238 U and 232 Th activity values are within ± 15% which are acceptable for environmental samples

  6. Determination of mercury in an assortment of dietary supplements using an inexpensive combustion atomic absorption spectrometry technique.

    Science.gov (United States)

    Levine, Keith E; Levine, Michael A; Weber, Frank X; Hu, Ye; Perlmutter, Jason; Grohse, Peter M

    2005-01-01

    The concentrations of mercury in forty, commercially available dietary supplements, were determined using a new, inexpensive analysis technique. The method involves thermal decomposition, amalgamation, and detection of mercury by atomic absorption spectrometry with an analysis time of approximately six minutes per sample. The primary cost savings from this approach is that labor-intensive sample digestion is not required prior to analysis, further automating the analytical procedure. As a result, manufacturers and regulatory agencies concerned with monitoring lot-to-lot product quality may find this approach an attractive alternative to the more classical acid-decomposition, cold vapor atomic absorption methodology. Dietary supplement samples analyzed included astragalus, calcium, chromium picolinate, echinacea, ephedra, fish oil, ginger, ginkgo biloba, ginseng, goldenseal, guggul, senna, St John's wort, and yohimbe products. Quality control samples analyzed with the dietary supplements indicated a high level of method accuracy and precision. Ten replicate preparations of a standard reference material (NIST 1573a, tomato leaves) were analyzed, and the average mercury recovery was 109% (2.0% RSD). The method quantitation limit was 0.3 ng, which corresponded to 1.5 ng/g sample. The highest found mercury concentration (123 ng/g) was measured in a concentrated salmon oil sample. When taken as directed by an adult, this product would result in an approximate mercury ingestion of 7 mug per week.

  7. Comparison of gas chromatography/mass spectrometry and immunoassay techniques on concentrations of atrazine in storm runoff

    Science.gov (United States)

    Lydy, Michael J.; Carter, D.S.; Crawford, Charles G.

    1996-01-01

    Gas chromatography/mass spectrometry (GC/MS) and enzyme-linked immunosorbent assay (ELISA) techniques were used to measure concentrations of dissolved atrazine in 149 surface-water samples. Samples were collected during May 1992–September 1993 near the mouth of the White River (Indiana) and in two small tributaries of the river. GC/MS was performed on a Hewlett-Packard 5971 A, with electron impact ionization and selected ion monitoring of filtered water samples extracted by C-18 solid phase extraction; ELISA was performed with a magnetic-particle-based assay with photometric analysis. ELISA results compared reasonably well to GC/MS measurements at concentrations below the Maximum Contaminant Level for drinking water set by the U.S. Environmental Protection Agency (3.0 μg/L), but a systematic negative bias was observed at higher concentrations. When higher concentration samples were diluted into the linear range of calibration, the relation improved. A slight positive bias was seen in all of the ELISA data compared to the GC/MS results, and the bias could be partially explained by correcting the ELISA data for cross reactivity with other triazine herbicides. The highest concentrations of atrazine were found during the first major runoff event after the atrazine was applied. Concentrations decreased throughout the rest of the sampling period even though large runoff events occurred during this time, indicating that most atrazine loading to surface waters in the study area occurs within a few weeks after application.

  8. Characterisation and discrimination of various types of lac resin using gas chromatography mass spectrometry techniques with quaternary ammonium reagents.

    Science.gov (United States)

    Sutherland, K; del Río, J C

    2014-04-18

    A variety of lac resin samples obtained from artists' suppliers, industrial manufacturers, and museum collections were analysed using gas chromatography mass spectrometry (GCMS) and reactive pyrolysis GCMS with quaternary ammonium reagents. These techniques allowed a detailed chemical characterisation of microgram-sized samples, based on the detection and identification of derivatives of the hydroxy aliphatic and cyclic (sesquiterpene) acids that compose the resin. Differences in composition could be related to the nature of the resin, e.g. wax-containing (unrefined), bleached, or aged samples. Furthermore, differences in the relative abundances of aliphatic hydroxyacids appear to be associated with the biological source of the resin. The diagnostic value of newly characterised lac components, including 8-hydroxyacids, is discussed here for the first time. Identification of derivatised components was aided by AMDIS deconvolution software, and discrimination of samples was enhanced by statistical evaluation of data using principal component analysis. The robustness of the analyses, together with the minimal sample size required, make these very powerful approaches for the characterisation of lac resin in museum objects. The value of such analyses for enhancing the understanding of museum collections is illustrated by two case studies of objects in the collection of the Philadelphia Museum of Art: a restorer's varnish on a painting by Luca Signorelli, and a pictorial inlay in an early nineteenth-century High Chest by George Dyer. Copyright © 2014 Elsevier B.V. All rights reserved.

  9. Multiple inert gas elimination technique by micropore membrane inlet mass spectrometry--a comparison with reference gas chromatography.

    Science.gov (United States)

    Kretzschmar, Moritz; Schilling, Thomas; Vogt, Andreas; Rothen, Hans Ulrich; Borges, João Batista; Hachenberg, Thomas; Larsson, Anders; Baumgardner, James E; Hedenstierna, Göran

    2013-10-15

    The mismatching of alveolar ventilation and perfusion (VA/Q) is the major determinant of impaired gas exchange. The gold standard for measuring VA/Q distributions is based on measurements of the elimination and retention of infused inert gases. Conventional multiple inert gas elimination technique (MIGET) uses gas chromatography (GC) to measure the inert gas partial pressures, which requires tonometry of blood samples with a gas that can then be injected into the chromatograph. The method is laborious and requires meticulous care. A new technique based on micropore membrane inlet mass spectrometry (MMIMS) facilitates the handling of blood and gas samples and provides nearly real-time analysis. In this study we compared MIGET by GC and MMIMS in 10 piglets: 1) 3 with healthy lungs; 2) 4 with oleic acid injury; and 3) 3 with isolated left lower lobe ventilation. The different protocols ensured a large range of normal and abnormal VA/Q distributions. Eight inert gases (SF6, krypton, ethane, cyclopropane, desflurane, enflurane, diethyl ether, and acetone) were infused; six of these gases were measured with MMIMS, and six were measured with GC. We found close agreement of retention and excretion of the gases and the constructed VA/Q distributions between GC and MMIMS, and predicted PaO2 from both methods compared well with measured PaO2. VA/Q by GC produced more widely dispersed modes than MMIMS, explained in part by differences in the algorithms used to calculate VA/Q distributions. In conclusion, MMIMS enables faster measurement of VA/Q, is less demanding than GC, and produces comparable results.

  10. An integrated strategy for in vivo metabolite profiling using high-resolution mass spectrometry based data processing techniques

    International Nuclear Information System (INIS)

    Guo, Jian; Zhang, Minli; Elmore, Charles S.; Vishwanathan, Karthick

    2013-01-01

    Graphical abstract: -- Highlights: •Profiling the metabolites of model compounds in rats using high resolution mass spectrometry based data processing techniques. •Demonstrating an integrated strategy in vivo metabolite profiling using data mining tools. •Unusual metabolites generated via thiazole-ring opening were characterized based on processed LC–MS.data. -- Abstract: An ongoing challenge of drug metabolite profiling is to detect and identify unknown or low-level metabolites in complex biological matrices. Here we present a generic strategy for metabolite detection using multiple accurate-mass-based data processing tools via the analysis of rat samples of two model drug candidates, AZD6280 and AZ12488024. First, the function of isotopic pattern recognition was proved to be highly effective in the detection of metabolites derived from [ 14 C]-AZD6280 that possesses a distinct isotopic pattern. The metabolites revealed using this approach were in excellent qualitative correlation to those observed in radiochromatograms. Second, the effectiveness of accurate mass based untargeted data mining tools such as background subtraction, mass defect filtering, or a data mining package (MZmine) used for metabolomic analysis in detection of metabolites of [ 14 C]-AZ12488024 in rat urine, feces, bile and plasma samples was examined and a total of 33 metabolites of AZ12488024 were detected. Among them, at least 16 metabolites were only detected by the aid of the data mining packages and not via radiochromatograms. New metabolic pathways such as S-oxidation and thiomethylation reactions occurring on the thiazole ring were proposed based on the processed data. The results of these experiments also demonstrated that accurate mass-based mass defect filtering (MDF) and data mining techniques used in metabolomics are complementary and can be valuable tools for delineating low-level metabolites in complex matrices. Furthermore, the application of distinct multiple data

  11. Técnica para o estudo da anatomia da epiderme foliar de batata A technique for the anatomical study of potato leaf epidermis

    Directory of Open Access Journals (Sweden)

    Fernanda Bastos Segatto

    2004-10-01

    Full Text Available Embora a batata (Solanum tuberosum seja uma espécie de grande valor econômico, são poucas as informações disponíveis sobre a anatomia foliar, principalmente de características estruturais da epiderme. O estudo da anatomia foliar assume grande importância básica, para a ecologia e fisiologia, e aplicada para a fitopatologia e o melhoramento genético. Este trabalho teve por objetivo identificar uma técnica histológica que permite a confecção de lâminas semipermanentes para avaliar a epiderme foliar, em vista frontal, de um grande número de plantas de batata em um curto período de tempo. O corte paradérmico a mão livre, o método de Jeffrey e as técnicas de hidróxido de potássio e de impressão da epiderme foram avaliados. Lâminas semipermanentes foram confeccionadas da secção frontal da epiderme de folíolos principais do terço médio de plantas de batata. A impressão da epiderme em lâmina foi a única técnica que possibilitou a avaliação adequada de todos os clones de batata utilizados. A impressão da epiderme é uma técnica muito rápida, de baixo custo e de fácil execução, que atende os requisitos necessários para a identificação e seleção de características anatômicas de um grande número de plantas em um programa de melhoramento genético de batata.Even though potato (Solanum tuberosum is an economically important crop, information about leaf characteristics of anatomical structure has not been well studied. Studies of leaf epidermis have significance for basic fields as ecology and physiology and for applied fields as plant pathology and breeding. The objective of this research was to identify a fast and easy technique to prepare semi-permanent slides for studying the anatomy of potato leaf epidermis. Para dermal free hand cut, Jeffrey method, potassium hydroxide and epidermal fingerprint on glass slide techniques were evaluated. Semi-permanent slides were prepared from the longitudinal section of

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

    International Nuclear Information System (INIS)

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

    2005-01-01

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

  13. Study of the porosity of synthetic sandstones by nondestructive nuclear techniques; Estudo da porosidade de arenitos sinteticos por tecnicas nucleares nao destrutivas

    Energy Technology Data Exchange (ETDEWEB)

    Marques, Leonardo Carmezini

    2008-07-01

    In this paper, nuclear techniques have been used to describe structural characteristics of ceramic samples. These samples were produced to serve as simulates of sandstones and their mainly component was silica (SiO{sub 2}). Three sets of these samples with different characteristics were analyzed with the gamma ray transmission and the X-ray microtomography. They had the function to describe parameters as porosity point to point and total average porosity, for the transmission case, and 2D sections average porosity, total average porosity and size porous distribution for microtomography, as well as to investigate possible irregularities in bulk sample. The experimental set up for the gamma ray transmission technique consisted of: a 2 x 2 crystal NaI(Tl) detector, an {sup 241}Am radioactive source (59.54 keV, 100 mCi), an automatic micrometric table for the sample XZ movement and standard gamma spectrometry electronics. Lead collimators with 2 mm diameter were placed on the source way out and on the detector entrance. The microtomographic measurements were done with a Skyscan system, model 1172, with a X-ray tube with 20-100 kV of voltage range and a CCD camera. Employing gamma ray transmission method was possible to obtain overall porosity values from 25.8 to 34.0 % and from 24.8 to 29.2 % for samples with parallelepiped and cylinder shape, respectively, for ceramic I set; from 58.5 to 61.0 % and from 57.1 to 61.7 % for the same geometric shape of ceramic II set. The samples analyzed by the microtomography achieved resolutions of 1.73 {mu}m, 0.64 {mu}m and 1.28 {mu}m for samples of ceramic set I, II and III, respectively. This methodology provided average total porosity values from 26.6 to 29.4 %, from 48.4 to 51.0 % and from 28.2 to 30.6 % to I, II and III ceramic sets, respectively. The porous size profiles of each ceramic sample were also measured. (author)

  14. Mass spectrometry imaging of illicit drugs in latent fingerprints by matrix-free and matrix-assisted desorption/ionization techniques.

    Science.gov (United States)

    Skriba, Anton; Havlicek, Vladimir

    2018-02-01

    Compared with classical matrix-assisted laser-desorption ionization mass spectrometry (MALDI), the matrix free-based strategies generate a cleaner background, without significant noise or interference coming from an applied matrix, which is beneficial for the analysis of small molecules, such as drugs of abuse. In this work, we probed the detection efficiency of methamphetamine, heroin and cocaine in nanostructure-assisted laser desorption-ionization (NALDI) and desorption electrospray ionization and compared the sensitivity of these two matrix-free tools with a standard MALDI mass spectrometry experiment. In a typical mass spectrometry imaging (MSI) setup, papillary line latent fingerprints were recorded as a mixture a common skin fatty acid or interfering cosmetics with a drug. In a separate experiment, all drugs (1 µL of 1 μM standard solution) were detected by all three ionization techniques on a target. In the case of cocaine and heroin, NALDI mass spectrometry was the most sensitive and revealed signals even from 0.1 μM solution. The drug/drug contaminant (fatty acid or cosmetics) MSI approach could be used by law enforcement personnel to confirm drug abusers of having come into contact with the suspected drug by use of fingerprint scans at time of apprehension which can aid in reducing the work of lab officials.

  15. Semi-automated technique for the separation and determination of barium and strontium in surface waters by ion exchange chromatography and atomic emission spectrometry

    International Nuclear Information System (INIS)

    Pierce, F.D.; Brown, H.R.

    1977-01-01

    A semi-automated method for the separation and the analysis of barium and strontium in surface waters by atomic emission spectrometry is described. The method employs a semi-automated separation technique using ion exchange and an automated aspiration-analysis procedure. Forty specimens can be prepared in approximately 90 min and can be analyzed for barium and strontium content in 20 min. The detection limits and sensitivities provided by the described technique are 0.003 mg/l and 0.01 mg/l respectively for barium and 0.00045 mg/l and 0.003 mg/l respectively for strontium

  16. Potential of MALDI-TOF mass spectrometry as a rapid detection technique in plant pathology: identification of plant-associated microorganisms.

    Science.gov (United States)

    Ahmad, Faheem; Babalola, Olubukola O; Tak, Hamid I

    2012-09-01

    Plant diseases caused by plant pathogens substantially reduce crop production every year, resulting in massive economic losses throughout the world. Accurate detection and identification of plant pathogens is fundamental to plant pathogen diagnostics and, thus, plant disease management. Diagnostics and disease-management strategies require techniques to enable simultaneous detection and quantification of a wide range of pathogenic and non-pathogenic microorganisms. Over the past decade, rapid development of matrix-assisted laser-desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) techniques for characterization of microorganisms has enabled substantially improved detection and identification of microorganisms. In the biological sciences, MALDI-TOF MS is used to analyze specific peptides or proteins directly desorbed from intact bacteria, fungal spores, nematodes, and other microorganisms. The ability to record biomarker ions, in a broad m/z range, which are unique to and representative of individual microorganisms, forms the basis of taxonomic identification of microorganisms by MALDI-TOF MS. Recent advances in mass spectrometry have initiated new research, i.e. analysis of more complex microbial communities. Such studies are just beginning but have great potential for elucidation not only of the interactions between microorganisms and their host plants but also those among different microbial taxa living in association with plants. There has been a recent effort by the mass spectrometry community to make data from large scale mass spectrometry experiments publicly available in the form of a centralized repository. Such a resource could enable the use of MALDI-TOF MS as a universal technique for detection of plant pathogens and non-pathogens. The effects of experimental conditions are sufficiently understood, reproducible spectra can be obtained from computational database search, and microorganisms can be rapidly characterized by genus, species

  17. Introduction to Body Composition Assessment Using the Deuterium Dilution Technique with Analysis of Urine Samples by Isotope Ratio Mass Spectrometry (French Edition)

    International Nuclear Information System (INIS)

    2013-01-01

    The IAEA has fostered the more widespread use of a stable isotope technique to assess body composition in different population groups to address priority areas in public health nutrition in Member States. It has done this by supporting national and regional nutrition projects through its technical cooperation programme and coordinated research projects over many years. This publication was developed by an international group of experts to provide practical hands-on guidance in the use of this technique in settings where analysis of stable isotope ratios in biological samples is to be made by isotope ratio mass spectrometry. The publication is targeted at new users of this technique, for example nutritionists, analytical chemists and other professionals. More detailed information on the theoretical background and the practical applications of state of the art methodologies to monitor changes in body composition can be found in IAEA Human Health Series No. 3, Assessment of Body Composition and Total Energy Expenditure in Humans by Stable Isotope Techniques

  18. Introduction to Body Composition Assessment Using the Deuterium Dilution Technique with Analysis of Urine Samples by Isotope Ratio Mass Spectrometry (Spanish Edition)

    International Nuclear Information System (INIS)

    2013-01-01

    The IAEA has fostered the more widespread use of a stable isotope technique to assess body composition in different population groups to address priority areas in public health nutrition in Member States. It has done this by supporting national and regional nutrition projects through its technical cooperation programme and coordinated research projects over many years. This publication was developed by an international group of experts to provide practical hands-on guidance in the use of this technique in settings where analysis of stable isotope ratios in biological samples is to be made by isotope ratio mass spectrometry. The publication is targeted at new users of this technique, for example nutritionists, analytical chemists and other professionals. More detailed information on the theoretical background and the practical applications of state of the art methodologies to monitor changes in body composition can be found in IAEA Human Health Series No. 3, Assessment of Body Composition and Total Energy Expenditure in Humans by Stable Isotope Techniques

  19. Application of neutron activation techniques and x-ray energy dispersion spectrometry, in analysis of metallic traces adsorbed by chelex-100 resin

    International Nuclear Information System (INIS)

    Fernandes, Jair C.; Amaral, Angela M.; Magalhaes, Jesus C.; Pereira, Jose S.J.; Silva, Juliana B. da; Auler, Lucia M.L.A.

    2000-01-01

    In this work, the authors have investigated optimal conditions of adsorption for several ion metallic groups (cations of heavy metals and transition metals, oxyanions metallics and metalloids and cations of rare earths), as traces (ppb), withdrawn and in mixture of groups, by chelex-100 resin. The experiments have been developed by bath techniques in ammonium acetate tamponade solution 40 mM pH 5,52 content 0,5 g of chelex-100 resin. After magnetic agitation for two hours, resins were dried and submitted to X-ray energy dispersion spectrometry, x-ray fluorescence spectrometry and neutron activation analysis. The results have demonstrated that chelex-100 resin adsorb quantitatively transition element groups and rare earth groups in two cases (withdrawn and simultaneously adsorption)

  20. Geographical provenancing of purple grape juices from different farming systems by proton transfer reaction mass spectrometry using supervised statistical techniques

    NARCIS (Netherlands)

    Granato, Daniel; Koot, Alex; Ruth, van S.M.

    2015-01-01

    BACKGROUND: Organic, biodynamic and conventional purple grape juices (PGJ; n = 79) produced in Brazil and Europe were characterized by volatile organic compounds (m/z 20-160) measured by proton transfer reaction mass spectrometry (PTR-MS), and classification models were built using supervised

  1. Study of Rn-222 exhalation in phosphogypsum through the adsorption technique in activated coal; Estudo da exalacao de Rn-222 em fosfogesso por meio da tecnica de adsorcao em carvao ativado

    Energy Technology Data Exchange (ETDEWEB)

    Nisti, Marcelo Bessa; Campos, Marcia Pires de, E-mail: mbnisti@ipen.b, E-mail: mpcampos@ipen.b [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

    2011-10-26

    The radon exhalation was estimated through the adsorption in activated carbon technique. Classified as TENORM, the radon exhalation determination on the phosphogypsum piles was performed through the adsorption ratio of radon in activated carbon, from the concentration of descendants of {sup 222}Rn, {sup 214}Pb and {sup 214}Bi obtained by gamma spectrometry. The results obtained in this work were compatibles with the values found in the literature

  2. Comparison of laser fluorimetry, high resolution gamma-ray spectrometry and neutron activation analysis techniques for determination of uranium content in soil samples

    International Nuclear Information System (INIS)

    Ghods, A.; Asgharizadeh, F.; Salimi, B.; Abbasi, A.

    2004-01-01

    Much more concern is given nowadays for exposure of the world population to natural radiation especially to uranium since 57% of that exposure is due to radon-222, which is a member of uranium decay series. Most of the methods used for uranium determination is low concentration require either tedious separation and preconcentration or the accessibility to special instrumentation for detection of uranium at this low level. this study compares three techniques and methods for uranium analysis among different soil sample with variable uranium contents. Two of these techniques, neutron activation analysis and high resolution gamma-ray spectrometry , are non-destructive while the other, laser fluorimetry is done via chemical extraction of uranium. Analysis of standard materials is done also to control the quality and accuracy of the work. In spite of having quite variable ranges of detection limit, results obtained by high resolution gamma-ray spectrometry based on the assumption of having secular equilibrium between uranium and its daughters, which causes deviation whenever this condition was missed. For samples with reasonable uranium content, neutron activation analysis would be a rapid and reliable technique, while for low uranium content laser fluorimetry would be the most appropriate and accurate technique

  3. Reactor gamma spectrometry: status

    International Nuclear Information System (INIS)

    Gold, R.; Kaiser, B.J.

    1979-01-01

    Current work is described for Compton Recoil Gamma-Ray Spectrometry including developments in experimental technique as well as recent reactor spectrometry measurements. The current status of the method is described concerning gamma spectromoetry probe design and response characteristics. Emphasis is given to gamma spectrometry work in US LWR and BR programs. Gamma spectrometry in BR environments are outlined by focussing on start-up plans for the Fast Test Reactor (FTR). Gamma spectrometry results are presented for a LWR pressure vessel mockup in the Poolside Critical Assembly (PCA) at Oak Ridge National Laboratory

  4. Study on the natural radioactivity from the region of Presidente Figueiredo (AM), Brazil, using gamma spectrometry; Estudo da radioatividade natural da regiao de Presidente Figueiredo (AM) utilizando espectrometria gama

    Energy Technology Data Exchange (ETDEWEB)

    Da Silva, Jose Ribamar Silveira

    1999-07-01

    A gamma spectrometry profile was carried out along BR174 highway, that crosses some lithostratigraphic units of the North portion of the Sedimentary Basin of Amazon. Measurements in situ were realized in 116 points, 1 km apart, using a GAD-6 gamma-spectrometer and samples of rocks and soils were collected in geologically representative points, for gamma measurements using a shielded detector of NaI(Tl) available in the Nuclear Geophysics Laboratory of IAG/USP. The criterion used for evaluating the reliability degree of the concentration values of eU (ppm), eTh (ppm) and %K was to establish mathematically detection limits, for all measurement points. Every these points had been located using GPS with accuracy of 50 m to become possible a future detailed study. The purpose of matching portable gamma spectrometer and laboratory determinations was to compare the 2 techniques, using the criterion of detectability limits, and to verify the influence of {sup 222} Rn atmospheric radioactive gas in field measurements. In the case of portable detector, it allows fast measurements and the sensor 'sees' a big volume of material (rock, soil...), that makes it more representative. In some situations where atmospheric phenomena of thermal inversion occurs, measurement can be affected by the {sup 222} Rn cosmic background. Presence of radon daughter elements, associated with aerosols, in this tropical environment (high values of temperature and humidity), where the speed of the wind that could exhaust this gas is practically zero. It is observed that the values of concentration in the some points, got with these 2 techniques, have the same trend, and the stretches where peaks of concentration of K also occur and U and Th are associated with the presence of granite out corps, great boulders, and clay soils from weathering of these rocks. (author)

  5. Study on the natural radioactivity from the region of Presidente Figueiredo (AM), Brazil, using gamma spectrometry; Estudo da radioatividade natural da regiao de Presidente Figueiredo (AM) utilizando espectrometria gama

    Energy Technology Data Exchange (ETDEWEB)

    Da Silva, Jose Ribamar Silveira

    1999-07-01

    A gamma spectrometry profile was carried out along BR174 highway, that crosses some lithostratigraphic units of the North portion of the Sedimentary Basin of Amazon. Measurements in situ were realized in 116 points, 1 km apart, using a GAD-6 gamma-spectrometer and samples of rocks and soils were collected in geologically representative points, for gamma measurements using a shielded detector of NaI(Tl) available in the Nuclear Geophysics Laboratory of IAG/USP. The criterion used for evaluating the reliability degree of the concentration values of eU (ppm), eTh (ppm) and %K was to establish mathematically detection limits, for all measurement points. Every these points had been located using GPS with accuracy of 50 m to become possible a future detailed study. The purpose of matching portable gamma spectrometer and laboratory determinations was to compare the 2 techniques, using the criterion of detectability limits, and to verify the influence of {sup 222} Rn atmospheric radioactive gas in field measurements. In the case of portable detector, it allows fast measurements and the sensor 'sees' a big volume of material (rock, soil...), that makes it more representative. In some situations where atmospheric phenomena of thermal inversion occurs, measurement can be affected by the {sup 222} Rn cosmic background. Presence of radon daughter elements, associated with aerosols, in this tropical environment (high values of temperature and humidity), where the speed of the wind that could exhaust this gas is practically zero. It is observed that the values of concentration in the some points, got with these 2 techniques, have the same trend, and the stretches where peaks of concentration of K also occur and U and Th are associated with the presence of granite out corps, great boulders, and clay soils from weathering of these rocks. (author)

  6. Determination of Endocrine Disrupting Compounds in surface waters by means of chromatographic techniques coupled to mass spectrometry

    Directory of Open Access Journals (Sweden)

    M. Di Carro

    2011-01-01

    Full Text Available Two analytical methods were developed to study five endocrine disrupting compounds (4-n-nonylphenol, bisphenol A, estrone, 17β-estradiol and 17α-ethinylestradiol in waters. One method includes a fast liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS-MS analysis, while the second comprise a Stir Bar Sorptive Extraction (SBSE followed by a headspace derivatization and gaschromatography-mass spectrometry (GC-MS analysis. Passive samplers POCIS (Polar Organic Chemical Integrative Samplers were used as sampling and preconcentration steps in order to reach the very low levels of the analytes in environmental waters. Both methods were then applied to the determination of the analytes in different water samples.

  7. A comparative study of 232Th and 238U activity estimation in soil samples by gamma spectrometry and neutron activation analysis technique

    International Nuclear Information System (INIS)

    Anilkumar, Rekha; Anilkumar, S.; Narayani, K.; Babu, D.A.R.; Sharma, D.N.

    2012-01-01

    Neutron activation analysis (NAA) is a well-established analytical technique. It has many advantages as compared to the other commonly used techniques. NAA can be performed in a variety of ways depending on the element, its activity level in the sample, interference from the sample matrix and other elements, etc. This technique is used to get high analytical sensitivity and low detection limits (ppm to ppb). The high sensitivity is due to the irradiation at high neutron flux available from the research reactors and the activity measurement is done using high resolution HPGe detectors. In this paper, the activity estimation of soil samples using neutron activation and direct gamma spectrometry methods are compared. Even though the weights of samples considered and samples preparation methods are different for these two methods, the estimated activity values are comparable. (author)

  8. Ion-trap tandem mass spectrometry. A reliable technique for the analysis of PCDD/Fs and dioxin-like PCBs in food and feed samples

    Energy Technology Data Exchange (ETDEWEB)

    Santos, F J; Malavia, J; Galceran, M T [Barcelona Univ. (Spain). Dept. of Analytical Chemistry; Abalos, M; Abad, E; Rivera, J [Mass Spectrometry Laboratory, Dept. of Ecotechnologies, IIQAB-CSIC, Barcelona (Spain)

    2004-09-15

    The recent establishment of maximum residue limits for polychlorodibenzo-pdioxins (PCDDs) and dibenzofurans (PCDFs) in food and feed samples by the European Community and the future inclusion of dioxin-like polychlorinated biphenyls (dl-PCBs) in these values at the end of 2006, has led to an important increase on the routine analysis of these compounds. Therefore, there is a clear need to have powerful sensitive and selective methods for the analysis of these compounds at low concentration levels. Actually, gas chromatography coupled with high resolution mass spectrometry (GC-HRMS) is the technique of reference for the determination of these analytes in environmental and food samples due to its high sensitivity and selectivity. Nevertheless, this technique is relatively expensive and requires qualifier personnel. Therefore, the development of more economical but reliable methods that can deliver results comparable to GC-HRMS is required. During the last years, gas chromatography coupled with ion trap mass spectrometry (GC-ITMS) working in MS/MS mode has become an interesting alternative technique to GC-HRMS for the analysis of PCDD/Fs and dl-PCBs. The aim of the present work is to demonstrate the ability of the gas chromatography coupled with ion-trap tandem mass spectrometry (GC-ITMS/MS) for the analysis of PCDD/Fs and dl-PCBs in food and feed samples. This work was performed on the framework of the European research project called DIFFERENCE (Dioxins in Food and Feed - Reference methods and New Certified Reference Materials) with the objective to validate the GC-ITMS/MS method as alternative to HRMS in order to reduce the cost of dioxin analysis. The results and conclusions of the evaluation study are presented here.

  9. Development of High Resolution Resonance Ionization Mass Spectrometry for Neutron Dosimetry Technique with93Nb(n,n'93mNb Reaction

    Directory of Open Access Journals (Sweden)

    Tomita Hideki

    2016-01-01

    Full Text Available We have proposed an advanced technique to measure the 93mNb yield precisely by Resonance Ionization Mass Spectrometry, instead of conventional characteristic X-ray spectroscopy. 93mNb-selective resonance ionization is achievable by distinguishing the hyperfine splitting of the atomic energy levels between 93Nb and 93mNb at high resolution. In advance of 93mNb detection, we could successfully demonstrate high resolution resonant ionization spectroscopy of stable 93Nb using an all solid-state, narrow-band and tunable Ti:Sapphire laser system operated at 1 kHz repetition rate.

  10. Spectroscopic techniques (Mössbauer spectrometry, NMR, ESR,…) as tools to resolve doubtful NMR images: Study of the craniopharyngioma tumor

    Science.gov (United States)

    Rimbert, J. N.; Dumas, F.; Lafargue, C.; Kellershohn, C.; Brunelle, F.; Lallemand, D.

    1990-07-01

    Craniopharyngioma, an intracranial tumor, exhibits hyperintensity in the Spin-Echo-T2-NMR image and a hyposignal in the SE-T1-image. However, in some cases (15-20% cases), hypersignals are seen in both SE-T1 and T2-MRI. Using spectroscopic techniques, Mössbauer spectrometry in particular, we have demonstrated that the T1 hypersignal is due to ferritin, dissolved in the cystic liquid, after tumor cell lysis, in the course of time. Other possible reasons inducing a shortening of the T1 relaxation time (presence of lipids, intratumoral hemorrhage) have been rejected.

  11. Hepatoblastoma Biology Using Isotope Ratio Mass Spectrometry: Utility of a Unique Technique for the Analysis of Oncological Specimens.

    Science.gov (United States)

    Taran, Katarzyna; Frączek, Tomasz; Sitkiewicz, Anna; Sikora-Szubert, Anita; Kobos, Józef; Paneth, Piotr

    2016-07-07

    Hepatoblastoma is the most common primary liver tumor in children. However, it occurs rarely, with an incidence of 0.5-1.5 cases per million children. There is no clear explanation of the relationship between clinicopathologic features, therapy, and outcome in hepatoblastoma cases, so far. One of the most widely accepted prognostic factors in hepatoblastoma is histology of the tumor. The aim of the study was to determine the potential differences in biology of hepatoblastoma histological subtypes at the atomic level using the unique method of isotope ratio mass spectrometry, which is especially valuable in examination of small groups of biological samples. Twenty-four measurements of nitrogen stable isotope ratio, carbon stable isotope ratio and total carbon to nitrogen mass ratio in fetal and embryonal hepatoblastoma tissue were performed using a Sercon 20-22 Continuous Flow Isotope Ratio Mass Spectrometer (CF-IRMS) coupled with a Sercon SL elemental analyzer for simultaneous carbon-nitrogen-sulfur (NCS) analysis. A difference of about 1.781‰ in stable nitrogen isotope 15N/14N ratio was found between examined hepatoblastoma histological subtypes. The prognosis in liver tumors cases in children may be challenging particularly because of the lack of versatile methods of its evaluation. Isotope ratio mass spectrometry allows one to determine the difference between hepatoblastoma histological subtypes and clearly indicates the cases with the best outcome.

  12. Hepatoblastoma Biology Using Isotope Ratio Mass Spectrometry: Utility of a Unique Technique for the Analysis of Oncological Specimens

    Directory of Open Access Journals (Sweden)

    Katarzyna Taran

    2016-07-01

    Full Text Available Introduction: Hepatoblastoma is the most common primary liver tumor in children. However, it occurs rarely, with an incidence of 0.5-1.5 cases per million children. There is no clear explanation of the relationship between clinicopathologic features, therapy, and outcome in hepatoblastoma cases, so far. One of the most widely accepted prognostic factors in hepatoblastoma is histology of the tumor. The aim of the study was to determine the potential differences in biology of hepatoblastoma histological subtypes at the atomic level using the unique method of isotope ratio mass spectrometry, which is especially valuable in examination of small groups of biological samples.Material/Methods: Twenty-four measurements of nitrogen stable isotope ratio, carbon stable isotope ratio and total carbon to nitrogen mass ratio in fetal and embryonal hepatoblastoma tissue were performed using a Sercon 20-22 Continuous Flow Isotope Ratio Mass Spectrometer (CF-IRMS coupled with a Sercon SL elemental analyzer for simultaneous carbon-nitrogen-sulfur (NCS analysis.Results: A difference of about 1.781‰ in stable nitrogen isotope 15N/14N ratio was found between examined hepatoblastoma histological subtypes.Conclusions: The prognosis in liver tumors cases in children may be challenging particularly because of the lack of versatile methods of its evaluation. Isotope ratio mass spectrometry allows one to determine the difference between hepatoblastoma histological subtypes and clearly indicates the cases with the best outcome.

  13. Improved diffusion technique for 15N:14N analysis of ammonium and nitrate from aqueous samples by stable isotope spectrometry

    International Nuclear Information System (INIS)

    Goerges, T.; Dittert, K.

    1998-01-01

    Nitrogen (N) isotope ratio mass spectrometry (IRMS) by Dumas combustion and continuous flow mass spectrometry has become a wide-spread tool for the studies of N turnover. The speed and labor efficiency of 15N determinations from aqueous solutions such as soil solutions or soil extracts are often limited by sample preparation. Several procedures for the conversion of dissolved ammonium (NH4+) or nitrate NO3- to gaseous ammonia and its subsequent trapping in acidified traps have been elaborated in the last decades. They are based on the use of acidified filters kept either above the respective solution or in floating PTFE envelopes. In this paper, we present an improved diffusion method with a fixed PTFE trap. The diffusion containers are continuously kept in a vertical rotary shaker. Quantitative diffusion can thus be achieved in only three days. For solutions with NH4+ levels of only 1 mg N kg-1 and NO3- concentrations of 12 mg N kg-1, recovery rates of 98.8-102% were obtained. By addition of 15N labeled and non-labeled NH4+ and NO3- it was shown that no cross-contamination from NH4+ to NO3- or vice versa takes place even when one form is labeled to more than 1 at %15N while the other form has natural 15N content. The method requires no intermediate step of ammonia volatilization before NO3- conversion

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

    Science.gov (United States)

    Helsper, Johannes P F G; Peters, Ruud J B; van Bemmel, Margaretha E M; Rivera, Zahira E Herrera; Wagner, Stephan; von der Kammer, Frank; Tromp, Peter C; Hofmann, Thilo; Weigel, Stefan

    2016-09-01

    Seven commercial titanium dioxide pigments and two other well-defined TiO2 materials (TiMs) were physicochemically characterised using asymmetric flow field flow fractionation (aF4) for separation, various techniques to determine size distribution and inductively coupled plasma mass spectrometry (ICPMS) for chemical characterization. The aF4-ICPMS conditions were optimised and validated for linearity, limit of detection, recovery, repeatability and reproducibility, all indicating good performance. Multi-element detection with aF4-ICPMS showed that some commercial pigments contained zirconium co-eluting with titanium in aF4. The other two TiMs, NM103 and NM104, contained aluminium as integral part of the titanium peak eluting in aF4. The materials were characterised using various size determination techniques: retention time in aF4, aF4 hyphenated with multi-angle laser light spectrometry (MALS), single particle ICPMS (spICPMS), scanning electron microscopy (SEM) and particle tracking analysis (PTA). PTA appeared inappropriate. For the other techniques, size distribution patterns were quite similar, i.e. high polydispersity with diameters from 20 to >700 nm, a modal peak between 200 and 500 nm and a shoulder at 600 nm. Number-based size distribution techniques as spICPMS and SEM showed smaller modal diameters than aF4-UV, from which mass-based diameters are calculated. With aF4-MALS calculated, light-scattering-based "diameters of gyration" (Øg) are similar to hydrodynamic diameters (Øh) from aF4-UV analyses and diameters observed with SEM, but much larger than with spICPMS. A Øg/Øh ratio of about 1 indicates that the TiMs are oblate spheres or fractal aggregates. SEM observations confirm the latter structure. The rationale for differences in modal peak diameter is discussed.

  15. Introduction to Body Composition Assessment Using the Deuterium Dilution Technique with Analysis of Saliva Samples by Fourier Transform Infrared Spectrometry (Spanish Edition)

    International Nuclear Information System (INIS)

    2013-01-01

    For many years, the IAEA has fostered the more widespread use of stable isotope techniques to assess body composition in different population groups to address priority areas in public health nutrition in Member States. The objective is to support national and regional nutrition projects through both the IAEA's technical cooperation programme and its coordinated research projects. In particular, during the last few years, the increased access to analyses of deuterium enrichment by Fourier transform infrared (FTIR) spectrometry has increased the application of this technique in Africa, Asia and Latin America. This publication was developed by an international group of experts to provide practical, hands-on guidance in the use of this technique in settings where the analysis of deuterium enrichment in saliva samples will be made by FTIR. It is targeted at new users of this technique, for example nutritionists, analytical chemists and other professionals. More detailed information on the theoretical background and the practical application of state of the art methodologies to monitor changes in body composition can be found in an IAEA publication entitled Assessment of Body Composition and Total Energy Expenditure in Humans by Stable Isotope Techniques (IAEA Human Health Series No. 3)

  16. Introduction to Body Composition Assessment Using the Deuterium Dilution Technique with Analysis of Saliva Samples by Fourier Transform Infrared Spectrometry (French Edition)

    International Nuclear Information System (INIS)

    2013-01-01

    For many years, the IAEA has fostered the more widespread use of stable isotope techniques to assess body composition in different population groups to address priority areas in public health nutrition in Member States. The objective is to support national and regional nutrition projects through both the IAEA's technical cooperation programme and its coordinated research projects. In particular, during the last few years, the increased access to analyses of deuterium enrichment by Fourier transform infrared (FTIR) spectrometry has increased the application of this technique in Africa, Asia and Latin America. This publication was developed by an international group of experts to provide practical, hands-on guidance in the use of this technique in settings where the analysis of deuterium enrichment in saliva samples will be made by FTIR. It is targeted at new users of this technique, for example nutritionists, analytical chemists and other professionals. More detailed information on the theoretical background and the practical application of state of the art methodologies to monitor changes in body composition can be found in an IAEA publication entitled Assessment of Body Composition and Total Energy Expenditure in Humans by Stable Isotope Techniques (IAEA Human Health Series No. 3)

  17. Assessment of elemental pollution in soil of Islamabad city using instrumental neutron activation analysis and atomic absorption spectrometry techniques

    International Nuclear Information System (INIS)

    Daud, M.; Wasim, M.; Khalid, N.; Zaidi, J.H.; Iqbal, J.

    2009-01-01

    The soil samples of nine different sites in Islamabad were studied for their elemental composition. Instrumental neutron activation analysis and atomic absorption spectrometry were employed and 33 elements were determined. The acquired data were analyzed using descriptive statistics, principal component analysis, cluster analysis, pollution level index and enrichment factor. A perusal of results shows a distribution of elemental concentration in two major groups, one along the highway and the other in industrial area of Islamabad. The soil along the highway sites was found to be relatively less polluted than at the sites in the industrial area. The enrichment factor indicates the presence of As, Pb, Sb, Se and Sn at higher levels. The method validation was done by analyzing IAEA reference materials SL-1 (lake sediment) and S7 (soil). (orig.)

  18. Neutron spectrometry with proton recoil proportional counters at the research and measurement reactor Braunschweig - status of the technique

    International Nuclear Information System (INIS)

    Knauf, K.; Wittstock, J.

    1987-07-01

    This status report is concerned with the facilities set up for neutron spectrometry at the Research and Measurement Reactor Braunschweig, based on proton recoil proportional counters. Cylindrical counters for irradiation by a neutron beam normal to the counter wire and commercial spherical counters are employed. They can be filled with hydrogen or a hydrogeneous gas up to a pressure of 1 MPa depending on their use. The filling method and the electronic pulse processing are described. The pulse analysis system includes a pulse shape discrimination branch in order to separate γ-ray induced pulses. Finally, experimental investigations with spherical counters are discussed regarding the region of proportionality and the influence of the counter voltage on the shape of the response function. (orig./HP) [de

  19. Estudo do gesto instrumental sob o prisma da Labanotation: o exemplo da Tapping Technique em Percussion Study I para violão solo de Arthur Kampela

    Directory of Open Access Journals (Sweden)

    Ledice Fernandes-Weiss

    2018-04-01

    Full Text Available Este estudo parte dos efeitos de percussão criados por Arthur Kampela em seu Percussion Study I visando compreender o movimento físico e o gesto instrumental do violonista como um fenômeno orgânico, intimamente relacionado com o gesto sonoro. Para tanto, utilizamos como ferramenta de análise a notação de movimentos coreográficos criada por Rudolf von Laban; este sistema é aplicado aos gestos requeridos para se realizarem cinco passagens da obra de Kampela onde os efeitos de percussão estão particularmente presentes. A partir da leitura dos cinetogramas criados, podemos observar uma predominância de movimentos em ricochete e outros efeitos percussivos que, além de promover um melhor relaxamento muscular, corroboram no impacto visual que a peça causa por sua gestualidade corporal. Observamos também que há uma notável exploração espacial do instrumento. Ao abordarmos o fazer musical de um ponto de vista coreográfico, entendemos este como um complexo que inclui o som produzido, os gestos e movimentos do performer, sua energia, seu corpo e o espaço que o circunda.

  20. X-ray spectrometry induced by electron and proton bombardment: Two complementary techniques for the micro-characterization of mineral materials

    International Nuclear Information System (INIS)

    Remond, G.; Gilles, C.; Isabelle, D.; Choi, C.G.; Rouer, O.; Cesbron, F.; Yang, C.

    1994-01-01

    Spatially resolved quantitative analysis by means of the Electron Probe Micro Analyser (EPMA) is now well established as a routine analytical method for point chemical analysis of a variety of mineral materials. Modern computer controlled EPMA are most often equipped with wavelength dispersive spectro- meters (WDS). Quantitative analyses are generally carried out according to a standard based approach, i. e, the x-ray intensities measured at the surface of the unknowns are normalized to those measured at the surface of reference specimens. By the use of energy dispersive spectrometry (EDS) a standardless quantitative based method is preferred when the incident beam current is not accurately known as for the case of EDS analysis coupled to Scanning Electron Microscopy (SEM). The accuracy of point analysis by means of electron beam induced x-ray spectrometry is discussed emphasizing the x-ray photon interactions respectively.The continuous x-ray emission is the physical limit of detection. The excitation conditions must be optimised in order to obtain the higher peak to continuous emission intensity ratios for each element within the matrix. Proton Induced X-ray Emission (PIXE) complements this electron induced x-ray emission for the localization of elements present at trace levels. The experimental procedure used for quantitative analysis by means of PIXE is illustrated emphasizing the use of a limited number of reference materials for deriving quantitative data from the raw PIXE spectra. The complementarity of EMPA/SEM and PIXE techniques is illustrated for the case of rare-earth elements (REE) bearing natural and synthetic doped zircon crystals (Si Zr O sub 4). For such compounds x-ray spectra are very complex because of the existence of severe peak overlaps between the L x-ray emission spectra of the REE. It is shown that cathodoluminescence (EPLA:SEM) and ionoluminescence (PIXE) may be an original alternative approach to x-ray spectrometry for studying REE

  1. Comparative studies of Yersinia pestis outer membrane isolation techniques and their potential use in plague epidemiology Estudo comparativo de técnicas de isolamento de membrana externa de Yersinia pestis e seu uso na epidemiologia da peste

    Directory of Open Access Journals (Sweden)

    Frederico Guilherme Coutinho Abath

    1990-04-01

    Full Text Available In the present study three techniques for obtaining outer membrane enriched fractions from Yersinia pestis were evaluated. The techniques analysed were: differential solubilization of the cytoplasmic membrane with Sarkosyl or Triton X-100, and centrifugation in sucrose density gradients. The sodium dodecyl-sulfate polyacrylamide gel electrophoresis (SDS-PAGE of outer membrane isolated by the different methods resulted in similar protein patterns. The measurement of NADH-dehydrogenase and succinate dehydrogenase (inner membrane enzymes indicated that the outer membrane preparations obtained by the three methods were pure enough for analytical studies. In addition, preliminary evidences on the potential use of outer membrane proteins for the identification of geographic variants of Y. pestis wild isolates are presented.No presente estudo três técnicas para isolamento de frações enriquecidas em membrana externa de Y. pestis foram avaliadas. As técnicas utilizadas foram: centrifugação em gradiente de densidade em sacarose e solubilização diferencial com Sarkosyl ou Triton X-100. A análise por eletroforese em gel de poliacrilamida na presença de dodecil sulfato de sódio (SDS-PAGE das membranas externas extraídas pelos diferentes métodos evidenciou perfis protéicos semelhantes. A determinação das atividades de NADH-desidrogenase e succinato-desidrogenase (enzimas de membrana interna indicou que todas as preparações estudadas eram adequadas a estudos analíticos. Obteve-se evidências preliminares sobre o possível uso de perfis protéicos de membrana externa na identificação de variantes geográficos entre isolados selvagens de Y. pestis.

  2. LabVIEW interface with Tango control system for a multi-technique X-ray spectrometry IAEA beamline end-station at Elettra Sincrotrone Trieste

    Energy Technology Data Exchange (ETDEWEB)

    Wrobel, P.M. [Physics Section, Nuclear Science and Instrumentation Laboratory (NSIL), IAEA Laboratories, A-2444 Seibersdorf (Austria); AGH University of Science and Technology, Faculty of Physics and Applied Computer Science, al. A. Mickiewicza 30, 30-059 Krakow (Poland); Bogovac, M. [Physics Section, Nuclear Science and Instrumentation Laboratory (NSIL), IAEA Laboratories, A-2444 Seibersdorf (Austria); Sghaier, H. [Physics Section, Nuclear Science and Instrumentation Laboratory (NSIL), IAEA Laboratories, A-2444 Seibersdorf (Austria); Institut Superieur d’Informatique et de Mathematiques de Monastir (ISIMM), Departement de technologie, 5000 Monastir (Tunisia); Leani, J.J. [Physics Section, Nuclear Science and Instrumentation Laboratory (NSIL), IAEA Laboratories, A-2444 Seibersdorf (Austria); IFEG – CONICET, Facultad de Matematica Astronomia y Fisica, Universidad Nacional de Cordoba, 5000 Cordoba (Argentina); Migliori, A.; Padilla-Alvarez, R. [Physics Section, Nuclear Science and Instrumentation Laboratory (NSIL), IAEA Laboratories, A-2444 Seibersdorf (Austria); Czyzycki, M. [Physics Section, Nuclear Science and Instrumentation Laboratory (NSIL), IAEA Laboratories, A-2444 Seibersdorf (Austria); AGH University of Science and Technology, Faculty of Physics and Applied Computer Science, al. A. Mickiewicza 30, 30-059 Krakow (Poland); Osan, J. [Physics Section, Nuclear Science and Instrumentation Laboratory (NSIL), IAEA Laboratories, A-2444 Seibersdorf (Austria); Environmental Physics Department, Hungarian Academy of Sciences Centre for Energy Research, Konkoly-Thege M. út 29-33., H-1121 Budapest (Hungary); Kaiser, R.B. [Physics Section, Nuclear Science and Instrumentation Laboratory (NSIL), IAEA Laboratories, A-2444 Seibersdorf (Austria); and others

    2016-10-11

    A new synchrotron beamline end-station for multipurpose X-ray spectrometry applications has been recently commissioned and it is currently accessible by end-users at the XRF beamline of Elettra Sincrotrone Trieste. The end-station consists of an ultra-high vacuum chamber that includes as main instrument a seven-axis motorized manipulator for sample and detectors positioning, different kinds of X-ray detectors and optical cameras. The beamline end-station allows performing measurements in different X-ray spectrometry techniques such as Microscopic X-Ray Fluorescence analysis (µXRF), Total Reflection X-Ray Fluorescence analysis (TXRF), Grazing Incidence/Exit X-Ray Fluorescence analysis (GI-XRF/GE-XRF), X-Ray Reflectometry (XRR), and X-Ray Absorption Spectroscopy (XAS). A LabVIEW Graphical User Interface (GUI) bound with Tango control system consisted of many custom made software modules is utilized as a user-friendly tool for control of the entire end-station hardware components. The present work describes this advanced Tango and LabVIEW software platform that utilizes in an optimal synergistic manner the merits and functionality of these well-established programming and equipment control tools. - Highlights: • A new methodology for control of a synchrotron beamline end-station is shown. • The new control system comprises a novel binding of Tango control system with LabVIEW interface. • The reliability of the control system is demonstrated by examples of analytical applications.

  3. Supercritical fluid chromatography coupled with tandem mass spectrometry: A high-efficiency detection technique to quantify Taxane drugs in whole-blood samples.

    Science.gov (United States)

    Jin, Chan; Guan, Jibin; Zhang, Dong; Li, Bing; Liu, Hongzhuo; He, Zhonggui

    2017-10-01

    We present a technique to rapid determine taxane in blood samples by supercritical fluid chromatography together with mass spectrometry. The aim of this study was to develop a supercritical fluid chromatography with mass spectrometry method for the analysis of paclitaxel, cabazitaxel, and docetaxel in whole-blood samples of rats. Liquid-dry matrix spot extraction was selected in sample preparation procedure. Supercritical fluid chromatography separation of paclitaxel, cabazitaxel, docetaxel, and glyburide (internal standard) was accomplished within 3 min by using the gradient mobile phase consisted of methanol as the compensation solvent and carbon dioxide at a flow rate of 1.0 mL/min. The method was validated regarding specificity, the lower limit of quantification, repeatability, and reproducibility of quantification, extraction recovery, and matrix effects. The lower limit of quantification was found to be 10 ng/mL since it exhibited acceptable precision and accuracy at the corresponding level. All interday accuracies and precisions were within the accepted criteria of ±15% of the nominal value and within ±20% at the lower limit of quantification, implying that the method was reliable and reproducible. In conclusion, this method is a promising tool to support and improve preclinical or clinical pharmacokinetic studies with the taxanes anticancer drugs. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Laparoscopia nas hérnias diafragmáticas: estudo experimental em cães Laparoscopic techniques in diaphragmatic hernias: experimental study in dogs

    Directory of Open Access Journals (Sweden)

    Carlos Afonso de Castro Beck

    2004-12-01

    Full Text Available A hérnia diafragmática traumática é a forma mais comum entre as hérnias diafragmáticas em cães e gatos e, por tratar-se de uma alteração anatômica, a terapêutica indicada é a sua correção cirúrgica. O presente estudo se propôs a avaliar a cirurgia videolaparoscópica no diagnóstico e tratamento dessa afecção em cães. Na primeira etapa do experimento, os animais foram submetidos à produção de um modelo de hérnia diafragmática. Após o período de uma semana, os cães foram submetidos à segunda etapa experimental por meio do acesso laparoscópico, tendo como finalidade o diagnóstico e a terapêutica cirúrgica. O acesso laparoscópico mostrou-se eficaz tanto na identificação das rupturas e dos deslocamentos como na correção cirúrgica de reposição visceral e rafia diafragmática nos oito cães do experimento.The most common type of diaphragmatic hernia in dogs and cats is the traumatic one. As an anatomic alteration, surgery is the elected treatment. The purpose of this study was to evaluate videolaparoscopic surgery in the diagnostic and treatment of diaphragmatic hernia in dogs. In the first phase of the study diaphragmatic hernias were performed in dogs. One week later the dogs were summited to a laparoscopic surgery to make diagnostic and surgical correction. Laparoscopic access showed to be efficient for identification of the defect and visceral displacement and for the surgical treatment.

  5. Application of Liquid Chromatography/Ion Trap Mass Spectrometry Technique to Determine Ergot Alkaloids in Grain Products

    Directory of Open Access Journals (Sweden)

    Krystyna Szymczyk

    2015-01-01

    Full Text Available A liquid chromatography/ion trap mass spectrometry-based method to determine six ergot alkaloids and their isomers is presented. The samples were cleaned on neutral alumina-based solid-phase extraction cartridges. The following method parameters were obtained (depending on the analyte and spiking level: method recovery from 63.0 to 104.6 %, relative standard deviation below 18 %, linear range from 1 to 325 μg/kg, linear correlation coefficient not less than 0.98. The developed analytical procedure was applied to determine the levels of ergot alkaloids in 65 samples of selected rye-based food products (flour– 34 samples, bran – 12 samples, rye – 18 samples, flakes – 1 sample. Measurable levels of alkaloids were found in majority of the analysed samples, particularly in rye flour. Additionally, alkaloids were determined in ergot sclerotia isolated from rye grains. Total content was nearly 0.01 % (97.9 mg/kg. However, the alkaloid profi le was dominated by ergocristine at 45.6 % (44.7 mg/kg, an alkaloid not commonly found in the tested food products. Ergocorninine at 0.2 % (0.2 mg/kg was the least abundant alkaloid.

  6. Application of Liquid Chromatography/Ion Trap Mass Spectrometry Technique to Determine Ergot Alkaloids in Grain Products.

    Science.gov (United States)

    Bryła, Marcin; Szymczyk, Krystyna; Jędrzejczak, Renata; Roszko, Marek

    2015-03-01

    A liquid chromatography/ion trap mass spectrometry-based method to determine six ergot alkaloids and their isomers is presented. The samples were cleaned on neutral alumina-based solid-phase extraction cartridges. The following method parameters were obtained (depending on the analyte and spiking level): method recovery from 63.0 to 104.6%, relative standard deviation below 18%, linear range from 1 to 325 µg/kg, linear correlation coefficient not less than 0.98. The developed analytical procedure was applied to determine the levels of ergot alkaloids in 65 samples of selected rye-based food products (flour - 34 samples, bran - 12 samples, rye - 18 samples, flakes - 1 sample). Measurable levels of alkaloids were found in majority of the analysed samples, particularly in rye flour. Additionally, alkaloids were determined in ergot sclerotia isolated from rye grains. Total content was nearly 0.01% (97.9 mg/kg). However, the alkaloid profile was dominated by ergocristine at 45.6% (44.7 mg/kg), an alkaloid not commonly found in the tested food products. Ergocorninine at 0.2% (0.2 mg/kg) was the least abundant alkaloid.

  7. Metabolite Analysis of Toosendanin by an Ultra-High Performance Liquid Chromatography-Quadrupole-Time of Flight Mass Spectrometry Technique

    Directory of Open Access Journals (Sweden)

    Na Li

    2013-09-01

    Full Text Available Toosendanin is the major bioactive component of Melia toosendan Sieb. et Zucc., which is traditionally used for treatment of abdominal pain and as an insecticide. Previous studies reported that toosendanin possesses hepatotoxicity, but the mechanism remains unknown. Its bioavailability in rats is low, which indicates the hepatotoxicity might be induced by its metabolites. In this connection, in the current study, we examined the metabolites obtained by incubating toosendanin with human live microsomes, and then six of these metabolites (M1–M6 were identified for the first time by ultra-high performance liquid chromatography-quadrupole-time of flight mass spectrometry (UHPLC-Q-TOF/MS. Further analysis on the MS spectra showed M1, M2, and M3 are oxidative products and M6 is a dehydrogenation product, while M4 and M5 are oxidative and dehydrogenation products of toosendanin. Moreover, their possible structures were deduced from the MS/MS spectral features. Quantitative analysis demonstrated that M1-M5 levels rapidly increased and reached a plateau at 30 min, while M6 rapidly reached a maximal level at 20 min and then decreased slowly afterwards. These findings have provided valuable data not only for understanding the metabolic fate of toosendanin in liver microsomes, but also for elucidating the possible molecular mechanism of its hepatotoxicity.

  8. Development of a gas chromatography-mass spectrometry technique to diagnose white snakeroot (Ageratina altissima) poisoning in a cow.

    Science.gov (United States)

    Meyerholtz, Kimberly A; Burcham, Grant N; Miller, Margaret A; Wilson, Christina R; Hooser, Stephen B; Lee, Stephen T

    2011-07-01

    An 8-year-old, crossbred beef cow was referred to the Indiana Animal Disease Diagnostic Laboratory at Purdue University for a complete necropsy in October 2009. The cow was the sixth to die in a 7-day period. Affected cows were reportedly stumbling and became weak, excitable, and recumbent. Histologically, myonecrosis was severe in the skeletal muscles and mild in the heart and tongue. According to the submitter, exposure to a poisonous plant was suspected, and a plant specimen received from this case was identified as white snakeroot (Ageratina altissima). Using the white snakeroot specimen, a gas chromatography-mass spectrometry analytical method for the detection of tremetone and dehydrotremetone (2 components of white snakeroot) was developed. Both tremetone and dehydrotremetone were detected in the plant specimen. Dehydrotremetone was recovered from the liver, while neither component was recovered in the rumen content. In the past, because of the lack of standard reference material, the diagnosis of white snakeroot poisoning was based mainly on history of exposure and the presence of the plant in the rumen. The analytical method described herein can be used to document exposure to tremetone or dehydrotremetone in cases of suspected white snakeroot poisoning when coupled with the appropriate clinical signs and lesions.

  9. Accelerator-based ultrasensitive mass spectrometry

    International Nuclear Information System (INIS)

    Gove, H.E.

    1985-01-01

    This chapter describes a new mass spectrometry technique involving charged particle accelerators normally used for basic research in nuclear science. Topics considered include the limitations of conventional mass spectrometry, the limitations of the direct measurement of radioactive decay, mass spectrometry using a tandem electrostatic accelerator, mass spectrometry using a cyclotron, how accelerator mass spectrometry circumvents the limitations of conventional mass spectrometry, measurements of stable isotopes, nuclear physics and astrophysics applications, modifications to existing accelerators, descriptions of dedicated systems, and future applications

  10. Toracoscopia nas hérnias diafragmáticas: estudo experimental em cães Thoracoscopic techniques in diaphragmatic hernias: experimental study in dogs

    Directory of Open Access Journals (Sweden)

    Carlos Afonso de Castro Beck

    2004-12-01

    Full Text Available Na classificação das hérnias diafragmáticas, a traumática é a forma mais prevalente em cães e gatos. A alteração, que se caracteriza por uma alteração anatômica, tem na correção cirúrgica, o tratamento recomendado. O presente estudo se propôs a avaliar a cirurgia videotoracoscópica no diagnóstico e tratamento de hérnias diafragmáticas em cães. Na primeira etapa do experimento, oito animais foram submetidos à produção de um modelo de hérnia diafragmática por meio do acesso laparoscópico. Após o período de uma semana, os cães foram submetidos à segunda etapa experimental através do acesso toracoscópico, tendo como finalidade o diagnóstico e a terapêutica cirúrgica. O acesso toracoscópico mostrou-se eficaz tanto no caráter diagnóstico das rupturas e dos deslocamentos, como na correção cirúrgica de reposição visceral e rafia diafragmática.The most common type of diaphragmatic hernia in dogs and cats is the traumatic one.As an anatomic alteration surgery is the elected treatment. The purpose of this study was to evaluate videothoracoscopic surgery in the diagnostic and treatment of diaphragmatic hernia in eight dogs. In the first phase of the study diaphragmatic hernias were performed in the dogs through laparoscopic access. One week later the dogs were summited to a thoracoscopic surgery to make diagnostic and surgical correction. Thoracoscopic access showed to be efficient for identification of the defects and visceral displacements and for the surgical treatment.

  11. Atomic mass spectrometry

    International Nuclear Information System (INIS)

    Sanz-Medel, A.

    1997-01-01

    The elemental inorganic analysis seems to be dominated today by techniques based on atomic spectrometry. After an evaluation of advantages and limitations of using mass analysers (ion detectors) versus conventional photomultipliers (photon detector) a brief review of the more popular techniques of the emerging Atomic Mass spectrometry is carried out. Their huge potential for inorganic trace analysis is such that in the future we could well witness how this end of the century and millennium marked the fall of the photons empire in Analytical Atomic Spectrometry. (Author)

  12. Noise-immune cavity-enhanced analytical atomic spectrometry — NICE-AAS — A technique for detection of elements down to zeptogram amounts

    International Nuclear Information System (INIS)

    Axner, Ove; Ehlers, Patrick; Hausmaninger, Thomas; Silander, Isak; Ma, Weiguang

    2014-01-01

    Noise-immune cavity-enhanced optical heterodyne molecular spectroscopy (NICE-OHMS) is a powerful technique for detection of molecular compounds in gas phase that is based on a combination of two important concepts: frequency modulation spectroscopy (FMS) for reduction of noise, and cavity enhancement, for prolongation of the interaction length between the light and the sample. Due to its unique properties, it has demonstrated unparalleled detection sensitivity when it comes to detection of molecular constituents in the gas phase. However, despite these, it has so far not been used for detection of atoms, i.e. for elemental analysis. The present work presents an assessment of the expected performance of Doppler-broadened (Db) NICE-OHMS for analytical atomic spectrometry, then referred to as noise-immune cavity-enhanced analytical atomic spectrometry (NICE-AAS). After a description of the basic principles of Db-NICE-OHMS, the modulation and detection conditions for optimum performance are identified. Based on a previous demonstrated detection sensitivity of Db-NICE-OHMS of 5 × 10 −12 cm −1 Hz −1∕2 (corresponding to a single-pass absorbance of 7 × 10 −11 over 10 s), the expected limits of detection (LODs) of Hg and Na by NICE-AAS are estimated. Hg is assumed to be detected in gas phase directly while Na is considered to be atomized in a graphite furnace (GF) prior to detection. It is shown that in the absence of spectral interferences, contaminated sample compartments, and optical saturation, it should be feasible to detect Hg down to 10 zg/cm 3 (10 fg/m 3 or 10 −5 ng/m 3 ), which corresponds to 25 atoms/cm 3 , and Na down to 0.5 zg (zg = zeptogram = 10 −21 g), representing 50 zg/mL (parts-per-sextillion, pps, 1:10 21 ) in liquid solution (assuming a sample of 10 μL) or solely 15 atoms injected into the GF, respectively. These LODs are several orders of magnitude lower (better) than any previous laser-based absorption technique previously demonstrated

  13. Flame emission, atomic absorption and fluorescence spectrometry

    International Nuclear Information System (INIS)

    Horlick, G.

    1980-01-01

    Six hundred and thirty references are cited in this review. The information in the review is divided into 12 major areas: books, reviews, and bibliographies; fundamental studies in flames; developments in instrumentation; measurement techniques and procedure; flame emission spectrometry; flame atomic absorption spectrometry; flame molecular absorption spectrometry; electrothermal atomization atomic absorption spectroscopy; hydride generation techniques; graphite furnace atomic emission spectrometry; atomic fluorescence spectrometry; and analytical comparisons

  14. Scattering recoil coincidence spectrometry: a new experimental technique for profiling hydrogen isotopes in LOW-Z thin films

    International Nuclear Information System (INIS)

    Forster, J.S.; Leslie, J.R.; Laursen, T.

    1990-01-01

    The new technique for profiling light elements in thin, self-supporting foils, which uses a coincidence measurement over very large solid angles, has been demonstrated experimentally. A beam of 2.0 MeV 4 He particles was used to bombard films of (i) cracked ethylene and (ii) evaporated carbon which was subsequently implanted with 7.5 keV 1 H + ions to a concentration of 10 17 /cm 2 . Plots of E α vs E p clearly show the 1 H distributions in the foil. (author)

  15. Laser ablation inductively coupled plasma mass spectrometry analysis of agricultural soils using the sol-gel technique of pellet preparation

    International Nuclear Information System (INIS)

    Hubova, I.; Hola, M.; Vaculovic, T.; Pinkas, J.; Prokes, L.; Stefan, I.; Kanicky, V.

    2009-01-01

    Full text: Monitoring of metals in agricultural soils is gaining importance as they are accumulated by plants. A LAICPQMS method with Nd:YAG 213 nm laser has been developed for determination of Cr, Ni, Cu, Zn and Pb in soil pellets prepared by the sol-gel technique. LA-ICPMS analysis of archive samples was verified by XRF of wax-soil pellets and ICPMS with nebulization of solutions obtained by total soil decomposition and by analysis of reference materials. Sequention extraction was used for fractionation analysis. (author)

  16. Development of isotope dilution-liquid chromatography/mass spectrometry combined with standard addition techniques for the accurate determination of tocopherols in infant formula

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Joonhee; Jang, Eun-Sil; Kim, Byungjoo, E-mail: byungjoo@kriss.re.kr

    2013-07-17

    Graphical abstract: -- Highlights: •ID-LC/MS method showed biased results for tocopherols analysis in infant formula. •H/D exchange of deuterated tocopherols in sample preparation was the source of bias. •Standard addition (SA)-ID-LC/MS was developed as an alternative to ID-LC/MS. •Details of calculation and uncertainty evaluation of the SA-IDMS were described. •SA-ID-LC/MS showed a higher-order metrological quality as a reference method. -- Abstract: During the development of isotope dilution-liquid chromatography/mass spectrometry (ID-LC/MS) for tocopherol analysis in infant formula, biased measurement results were observed when deuterium-labeled tocopherols were used as internal standards. It turned out that the biases came from intermolecular H/D exchange and intramolecular H/D scrambling of internal standards in sample preparation processes. Degrees of H/D exchange and scrambling showed considerable dependence on sample matrix. Standard addition-isotope dilution mass spectrometry (SA-IDMS) based on LC/MS was developed in this study to overcome the shortcomings of using deuterium-labeled internal standards while the inherent advantage of isotope dilution techniques is utilized for the accurate recovery correction in sample preparation processes. Details of experimental scheme, calculation equation, and uncertainty evaluation scheme are described in this article. The proposed SA-IDMS method was applied to several infant formula samples to test its validity. The method was proven to have a higher-order metrological quality with providing very accurate and precise measurement results.

  17. Application of the mass spectrometry-isotope dilution technique for the determination of uranium contents in rocks

    International Nuclear Information System (INIS)

    Kakazu, M.H.; Iyer, S.S.

    1980-01-01

    Application of the spectrometric isotope dilution technique for the accurate determination of parts per million range of uranium in rock samples is described. The various aspects of the method like sample dissolution, ion exchange separation, mass spectrometric procedures are discussed. A single filament ionization source was employed for the isotope analysis. A carbon reduction method was used to reduce uranium oxide ions to uranium metal ions. The tracer solution for isotope dilution was prepared from National Bureau of Standards uranium isotopic Standard NBS U-970. Uranium contents are meassured for nine rock samples and the values obtained are compared with the uranium values measured by others workers. Errors caused in the uranium determination due to sample splitting problems as well as the incomplete acid digestion of the samples are discussed. (Author) [pt

  18. Experimental study of natural two-phase flow circulation using a visualization technique; Estudo experimental da circulacao natural bifasica utilizando uma tecnica de visualizacao

    Energy Technology Data Exchange (ETDEWEB)

    Vinhas, Pedro A.M., E-mail: Pedro_mvinhas@poli.ufrj.br [Universidade Federal do Rio de Janeiro (UFRJ), Rio de Janeiro, RJ (Brazil). Dept. de Engenharia Nuclear; Faccini, Jose L.H., E-mail: faccini@ien.gov.br [Instituto de Engenharia Nuclear (IEN/CNEN-RJ), Rio de Janeiro, RJ (Brazil); Su, Jian, E-mail: sujian@lasme.coppe.ufrj.br [Coordenacao dos Programas de Pos-Graduacao em Engenharia (COPPE/UFRJ), Rio de Janeiro, RJ (Brazil). Programa de Engenharia Nuclear

    2013-07-01

    This paper presents an experimental study of natural two-phase flow in a circuit that simulates, on a smaller scale, a typical residual heat removal system of passive reactors APWR (Advanced Pressurized Water Reactor). The circuit was formed by a heater, a heat exchanger and piping. The experimental study was the application of a visualization technique, using a high speed camera, for measuring the size and speed of vapor bubbles generated in the heater with different power heating. The camera was positioned in the central region of the pipe connecting the heater to the heat exchanger, where there is a clear passage. The flow of images were processed and analyzed using commercial software that allowed the determination of the length and velocity of the bubbles. The results were then compared with correlations available in literature.

  19. Preparation of mixed oxides (Th,U)O{sub 2}: an evaluation of different techniques; Estudos de diferentes rotas de preparacao de oxidos binarios de torio e uranio

    Energy Technology Data Exchange (ETDEWEB)

    Ayoub, Jamil Mahmoud Said

    1999-07-01

    An evaluation of different ways of obtaining (Th-U)O{sub 2} mixed oxides is described. Coprecipitation, mechanical mixing of uranium and thorium powders, and the sol-gel technique were studied in order to get a large spectrum of knowledge of the process performance. The use of ultrasonic waves for the homogenization of the hydroxide mixture and microwave heating for powder drying was also investigated. Sol-gel showed the best results regarding the specific area for obtained samples. Oxide drying by microwave is an effective method to get mixed oxides for fuel fabrication. Neither coprecipitation nor mechanical mixing of the thorium and uranium oxide powders is suitable for the purpose. The obtained data are less than 70% than those achieved when sol-gel process is performed. Electronic microscopy, X-ray fluorescence and diffraction, thermogravimetry, specific gravidity and specific area determination (BET) used for sample characterization were convenient and accomplished good results. (author)

  20. Determination of {sup 226}Ra by gamma spectrometry: study of packaging vial of sample for analysis; Determinacao de {sup 226}Ra por espectrometria gama: estudo do recipiente de acondicionamento de amostra para analise

    Energy Technology Data Exchange (ETDEWEB)

    Carneiro, Andre Cavalcanti

    2015-07-01

    Determination of radioactivity levels of {sup 226}Ra by gamma spectrometry in a sample is based on measurements of {sup 214}Pb and {sup 214}Bi, daughters of {sup 222}Rn. Because radon is a gas, it can leak from the sample vial or accumulate on the upper empty it. If the vial has any crack, there will be loss of gas, which will cause error in determining the {sup 226}Ra concentration. One possible cause of cracks in the vials, that houses standards and samples, is the radiolysis action in the vial material, usually a polymer. As the demand {sup 226}Ra analysis in different matrices (geological samples, food, plants, etc.) is increasing, it was decided to study some polymer vials available on the market, to verify the feasibility to be used when is applied the analysis method using gamma spectrometry. Four types of polymer vials have been studied. The radiation doses in walls of the vials caused by natural radionuclides present in the sample were simulated using gamma irradiation. Tests, such as compressive strength test and tightness, were applied to the irradiated and non-irradiated vials. First, to verify the effect of radiolysis on the vial material and also if there was {sup 222}Rn diffusion in their walls. These preliminary results pointed out that the acrylic vials are the best option of packaging samples for analysis. This study should be repeated in a larger number of samples for a better evaluation. (author)

  1. Noise-immune cavity-enhanced analytical atomic spectrometry - NICE-AAS - A technique for detection of elements down to zeptogram amounts

    Science.gov (United States)

    Axner, Ove; Ehlers, Patrick; Hausmaninger, Thomas; Silander, Isak; Ma, Weiguang

    2014-10-01

    Noise-immune cavity-enhanced optical heterodyne molecular spectroscopy (NICE-OHMS) is a powerful technique for detection of molecular compounds in gas phase that is based on a combination of two important concepts: frequency modulation spectroscopy (FMS) for reduction of noise, and cavity enhancement, for prolongation of the interaction length between the light and the sample. Due to its unique properties, it has demonstrated unparalleled detection sensitivity when it comes to detection of molecular constituents in the gas phase. However, despite these, it has so far not been used for detection of atoms, i.e. for elemental analysis. The present work presents an assessment of the expected performance of Doppler-broadened (Db) NICE-OHMS for analytical atomic spectrometry, then referred to as noise-immune cavity-enhanced analytical atomic spectrometry (NICE-AAS). After a description of the basic principles of Db-NICE-OHMS, the modulation and detection conditions for optimum performance are identified. Based on a previous demonstrated detection sensitivity of Db-NICE-OHMS of 5 × 10- 12 cm- 1 Hz- 1/2 (corresponding to a single-pass absorbance of 7 × 10- 11 over 10 s), the expected limits of detection (LODs) of Hg and Na by NICE-AAS are estimated. Hg is assumed to be detected in gas phase directly while Na is considered to be atomized in a graphite furnace (GF) prior to detection. It is shown that in the absence of spectral interferences, contaminated sample compartments, and optical saturation, it should be feasible to detect Hg down to 10 zg/cm3 (10 fg/m3 or 10- 5 ng/m3), which corresponds to 25 atoms/cm3, and Na down to 0.5 zg (zg = zeptogram = 10- 21 g), representing 50 zg/mL (parts-per-sextillion, pps, 1:1021) in liquid solution (assuming a sample of 10 μL) or solely 15 atoms injected into the GF, respectively. These LODs are several orders of magnitude lower (better) than any previous laser-based absorption technique previously demonstrated under atmospheric

  2. Application of the coincidence counting technique to DD neutron spectrometry data at the NIF, OMEGA, and Z

    Energy Technology Data Exchange (ETDEWEB)

    Lahmann, B., E-mail: lahmann@mit.edu; Milanese, L. M.; Han, W.; Gatu Johnson, M.; Séguin, F. H.; Frenje, J. A.; Petrasso, R. D. [Massachusetts Institute of Technology, Cambridge, Massachusetts 02139 (United States); Hahn, K. D.; Jones, B. [Sandia National Laboratory, Albuquerque, New Mexico 87123 (United States)

    2016-11-15

    A compact neutron spectrometer, based on a CH foil for the production of recoil protons and CR-39 detection, is being developed for the measurements of the DD-neutron spectrum at the NIF, OMEGA, and Z facilities. As a CR-39 detector will be used in the spectrometer, the principal sources of background are neutron-induced tracks and intrinsic tracks (defects in the CR-39). To reject the background to the required level for measurements of the down-scattered and primary DD-neutron components in the spectrum, the Coincidence Counting Technique (CCT) must be applied to the data. Using a piece of CR-39 exposed to 2.5-MeV protons at the MIT HEDP accelerator facility and DD-neutrons at Z, a significant improvement of a DD-neutron signal-to-background level has been demonstrated for the first time using the CCT. These results are in excellent agreement with previous work applied to DT neutrons.

  3. Application of the coincidence counting technique to DD neutron spectrometry data at the NIF, OMEGA, and Z

    International Nuclear Information System (INIS)

    Lahmann, B.; Milanese, L. M.; Han, W.; Gatu Johnson, M.; Séguin, F. H.; Frenje, J. A.; Petrasso, R. D.; Hahn, K. D.; Jones, B.

    2016-01-01

    A compact neutron spectrometer, based on a CH foil for the production of recoil protons and CR-39 detection, is being developed for the measurements of the DD-neutron spectrum at the NIF, OMEGA, and Z facilities. As a CR-39 detector will be used in the spectrometer, the principal sources of background are neutron-induced tracks and intrinsic tracks (defects in the CR-39). To reject the background to the required level for measurements of the down-scattered and primary DD-neutron components in the spectrum, the Coincidence Counting Technique (CCT) must be applied to the data. Using a piece of CR-39 exposed to 2.5-MeV protons at the MIT HEDP accelerator facility and DD-neutrons at Z, a significant improvement of a DD-neutron signal-to-background level has been demonstrated for the first time using the CCT. These results are in excellent agreement with previous work applied to DT neutrons.

  4. Application of the coincidence counting technique to DD neutron spectrometry data at the NIF, OMEGA, and Z.

    Science.gov (United States)

    Lahmann, B; Milanese, L M; Han, W; Gatu Johnson, M; Séguin, F H; Frenje, J A; Petrasso, R D; Hahn, K D; Jones, B

    2016-11-01

    A compact neutron spectrometer, based on a CH foil for the production of recoil protons and CR-39 detection, is being developed for the measurements of the DD-neutron spectrum at the NIF, OMEGA, and Z facilities. As a CR-39 detector will be used in the spectrometer, the principal sources of background are neutron-induced tracks and intrinsic tracks (defects in the CR-39). To reject the background to the required level for measurements of the down-scattered and primary DD-neutron components in the spectrum, the Coincidence Counting Technique (CCT) must be applied to the data. Using a piece of CR-39 exposed to 2.5-MeV protons at the MIT HEDP accelerator facility and DD-neutrons at Z, a significant improvement of a DD-neutron signal-to-background level has been demonstrated for the first time using the CCT. These results are in excellent agreement with previous work applied to DT neutrons.

  5. Study of an optimization protocol for radiographic techniques in computerized radiology; Estudo de um protocolo de otimizacao para as tecnicas radiograficas em radiologia computadorizada

    Energy Technology Data Exchange (ETDEWEB)

    Abrantes, Marcos Eugenio Silva

    2015-07-01

    This work is designed to produce information for the improvement of image quality to deployment in a radiology department based on previous reviews of the images by questionnaires of acceptance and quality e recognition of the parameters used in chest radiographic techniques. The data collected were divided by male, female, PA and LAT thickness, body mass index, biotypes, anthropomorphic parameters and body evaluation associated with constant voltage and the additional filtration. The results show the predominance of 35 and 40 constants with additional filtration from 0.5 to 1.5 mmAl, voltage in male: (PA and LAT) 86-92 kV and 96-112 kV, female: 85-98 kV and 96-112 kV. The charge applied to the tube for males: (PA and LAT) 5-10 mA.s and 5-16 mA.s, female: (PA and LAT) 6.3-8 mA.s and 9-14 mA.s. Absorbed doses for males: (PA and PF) 0.04-0.17 mGy and 0.03-0.19 mGy and from female (PA and PF) from 0.03-0.22 mGy and 0, 04-0.17 mGy. This procedure can be used in radiology department to implement and acceptance in the quality of images. (author)

  6. One-step derivatization and preconcentration microextraction technique for determination of bisphenol A in beverage samples by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Fontana, Ariel R; Muñoz de Toro, Mónica; Altamirano, Jorgelina C

    2011-04-27

    A simple technique based on ultrasound-assisted emulsification microextraction in situ derivatization (USAEME-ISD) is proposed for the one-step derivatization, extraction, and preconcentration of bisphenol A (BPA) in beverage samples prior to gas chromatography-mass spectrometry (GC-MS) analysis. BPA was in situ derivatized with acetic anhydride and simultaneously extracted and preconcentrated by using USAEME. Variables affecting the extraction efficiency of BPA were evaluated. Under optimal experimental conditions, the detection limit (LOD) was 38 ng L(-1) with a relative standard deviation (RSD) value of 11.6%. The linear working range was 100-1250 ng L(-1), and the coefficient of estimation (r(2)) of the calibration curve was ≥0.9971. The robustness of the proposed methodology was probed by developing a recovery study at two concentrations (125 and 500 ng L(-1)) over different beverage samples. This study led to a satisfactory result achieving recoveries of ≥82%, which showed acceptable robustness for determination of nanograms per liter of BPA in samples of food safety interest.

  7. Ultrasound-assisted extraction technique for establishing selenium contents in breast cancer biopsies by Zeeman-electrothermal atomic absorption spectrometry using multi-injection

    International Nuclear Information System (INIS)

    Lavilla, I.; Mosquera, A.; Millos, J.; Cameselle, J.; Bendicho, C.

    2006-01-01

    A solid-liquid extraction method is developed to establish the contents of selenium in breast cancer biopsies. The method is based on the ultrasound-assisted extraction of selenium from pretreated biopsies prior to Se determination by atomic absorption spectrometry with longitudinal-Zeeman background correction. Fifty-one breast biopsies were collected from the Cies Hospital (Vigo, Spain), 32 of which correspond to tumor tissue and 19 to normal tissue (parenchyma). Difficulties arising from the samples analyzed, i.e. small samples mass (50-100 mg), extremely low Se contents and sample texture modification including tissue hardening due to formaldehyde preservation are addressed and overcome. High intensity sonication using a probe together with addition of hydrogen peroxide succeeded in completely extracting Se from biopsies. The multiple injection technique was useful to tackle the low Se contents present in some biopsies. The detection limit was 25 ng g -1 of Se and the precision, expressed as relative standard deviation, was less than 10%. Se contents ranged from 0.08 to 0.4 μg g -1 for parenchyma samples and from 0.09 to 0.8 μg g -1 for tumor samples. In general, Se levels in tumor biopsies were higher as compared with the adjacent normal tissue in 19 patients by a factor of up to 6. Analytical data confirmed Se accumulation in the breast tumors

  8. Analysis of heavy metals and minerals elements in the turmeric using Total-Reflection X-ray Fluorescence analysis technique and Atomic Absorption Spectrometry

    International Nuclear Information System (INIS)

    Andriamisetra, V.M.Z.

    2014-01-01

    Currently, many studies demonstrate anti-cancer and anti-inflammatory benefits of turmeric. The aims of this work is to perform analysis of metals such as calcium, chromium, manganese, iron, cobalt, nickel, copper, zinc, arsenic, bromine, rubidium, strontium, cadmium and lead in the turmeric collected from various places in Madagascar. The analysis by total reflection X-ray fluorescence technique is used to determine the concentrations of heavy metals, while the atomic absorption spectrometry is used for the determination of trace elements. Analysis results show that the concentration of calcium in the turmeric is very high, its average concentration is 1025.8 mg.kg -1 . The average concentrations of manganese, of copper and of iron are respectively 44.7 mg.kg -1 ; 19.7 mg.kg -1 and 53.6 mg.kg -1 . The average concentrations of zinc, of rubidium and of strontium are respectively 17.3 mg.kg -1 ; 35.2 mg.kg -1 and 21.7 mg.kg -1 [fr

  9. An automated flow injection system for metal determination by flame atomic absorption spectrometry involving on-line fabric disk sorptive extraction technique.

    Science.gov (United States)

    Anthemidis, A; Kazantzi, V; Samanidou, V; Kabir, A; Furton, K G

    2016-08-15

    A novel flow injection-fabric disk sorptive extraction (FI-FDSE) system was developed for automated determination of trace metals. The platform was based on a minicolumn packed with sol-gel coated fabric media in the form of disks, incorporated into an on-line solid-phase extraction system, coupled with flame atomic absorption spectrometry (FAAS). This configuration provides minor backpressure, resulting in high loading flow rates and shorter analytical cycles. The potentials of this technique were demonstrated for trace lead and cadmium determination in environmental water samples. The applicability of different sol-gel coated FPSE media was investigated. The on-line formed complex of metal with ammonium pyrrolidine dithiocarbamate (APDC) was retained onto the fabric surface and methyl isobutyl ketone (MIBK) was used to elute the analytes prior to atomization. For 90s preconcentration time, enrichment factors of 140 and 38 and detection limits (3σ) of 1.8 and 0.4μgL(-1) were achieved for lead and cadmium determination, respectively, with a sampling frequency of 30h(-1). The accuracy of the proposed method was estimated by analyzing standard reference materials and spiked water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  10. Gas chromatography/ion trap mass spectrometry applied for the analysis of triazine herbicides in environmental waters by an isotope dilution technique

    International Nuclear Information System (INIS)

    Cai Zongwei; Wang Dongli; Ma, W.T.

    2004-01-01

    A gas chromatography/ion trap mass spectrometry method was developed for the analysis of simazine, atrazine, cyanazine, as well as the degradation products of atrazine, such as deethylatrazine and deisopropylatrazine in environmental water samples. Isotope dilution technique was applied for the quantitative analysis of atrazine in water at low ng/l levels. One liter of water sample spiked with stable isotope internal standard atrazine-d 5 was extracted with a C 18 solid-phase extraction cartridge. The analysis was performed on an ion trap mass spectrometer operated in MS/MS method. The extraction recoveries were in the range of 83-94% for the triazine herbicides in water at the concentrations of 24, 200, and 1000 ng/l, while poor recoveries were obtained for the degradation products of atrazine. The relative standard deviation (R.S.D.) were within the range of 3.2-16.1%. The detection limits of the method were between 0.75 and 12 ng/l when 1 l of water was analyzed. The method was successfully applied to analyze environmental water samples collected from a reservoir and a river in Hong Kong for atrazine detected at concentrations between 3.4 and 26 ng/l

  11. Development of an analytical method for polycyclic aromatic hydrocarbons in coffee beverages and dark beer using novel high-sensitivity technique of supercritical fluid chromatography/mass spectrometry.

    Science.gov (United States)

    Yoshioka, Toshiaki; Nagatomi, Yasushi; Harayama, Koichi; Bamba, Takeshi

    2018-07-01

    Polycyclic aromatic hydrocarbons (PAHs) are carcinogenic substances that are mainly generated during heating in food; therefore, the European Union (EU) has regulated the amount of benzo[a]pyrene and PAH4 in various types of food. In addition, the Scientific Committee on Food of the EU and the Joint Food and Agriculture Organization/World Health Organization Expert Committee on Food Additives have recommended that 16 PAHs should be monitored. Since coffee beverages and dark beer are roasted during manufacture, monitoring these 16 PAHs is of great importance. On the other hand, supercritical fluid chromatography (SFC) is a separation method that has garnered attention in recent years as a complement for liquid and gas chromatography. Therefore, we developed a rapid high-sensitivity analytical method for the above-mentioned 16 PAHs in coffee beverages and dark beer involving supercritical fluid chromatography/atmospheric pressure chemical ionization-mass spectrometry (SFC/APCI-MS) and simple sample preparation. In this study, we developed a novel analytical technique that increased the sensitivity of MS detection by varying the back-pressure in SFC depending on the elution of PAHs. In addition, analysis of commercially available coffee and dark beer samples in Japan showed that the risk of containing the 16 PAHs may be low. Copyright © 2018 The Society for Biotechnology, Japan. Published by Elsevier B.V. All rights reserved.

  12. Proposta metodológica para a avaliação da técnica da pedalada de ciclistas: estudo de caso Methodological proposal for evaluation of the pedaling technique of cyclists: a case study

    Directory of Open Access Journals (Sweden)

    Fernando Diefenthaeler

    2008-04-01

    Full Text Available No estudo da biomecânica do ciclismo diversas técnicas têm sido utilizadas para descrever e compreender o movimento da pedalada. O objetivo deste estudo é propor uma metodologia para a avaliação de ciclistas sob o ponto de vista das forças aplicadas no pedal. Um ciclista de elite foi avaliado por meio de um protocolo que consistiu em alterar o selim em quatro diferentes posições (deslocado para cima, para baixo, para frente e para trás a partir da posição de referência, especificamente, aquela adotada para treinamento pelo ciclista. A mudança no ajuste do selim foi de 1 cm. A bicicleta do atleta foi acoplada a um ciclossimulador magnético. A carga do teste foi normalizada por um critério fisiológico (segundo limiar ventilatório, simulando o ritmo de prova do atleta. O pedal direito foi substituído por um pedal bidimensional instrumentado para registrar as forças normal e tangencial. A média do impulso angular da força efetiva foi calculada a partir de dez ciclos consecutivos de pedalada. As mudanças na posição do selim modificaram o impulso da força efetiva em relação à posição de referência. Sendo assim, o protocolo é eficaz e pode ser aplicado em diferentes situações.Many techniques have been used in biomechanics to describe the cycling movement. The purpose of this study is to proposal a specific methodology to evaluation the forces applied on the pedal. An experienced elite cyclist was submitted to a protocol which consisted of four different saddle positions (upward, downward, forward, and backward assuming as reference position the one used by the cyclist in training and competition. The displacement of the saddle was of 1cm in all tests. The individual's bicycle was connected to a magnetic cycle simulator. The load was normalized by a physiological criterion (ventilatory threshold, to simulate the cyclist's race rhythm. The right regular pedal was replaced by a 2D instrumented pedal to record the force

  13. Development of an analytical model for the determination of 60Co in aqueous samples by atomic absorption and gamma spectrometry techniques

    International Nuclear Information System (INIS)

    Solis A, N. A.

    2015-01-01

    The applications of the nuclear energy in industry and medicine generate radioactive wastes that must be isolated and confined in order to limit its spread in the biosphere. These types of wastes are generated in hospitals, industry, research centers and nuclear power plants (during de fuel cycle). The radioactive elements (radionuclides) cannot be destroyed by any known method, either chemical or mechanical. Its final destruction is produced by radioactive decay, which makes them stable isotopes, or nuclear transmutation being bombarded with atomic particles. Consequently, the radioactive waste management is to control the radioactive discharges and reduce to tolerable limits, eliminating of effluents and wastes the radionuclides of interest, concentrating them so they can be stored or evacuated so that later not appear in dangerous concentration in the biosphere. In Mexico, the main generators of radioactive wastes are the nuclear power plant of Laguna Verde in Veracruz, Hospitals of the public and private sector, in addition Instituto Nacional de Investigaciones Nucleares (ININ) some institutes and facilities of the UNAM and Instituto Politecnico Nacional (IPN) and industries among others. The aqueous radioactive wastes, particularly those from the nuclear power plants contain traces of cobalt-60. Currently there is no model or analytical technique for the separation of this radionuclide, so it became necessary to develop an analytical model for separation and facilitate their disposal. In this paper was shown that atomic absorption and gamma spectrometry techniques can separate the active concentration of the inactive, which is important because the total concentration can be associated through direct relationships with the wear of metal parts of the nuclear reactor, since the metal alloys of the same reactor containing a fraction of cobalt. Also this analytical and mathematical model that can be reproducible and applicable to full sets of samples and that this

  14. Assessment of the plasma desorption time-of-flight mass spectrometry technique for pesticide adsorption and degradation on 'as-received' treated soil samples.

    Science.gov (United States)

    Thomas, J P; Nsouli, B; Darwish, T; Fallavier, M; Khoury, R; Wehbé, N

    2005-01-01

    The assessment of the plasma desorption time-of-flight mass spectrometry (PD-TOFMS) technique as a tool for direct characterization of pesticides adsorbed on agricultural soil is made for the first time in this study. Pellets of soils impregnated by solutions of three pesticides, namely norflurazon, malathion and oxyfluorfen, as well as deposits of these solutions onto aluminum surfaces, were investigated to this end. The yield values of the most characteristic peaks of the negative ion mass spectra were used to determine both the lowest concentrations detected on soils and limits of detection from thin films. The lowest values on soils are for malathion (1000 ppm range), and the largest for norflurazon (20,000 ppm), which is close to the limit of detection (LOD) found for the pesticide on the aluminum substrate (approximately 0.2 microg . cm(-2)). Different behaviors were observed as a function of time of storage in the ambient atmosphere or under vacuum; norflurazon adsorbed on soil exhibited high stability for a long period of time, and a rapid degradation of malathion with the elapsed time was clearly observed. The behavior of oxyfluorfen was also investigated but segregation processes seem to occur after several days. Although by far less sensitive than conventional methods based on extraction processes and used for real-world analytical applications, this technique is well suited to the study of the transformations occurring at the sample surface. A discussion is presented of the future prospects of such experiments in degradation studies. Copyright (c) 2005 John Wiley & Sons, Ltd.

  15. Analysis of neutral volatile aroma components in Tilsit cheese using a combination of dynamic headspace technique, capillary gas chromatography and mass spectrometry

    International Nuclear Information System (INIS)

    Dillinger, K.H.

    2000-03-01

    Tilsit cheese is made by the influence of lab ferment and starter cultures on milk. The ripening is done by repeated inoculation of the surface of the Tilsit cheese with yeasts and read smear cultures. This surface flora forms the typical aroma of the Tilsit cheese during the ripening process. The aim of the work was to receive general knowledge about the kind and amount of the neutral volatile aroma components of Tilsit cheese. Beyond this the ability of forming aroma components by read smear cultures and the dispersion of these components in cheese was to be examined. The results were intended to evaluate the formation of aroma components in Tilsit cheese. The semi-quantitative analyses of the aroma components of all samples were done by combining dynamic headspace extraction, gas chromatography and mass spectrometry. In this process the neutral volatile aroma components were extracted by dynamic headspace technique, adsorbed on a trap, thermally desorbed, separated by gas chromatography, detected and identified by mass spectrometry. 63 components belonging to the chemical classes of esters, ketones, aldehydes, alcohols and sulfur containing substances as well as aromatic hydrocarbons, chlorinated hydrocarbons and hydrocarbons were found in the analysed cheese samples of different Austrian Tilsit manufacturing plants. All cheese samples showed a qualitative equal but quantitative varied spectrum of aroma components. The cultivation of pure cultures on a cheese agar medium showed all analysed aroma components to be involved in the biochemical metabolism of these cultures. The ability to produce aroma components greatly differed between the strains and it was not possible to correlate this ability with the taxonomic classification of the strains. The majority of the components had a non-homogeneous concentration profile in the cheese body. This was explained by effects of diffusion and temporal and spatial different forming of components by the metabolism of the

  16. Estudo comparativo das medidas ecobiométricas pelos métodos de imersão e contato Comparative study of the biometric measurements made by immersion and contact techniques

    Directory of Open Access Journals (Sweden)

    Airton Leite Kronbauer

    2006-12-01

    Full Text Available OBJETIVO: Comparar os achados clínicos ecobiométricos das medidas dos métodos de imersão e contato. MÉTODOS: O comprimento axial foi medido em 120 ecobiometrias por onda "A" em 60 pacientes com catarata, usando o método de imersão (não-contato e de contato, em amostra pareada. RESULTADOS: A média do comprimento axial encontrada foi de 23,19 mm (DP 1,32 com o método de imersão e 22,93 mm (DP 1,32 com o método de contato, usando a mesma sonda ultra-sônica. A diferença de 0,255 mm (DP 0,3 foi estatisticamente significativa para o nível de 0,01. A diferença deve ser levada em conta quando se estima precisão no cálculo de lente intra-ocular. A média do desvio padrão entre as repetidas medidas no mesmo olho foi de 0,04 com o método de imersão e 0,19 com o método de contato. A diferença de 0,15 foi estatisticamente significativa para o nível de 0,01. A diferença deve ser levada em conta quando se estima precisão na reprodutibilidade da técnica de exame. CONCLUSÃO: Esses dados fornecem parâmetros que podem ser usados para monitorar a prática clínica e para realizar outros estudos.PURPOSE: To compare clinical biometric findings between measurements of immersion technique and contact technique. METHODS: Axial length was measured by A-scan in 120 medical examinations in 60 patients with cataract using a non-contact (immersion and a contact technique in paired-samples by ultrasound. RESULTS: The mean axial length was found to be 23.19 mm (SD 1.32 with the immersion technique and 22.93 mm (SD 1.32 with the contact technique, using the same transducer probe. The difference of 0.255 mm (SD 0.3 was significant at the 0.01 level. The difference should be taken into account when evaluating the accuracy of IOL calculation. The mean standard deviation between recurrent measures in same eye was found to be 0.04 with the immersion technique and 0.19 with the contact technique. The difference of 0.15 was significant at the 0.01 level

  17. Estudo comparativo das técnicas radiográficas e doses entre o Brasil e a Austrália Comparison between radiological techniques and doses used in Brazil and in Australia

    Directory of Open Access Journals (Sweden)

    Ana Cecília Pedrosa de Azevedo

    2005-09-01

    Full Text Available OBJETIVO: O objetivo deste trabalho é fazer um estudo comparativo das técnicas radiográficas entre o Brasil e a Austrália e avaliar as doses de radiação para os exames radiológicos mais comuns. MATERIAIS E MÉTODOS: A dose de entrada na pele (DEP e a dose efetiva (DE foram obtidas com o uso do programa DoseCal. Em ambos os países, o estudo foi realizado em hospitais de grande porte da rede pública. Quatro tipos de exames foram avaliados: tórax, abdome, pelve e coluna torácica em três projeções (ântero-posterior, póstero-anterior e lateral. Na Austrália, todos os equipamentos são digitais e operam no sistema PACS. No Brasil, os aparelhos são convencionais. RESULTADOS: Os valores médios da DEP e da DE são consideravelmente mais altos no Brasil, exceto para os exames de tórax, cujos resultados indicaram índices menores. As maiores diferenças encontradas foram para os exames de pelve (26 vezes maior no Brasil e de coluna torácica (43 vezes maior no Brasil. O mesmo acontece para os valores da DE. CONCLUSÃO: Nos hospitais australianos, os programas de controle e garantia de qualidade (PCGQ fazem parte da rotina nos serviços de radiologia. Contam com equipamentos digitais de última geração e os serviços possuem uma equipe de física médica atuante. Esse conjunto de iniciativas resulta na produção de imagens radiográficas de alta qualidade, com baixas doses e índices de rejeição próximos a zero. Tais resultados apontam para a necessidade de se estimular a implantação de PCGQ em toda a rede hospitalar brasileira. No entanto, analisando os resultados de DEP nos exames de tórax, concluímos que doses baixas também são possíveis no Brasil se forem empregadas técnicas radiográficas adequadas.OBJECTIVE: To compare radiological techniques used in Brazil and in Australia, and to evaluate radiation doses of the most common x-ray procedures. MATERIALS AND METHODS: The entrance skin dose (ESD and the effective dose

  18. New analytical technique for establishing the quality of Soil Organic Matter affected by a wildfire. A first approach using Fourier transform ion cyclotron resonance mass spectrometry

    Science.gov (United States)

    Jiménez-Morillo, Nicasio T.; González-Pérez, José A.; Waggoner, Derek C.; Almendros, Gonzalo; González-Vila, Francisco J.; Hatcher, Patrick G.

    2016-04-01

    Introduction: Fire is one of the most important modulator factors of the environment and the forest. It is able to induce chemical and biological shifts and these, in turn, can alter the physical properties of soil. Generally, fire affects the most reactive fraction, soil organic matter (SOM) (González-Pérez et al., 2004) resulting in changes to several soil properties and functions. To study changes in SOM following a wildfire, researchers can count on several traditional as well as new analytical techniques. One of the most recently employed techniques is Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR-MS). This new powerful ultra-high resolution mass spectral technique, together with graphic interpretation tools such as van Krevelen diagrams (Kim et al, 2003), may be used to shed light on alterations caused by the burning of SOM. The objective of this research is to study fire impacts on SOM, using a sandy soil collected under a Cork oak (Quercus suber) in Doñana National Park, Southwest Spain. that was affected by a wildfire in August 2012. Methods: The impact of fire on SOM was studied in various different sieve fractions (coarse, 1-2 mm, and fine, tannins, lignin, lipids, protein and carbohydrate derived. The unburnt SOM in the coarse fraction was mainly composed of compounds with a high intensity in the tannin-like, lignin-like and carbohydrate-like regions of the van Krevelen diagram, whereas the SOM in the fine fraction showed a high intensity in the lipid-like and protein-like regions. These results suggest that the SOM in the coarse fraction was less altered than that of the fine fraction; the latter believed to be subjected to higher microbial activity. We suggest that the observed changes occurs via a methylation process, producing a SOM that is highly humified (Jiménez-Morillo et al., 2014). The SOM in the coarse fraction affected by fire, showed a high relative intensity of chemical compounds in the carbohydrate-like and

  19. Forensic Mass Spectrometry

    Science.gov (United States)

    Hoffmann, William D.; Jackson, Glen P.

    2015-07-01

    Developments in forensic mass spectrometry tend to follow, rather than lead, the developments in other disciplines. Examples of techniques having forensic potential born independently of forensic applications include ambient ionization, imaging mass spectrometry, isotope ratio mass spectrometry, portable mass spectrometers, and hyphenated chromatography-mass spectrometry instruments, to name a few. Forensic science has the potential to benefit enormously from developments that are funded by other means, if only the infrastructure and personnel existed to adopt, validate, and implement the new technologies into casework. Perhaps one unique area in which forensic science is at the cutting edge is in the area of chemometrics and the determination of likelihood ratios for the evaluation of the weight of evidence. Such statistical techniques have been developed most extensively for ignitable-liquid residue analyses and isotope ratio analysis. This review attempts to capture the trends, motivating forces, and likely impact of developing areas of forensic mass spectrometry, with the caveat that none of this research is likely to have any real impact in the forensic community unless: (a) The instruments developed are turned into robust black boxes with red and green lights for positives and negatives, respectively, or (b) there are PhD graduates in the workforce who can help adopt these sophisticated techniques.

  20. Preface Miniaturization and Mass Spectrometry

    NARCIS (Netherlands)

    Unknown, [Unknown; le Gac, Severine; le Gac, S.; van den Berg, Albert; van den Berg, A.

    2009-01-01

    Miniaturization and Mass Spectrometry illustrates this trend and focuses on one particular analysis technique, mass spectrometry whose popularity has "dramatically" increased in the last two decades with the explosion of the field of biological analysis and the development of two "soft" ionization

  1. Técnicas da carta-perdida como instrumento de pesquisa social: um estudo sobre preconceito e ajuda The lost letter technique as a social research instrument: a study of prejudice and helping

    Directory of Open Access Journals (Sweden)

    Abelardo Vinagre da Silva

    1998-01-01

    Full Text Available A técnica da carta perdida foi adaptada para o contexto cultural brasileiro. Trezentas cartas endereçadas e seladas, foram colocadas "por engano", simulando perda, nos pára-brisas de veículos em dois estacionamentos. Um bilhete anexo explicava que o autor se desencontrara do amigo, "dono do carro". O bilhete variou, dando a entender que seu autor era masculino ou feminino (fator 1; tinha características pessoais distintas: homossexual, negro ou grupo controle (fator 2; permitindo a possibilidade de contatos telefônicos, ou não (fator 3, num delineamento 2 x 3 x 2. Quem encontrava a carta, podia enviá-la (comportamento pró-social ou descartá-la. Sessenta e um por cento das cartas foram enviadas. Nenhuma diferença significativa foi encontrada em função das características dos três grupos (controle, negro ou homossexual, de gênero, da interação destes fatores. A possibilidade de telefonar para o remetente, aumentou significativamente o envio de cartas. A técnica mostrou-se promissora por possibilitar, enquanto instrumento não-reativo, o estudo de preconceito e ajuda.The lost-letter technique was adapted to the cultural context of Brazil. Three hundred stamped and addressed letters were placed "by accident", i.e., simulating loss, on the wind shields of private cars in two large parking areas. A attached note explained that the author had missed the owner of the car. The note varied such that the author appeared to be either male or female (Factor 1, have certain personal characteristics, such as being black, homosexual, or control group (Factor 2, and allowed for telephone contact or not with the author (Factor 3 in a 2 x 3 x 2 experimental design. The finder of the letter could either (a post the letter (pro-social behavior or (b ignore it. 60.7% of the letters were posted. No significant difference was found in terms of sex or personal characteristics, nor interaction between these two factors. Being able to telephone the

  2. Development and application of compact denuder sampling techniques with in situ derivatization followed by gas chromatography-mass spectrometry for halogen speciation in volcanic plumes

    Science.gov (United States)

    Rüdiger, Julian; Bobrowski, Nicole; Hoffmann, Thorsten

    2015-04-01

    Volcanoes are a large source for several reactive atmospheric trace gases including sulphur and halogen containing species. The detailed knowledge of volcanic plume chemistry can give insights into subsurface processes and can be considered as a useful geochemical tool for monitoring of volcanic activity, especially halogen to sulphur ratios (e.g. Bobrowski and Giuffrida, 2012; Donovan et al., 2014). The reactive bromine species bromine monoxide (BrO) is of particular interest, because BrO as well as SO2 are readily measurable by UV spectrometers at a safe distance. Furthermore it is formed in the plume by a multiphase reaction mechanism under depletion of ozone in the plume. The abundance of BrO changes as a function of the reaction time and therefore distance from the vent as well as the spatial position in the plume. Due to the lack of analytical approaches for the accurate speciation of certain halogens (HBr, Br2, Br, BrCl, HOBr etc.) there are still uncertainties about the magnitude of volcanic halogen emissions and in particular their specificationtheir species and therefore also in the understanding of the bromine chemistry in volcanic plumes (Bobrowski et al., 2007). In this study, the first application of a 1,3,5-trimethoxybenzene (1,3,5-TMB)-coated gas diffusion denuder (Huang and Hoffmann, 2008) on volcanic gases proved to be suitable to collect selectively gaseous bromine species with oxidation states of +1 or 0 (Br2 and BrO(H)), while being ignorant to HBr (OS -1). The reaction of 1,3,5-TMB with bromine gives 1-bromo-2,4,6-trimethoxybenzene (1-bromo-2,4,6-TMB) - other halogens give corresponding products. The diffusion denuder technique allows sampling of gaseous compounds exclusively without collecting particulate matter. Choosing a flow rate of 500 mL-min-1 and a denuder length of 0.5 m a nearly quantitative collection efficiency was achieved. Solvent elution of the derivatized analytes and subsequent analysis with gas chromatography

  3. Aplicação de técnicas multivariadas no estudo da divergência genética em cana-de-açúcar Application of multivariate techniques in the study of genetic diversity in sugarcane

    Directory of Open Access Journals (Sweden)

    João de Andrade Dutra Filho

    2011-03-01

    Full Text Available Estudos sobre divergência genética são importantes na identificação de genitores potenciais para a obtenção de novos indivíduos com maior efeito heterótico. Em cana-de-açúcar esses estudos assumem fundamental importância, pois com o passar do tempo as variedades comerciais devem ser substituídas de suas áreas de cultivo, devido a sérios declínios agronômicos e industriais ocasionados pela degenerescência varietal. Sendo assim, o objetivo deste trabalho foi avaliar a divergência genética em progênies de cana-de-açúcar, através de técnicas multivariadas, com base em oito caracteres agroindustriais. O trabalho foi conduzido na área agrícola da Usina Santa Tereza, município de Goiana (PE, durante o ano agrícola 2007/2008. Foi utilizado o delineamento experimental casualizado em blocos completos com cinco repetições. As variáveis analisadas foram: toneladas de pol por hectare, toneladas de cana por hectare, fibra, pol % corrigida, pureza, teor de sólidos solúveis, açúcares redutores e açúcar total recuperável. Após análise de variância e estimação de parâmetros genéticos, a distância generalizada de Mahalanobis foi calculada para quantificar a dissimilaridade. Foram utilizados o método hierárquico de ligações médias (UPGMA e o método de otimização de Tocher. O coeficiente de herdabilidade média foi de alta magnitude para as variáveis TPH e TCH, indicando possibilidade de sucesso na seleção com base nesses caracteres. A metodologia aplicada permitiu a identificação de progênies de maior divergência genética proporcionando ao fitomelhoramento canavieiro da RIDESA sugestão de cruzamentos a serem realizados futuramente.This study aimed to evaluate the genetic diversity in progenies of sugar cane by means of multivariate techniques based on eight agroindustrial traits. The work was carried out in the agricultural area of Usina Santa Teresa, Goiana (PE, during the agricultural year 2007

  4. Mass spectrometry in clinical chemistry

    International Nuclear Information System (INIS)

    Pettersen, J.E.

    1977-01-01

    A brief description is given of the functional elements of a mass spectrometer and of some currently employed mass spectrometric techniques, such as combined gas chromatography-mass spectrometry, mass chromatography, and selected ion monitoring. Various areas of application of mass spectrometry in clinical chemistry are discussed, such as inborn errors of metabolism and other metabolic disorders, intoxications, quantitative determinations of drugs, hormones, gases, and trace elements, and the use of isotope dilution mass spectrometry as a definitive method for the establishment of true values for concentrations of various compounds in reference sera. It is concluded that mass spectrometry is of great value in clinical chemistry. (Auth.)

  5. Proposta metodológica para a avaliação da técnica da pedalada de ciclistas: estudo de caso Methodological proposal for evaluation of the pedaling technique of cyclists: a case study

    OpenAIRE

    Fernando Diefenthaeler; Rodrigo Rico Bini; Eduardo Nabinger; Orlando Laitano; Felipe Pivetta Carpes; Carlos Bolli Mota; Antônio Carlos Stringhini Guimarães

    2008-01-01

    No estudo da biomecânica do ciclismo diversas técnicas têm sido utilizadas para descrever e compreender o movimento da pedalada. O objetivo deste estudo é propor uma metodologia para a avaliação de ciclistas sob o ponto de vista das forças aplicadas no pedal. Um ciclista de elite foi avaliado por meio de um protocolo que consistiu em alterar o selim em quatro diferentes posições (deslocado para cima, para baixo, para frente e para trás) a partir da posição de referência, especificamente, aque...

  6. Hálux valgo: estudo comparativo entre duas técnicas cirúrgicas de osteotomia proximal de adição Hallux valgus: comparative study between two surgical techniques of proximal addition osteotomy

    Directory of Open Access Journals (Sweden)

    Luiz Carlos Ribeiro Lara

    2012-12-01

    Full Text Available OBJETIVO: Comparar clínica e radiograficamente os resultados da correção do hálux valgo, através de duas técnicas de osteotomia de adição: uma utilizando-se da exostose ressecada e outra, mediante a fixação com placa para cunha de adição. MÉTODOS: Avaliamos 24 pés em 19 pacientes, com média de idade de 51,3 anos, portadores de hálux valgo, com seguimento médio de 50,1 meses. Submeteram-se à técnica de osteotomia de adição com exostose óssea (OAEO 13 pés e à osteotomia de adição com placa para cunha de adição (OPCA 11 pés. Foram avaliados no pré e pós operatório o escore AOFAS, os ângulos intermetatársicos 1 e 2, e ângulo de valgismo do hálux. RESULTADOS: Na técnica OAEO a média no pré-operatório do AOFAS foi 46,6 pontos, AIM 14º e AVH 32º, enquanto no pós-operatório AOFAS 81,3 pontos, AIM 9º e AVH 25ºcom 92,3% de resultados satisfatórios. Na técnica OPCA a média no pré-operatório do AOFAS foi 42,1 pontos, AIM 15º e AVH 29º, enquanto no pós-operatório AOFAS 77,4 pontos, AIM 11º e AMF 23º com 81,8% de resultados satisfatórios. CONCLUSÕES: Ambas as técnicas cirúrgicas mostraram-se eficazes no tratamento do hálux valgo, clínica e radiograficamente, sem diferença estatística entre elas. Nível de evidência III, Estudo retrospectivo comparativo.OBJECTIVE: To clinically and radiographically compare the results of treatment of hallux valgus, by two addition osteotomy techniques: one using resected exostosis, and the other using a plate fixation for addition wedge. METHODS: We evaluated 24 feet of 19 patients, mean age 51.3 years, affected by hallux valgus, with a mean follow-up of 50.1 months. 13 feet underwent addition osteotomy with resected exostosis (AORE and 11 patients (11 feet underwent addition osteotomy with plate (AOP. The AOFAS score, intermetatarsal 1 and 2 angles, and hallux valgus angle were evaluated before and after surgery. RESULTS: In the AORE technique, the mean

  7. Estudos de atmosfera

    Directory of Open Access Journals (Sweden)

    Carlos Eduardo Riccioppo

    2016-11-01

    Full Text Available Joker e Estudos de balística possuíam formas distintas dos cadernos ou livros quando foram exibidos pela primeira vez, na mostra Dual Overdrive. De algum modo, o flagrante das imagens dos cartazes da campanha política parisiense e daquelas cusparadas sobre o asfalto era preservado no modo como eram mostrados os trabalhos, que repunham não apenas a orientação espacial dos objetos fotografados, mas, igualmente, sua escala: Joker apresentava-se na parede, em dimensões relativamente próximas às dos cartazes lambe-lambe que retratavam; e Estudos de balística, no chão da galeria, também com ampliação suficiente para que se tivesse a impressão de que se tratava de imagens “em tamanho real”.

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

    Science.gov (United States)

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

    2015-09-03

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

  9. Determination of mercury species by the diffusive gradient in thin film technique and liquid chromatography – atomic fluorescence spectrometry after microwave extraction

    Energy Technology Data Exchange (ETDEWEB)

    Pelcová, Pavlína, E-mail: pavlina.pelcova@mendelu.cz; Dočekalová, Hana, E-mail: hana.docekalova@mendelu.cz; Kleckerová, Andrea, E-mail: andrea.kleckerova@mendelu.cz

    2015-03-25

    Highlights: • DGT–MAE–LC–CV-AFS method was developed for determination of four mercury species. • The microwave extraction was used for isolation of mercury species from resin gels. • Optimized DGT–MAE–LC–CV-AFS method provides low detection limits (13–38 ng L{sup −1}). • The diffusion coefficients of four mercury species were simultaneously determined. - Abstract: A diffusive gradient in thin films technique (DGT) was combined with liquid chromatography (LC) and cold vapor atomic fluorescence spectrometry (CV-AFS) for the simultaneous quantification of four mercury species (Hg{sup 2+}, CH{sub 3}Hg{sup +}, C{sub 2}H{sub 5}Hg{sup +}, and C{sub 6}H{sub 5}Hg{sup +}). After diffusion through an agarose diffusive layer, the mercury species were accumulated in resin gels containing thiol-functionalized ion-exchange resins (Duolite GT73, and Ambersep GT74). A microwave-assisted extraction (MAE) in the presence of 6 M HCl and 5 M HCl (55 °C, 15 min) was used for isolation of mercury species from Ambersep and Duolite resin gels, respectively. The extraction efficiency was higher than 95.0% (RSD 3.5%). The mercury species were separated with a mobile phase containing 6.2% methanol + 0.05% 2-mercaptoethanol + 0.02 M ammonium acetate with a stepwise increase of methanol content up to 80% in the 16th min on a Zorbax C18 reverse phase column. The LODs of DGT–MAE–LC–CV-AFS method were 38 ng L{sup −1} for CH{sub 3}Hg{sup +}, 13 ng L{sup −1} for Hg{sup 2+}, 34 ng L{sup −1} for C{sub 2}H{sub 5}Hg{sup +} and 30 ng L{sup −1} for C{sub 6}H{sub 5}Hg{sup +} for 24 h DGT accumulation at 25 °C.

  10. Mass spectrometry in oceanography

    International Nuclear Information System (INIS)

    Aggarwal, Suresh K.

    2000-01-01

    Mass spectrometry plays an important role in oceanography for various applications. Different types of inorganic as well as organic mass spectrometric techniques are being exploited world-wide to understand the different aspects of marine science, for palaeogeography, palaeoclimatology and palaeoecology, for isotopic composition and concentrations of different elements as well as for speciation studies. The present paper reviews some of the applications of atomic mass spectrometric techniques in the area of oceanography

  11. Comparative study of two autogenous graft techniques using piezosurgery for sinus lifting Estudo comparativo de duas técnicas de enxerto autógeno utilizando piezocirurgia para levantamento de seio maxilar

    Directory of Open Access Journals (Sweden)

    Geraldo Prestes de Camargo Filho

    2010-12-01

    Full Text Available PURPOSE: Maxillary sinus lifting is a technique, in which, a possible complication is sinus membrane perforation. The aim of this study was to compare two techniques using ultrasound surgery to perform autogenous graft for maxillary sinus lifting. METHODS: Ten rabbits were used in the study, one of them did not undergo surgery. The other nine rabbits had their maxillary sinuses filled with autogenous bone grafts collected from the external skull diploe in particulate form on the right side, and shaved on the left side, both with ultrasonic device. Data on bone density in left and right maxillary sinus, obtained by computed tomography in transverse and longitudinal sections, recorded 90 days after the grafts, were statistically compared. RESULTS: There were no statistically significant differences between the two techniques that used shaved and particulate bone collected by means of ultrasonic device from rabbit skulls. CONCLUSION: Assessment of operative procedures led to the conclusion that piezoelectric ultrasound was shown to be a safe tool in the surgical approach to the maxillary sinus of rabbits, allowing sinus membrane integrity to be maintained during surgical procedures.OBJETIVO: A técnica de levantamento de seio maxilar apresenta como possível complicação a perfuração da membrana sinusal. O presente trabalho teve por objetivo comparar duas técnicas que utilizam a cirurgia ultrassônica para realização de enxerto autógeno para levantamento de seio maxilar. MÉTODOS: Dez coelhos foram utilizados no estudo, sendo que um deles não foi submetido a procedimento cirúrgico. Os nove coelhos operados tiveram os seios maxilares preenchidos com enxertos autógenos coletados de díploe externa de calota craniana, nas formas particulado do lado direito e raspado do lado esquerdo, ambos com aparelho ultrassônico. Os dados de densidade óssea nos seios maxilares esquerdo e direito, obtidos por meio de tomografia computadorizada nos

  12. The Use of Atmospheric Pressure Chemical Ionization Mass Spectrometry with High Performance Liquid Chromatography and Other Separation Techniques for Identification of Triacylglycerols

    Czech Academy of Sciences Publication Activity Database

    Řezanka, Tomáš; Sigler, Karel

    2007-01-01

    Roč. 3, - (2007), s. 252-271 ISSN 1573-4110 R&D Projects: GA ČR GA203/06/0219 Institutional research plan: CEZ:AV0Z50200510 Keywords : triacylglycerols * atmospheric presssure chemical ionization * mass spectrometry Subject RIV: EE - Microbiology, Virology Impact factor: 1.815, year: 2007

  13. Screening and confirmation criteria for hormone residue analysis using liquid chromatography accurate mass time-of-flight, Fourier transform ion cyclotron resonance and orbitrap mass spectrometry techniques

    NARCIS (Netherlands)

    Nielen, M.W.F.; Engelen, M.C. van; Zuiderent, R.; Ramaker, R.

    2007-01-01

    An emerging trend is recognised in hormone and veterinary drug residue analysis from liquid chromatography tandem mass spectrometry (LC/MS/MS) based screening and confirmation towards accurate mass alternatives such as LC coupled with time-of-flight (TOF), Fourier transform ion cyclotron resonance

  14. Mass spectrometry imaging of illicit drugs in latent fingerprints by matrix-free and matrix-assisted desorption/ionization techniques.

    Czech Academy of Sciences Publication Activity Database

    Škríba, Anton; Havlíček, Vladimír

    2018-01-01

    Roč. 24, č. 1 (2018), s. 124-128 ISSN 1469-0667 R&D Projects: GA MŠk(CZ) LO1509; GA ČR(CZ) GA16-20229S Institutional support: RVO:61388971 Keywords : MALDI * Mass spectrometry imaging * NALDI Subject RIV: CB - Analytical Chemistry, Separation OBOR OECD: Analytical chemistry Impact factor: 1.022, year: 2016

  15. Tissue-specific metabolite profiling of Cyperus rotundus L. rhizomes and (+)-nootkatone quantitation by laser microdissection, ultra-high-performance liquid chromatography-quadrupole time-of-flight mass spectrometry, and gas chromatography-mass spectrometry techniques.

    Science.gov (United States)

    Jaiswal, Yogini; Liang, Zhitao; Guo, Ping; Ho, Hing-Man; Chen, Hubiao; Zhao, Zhongzhen

    2014-07-23

    Cyperus rotundus L. is a plant species commonly found in both India and China. The caused destruction of this plant is of critical concern for agricultural produce. Nevertheless, it can serve as a potential source of the commercially important sesquiterpenoid (+)-nootkatone. The present work describes comparative metabolite profiling and (+)-nootkatone content determination in rhizome samples collected from these two countries. Laser dissected tissues, namely, the cortex, hypodermal fiber bundles, endodermis, amphivasal vascular bundles, and whole rhizomes were analyzed by ultra-high-performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UHPLC-QTOF MS). Gas chromatography-mass spectrometry (GC-MS) analysis was used for profiling of essential oil constituents and quantitation of (+)-nootkatone. The content of (+)-nootkatone was found to be higher in samples from India (30.47 μg/10 g) compared to samples from China (21.72 μg/10 g). The method was validated as per International Conference on Harmonisation (ICH) guidelines (Q2 R1). The results from this study can be applied for quality control and efficient utilization of this terpenoid-rich plant for several applications in food-based industries.

  16. Técnica de implante subpeitoral para tratamento de infecção de loja de marcapasso: estudo inicial Subpectoral pacemaker implantation technique for treatment of generator pocket infection: initial study

    Directory of Open Access Journals (Sweden)

    Acrisio Sales VALENTE

    2001-03-01

    Full Text Available Introdução/Objetivo: O implante de marcapasso cardíaco definitivo é um procedimento caracterizado por um baixo índice de complicações. No entanto, a infecção, principalmente a de loja de fonte geradora, caracteriza-se como uma das complicações mais comuns, com incidências variando entre 1-5% na maioria dos centros. Diversas abordagens terapêuticas para o tratamento desta afecção vêm sendo descritas com resultados controversos. Observa-se, entretanto, uma tendência a melhores resultados, com menores índices de falência de tratamento ou reinfecção, nas abordagens mais agressivas, estas sempre relacionadas à alta morbidade e a altos custos finais. Com base nos princípios já bem descritos do poder bactericida dos flaps musculocutâneos associados à antibioticoterapia na esterilização de áreas pouco vascularizadas infectadas, foi desenvolvida e avaliada neste estudo inicial a técnica de implante subpeitoral para o tratamento dos casos de infecção restrita de loja de fonte geradora, objetivando-se menores morbidades e custos com, bons resultados. Casuística e Método: Foi considerado no presente estudo o período de janeiro de 1996 a março de 2000 onde foram realizados 574 procedimentos, entre implantes e trocas de fontes geradoras, na Santa Casa de São Paulo, com um índice de infecção de 1,11% (6 casos e 2 casos de extrusão de fonte geradora sem infecção aparente. Quatro casos tratavam-se de infecção exclusiva de loja de fonte e em 2 casos houve comprometimento sistêmico com sepse. Os germes infectantes foram S.aureus, S.epidermidis e Pseudomonas. Foi utilizada como abordagem terapêutica para todos os casos sem comprometimento sistêmico a técnica de implante subpeitoral da mesma fonte geradora associada à antibioticoterapia específica. Resultados: Não houve óbitos, casos de reinfecção ou falência de tratamento nos pacientes submetidos à técnica. O tempo médio de internação foi 7,3 dias. O

  17. Estudos de atmosfera

    OpenAIRE

    Carlos Eduardo Riccioppo

    2016-01-01

    Joker e Estudos de balística possuíam formas distintas dos cadernos ou livros quando foram exibidos pela primeira vez, na mostra Dual Overdrive. De algum modo, o flagrante das imagens dos cartazes da campanha política parisiense e daquelas cusparadas sobre o asfalto era preservado no modo como eram mostrados os trabalhos, que repunham não apenas a orientação espacial dos objetos fotografados, mas, igualmente, sua escala: Joker apresentava-se na parede, em dimensões relativamente próximas às d...

  18. um estudo de caso

    OpenAIRE

    Costa, Cátia Filipa Pereira da

    2011-01-01

    Dissertação apresentada à Universidade Fernando Pessoa como parte dos requisitos para obtenção do grau de Mestre em Psicologia Jurídica As situações de abuso sexual de crianças nas quais o perpetrador pertence ao sexo feminino obtiveram ao longo dos últimos anos um acrescido reconhecimento por parte da comunidade científica, evidenciado pelo significativo incremento das investigações no âmbito desta temática consistindo na sua maioria estudos de caso. Um conjunto de particularidades encont...

  19. Comparison of different mass spectrometry techniques in the measurement of L-[ring-13C6]phenylalanine incorporation into mixed muscle proteins

    Science.gov (United States)

    Zabielski, Piotr; Ford, G. Charles; Persson, X. Mai; Jaleel, Abdul; Dewey, Jerry D.; Nair, K Sreekumaran

    2013-01-01

    Precise measurement of low enrichment of stable isotope labeled amino-acid tracers in tissue samples is a prerequisite in measuring tissue protein synthesis rates. The challenge of this analysis is augmented when small sample size is a critical factor. Muscle samples from human participants following an 8 hour intravenous infusion of L-[ring-13C6]phenylalanine and a bolus dose of L-[ring-13C6]phenylalanine in a mouse were utilized. Liquid Chromatography tandem mass spectrometry (LC/MS/MS), Gas Chromatography tandem mass spectrometry (GC/MS/MS) and Gas Chromatography/Mass spectrometry (GC/MS) were compared to the Gas Chromatography-Combustion-Isotope Ratio mass spectrometry (GC/C/IRMS), to measure mixed muscle protein enrichment of [ring13C6]phenylalanine enrichment. The sample isotope enrichment ranged from 0.0091 to 0.1312 Molar Percent excess (MPE). As compared with GC/C/IRMS, LC/MS/MS, GC/MS/MS and GC/MS showed coefficients of determination of R2 = 0.9962 and R2 = 0.9942, and 0.9217 respectively. However, the precision of measurements (coefficients of variation) for intra-assay are 13.0%, 1.7%, 6.3% and 13.5% and for inter-assay are 9.2%, 3.2%, 10.2% and 25% for GC/C/IRMS, LC/MS/MS, GC/MS/MS and GC/MS respectively. The muscle sample sizes required to obtain these results were 8μg, 0.8μg, 3μg and 3μg for GC/C/IRMS, LC/MS/MS, GC/MS/MS, and GC/MS respectively. We conclude that LC/MS/MS is optimally suited for precise measurements of L-[ring-13C6]phenylalanine tracer enrichment in low abundance and in small quantity samples. PMID:23378099

  20. Mass spectrometry

    DEFF Research Database (Denmark)

    Nyvang Hartmeyer, Gitte; Jensen, Anne Kvistholm; Böcher, Sidsel

    2010-01-01

    Matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF MS) is currently being introduced for the rapid and accurate identification of bacteria. We describe 2 MALDI-TOF MS identification cases - 1 directly on spinal fluid and 1 on grown bacteria. Rapidly obtained...

  1. The application of an emerging technique for protein-protein interaction interface mapping: the combination of photo-initiated cross-linking protein nanoprobes with mass spectrometry

    Czech Academy of Sciences Publication Activity Database

    Ptáčková, Renata; Ječmen, Tomáš; Novák, Petr; Šulc, Miroslav; Hudeček, J.; Stiborová, M.

    2014-01-01

    Roč. 15, č. 6 (2014), s. 9224-9241 E-ISSN 1422-0067 R&D Projects: GA ČR(CZ) GAP207/12/0627 Grant - others:Universita Karlova(CZ) 903413; Magistrát hlavního města Prahy(CZ) CZ.2.16/3.1.00/24023; UNCE(BE) 204025/2012 Institutional support: RVO:61388971 Keywords : nanoprobes * mass spectrometry * protein-protein interactions Subject RIV: CE - Biochemistry Impact factor: 2.862, year: 2014

  2. Applicability study of using in-situ gamma-ray spectrometry technique for 137Cs and 210Pbex inventories measurement in grassland environments

    International Nuclear Information System (INIS)

    Li Junjie; Li Yong; Wang Yanglin; Wu Jiansheng

    2010-01-01

    In-situ measurement of fallout radionuclides 137 Cs and 210 Pb ex has the potential to assess soil erosion and sedimentation rapidly. In this study, inventories of 137 Cs and 210 Pb ex in the soil of Inner Mongolia grassland were measured using an In-situ Object Counting System (ISOCS). The results from the field study indicate that in-situ gamma-ray spectrometry has the following advantages over traditional laboratory measurements: no extra time is required for sample collection, no reference inventories are required, more economic, prompt availability of the results, the ability to average radionuclide inventory over a large area, and high precision.

  3. Study of radionuclide and element characterization of Angola marine sediment using low background gamma spectrometry and instrumental neutron activation analysis techniques

    International Nuclear Information System (INIS)

    Teixeira, M.C.P.; Vuong Huu Tan; Truong Y; Ho Manh Dung; Le Nhu Sieu; Cao Dong Vu; Nguyen Thanh Binh

    2007-01-01

    The concentrations of radionuclides and chemical elements in Angola marine sediment samples were determined by using low background gamma (LBG) spectrometry and instrumental neutron activation analysis (INAA). The combination of radionuclide and elemental concentration values yielded synergy in the validation of analytical data and identification of sediment sources modeled by multivariate factor analysis. Varimax rotation factor analysis based on the elemental concentrations revealed five sources contributed to the sediment composition, i.e. crustal, sea-salt, industrial, coal-related and Se-related sources. (author)

  4. Extension of the analytical window for characterizing aromatic compounds in oils using a comprehensive suite of high-resolution mass spectrometry techniques and double bond equivalence versus carbon number plot

    Science.gov (United States)

    Cho, Yunju; Birdwell, Justin E.; Hur, Manhoi; Lee, Joonhee; Kim, Byungjoo; Kim, Sunghwan

    2017-01-01

    In this study, comprehensive two-dimensional (2D) gas chromatography–mass spectrometry (GC–MS), atmospheric pressure photoionization (APPI) quadrupole-Orbitrap mass spectrometry (MS), and Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS) were used to study the aromatic fractions of crude oil and oil shale pyrolysates (shale oils). The collected data were compared and combined in the double bond equivalence (DBE) versus carbon number plot to obtain a more complete understanding of the composition of the oil fractions. The numbers of peaks observed by each technique followed the order 2D GC–MS plots of DBE and carbon number showed an extended range of higher values relative to the other methods. For the aromatic fraction of an oil shale pyrolysate generated by the Fischer assay, only a few nitrogen-containing compounds were observed by 2D GC–MS but a large number of these compounds were detected by Orbitrap MS and FT-ICR MS. This comparison clearly shows that the data obtained from these three techniques can be combined to more completely characterize oil composition. The data obtained by Orbitrap MS and FT-ICR MS agreed well with one another, and the combined DBE versus carbon number plot provided more complete coverage of compounds present in the fractions. In addition, the chemical structure information provided by 2D GC–MS could be matched with the chemical formulas in the DBE versus carbon number plots, providing information not available in ultrahigh-resolution MS results. It was therefore concluded that the combination of 2D GC–MS, Orbitrap MS, and FT-ICR MS in the DBE versus carbon number space facilitates structural assignment of heavy oil components.

  5. Mass spectrometry. [in organic chemistry

    Science.gov (United States)

    Burlingame, A. L.; Shackleton, C. H. L.; Howe, I.; Chizhov, O. S.

    1978-01-01

    A review of mass spectrometry in organic chemistry is given, dealing with advances in instrumentation and computer techniques, selected topics in gas-phase ion chemistry, and applications in such fields as biomedicine, natural-product studies, and environmental pollution analysis. Innovative techniques and instrumentation are discussed, along with chromatographic-mass spectrometric on-line computer techniques, mass spectral interpretation and management techniques, and such topics in gas-phase ion chemistry as electron-impact ionization and decomposition, photoionization, field ionization and desorption, high-pressure mass spectrometry, ion cyclotron resonance, and isomerization reactions of organic ions. Applications of mass spectrometry are examined with respect to bio-oligomers and their constituents, biomedically important substances, microbiology, environmental organic analysis, and organic geochemistry.

  6. Application of gamma spectrometry technique in combination with weighing for material balance taking in the production of highly enriched U-A1 fuel

    International Nuclear Information System (INIS)

    Serin, P.A.

    1975-07-01

    The purpose of this project is to obtain the data on material balance for a batch of highly enriched U-Al alloys (used in the NRX and NRU reactors) during production of fuel, using gamma spectrometry (mainly the 186 KeV photopeak) and weighing, and to determine operational data of the Agency's single channel stabilized spectrometer (SAM-1) for measurement of the product typical for the production of highly enriched U-Al fuel (U-Al billets, fuel elements, scrap). The data collected indicates that gamma spectrometry using the single channel stabilized spectrometer is a valid non-destructive method of determining quantitatively U-235 content of U-Al alloy in the form of cast billets or extruded fuel elements providing that adequate standards are available. An accuracy of better than + 1% relative can be obtained using a simple jig to provide reproducible counting geometry. Count rates should be kept well below the saturation level of the detector and counter, preferably by a lead collimator in front of the detector. This non-destructive method is not easily applicable to scrap because of the inability to maintain constant geometry and to prepare standards closely similar in size and shape to the samples

  7. Determination of uranium and thorium in complex matrices by two solvent extraction separation techniques and photon electron rejecting alpha liquid spectrometry

    International Nuclear Information System (INIS)

    Ayranov, M.; Wacker, L.; Kraehenbuehl, U.

    2001-01-01

    The separation of uranium and thorium from complex matrixes such as marine sediments using solvent extraction and determination by means of photon-electron rejecting liquid alpha spectrometry (PERALS trademark) has successfully been performed. Two extraction schemes, using TOPO and HDEHP, respectively, were compared for the separation of uranium and thorium from the matrix components. The results show recoveries between 73 and 92% for 234 U, 238 U, 232 Th, 230 Th and 238 Th with an accuracy of the methods ±12%. Minimum detectable activities for counting time up to 500 000 seconds for 0.5 g sample material were between 0.34-1.15 Bq/kg for uranium and 0.31-1.66 Bq/kg for thorium. (orig.)

  8. A paeudorandom pulser technique for the correction of dead-time and pile-up losses in γ-ray spectrometry

    International Nuclear Information System (INIS)

    Doerfel, G.; Kluge, W.; Kubsch, M.

    1983-01-01

    A pseudorandom pulser and its application in high precision gamma-ray spectrometry is described. A pulse train suitable for modelling dead-time and pile-up effects is obtained by an AND-connection of delayed pulse sequences delivered by a maximum length shift register generator. The heart of the problem consists in finding the appropriate delay indices and in implementing these indices by 'add and shift'. The related conditions and rules are described. These conditions ensure the occurrence of multiple pulses according to the binomial and Poisson distribution, respectively, within a predetermined range of multiplicity as well as ensuring other statistical properties. Results are given in a form comparable with the description of the results of a well-known international test. (orig.)

  9. Sm isotope composition and Sm/Eu ratio determination in an irradiated 153Eu sample by ion exchange chromatography-quadrupole inductively coupled plasma mass spectrometry combined with double spike isotope dilution technique

    International Nuclear Information System (INIS)

    Bourgeois, M.; Isnard, H.; Gourgiotis, A.; Stadelmann, G.; Gautier, C.; Mialle, S.; Nonell, A.; Chartier, F.

    2011-01-01

    Within the framework of the research undertaken by the French Atomic Energy Commission on transmutation of long-lived radionuclides, targets of highly enriched actinides and fission products were irradiated in the fast neutron reactor Phenix. Precise and accurate measurements of the isotopic and elemental composition of the enriched elements are therefore required. In order to obtain the uncertainties of several per mil and to reduce handling time and exposure to analyst on radioactive material, the on-line coupling of ion exchange chromatography with quadrupole inductively coupled plasma mass spectrometry has been associated with the technique of the double spike isotope dilution. We present in this paper the results obtained on an irradiated sample of Europium oxide powder (enriched at 99.13% in 153 Eu). After irradiation of around 5 mg of Eu 2 O 3 powder the theoretical calculations predict the formation of several micrograms of gadolinium and samarium isotopes. In relation to the very high activity of the sample after irradiation and the very low quantity of Sm formed, the on-line ion exchange chromatography separation of Gd, Sm and Eu before Sm isotope ratio measurements has been developed for the quantification of the 152 Sm/ 153 Eu ratio. These on-line measurements were associated with the double spike isotope dilution technique after calibration of a 147 Sm/ 151 Eu spike solution. The external reproducibility of Sm isotopic ratios was determined to be around 0.5% (2 σ) resulting in a final uncertainty on the 152 Sm/ 153 Eu ratio of around 1% (2 σ). These on-line measurements present therefore a robust and high-throughput alternative to the thermal-ionisation mass spectrometry technique used so far in combination with off-line chromatographic separation, particularly in nuclear applications where characterisation of high activity sample solutions is required. (authors)

  10. Dispersive liquid–liquid microextraction using diethyldithiocarbamate as a chelating agent and the dried-spot technique for the determination of Fe, Co, Ni, Cu, Zn, Se and Pb by energy-dispersive X-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    Kocot, Karina; Zawisza, Beata; Sitko, Rafal

    2012-01-01

    Dispersive liquid–liquid microextraction (DLLME) using sodium diethyldithiocarbamate (DDTC) as a chelating agent was investigated for the simultaneous determination of iron, cobalt, nickel, copper, zinc, selenium and lead ions in water samples. The procedure was performed using 5 mL of the sample, 100 μL of a 0.5% solution of DDTC, 30 μL of carbon tetrachloride (extraction phase) and 500 μL of methanol (disperser solvent). The experiments showed that Fe, Co, Ni, Cu, Zn and Pb can be simultaneously extracted at a pH of 5 and that Se can be extracted at a pH of 2–3. The results were compared with those obtained using ammonium pyrrolidine dithiocarbamate as a chelating agent. For all analytes, a linear range was observed up to 0.4 μg mL −1 . If Fe and Zn are present in concentrations 10 times higher than those of the other analytes, then the linearity is observed up to 0.2 μg mL −1 . In the present study, the organic phase that contained preconcentrated elements was deposited onto a Millipore filter and measured using energy-dispersive X-ray fluorescence spectrometry. The obtained detection limits were 2.9, 1.5, 2.0, 2.3, 2.5, 2.0 and 3.9 ng mL −1 for Fe, Co, Ni, Cu, Zn, Se and Pb, respectively. This combination of DLLME and the dried-spot technique is promising for multielement analyses using other spectroscopy techniques, such as laser ablation‐inductively coupled plasma‐mass spectrometry, laser-induced breakdown spectroscopy or total-reflection X-ray fluorescence spectrometry. - Highlights: ► Multielement trace analysis using dried-spot technique and dispersive liquid–liquid microextraction. ► Possibility of combination of LPME with EDXRF, LIBS or LA-ICP-MS. ► Comparison of APDC and DDTC as chelating agents.

  11. Correct primary structure assessment and extensive glyco-profiling of cetuximab by a combination of intact, middle-up, middle-down and bottom-up ESI and MALDI mass spectrometry techniques.

    Science.gov (United States)

    Ayoub, Daniel; Jabs, Wolfgang; Resemann, Anja; Evers, Waltraud; Evans, Catherine; Main, Laura; Baessmann, Carsten; Wagner-Rousset, Elsa; Suckau, Detlev; Beck, Alain

    2013-01-01

    The European Medicines Agency received recently the first marketing authorization application for a biosimilar monoclonal antibody (mAb) and adopted the final guidelines on biosimilar mAbs and Fc-fusion proteins. The agency requires high similarity between biosimilar and reference products for approval. Specifically, the amino acid sequences must be identical. The glycosylation pattern of the antibody is also often considered to be a very important quality attribute due to its strong effect on quality, safety, immunogenicity, pharmacokinetics and potency. Here, we describe a case study of cetuximab, which has been marketed since 2004. Biosimilar versions of the product are now in the pipelines of numerous therapeutic antibody biosimilar developers. We applied a combination of intact, middle-down, middle-up and bottom-up electrospray ionization and matrix assisted laser desorption ionization mass spectrometry techniques to characterize the amino acid sequence and major post-translational modifications of the marketed cetuximab product, with special emphasis on glycosylation. Our results revealed a sequence error in the reported sequence of the light chain in databases and in publications, thus highlighting the potency of mass spectrometry to establish correct antibody sequences. We were also able to achieve a comprehensive identification of cetuximab's glycoforms and glycosylation profile assessment on both Fab and Fc domains. Taken together, the reported approaches and data form a solid framework for the comparability of antibodies and their biosimilar candidates that could be further applied to routine structural assessments of these and other antibody-based products.

  12. Beta spectrometry

    International Nuclear Information System (INIS)

    Dryak, P.; Zderadicka, J.; Plch, J.; Kokta, L.; Novotna, P.

    1977-01-01

    For the purpose of beta spectrometry, a semiconductor spectrometer with one Si(Li) detector cooled with liquid nitrogen was designed. Geometrical detection efficiency is about 10% 4 sr. The achieved resolution for 624 keV conversion electrons of sup(137m)Ba is 2.6 keV (FWHM). A program was written in the FORTRAN language for the correction of the deformation of the measured spectra by backscattering in the analysis of continuous beta spectra. The method permits the determination of the maximum energy of the beta spectrum with an accuracy of +-5 keV. (author)

  13. 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.

  14. Comparison of sample digestion techniques for the determination of trace and residual catalyst metal content in single-wall carbon nanotubes by inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Grinberg, Patricia, E-mail: patricia.grinberg@nrc.ca [Measurement Science and Standards, National Research Council Canada, Ottawa (Canada); Sturgeon, Ralph E. [Measurement Science and Standards, National Research Council Canada, Ottawa (Canada); Diehl, Liange de O.; Bizzi, Cezar A. [Measurement Science and Standards, National Research Council Canada, Ottawa (Canada); Chemistry Department, Universidade Federal de Santa Maria, Santa Maria (Brazil); Flores, Erico M.M. [Chemistry Department, Universidade Federal de Santa Maria, Santa Maria (Brazil)

    2015-03-01

    A single-wall carbon nanotube material produced by laser ablation of renewable biochar in the presence of Ni and Co catalyst was characterized for residual catalyst (Co and Ni) as well as trace metal impurity content (Fe, Mo, Cr, Pb and Hg) by isotope dilution ICP-MS following sample digestion. Several matrix destruction procedures were evaluated, including a multi-step microwave-assisted acid digestion, dry ashing at 450 °C and microwave-induced combustion with oxygen. Results were benchmarked against those derived from neutron activation analysis and also supported by solid sampling continuum source GF-AAS for several of the elements. Although laborious to execute, the multi-step microwave-assisted acid digestion proved to be most reliable for recovery of the majority of the analytes, although content of Cr remained biased low for each approach, likely due to its presence as refractory carbide. - Highlights: • Determination of trace and residual catalyst metal content in Single-Wall Carbon Nanotubes by Inductively Coupled Plasma Mass Spectrometry. • Comparative study of digestion methodology combined with high precision isotope dilution ICP-MS for quantitation of elements of toxicologic relevance. • Results were benchmarked against those derived from neutron activation analysis and also supported by solid sampling continuum source GF-AAS for several of the elements.

  15. Comparison of green sample preparation techniques in the analysis of pyrethrins and pyrethroids in baby food by liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Petrarca, Mateus Henrique; Ccanccapa-Cartagena, Alexander; Masiá, Ana; Godoy, Helena Teixeira; Picó, Yolanda

    2017-05-12

    A new selective and sensitive liquid chromatography triple quadrupole mass spectrometry method was developed for simultaneous analysis of natural pyrethrins and synthetic pyrethroids residues in baby food. In this study, two sample preparation methods based on ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) and salting-out assisted liquid-liquid extraction (SALLE) were optimized, and then, compared regarding the performance criteria. Appropriate linearity in solvent and matrix-based calibrations, and suitable recoveries (75-120%) and precision (RSD values≤16%) were achieved for selected analytes by any of the sample preparation procedures. Both methods provided the analytical selectivity required for the monitoring of the insecticides in fruit-, cereal- and milk-based baby foods. SALLE, recognized by cost-effectiveness, and simple and fast execution, provided a lower enrichment factor, consequently, higher limits of quantification (LOQs) were obtained. Some of them too high to meet the strict legislation regarding baby food. Nonetheless, the combination of ultrasound and DLLME also resulted in a high sample throughput and environmental-friendly method, whose LOQs were lower than the default maximum residue limit (MRL) of 10μgkg -1 set by European Community for baby foods. In the commercial baby foods analyzed, cyhalothrin and etofenprox were detected in different samples, demonstrating the suitability of proposed method for baby food control. Copyright © 2017 Elsevier B.V. All rights reserved.

  16. A novel separation/preconcentration technique based on ultrasonic dispersion liquid-liquid microextraction for determination of trace cobalt by flame atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Jingci Li

    2012-12-01

    Full Text Available An improved method for the determination of trace cobalt in water samples has been developed using ultrasonic dispersion liquid-liquid microextraction (US-DLLME prior to flame atomic absorption spectrometry (FAAS analysis. In this method, cobalt was extracted into the fine droplets of carbon tetrachloride after chelate formation with the water soluble ligand, ammonium pyrrolidine dithiocarbamate (APDC. The fine droplets of carbon tetrachloride were formed and dispersed in the aqueous sample with the help of ultrasonic waves which accelerated the formation of the fine cloudy solution without using disperser solvents. Under optimum conditions, the calibration curve was linear in the range of 2.5-500 μg L-1, with a detection limit of 0.8 μg L-1. The relative standard deviation (RSD for ten replicate measurements of 20 and 500 μg L-1 of cobalt were 3.3 and 2.2%. This proposed method was successfully applied to tap water, river water, and sea water, and accuracy was assessed through the analysis of certified reference water or recovery experiments. Operation simplicity, low cost, high enrichment factor, and low consumption of the extraction solvent are the main advantages of the proposed method.DOI: http://dx.doi.org/10.4314/bcse.v26i1.2

  17. Detailed characterization of bio-oil from pyrolysis of non-edible seed-cakes by Fourier Transform Infrared Spectroscopy (FTIR) and gas chromatography mass spectrometry (GC-MS) techniques.

    Science.gov (United States)

    Sugumaran, Vatsala; Prakash, Shanti; Ramu, Emmandi; Arora, Ajay Kumar; Bansal, Veena; Kagdiyal, Vivekanand; Saxena, Deepak

    2017-07-15

    Bio-oil obtained from pyrolysis is highly complicated mixture with valued chemicals. In order to reduce the complexity for unambiguous characterization of components present in bio-oil, solvent extractions using different solvents with increasing polarity have been adopted. The fractions have been analyzed by Fourier transform infrared (FTIR) spectroscopy for identifying the functional groups and Gas chromatography-mass spectrometry (GC-MS), for detailed characterization of components present in various fractions, thereby providing in-depth information at molecular level of various components in bio-oil. This paper reveals the potential of the analytical techniques in identification and brings out the similarities as well as differences in the components present in the bio-oil obtained from two non-edible oil seed-cakes, viz., Jatropha and Karanjia. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Micro-electrodeposition techniques for the preparation of small actinide counting sources for ultra-high resolution alpha spectrometry by microcalorimetry

    International Nuclear Information System (INIS)

    Plionis, A.A.; Hastings, E.P.; LaMont, S.P.; Dry, D.E.; Bacrania, M.K.; Rabin, M.W.; Rim, J.H.

    2009-01-01

    Special considerations and techniques are desired for the preparation of small actinide counting sources. Counting sources have been prepared on metal disk substrates (planchets) with an active area of only 0.079 mm 2 . This represents a 93.75% reduction in deposition area from standard electrodeposition methods. The actinide distribution upon the smaller planchet must remain thin and uniform to allow alpha particle emissions to escape the counting source with a minimal amount of self-attenuation. This work describes the development of micro-electrodeposition methods and optimization of the technique with respect to deposition time and current density for various planchet sizes. (author)

  19. Determination of plutonium isotopic abundances by gamma-ray spectrometry. Interim report on the status of methods and techniques developed by the Lawrence Livermore Laboratory

    International Nuclear Information System (INIS)

    Gunnink, R.

    1980-03-01

    This report presents an overview of methods and techniques developed by the Lawrence Livermore Laboratory for determining plutonium isotopic abundances from gamma-ray spectra that have been measured with germanium detectors. The methodology of fitting the spectral features includes discussions of algorithms for gamma-ray and x-ray peak shape fitting and generation of response spectra profiles characteristic of specific isotopes. Applications of the techniques developed at government, commercial, and Japanese reprocessing plants are described. Current development of the methodology for the nondestructive analysis of samples containing nondescript solid materials is also presented

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

    International Nuclear Information System (INIS)

    Aggarwal, S.K.

    2002-01-01

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

  1. Tuberculose infantil: estudo retrospectivo

    Directory of Open Access Journals (Sweden)

    Boaventura Antonio dos Santos

    2011-10-01

    Full Text Available Introdução: A tuberculose (TB infantil permanece como uma das doenças mais prevalentes e preocupantes no mundo, sobretudo em nações em desenvolvimento, onde as taxas são ainda mais elevadas e os casos descritos subestimados pela dificuldade em se estabelecer um diagnóstico definitivo. Dessa forma, este estudo tem como objetivo descrever o perfil clínico e epidemiológico dos pacientes com TB infantil pulmonar e extrapulmonar. Métodos: Foram avaliados retrospectivamente, através de questionário, pacientes com idade de até 15 anos, internados no Serviço de Pediatria do HCPA, no período de janeiro de 2002 a setembro de 2007.   Resultados: Dos 52 pacientes incluídos, 63% apresentavam TB pulmonar. Das formas extra-pulmonares, a meningoencefalite foi a mais prevalente (22%. Comorbidades foram dectadas em 31 (60% pacientes, dos quais 15 (29% apresentavam desnutrição grave, 9 (18% HIV positivo e 7 (13% pneumopatia crônica. Das manifestações clínicas, febre e tosse estavam presentes na maioria dos pacientes. O padrão radiológico predominante foi o de consolidação pulmonar (51%. A maioria dos pacientes referia história de contato com paciente bacilífero (64%. Conclusão: A TB pulmonar representa a principal forma de apresentação clínica da TB, sendo o diagnóstico feito de forma presuntiva na maioria dos casos. O diagnóstico baseado na comprovação bacteriológica foi obtido numa minoria de pacientes, demonstrando a importância dos achados clínico-laboratoriais, história epidemiológica e vacinal para o diagnóstico. Nesse sentido, a criação de escores tem se tornado uma ferramenta de fácil acesso e com razoável acurácia para auxiliar o diagnóstico de TB em serviços de baixa complexidade, especialmente o ambulatorial.

  2. Evaluation of electro-spray ionisation mass spectrometry as a technique for the investigation of competitive interactions: A case study of the ternary Th-Mn-EDTA system

    International Nuclear Information System (INIS)

    Reinoso-Maset, Estela; Worsfold, Paul J.; Keith-Roach, Miranda J.

    2012-01-01

    Rationale: Electro-spray ionisation mass spectrometry (ESI-MS) is a useful tool for exploring the speciation of solution-phase metal complexes; however, the quantification of ternary systems is challenging due to the differences in the electro-spray response of different species. Here, the Th-Mn-EDTA system was investigated to evaluate the capability of ESI-MS for quantifying the species present. Methods: Increasingly complex mixtures of Th(IV), Mn(II) and EDTA were analysed using manual flow injection of samples into an HPLC grade water mobile phase delivered to an ion trap mass spectrometer fitted with an ESI interface (ThermoQuest Finnigan Mat LCQ). Mass spectra were obtained in the positive and negative ion modes over a mass-to-charge (m/z) range from 50-2000. Results: The instrumental response to EDTA was affected by the addition of Th(NO 3 ) 4 but not MnCl 2 , while the response to both Th-EDTA and Mn-EDTA species was affected by addition of the other metal salt. Internal standards were also found to suppress signals to different extents. Therefore, each signal suppression was carefully quantified as the solution became more complex, and signal correction factors were used in conjunction with regular external calibration. Mixed metal signals were quantified adequately. Conclusions: This study showed the complexity of quantifying a ternary system involving different co-existing species. Nonetheless, the step-wise protocol developed provided quantitative data on the displacement of Mn from its EDTA complex by Th. (authors)

  3. Determination of Phenolic Acids and Flavonoids in Taraxacum formosanum Kitam by Liquid Chromatography-Tandem Mass Spectrometry Coupled with a Post-Column Derivatization Technique

    Directory of Open Access Journals (Sweden)

    Hung-Ju Chen

    2011-12-01

    Full Text Available A liquid chromatography-tandem mass spectrometry method (LC-MS/MS was developed for the determination of phenolic acids and flavonoids in a medicinal Chinese herb Taraxacum formosanum Kitam. Initially, both phenolic acids and flavonoids were extracted with 50% ethanol in a water-bath at 60 °C for 3 h and eventually separated into acidic fraction and neutral fraction by using a C18 cartridge. A total of 29 compounds were separated within 68 min by employing a Gemini C18 column and a gradient solvent system of 0.1% formic acid and acetonitrile at a flow rate of 1.0 mL/min. Based on the retention behavior as well as absorption and mass spectra, 19 phenolic acids and 10 flavonoids were identified and quantified in T. formosanum, with the former ranging from 14.1 μg/g to 10,870.4 μg/g, and the latter from 9.9 μg/g to 325.8 μg/g. For further identification of flavonoids, a post-column derivatization method involving shift reagents such as sodium acetate or aluminum chloride was used and the absorption spectral characteristics without or with shift reagents were compared. An internal standard syringic acid was used for quantitation of phenolic acids, whereas (± naringenin was found suitable for quantitation of flavonoids. The developed LC-MS/MS method showed high reproducibility, as evident from the relative standard deviation (RSD values for intra-day and inter-day variability being 1.0–6.8% and 2.0–7.7% for phenolic acids and 3.7–7.4% and 1.5–8.1% for flavonoids, respectively, and thus may be applied for simultaneous determination of phenolic acids and flavonoids in Chinese herb and nutraceuticals.

  4. Evaluation of a Bead-Free Coimmunoprecipitation Technique for Identification of Virus-Host Protein Interactions Using High-Resolution Mass Spectrometry.

    Science.gov (United States)

    DeBlasio, Stacy L; Bereman, Michael S; Mahoney, Jaclyn; Thannhauser, Theodore W; Gray, Stewart M; MacCoss, Michael J; Cilia Heck, Michelle

    2017-09-01

    Protein interactions between virus and host are essential for viral propagation and movement, as viruses lack most of the proteins required to thrive on their own. Precision methods aimed at disrupting virus-host interactions represent new approaches to disease management but require in-depth knowledge of the identity and binding specificity of host proteins within these interaction networks. Protein coimmunoprecipitation (co-IP) coupled with mass spectrometry (MS) provides a high-throughput way to characterize virus-host interactomes in a single experiment. Common co-IP methods use antibodies immobilized on agarose or magnetic beads to isolate virus-host complexes in solutions of host tissue homogenate. Although these workflows are well established, they can be fairly laborious and expensive. Therefore, we evaluated the feasibility of using antibody-coated microtiter plates coupled with MS analysis as an easy, less expensive way to identify host proteins that interact with Potato leafroll virus (PLRV), an insect-borne RNA virus that infects potatoes. With the use of the bead-free platform, we were able to detect 36 plant and 1 nonstructural viral protein significantly coimmunoprecipitating with PLRV. Two of these proteins, a 14-3-3 signal transduction protein and malate dehydrogenase 2 (mMDH2), were detected as having a weakened or lost association with a structural mutant of the virus, demonstrating that the bead-free method is sensitive enough to detect quantitative differences that can be used to pin-point domains of interaction. Collectively, our analysis shows that the bead-free platform is a low-cost alternative that can be used by core facilities and other investigators to identify plant and viral proteins interacting with virions and/or the viral structural proteins.

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

    NARCIS (Netherlands)

    Helsper, Hans; Peters, Ruud J.B.; Bemmel, van Greet; Herrera Rivera, Zahira; Wagner, Stephan; Kammer, von der Frank; Tromp, Peter C.; Hofmann, Thilo; Weigel, Stefan

    2016-01-01

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

  6. Development of a broad toxicological screening technique for urine using ultra-performance liquid chromatography and time-of-flight mass spectrometry

    DEFF Research Database (Denmark)

    Lee, Hon Kit; Ho, Chung Shun; Iu, Yan Ping Heidi

    2009-01-01

    Withdrawal of the support for the REMEDi HS drug profiling system has necessitated its replacement within our laboratories with an alternative broad toxicological screening technique. To this end, a novel method, based on ultra-performance liquid chromatography (UPLC) and time-of-flight (TOF) mass...

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

    Science.gov (United States)

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

    2009-08-15

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

  8. Mass spectrometry with accelerators.

    Science.gov (United States)

    Litherland, A E; Zhao, X-L; Kieser, W E

    2011-01-01

    As one in a series of articles on Canadian contributions to mass spectrometry, this review begins with an outline of the history of accelerator mass spectrometry (AMS), noting roles played by researchers at three Canadian AMS laboratories. After a description of the unique features of AMS, three examples, (14)C, (10)Be, and (129)I are given to illustrate the methods. The capabilities of mass spectrometry have been extended by the addition of atomic isobar selection, molecular isobar attenuation, further ion acceleration, followed by ion detection and ion identification at essentially zero dark current or ion flux. This has been accomplished by exploiting the techniques and accelerators of atomic and nuclear physics. In 1939, the first principles of AMS were established using a cyclotron. In 1977 the selection of isobars in the ion source was established when it was shown that the (14)N(-) ion was very unstable, or extremely difficult to create, making a tandem electrostatic accelerator highly suitable for assisting the mass spectrometric measurement of the rare long-lived radioactive isotope (14)C in the environment. This observation, together with the large attenuation of the molecular isobars (13)CH(-) and (12)CH 2(-) during tandem acceleration and the observed very low background contamination from the ion source, was found to facilitate the mass spectrometry of (14)C to at least a level of (14)C/C ~ 6 × 10(-16), the equivalent of a radiocarbon age of 60,000 years. Tandem Accelerator Mass Spectrometry, or AMS, has now made possible the accurate radiocarbon dating of milligram-sized carbon samples by ion counting as well as dating and tracing with many other long-lived radioactive isotopes such as (10)Be, (26)Al, (36)Cl, and (129)I. The difficulty of obtaining large anion currents with low electron affinities and the difficulties of isobar separation, especially for the heavier mass ions, has prompted the use of molecular anions and the search for alternative

  9. Gamma and X 93 spectrometry

    International Nuclear Information System (INIS)

    1994-05-01

    The Meetings of Gamma and X 93 Spectrometry were held on 12-14 October 1993. The symposium was organized into six sessions: Instrumentation development, Nuclear matter measurement, Method and calibration, Medical applications, Environment survey (radioactive traces measurement), other applications (spent fuels analysis, various techniques). Separate abstracts were prepared for all the papers in this volume. (TEC)

  10. Feline immunodeficiency virusinfection: a comparative study of different diagnostic techniques Infecção pelo vírus da imunodeficiência felina: estudo comparativo de diferentes técnicas de diagnóstico

    Directory of Open Access Journals (Sweden)

    E. Mortola

    2004-02-01

    Full Text Available This study evaluated an indirect immunofluorescence assay (IFA to detect feline immunodeficiency virus infection (FIV antibody in a comprehensive epidemiological survey of FIV in Argentina. IFA modified in our laboratory, was compared with two other immunoassays, western blot (WB and a sandwich immunochromatographic commercial kit (SI, and also with a direct polymerase chain reaction (PCR method that detects proviral DNA. IFA showed to be a test with high sensitivity and specificity, and could be useful as a diagnostic tool in epidemiological studies. The presence of a low percentage of results with non-specific reactivity in the IFA could be resolved with further testing or use of an alternative method.Avaliou-se a técnica de imunofluorescência indireta (IFA na detecção de anticorpos contra o vírus da imunodeficiência felina (FIV numa pesquisa epidemiológica do FIV na Argentina. A IFA foi modificada e comparada com duas outras técnicas imunológicas: western blot (WB e imunocromatografia em camadas (SI com kit comercial e também com reação em cadeia de polimerase (PCR para detecção do DNA proviral. A IFA mostrou ser um teste com alta sensibilidade e especificidade e poderá ser empregada como ferramenta útil em estudos epidemiológicos. A baixa porcentagem de reatividade não específica pode ser esclarecida com testes mais avançados ou usando métodos alternativos.

  11. Software tool for resolution of inverse problems using artificial intelligence techniques: an application in neutron spectrometry; Herramienta en software para resolucion de problemas inversos mediante tecnicas de inteligencia artificial: una aplicacion en espectrometria neutronica

    Energy Technology Data Exchange (ETDEWEB)

    Castaneda M, V. H.; Martinez B, M. R.; Solis S, L. O.; Castaneda M, R.; Leon P, A. A.; Hernandez P, C. F.; Espinoza G, J. G.; Ortiz R, J. M.; Vega C, H. R. [Universidad Autonoma de Zacatecas, 98000 Zacatecas, Zac. (Mexico); Mendez, R. [CIEMAT, Departamento de Metrologia de Radiaciones Ionizantes, Laboratorio de Patrones Neutronicos, Av. Complutense 22, 28040 Madrid (Spain); Gallego, E. [Universidad Politecnica de Madrid, Departamento de Ingenieria Nuclear, C. Jose Gutierrez Abascal 2, 28006 Madrid (Spain); Sousa L, M. A. [Comision Nacional de Energia Nuclear, Centro de Investigacion de Tecnologia Nuclear, Av. Pte. Antonio Carlos 6627, Pampulha, 31270-901 Belo Horizonte, Minas Gerais (Brazil)

    2016-10-15

    The Taguchi methodology has proved to be highly efficient to solve inverse problems, in which the values of some parameters of the model must be obtained from the observed data. There are intrinsic mathematical characteristics that make a problem known as inverse. Inverse problems appear in many branches of science, engineering and mathematics. To solve this type of problem, researches have used different techniques. Recently, the use of techniques based on Artificial Intelligence technology is being explored by researches. This paper presents the use of a software tool based on artificial neural networks of generalized regression in the solution of inverse problems with application in high energy physics, specifically in the solution of the problem of neutron spectrometry. To solve this problem we use a software tool developed in the Mat Lab programming environment, which employs a friendly user interface, intuitive and easy to use for the user. This computational tool solves the inverse problem involved in the reconstruction of the neutron spectrum based on measurements made with a Bonner spheres spectrometric system. Introducing this information, the neural network is able to reconstruct the neutron spectrum with high performance and generalization capability. The tool allows that the end user does not require great training or technical knowledge in development and/or use of software, so it facilitates the use of the program for the resolution of inverse problems that are in several areas of knowledge. The techniques of Artificial Intelligence present singular veracity to solve inverse problems, given the characteristics of artificial neural networks and their network topology, therefore, the tool developed has been very useful, since the results generated by the Artificial Neural Network require few time in comparison to other techniques and are correct results comparing them with the actual data of the experiment. (Author)

  12. Screening for illicit drugs in pooled human urine and urinated soil samples and studies on the stability of urinary excretion products of cocaine, MDMA, and MDEA in wastewater by hyphenated mass spectrometry techniques.

    Science.gov (United States)

    Mardal, Marie; Kinyua, Juliet; Ramin, Pedram; Miserez, Bram; Van Nuijs, Alexander L N; Covaci, Adrian; Meyer, Markus R

    2017-01-01

    Monitoring population drug use through wastewater-based epidemiology (WBE) is a useful method to quantitatively follow trends and estimate total drug consumption in communities. Concentrations of drug biomarkers might be low in wastewater due to dilution; and therefore analysis of pooled urine (PU) is useful to detect consumed drugs and identify targets of illicit drugs use. The aims of the study were (1) to screen PU and urinated soil (US) samples collected at festivals for illicit drug excretion products using hyphenated techniques; (2) to develop and validate a hydrophilic interaction liquid chromatography - mass spectrometry / mass spectrometry (HILIC-MS/MS) method of quantifying urinary targets of identified drugs in wastewater; and (3) to conduct a 24 h stability study, using PU and US to better reflect the chemical environment for targets in wastewater. Cocaine (COC) and ecstasy-like compounds were the most frequently detected illicit drugs; an analytical method was developed to quantify their excretion products. Hydroxymethoxymethamphetamine (HMMA), 3,4-methylenedioxymethamphetamine (MDMA), 3,4-methylenedioxyamphetamine (MDA), HMMA sulfate (HMMA-S), benzoylecgonine (BE), and cocaethylene (CE) had 85-102% of initial concentration after 8 h of incubation, whereas COC and ecgonine methyl ester (EME) had 74 and 67% after 8 h, respectively. HMMA showed a net increase during 24 h of incubation (107% ± 27, n = 8), possibly due to the cleavage of HMMA conjugates, and biotransformation of MDMA. The results suggest HMMA as analytical target for MDMA consumption in WBE, due to its stability in wastewater and its excretion as the main phase I metabolite of MDMA. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  13. Study of a new technique for measuring the travel time of ultrasonic waves using the frequency spectrum; Estudo de uma nova tecnica de medida do tempo de percurso da onda ultra-sonica usando o espectro de frequencia

    Energy Technology Data Exchange (ETDEWEB)

    Santos, Allan Xavier dos

    2010-07-01

    During the operation of a nuclear plant and other industrial plants, the operational time and the exposition to severe working conditions may cause the wear of its components, consequently, compromising the safety and the performance of the installation. The implementation of periodical inspections helps to ensure the safe operation and the best performance of the plant. In this way, the use of ultrasonic techniques for inspection and materials characterization becomes more and more attractive, since they offer quick, precise results and are technically ease to implement. The usual ultrasonic techniques, need to the measure the travelling time of the ultrasonic wave in the material examined in order to extract information useful to characterize it. Thus, the measurement of the travelling time of the ultrasonic wave is the overriding factor in most of the applications made with ultrasound. In this work a new technique was developed for measuring the travelling time of the ultrasonic wave using a Fourier's Fast Transformer (FFT). It will be shown mathematically and experimentally that it is possible to use the ultrasonic signal in the frequency domain to determine the travelling time of the ultrasonic wave. Five experiments were carried out for the experimental validation of this new technique. The materials used were 20 ceramic pastilles with different porosities and 3 aluminum plates of different thicknesses. The obtained results have shown that the new technique proposed in this work was able to determine the travelling time of the ultrasonic wave with the same precision as the conventional technique. It was shown, furthermore, that this new technique is able to measure the travelling time of the ultrasonic wave in situations where the conventional technique cannot be applied greatly expanding the range of application of ultrasonic testing and inspections. (author)

  14. Direct identification of microorganisms from positive blood cultures using the lysis-filtration technique and matrix assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF MS): a multicentre study.

    Science.gov (United States)

    Farina, Claudio; Arena, Fabio; Casprini, Patrizia; Cichero, Paola; Clementi, Massimo; Cosentino, Marina; Degl'Innocenti, Roberto; Giani, Tommaso; Luzzaro, Francesco; Mattei, Romano; Mauri, Carola; Nardone, Maria; Rossolini, Gian Maria; Serna Ortega, Paula Andrea; Vailati, Francesca

    2015-04-01

    Microbial identification from blood cultures is essential to institute optimal antibiotic therapy and improve survival possibilities. Matrix-assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF MS) has been successfully applied to identify bacteria and yeasts from positive blood cultures broths. The aim of this multicentre study was to evaluate the reliability of the lysis-filtration technique associated with MALDI-TOF MS to directly identify microorganisms from 765 positive blood cultures collected in six Italian hospitals. Overall, 675/765 (78.1%) blood isolates were correctly identified at the species level, with significant differences between Gram-negative and Gram-positive bacteria (92.6%, and 69.8%, respectively). Some difficulties arise in identifying Streptococcus pneumoniae, Staphylococcus aureus, yeasts and anaerobes. The lysis-filtration protocol is a suitable procedure in terms of performance in identifying microorganisms, but it is quite expensive and technically time-consuming since the time of filtration is not regular for all the samples. The application of the MALDI-TOF MS technique to the direct microbial identification from positive blood cultures is a very promising approach, even if more experience must be gained to minimize errors and costs.

  15. Simultaneous determination of major to ultratrace elements in geological samples by fusion-dissolution and inductively coupled plasma mass spectrometry techniques

    Energy Technology Data Exchange (ETDEWEB)

    Madinabeitia, S. Garcia de [Servicio de Geocronologia y Geoquimica Isotopica, Facultad de Ciencia y Tecnologia, Universidad del Pais Vasco/EHU, Sarriena s/n, 48940 Leioa (Spain); Lorda, M.E. Sanchez [Servicio de Geocronologia y Geoquimica Isotopica, Facultad de Ciencia y Tecnologia, Universidad del Pais Vasco/EHU, Sarriena s/n, 48940 Leioa (Spain); Departamento de Mineralogia-Petrologia, Facultad de Ciencia y Tecnologia, Universidad del Pais Vasco/EHU, Sarriena s/n, 48940 Leioa (Spain); Ibarguchi, J.I. Gil [Servicio de Geocronologia y Geoquimica Isotopica, Facultad de Ciencia y Tecnologia, Universidad del Pais Vasco/EHU, Sarriena s/n, 48940 Leioa (Spain)], E-mail: josei.gil@ehu.es

    2008-09-12

    A method has been developed for the simultaneous quantification of major to ultratrace elements in geological samples using quadrupole ICP-MS techniques. The sample preparation involves fusion with LiBO{sub 2} and dilution in HNO{sub 3}-HF which allows complete decomposition of refractory minerals and quantification of the elements of interest. The effects of high Total Dissolved Solids (TDS) and Li in the solution are minimized using a matrix-tolerant interface and conditioning the instrument with LiBO{sub 2} solution. The signal drift is moreover controlled using conventional internal standards and specific Drift Correction Standards (DCS). A key issue of the technique is the external calibration using selected Certified Reference Materials (CRM). Depending on the sample type and analytes of interest three optimized programmable modes are used sequentially: Standard, Collision Cell (CCT) and Kinetic Energy Discrimination (KED) mode. The method allows to quantify more than 40 elements in concentrations from tens-of-percent to <0.1 ppm levels during a single experiment. The method has been validated through the analysis of different CRMs with recovery factors of ca. 100% and typical 2{sigma} errors of <10%.

  16. Simultaneous determination of major to ultratrace elements in geological samples by fusion-dissolution and inductively coupled plasma mass spectrometry techniques

    International Nuclear Information System (INIS)

    Madinabeitia, S. Garcia de; Lorda, M.E. Sanchez; Ibarguchi, J.I. Gil

    2008-01-01

    A method has been developed for the simultaneous quantification of major to ultratrace elements in geological samples using quadrupole ICP-MS techniques. The sample preparation involves fusion with LiBO 2 and dilution in HNO 3 -HF which allows complete decomposition of refractory minerals and quantification of the elements of interest. The effects of high Total Dissolved Solids (TDS) and Li in the solution are minimized using a matrix-tolerant interface and conditioning the instrument with LiBO 2 solution. The signal drift is moreover controlled using conventional internal standards and specific Drift Correction Standards (DCS). A key issue of the technique is the external calibration using selected Certified Reference Materials (CRM). Depending on the sample type and analytes of interest three optimized programmable modes are used sequentially: Standard, Collision Cell (CCT) and Kinetic Energy Discrimination (KED) mode. The method allows to quantify more than 40 elements in concentrations from tens-of-percent to <0.1 ppm levels during a single experiment. The method has been validated through the analysis of different CRMs with recovery factors of ca. 100% and typical 2σ errors of <10%

  17. Study of the interactions between the transuranic elements and some environmental ligands by the hyphenated technique capillary electrophoresis: inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Topin, S.

    2009-09-01

    In this work, the capabilities of the hyphenated Capillary Electrophoresis-ICP-MS technique are used to improve the knowledge on the transuranic element speciation in the environment (nuclear waste management) and in the framework of spent fuel reprocessing. Essential thermodynamical data have been determined for the first time for the interactions of the plutonium at the (5+) oxidation state (main soluble species of Pu of the surface water) in inorganic media (chloride, nitrate, sulfate, carbonate). This study enables to correct the existing model, based on the thermodynamical data of the neptunium at the (5+) oxidation state (analogue of the pentavalent plutonium). Furthermore, the hyphenated CE-ICP-MS technique has also been applied to study the interactions between DTPA, widely used in the nuclear industry, and the elements at the (3+) oxidation state (Pu, Am, Cm, Cf) and at the (4+) oxidation state (Pu, Np, Th). The results show for the first time the formation of mixed An(IV)/DTPA/OH complexes likely to play a key role on the actinide behavior in the field of the waste management. The study on the trivalent elements confirms the selectivity of DTPA versus the actinide in the framework of the actinide/lanthanide separation but proves that the covalency, responsible of the selectivity, are less important than the ionicity in the binding. (author)

  18. The determination of gold in activated charcoal by use of a loose-powder technique and x-ray-fluorescence spectrometry

    International Nuclear Information System (INIS)

    Balaes, A.M.E.

    1984-01-01

    The method of analysis described is applicable to samples of activated charcoal with a gold concentration of 15g/t and higher. The use of a loose-powder technique minimizes the time taken for the preparation of samples. A platinum internal standard is used for the correction for matrix effects and for differences that could be caused by the packing of the loose charcoal into liquid-sample cups. The precision of the method ranges from a relative standard deviation of 0,085 to 0,016 for concentrations of gold from 67 to 3800g/t respectively. The agreement between the recommended values for a set of reference samples and the values obtained by the X-ray-fluorescence method is better than 3 per cent. The overall time required for the analysis of ten samples and standards is approximately 1 hour. A detailed laboratory method and a computer programme for the calculations are given as appendices

  19. Coincidence gamma-ray spectrometry

    DEFF Research Database (Denmark)

    Markovic, Nikola; Roos, Per; Nielsen, Sven Poul

    2017-01-01

    Gamma-ray spectrometry with high-purity germanium (HPGe) detectors is often the technique of choice in an environmental radioactivity laboratory. When measuring environmental samples associated activities are usually low so an important parameter that describes the performance of the spectrometer...... for a nuclide of interest is the minimum detectable activity (MDA). There are many ways for lowering the MDAs in gamma spectrometry. Recently, developments of fast and compact digital acquisition systems have led to growing number of multiple HPGe detector spectrometers. In these applications all detected...

  20. Analysis of the differentially expressed low molecular weight peptides in human serum via an N-terminal isotope labeling technique combining nano-liquid chromatography/matrix-assisted laser desorption/ionization mass spectrometry.

    Science.gov (United States)

    Leng, Jiapeng; Zhu, Dong; Wu, Duojiao; Zhu, Tongyu; Zhao, Ningwei; Guo, Yinlong

    2012-11-15

    Peptidomics analysis of human serum is challenging due to the low abundance of serum peptides and interference from the complex matrix. This study analyzed the differentially expressed (DE) low molecular weight peptides in human serum integrating a DMPITC-based N-terminal isotope labeling technique with nano-liquid chromatography and matrix-assisted laser desorption/ionization mass spectrometry (nano-LC/MALDI-MS). The workflow introduced a [d(6)]-4,6-dimethoxypyrimidine-2-isothiocyanate (DMPITC)-labeled mixture of aliquots from test samples as the internal standard. The spiked [d(0)]-DMPITC-labeled samples were separated by nano-LC then spotted on the MALDI target. Both quantitative and qualitative studies for serum peptides were achieved based on the isotope-labeled peaks. The DMPITC labeling technique combined with nano-LC/MALDI-MS not only minimized the errors in peptide quantitation, but also allowed convenient recognition of the labeled peptides due to the 6 Da mass difference. The data showed that the entire research procedure as well as the subsequent data analysis method were effective, reproducible, and sensitive for the analysis of DE serum peptides. This study successfully established a research model for DE serum peptides using DMPITC-based N-terminal isotope labeling and nano-LC/MALDI-MS. Application of the DMPITC-based N-terminal labeling technique is expected to provide a promising tool for the investigation of peptides in vivo, especially for the analysis of DE peptides under different biological conditions. Copyright © 2012 John Wiley & Sons, Ltd.

  1. Quantifying uncertainty in measurement of mercury in suspended particulate matter by cold vapor technique using atomic absorption spectrometry with hydride generator.

    Science.gov (United States)

    Singh, Nahar; Ahuja, Tarushee; Ojha, Vijay Narain; Soni, Daya; Tripathy, S Swarupa; Leito, Ivo

    2013-01-01

    As a result of rapid industrialization several chemical forms of organic and inorganic mercury are constantly introduced to the environment and affect humans and animals directly. All forms of mercury have toxic effects; therefore accurate measurement of mercury is of prime importance especially in suspended particulate matter (SPM) collected through high volume sampler (HVS). In the quantification of mercury in SPM samples several steps are involved from sampling to final result. The quality, reliability and confidence level of the analyzed data depends upon the measurement uncertainty of the whole process. Evaluation of measurement uncertainty of results is one of the requirements of the standard ISO/IEC 17025:2005 (European Standard EN IS/ISO/IEC 17025:2005, issue1:1-28, 2006). In the presented study the uncertainty estimation in mercury determination in suspended particulate matter (SPM) has been carried out using cold vapor Atomic Absorption Spectrometer-Hydride Generator (AAS-HG) technique followed by wet chemical digestion process. For the calculation of uncertainty, we have considered many general potential sources of uncertainty. After the analysis of data of seven diverse sites of Delhi, it has been concluded that the mercury concentration varies from 1.59 ± 0.37 to 14.5 ± 2.9 ng/m(3) with 95% confidence level (k = 2).

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

    International Nuclear Information System (INIS)

    Povinec, P.P.

    2005-01-01

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

  3. Cluster secondary ion mass spectrometry microscope mode mass spectrometry imaging.

    Science.gov (United States)

    Kiss, András; Smith, Donald F; Jungmann, Julia H; Heeren, Ron M A

    2013-12-30

    Microscope mode imaging for secondary ion mass spectrometry is a technique with the promise of simultaneous high spatial resolution and high-speed imaging of biomolecules from complex surfaces. Technological developments such as new position-sensitive detectors, in combination with polyatomic primary ion sources, are required to exploit the full potential of microscope mode mass spectrometry imaging, i.e. to efficiently push the limits of ultra-high spatial resolution, sample throughput and sensitivity. In this work, a C60 primary source was combined with a commercial mass microscope for microscope mode secondary ion mass spectrometry imaging. The detector setup is a pixelated detector from the Medipix/Timepix family with high-voltage post-acceleration capabilities. The system's mass spectral and imaging performance is tested with various benchmark samples and thin tissue sections. The high secondary ion yield (with respect to 'traditional' monatomic primary ion sources) of the C60 primary ion source and the increased sensitivity of the high voltage detector setup improve microscope mode secondary ion mass spectrometry imaging. The analysis time and the signal-to-noise ratio are improved compared with other microscope mode imaging systems, all at high spatial resolution. We have demonstrated the unique capabilities of a C60 ion microscope with a Timepix detector for high spatial resolution microscope mode secondary ion mass spectrometry imaging. Copyright © 2013 John Wiley & Sons, Ltd.

  4. An evaporation-assisted dispersive liquid-liquid microextraction technique as a simple tool for high performance liquid chromatography tandem-mass spectrometry determination of insecticides in wine.

    Science.gov (United States)

    Timofeeva, Irina; Kanashina, Daria; Moskvin, Leonid; Bulatov, Andrey

    2017-08-25

    A sample pre-treatment technique based on evaporation-assisted dispersive liquid-liquid microextraction (EVA-DLLME), followed by HPLC-MS/MS has been developed for the determination of organophosphate insecticides (malathion, diazinon, phosalone) in wine samples. The procedure includes the addition of mixture of organic solvents (with density higher than water), consisting of the extraction (low density) and volatile (high density) solvents, to aqueous sample followed by heating of the mixture obtained, what promotes the volatile solvent evaporation and moving extraction solvent droplets from down to top of the aqueous sample and, as a consequence, microextraction of target analytes. To initiate the evaporation process an initiator is required. It was established that hexanol (extraction solvent) and dichloromethane (volatile solvent) mixture (1:1, v/v) provides effective microextraction of the insecticides from wine samples with recovery from 92 to 103%. The conditions of insecticides' microextraction such as selection of extraction solvent, ratio of hexanol/dichloromethane and hexanol/sample, type and concentration of initiator, and effect of ethanol as one of the main components of wine have been studied. Under optimal experimental conditions the linear detection ranges were found to be 10 -7 -10 -3 gL -1 for malathion, 10 -9 -10 -4 gL -1 for diazinon, and 10 -6 -10 -2 gL -1 for phosalone. The LODs, calculated from a blank test, based on 3σ, found to be 3×10 -8 gL -1 for malathion, 3×10 -10 gL -1 for diazinon and 3×10 -7 gL -1 for phosalone. The advantages of EVA-DLLME are the rapidity, simplicity, high sample throughput and low cost. As an outcome, the analytical results agreed fairly well with the results obtained by a reference GC-MS method. Copyright © 2017 Elsevier B.V. All rights reserved.

  5. Developments in gamma-ray spectrometry: systems, software, and methods-I. 5. Nuclear Spectral Analysis with Nonlinear Robust Fitting Techniques

    International Nuclear Information System (INIS)

    Lasche, G.P.; Coldwell, R.L.

    2001-01-01

    A new approach to nuclear spectral analysis based on nonlinear robust fitting techniques has been recently developed into a package suitable for public use. The methodology behind this approach was originally made available to the public as the RobFit command-line code, but it was extremely slow and difficult to use. Recent advances in microprocessor power and the development of a graphical user interface to make its use more intuitive have made this approach, which is quite computationally intensive, feasible for more routine applications. A brief description of some of the fundamental differences in the approach used by RobFit from the more common methods of nuclear spectral analysis involving local peak searches is presented here. Popular nuclear spectral analysis applications generally perform a peak search at their heart. The continuum in the neighborhood of each peak is estimated from local data and is subtracted from the data to yield the area and the energy of the peak. These are matched to a user-selected library of radionuclides containing the energies and areas of the most significant peaks, after accounting for the effects of detector efficiency and attenuation. With these codes, the energy-to-channel calibration, the peak width as a function of energy (or 'resolution calibration'), the detector intrinsic efficiency, and attenuation effects must usually be predetermined and provided as static input for the analysis. Most of these codes focus on regions of interest that represent many small pieces of the sample spectrum. In contrast, the RobFit approach works with an entire continuous spectrum to simultaneously determine the coefficients of all of the user-selected free variables that yield the best fit to the data. Peak searches are generally used only in interim steps to help suggest new radionuclides to include in the search library. Rather than first concentrate on the location of peaks, RobFit first concentrates on the determination of the continuum

  6. Imaging Mass Spectrometry in Neuroscience

    Science.gov (United States)

    2013-01-01

    Imaging mass spectrometry is an emerging technique of great potential for investigating the chemical architecture in biological matrices. Although the potential for studying neurobiological systems is evident, the relevance of the technique for application in neuroscience is still in its infancy. In the present Review, a principal overview of the different approaches, including matrix assisted laser desorption ionization and secondary ion mass spectrometry, is provided with particular focus on their strengths and limitations for studying different neurochemical species in situ and in vitro. The potential of the various approaches is discussed based on both fundamental and biomedical neuroscience research. This Review aims to serve as a general guide to familiarize the neuroscience community and other biomedical researchers with the technique, highlighting its great potential and suitability for comprehensive and specific chemical imaging. PMID:23530951

  7. Biópsia mamária realizada pela técnica de biópsia helicoide: estudo experimental Breast biopsy performed by the helicoid biopsy technique: an experimental study

    Directory of Open Access Journals (Sweden)

    Eliel de Souza

    2010-12-01

    Full Text Available OBJETIVO: avaliar o desempenho da biópsia helicoide na realização de biópsias mamárias. MÉTODOS: foi selecionado aleatoriamente uma amostra composta de 30 pacientes portadoras de câncer de mama submetidas à mastectomia. Foram excluídas as mulheres portadoras de tumor que tivessem consistência pétrea, não-palpável, com manipulação cirúrgica prévia ou que contivesse líquido. Utilizando-se o kit de biópsia helicoide e um equipamento de core biopsy com cânula e agulha de 14 gauge, respectivamente, coletou-se um fragmento por equipamento em área sã e nos tumores, em cada peça cirúrgica, totalizando 120 fragmentos para estudo histológico. Para a análise dos dados, definiu-se um nível de confiança de 95% e utilizou-se o software SPSS, versão 13; o índice de concordância Kappa e o teste paramétrico t de Student. RESULTADOS: a média das idades das pacientes foi de 51,6 anos (±11,1 anos. A core biopsy apresentou sensibilidade de 93,3%, especificidade de 100% e acurácia de 96,7%, enquanto a biópsia helicoide teve sensibilidade de 96,7%, especificidade de 100% e acurácia de 98,3%. Na comparação entre a histologia dos tumores e dos fragmentos de biópsias, houve alto grau de concordância nos diagnósticos (Kappa igual a 0,9, com pPURPOSE: to assess the helicoid biopsy performance when carrying out breast biopsies. METHODS: thirty patients with breast cancer submitted to mastectomy were selected at random. Women with a tumor of petreous consistency, nonpalpable, submitted to previous surgical manipulation or containing fluid were excluded. The helicoid biopsy kit and a core biopsy device with a cannula and a 14-gauge-needle, respectively, were used to collect a fragment each from a healthy area and from the tumor of each surgical specimen, for a total of 120 fragments for histological study. Data were analyzed statistically by the parametric Student's t-test and by the Kappa concordance index at the 95% confidence level

  8. Study of the parameters solution blow spinning technique in the obtaining of mullite nanofibers; Estudo de parametros da tecnica de fiacao por sopro em solucao na obtencao de nanofibras de mulita

    Energy Technology Data Exchange (ETDEWEB)

    Severo, L.L.; Farias, R.M.C.; Menezes, R.R.; Santos, M.A., E-mail: lucasleite_14.1@hotmail.com [Universidade Federal de Campina Grande (UFCG), PB (Brazil)

    2016-07-01

    The Solution Blow Spinning (SBS) technique which use aerodynamic forces and has a high production rate, was created for production of nanofiber with versatile way, such as electrospinning. Therefore, the objective is to analyze the process parameters in order to optimize the production of mullite nanofiber using the SBS technique to determine the influence of air pressure, the concentration of the polymer and ejection rate in the diameter of the fibers. For this, it was used PVC as polymer in spinning, tetrahydrofuran as the solvent, HCl as acidifying, aluminum nitrate nonahydrate and tetraethylorthosilicate as precursors of mullite. The nanofibers obtained were heat treated at 1100°C. From of XRD and SEM results, it was proved the achievement of mullite nanofiber, and STATISTICA 7 software revealed that only ejection rate and the concentration influence in the average diameters of the fibers. (author)

  9. Ampliação da técnica violonística de mão esquerda: um estudo sobre a pestana Extended left-hand guitar technique: a study on the barré

    Directory of Open Access Journals (Sweden)

    Bruno Madeira

    2013-06-01

    Full Text Available A técnica instrumental é um elemento da performance musical em constantes reformulações. Com o objetivo principal de estender a técnica violonística da pestana, o presente artigo foi dividido em três partes: (1 conceituações gerais sobre técnica instrumental; (2 a partir de métodos instrumentais dos últimos quatrocentos anos, um breve histórico da pestana foi delineado com o objetivo de recolher informações técnicas sobre sua realização, (3 sugestões e exemplificações de procedimentos não usuais de pestana (com dedos diferentes do indicador, de falange, bisagra e cruzada, encontrados de forma muito resumida na escassa bibliografia sobre o assunto e cuja aplicabilidade é verificada no repertório.Instrumental technique is an element of musical performance in constant reformulation. With the main objective of expanding the guitar technique of barring, this study was divided into three parts: (1 general concepts about instrumental technique; (2 from instrumental methods of the past four hundred years, a brief history of the barré was outlined in order to collect technical information about its realization, (3 suggestions and examples of unusual barring procedures (with different fingers, phalanx barré, hinge barré, crossed barré, found in the scarce bibliography and which applicability is verified in the repertoire.

  10. A new technique for the deposition of standard solutions in total reflection X-ray fluorescence spectrometry (TXRF) using pico-droplets generated by inkjet printers and its applicability for aerosol analysis with SR-TXRF

    International Nuclear Information System (INIS)

    Fittschen, U.E.A.; Hauschild, S.; Amberger, M.A.; Lammel, G.; Streli, C.; Foerster, S.; Wobrauschek, P.; Jokubonis, C.; Pepponi, G.; Falkenberg, G.; Broekaert, J.A.C.

    2006-01-01

    A new technique for the deposition of standard solutions on particulate aerosol samples using pico-droplets for elemental determinations with total reflection X-ray fluorescence spectrometry (TXRF) is described. It enables short analysis times without influencing the sample structure and avoids time consuming scanning of the sample with the exciting beam in SR-TXRF analysis. Droplets of picoliter volume (∼ 5-130 pL) were generated with commercially available and slightly modified inkjet printers operated with popular image processing software. The size of the dried droplets on surfaces of different polarity namely silicone coated and untreated quartz reflectors, was determined for five different printer types and ten different cartridge types. The results show that droplets generated by inkjet printers are between 50 and 200 μm in diameter (corresponding to volumes of 5 to 130 pL) depending on the cartridge type, which is smaller than the width of the synchrotron beam used in the experiments (< 1 mm at an energy of 17 keV at the beamline L at HASYLAB, Hamburg). The precision of the printing of a certain amount of a single element standard solution was found to be comparable to aliquoting with micropipettes in TXRF, where for 2.5 ng of cobalt relative standard deviations of 12% are found. However, it could be shown that the printing of simple patterns is possible, which is important when structured samples have to be analysed

  11. Estudos sobre o comportamento dos Planorbídeos: I - uma técnica de observação e registro comportamental por cinematografia Studies on the behavior of planorbids: I - a technique for behavioral observation and recording by use of cinematography

    Directory of Open Access Journals (Sweden)

    Otávio S. Pieri

    1980-01-01

    Full Text Available Uma técnica envolvendo cinematografia com lapso de tempo foi elaborada para o estudo da atividade comportamental dos planorbídeos em condições de laboratório. As observações realizam-se em uma câmara dotada de ciclo de iluminação dia-noite, e os registros são feitos com uma filmadora super-8, operada quadro a quadro, sob luz de flash estroboscópico. Essa técnica tem permitido mensurações rigorosas de diferentes aspectos do comportamento de Biomphalaria glabrata (say, 1818, e pode ser utilizada na análise do nível de resposta dos planorbídeos aos moluscicidas, em testes experimentais, e dos comportamentos de proteção frente a condições adversas em geral.A technique involving time-lapse cinematography was developed for studying the behavioral repertoire of planorbids in laboratory conditions. Observations were carried out within a chamber with controlled light and temperature; recording was done by single frame shooting at 10 second intervals, with synchronized strobed flash. This technique has allowed accurate measurements of different aspects of the activity of Biomphalaria glabrata (Say, 1818, and can be useful in analysing the level of response of planorbids to molluscicides, in experimental tests, as well as their protective behavior under general adverse conditions.

  12. Study of immobilization of radioactive wastes in asphaltic matrices and elastomeric residues by using microwave technique; Estudo da imobilizacao de rejeitos radioativos em matrizes asfalticas e residuos elastomericos utilizando a tecnica de microondas

    Energy Technology Data Exchange (ETDEWEB)

    Caratin, Reinaldo Leonel

    2007-07-01

    In the present work, the technique of microwave heating was used to study the immobilization of low and intermediate activity level radioactive waste, such as spent ion exchange resin used to remove undesirable ions of primary circuits of refrigeration in water refrigerated nuclear reactors, and those used in chemical and radionuclide separation columns in the quality control of radioisotopes. Bitumen matrices reinforced with some kinds of rubber (Neoprene{sup R}, silicon and ethylene-vinyl-acetate), from production leftovers or scraps, were used for incorporation of radioactive waste. The samples irradiation was made in a home microwave oven that operates at a frequency of 2.450 MHZ with 1.000 W power. The samples were characterized by developing assays on penetration, leaching resistance, softening, flash and combustion points, thermogravimetry and optical microscopy. The obtained results were compatible with the pattern of matrices components, which shows that technique is a very useful alternative to conventional immobilization methods and to those kinds of radioactive waste. (author)

  13. Comparative study of excipients for propanolol hydrochloryde tablets prepared by means of diferent techniques Estudo comparativo de excipientes em diferentes técnicas de preparação de comprimidos de cloridrato de propranolol

    Directory of Open Access Journals (Sweden)

    Cinara Maistro Mamprim

    2001-11-01

    Full Text Available Systemic arterial hipertension (SAH is one of the major factors in cardiovascular risk, since it contributes to the existence of more than 500 thousand cases of cerebral vascular accidents (CVA, 150 thousand deaths by cerebral hemorrhage and approximately a million myocardium infarctions (IAM. In Brazil, it is estimated that about 15% of the adult population can be considered hypertensive. Hypertension can be prevented by changes in lifestyle, although in most cases, the treatment with drugs becomes necessary. Propranolol hydrochloride is the drug chosen for the hypertensive elderly population who has had myocardium infarctation previously. The drug is commercially available as injections, solutions, capsules and tablets. Tablets can be prepared using three different techniques. The most used technique is the granulation by moisture. With the advance of new excipients available in the market for the Pharmaceutical Industry, a more simple and economical technique became possible, improving the physical and chemical stability of the product, reaching the goal of getting more efficient and safer medicine. The purpose of this study was to develop formulations of propranolol hydrochloride tablets through the variation of excipients and manufacture techniques. The propranolol hydrochloryde tablets were stored at 37o C and 50o C with 90% UR for 90 days, and analysed in pre-established time intervals the formulations were evaluated as for the physical and physical-chemical aspects.   A hipertensão arterial sistêmica (HAS é um dos mais importantes fatores de risco cardiovascular uma vez que contribui, mundialmente, com mais de 500 mil casos de acidentes cerebrovasculares (AVC, 150 mil mortes por hemorragia cerebral e aproximadamente um milhão de infartos de miocárdio (IAM. No Brasil estima-se que cerca de15% dos indivíduos adultos possam ser rotulados como hipertensos. A hipertensão pode ser prevenida com a mudança no estilo de vida, embora na

  14. Comparative study of AISI M3:2 high speed steel produced through different techniques of manufacturing; Estudo comparativo de acos rapidos AISI M3:2 produzidos por diferentes processos de fabricacao

    Energy Technology Data Exchange (ETDEWEB)

    Araujo Filho, Oscar Olimpio de

    2006-07-01

    In this work AISI M3:2 high speed steels obtained through different techniques of manufacturing, submitted to the same heat treatment procedure were evaluated by measuring their mechanical properties of transverse rupture strength and hardness. Sinter 23 obtained by hot isostatic pressing (HIP), VWM3C obtained by the conventional route and a M3:2 high speed steel obtained by cold compaction of water atomized powders and vacuum sintered with and without the addition of a small quantity of carbon were evaluated after the same heat treatment procedure. The vacuum sintered M3:2 high speed steel can be an alternative to the more expensive high speed steel produced by hot isostatic pressing and with similar properties presented by the conventional one. The characterization of the vacuum sintered M3:2 high speed steel was performed by measuring the densities of the green compacts and after the sintering cycle. The sintering produced an acceptable microstructure and densities near to the theoretical. The transverse rupture strength was evaluated by means of three point bending tests and the hardness by means of Rockwell C and Vickers tests. The technique of scanning electronic microscopy (SEM) was used to evaluate the microstructure and to establish a relation with the property of transverse rupture strength. The structure was determined by means of X-ray diffraction (XRD) patterns and the retained austenite was detected to all the conditions of heat treatment. The main contribution of this work is to establish a relation between the microstructure and the mechanical property of transverse rupture strength and to evaluate the AISI M3:2 vacuum sintered high speed steel as an alternative to the similar commercial high speed steels. (author)

  15. 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

  16. Comparação entre duas técnicas sorológicas aplicados ao estudo do sangue ingerido por triatomíneos Comparison between two serological technique used in the study of bloon sucked by arthropods

    Directory of Open Access Journals (Sweden)

    José Carlos Rehder de Andrade

    1975-12-01

    Full Text Available Comparou-se a técnica de reação de precipitina em tubos capilares com a de imunodifusão em gel de agar, em papéis contendo sangue de aves (galos ingerido por triatomíneos. Usaram-se 360 T. infestans e 270 P. megistus, estudando-se também a mortalidade comparativa das duas espécies. Os resultados sugerem que o método capilar apresenta ligeira vantagem. Quanto à mortalidade, a resistência ao jejum do T. infestans foi uniforme durante todo o tempo de observação, enquanto que, para o P. megistus a força de mortalidade foi pequena até o 50° dia de jejum, aumentando acentuadamente a seguir.The techniques of precipitin in capilar tubes and imunodifusion in agar jelly, for human blood sucked by arthropods were compared. 360 T. infestans and 270 P. megistus were observed, and the comparative mortality of both species was also studied. The results suggest that the capilar method is slightly better. As regards mortality, the resistance to fasting by the T. infestans was uniform during the whole period of observation, while for the P. megistus mortality was low until the 50th day of fasting, increasing markedly from then onwards.

  17. RETRATAMENTO ENDODÔNTICO: ESTUDO COMPARATIVO ENTRE TÉCNICA MANUAL, ULTRA-SOM E CANAL FINDER ENDODONTIC RETREATMENT: COMPARATIVE STUDY BETWEEN MANUAL TECHNIQUE, ULTRASONIC SCALER, AND CANAL FINDER

    Directory of Open Access Journals (Sweden)

    Clovis Monteiro BRAMANTE

    1998-01-01

    Full Text Available Instrumentações manual, ultra-sônica e com Canal Finder foram utilizadas para retratamento de 30 dentes com canais obturados com guta-percha e óxido de zinco e eugenol. Avaliaram-se: 1. tempo gasto para a penetração inicial até o ápice; 2. tempo para completar a limpeza; 3. extrusão de material e 4. limpeza dos canais. O Canal Finder foi a técnica que propiciou melhor limpeza, seguida da manual e da ultra-sônica. A parede palatina do canal foi constantemente mais limpa do que a vestibular. Quanto à extrusão, a técnica de ultra-som foi a que propiciou mais extravasamento de material obturador.Endodontic retreatment of 30 teeth filled with guta percha and zinc oxide-eugenol was carried out using manual instrumentation, ultrasonic scaler, and the Canal Finder System. The following variables were evaluated: time spent to reach the apex; time spent to complete cleaning of the canal; apical extrusion of material; and cleanliness of the canals. Results showed the Canal Finder System as providing the highest level of cleanliness of the canal system; lingual walls were constantly cleaner than buccal walls; ultrasonic technique presented a greater degree of apical extrusion of filling material.

  18. Mass Spectrometry Applications for Toxicology

    OpenAIRE

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

    2016-01-01

    Toxicology is a multidisciplinary study of poisons, aimed to correlate the quantitative and qualitative relationships between poisons and their physiological and behavioural effects in living systems. Other key aspects of toxicology focus on elucidation of the mechanisms of action of poisons and development of remedies and treatment plans for associated toxic effects. In these endeavours, Mass spectrometry (MS) has become a powerful analytical technique with a wide range of application used i...

  19. A REVIEW ON MASS SPECTROMETRY DETECTORS

    OpenAIRE

    Khatri Neetu; Gupta Ankit; Taneja Ruchi; Bilandi Ajay; Beniwal Prashant

    2012-01-01

    Mass spectrometry is an analytical technique for "weighing" molecules. Obviously, this is not done with a conventional scale or balance. Instead, mass spectrometry is based upon the principle of the motion of a charged particle that is called an ion, in an electric or magnetic field. The mass to charge ratio (m/z) of the ion affects particles motion. Since the charge of an electron is known, the mass to charge ratio (m/z) is a measurement of mass of an ion. Mass spectrometry research focuses ...

  20. Sea-to-air flux of dimethyl sulfide in the South and North Pacific Ocean as measured by proton transfer reaction-mass spectrometry coupled with the gradient flux technique

    Science.gov (United States)

    Omori, Yuko; Tanimoto, Hiroshi; Inomata, Satoshi; Ikeda, Kohei; Iwata, Toru; Kameyama, Sohiko; Uematsu, Mitsuo; Gamo, Toshitaka; Ogawa, Hiroshi; Furuya, Ken

    2017-07-01

    Exchange of dimethyl sulfide (DMS) between the surface ocean and the lower atmosphere was examined by using proton transfer reaction-mass spectrometry coupled with the gradient flux (PTR-MS/GF) system. We deployed the PTR-MS/GF system and observed vertical gradients of atmospheric DMS just above the sea surface in the subtropical and transitional South Pacific Ocean and the subarctic North Pacific Ocean. In total, we obtained 370 in situ profiles, and of these we used 46 data sets to calculate the sea-to-air flux of DMS. The DMS flux determined was in the range from 1.9 to 31 μmol m-2 d-1 and increased with wind speed and biological activity, in reasonable accordance with previous observations in the open ocean. The gas transfer velocity of DMS derived from the PTR-MS/GF measurements was similar to either that of DMS determined by the eddy covariance technique or that of insoluble gases derived from the dual tracer experiments, depending on the observation sites located in different geographic regions. When atmospheric conditions were strongly stable during the daytime in the subtropical ocean, the PTR-MS/GF observations captured a daytime versus nighttime difference in DMS mixing ratios in the surface air overlying the ocean surface. The difference was mainly due to the sea-to-air DMS emissions and stable atmospheric conditions, thus affecting the gradient of DMS. This indicates that the DMS gradient is strongly controlled by diurnal variations in the vertical structure of the lower atmosphere above the ocean surface.

  1. Evaluation of laser diode thermal desorption (LDTD) coupled with tandem mass spectrometry (MS/MS) for support of in vitro drug discovery assays: increasing scope, robustness and throughput of the LDTD technique for use with chemically diverse compound libraries.

    Science.gov (United States)

    Beattie, Iain; Smith, Aaron; Weston, Daniel J; White, Peter; Szwandt, Simon; Sealey, Laura

    2012-02-05

    Within the drug discovery environment, the key process in optimising the chemistry of a structural series toward a potential drug candidate is the design, make and test cycle, in which the primary screens consist of a number of in vitro assays, including metabolic stability, cytochrome P450 inhibition, and time-dependent inhibition assays. These assays are often carried out using multiple drug compounds with chemically diverse structural features, often in a 96 well-plate format for maximum time-efficiency, and are supported using rapid liquid chromatographic (LC) sample introduction with a tandem mass spectrometry (MS/MS) selected reaction monitoring (SRM) endpoint, taking around 6.5 h per plate. To provide a faster time-to-decision at this critical point, there exists a requirement for higher sample throughput and a robust, well-characterized analytical alternative. This paper presents a detailed evaluation of laser diode thermal desorption (LDTD), a relatively new ambient sample ionization technique, for compound screening assays. By systematic modification of typical LDTD instrumentation and workflow, and providing deeper understanding around overcoming a number of key issues, this work establishes LDTD as a practical, rapid alternative to conventional LC-MS/MS in drug discovery, without need for extensive sample preparation or expensive, scope-limiting internal standards. Analysis of both the five and three cytochrome P450 competitive inhibition assay samples by LDTD gave improved sample throughput (0.75 h per plate) and provided comparable data quality as the IC₅₀ values obtained were within 3 fold of those calculated from the LC-MS/MS data. Additionally when applied generically to a chemically diverse library of over 250 proprietary compounds from the AstraZeneca design, make and test cycle, LDTD demonstrated a success rate of 98%. Copyright © 2011 Elsevier B.V. All rights reserved.

  2. Investigation into the determination of trimethylarsine in natural gas and its partitioning into gas and condensate phases using (cryotrapping)/gas chromatography coupled to inductively coupled plasma mass spectrometry and liquid/solid sorption techniques

    International Nuclear Information System (INIS)

    Krupp, E.M.; Johnson, C.; Rechsteiner, C.; Moir, M.; Leong, D.; Feldmann, J.

    2007-01-01

    Speciation of trialkylated arsenic compunds in natural gas, pressurized and stable condensate samples from the same gas well was performed using (Cryotrapping) Gas Chromatography-Inductively Coupled Plasma Mass Spectrometry. The major species in all phases investigated was found to be trimethylarsine with a highest concentration of 17.8 ng/L (As) in the gas phase and 33.2 μg/L (As) in the stable condensate phase. The highest amount of trimethylarsine (121 μg/L (As)) was found in the pressurized condensate, along with trace amounts of non-identified higher alkylated arsines. Volatile arsenic species in natural gas and its related products cause concern with regards to environment, safety, occupational health and gas processing. Therefore, interest lies in a fast and simple field method for the determination of volatile arsenicals. Here, we use simple liquid and solid sorption techniques, namely absorption in silver nitrate solution and adsorption on silver nitrate impregnated silica gel tubes followed by total arsenic determination as a promising tool for field monitoring of volatile arsenicals in natural gas and gas condensates. Preliminary results obtained for the sorption-based methods show that around 70% of the arsenic is determined with these methods in comparison to volatile arsenic determination using GC-ICP-MS. Furthermore, an inter-laboratory- and inter-method comparison was performed using silver nitrate impregnated silica tubes on 14 different gas samples with concentrations varying from below 1 to 1000 μg As/m 3 natural gas. The results obtained from the two laboratories differ in a range of 10 to 60%, but agree within the order of magnitude, which is satisfactory for our purposes

  3. 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

  4. Estudo multicasos sobre atividades inovativas

    Directory of Open Access Journals (Sweden)

    Sonia Regina Hierro Parolin

    2013-09-01

    Full Text Available Em estudos sobre competitividade argumenta-se que as empresas necessitam de estratégias baseadas em inovações e de capacidades internas em constantes e intensas transformações, não somente nos padrões tecnológicos, mas também no encadeamento do processo de gestão das atividades inovativas, como processos dinâmicos, não lineares e diversificados, em função de múltiplos fatores dos ambientes interno e externo. Para contribuir com essas discussões, neste artigo apresenta-se um estudo multicasos em quatro indústrias de médio e grande portes, de segmentos, densidades tecnológicas e históricos com inovações diferentes entre si. Como principais resultados, salientam-se o encadeamento das atividades inovativas como parte de uma estratégia organizacional para obter resultados com inovação e a afluência de todas as pessoas, e não somente as alocadas em pesquisa e desenvolvimento, para o cumprimento dessa estratégia.

  5. Mass spectrometry of long-lived radionuclides

    International Nuclear Information System (INIS)

    Becker, Johanna Sabine.

    2003-01-01

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

  6. Eficácia de duas técnicas fonoaudiológicas da estética facial no músculo orbicular dos olhos: estudo piloto Efficacy of two techniques of speech-language pathologists of facial esthetic in the orbicular oculi muscle: a pilot study

    Directory of Open Access Journals (Sweden)

    Nayara Lana e Silva

    2010-08-01

    Full Text Available OBJETIVO: comparar a eficácia de duas técnicas fonoaudiológicas utilizadas no músculo orbicular dos olhos. MÉTODOS: foi realizado um estudo piloto com quatro pacientes, com idades entre 40 e 51 anos. As mesmas foram submetidas a um exercício miofuncional na hemiface esquerda e à massagem na hemiface direita, por um período de 20 dias. A coleta de dados foi realizada por meio de protocolos de anamnese, avaliação e reavaliação aplicados por uma dermatologista e por um cirurgião plástico, e pela avaliação de fotos realizada por 10 fonoaudiólogas especializandas em Motricidade Orofacial. RESULTADOS: foi constatado que não houve diferença nos resultados em relação às técnicas utilizadas no tratamento. Para a dermatologista e o cirurgião plástico todas as pacientes obtiveram melhora, sendo esta mais evidente na paciente 2 para a dermatologista e na paciente 4 para o cirurgião plástico. De acordo com as fonoaudiólogas houve melhora em todas as pacientes, sendo que a paciente 1 apresentou melhor resultado na hemiface esquerda e as demais mantiveram equilíbrio entre as hemifaces. CONCLUSÃO: com a realização deste estudo constatou-se que, na amostra avaliada, houve melhora nas rugas de expressão do músculo orbicular dos olhos sem diferenças entre as técnicas estudadas.PURPOSE: to compare the efficacy of two techniques speech-language pathologists used in the orbicular oculi muscle. METHODS: we conducted a pilot study with four patients, aged between 40 and 51 years. They were submitted to a myofunctional exercise in the left hemiface and to a massage in the right hemiface for a period of 20 days. Data collection was performed followed by historical protocols, then evaluation and review applied by dermatologist and plastic surgeon and by photos evaluation made by 10 speech therapist specializing in orofacial myology. RESULTS: it revealed that there were no differences on the results related to the techniques used during

  7. Mass spectrometry: a revolution in clinical microbiology?

    Science.gov (United States)

    Lavigne, Jean-Philippe; Espinal, Paula; Dunyach-Remy, Catherine; Messad, Nourredine; Pantel, Alix; Sotto, Albert

    2013-02-01

    Recently, different bacteriological laboratory interventions that decrease reporting time have been developed. These promising new broad-based techniques have merit, based on their ability to identify rapidly many bacteria, organisms difficult to grow or newly emerging strains, as well as their capacity to track disease transmission. The benefit of rapid reporting of identification and/or resistance of bacteria can greatly impact patient outcomes, with an improvement in the use of antibiotics, in the reduction of the emergence of multidrug resistant bacteria and in mortality rates. Different techniques revolve around mass spectrometry (MS) technology: matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF MS), PCR combined with electrospray ionization-mass spectrometry (PCR/ESIMS), iPLEX MassArray system and other new evolutions combining different techniques. This report emphasizes the (r)evolution of these technologies in clinical microbiology.

  8. Colestase neonatal prolongada: estudo prospectivo

    Directory of Open Access Journals (Sweden)

    PRADO Elizabeth Teixeira Mendes Livramento

    1999-01-01

    Full Text Available Em razão da urgência de se decidir por um tratamento clínico ou por uma intervenção cirúrgica imediata, o estudo da colestase neonatal prolongada envolve dois objetivos básicos: o diagnóstico diferencial entre atresia biliar e hepatite neonatal e a pesquisa dos agentes etiológicos associados. Desta maneira, através de estudo prospectivo desenvolvido na década de 1970, foram avaliadas 77 crianças portadoras de colestase neonatal prolongada para estabelecer o diagnóstico diferencial entre atresia biliar e hepatite neonatal e, numa segunda fase, 108 crianças, visando esclarecer a etiopatogenia da colestase neonatal prolongada. Os resultados do diagnóstico diferencial revelaram que, dos 18 atributos avaliados, apenas oito mostraram-se bons indicadores de atresia biliar, em ordem decrescente: ductos proliferados (espaço-porta, fibrose (espaço-porta, colestase (espaço-porta, cor das fezes -- acolia, hepatomegalia, colestase canalicular (lóbulo, infiltrado (espaço-porta, células gigantes (lóbulo. Estes oito atributos foram então compostos, mediante uma ponderação, em um único indicador de grande poder discriminativo, capaz de decidir o diagnóstico diferencial em 99% dos casos. Quanto à etiopatogenia, registrou-se: vírus rubéola 0%, vírus herpes simples 0%, listeriose 0%, citomegalovirose 2,2%, vírus hepatite B 2,4%, toxoplasmose 2,8%, deficiência de alfa-1-antitripsina 13,1%, sífilis 21,1 %, auto-anticorpos hepáticos 58,4%. O trabalho desenvolvido mostra que as 8 variáveis mais decisivas, como indicadoras diferenciais entre atresia biliar e hepatite neonatal, permanecem como índices fundamentais, auxiliando, em conjunto com novos métodos diagnósticos, na composição de uma estratégia multifatorial cada vez menos invasiva e mais precisa. O estudo da etiopatogenia, dependente das condições epidemiológicas locais e da época, com a introdução de novos métodos diagnósticos, torna-se atualmente cada vez mais

  9. Laser sputter neutral mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    King, B V; Clarke, M; Hu, H; Betz, [Newcastle Univ., NSW (Australia). Dept. of Physics

    1994-12-31

    Laser sputter neutral mass spectrometry (LSNMS) is an emerging technique for highly sensitive surface analysis. In this technique a target is bombarded with a pulsed beam of keV ions. The sputtered particles are intercepted by a high intensity pulsed laser beam above the surface and ionised with almost 100% efficiency. The photions may then be mass analysed using a quadrupole or, more commonly, using time of flight (TOF) techniques. In this method photoions are extracted from the ionisation region, accelerated to a known energy E{sub o} and strike a channelplate detector a distance `d` away. The flight time `t` of the photoions is then related to their mass by `d` {radical}m / {radical} 2E{sub o} so measurement of `t` allows mass spectra to be obtained. It is found that LSNMS is an emerging technique of great sensitivity and flexibility, useful for both applied analysis and to investigate basic sputtering processes. 4 refs., 3 figs.

  10. Laser sputter neutral mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    King, B.V.; Clarke, M.; Hu, H.; Betz [Newcastle Univ., NSW (Australia). Dept. of Physics

    1993-12-31

    Laser sputter neutral mass spectrometry (LSNMS) is an emerging technique for highly sensitive surface analysis. In this technique a target is bombarded with a pulsed beam of keV ions. The sputtered particles are intercepted by a high intensity pulsed laser beam above the surface and ionised with almost 100% efficiency. The photions may then be mass analysed using a quadrupole or, more commonly, using time of flight (TOF) techniques. In this method photoions are extracted from the ionisation region, accelerated to a known energy E{sub o} and strike a channelplate detector a distance `d` away. The flight time `t` of the photoions is then related to their mass by `d` {radical}m / {radical} 2E{sub o} so measurement of `t` allows mass spectra to be obtained. It is found that LSNMS is an emerging technique of great sensitivity and flexibility, useful for both applied analysis and to investigate basic sputtering processes. 4 refs., 3 figs.

  11. Analog to digital conversion for nuclear spectrometry

    International Nuclear Information System (INIS)

    Carvalho, P.V.R. de.

    1982-04-01

    A study of the analog to digital conversion techniques for nuclear spectrometry is presented and the main design philosophies of nuclear ADC's are compared. Among them, the most suitable for the current Brazilian conditions, concerning the specifications and components avaiability is the one that employs a statistical correction of successive approximation converters. This technique is described in full detail. A prototype has been developed an tested for the practical demonstration of the theoretical conclusions. These tests was carried on nuclear spectrometry data aquisition system whose implementation is also described. (Author) [pt

  12. Introduction to Body Composition Assessment Using the Deuterium Dilution Technique with Analysis of Urine Samples by Isotope Ratio Mass Spectrometry (Spanish Edition); Introduccion a la determinacion de la composicion corporal mediante la tecnica de dilucion de deuterio con analisis de muestras de orina por espectrometria de masas de relacion isotopica

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2013-11-15

    The IAEA has fostered the more widespread use of a stable isotope technique to assess body composition in different population groups to address priority areas in public health nutrition in Member States. It has done this by supporting national and regional nutrition projects through its technical cooperation programme and coordinated research projects over many years. This publication was developed by an international group of experts to provide practical hands-on guidance in the use of this technique in settings where analysis of stable isotope ratios in biological samples is to be made by isotope ratio mass spectrometry. The publication is targeted at new users of this technique, for example nutritionists, analytical chemists and other professionals. More detailed information on the theoretical background and the practical applications of state of the art methodologies to monitor changes in body composition can be found in IAEA Human Health Series No. 3, Assessment of Body Composition and Total Energy Expenditure in Humans by Stable Isotope Techniques.

  13. Halogen speciation in volcanic plumes - Development of compact denuder sampling techniques with in-situ derivatization followed by gas chromatography-mass spectrometry and their application at Mt. Etna, Mt. Nyiragongo and Mt. Nyamulagira in 2015.

    Science.gov (United States)

    Rüdiger, Julian; Bobrowski, Nicole; Hoffmann, Thorsten

    2016-04-01

    products. The diffusion denuder technique allows sampling of gaseous compounds exclusively without collecting particulate matter. Solvent elution of the derivatized analytes and subsequent analysis with gas chromatography-mass spectrometry gives a limit of detection below 1 ng of bromine. The method was applied in 2015 on volcanic gas plumes at Mt. Etna (Italy), Mt. Nyiragongo and Mt. Nyamulagira (DR Congo) giving reactive bromine mixing ratios from 0.3 ppb (Nyiragongo) up to 22 ppb (Etna, NEC). Compared with total halogen data derived by alkaline trap sampling (Raschig-tube) and ion-chromatography analysis the reactive bromine mixing ratios allow the investigation of the conversion of HBr into reactive species due to plume chemistry with progressing plume age. The new method will be described in detail and the first results on the reactive halogen to total halogen output will be discussed (for bromine and chlorine) and compared to earlier volcanic plume chemistry model studies. References Bobrowski, N. and G. Giuffrida: Bromine monoxide / sulphur dioxide ratios in relation to volcanological observations at Mt. Etna 2006-2009. Solid Earth, 3, 433-445, 2012 Bobrowski, N., R. von Glasow, A. Aiuppa, S. Inguaggiato, I. Louban, O. W. Ibrahim and U. Platt: Reactive halogen chemistry in volcanic plumes. J. Geophys. Res., 112, 2007 Donovan A., V. Tsanev, C. Oppenheimer and M. Edmonds: Reactive halogens (BrO and OClO) detected in the plume of Soufrière Hills Volcano during an eruption hiatus. Geochem. Geophys. Geosyst., 15, 3346-3363, 2014 Rüdiger, J., N. Bobrowski, T. Hoffmann (2015), Development and application of compact denuder sampling techniques with in situ derivatization followed by gas chromatography-mass spectrometry for halogen speciation in volcanic plumes (EGU2015-2392-2), EGU General Assembly 2015

  14. Application of neutron activation techniques and x-ray energy dispersion spectrometry, in analysis of metallic traces adsorbed by chelex-100 resin; Ativacao das tecnicas de ativacao neutronica e espectrometria por dispersao de onda e de energia de raios X, na analise de tracos metalicos adsorvidos pela resina chelex-100

    Energy Technology Data Exchange (ETDEWEB)

    Fernandes, Jair C.; Amaral, Angela M.; Magalhaes, Jesus C.; Pereira, Jose S.J.; Silva, Juliana B. da; Auler, Lucia M.L.A. [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN), Belo Horizonte, MG (Brazil)]. E-mail: jcf@urano.cdtn.br

    2000-07-01

    In this work, the authors have investigated optimal conditions of adsorption for several ion metallic groups (cations of heavy metals and transition metals, oxyanions metallics and metalloids and cations of rare earths), as traces (ppb), withdrawn and in mixture of groups, by chelex-100 resin. The experiments have been developed by bath techniques in ammonium acetate tamponade solution 40 mM pH 5,52 content 0,5 g of chelex-100 resin. After magnetic agitation for two hours, resins were dried and submitted to X-ray energy dispersion spectrometry, x-ray fluorescence spectrometry and neutron activation analysis. The results have demonstrated that chelex-100 resin adsorb quantitatively transition element groups and rare earth groups in two cases (withdrawn and simultaneously adsorption)

  15. Precision measurement of radioactivity in gamma-rays spectrometry using two HPGe detectors (BEGe-6530 and GC0818-7600SL models comparison techniques: Application to the soil measurement

    Directory of Open Access Journals (Sweden)

    Guembou Shouop Cebastien Joel

    2017-01-01

    • Proved that the activity concentration determination in gamma spectrometry depended on the energy range emitted by a radionuclide. This study showed that the standard deviation measurement was less important to the result realized with BEGe-6530 HPGe model. Our findings were demonstrated that the results of the Broad Energy Germanium detector were more reliable.

  16. Dehydroepiandrosterone sulfate quantification in serum using high-performance liquid chromatography/mass spectrometry and a deuterated internal standard: a technique suitable for routine use or as a reference method

    International Nuclear Information System (INIS)

    Shackleton, C.H.; Kletke, C.; Wudy, S.; Pratt, J.H.

    1990-01-01

    A thermospray high-performance liquid chromatography/mass spectrometry method for determination of serum dehydroepiandrosterone sulfate is described. The steroid was measured intact using [7,7-2H2]dehydroepiandrosterone sulfate as internal standard. The analysis was carried out in the negative ion mode by determining the peak height ratio of the molecular anions of the analyte and internal standard. The method was used to determine the steroid in serum from 15 male and female normal adults and the following values were obtained: males, 272 +/- 45 micrograms/dl (range, 197 to 331 micrograms/dl) and females, 215 +/- 67 micrograms/dl (range, 107 to 347 micrograms/dl). In addition, dehydroepiandrosterone sulfate was measured by high-performance liquid chromatography/mass spectrometry and radioimmunoassay (a commercial kit) on 25 individuals of all age groups. There was strong correlation between the values obtained, but the radioimmunoassay values were generally double those obtained by high-performance liquid chromatography/mass spectrometry. Three other steroid sulfates, androsterone sulfate, epiandrosterone sulfate, and androst-5-ene-3 beta, 17 beta-diol sulfate, were also assayed. In males, these had mean values of 112, 44, and 13 micrograms/dl and, in females, they had mean values of 84, 25, and 6 micrograms/dl, respectively. Radioimmunoassay cross-reactivity measurement for these steroids (as reference compounds) showed that they were unlikely to contribute greatly to the discrepancy between radioimmunoassay and high-performance liquid chromatography/mass spectrometry values

  17. [Latest development in mass spectrometry for clinical application].

    Science.gov (United States)

    Takino, Masahiko

    2013-09-01

    Liquid chromatography-tandem mass spectrometry (LC-MS/MS) has seen enormous growth in special clinical chemistry laboratories. It significantly increases the analytic potential in clinical chemistry, especially in the field of low molecular weight biomarker analysis. This review summarizes the state of the art in mass spectrometry and related techniques for clinical application with a main focus on recent developments in LC-MS. Current trends in ionization techniques, automated online sample preparation techniques coupled with LC-MS, and ion mobility spectrometry are discussed. Emerging mass spectrometric approaches complementary to LC-MS are discussed as well.

  18. Accelerator mass spectrometry.

    Science.gov (United States)

    Hellborg, Ragnar; Skog, Göran

    2008-01-01

    In this overview the technique of accelerator mass spectrometry (AMS) and its use are described. AMS is a highly sensitive method of counting atoms. It is used to detect very low concentrations of natural isotopic abundances (typically in the range between 10(-12) and 10(-16)) of both radionuclides and stable nuclides. The main advantages of AMS compared to conventional radiometric methods are the use of smaller samples (mg and even sub-mg size) and shorter measuring times (less than 1 hr). The equipment used for AMS is almost exclusively based on the electrostatic tandem accelerator, although some of the newest systems are based on a slightly different principle. Dedicated accelerators as well as older "nuclear physics machines" can be found in the 80 or so AMS laboratories in existence today. The most widely used isotope studied with AMS is 14C. Besides radiocarbon dating this isotope is used in climate studies, biomedicine applications and many other fields. More than 100,000 14C samples are measured per year. Other isotopes studied include 10Be, 26Al, 36Cl, 41Ca, 59Ni, 129I, U, and Pu. Although these measurements are important, the number of samples of these other isotopes measured each year is estimated to be less than 10% of the number of 14C samples. Copyright 2008 Wiley Periodicals, Inc.

  19. Atomic Absorption, Atomic Fluorescence, and Flame Emission Spectrometry.

    Science.gov (United States)

    Horlick, Gary

    1984-01-01

    This review is presented in six sections. Sections focus on literature related to: (1) developments in instrumentation, measurement techniques, and procedures; (2) performance studies of flames and electrothermal atomizers; (3) applications of atomic absorption spectrometry; (4) analytical comparisons; (5) atomic fluorescence spectrometry; and (6)…

  20. X-ray spectrometry for preventive conservation of cultural heritage

    Indian Academy of Sciences (India)

    Analytical chemistry does play a key role in the chemical characterization of the environment and it appears that X-ray spectrometry, in its many forms, is one of the most relevant analytical techniques in preventive conservation, as it is in cultural heritage research in general. X-ray spectrometry has indeed been the method ...

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

    International Nuclear Information System (INIS)

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

    1995-01-01

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

  2. Methods of neutron spectrometry

    International Nuclear Information System (INIS)

    Doerschel, B.

    1981-01-01

    The different methods of neutron spectrometry are based on the direct measurement of neutron velocity or on the use of suitable energy-dependent interaction processes. In the latter case the measuring effect of a detector is connected with the searched neutron spectrum by an integral equation. The solution needs suitable unfolding procedures. The most important methods of neutron spectrometry are the time-of-flight method, the crystal spectrometry, the neutron spectrometry by use of elastic collisions with hydrogen nuclei, and neutron spectrometry with the aid of nuclear reactions, especially of the neutron-induced activation. The advantages and disadvantages of these methods are contrasted considering the resolution, the measurable energy range, the sensitivity, and the experimental and computational efforts. (author)

  3. Grau de infiltração marginal de duas técnicas restauradoras com cimento de ionômero de vidro em molares decíduos: estudo comparativo " in vitro Microleakage between two filling restorative techniques using glass ionomer cement in primary molars: comparative "in vitro " study

    Directory of Open Access Journals (Sweden)

    Paulo Floriani Kramer

    2003-06-01

    Full Text Available A técnica do condicionamento ácido e o desenvolvimento e aprimoramento de novos materiais restauradores com características adesivas têm levado a mudanças importantes nas concepções e nos princípios da dentística operatória e restauradora. O objetivo deste estudo foi avaliar a microinfiltração marginal em cavidades proximais de molares decíduos restaurados com cimento de ionômero de vidro modificado por resina (Vitremer, 3M comparando duas diferentes técnicas: a técnica convencional (conforme recomendações do fabricante e a técnica de hibridização (ácido fosfórico-37% e sistema adesivo Scotchbond Multi-Uso, 3M . Foram utilizados 20 molares decíduos hígidos, onde foram preparadas cavidades proximais. A amostra foi dividida aleatoriamente em 2 grupos. No grupo 1 foi utilizado a técnica convencional e no grupo 2 a técnica com condicionamento ácido e aplicação de sistema adesivo. Os dentes foram submetidos ao processo de ciclagem térmica, impermeabilizados, mantendo uma área de 2mm² na margem cervical da restauração e imersos em solução de azul de metileno a 0,5%, por 72 horas. A seguir, foram seccionados e avaliados por um único examinador, que estabeleceu o grau de microinfiltração. Os dados obtidos revelaram que as duas técnicas utilizadas apresentaram microinfiltração marginal em diferentes graus, e que não houve diferença estatisticamente significante entre elas.This study evaluate the marginal microleakage in deciduous molars cavities restored with ionomer cement modified by resin (Vitremer, 3 M comparing two different techniques: the conventional (according to manufacturer instructions and with the hybridization technique (acid phosphoric 37% and adhesive system Scotchbond Multi Pourpose , 3M. Proximal cavities were prepared in 20 sound deciduous molars, right after extraction. The samples were randomly divided in two groups. Group 1 consisted in teeth prepared with the conventional technique and

  4. Estudo comparativo entre duas técnicas de tonsilectomia: bisturi harmônico (Ultracision e dissecção tradicional com bisturi de lâmina fria Comparative study between two tonsillectomy techniques: Ultracision harmonic scalpel and traditional dissection with cold scalpel

    Directory of Open Access Journals (Sweden)

    Fernando A. Ramos

    2004-06-01

    Full Text Available Tonsilectomia é a cirurgia realizada com maior frequência na clínica otorrinolaringológica. As modificações e as evoluções da técnica ocorrem no sentido de simplificar o procedimento e minimizar as complicações. O bisturi harmônico (Ultracision começou a ser utilizado na Otorrinolaringologia em 1999 para tonsilectomia com bons resultados. OBJETIVO: O objetivo deste estudo foi comparar o tempo cirúrgico, sangramento e hemostasia trans-operatórios, dor pós-operatória, aspecto cicatricial da loja tonsilar e intercorrências no trans e pós-operatório em pacientes submetidos a tonsilectomia pela técnica tradicional com lâmina fria e pela técnica utilizando lâmina cirúrgica em ganchos de coagulação Ultracision. FORMA DE ESTUDO: Coorte transversal. CASUÍSTICA E MÉTODO: Vinte e seis pacientes foram submetidos a tonsilectomia: 13 pela técnica tradicional com bisturi de lâmina fria e 13 pela técnica com Ultracision, avaliando os parâmetros previamente estabelecidos através de um protocolo padrão. Os pacientes foram submetidos a uma análise da intensidade da dor através da escala analógica visual horizontal. RESULTADOS: O tempo cirúrgico foi estatisticamente menor na cirurgia realizada pela técnica com o bisturi harmônico comparada com a técnica tradicional. O percentual de pontos dados na loja tonsilar também mostrou-se mais baixo do que pela técnica tradicional. Não houve diferença significativa em relação ao padrão de dor e a evolução pós-operatória do aspecto cicatricial da loja. CONCLUSÃO: O bisturi harmônico mostrou ser um excelente recurso para a realização de cirurgias onde o tempo cirúrgico e o sangramento trans-operatório são de grande importância.Tonsillectomy is the most commom surgical procedure in Otolaringology. The modifications and the technique surgical evolutions aim to simplifly and reduce the complications. The UltacisionÒ harmonic scalpel begin to be used in 1999 in

  5. Functional genomics by mass spectrometry

    DEFF Research Database (Denmark)

    Andersen, Jens S.; Mann, M

    2000-01-01

    Systematic analysis of the function of genes can take place at the oligonucleotide or protein level. The latter has the advantage of being closest to function, since it is proteins that perform most of the reactions necessary for the cell. For most protein based ('proteomic') approaches to gene f...... numbers of intact proteins by mass spectrometry directly. Examples from this laboratory illustrate biological problem solving by modern mass spectrometric techniques. These include the analysis of the structure and function of the nucleolus and the analysis of signaling complexes....

  6. Mass spectrometry a versatile aid to inorganic analysis

    International Nuclear Information System (INIS)

    Stefani, Rene

    1976-01-01

    Several hundred publications have appeared in the last three years that deal with applications of Mass Spectrometry to inorganic analysis. Bulk and localized trace analysis, surface and thin film characterization and microstructure examination are currently performed by Secondary Ion Mass Spectrometry, Spark Source Mass Spectrometry and the newly developed Laser Probe Mass Spectrometry. Suitable experimental procedures allow insulators, biologic materials and microsamples to be analysed. In spite of the classification by techniques this review is essentially devoted to the most significant papers in analytical applications but instrumental and basic features are sometimes introduced to support the discussions

  7. Thirteenth ISMAS symposium cum workshop on spectrometry

    International Nuclear Information System (INIS)

    Aggarwal, S.K.; Jaison, P.G.; Alamelu, D.

    2008-01-01

    Mass spectrometry is an important analytical tool and finds applications in almost all branches of science and technology like Physics, Chemistry, Biology, Material Science, Geology, Nuclear Science, Industry, Oceanography, Environment etc. Innovations in the designs of mass spectrometers coupled with new ionization techniques have further strengthened the capabilities of mass spectrometry for analyzing all types of molecules including thermally labile and non-volatile at concentrations down to femto gram levels. The applications of mass spectrometry to the biomedical sciences have provided a unique, easy and fast approach to genomics, proteomics and metabolomics. The availability of different types of mass spectrometers for inorganic elemental and isotopic composition determination have strengthened the role of mass spectrometry for analyzing all elements starting from hydrogen onwards. It is now possible to carry out speciation analysis using electrospray mass spectrometry. The individual conference papers in the proceedings covers fundamentals of mass spectrometry, qualitative and quantitative aspects and data interpretation, maintenance of mass spectrometers, selection of mass spectrometer, and recent advances in the field. Papers relevant to INIS are indexed separately

  8. Mass spectrometry in nuclear science and technology

    International Nuclear Information System (INIS)

    Komori, Takuji

    1985-01-01

    Mass spectrometry has been widely used and playing a very important role in the field of nuclear science and technology. A major reason for this is that not only the types of element but also its isotopes have to be identified and measured in this field. Thus, some applications of this analytical method are reviewed and discussed in this article. Its application to analytical chemistry is described in the second section following an introductory section, which includes subsections for isotropic dilution mass spectrometry, resonance ionization mass spectrometry and isotopic correlation technique. The isotopic ratio measurement for hydrogen, uranium and plutonium as well as nuclear material control and safeguards are also reviewed in this section. In the third section, mass spectrometry is discussed in relation to nuclear reactors, with subsections on natural uranium reactor and neutron flux observation. Some techniques for measuring the burnup fraction, including the heavy isotopic ratio method and fission product monitoring, are also described. In the fourth section, application of mass spectrometry to measurement of nuclear constants, such as ratio of effective cross-sectional area for 235 U, half-life and fission yield is reviewed. (Nogami, K.)

  9. Gamma ray spectrometry: applications in uranium prospecting and environment

    International Nuclear Information System (INIS)

    Lopez, Luis E.

    1999-01-01

    The experience in the use of gamma spectrometry for uranium prospecting and for the determination of natural radiation background is described. The basic principles of the techniques are also given. (author)

  10. Gas Chromatography Mass Spectrometry of Quassia undulata Seed ...

    African Journals Online (AJOL)

    Prof. Ogunji

    The use of gas chromatography mass spectrometry (GC MS) as a sensitive and specific technique ... cold flow properties and stability of the fuel to oxidation, peroxidation and polymerization .... determinants of both the physical and chemical ...

  11. Hands-on Electrospray Ionization-Mass Spectrometry for Upper-Level Undergraduate and Graduate Students

    Science.gov (United States)

    Stock, Naomi L.; March, Raymond E.

    2014-01-01

    Electrospray ionization-mass spectrometry (ESI-MS) is a powerful technique for the detection, identification, and quantification of organic compounds. As mass spectrometers have become more user-friendly and affordable, many students--often with little experience in mass spectrometry--find themselves needing to incorporate mass spectrometry into…

  12. Disturbios da olfacao: estudo retrospectivo

    Directory of Open Access Journals (Sweden)

    Luciano Lobato Gregorio

    2014-01-01

    Full Text Available Introdução: O olfato, fenômeno subjetivo de grande importância, é pouco compreendido e estudado no ser humano. Médicos com maior conhecimento sobre os distúrbios desse sentido tendem a considerar a doença mais importante e manejar melhor o diagnóstico e o tratamento. Objetivo: Descrever a amostra dos pacientes com queixa principal de distúrbios do olfato e mostrar a experiência do serviço no manejo e tratamento. Delineamento: Estudo retrospectivo de coorte histórica com corte transversal. Materiais e métodos: Descrição da amostra e avaliação de resposta ao tratamento de pacientes com queixa principal de hiposmia ou anosmia atendidos no ambulatório de Rinologia no período de janeiro de 2005 a outubro de 2011. Resultados: Dos 38 pacientes com distúrbio da olfação, 68,4% dos pacientes apresentaram queixa de hiposmia e 31,5% de anosmia, com duração média de 30,8 meses. Os diagnósticos etiológicos principais foram idiopática (31,5%, rinopatia alérgica (28,9% e RSC com pólipos (10,5%. As respostas ao tratamento com corticosteroide tópico e ácido alfa-lipoico foram variáveis, assim como na literatura. Conclusão: Maior importância deve ser dada aos distúrbios do olfato na prática do otorrinolaringologista, uma vez que o diagnóstico diferencial é amplo e pode trazer grande morbidade ao paciente, com impacto na sua qualidade de vida.

  13. Polymer and Additive Mass Spectrometry Literature Review

    Energy Technology Data Exchange (ETDEWEB)

    Shear, Trevor Allan [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

    2017-06-06

    The use of mass spectrometry in fields related to polymers has increased significantly over the past three decades and will be explored in this literature review. The importance of this technique is highlighted when exploring how polymers degrade, verifying purchased materials, and as internal requirements change. The primary focus will be on four ionization techniques and the triple quadrupole and quadrupole / time-of-flight mass spectrometers. The advantages and limitations of each will also be explored.

  14. Mass spectrometry and tandem mass spectrometry of citrus limonoids.

    Science.gov (United States)

    Tian, Qingguo; Schwartz, Steven J

    2003-10-15

    structure. CAD of the adduct ion [M + H + NH3]+ of limonoid glucosides produced the aglycone moiety corresponding to each glucoside. The combination of mass spectrometry and tandem mass spectrometry provides a powerful technique for identification and characterization of citrus limonoids.

  15. Estudo prospectivo comparativo de duas modalidades de posicionamento do sensor de phmetria esofágica prolongada: por manometria esofágica e pela viragem do Ph Comparative prospective study of two positioning modes of 24-hour esophageal pH monitoring: by esophageal manometry and by the pH step-up technique

    Directory of Open Access Journals (Sweden)

    Ary Nasi

    2008-12-01

    incluídos todos pacientes que aceitaram participar da pesquisa e excluídos os casos nos quais não se identificou acidificação intragástrica. RESULTADOS: Se fosse adotada a técnica da viragem, haveria erro no posicionamento do sensor em 945 pacientes (91,6%, portanto, o sensor seria posicionado na posição padronizada em apenas 86 (8,4% casos. Em relação à caracterização do grau de erro, haveria erro considerado grosseiro em 597 (63,2% pacientes. Em relação ao tipo de erro, o sensor seria posicionado abaixo do local padronizado em 857 (90,7% casos. Não houve diferença significante entre os dois grupos de estudo em relação a nenhum dos parâmetros analisados, indicando que a posição adotada pelo paciente durante a manobra da viragem não interfere no erro inerente à técnica. CONCLUSÕES: 1. O posicionamento do sensor distal de pHmetria pela técnica da viragem do pH não é confiável. 2. A técnica da viragem proporciona margem de erro expressiva. 3. O tipo de erro mais comum que tal modalidade técnica proporciona é o posicionamento mais distal do sensor, que pode superestimar a ocorrência de refluxo. 4. Não há influência da posição adotada pelo paciente durante a realização da técnica da viragem do pH na eficiência do método.BACKGROUND: By internationally accepted standardization, the esophageal pH-meter distal sensor is positioned 5 cm above the superior border of the lower esophageal sphincter, identified by esophageal manometry. However, several authors suggest alternative positioning techniques that leave out the manometry; among such techniques, the pH step-up is the one to be pointed out. This subject is controversial; some publications state that the step-up technique is not reliable while some others consider it reliable. AIMS: Considering the existent controversy and the small number of prospective works with suitable sample and methodology, we have idealized the present study, that aims the evaluation of the suitability of

  16. Atomic electron spectrometry with synchrotron radiation

    International Nuclear Information System (INIS)

    Sorensen, S.L.

    1989-01-01

    Techniques of atomic electron spectrometry were applied to atoms in the gaseous and solid states to derive information about fundamental atomic properties. A new method was developed to measure Coster-Kronig yields in metals by photoionization with synchrotron radiation. Photon-energy sensitive Si L-VV Auger satellites were investigated via electron spectrometry. The krypton 1s photoionization spectrum was measured in an experiment which was motivated by the need to understand the krypton 1s satellite spectrum for calibration of an experiment to measure the mass of the electron antineutrino

  17. Chemical analysis of refractories by plasma spectrometry

    International Nuclear Information System (INIS)

    Coutinho, C.A.

    1990-01-01

    X-ray spectrometry has been, since the last two or three decades, the traditional procedure for the chemical analysis of refractories, due to its high degree of accuracy and speed to produce analytical results. An interesting alternative to X-ray fluorescence is provided by the Inductively Coupled Plasma Spectrometry technique, for those laboratories where wet chemistry facilities are already available or process control is not required at high speed, or investiment costs have to be low. This paper presents results obtained by plasma spectroscopy for the analysis of silico - aluminous refractories, showing calibration curves, precion and detection limits. Considerations and comparisons with X-ray fluorescence are also made. (author) [pt

  18. Software for nuclear spectrometry

    International Nuclear Information System (INIS)

    1998-10-01

    The Advisory Group Meeting (AGM) on Software for Nuclear Spectrometry was dedicated to review the present status of software for nuclear spectrometry and to advise on future activities in this field. Because similar AGM and consultant's meetings had been held in the past; together with an attempt to get more streamlined, this AGM was devoted to the specific field of software for gamma ray spectrometry. Nevertheless, many of the issues discussed and the recommendations made are of general concern for any software on nuclear spectrometry. The report is organized by sections. The 'Summary' gives conclusions and recommendations adopted at the AGM. These conclusions and recommendations resulted from the discussions held during and after presentations of the scientific and technical papers. These papers are reported here in their integral form in the following Sections

  19. Mass spectrometry for characterizing plant cell wall polysaccharides

    Directory of Open Access Journals (Sweden)

    Stefan eBauer

    2012-03-01

    Full Text Available Mass spectrometry is a selective and powerful technique to obtain identification and structural information on compounds present in complex mixtures. Since it requires only small sample amount it is an excellent tool for researchers interested in detecting changes in composition of complex carbohydrates of plants. This mini-review gives an overview of common mass spectrometry techniques applied to the analysis of plant cell wall carbohydrates. It presents examples in which mass spectrometry has been used to elucidate the structure of oligosaccharides derived from hemicelluloses and pectins and illustrates how information on sequence, linkages, branching and modifications are obtained from characteristic fragmentation patterns.

  20. Glycomics using mass spectrometry

    OpenAIRE

    Wuhrer, Manfred

    2013-01-01

    Mass spectrometry plays an increasingly important role in structural glycomics. This review provides an overview on currently used mass spectrometric approaches such as the characterization of glycans, the analysis of glycopeptides obtained by proteolytic cleavage of proteins and the analysis of glycosphingolipids. The given examples are demonstrating the application of mass spectrometry to study glycosylation changes associated with congenital disorders of glycosylation, lysosomal storage di...

  1. Ion mobility spectrometry

    CERN Document Server

    Eiceman, GA

    2005-01-01

    Key Developments for Faster, More Precise Detection Capabilities Driven by the demand for the rapid and advanced detection of explosives, chemical and biological warfare agents, and narcotics, ion mobility spectrometry (IMS) undergone significant refinements in technology, computational capabilities, and understanding of the principles of gas phase ion chemistry and mobility. Beginning with a thorough discussion of the fundamental theories and physics of ion mobility, Ion Mobility Spectrometry, Second Edition describes the recent advances in instrumentation and newly

  2. High-Performance Liquid Chromatography-Mass Spectrometry.

    Science.gov (United States)

    Vestal, Marvin L.

    1984-01-01

    Reviews techniques for online coupling of high-performance liquid chromatography with mass spectrometry, emphasizing those suitable for application to nonvolatile samples. Also summarizes the present status, strengths, and weaknesses of various techniques and discusses potential applications of recently developed techniques for combined liquid…

  3. [Imaging Mass Spectrometry in Histopathologic Analysis].

    Science.gov (United States)

    Yamazaki, Fumiyoshi; Seto, Mitsutoshi

    2015-04-01

    Matrix-assisted laser desorption/ionization (MALDI)-imaging mass spectrometry (IMS) enables visualization of the distribution of a range of biomolecules by integrating biochemical information from mass spectrometry with positional information from microscopy. IMS identifies a target molecule. In addition, IMS enables global analysis of biomolecules containing unknown molecules by detecting the ratio of the molecular weight to electric charge without any target, which makes it possible to identify novel molecules. IMS generates data on the distribution of lipids and small molecules in tissues, which is difficult to visualize with either conventional counter-staining or immunohistochemistry. In this review, we firstly introduce the principle of imaging mass spectrometry and recent advances in the sample preparation method. Secondly, we present findings regarding biological samples, especially pathological ones. Finally, we discuss the limitations and problems of the IMS technique and clinical application, such as in drug development.

  4. Sequencing Cyclic Peptides by Multistage Mass Spectrometry

    Science.gov (United States)

    Mohimani, Hosein; Yang, Yu-Liang; Liu, Wei-Ting; Hsieh, Pei-Wen; Dorrestein, Pieter C.; Pevzner, Pavel A.

    2012-01-01

    Some of the most effective antibiotics (e.g., Vancomycin and Daptomycin) are cyclic peptides produced by non-ribosomal biosynthetic pathways. While hundreds of biomedically important cyclic peptides have been sequenced, the computational techniques for sequencing cyclic peptides are still in their infancy. Previous methods for sequencing peptide antibiotics and other cyclic peptides are based on Nuclear Magnetic Resonance spectroscopy, and require large amount (miligrams) of purified materials that, for most compounds, are not possible to obtain. Recently, development of mass spectrometry based methods has provided some hope for accurate sequencing of cyclic peptides using picograms of materials. In this paper we develop a method for sequencing of cyclic peptides by multistage mass spectrometry, and show its advantages over single stage mass spectrometry. The method is tested on known and new cyclic peptides from Bacillus brevis, Dianthus superbus and Streptomyces griseus, as well as a new family of cyclic peptides produced by marine bacteria. PMID:21751357

  5. Recent advances in nuclear techniques for environmental radioactivity monitoring

    International Nuclear Information System (INIS)

    Kumar, Ajay; Tripathi, R.M.

    2016-01-01

    The environmental radioactivity monitoring was first started in the late 1950s following the global fallout from testing of nuclear weapons in the atmosphere. Nuclear analytical techniques are generally classified into two categories: destructive and non-destructive. Destructive techniques are carried out through several analytical methods such as α-spectrometry, liquid Scintillation counting system, solid state nuclear track detector, spectrophotometry, fluorimetry, atomic absorption spectrometry (AAS), inductively coupled plasma mass spectrometry (ICP-MS), inductively coupled plasma optical emission spectrometry (ICP-OES), chromatography techniques, electro-analytical techniques etc. However, nondestructive methods include gamma spectrometry, X-Ray fluorescence (XRF) spectrometry, neutron activation analysis (NAA) etc. The development of radiochemical methods and measurement techniques using alpha and gamma spectrometry have been described in brief

  6. Characterizing the lipid and metabolite changes associated with placental function and pregnancy complications using ion mobility spectrometry-mass spectrometry and mass spectrometry imaging

    Energy Technology Data Exchange (ETDEWEB)

    Burnum-Johnson, Kristin E.; Baker, Erin S.; Metz, Thomas O.

    2017-12-01

    Successful pregnancy is dependent upon discrete biological events, which include embryo implantation, decidualization, and placentation. Problems associated with each of these events can cause infertility or conditions such as preeclampsia. A greater understanding of the molecular changes associated with these complex processes is necessary to aid in identifying treatments for each condition. Previous nuclear magnetic resonance spectroscopy and mass spectrometry studies have been used to identify metabolites and lipids associated with pregnancy-related complications. However, due to limitations associated with conventional implementations of both techniques, novel technology developments are needed to more fully understand the initiation and development of pregnancy related problems at the molecular level. In this perspective, we describe current analytical techniques for metabolomic and lipidomic characterization of pregnancy complications and discuss the potential for new technologies such as ion mobility spectrometry-mass spectrometry and mass spectrometry imaging to contribute to a better understanding of the molecular changes that affect the placenta and pregnancy outcomes.

  7. Introduction to Body Composition Assessment Using the Deuterium Dilution Technique with Analysis of Saliva Samples by Fourier Transform Infrared Spectrometry (Spanish Edition); Introduccion a la determinacion de la composicion corporal mediante la tecnica de dilucion de deuterio con analisis de muestras de saliva por espectrometria infrarroja por transformada de Fourier

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2013-12-15

    For many years, the IAEA has fostered the more widespread use of stable isotope techniques to assess body composition in different population groups to address priority areas in public health nutrition in Member States. The objective is to support national and regional nutrition projects through both the IAEA's technical cooperation programme and its coordinated research projects. In particular, during the last few years, the increased access to analyses of deuterium enrichment by Fourier transform infrared (FTIR) spectrometry has increased the application of this technique in Africa, Asia and Latin America. This publication was developed by an international group of experts to provide practical, hands-on guidance in the use of this technique in settings where the analysis of deuterium enrichment in saliva samples will be made by FTIR. It is targeted at new users of this technique, for example nutritionists, analytical chemists and other professionals. More detailed information on the theoretical background and the practical application of state of the art methodologies to monitor changes in body composition can be found in an IAEA publication entitled Assessment of Body Composition and Total Energy Expenditure in Humans by Stable Isotope Techniques (IAEA Human Health Series No. 3)

  8. ESTUDOS ESTILÍSTICOS NO BRASIL

    Directory of Open Access Journals (Sweden)

    Carlos Eduardo Falcão Uchôa

    2013-06-01

    Full Text Available Este artigo objetiva mostrar os inícios e a progressão dos estudos estilísticos no Brasil. Após uma introdução sobre o surgimento, na Europa, da Estilística como disciplina de pesquisa no campo da linguagem, detém-se, sucessivamente, nas contribuições de filólogos, linguistas, teóricos da literatura e gramáticos para o estudo dos mais variados recursos estilísticos ocorrentes sobretudo em autores brasileiros.

  9. The evaluation of the x-ray fluorescence (XRF) technique for process monitoring of vitreous slag from thermal waste treatment systems: A comparative study of the analysis of Plasma Hearth slag for Ce, Fe and Cr by XRF and inductively coupled plasma spectrometries

    International Nuclear Information System (INIS)

    Sutton, M.A.H.; Crane, P.J.; Cummings, D.G.; Carney, K.P.

    1995-05-01

    Slag material produced by the Plasma Hearth Process (PHP) varies in chemical composition due to the heterogeneous nature of the input sample feed. X-ray fluorescence (XRF) is a spectroscopic technique which has been evaluated to perform elemental analyses on surrogate slag material for process control. Vitreous slag samples were ground to a fine powder in an impact ball mill and analyzed directly using laboratory prepared standards. The fluorescent intensities of Si, Al and Fe in the slag samples was utilized to determine the appropriate matrix standard set for the determination of Ce. The samples were analyzed for Cr, Ni, Fe and Ce using a wavelength dispersive XRF polychromator. Split samples were dissolved and analyzed by Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES). The precision of the XRF technique was better than 5% RSD. The limit of detection for Ce varied with sample matrix and was typically below 0.01% by weight. The linear dynamic range for the technique was evaluated over two orders of magnitude. Typical calibration standards ranged from 0.01% Ce to 1% Ce. The Ce determinations performed directly on ground slag material by the XRF techniques were similar to ICP-AES analyses. Various chemical dissolution and sample preparation techniques were evaluated for the analysis of Ce in slag samples. A fusion procedure utilizing LiBO 2 was found to provide reliable analyses for the actinide surrogate in a variety of slag matrices. The use of the XRF technique reduced the time of analysis for Ce and Cr from three days to one day for five samples. No additional waste streams were created from the analyses by the XRF technique, while the ICP technique generated several liters of liquid waste

  10. Quantitative mass spectrometry: an overview

    Science.gov (United States)

    Urban, Pawel L.

    2016-10-01

    Mass spectrometry (MS) is a mainstream chemical analysis technique in the twenty-first century. It has contributed to numerous discoveries in chemistry, physics and biochemistry. Hundreds of research laboratories scattered all over the world use MS every day to investigate fundamental phenomena on the molecular level. MS is also widely used by industry-especially in drug discovery, quality control and food safety protocols. In some cases, mass spectrometers are indispensable and irreplaceable by any other metrological tools. The uniqueness of MS is due to the fact that it enables direct identification of molecules based on the mass-to-charge ratios as well as fragmentation patterns. Thus, for several decades now, MS has been used in qualitative chemical analysis. To address the pressing need for quantitative molecular measurements, a number of laboratories focused on technological and methodological improvements that could render MS a fully quantitative metrological platform. In this theme issue, the experts working for some of those laboratories share their knowledge and enthusiasm about quantitative MS. I hope this theme issue will benefit readers, and foster fundamental and applied research based on quantitative MS measurements. This article is part of the themed issue 'Quantitative mass spectrometry'.

  11. Mass Spectrometry Applications for Toxicology.

    Science.gov (United States)

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

    2016-12-01

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

  12. Mass Spectrometry Applications for Toxicology

    Science.gov (United States)

    Mbughuni, Michael M.; Jannetto, Paul J.

    2016-01-01

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

  13. Fourier Transform Mass Spectrometry

    Science.gov (United States)

    Scigelova, Michaela; Hornshaw, Martin; Giannakopulos, Anastassios; Makarov, Alexander

    2011-01-01

    This article provides an introduction to Fourier transform-based mass spectrometry. The key performance characteristics of Fourier transform-based mass spectrometry, mass accuracy and resolution, are presented in the view of how they impact the interpretation of measurements in proteomic applications. The theory and principles of operation of two types of mass analyzer, Fourier transform ion cyclotron resonance and Orbitrap, are described. Major benefits as well as limitations of Fourier transform-based mass spectrometry technology are discussed in the context of practical sample analysis, and illustrated with examples included as figures in this text and in the accompanying slide set. Comparisons highlighting the performance differences between the two mass analyzers are made where deemed useful in assisting the user with choosing the most appropriate technology for an application. Recent developments of these high-performing mass spectrometers are mentioned to provide a future outlook. PMID:21742802

  14. Ambient ionization mass spectrometry

    International Nuclear Information System (INIS)

    Lebedev, A T

    2015-01-01

    Ambient ionization mass spectrometry emerged as a new scientific discipline only about ten years ago. A considerable body of information has been reported since that time. Keeping the sensitivity, performance and informativity of classical mass spectrometry methods, the new approach made it possible to eliminate laborious sample preparation procedures and triggered the development of miniaturized instruments to work directly in the field. The review concerns the theoretical foundations and design of ambient ionization methods. Their advantages and drawbacks, as well as prospects for application in chemistry, biology, medicine, environmetal analysis, etc., are discussed. The bibliography includes 194 references

  15. O desamparo aprendido revisitado: estudos com animais

    Directory of Open Access Journals (Sweden)

    Maria Helena Leite Hunziker

    Full Text Available O desamparo aprendido tem sido definido como a dificuldade de aprendizagem apresentada por indivíduos que tiveram experiência prévia com estímulos aversivos incontroláveis. O objetivo deste trabalho é fazer uma revisão crítica dos estudos sobre o desamparo aprendido, com animais. Nessa análise, são considerados aspectos conceituais e metodológicos dos estudos em questão e as interpretações teóricas sobre esse efeito comportamental. Aborda-se a evolução histórica desses estudos, bem como alguns aspectos controversos das publicações que se acumularam ao longo de quatro décadas de pesquisa. A associação do desamparo aprendido com a depressão clínica é analisada criticamente, destacando-se a necessidade de maior rigor metodológico e conceitual nos estudos da área.

  16. Neutron fluence spectrometry using disk activation

    International Nuclear Information System (INIS)

    Loevestam, Goeran; Hult, Mikael; Fessler, Andreas; Gasparro, Joel; Kockerols, Pierre; Okkinga, Klaas; Tagziria, Hamid; Vanhavere, Filip; Wieslander, J.S. Elisabeth

    2009-01-01

    A simple and robust detector for spectrometry of environmental neutrons has been developed. The technique is based on neutron activation of a series of different metal disks followed by low-level gamma-ray spectrometry of the activated disks and subsequent neutron spectrum unfolding. The technique is similar to foil activation but here the applied neutron fluence rates are much lower than usually in the case of foil activation. The detector has been tested in quasi mono-energetic neutron fields with fluence rates in the order of 1000-10000 cm -2 s -1 , where the obtained spectra showed good agreement with spectra measured using a Bonner sphere spectrometer. The detector has also been tested using an AmBe source and at a neutron fluence rate of about 40 cm -2 s -1 , again, a good agreement with the assumed spectrum was achieved

  17. Neutron fluence spectrometry using disk activation

    Energy Technology Data Exchange (ETDEWEB)

    Loevestam, Goeran [EC-JRC-Institute for Reference Materials and Measurements (IRMM), Retieseweg 111, B-2440 Geel (Belgium)], E-mail: goeran.loevestam@ec.europa.eu; Hult, Mikael; Fessler, Andreas; Gasparro, Joel; Kockerols, Pierre; Okkinga, Klaas [EC-JRC-Institute for Reference Materials and Measurements (IRMM), Retieseweg 111, B-2440 Geel (Belgium); Tagziria, Hamid [EC-JRC-Institute for the Protection and the Security of the Citizen (IPSC), Via E. Fermi 1, I-21020 Ispra (Vatican City State, Holy See,) (Italy); Vanhavere, Filip [SCK-CEN, Boeretang, 2400 Mol (Belgium); Wieslander, J.S. Elisabeth [EC-JRC-Institute for Reference Materials and Measurements (IRMM), Retieseweg 111, B-2440 Geel (Belgium); Department of Physics, P.O. Box 35 (YFL), FIN-40014, University of Jyvaeskylae (Finland)

    2009-01-15

    A simple and robust detector for spectrometry of environmental neutrons has been developed. The technique is based on neutron activation of a series of different metal disks followed by low-level gamma-ray spectrometry of the activated disks and subsequent neutron spectrum unfolding. The technique is similar to foil activation but here the applied neutron fluence rates are much lower than usually in the case of foil activation. The detector has been tested in quasi mono-energetic neutron fields with fluence rates in the order of 1000-10000 cm{sup -2} s{sup -1}, where the obtained spectra showed good agreement with spectra measured using a Bonner sphere spectrometer. The detector has also been tested using an AmBe source and at a neutron fluence rate of about 40 cm{sup -2} s{sup -1}, again, a good agreement with the assumed spectrum was achieved.

  18. Miniaturization and Mass Spectrometry

    NARCIS (Netherlands)

    le Gac, S.; le Gac, Severine; van den Berg, Albert; van den Berg, A.; Unknown, [Unknown

    2009-01-01

    With this book we want to illustrate how two quickly growing fields of instrumentation and technology, both applied to life sciences, mass spectrometry and microfluidics (or microfabrication) naturally came to meet at the end of the last century and how this marriage impacts on several types of

  19. Fourier Transform Mass Spectrometry.

    Science.gov (United States)

    Gross, Michael L.; Rempel, Don L.

    1984-01-01

    Discusses the nature of Fourier transform mass spectrometry and its unique combination of high mass resolution, high upper mass limit, and multichannel advantage. Examines its operation, capabilities and limitations, applications (ion storage, ion manipulation, ion chemistry), and future applications and developments. (JN)

  20. Analytical mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    1990-01-01

    This 43rd Annual Summer Symposium on Analytical Chemistry was held July 24--27, 1990 at Oak Ridge, TN and contained sessions on the following topics: Fundamentals of Analytical Mass Spectrometry (MS), MS in the National Laboratories, Lasers and Fourier Transform Methods, Future of MS, New Ionization and LC/MS Methods, and an extra session. (WET)

  1. Analytical mass spectrometry. Abstracts

    Energy Technology Data Exchange (ETDEWEB)

    1990-12-31

    This 43rd Annual Summer Symposium on Analytical Chemistry was held July 24--27, 1990 at Oak Ridge, TN and contained sessions on the following topics: Fundamentals of Analytical Mass Spectrometry (MS), MS in the National Laboratories, Lasers and Fourier Transform Methods, Future of MS, New Ionization and LC/MS Methods, and an extra session. (WET)

  2. Monolithic multinozzle emitters for nanoelectrospray mass spectrometry

    Science.gov (United States)

    Wang, Daojing [Daly City, CA; Yang, Peidong [Kensington, CA; Kim, Woong [Seoul, KR; Fan, Rong [Pasadena, CA

    2011-09-20

    Novel and significantly simplified procedures for fabrication of fully integrated nanoelectrospray emitters have been described. For nanofabricated monolithic multinozzle emitters (NM.sup.2 emitters), a bottom up approach using silicon nanowires on a silicon sliver is used. For microfabricated monolithic multinozzle emitters (M.sup.3 emitters), a top down approach using MEMS techniques on silicon wafers is used. The emitters have performance comparable to that of commercially-available silica capillary emitters for nanoelectrospray mass spectrometry.

  3. High resolution spectrometry for relativistic heavy ions

    Energy Technology Data Exchange (ETDEWEB)

    Gabor, G; Schimmerling, W; Greiner, D; Bieser, F; Lindstrom, P [California Univ., Berkeley (USA). Lawrence Berkeley Lab.

    1975-12-01

    Several techniques are discussed for velocity and energy spectrometry of relativistic heavy ions with good resolution. A foil telescope with chevron channel plate detectors is described. A test of this telescope was performed using 2.1 GeV/A C/sup 6 +/ ions, and a time-of-flight resolution of 160 ps was measured. Qualitative information on the effect of foil thickness was also obtained.

  4. X-ray spectrometry with synchrotron radiation; Roentgenspektrometrie mit Synchrotronstrahlung

    Energy Technology Data Exchange (ETDEWEB)

    Mueller, Matthias [Physikalisch-Technische Bundesanstalt (PTB), Berlin (Germany). Arbeitsgruppe ' Roentgen- und IR-Spektrometrie' ; Gerlach, Martin; Holfelder, Ina; Hoenicke, Philipp; Lubeck, Janin; Nutsch, Andreas; Pollakowski, Beatrix; Streeck, Cornelia; Unterumsberger, Rainer; Weser, Jan; Beckhoff, Burkhard

    2014-12-15

    The X-ray spectrometry of the PTB at the BESSY II storage ring with radiation in the range from 78 eV to 10.5 keV is described. After a description of the instrumentation development reference-sample free X-ray fluorescence analysis, the determination of fundamental atomic parameters, X-ray fluorescence analysis under glance-angle incidence, highly-resolving absorption spectrometry, and emission spectrometry are considered. Finally liquid cells and in-situ measurement techniques are described. (HSI)

  5. Fourier transform ion cyclotron resonance mass spectrometry

    Science.gov (United States)

    Marshall, Alan G.

    1998-06-01

    As for Fourier transform infrared (FT-IR) interferometry and nuclear magnetic resonance (NMR) spectroscopy, the introduction of pulsed Fourier transform techniques revolutionized ion cyclotron resonance mass spectrometry: increased speed (factor of 10,000), increased sensitivity (factor of 100), increased mass resolution (factor of 10,000-an improvement not shared by the introduction of FT techniques to IR or NMR spectroscopy), increased mass range (factor of 500), and automated operation. FT-ICR mass spectrometry is the most versatile technique for unscrambling and quantifying ion-molecule reaction kinetics and equilibria in the absence of solvent (i.e., the gas phase). In addition, FT-ICR MS has the following analytically important features: speed (~1 second per spectrum); ultrahigh mass resolution and ultrahigh mass accuracy for analysis of mixtures and polymers; attomole sensitivity; MSn with one spectrometer, including two-dimensional FT/FT-ICR/MS; positive and/or negative ions; multiple ion sources (especially MALDI and electrospray); biomolecular molecular weight and sequencing; LC/MS; and single-molecule detection up to 108 Dalton. Here, some basic features and recent developments of FT-ICR mass spectrometry are reviewed, with applications ranging from crude oil to molecular biology.

  6. 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.

  7. 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

  8. Analysis of major antioxidants from extracts of Myrmecodia pendans by UV/visible spectrophotometer, liquid chromatography/tandem mass spectrometry, and high-performance liquid chromatography/UV techniques.

    Science.gov (United States)

    Engida, Adam Mekonnen; Faika, Sitti; Nguyen-Thi, Bich Thuyen; Ju, Yi-Hsu

    2015-06-01

    In the present work, heat reflux extraction with ethanol/water (80:20; v/v) as the solvent was used to extract antioxidants from Myrmecodia pendans. The crude extract (CE) was fractionated using hexane and ethyl acetate. Ethyl acetate fraction (EAF) and aqueous fraction were collected. Antioxidant activity against 1,1-diphenyl-2-picrylhydrazyl-radical radical and ferric reducing power of the CE, EAF, and aqueous fraction were evaluated. EAF showed comparable antioxidant activity against 1,1-diphenyl-2-picrylhydrazyl-radical radical and ferric reducing power to those of the CE. UV/visible, liquid chromatography/electrospray ionization/tandem mass spectrometry, and high-performance liquid chromatography were employed for identifying the major antioxidant compounds in the EAF. Three major phenolic compounds (rosmarinic acid, procyanidin B1, and polymer of procyanidin B1) were identified. The first two compounds were confirmed and quantified by high-performance liquid chromatography using authentic standards, but confirmation of the third compound was hampered by a lack of commercial standard. Concentrations of rosmarinic acid and procyanidin B1 in the EAF were found to be 20.688 ± 1.573 mg/g dry sample and 3.236 ± 0.280 mg/g dry sample, respectively. All these three compounds are reported for the first time in sarang semut. Copyright © 2014. Published by Elsevier B.V.

  9. High-throughput method for macrolides and lincosamides antibiotics residues analysis in milk and muscle using a simple liquid-liquid extraction technique and liquid chromatography-electrospray-tandem mass spectrometry analysis (LC-MS/MS).

    Science.gov (United States)

    Jank, Louise; Martins, Magda Targa; Arsand, Juliana Bazzan; Campos Motta, Tanara Magalhães; Hoff, Rodrigo Barcellos; Barreto, Fabiano; Pizzolato, Tânia Mara

    2015-11-01

    A fast and simple method for residue analysis of the antibiotics classes of macrolides (erythromycin, azithromycin, tylosin, tilmicosin and spiramycin) and lincosamides (lincomycin and clindamycin) was developed and validated for cattle, swine and chicken muscle and for bovine milk. Sample preparation consists in a liquid-liquid extraction (LLE) with acetonitrile, followed by liquid chromatography-electrospray-tandem mass spectrometry analysis (LC-ESI-MS/MS), without the need of any additional clean-up steps. Chromatographic separation was achieved using a C18 column and a mobile phase composed by acidified acetonitrile and water. The method was fully validated according the criteria of the Commission Decision 2002/657/EC. Validation parameters such as limit of detection, limit of quantification, linearity, accuracy, repeatability, specificity, reproducibility, decision limit (CCα) and detection capability (CCβ) were evaluated. All calculated values met the established criteria. Reproducibility values, expressed as coefficient of variation, were all lower than 19.1%. Recoveries range from 60% to 107%. Limits of detection were from 5 to 25 µg kg(-1).The present method is able to be applied in routine analysis, with adequate time of analysis, low cost and a simple sample preparation protocol. Copyright © 2015. Published by Elsevier B.V.

  10. Application of ultraperformance liquid chromatography/mass spectrometry-based metabonomic techniques to analyze the joint toxic action of long-term low-level exposure to a mixture of organophosphate pesticides on rat urine profile.

    Science.gov (United States)

    Du, Longfei; Wang, Hong; Xu, Wei; Zeng, Yan; Hou, Yurong; Zhang, Yuqiu; Zhao, Xiujuan; Sun, Changhao

    2013-07-01

    In previously published articles, we evaluated the toxicity of four organophosphate (OP) pesticides (dichlorvos, dimethoate, acephate, and phorate) to rats using metabonomic technology at their corresponding no observed adverse effect level (NOAEL). Results show that a single pesticide elicits no toxic response. This study aimed to determine whether chronic exposure to a mixture of the above four pesticides (at their corresponding NOAEL) can lead to joint toxic action in rats using the same technology. Pesticides were administered daily to rats through drinking water for 24 weeks. The above mixture of the four pesticides showed joint toxic action at the NOAEL of each pesticide. The metabonomic profiles of rats urine were analyzed by ultraperformance liquid chromatography/mass spectrometry. The 16 metabolites statistically significantly changed in all treated groups compared with the control group. Dimethylphosphate and dimethyldithiophosphate exclusively detected in all treated groups can be used as early, sensitive biomarkers for exposure to a mixture of the OP pesticides. Moreover, exposure to the OP pesticides resulted in increased 7-methylguanine, ribothymidine, cholic acid, 4-pyridoxic acid, kynurenine, and indoxyl sulfate levels, as well as decreased hippuric acid, creatinine, uric acid, gentisic acid, C18-dihydrosphingosine, phytosphingosine, suberic acid, and citric acid. The results indicated that a mixture of OP pesticides induced DNA damage and oxidative stress, disturbed the metabolism of lipids, and interfered with the tricarboxylic acid cycle. Ensuring food safety requires not only the toxicology test data of each pesticide for the calculation of the acceptable daily intake but also the joint toxic action.

  11. Analysis of major antioxidants from extracts of Myrmecodia pendans by UV/visible spectrophotometer, liquid chromatography/tandem mass spectrometry, and high-performance liquid chromatography/UV techniques

    Directory of Open Access Journals (Sweden)

    Adam Mekonnen Engida

    2015-06-01

    Full Text Available In the present work, heat reflux extraction with ethanol/water (80:20; v/v as the solvent was used to extract antioxidants from Myrmecodia pendans. The crude extract (CE was fractionated using hexane and ethyl acetate. Ethyl acetate fraction (EAF and aqueous fraction were collected. Antioxidant activity against 1,1-diphenyl-2-picrylhydrazyl-radical radical and ferric reducing power of the CE, EAF, and aqueous fraction were evaluated. EAF showed comparable antioxidant activity against 1,1-diphenyl-2-picrylhydrazyl-radical radical and ferric reducing power to those of the CE. UV/visible, liquid chromatography/electrospray ionization/tandem mass spectrometry, and high-performance liquid chromatography were employed for identifying the major antioxidant compounds in the EAF. Three major phenolic compounds (rosmarinic acid, procyanidin B1, and polymer of procyanidin B1 were identified. The first two compounds were confirmed and quantified by high-performance liquid chromatography using authentic standards, but confirmation of the third compound was hampered by a lack of commercial standard. Concentrations of rosmarinic acid and procyanidin B1 in the EAF were found to be 20.688 ± 1.573 mg/g dry sample and 3.236 ± 0.280 mg/g dry sample, respectively. All these three compounds are reported for the first time in sarang semut.

  12. The use of lasers as sources for Raman spectrometry, resonance Raman spectrometry, and light scattering

    International Nuclear Information System (INIS)

    Capitini, R.; Ceccaldi, M.; Leicknam, J.P.; Plus, R.

    1975-01-01

    The activity of the laboratory is principally centred on the determination of molecular structures and the study of molecular interactions in solution by infrared and Raman spectrometry. With the development of work on relatively large molecules, particularly biological molecules, it became necessary to complete information on the molecular weight and on the intra and intermolecular geometry and interactions of these bodies. In order to obtain these informations Rayleigh scattering and resonance Raman spectrometry were used. The advantages of using vibrational spectrometry, particularly Raman, in conjunction with the diffusion of light for these structural and molecular interaction studies is emphasized. It is shown that these two techniques could not have developed as they have done in the last few years without the use of lasers as light source [fr

  13. Coupling Front-End Separations, Ion Mobility Spectrometry, and Mass Spectrometry For Enhanced Multidimensional Biological and Environmental Analyses

    Energy Technology Data Exchange (ETDEWEB)

    Zheng, Xueyun; Wojcik, Roza; Zhang, Xing; Ibrahim, Yehia M.; Burnum-Johnson, Kristin E.; Orton, Daniel J.; Monroe, Matthew E.; Moore, Ronald J.; Smith, Richard D.; Baker, Erin M.

    2017-06-12

    Ion mobility spectrometry (IMS) is a widely used analytical technique for rapid molecular separations in the gas phase. IMS alone is useful, but its coupling with mass spectrometry (MS) and front-end separations has been extremely beneficial for increasing measurement sensitivity, peak capacity of complex mixtures, and the scope of molecular information in biological and environmental sample analyses. Multiple studies in disease screening and environmental evaluations have even shown these IMS-based multidimensional separations extract information not possible with each technique individually. This review highlights 3-dimensional separations using IMS-MS in conjunction with a range of front-end techniques, such as gas chromatography (GC), supercritical fluid chromatography (SFC), liquid chromatography (LC), solid phase extractions (SPE), capillary electrophoresis (CE), field asymmetric ion mobility spectrometry (FAIMS), and microfluidic devices. The origination, current state, various applications, and future capabilities for these multidimensional approaches are described to provide insight into the utility and potential of each technique.

  14. Spectrometric techniques 4

    CERN Document Server

    Vanasse, George A

    2013-01-01

    Spectrometric Techniques, Volume IV discusses three widely diversified areas of spectrometric techniques. The book focuses on three spectrometric methods. Chapter 1 discusses the phenomenology and applications of Coherent Anti-Stokes Raman Spectroscopy (CARS), the most commonly used optical technique that exploit the Raman effect. The second chapter is concerned with diffraction gratings and mountings for the Vacuum Ultraviolet Spectral Region. Chapter 3 accounts the uses of mass spectrometry, detectors, types of spectrometers, and ion sources. Physicists and chemists will find the book a go

  15. Hydrogen Exchange Mass Spectrometry

    Science.gov (United States)

    Mayne, Leland

    2018-01-01

    Hydrogen exchange (HX) methods can reveal much about the structure, energetics, and dynamics of proteins. The addition of mass spectrometry (MS) to an earlier fragmentation-separation HX analysis now extends HX studies to larger proteins at high structural resolution and can provide information not available before. This chapter discusses experimental aspects of HX labeling, especially with respect to the use of MS and the analysis of MS data. PMID:26791986

  16. Determination of radium isotopes in environmental samples by gamma spectrometry, liquid scintillation counting and alpha spectrometry: a review of analytical methodology

    International Nuclear Information System (INIS)

    Jia, Guogang; Jia, Jing

    2012-01-01

    Radium (Ra) isotopes are important from the viewpoints of radiation protection and environmental protection. Their high toxicity has stimulated the continuing interest in methodology research for determination of Ra isotopes in various media. In this paper, the three most routinely used analytical techniques for Ra isotope determination in biological and environmental samples, i.e. low-background γ-spectrometry, liquid scintillation counting and α-spectrometry, were reviewed, with emphasis on new methodological developments in sample preparation, preconcentration, separation, purification, source preparation and measurement techniques. The accuracy, selectivity, traceability, applicability and minimum detectable activity (MDA) of the three techniques were discussed. It was concluded that the MDA (0.1 mBq L −1 ) of the α-spectrometry technique coupled with chemical separation is about two orders of magnitude lower than that of low-background HPGe γ-spectrometry and LSC techniques. Therefore, when maximum sensitivity is required, the α-spectrometry technique remains the first choice. - Highlights: ► A review is made for determination of Ra isotopes in environmental samples. ► Gamma spectrometry, LSC and a-spectrometry are the main concerned radiometric approach. ► Sample preparation, preconcentration, separation and source preparation are discussed. ► The methods can analyse air, water, seawater, soil, sediment and foodstuffs samples. ► Some new data obtained recently from our laboratory for Ra method study are included.

  17. Identification of Fatty Acids, Phospholipids, and Their Oxidation Products Using Matrix-Assisted Laser Desorption Ionization Mass Spectrometry and Electrospray Ionization Mass Spectrometry

    Science.gov (United States)

    Harmon, Christopher W.; Mang, Stephen A.; Greaves, John; Finlayson-Pitts, Barbara J.

    2010-01-01

    Electrospray ionization mass spectrometry (ESI-MS) and matrix-assisted laser desorption ionization mass spectrometry (MALDI-MS) have found increasing application in the analysis of biological samples. Using these techniques to solve problems in analytical chemistry should be an essential component of the training of undergraduate chemists. We…

  18. Accelerator mass spectrometry: state of the art

    Energy Technology Data Exchange (ETDEWEB)

    Tuniz, C. [Australian Nuclear Science and Technology Organisation, Lucas Heights, NSW (Australia)

    1996-12-31

    Accelerator Mass Spectrometry (AMS) is the analytical technique of choice for the detection of long-lived radionuclides which cannot be practically analysed with decay counting or conventional mass spectrometry. The main use of AMS has been in the analysis of radiocarbon and other cosmogenic radionuclides for archaeological, geological and environmental applications. In addition, AMS has been recently applied in biomedicine to study exposure of human tissues to chemicals and biomolecules at attomole levels. There is also a world-wide effort to analyse rare nuclides of heavier masses, such as long-lived actinides, with important applications in safeguards and nuclear waste disposal. The use of AMS is limited by the expensive accelerator technology required and there are several attempts to develop smaller and cheaper AMS spectrometers. 5 refs.

  19. Accelerator mass spectrometry: state of the art

    Energy Technology Data Exchange (ETDEWEB)

    Tuniz, C [Australian Nuclear Science and Technology Organisation, Lucas Heights, NSW (Australia)

    1997-12-31

    Accelerator Mass Spectrometry (AMS) is the analytical technique of choice for the detection of long-lived radionuclides which cannot be practically analysed with decay counting or conventional mass spectrometry. The main use of AMS has been in the analysis of radiocarbon and other cosmogenic radionuclides for archaeological, geological and environmental applications. In addition, AMS has been recently applied in biomedicine to study exposure of human tissues to chemicals and biomolecules at attomole levels. There is also a world-wide effort to analyse rare nuclides of heavier masses, such as long-lived actinides, with important applications in safeguards and nuclear waste disposal. The use of AMS is limited by the expensive accelerator technology required and there are several attempts to develop smaller and cheaper AMS spectrometers. 5 refs.

  20. [Sample preparation and bioanalysis in mass spectrometry].

    Science.gov (United States)

    Bourgogne, Emmanuel; Wagner, Michel

    2015-01-01

    The quantitative analysis of compounds of clinical interest of low molecular weight (sample preparation. Sample preparation is a crucial part of chemical/biological analysis and in a sense is considered the bottleneck of the whole analytical process. The main objectives of sample preparation are the removal of potential interferences, analyte preconcentration, and converting (if needed) the analyte into a more suitable form for detection or separation. Without chromatographic separation, endogenous compounds, co-eluted products may affect a quantitative method in mass spectrometry performance. This work focuses on three distinct parts. First, quantitative bioanalysis will be defined, different matrices and sample preparation techniques currently used in bioanalysis by mass spectrometry of/for small molecules of clinical interest in biological fluids. In a second step the goals of sample preparation will be described. Finally, in a third step, sample preparation strategies will be made either directly ("dilute and shoot") or after precipitation.

  1. Guideline on Isotope Dilution Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Gaffney, Amy [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

    2017-05-19

    Isotope dilution mass spectrometry is used to determine the concentration of an element of interest in a bulk sample. It is a destructive analysis technique that is applicable to a wide range of analytes and bulk sample types. With this method, a known amount of a rare isotope, or ‘spike’, of the element of interest is added to a known amount of sample. The element of interest is chemically purified from the bulk sample, the isotope ratio of the spiked sample is measured by mass spectrometry, and the concentration of the element of interest is calculated from this result. This method is widely used, although a mass spectrometer required for this analysis may be fairly expensive.

  2. Coupling Front-End Separations, Ion Mobility Spectrometry, and Mass Spectrometry For Enhanced Multidimensional Biological and Environmental Analyses

    Science.gov (United States)

    Zheng, Xueyun; Wojcik, Roza; Zhang, Xing; Ibrahim, Yehia M.; Burnum-Johnson, Kristin E.; Orton, Daniel J.; Monroe, Matthew E.; Moore, Ronald J.; Smith, Richard D.; Baker, Erin S.

    2017-01-01

    Ion mobility spectrometry (IMS) is a widely used analytical technique for rapid molecular separations in the gas phase. Though IMS alone is useful, its coupling with mass spectrometry (MS) and front-end separations is extremely beneficial for increasing measurement sensitivity, peak capacity of complex mixtures, and the scope of molecular information available from biological and environmental sample analyses. In fact, multiple disease screening and environmental evaluations have illustrated that the IMS-based multidimensional separations extract information that cannot be acquired with each technique individually. This review highlights three-dimensional separations using IMS-MS in conjunction with a range of front-end techniques, such as gas chromatography, supercritical fluid chromatography, liquid chromatography, solid-phase extractions, capillary electrophoresis, field asymmetric ion mobility spectrometry, and microfluidic devices. The origination, current state, various applications, and future capabilities of these multidimensional approaches are described in detail to provide insight into their uses and benefits. PMID:28301728

  3. Mass Spectrometry Imaging under Ambient Conditions

    Science.gov (United States)

    Wu, Chunping; Dill, Allison L.; Eberlin, Livia S.; Cooks, R. Graham; Ifa, Demian R.

    2012-01-01

    Mass spectrometry imaging (MSI) has emerged as an important tool in the last decade and it is beginning to show potential to provide new information in many fields owing to its unique ability to acquire molecularly specific images and to provide multiplexed information, without the need for labeling or staining. In MSI, the chemical identity of molecules present on a surface is investigated as a function of spatial distribution. In addition to now standard methods involving MSI in vacuum, recently developed ambient ionization techniques allow MSI to be performed under atmospheric pressure on untreated samples outside the mass spectrometer. Here we review recent developments and applications of MSI emphasizing the ambient ionization techniques of desorption electrospray ionization (DESI), laser ablation electrospray ionization (LAESI), probe electrospray ionization (PESI), desorption atmospheric pressure photoionization (DAPPI), femtosecond laser desorption ionization (fs-LDI), laser electrospray mass spectrometry (LEMS), infrared laser ablation metastable-induced chemical ionization (IR-LAMICI), liquid microjunction surface sampling probe mass spectrometry (LMJ-SSP MS), nanospray desorption electrospray ionization (nano-DESI), and plasma sources such as the low temperature plasma (LTP) probe and laser ablation coupled to flowing atmospheric-pressure afterglow (LA-FAPA). Included are discussions of some of the features of ambient MSI including the ability to implement chemical reactions with the goal of providing high abundance ions characteristic of specific compounds of interest and the use of tandem mass spectrometry to either map the distribution of targeted molecules with high specificity or to provide additional MS information in the structural identification of compounds. We also describe the role of bioinformatics in acquiring and interpreting the chemical and spatial information obtained through MSI, especially in biological applications for tissue

  4. Lipid imaging by mass spectrometry - a review.

    Science.gov (United States)

    Gode, David; Volmer, Dietrich A

    2013-03-07

    Mass spectrometry imaging (MSI) has proven to be extremely useful for applications such as the spatial analysis of peptides and proteins in biological tissue, the performance assessment of drugs in vivo or the measurement of protein or metabolite expression as tissue classifiers or biomarkers from disease versus control tissue comparisons. The most popular MSI technique is MALDI mass spectrometry. First invented by Richard Caprioli in the mid-1990s, it is the highest performing MSI technique in terms of spatial resolution, sensitivity for intact biomolecules and application range today. The unique ability to identify and spatially resolve numerous compounds simultaneously, based on m/z values has inter alia been applied to untargeted and targeted chemical mapping of biological compartments, revealing changes of physiological states, disease pathologies and metabolic faith and distribution of xenobiotics. Many MSI applications focus on lipid species because of the lipids' diverse roles as structural components of cell membranes, their function in the surfactant cycle, and their involvement as second messengers in signalling cascades of tissues and cells. This article gives a comprehensive overview of lipid imaging techniques and applications using established MALDI and SIMS methods but also other promising MSI techniques such as DESI.

  5. Sample Preprocessing For Atomic Spectrometry

    International Nuclear Information System (INIS)

    Kim, Sun Tae

    2004-08-01

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

  6. Pensamento, Teoria e Estudos Latino-americanos

    Directory of Open Access Journals (Sweden)

    Jacques de Novion

    2014-12-01

    Full Text Available RESUMO O presente trabalho configura como artigo inicial do Dossiê Especial – Pensamento, Teoria e Estudos Latino-americanos, organizado conjuntamente por nós, a pedido da Revista de Estudos e Pesquisas sobre as Américas (CEPPAC, do Instituto de Ciências Sociais (ICS, da Universidade de Brasília (UnB. De forma breve, este artigo apresenta a importância alcançada pelo Pensamento, pela Teoria, e, sobre tudo, pelos Estudos Latino-americanos nas últimas décadas. Em seguida, o artigo apresenta os quatorze trabalhos e uma resenha que compõem este Dossiê, resultado da contribuição de diferentes pesquisadores de distintas localidades da região, organizados em três blocos: Ciências Sociais Latino-americanas, Pensamento e Estudos. PALAVRAS CHAVE: Ciências Sociais Latino-americanas; Pensamento Latino-americanos; Teoria Latino-americana; Estudos Latino-americanos. --- RESUMEN El presente trabajo configura como articulo inicial del Dossier Especial – Pensamiento Teoría y Estudios Latinoamericanos, organizado conjuntamente por nosotros, a pedido de la Revista de Estudos e Pesquisas sobre as Américas (CEPPAC, del Instituto de Ciências Sociais (ICS, de la Universidade de Brasília (UnB. De forma breve, este articulo presenta la importancia alcanzada por el Pensamiento, por la Teoría, y, sobre todo, por los Estudios Latinoamericanos en las últimas décadas. En seguida, el articulo presenta los catorce trabajos e una reseña que componen este Dossier, resultado de la contribución de diferentes investigadores de distintas localidades de la región, organizados en tres bloques: Ciencias Sociales Latinoamericanas, Pensamiento y Estudios. PALABRAS CLAVE: Ciencias Sociales Latinoamericanas; Pensamiento Latinoamericano; Teoría Latinoamericana; Estudios Latinoamericanos. --- ABSTRACT This paper is set up as the initial article of this Special Dossier - Thought, Theory and Latin American Studies, which we organized collectively, at the request

  7. EMPREENDEDORISMO E VALORES HUMANOS: UM ESTUDO CONCEITUAL

    Directory of Open Access Journals (Sweden)

    Luciano Vignochi

    2013-09-01

    Full Text Available O objetivo principal deste artigo foi identificar conceitos de valores humanos em publicações científicas sobre empreendedorismo. Não há um único conceito de valores humanos, gerando diversas abordagens e aplicações do termo em estudos sobre empreendedorismo. Para identificar diferenças conceituais e aplicações práticas, optou-se por realizar uma análise de conteúdo em um portfólio de artigos selecionados em bases de dados. O principal critério de seleção das publicações foi aderência ao tema. Os resultados mostram que valores podem ser definidos como: critérios de julgamento da realidade; aspectos abstratos, cognitivos e afetivos ou características determinantes da personalidade e do comportamento de empreendedores. Valores influenciam a sobrevivência do indivíduo, o crescimento do empreendimento e podem nivelar a congruência do empreendedor e seu propósito de empreendimento com os critérios de convivência social. Ainda foram discriminados resultados de estudos aplicados com vistas a destacar evidências de contribuições práticas de pesquisas sobre valores humanos em empreendedorismo. Futuras investigações para aprofundar e replicar as análises realizadas neste estudo podem contribuir com a formação de empreendedores, a realização de diagnóstico empresarial e com avanços para a consolidação um modelo de desenvolvimento de empresas baseado em valores humanos.

  8. Sample preparation techniques for the determination of natural 15N/14N variations in amino acids by gas chromatography-combustion-isotope ratio mass spectrometry (GC-C-IRMS).

    Science.gov (United States)

    Hofmann, D; Gehre, M; Jung, K

    2003-09-01

    In order to identify natural nitrogen isotope variations of biologically important amino acids four derivatization reactions (t-butylmethylsilylation, esterification with subsequent trifluoroacetylation, acetylation and pivaloylation) were tested with standard mixtures of 17 proteinogenic amino acids and plant (moss) samples using GC-C-IRMS. The possible fractionation of the nitrogen isotopes, caused for instance by the formation of multiple reaction products, was investigated. For biological samples, the esterification of the amino acids with subsequent trifluoroacetylation is recommended for nitrogen isotope ratio analysis. A sample preparation technique is described for the isotope ratio mass spectrometric analysis of amino acids from the non-protein (NPN) fraction of terrestrial moss. 14N/15N ratios from moss (Scleropodium spec.) samples from different anthropogenically polluted areas were studied with respect to ecotoxicologal bioindication.

  9. Antecedentes do Conflito Intragrupal: Um Estudo Comparativo

    OpenAIRE

    XAVIER, Tércio Antonio de Souza

    2002-01-01

    No campo do comportamento organizacional vem crescendo a importância dos grupos para as organizações, também têm crescido os problemas relacionados à motivação, à coordenação e aos conflitos. Nesse sentido, este estudo visa estudar e entender o conflito intragrupal em situações de trabalho e seus antecedentes na ótica dos funcionários. Buscam-se os prováveis determinantes das diferenças significativas nos graus de conflito de unidades organizacionais, a fim de subsidiar program...

  10. Habilidades auditivas e afasia: um estudo comparativo

    OpenAIRE

    Nascimento, Maria da Soledade Rolim do

    2012-01-01

    A compreensão da informação recebida pela modalidade auditiva é um requisito importante para a efetividade da comunicação, especialmente na linguagem expressiva. Este trabalho teve como objetivo avaliar a relação das habilidades auditivas com o processo de compreensão da linguagem em pacientes com afasia. Trata-se de um estudo descritivo, transversal, comparativo, com 32 sujeitos, distribuídos em dois grupos: Grupo com afasia (n=16) e Grupo controle (n=16). Os indivíduos foram ...

  11. Alpha spectrometry and secondary ion mass spectrometry of thorium

    International Nuclear Information System (INIS)

    Strisovska, Jana; Kuruc, Jozef; Galanda, Dusan; Matel, Lubomir; Velic, Dusan; Aranyosiova, Monika

    2009-01-01

    A sample of thorium content on steel discs was prepared by electrodeposition with a view to determining the natural thorium isotope. Thorium was determined by alpha spectrometry and by secondary ion mass spectrometry and the results of the two methods were compared

  12. Study and development of a method allowing the identification of actinides inside nuclear waste packages, by active neutron or photon interrogation and delayed gamma-ray spectrometry; Etude et developpement d'une technique de dosage des actinides dans les colis de dechets radioactifs par interrogation photonique ou neutronique active et spectrometrie des gamma retardes

    Energy Technology Data Exchange (ETDEWEB)

    Carrel, F

    2007-10-15

    An accurate estimation of the alpha-activity of a nuclear waste package is necessary to select the best mode of storage. The main purpose of this work is to develop a non-destructive active method, based on the fission process and allowing the identification of actinides ({sup 235}U, {sup 238}U, {sup 239}Pu). These three elements are the main alpha emitters contained inside a package. Our technique is based on the detection of delayed gammas emitted by fission products. These latter are created by irradiation with the help of a neutron or photon beam. Performances of this method have been investigated after an Active Photon or Neutron Interrogation (INA or IPA). Three main objectives were fixed in the framework of this thesis. First, we measured many yields of photofission products to compensate the lack of data in the literature. Then, we studied experimental performances of this method to identify a given actinide ({sup 239}Pu in fission, {sup 235}U in photofission) present in an irradiated mixture. Finally, we assessed the application of this technique on different mock-up packages for both types of interrogation (118 l mock-up package containing EVA in fission, 220 l mock-up package with a wall of concrete in photofission). (author)

  13. Nanoscience, nanotechnology and spectrometry

    International Nuclear Information System (INIS)

    Adams, Freddy C.; Barbante, Carlo

    2013-01-01

    Nanoscience has outgrown its infancy, and nanotechnology has found important applications in our daily life — with many more to come. Although the central concepts of the nano world, namely the changes of particular physical properties on the length scale of individual atoms and molecules, have been known and developed for quite some time already, experimental advances since the 1980s and recognition of the potential of nanomaterials led to a genuine breakthrough of the inherently multidisciplinary nanoscience field. Analytical nanoscience and nanotechnology and especially the use of micro and nano electro mechanical systems, of the quantum dots and of mass spectrometry, currently provide one of the most promising avenues for developments in analytical science, derived from their two main fields of action, namely (a) the analysis of nano-structured materials and (b) their use as new tools for analysis. An overview is given of recent developments and trends in the field, highlighting the importance and point out future directions, while also touching drawbacks, such as emerging concerns about health and environmental issues. - Highlights: • We review the analysis of nano-structured materials. • Nano-structured materials can be used as new tools for analysis. • Use of nano electro mechanical systems, of quantum dots and of mass spectrometry • Nanotechnologies are among the most promising tools in analytical science

  14. Nanoscience, nanotechnology and spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Adams, Freddy C. [Department of Chemistry, University of Antwerp, B-2610 Wilrijk (Belgium); Barbante, Carlo, E-mail: barbante@unive.it [Institute for the Dynamics of Environmental Processes — CNR, Venice (Italy); Department of Environmental Sciences, Informatics and Statistics, Ca' Foscari University, Venice (Italy)

    2013-08-01

    Nanoscience has outgrown its infancy, and nanotechnology has found important applications in our daily life — with many more to come. Although the central concepts of the nano world, namely the changes of particular physical properties on the length scale of individual atoms and molecules, have been known and developed for quite some time already, experimental advances since the 1980s and recognition of the potential of nanomaterials led to a genuine breakthrough of the inherently multidisciplinary nanoscience field. Analytical nanoscience and nanotechnology and especially the use of micro and nano electro mechanical systems, of the quantum dots and of mass spectrometry, currently provide one of the most promising avenues for developments in analytical science, derived from their two main fields of action, namely (a) the analysis of nano-structured materials and (b) their use as new tools for analysis. An overview is given of recent developments and trends in the field, highlighting the importance and point out future directions, while also touching drawbacks, such as emerging concerns about health and environmental issues. - Highlights: • We review the analysis of nano-structured materials. • Nano-structured materials can be used as new tools for analysis. • Use of nano electro mechanical systems, of quantum dots and of mass spectrometry • Nanotechnologies are among the most promising tools in analytical science.

  15. Protein Analysis by Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Cindic, M.

    2008-04-01

    Full Text Available Soft ionization techniques, electrospray (ESI and matrix-assisted laser desorption/ionization (MALDI make the analysis of biomolecules by mass spectrometry (MS possible. MS is used for determination of the molecular weight of peptides and protein, sequence analysis, characterization of protein-ligand interactions etc. The detection limit, resolution and mass accuracy depend on instrument used (Table 1. Impurities (buffers, salts, detergents can reduce the ion intensities or even totally suppress them, so a separation method (chromatography, 2D-gel electrophoresis must be used for purification of the sample.Molecular mass of intact protein can be determined by ESI or MALDI MS. Multiply charged ions are produced by ESI MS, while singly charged ions are predominant in MALDI spectra (Fig. 2.Sequence analysis of proteins by MS can be performed using peptide mass fingerprint. In this method, proteins are separated by 2-D gel electrophoresis and digested with specific protease (Table 2 or digested and then separated by two-dimensional chromatography (Fig. 1. The obtained peptide mixtures are analyzed by MS or MALDI-TOF technique. The masses determined by MS are compared with calculated masses from database entries. Different algorithms have been developed for protein identification. Example of posttranslational modifications (N- and O-glycosylation and protein sequence complex analysis after dual digestion (endoproteinase digestion followed by endoglycosidase digestion is shown in Fig. 3.It is known that detection of peptides by MS is influenced by intrinsic properties like amino acid composition, the basicity of the C-terminal amino acid, hydrophobicity, etc. Arginine-containing peptides dominate in MS spectra of tryptic digest, so the chemical derivatization of lysine terminal residue by O-methilisourea or 2-methoxy-4,5-1H-imidazole was suggested (Fig. 4.The peptide mass fingerprint method can be improved further by peptide fragmentation using tandem

  16. The allure of mass spectrometry: From an earlyday chemist's perspective.

    Science.gov (United States)

    Tőkés, László

    2017-07-01

    This reminiscing review article is an account of the author's fascination and involvements with mass spectrometry from the perspective of an organic chemist with an interest in natural product chemistry. It covers a period from 1961 through the mid 1990s as mass spectrometry evolved form a novelty technique to become a most widely used analytical technique. Following a brief synopsis of my pathway to mass spectrometry, my research efforts in this field are presented with a focus mainly on evolving principles and technologies which I had personal involvements with. To provide historical perspectives, discussions of these developments are accompanied by brief outlines of the relevant state-of-the-art, shedding light on the technical and conceptual challenges encountered during those early days in mass spectrometry. Examples are presented of my involvements with basic and applied research in mass spectrometry during graduate studies at Stanford University and close to three decade tenure in pharmaceutical research at Syntex Research. My basic research interests focused mainly on principles of electron ionization induced fragmentation mechanisms, with an emphasis on steroids and other model compounds. Extensive deuterium labeling evidence was used to determine the fragmentation mechanisms of the diagnostically significant ions in the spectra of numerous model compounds, uncovering examples of wide-ranging hydrogen transfers, skeletal rearrangements, methyl and phenyl migrations, stereoselective fragmentations and low and high energy fragmentation processes. Depiction of the industrial research phase of my career includes comments on the pivotal role mass spectrometry played on advancing modern pharmaceutical research. Examples are presented of involvements with instrumental developments and a few select cases of applied research, including studies of bile mechanisms in vertebrates, identification of bisphenol-A leaching from sterilized polycarbonate containers, high

  17. Difraction spectrometry by laser beams

    Directory of Open Access Journals (Sweden)

    Frías, M.

    1988-12-01

    Full Text Available The advances in laser technology have permitted the development of numerous applications, in particular diffraction spectrometry by laser beams for the determination of the distribution curve of the particle sizes of different materials; this permits one to obtain the distribution of particle size in both wet and dry materials. In the present paper a brief description of the technique and its principles is offered. The results obtained with different materials-limestone clay, gypsum, Portland cement and siliceous materials are given.

    Los avances en la tecnología laser han permitido el desarrollo de múltiples aplicaciones, en concreto la espectrometría de difracción de rayos laser para la determinación de la curva de distribución del tamaño de partícula de diferentes materiales, y que permite la obtención de la misma tanto en seco como en húmedo. En este trabajo se hace una descripción breve de la técnica y de sus fundamentos. Se presentan resultados con diferentes materiales: caliza, arcilla, yeso, cemento Portland y materiales silíceos.

  18. Incorporating Biological Mass Spectrometry into Undergraduate Teaching Labs, Part 2: Peptide Identification via Molecular Mass Determination

    Science.gov (United States)

    Arnquist, Isaac J.; Beussman, Douglas J.

    2009-01-01

    Mass spectrometry has become a routine analytical tool in the undergraduate curriculum in the form of GC-MS. While relatively few undergraduate programs have incorporated biological mass spectrometry into their programs, the importance of these techniques, as demonstrated by their recognition with the 2002 Nobel Prize, will hopefully lead to…

  19. Derivative flame atomic absorption spectrometry and its application in trace analysis

    International Nuclear Information System (INIS)

    Sun, H. W.; Li, L. Q.

    2005-01-01

    Flame atomic absorption spectrometry is an accepted and widely used method for the determination of trace elements in a great variety of samples. But its sensitivity doesn't meet the demands of trace and ultra-trace analysis for some samples. The derivative signal processing technique, with a very high capability for enhancing sensitivity, was developed for flame atomic absorption spectrometry. The signal models of conventional flame atomic absorption spectrometry are described. The equations of derivative signals are established for flame atomic absorption spectrometry, flow injection atomic absorption spectrometry (FI-FAAS) and atom trapping flame atomic absorption spectrometry (AT-FAAS). The principle and performance of the derivative atomic absorption spectrometry are evaluated. The derivative technique based on determination of variation rate of signal intensity with time (dl/dt) is different from the derivative spectrophotometry based on determination of variation rate of signal intensity with wavelength (dl/dhλ). Derivative flame atomic absorption spectrometry has higher sensitivity, lower detection limits and better accuracy. It has been applied to the direct determination of trace elements without preconcentration. If the derivative technique was combined with several preconcentration techniques, the sensitivity would be enhanced further for ultra-trace analysis with good linearity. The applications of derivative flame atomic absorption spectroscopy are reviewed for trace element analysis in biological, pharmaceutical, environmental and food samples

  20. Os estudos brasileiros e os 'brazilianists'

    Directory of Open Access Journals (Sweden)

    José Honório Rodrigues

    1976-09-01

    Full Text Available (primeiro parágrafo do artigo Quando, em 1943-1944, estive nos Estados Unidos, estudando e pesquisando, conheci muitas bibliotecas públicas e universitárias, e o grande Arquivo Nacional dos Estados Unidos. Nas Universidades já se ofereciam cursos de estudos latino-americanos, centralizados sobretudo no estudo da língua espanhola, portuguesa em menor escala, estenografía em espanhol, e raras propunham o ensino da literatura comparativa, antropologia, economia, geografia, política e história latino-americana, sempre em conjunto; raríssimas, como a Columbia, ofereciam aulas de história social e econômica do Brasil, e tambem do México e da América Central, e ainda da Argentina, Uruguai e Paraguai. Havia pouca especialização por paises e áreas, e se via predominantemente a América Latina como um bloco uno e uniforme.

  1. Novas tecnologias no estudo de ondas sonoras

    Directory of Open Access Journals (Sweden)

    Marisa Almeida Cavalcante

    2013-10-01

    Full Text Available http://dx.doi.org/10.5007/2175-7941.2013v30n3p579 O presente trabalho propõe a construção de um Tubo de Kundt adaptado às novas tecnologias disponíveis para o ensino de física. Tem como principal objetivo utilizar a placa Arduino em experimentos didáticos envolvendo o estudo de ondas sonoras. O Arduino é uma placa de controle I/O baseada no micro-controlador Atmega (Atmel e foi projetado inicialmente para fins didáticos. O fato da linguagem de programação utilizada e hardware serem do tipo open source (código aberto possibilitou sua ampla difusão em diversas áreas. Uma das intenções deste projeto é difundir o uso deste recurso para fins educacionais e particularmente no estudo de ondas sonoras estacionarias em tubos, contribuindo com a melhora na abordagem deste conteúdo no ensino e aprendizagem de Física.

  2. Negative chemical ionization mass spectrometry

    International Nuclear Information System (INIS)

    Smit, A.L.C.

    1979-01-01

    This thesis describes some aspects of Negative Chemical Ionization (NCI) mass spectrometry. The reasons for the growing interest in NCI are: (i) to extend the basic knowledge of negative ions and their reactions in the gas phase; (ii) to investigate whether or not this knowledge of negative ions can be used successfully to elucidate the structure of molecules by mass spectrometry. (Auth.)

  3. Laboratory of acceleration mass spectrometry

    International Nuclear Information System (INIS)

    Hybler, P.; Chrapan, J.

    2002-01-01

    In this paper authors describe the principle of the method of acceleration mass spectrometry and the construction plans of this instrument at the Faculty of ecology and environmental sciences in Banska Stiavnica. Using of this instrument for radiocarbon dating is discussed. A review of laboratories with acceleration mass spectrometry is presented

  4. Mass spectrometry imaging: Towards a lipid microscope?

    Science.gov (United States)

    Touboul, David; Brunelle, Alain; Laprévote, Olivier

    2011-01-01

    Biological imaging techniques are the most efficient way to locally measure the variation of different parameters on tissue sections. These analyses are gaining increasing interest since 20 years and allow observing extremely complex biological phenomena at lower and lower time and resolution scale. Nevertheless, most of them only target very few compounds of interest, which are chosen a priori, due to their low resolution power and sensitivity. New chemical imaging technique has to be introduced in order to overcome these limitations, leading to more informative and sensitive analyses for biologists and physicians. Two major mass spectrometry methods can be efficiently used to generate the distribution of biological compounds over a tissue section. Matrix-Assisted Laser Desorption/Ionisation-Mass Spectrometry (MALDI-MS) needs the co-crystallization of the sample with a matrix before to be irradiated by a laser, whereas the analyte is directly desorbed by a primary ion bombardment for Secondary Ion Mass Spectrometry (SIMS) experiments. In both cases, energy used for desorption/ionization is locally deposited -some tens of microns for the laser and some hundreds of nanometers for the ion beam- meaning that small areas over the surface sample can be separately analyzed. Step by step analysis allows spectrum acquisitions over the tissue sections and the data are treated by modern informatics software in order to create ion density maps, i.e., the intensity plot of one specific ion versus the (x,y) position. Main advantages of SIMS and MALDI compared to other chemical imaging techniques lie in the simultaneous acquisition of a large number of biological compounds in mixture with an excellent sensitivity obtained by Time-of-Flight (ToF) mass analyzer. Moreover, data treatment is done a posteriori, due to the fact that no compound is selectively marked, and let us access to the localization of different lipid classes in only one complete acquisition. Copyright © 2010

  5. Spectrometry of degraded neutrons with SSNTDs

    International Nuclear Information System (INIS)

    Gopalani, Deepak; Kumar, S.; Jodha, A.S.; Reddy, A.R.

    1993-01-01

    Considerable interest has grown during the last decade in the use of solid state nuclear track detectors (SSNTDs) for routine neutron monitoring and dosimetry work. In addition, using these detectors neutron spectrometry has also been undertaken by some investigators. In spectrometry the energy of neutrons was determined either from minor axis of proton tracks observed on the surface of detector or from the use of polyethylene radiators of selected thickness with varying etching time. Using this latter method in the present work fast neutron spectrometry is made. The method involves the measurement of etch induction time, thickness of removed critical layer for constant radiator thickness with varying etching time. Besides a computer programme has been developed for the calculation of neutron sensitivity at different critical removal layers. The degraded neutron spectra of 252 Cf with shield materials of different thickness but of same composition and shield materials of same thickness but of different compositions have been obtained. The study shows that SSNTD films can be used for recording the transmitted neutron spectra from different shield materials. This spectrometric capability added to the technique advantages of SSNTDs such as integrating nature and small size make them important for nuclear engineering applications. (author). 7 refs., 4 figs., 1 tab

  6. Limit of detection in the presence of instrumental and non-instrumental errors: study of the possible sources of error and application to the analysis of 41 elements at trace levels by inductively coupled plasma-mass spectrometry technique

    International Nuclear Information System (INIS)

    Badocco, Denis; Lavagnini, Irma; Mondin, Andrea; Tapparo, Andrea; Pastore, Paolo

    2015-01-01

    In this paper the detection limit was estimated when signals were affected by two error contributions, namely instrumental errors and operational-non-instrumental errors. The detection limit was theoretically obtained following the hypothesis testing schema implemented with the calibration curve methodology. The experimental calibration design was based on J standards measured I times with non-instrumental errors affecting each standard systematically but randomly among the J levels. A two-component variance regression was performed to determine the calibration curve and to define the detection limit in these conditions. The detection limit values obtained from the calibration at trace levels of 41 elements by ICP-MS resulted larger than those obtainable from a one component variance regression. The role of the reagent impurities on the instrumental errors was ascertained and taken into account. Environmental pollution was studied as source of non-instrumental errors. The environmental pollution role was evaluated by Principal Component Analysis technique (PCA) applied to a series of nine calibrations performed in fourteen months. The influence of the seasonality of the environmental pollution on the detection limit was evidenced for many elements usually present in the urban air particulate. The obtained results clearly indicated the need of using the two-component variance regression approach for the calibration of all the elements usually present in the environment at significant concentration levels. - Highlights: • Limit of detection was obtained considering a two variance component regression. • Calibration data may be affected by instrumental and operational conditions errors. • Calibration model was applied to determine 41 elements at trace level by ICP-MS. • Non instrumental errors were evidenced by PCA analysis

  7. Symposium on fast atom and ion induced mass spectrometry of nonvolatile organic solids

    International Nuclear Information System (INIS)

    McNeal, C.J.

    1982-01-01

    The mechanisms of molecular and fragment ion production and the various parameters affecting ion yields were discussed by 6 invited speakers from Europe, Canada, and the US at this symposium. The work reported was almost equally divided between that using low-energy (keV) primary ion (or atom) beams, e.g. fast atom bombardment mass spectrometry (FABMS) and secondary ion mass spectrometry (SIMS) and that using high energy (MeV) particles, e.g. heavy ion induced mass spectrometry (HIIDMS) and 252 Cf-plasma desorption mass spectrometry ( 252 Cf-PDMS). Both theoretical foundations and observed experimental results for both techniques are included

  8. Ambient ionization mass spectrometry: A tutorial

    Energy Technology Data Exchange (ETDEWEB)

    Huang, Min-Zong; Cheng, Sy-Chi; Cho, Yi-Tzu [Department of Chemistry, National Sun Yat-Sen University, Kaohsiung, Taiwan (China); Shiea, Jentaie, E-mail: jetea@fac.nsysu.edu.tw [Department of Chemistry, National Sun Yat-Sen University, Kaohsiung, Taiwan (China); Cancer Center, Kaohsiung Medical University, Kaohsiung, Taiwan (China)

    2011-09-19

    Highlights: {yields} Ambient ionization technique allows the direct analysis of sample surfaces with little or no sample pretreatment. {yields} We sort ambient ionization techniques into three main analytical strategies, direct ionization, direct desorption/ionization, and two-step ionization. {yields} The underlying principles of operation, ionization processes, detecting mass ranges, sensitivity, and representative applications of these techniques are described and compared. - Abstract: Ambient ionization is a set of mass spectrometric ionization techniques performed under ambient conditions that allows the direct analysis of sample surfaces with little or no sample pretreatment. Using combinations of different types of sample introduction systems and ionization methods, several novel techniques have been developed over the last few years with many applications (e.g., food safety screening; detection of pharmaceuticals and drug abuse; monitoring of environmental pollutants; detection of explosives for antiterrorism and forensics; characterization of biological compounds for proteomics and metabolomics; molecular imaging analysis; and monitoring chemical and biochemical reactions). Electrospray ionization and atmospheric pressure chemical ionization are the two main ionization principles most commonly used in ambient ionization mass spectrometry. This tutorial paper provides a review of the publications related to ambient ionization techniques. We describe and compare the underlying principles of operation, ionization processes, detecting mass ranges, sensitivity, and representative applications of these techniques.

  9. Ambient ionization mass spectrometry: A tutorial

    International Nuclear Information System (INIS)

    Huang, Min-Zong; Cheng, Sy-Chi; Cho, Yi-Tzu; Shiea, Jentaie

    2011-01-01

    Highlights: → Ambient ionization technique allows the direct analysis of sample surfaces with little or no sample pretreatment. → We sort ambient ionization techniques into three main analytical strategies, direct ionization, direct desorption/ionization, and two-step ionization. → The underlying principles of operation, ionization processes, detecting mass ranges, sensitivity, and representative applications of these techniques are described and compared. - Abstract: Ambient ionization is a set of mass spectrometric ionization techniques performed under ambient conditions that allows the direct analysis of sample surfaces with little or no sample pretreatment. Using combinations of different types of sample introduction systems and ionization methods, several novel techniques have been developed over the last few years with many applications (e.g., food safety screening; detection of pharmaceuticals and drug abuse; monitoring of environmental pollutants; detection of explosives for antiterrorism and forensics; characterization of biological compounds for proteomics and metabolomics; molecular imaging analysis; and monitoring chemical and biochemical reactions). Electrospray ionization and atmospheric pressure chemical ionization are the two main ionization principles most commonly used in ambient ionization mass spectrometry. This tutorial paper provides a review of the publications related to ambient ionization techniques. We describe and compare the underlying principles of operation, ionization processes, detecting mass ranges, sensitivity, and representative applications of these techniques.

  10. Estudo multivariado de solos urbanos da cidade de Teresina

    Directory of Open Access Journals (Sweden)

    Moura Márcio Cleto Soares de

    2006-01-01

    Full Text Available The concentrations of Cu, Pb, Zn, Cr, Ni, Al, Mn and Fe were measured by atomic absorption spectrometry, of 19 topsoil samples collected in the Teresina city urban area to discriminate natural and anthropic contributions and identify possible sources of pollution. The average concentrations of Cu, Zn, Pb and Cr of the urban soils were 6.11, 8.56, 32.12 and 7,17 mg/kg-1, respectively. Statistical analysis techniques, such as principal component analysis (PCA and hierarchical cluster analysis (HCA, were used to analyze the data. Mn, Ni and Cr levels were interpreted as natural contributions, whereas Pb, Zn and, in part, Cu were accounted for mainly by anthropic activities. High Pb levels were observed in the ancient avenues.

  11. Identification of Secreted Candida Proteins Using Mass Spectrometry

    NARCIS (Netherlands)

    Gómez-Molero, E.; Dekker, H.L.; de Boer, A.D.; de Groot, P.W.; Calderone, R.; Cihlar, R.

    2016-01-01

    Analysis of fungal secretomes using mass spectrometry is a useful technique in cell biology. Knowledge of the secretome of a human fungal pathogen may yield important information of host-pathogen interactions and may be useful for identifying vaccines candidates or diagnostic markers for antifungal

  12. X-ray fluorescence spectrometry applied to soil analysis

    International Nuclear Information System (INIS)

    Salvador, Vera Lucia Ribeiro; Sato, Ivone Mulako; Scapin Junior, Wilson Santo; Scapin, Marcos Antonio; Imakima, Kengo

    1997-01-01

    This paper studies the X-ray fluorescence spectrometry applied to the soil analysis. A comparative study of the WD-XRFS and ED-XRFS techniques was carried out by using the following soil samples: SL-1, SOIL-7 and marine sediment SD-M-2/TM, from IAEA, and clay, JG-1a from Geological Survey of Japan (GSJ)

  13. Fast atom bombardment mass spectrometry of condensed tannin sulfonate derivatives

    Science.gov (United States)

    J.J. Karchesy; L.Y. Foo; Richard W. Hemingway; E. Barofsky; D.F. Barofsky

    1989-01-01

    Condensed tannin sulfonate derivatives were studied by fast atom bombardment mass spectrometry (FAB-MS) to assess the feasibility of using this technique for determining molecular weight and structural information about these compounds. Both positive- and negative-ion spectra provided useful data with regard to molecular weight, cation species present, and presence of...

  14. Application of Ge/Li/-spectrometry in boreholes

    International Nuclear Information System (INIS)

    Chrusciel, E.

    1976-01-01

    The paper presents the results of Ge/Li/ spectrometry applications in boreholes. The natural radioactivity measurements as well as rare elements determinations with the use of 252 Cf neutron source and capture-gamma and activation techniques are described. The minimum concentrations of certain elements to be determined in the field circumstances are evaluated on the basis of the model experiments. (author)

  15. 14 C dating by using mass spectrometry with particle accelerator

    International Nuclear Information System (INIS)

    Santos, G.M.; Gomes, P.R.S.; Yokoyama, Y.; Tada, M.L. di; Cresswell, R.G.; Fifield, L.K.

    1999-01-01

    The different aspects concerning the 14 C dating are described, including the cosmogenic origin of 14 C, its production and absorption by matter, the procedures to be followed for the age determination and the associated errors, particularly by the Accelerator Mass Spectrometry (AMS) technique, and the different steps of the sample preparation process. (author)

  16. Statistical analysis of proteomics, metabolomics, and lipidomics data using mass spectrometry

    CERN Document Server

    Mertens, Bart

    2017-01-01

    This book presents an overview of computational and statistical design and analysis of mass spectrometry-based proteomics, metabolomics, and lipidomics data. This contributed volume provides an introduction to the special aspects of statistical design and analysis with mass spectrometry data for the new omic sciences. The text discusses common aspects of design and analysis between and across all (or most) forms of mass spectrometry, while also providing special examples of application with the most common forms of mass spectrometry. Also covered are applications of computational mass spectrometry not only in clinical study but also in the interpretation of omics data in plant biology studies. Omics research fields are expected to revolutionize biomolecular research by the ability to simultaneously profile many compounds within either patient blood, urine, tissue, or other biological samples. Mass spectrometry is one of the key analytical techniques used in these new omic sciences. Liquid chromatography mass ...

  17. Imaging mass spectrometry statistical analysis.

    Science.gov (United States)

    Jones, Emrys A; Deininger, Sören-Oliver; Hogendoorn, Pancras C W; Deelder, André M; McDonnell, Liam A

    2012-08-30

    Imaging mass spectrometry is increasingly used to identify new candidate biomarkers. This clinical application of imaging mass spectrometry is highly multidisciplinary: expertise in mass spectrometry is necessary to acquire high quality data, histology is required to accurately label the origin of each pixel's mass spectrum, disease biology is necessary to understand the potential meaning of the imaging mass spectrometry results, and statistics to assess the confidence of any findings. Imaging mass spectrometry data analysis is further complicated because of the unique nature of the data (within the mass spectrometry field); several of the assumptions implicit in the analysis of LC-MS/profiling datasets are not applicable to imaging. The very large size of imaging datasets and the reporting of many data analysis routines, combined with inadequate training and accessible reviews, have exacerbated this problem. In this paper we provide an accessible review of the nature of imaging data and the different strategies by which the data may be analyzed. Particular attention is paid to the assumptions of the data analysis routines to ensure that the reader is apprised of their correct usage in imaging mass spectrometry research. Copyright © 2012 Elsevier B.V. All rights reserved.

  18. Development of an analytical model for the determination of {sup 60}Co in aqueous samples by atomic absorption and gamma spectrometry techniques; Elaboracion de un modelo analitico para la determinacion de {sup 60}Co en muestras acuosas mediante tecnicas de absorcion atomica y espectrometria gamma

    Energy Technology Data Exchange (ETDEWEB)

    Solis A, N. A.

    2015-07-01

    The applications of the nuclear energy in industry and medicine generate radioactive wastes that must be isolated and confined in order to limit its spread in the biosphere. These types of wastes are generated in hospitals, industry, research centers and nuclear power plants (during de fuel cycle). The radioactive elements (radionuclides) cannot be destroyed by any known method, either chemical or mechanical. Its final destruction is produced by radioactive decay, which makes them stable isotopes, or nuclear transmutation being bombarded with atomic particles. Consequently, the radioactive waste management is to control the radioactive discharges and reduce to tolerable limits, eliminating of effluents and wastes the radionuclides of interest, concentrating them so they can be stored or evacuated so that later not appear in dangerous concentration in the biosphere. In Mexico, the main generators of radioactive wastes are the nuclear power plant of Laguna Verde in Veracruz, Hospitals of the public and private sector, in addition Instituto Nacional de Investigaciones Nucleares (ININ) some institutes and facilities of the UNAM and Instituto Politecnico Nacional (IPN) and industries among others. The aqueous radioactive wastes, particularly those from the nuclear power plants contain traces of cobalt-60. Currently there is no model or analytical technique for the separation of this radionuclide, so it became necessary to develop an analytical model for separation and facilitate their disposal. In this paper was shown that atomic absorption and gamma spectrometry techniques can separate the active concentration of the inactive, which is important because the total concentration can be associated through direct relationships with the wear of metal parts of the nuclear reactor, since the metal alloys of the same reactor containing a fraction of cobalt. Also this analytical and mathematical model that can be reproducible and applicable to full sets of samples and that this

  19. Calibration procedures for in vivo sodium iodide spectrometry of plutonium and americium in the human lung

    International Nuclear Information System (INIS)

    Umbarger, C.J.; Jett, J.H.

    1976-01-01

    This paper describes the calibration techniques and associated error analysis for the in vivo measurement by NaI spectrometry of heavy elements in the lung, specifically plutonium and americium. A very brief description of the instrumentation system is included

  20. Characterisation of uremic "Middle molecular"fractions by gas chromatography mass spectrometry, isotachophoresis, and liquid chromatography

    NARCIS (Netherlands)

    Schoots, A.C.; Mikkers, F.E.P.; Claessens, H.A.; Smet, de R.; Landschoot, van N.; Ringoir, S.M.G.

    1982-01-01

    Uremic ultrafiltrates (and normal serum, for comparison) were fractionated by means of gel filtration. The collected fractions were further investigated by combined analytical techniques: "high- performance" liquid chromatography, gas chromatography, mass spectrometry, and isotachophoresis.

  1. DETERMINATION OF TOTAL MERCURY IN FISH TISSUES USING PYROLYSIS ATOMIC ABSORPTION SPECTROMETRY WITH GOLD AMALGAMATION

    Science.gov (United States)

    A simple and rapid procedure for measuring total mercury in fish tissues is evaluated and compared with conventional techniques. Using an automated instrument incorporating combustion, preconcentration by amalgamation with gold, and atomic absorption spectrometry (AAS), mill...

  2. High-field asymmetric waveform ion mobility spectrometry for mass spectrometry-based proteomics.

    Science.gov (United States)

    Swearingen, Kristian E; Moritz, Robert L

    2012-10-01

    High-field asymmetric waveform ion mobility spectrometry (FAIMS) is an atmospheric pressure ion mobility technique that separates gas-phase ions by their behavior in strong and weak electric fields. FAIMS is easily interfaced with electrospray ionization and has been implemented as an additional separation mode between liquid chromatography (LC) and mass spectrometry (MS) in proteomic studies. FAIMS separation is orthogonal to both LC and MS and is used as a means of on-line fractionation to improve the detection of peptides in complex samples. FAIMS improves dynamic range and concomitantly the detection limits of ions by filtering out chemical noise. FAIMS can also be used to remove interfering ion species and to select peptide charge states optimal for identification by tandem MS. Here, the authors review recent developments in LC-FAIMS-MS and its application to MS-based proteomics.

  3. High Field Asymmetric Waveform Ion Mobility Spectrometry (FAIMS) for Mass Spectrometry-Based Proteomics

    Science.gov (United States)

    Swearingen, Kristian E.; Moritz, Robert L.

    2013-01-01

    SUMMARY High field asymmetric waveform ion mobility spectrometry (FAIMS) is an atmospheric pressure ion mobility technique that separates gas-phase ions by their behavior in strong and weak electric fields. FAIMS is easily interfaced with electrospray ionization and has been implemented as an additional separation mode between liquid chromatography (LC) and mass spectrometry (MS) in proteomic studies. FAIMS separation is orthogonal to both LC and MS and is used as a means of on-line fractionation to improve detection of peptides in complex samples. FAIMS improves dynamic range and concomitantly the detection limits of ions by filtering out chemical noise. FAIMS can also be used to remove interfering ion species and to select peptide charge states optimal for identification by tandem MS. Here, we review recent developments in LC-FAIMS-MS and its application to MS-based proteomics. PMID:23194268

  4. Elucidating rhizosphere processes by mass spectrometry – A review

    Energy Technology Data Exchange (ETDEWEB)

    Rugova, Ariana [Division of Analytical Chemistry, Department of Chemistry, University of Natural Resources and Life Sciences-BOKU, Vienna (Austria); Puschenreiter, Markus [Department of Forest and Soil Sciences, Rhizosphere Ecology and Biogeochemistry Group, University of Natural Resources and Life Sciences-BOKU, Vienna (Austria); Koellensperger, Gunda [Institute of Analytical Chemistry, Faculty of Chemistry, University of Vienna, Vienna (Austria); Hann, Stephan, E-mail: stephan.hann@boku.ac.at [Division of Analytical Chemistry, Department of Chemistry, University of Natural Resources and Life Sciences-BOKU, Vienna (Austria)

    2017-03-01

    The presented review discusses state-of-the-art mass spectrometric methods, which have been developed and applied for investigation of chemical processes in the soil-root interface, the so-called rhizosphere. Rhizosphere soil's physical and chemical characteristics are to a great extent influenced by a complex mixture of compounds released from plant roots, i.e. root exudates, which have a high impact on nutrient and trace element dynamics in the soil-root interface as well as on microbial activities or soil physico-chemical characteristics. Chemical characterization as well as accurate quantification of the compounds present in the rhizosphere is a major prerequisite for a better understanding of rhizosphere processes and requires the development and application of advanced sampling procedures in combination with highly selective and sensitive analytical techniques. During the last years, targeted and non-targeted mass spectrometry-based methods have emerged and their combination with specific separation methods for various elements and compounds of a wide polarity range have been successfully applied in several studies. With this review we critically discuss the work that has been conducted within the last decade in the context of rhizosphere research and elemental or molecular mass spectrometry emphasizing different separation techniques as GC, LC and CE. Moreover, selected applications such as metal detoxification or nutrient acquisition will be discussed regarding the mass spectrometric techniques applied in studies of root exudates in plant-bacteria interactions. Additionally, a more recent isotope probing technique as novel mass spectrometry based application is highlighted. - Highlights: • State-of-the-art mass spectrometry methods developed and applied in rhizosphere research are reviewed. • Elemental and molecular mass spectrometry emphasizing different separation techniques (GC, LC or CE) are discussed. • Case studies on metal detoxification

  5. Elucidating rhizosphere processes by mass spectrometry – A review

    International Nuclear Information System (INIS)

    Rugova, Ariana; Puschenreiter, Markus; Koellensperger, Gunda; Hann, Stephan

    2017-01-01

    The presented review discusses state-of-the-art mass spectrometric methods, which have been developed and applied for investigation of chemical processes in the soil-root interface, the so-called rhizosphere. Rhizosphere soil's physical and chemical characteristics are to a great extent influenced by a complex mixture of compounds released from plant roots, i.e. root exudates, which have a high impact on nutrient and trace element dynamics in the soil-root interface as well as on microbial activities or soil physico-chemical characteristics. Chemical characterization as well as accurate quantification of the compounds present in the rhizosphere is a major prerequisite for a better understanding of rhizosphere processes and requires the development and application of advanced sampling procedures in combination with highly selective and sensitive analytical techniques. During the last years, targeted and non-targeted mass spectrometry-based methods have emerged and their combination with specific separation methods for various elements and compounds of a wide polarity range have been successfully applied in several studies. With this review we critically discuss the work that has been conducted within the last decade in the context of rhizosphere research and elemental or molecular mass spectrometry emphasizing different separation techniques as GC, LC and CE. Moreover, selected applications such as metal detoxification or nutrient acquisition will be discussed regarding the mass spectrometric techniques applied in studies of root exudates in plant-bacteria interactions. Additionally, a more recent isotope probing technique as novel mass spectrometry based application is highlighted. - Highlights: • State-of-the-art mass spectrometry methods developed and applied in rhizosphere research are reviewed. • Elemental and molecular mass spectrometry emphasizing different separation techniques (GC, LC or CE) are discussed. • Case studies on metal detoxification and

  6. Capillary supercritical fluid chromatography - Fourier transform infrared spectrometry

    International Nuclear Information System (INIS)

    Olesik, S.V.; French, S.B.; Movotny, M.

    1984-01-01

    One of the most demanding tasks asked of an analytical chemist today is to separate and identify the components of a nonvolatile complex mixture. An efficient separation technique combined with a universal detector that provides structural information, therefore, would be a great asset to analytical chemists. Capillary supercritical fluid chromatography (SFC) - Fourier transform infrared spectrometry (FTIR) shows great potential for being such a technique. SFC-FTIR shows great potential as a very powerful technique for separation and identification of thermally labile and nonvolatile compounds. Research is continuing in these labs to further optimize the technique. 2 refs

  7. Study on the GaAs(110) surface using emitted atom spectrometry

    International Nuclear Information System (INIS)

    Gayone, J.E.; Sanchez, E.A.; Grizzi, O.; Universidad Nacional de Cuyo, Mendoza

    1998-01-01

    The facilities implemented at Bariloche for the ion scattering spectrometry is described, and recent examples of the technique application to determine the atomic structure and the composition of metallic and semiconductor surfaces, pure and with different adsorbates. The surface analysis technique using emitted atom spectrometry is discussed. The sensitivity to the GaAs(110) surface atomic relaxation is presented, and the kinetic of hydrogen adsorption by the mentioned surface is studied

  8. X-ray spectrometry

    International Nuclear Information System (INIS)

    Markowicz, A.A.; Van Grieken, R.E.

    1986-01-01

    In the period under review, i.e, through 1984 and 1985, some 600 articles on XRS (X-ray spectrometry) were published; most of these have been scanned and the most fundamental ones are discussed. All references will refer to English-language articles, unless states otherwise. Also general books have appeared on quantitative EPXMA (electron-probe X-ray microanalysis) and analytical electron microscopy (AEM) as well as an extensive review on the application of XRS to trace analysis of environmental samples. In the period under review no radically new developments have been seen in XRS. However, significant improvements have been made. Gain in intensities has been achieved by more efficient excitation, higher reflectivity of dispersing media, and better geometry. Better understanding of the physical process of photon- and electron-specimen interactions led to complex but more accurate equations for correction of various interelement effects. Extensive use of micro- and minicomputers now enables fully automatic operation, including qualitative analysis. However, sample preparation and presentation still put a limit to further progress. Although some authors find XRS in the phase of stabilization or even stagnation, further gradual developments are expected, particularly toward more dedicated equipment, advanced automation, and image analysis systems. Ways are outlined in which XRS has been improved in the 2 last years by excitation, detection, instrumental, methodological, and theoretical advances. 340 references

  9. Correction factors for photon spectrometry in nuclear parameters study

    International Nuclear Information System (INIS)

    Patrao, Karla Cristina de Souza

    2004-10-01

    The goal of this work was the determination, using metrologic severity, the factors of correction for coincidences XX, Xγ and γγ and the factors of transference of efficiency for use in gamma spectrometry. On this way, it was carried through by determination of nuclear parameters of a nuclide used in medicine diagnostic ( 201 Tl) and the standardization of two environmental samples, of regular and irregular geometry, proceeding from the residual (ashes and slag) from the nuclear industry. The results shows that this adopted methodology is valid, and it allows its application for many different nuclides, including complex decay schema nuclides, using only photons spectrometry techniques on semiconductor detectors. (author)

  10. Native Mass Spectrometry in Fragment-Based Drug Discovery.

    Science.gov (United States)

    Pedro, Liliana; Quinn, Ronald J

    2016-07-28

    The advent of native mass spectrometry (MS) in 1990 led to the development of new mass spectrometry instrumentation and methodologies for the analysis of noncovalent protein-ligand complexes. Native MS has matured to become a fast, simple, highly sensitive and automatable technique with well-established utility for fragment-based drug discovery (FBDD). Native MS has the capability to directly detect weak ligand binding to proteins, to determine stoichiometry, relative or absolute binding affinities and specificities. Native MS can be used to delineate ligand-binding sites, to elucidate mechanisms of cooperativity and to study the thermodynamics of binding. This review highlights key attributes of native MS for FBDD campaigns.

  11. Fast neutron spectrometry and dosimetry

    International Nuclear Information System (INIS)

    Blaize, S.; Ailloud, J.; Mariani, J.; Millot, J.P.

    1958-01-01

    We have studied fast neutron spectrometry and dosimetry through the recoil protons they produce in hydrogenated samples. In spectrometric, we used nuclear emulsions, in dosimetric, we used polyethylene coated with zinc sulphide and placed before a photomultiplier. (author) [fr

  12. Mass Spectrometry of Halopyrazolium Salts

    DEFF Research Database (Denmark)

    Larsen, Elfinn; Egsgaard, Helge; Pande, U. C.

    1983-01-01

    Eleven halogen substituted 1-methyl-2-phenylpyrazolium bromides or chlorides were investigated by field desorption, field ionization, and electron impact mass spectrometry. Dealkylation was found to be the predominant thermal decomposition. An exchange between covalent and ionic halogen prior...

  13. 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

  14. Enantioselectivity of mass spectrometry: challenges and promises.

    Science.gov (United States)

    Awad, Hanan; El-Aneed, Anas

    2013-01-01

    With the fast growing market of pure enantiomer drugs and bioactive molecules, new chiral-selective analytical tools have been instigated including the use of mass spectrometry (MS). Even though MS is one of the best analytical tools that has efficiently been used in several pharmaceutical and biological applications, traditionally MS is considered as a "chiral-blind" technique. This limitation is due to the MS inability to differentiate between two enantiomers of a chiral molecule based merely on their masses. Several approaches have been explored to assess the potential role of MS in chiral analysis. The first approach depends on the use of MS-hyphenated techniques utilizing fast and sensitive chiral separation tools such as liquid chromatography (LC), gas chromatography (GC), and capillary electrophoresis (CE) coupled to MS detector. More recently, several alternative separation techniques have been evaluated such as supercritical fluid chromatography (SFC) and capillary electrochromatography (CEC); the latter being a hybrid technique that combines the efficiency of CE with the selectivity of LC. The second approach is based on using the MS instrument solely for the chiral recognition. This method depends on the behavioral differences between enantiomers towards a foreign molecule and the ability of MS to monitor such differences. These behavioral differences can be divided into three types: (i) differences in the enantiomeric affinity for association with the chiral selector, (ii) differences of the enantiomeric exchange rate with a foreign reagent, and (iii) differences in the complex MS dissociation behaviors of the enantiomers. Most recently, ion mobility spectrometry was introduced to qualitatively and quantitatively evaluate chiral compounds. This article provides an overview of MS role in chiral analysis by discussing MS based methodologies and presenting the challenges and promises associated with each approach. © 2013 Wiley Periodicals, Inc.

  15. Atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Haswell, S.J.

    1991-01-01

    Atomic absorption spectroscopy is now well established and widely used technique for the determination of trace and major elements in a wide range analyte types. There have been many advances in the atomic spectroscopy over the last decade and for this reason and to meet the demand, it was felt that there was a need for an updated book. Whilst interest in instrumental design has tended to dominate the minds of the spectrocopist, the analyst concerned with obtaining reliable and representative data, in diverse areas of application, has been diligently modifying and developing sample treatment and instrumental introduction techniques. Such methodology is de fundamental part of analysis and form the basis of the fourteen application chapters of this book. The text focuses in the main on AAS; however, the sample handling techniques described are in many cases equally applicable to ICP-OES and ICP-MS analysis. (author). refs.; figs.; tabs

  16. ESTUDO PROSPECTIVO SOBRE ENCAPSULAMENTO DE COMPOSTOS BIOATIVOS

    Directory of Open Access Journals (Sweden)

    Larissa Assunção

    2014-12-01

    Full Text Available Com o advento da nanotecnologia, houve o desenvolvimento de técnicas envolvendo processamento, fabricação e aplicação de estruturas, com forma e tamanho controlados, sendo que na indústria de alimentos, estas formulações, tanto na faixa micrométrica como nanométrica, vêm sendo utilizadas com o objetivo de favorecer o produto final. Tendo em vista a importância tecnológica dessa técnica e do grande interesse nacional e internacional, principalmente no ramo da indústria alimentícia, sobre os benefícios do encapsulamento, o presente estudo prospectivo teve como objetivo avaliar o panorama mundial relativo ao tema em questão, correlacionando-o com os documentos de patentes depositados. Para tanto, realizou-se uma pesquisa das patentes na base de dados europeia Espacenet®, utilizando os descritores do tema em estudo associados aos códigos de classificação. As informações encontradas foram compiladas em gráficos e discutidas. Pôde-se observar que o maior número de patentes referiu-se ao código A23L1/00 - alimentos ou produtos alimentícios: a sua preparação ou tratamento e houve um crescimento exponencial em relação ao depósito de patentes nos últimos 10 anos, sendo os Estados Unidos o país líder em número de patentes depositadas (60%. A Firmenich e CIE lidera o ranking com mais patentes depositadas. Em relação à área de atuação, predomina a indústria alimentícia (69%. No que diz respeito ao Brasil, o país aparece com apenas 1 patente detentora desta tecnologia, sendo um número bastante reduzido o que mostra a falta de incentivo neste setor. Diante dos resultados obtidos, concluiu-se que, apesar de ser uma tecnologia recente, observa-se uma tendência ao crescimento de depósito de patentes.

  17. Radio-frequency glow discharge spectrometry: A critical review

    International Nuclear Information System (INIS)

    Winchester, Michael R.; Payling, Richard

    2004-01-01

    This paper presents a critical review of analytical radio frequency glow discharge spectrometry (rf-GDS). The historical foundations of rf-GDS are described, and current knowledge of the fundamental physics of analytical rf glow discharges is discussed. Additionally, instrumentation, methodologies, and applications of rf glow discharge optical emission spectrometry (rf-GDOES) and mass spectrometry (rf-GDMS) are reviewed. Although other rf-GDS techniques have appeared [e.g. rf glow discharge atomic absorption spectrophotometry (rf-GDAAS)], the emphasis is placed upon rf-GDOES and rf-GDMS, because they have received by far the most interest from analytical chemical metrologists. This review also provides explanations of some developments that are needed for further progress in the field of analytical rf-GDS

  18. Further development of IDGS: Isotope dilution gamma-ray spectrometry

    International Nuclear Information System (INIS)

    Li, T.K.; Parker, J.L.; Kuno, Y.; Sato, S.; Kamata, M.; Akiyama, T.

    1991-01-01

    The isotope dilution gamma-ray spectrometry (IDGS) technique for determining the plutonium concentration and isotopic composition of highly radioactive spent-fuel dissolver solutions has been further developed. Both the sample preparation and the analysis have been improved. The plutonium isotopic analysis is based on high-resolution, low-energy gamma-ray spectrometry. The plutonium concentration in the dissolver solutions then is calculated from the measured isotopic differences among the spike, the dissolver solution, and the spiked dissolver solution. Plutonium concentrations and isotopic compositions of dissolver solutions analyzed from this study agree well with those obtained by traditional isotope dilution mass spectrometry (IDMS) and are consistent with the first IDGS experimental result. With the current detector efficiency, sample size, and a 100-min count time, the estimated precision is ∼0.5% for 239 Pu and 240 Pu isotopic analyses and ∼1% for the plutonium concentration analysis. 5 refs., 2 figs., 7 tabs

  19. Detector calibration for in-situ gamma ray spectrometry

    CERN Document Server

    Balea, G

    2002-01-01

    The power in the technique of in-situ spectrometry lies in the fact that a detector placed on ground measures gamma radiation from sources situated over an area of several hundred square meters. The 'field of view' for the detector would be larger for high energy radiation sources and for sources closer to the soil surface. In contrast, a soil sample would represent an area of a few tens of hundreds of square centimeters. In practice, an effective characterization of a site would involve in-situ gamma ray spectrometry in conjunction with soil sampling. As part of an overall program, in-situ gamma ray spectrometry provides a means to assess the degree of contamination in areas during the course of operations in the field, thus guiding the investigator on where to collect samples. It can also substantially reduce the number of samples need to be collected and subsequently analyzed. (author)

  20. Marketing do mercado de luxo: Estudo de caso Victoria's Secret

    OpenAIRE

    Ana Francisca Giuliani

    2013-01-01

    Este artigo teve por objetivo identificar quais são as estratégias de marketing utilizadas pela empresa varejista Victoria’s Secret para a fidelização do consumidor de luxo em nível global. O estudo caracterizou-se como uma pesquisa qualitativa, utilizando-se como estratégia de campo o estudo de caso de caráter ilustrativo. Para o alcance do objetivo proposto, dividiu-se o estudo em duas fases. Na primeira, denominada exploratória, buscou-se em dados secundários o embasamento para a construçã...

  1. Ambient mass spectrometry imaging

    DEFF Research Database (Denmark)

    Janfelt, Christian; Nørgaard, Asger W

    2012-01-01

    , resulting in images of similar quality as DESI. EASI can thus be used in imaging experiments where the application of high voltage is impractical or undesirable. The present study is in its nature also a comparison of the characteristics of the two techniques, showing results also applicable for non-imaging...

  2. Comparative study between endoscopic technique by a proximal port and mini palmary incision in the surgical treatment of carpal tunnel syndrome Estudo comparativo entre a técnica endoscópica pelo portal proximal e a técnica de mini-incisão palmar no tratamento cirúrgico da síndrome do túnel do carpo

    Directory of Open Access Journals (Sweden)

    Eduardo A.R. Pereira

    2003-01-01

    Full Text Available The authors present a prospective study comparing two surgical techniques for carpal tunnel release. A minimal - incision open decompression(3 is compared with an endoscopic release(2, that utilizes only a single proximal portal. There were operated on, 28 wrists in 28 patients, with clinical signs and EMG changes consistent on idiopathic carpal tunnel syndrome, that failed under previous conservative treatment. They were randomized into two groups , undertaken surgical treatment, either by endoscopic release or by open decompression. Grip strength (measured by dynamometric, sensitivity (measured by Semmes-Weinstein monofilaments, presence of pain and paresthesia, date of return to activities of daily living and complications were evaluated pre-operative and at 1, 2, 4, 6, 12 weeks after surgery. After 12 months average follow up, the results indicated that this proximal portal endoscopic technique can be safely performed, showing advantages over open conventional method, in terms of sooner return of grip strength, date of return to activities of daily living, and less incidence of pillar pain. No differences in paresthesia resolution, sensibility improvement or complications incidence were found.Os autores apresentam estudo prospectivo onde comparam duas técnicas cirúrgicas empregadas no tratamento de pacientes acometidos pela síndrome do túnel do carpo. A técnica de descompressão por via aberta, através de mini-incisão palmar(3, é analisada em relação à técnica por via endoscópica, descrita por Agee et al.(2, que utiliza apenas um único portal proximal. Foram operados, de forma randomizada, 28 punhos em 28 pacientes com o diagnóstico clínico e eletromiográfico de síndrome do túnel do carpo idiopático, e que não obtiveram melhora com o tratamento conservador prévio. Os seguintes parâmetros, foram analisados no pré-operatório e na primeira, segunda, quarta, sexta e décima segunda semanas de pós-operatório: força de

  3. Bibliotecas domiciliares: um estudo de caso

    Directory of Open Access Journals (Sweden)

    Adalberto Rego Maciel Filho

    Full Text Available Pesquisa empírica sobre o papel da biblioteca domiciliar e do hábito de leitura dos pais dos professores da Universidade de Pernambuco, na escolaridade dos educadores. 107 professores foram entrevistados (24 especialistas, 60 mestres, 25 doutores. Constatou-se que a residência na infância dos professores da UPE, na média, teria uma biblioteca domiciliar de 119,7 volumes (no Fundamental I; e seus pais, na maioria, liam e tinham quase 11,1 anos de estudo. Simulações também foram realizadas, analisando as relações entre o tamanho das bibliotecas domiciliares e desempenho escolar com dados do PISA, referentes a 27 países e, no caso do Brasil, com 2000 alunos. Os resultados acompanham as conclusões apresentadas na revisão da literatura, que apontam uma correlação positiva entre as duas variáveis. São sugeridas políticas que poderiam influenciar programas já existentes e novos projetos, ou, ainda, incentivar novas pesquisas na área de bibliotecas domiciliares e públicas.

  4. Experimental techniques; Techniques experimentales

    Energy Technology Data Exchange (ETDEWEB)

    Roussel-Chomaz, P. [GANIL CNRS/IN2P3, CEA/DSM, 14 - Caen (France)

    2007-07-01

    This lecture presents the experimental techniques, developed in the last 10 or 15 years, in order to perform a new class of experiments with exotic nuclei, where the reactions induced by these nuclei allow to get information on their structure. A brief review of the secondary beams production methods will be given, with some examples of facilities in operation or under project. The important developments performed recently on cryogenic targets will be presented. The different detection systems will be reviewed, both the beam detectors before the targets, and the many kind of detectors necessary to detect all outgoing particles after the reaction: magnetic spectrometer for the heavy fragment, detection systems for the target recoil nucleus, {gamma} detectors. Finally, several typical examples of experiments will be detailed, in order to illustrate the use of each detector either alone, or in coincidence with others. (author)

  5. Sutura arterial com técnicas contínua e de pontos separados, utilizando-se os fios polipropilene e polidioxanone: estudo experimental em coelhos Arterial suture with continuous and interrupted techniques, using polypropylene and polydioxanone threads: experimental study in rabbits

    Directory of Open Access Journals (Sweden)

    Nelson Leonardo Kerdahi Leite de Campos

    2003-10-01

    Full Text Available OBJETIVO: Observar o comportamento da sutura arterial em aortas abdominais de coelhos em crescimento, comparando-se as técnicas contínua e com pontos separados, empregando-se dois tipos de fios: Polipropilene 7-0 (inabsorvível e Polidioxanone 7-0 (absorvível. MÉTODOS: Grupos: GI - Controle (sem sutura; GII - Polipropilene, Pontos Separados; GIII - Polipropilene, Contínua; GIV - Polidioxanone, Pontos Separados e GV - Polidioxanone, Contínua. Cada grupo foi subdividido em quatro Momentos de Eutanásia: aos 7, 14, 30 e 60 dias de pós-operatório. Foram avaliados: peso dos animais, diâmetros e pulsos arteriais, estenose, trombose, aderências, aortografia, visibilidade do fio, cicatrização e microscopia. RESULTADOS: a após 60 dias, o local da linha de sutura cresceu de forma significativa em todos os grupos; b a técnica de sutura com pontos separados causou menor estenose da linha de sutura, observada tanto no ato cirúrgico, como na eutanásia dos animais; c no exame histopatológico, as diferenças encontradas entre grupos foram transitórias, não persistindo após 60 dias de pós-operatório. CONCLUSÃO: O polidioxanone mostrou ser a melhor opção, entre os dois fios, para sutura de artérias em crescimento, pois causa pouca ou nenhuma restrição ao crescimento arterial na linha de sutura, mesmo quando se emprega a técnica contínua.PURPOSE: To assess the arterial suture, comparing continuous and interrupted techniques, in abdominal aorta of growing rabbbits, using two types of suture material: Polypropylene 7-0 (nonabsorbable and Polydioxanone 7-0 (absorbable. METHODS: Groups: GI - Control, without arterial suture; GII - Polypropylene, Interrupted technique; GIII - Polipropilene, Continuous technique; GIV - Polydioxanone, Interrupted technique and GV - Polydioxanone, Continuous technique. Each group was subdivided in four Moments of Euthanasia , according with the number of days after surgery: 7 , 14 , 30 and 60 days. The

  6. Nuclear magnetic resonance spectrometry

    International Nuclear Information System (INIS)

    Wasson, J.R.; Salinas, J.E.

    1980-01-01

    Of the thousands of publications available for the period from July 1977 to July 1979, only a few were selected for this review. Approximately 130 review sources are summarized in tabular form as to topic(s) covered in the review. Other parts of the review article deal with apparatus and techniques, spectral analysis, computer applications, analytical applications, selected organic systems, and selected inorganic systems. A total of 257 references are cited

  7. Estudo comparativo entre três técnicas de anestesia geral para biópsia de próstata dirigida por ultrassonografia transretal Estudio comparativo entre tres técnicas de anestesia general para biopsia de próstata dirigida por ultrasonido transrectal A comparative study among three techniques of general anesthesia for ultrasound-guided transrectal prostate biopsy

    Directory of Open Access Journals (Sweden)

    Ricardo Antônio Guimarães Barbosa

    2010-10-01

    Full Text Available JUSTIFICATIVA E OBJETIVOS: A biópsia de próstata dirigida por ultrassonografia transretal constitui referência no diagnóstico das neoplasias da próstata. Quanto maior o número de amostras colhidas, maiores a dor e o desconforto relatados pelo paciente. O objetivo do estudo foi comparar três técnicas anestésicas neste grupo de pacientes. MÉTODO: Foram estudados 45 pacientes separados em três grupos: 1 - Propofol; 2 - Propofol + Bloqueio de Plexo Prostático; 3 - Propofol + Fentanil. Os pacientes foram monitorados com pressão arterial não invasiva, eletrocardioscopia contínua, oximetria de pulso (SpO2 e Índice Bispectral. Não receberam medicação pré-anestésica. Foram avaliados os parâmetros hemodinâmicos no intra e pós-operatório, Índice bispectral no intraoperatório, avaliação da dor pela escala numérica verbal (ENV no pós-operatório imediato e uso de dipirona como tratamento da dor pós-operatória. RESULTADOS: Não houve diferença significativa entre os três grupos: variáveis antropométricas, quantidade de propofol, número de fragmentos e tempo do exame. Os parâmetros hemodinâmicos e a SpO2 apresentaram comportamento semelhante nos três grupos durante o estudo. No grupo 1, a dor avaliada pela ENV foi mais elevada e houve maior necessidade de dipirona que nos outros grupos. CONCLUSÕES: Sedação com propofol isolado para biópsia causa maior dor e desconforto pós-operatório do que quando associado a bloqueio do plexo prostático ou a fentanil sistêmico. Além de hipnose, é necessária a realização de analgesia intraoperatória para garantir conforto pósoperatórioJUSTIFICATIVA Y OBJETIVOS: La biopsia de próstata dirigida por ultrasonido transrectal constituye una referencia en el diagnóstico de las neoplasias de la próstata. Mientras mayor es el número de muestras escogidas, mayores son el dolor y la incomodidad relatados por el paciente. El objetivo del estudio fue comparar tres técnicas anest

  8. A technique developed for labeling the green manures (sunnhemp and velvet bean) with {sup 15} N for nitrogen dynamic studies; Tecnica para marcacao dos adubos verdes crotalaria juncea e mucuna-preta com {sup 15} N para estudos de dinamica do nitrogenio

    Energy Technology Data Exchange (ETDEWEB)

    Ambrosano, Edmilson Jose [Instituto Agronomico de Campinas, SP (Brazil). Secao de Leguminosas; Trivelin, Paulo Cesar Ocheuze; Muruoka, Takashi [Centro de Energia Nuclear na Agricultura (CENA), Piracicaba, SP (Brazil)

    1997-07-01

    A technique was developed for labeling the leguminous plant tissue with nitrogen ({sup 15} N) to obtain labelled material for nitrogen dynamic studies. Sunnhemp (crotalaria juncea L.) and velvet beans (Mucuna aterrima, sinonimia Stizolobium aterrimum Piper and Tracy) were grown in pots containing 10 kg of a Red Yellow Podzolic soil, under greenhouse conditions. The rate of 1.2 of nitrogen (ammonium sulphate with 11.37 atom % {sup 15} N) per pot was applied three times. The labelled dried plant material showed 3.177 and 4.337 of atom % {sup 15} N, respectively for velvet beans and sunnhemp. (author)

  9. Mass Spectrometry Imaging, an Emerging Technology in Neuropsychopharmacology

    Science.gov (United States)

    Shariatgorji, Mohammadreza; Svenningsson, Per; Andrén, Per E

    2014-01-01

    Mass spectrometry imaging is a powerful tool for directly determining the distribution of proteins, peptides, lipids, neurotransmitters, metabolites and drugs in neural tissue sections in situ. Molecule-specific imaging can be achieved using various ionization techniques that are suited to different applications but which all yield data with high mass accuracies and spatial resolutions. The ability to simultaneously obtain images showing the distributions of chemical species ranging from metal ions to macromolecules makes it possible to explore the chemical organization of a sample and to correlate the results obtained with specific anatomical features. The imaging of biomolecules has provided new insights into multiple neurological diseases, including Parkinson's and Alzheimer's disease. Mass spectrometry imaging can also be used in conjunction with other imaging techniques in order to identify correlations between changes in the distribution of important chemical species and other changes in the properties of the tissue. Here we review the applications of mass spectrometry imaging in neuroscience research and discuss its potential. The results presented demonstrate that mass spectrometry imaging is a useful experimental method with diverse applications in neuroscience. PMID:23966069

  10. Mass spectrometry imaging, an emerging technology in neuropsychopharmacology.

    Science.gov (United States)

    Shariatgorji, Mohammadreza; Svenningsson, Per; Andrén, Per E

    2014-01-01

    Mass spectrometry imaging is a powerful tool for directly determining the distribution of proteins, peptides, lipids, neurotransmitters, metabolites and drugs in neural tissue sections in situ. Molecule-specific imaging can be achieved using various ionization techniques that are suited to different applications but which all yield data with high mass accuracies and spatial resolutions. The ability to simultaneously obtain images showing the distributions of chemical species ranging from metal ions to macromolecules makes it possible to explore the chemical organization of a sample and to correlate the results obtained with specific anatomical features. The imaging of biomolecules has provided new insights into multiple neurological diseases, including Parkinson's and Alzheimer's disease. Mass spectrometry imaging can also be used in conjunction with other imaging techniques in order to identify correlations between changes in the distribution of important chemical species and other changes in the properties of the tissue. Here we review the applications of mass spectrometry imaging in neuroscience research and discuss its potential. The results presented demonstrate that mass spectrometry imaging is a useful experimental method with diverse applications in neuroscience.

  11. Estudo macroscópico e dinamométrico comparativo de implantes (ímãs recobertos e de suas técnicas de fixação em órbitas de coelhas Comparative macroscopic and dynamometric study of implants (covered magnets and techniques of their fixation in orbits of female rabbits

    Directory of Open Access Journals (Sweden)

    Elcio Roque Kleinpaul

    2004-06-01

    Full Text Available OBJETIVOS: Avaliação clínica dos sinais da reação inflamatória de fixação de implante orbitário (ímã recoberto por ouro e avaliação macroscópica de sua resistência aos fluidos orgânicos. MÉTODOS: Estudo experimental em 54 coelhas adultas, divididas em três grupos de 18, com 3 subgrupos de 6 de acordo com o material usado para fixação, avaliação com uma, três e seis semanas de pós-operatório. Fixação, no rebordo inferior da órbita, de implante (ímã e ouro por meio de cola ou parafuso ou fio inabsorvível (Mersilene 5.0®. As órbitas contralaterais (sem implante compuseram o grupo-controle. Medidas da resistência à tração tangencial do implante fixado. RESULTADOS: Sinais clínicos de reação inflamatória à fixação orbitária do implante foram observados com cianoacrilato, parafuso, ou sutura inabsorvível (Mersilene 5.0®, até a sexta semana de pós-operatório, sendo mais intensa no grupo F (fixação com fio. A força de tração de 80 gf, independentemente do tipo de fixação, não produziu arrancamentos em 94,5% dos implantes na primeira semana, 100% na terceira semana e em 94,5% dos casos na sexta semana. CONCLUSÃO: Sinais clínicos de reação inflamatória do implante e sua fixação foram observados com cianoacrilato ou parafuso ou sutura inabsorvível (Mersilene 5.0® até a sexta semana pós-operatória, sendo mais intensa no grupo F (fio. A resistência do implante aos fluídos orgânicos mostrou falha em 9,3% (implante com dano.PURPOSE: To evaluate the clinical signs of inflammatory reaction in the fixation of an orbitary implant (magnet, covered by gold, and to evaluate the macroscopic resistance to organic fluids of the used implants. METHODS: An experimental study was performed in 54 adult female rabbits, divided into 3 groups of eighteen with 3 subgroups of 6 according to the material used for fixation; the implants were evaluated at weeks 1, 3 and 6 after surgery. An implant (magnet

  12. Impact of automation on mass spectrometry.

    Science.gov (United States)

    Zhang, Yan Victoria; Rockwood, Alan

    2015-10-23

    Mass spectrometry coupled to liquid chromatography (LC-MS and LC-MS/MS) is an analytical technique that has rapidly grown in popularity in clinical practice. In contrast to traditional technology, mass spectrometry is superior in many respects including resolution, specificity, multiplex capability and has the ability to measure analytes in various matrices. Despite these advantages, LC-MS/MS remains high cost, labor intensive and has limited throughput. This specialized technology requires highly trained personnel and therefore has largely been limited to large institutions, academic organizations and reference laboratories. Advances in automation will be paramount to break through this bottleneck and increase its appeal for routine use. This article reviews these challenges, shares perspectives on essential features for LC-MS/MS total automation and proposes a step-wise and incremental approach to achieve total automation through reducing human intervention, increasing throughput and eventually integrating the LC-MS/MS system into the automated clinical laboratory operations. Copyright © 2015 Elsevier B.V. All rights reserved.

  13. [Mass spectrometry in the clinical microbiology laboratory].

    Science.gov (United States)

    Jordana-Lluch, Elena; Martró Català, Elisa; Ausina Ruiz, Vicente

    2012-12-01

    Infectious diseases are still a cause of high mortality and morbidity rates. Current microbiological diagnostic methods are based on culture and phenotypic identification of isolated microorganisms, which can be obtained in about 24-48 h. Given that the microbiological identification is of major importance for patient management, new diagnostic methods are needed in order to detect and identify microorganisms in a timely and accurate manner. Over the last few years, several molecular techniques based on the amplification of microbial nucleic acids have been developed with the aim of reducing the time needed for the identification of the microorganisms involved in different infectious processes. On the other hand, mass spectrometry has emerged as a rapid and consistent alternative to conventional methods for microorganism identification. This review describes the most widely used mass spectrometry technologies -matrix-assisted laser desorption/ionization time-of-flight (MALDI-TOF) and electrospray ionization time-of-flight (ESI-TOF)-, both for protein and nucleic acid analysis, as well as the commercial platforms available. Related publications of most interest in clinical microbiology are also reviewed. Copyright © 2011 Elsevier España, S.L. All rights reserved.

  14. Valor do estudo citogenetico no transexualismo

    Directory of Open Access Journals (Sweden)

    P. H. Saldanha

    1976-09-01

    Full Text Available O transexualismo é caracterizado como uma entidade psiquiátrica, distinta do homossexualismo e travestismo, revendo-se suas manifestações sindrômicas. Discutem-se as duas principais causas etiológicas plausíveis do transexualismo, a saber: a hipótese psicoanalítica fundamentada na regressão psicossexual com estampagem da figura materna e o modelo neuro-endócrino que pressupõe alterações nos centros de identidade sexual do hipotámo. Com base nesta última explicação propõe-se, a exemplo do que parece ocorrer na síndrome de Morris, cujas células (XY não respondem ao efeito masculinizante da testosterona plasmática, que os transexuais devem possuir mosaicismo detectável ou críptico, quanto aos cromossomos sexuais, nos centros hipotalâmicos de identidade sexual que não respondem à secreção androgênica produzida pela gônada primitiva. Esta possibilidade explicaria a excessiva prevalência da síndrome entre homens, bem como a sua manifestação com feições típicas no sexo masculino e ainda a ocorrência esporádica da síndrome. O estudo citogenético revelou que a frequência (32% de mosaicismo quanto aos cromossomos sexuais em 25 transexuais é estatisticamente superior aos valores observados em 14 homossexuais e 40 controles normais, nos quais a proporção de mosaicismo é praticamente nula. Considera-se a possibilidade do critério cariotípico constituir valioso subsídio na diagnose da síndrome.

  15. Symposium on accelerator mass spectrometry

    International Nuclear Information System (INIS)

    1981-01-01

    The area of accelerator mass spectrometry has expanded considerably over the past few years and established itself as an independent and interdisciplinary research field. Three years have passed since the first meeting was held at Rochester. A Symposium on Accelerator Mass Spectrometry was held at Argonne on May 11-13, 1981. In attendance were 96 scientists of whom 26 were from outside the United States. The present proceedings document the program and excitement of the field. Papers are arranged according to the original program. A few papers not presented at the meeting have been added to complete the information on the status of accelerator mass spectrometry. Individual papers were prepared separately for the data base

  16. Symposium on accelerator mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    None

    1981-01-01

    The area of accelerator mass spectrometry has expanded considerably over the past few years and established itself as an independent and interdisciplinary research field. Three years have passed since the first meeting was held at Rochester. A Symposium on Accelerator Mass Spectrometry was held at Argonne on May 11-13, 1981. In attendance were 96 scientists of whom 26 were from outside the United States. The present proceedings document the program and excitement of the field. Papers are arranged according to the original program. A few papers not presented at the meeting have been added to complete the information on the status of accelerator mass spectrometry. Individual papers were prepared separately for the data base.

  17. New trends in nuclear spectrometry

    International Nuclear Information System (INIS)

    Westmeier, W.; Siemon, K.

    2013-01-01

    An overview on the status and function of current spectrometry hardware, of detectors having energy-dispersive (spectrometric) properties as well as of the latest developments in quantitative spectrometry software is presented. Making extensive use of modern computing power, new strategies in high-precision spectrum analysis have been developed which enhance the quality of results and also open new fields of spectrometric applications. Three principles have been newly introduced to spectrum analysis software: -use no approximations in modelling (Physics, no numerology) -apply all available models to find a solution (Fuzzy Logic) -repeat complete analyses for iterative improvement (Learn from results). -- Highlights: ► We present an overview of MCA hardware and detectors for nuclear spectrometry. ► Physics-oriented descriptions, Fuzzy Logic and multiple repetitive analyses lead to improved results in spectrum analysis. ► New strategies allow the successful deconvolution of spectra that could not be analysed before

  18. Estudos sobre a Esquistosomose em Pernambuco, Brasil

    Directory of Open Access Journals (Sweden)

    Aggeu Magalhães

    1940-01-01

    Full Text Available Os autores referem os resultados dos estudos sobre esquistosomose realisados, em Pernambuco, de Novembro de 1938 a Dezembro de 1939. Não se extendem em discussão, nem comentarios, tampouco, relacionam suas verificações com o que já foi relatado sobre o assunto em trabalhos nacionais e estrangeiros, pelo fato de que, não se trata de um resultado definitivo e sim de atividades que irão proseguir. Os estudos sistematicos em torno da endemia esquistosomica foram executados em duas localidades diversas pela população e pela situação geografica e ecologica. Pontezinha é uma povoação de 1200 habitantes localizada proximo a um conjunto de charcos e lagõas de agua dôce onde pululam caramujos do tipo olivaceus de Spix, e apresenta uma taxa de infestação de 21,4% para individuos do sexo masculino, e de 14,7% para os do sexo feminino. A distribuição por grupos de idade mostra que a incidencia cresce até o grupo de 16 a 20 anos de idade, quando atinge a percentagem de 37,8%, para decrescer em seguida. Em Vitoria a incidencia foi maior nos indivíduos do sexo feminino, atingindo a taxa de 41,4%, dando o sexo masculino a taxa de 36,9%. Por idade a percentagem maxima é atingida pelo grupo de 11 a 15 anos. Vitoria é uma cidade de 1500 habitantes, construida á margem do rio Tapacurá, onde se encontram numerosos caramujos do tipo centimetralis Lutz. A divergencia de incidencia corre por conta dos habitos da população e pela utilização que ela faz do rio, sendo maior em Vitoria porque a proximidade do rio facilita o uso de suas aguas para banho e serviços domesticos, condicionando este ultimo fato, a maior infestação das mulheres. O estudo da frequencia da infestação dos caramujos por cercarias de diversos trematodios, permite suspeitar uma relação inversa entre a taxa de infestação e o diametro maximo atingido pelos caramujos, parecendo este fato confirmar os trabalhos de Vianna Martins sobre a identidade dos hospedeiros

  19. Study of deformation and fracture micro mechanisms of titanium alloy Ti-6Al-4V using electron microscopy and and X-ray diffraction techniques; Estudo dos micromecanismo de deformacao e fratura da liga de titanio Ti-6Al-4V utizando-se tecnicas de microscopia eletronica e difracao de raios X

    Energy Technology Data Exchange (ETDEWEB)

    Morcelli, Aparecido Edilson

    2009-07-01

    This present work allowed the study of deformation and fracture micro mechanisms of titanium alloy Ti-6Al-4V, used commercially for the manufacture of metallic biomaterials. The techniques employed for the analysis of the material under study were: scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray diffraction (XRD). The study of the influence and behavior of the phases present in titanium alloys is important to evaluate the behavior of cracks in titanium alloys with high mechanical strength, which have fine alpha ({alpha}), beta ({beta}) and ({alpha}{+-}{beta}) microstructure, linking the presence of the phases with the strength of the material. The evaluation in situ of deformation and fracture micro mechanisms were performed by TEM and was also a study of phase transformations during cooling in titanium alloys, using the techniques of bright field, dark field and diffraction of electrons in the selected area. After heat treatment differences were observed between the amount of in relation to the original microstructure of the {beta} and {alpha} phases material for different conditions used in heat treatment applied to the alloy. The presence of lamellar microstructure formed during cooling in the {beta} field was observed, promoting the conversion of part of the secondary alpha structure in {beta} phase, which was trapped between the lamellar of alpha. (author)

  20. Cortisol production rates measured by liquid chromatography/mass spectrometry

    International Nuclear Information System (INIS)

    Esteban, N.V.; Yergey, A.L.

    1990-01-01

    Cortisol production rates (FPRs) in physiologic and pathologic states in humans have been investigated over the past 30 years. However, there has been conflicting evidence concerning the validity of the currently accepted value of FPRs in humans (12 to 15 mg/m2/d) as determined by radiotracer methodology. The present study reviews previous methods proposed for the measurement of FPRs in humans and discusses the applications of the first method for the direct determination of 24-hour plasma FPRs during continuous administration of a stable isotope, using a thermospray high-pressure liquid chromatography-mass spectrometry technique. The technique is fast, sensitive, and, unlike gas chromatography-mass spectrometry methods, does not require derivatization, allowing on-line detection and quantification of plasma cortisol after a simple extraction procedure. The results of determination of plasma FPRs by stable tracer/mass spectrometry are directly in units of mass/time and, unlike radiotracer methods, are independent of any determination of volume of distribution or cortisol concentration. Our methodology offers distinct advantages over radiotracer techniques in simplicity and reliability since only single measurements of isotope ratios are required. The technique was validated in adrenalectomized patients. Circadian variations in daily FRPs were observed in normal volunteers, and, to date, results suggest a lower FRP in normal children and adults than previously believed. 88 references

  1. Estudo comparativo da eficiência de diferentes técnicas de mensuração da concentração espermática em suínos Efficiency of different measurement techniques of sperm concentration in swine

    Directory of Open Access Journals (Sweden)

    Wagner Loesch Vianna

    2004-12-01

    Full Text Available A inseminação artificial (IA em suínos é uma técnica cada vez mais utilizada na suinocultura moderna, pois propicia ao suinocultor vantagens quanto ao desempenho dos reprodutores, ao controle dos cruzamentos e à facilidade na introdução de material genético. Objetivando o aperfeiçoamento da técnica de IA, foram avaliadas a acurácia, a precisão e a robustez do Espermiodensímetro (ESPERMIO e do Espectrofotômetro (ESPECTRO, em comparação à Câmara de Neubauer. Utilizaram-se 142 ejaculados, que revelaram concentrações espermáticas médias (em milhões de sptz/mL e número médio de doses que poderiam ser produzidas, respectivamente, de 229,1 e 22,6; 185,0 e 18,5; 283,6 e 28,0 para a Câmara de Neubauer, o Espectrofotômetro e o Espermiodensímetro. O viés médio (acurácia e o desvio-padrão do viés médio (precisão do ESPECTRO, em comparação à Câmara de Neubauer, foram, respectivamente, de - 44,1 e 52,6, enquanto para o ESPERMIO foram de 54,5 e 44,8 (milhões de sptz/mL. Pode-se inferir que o ESPECTRO tende a subestimar e o ESPERMIO, a superestimar a concentração espermática, em comparação à Câmara de Neubauer. O ESPECTRO foi mais acurado e igualmente preciso que o ESPERMIO. A influência do volume de ejaculado sobre os resultados do ESPERMIO e do ESPECTRO pode ser comprovada pelos resultados de robustez para o volume do ejaculado.Artificial Insemination (AI in swines is a rising technique that has been used during the last years at the swine production systems, because it furnish several advantages to the producers just like boar high efficiency, better breeding control and easiness in introducing foreign genetic materials. Accuracy, precision and robustness for ejaculation volume of spermdensimeter (ESPERMIO and spectrofotometer (ESPECTRO in relation to the Neubauer Count, designed as the standard technique, were evaluated objectifying higher performance of AI technique. A total of 142 boar ejaculation was used

  2. Study of the areas and thicknesses of mesiobucal root canals prepared by three endodontic techniques Estudo das áreas e espessuras de canais radiculares mésio-vestibulares preparados por três técnicas endodônticas

    Directory of Open Access Journals (Sweden)

    Isa Geralda Teixeira Constante

    2007-06-01

    Full Text Available The purpose of this study was to compare, in vitro, by means of computerized analysis of digital radiographic images, the anatomic alterations produced in the mandibular molar tooth dentinal walls of mesiobucal canals with severe curvature by three different endodontic techniques: Progressive Preparation, Staged and Serial Preparation. A selection was made of 45 extracted, human, mandibular molars, with root curvatures greater than 25°. They were divided into three groups for every technique studied, which were then sub-divided into three sub-groups in accordance with the position of the curvature along the root: cervical, median or apical. After access surgery and tooth length determination, the canals were filled with 100% Barium Sulphate radiological contrast and the teeth were then radiographed with a direct digital radiography system, using a special apparatus capable of keeping the samples in the same spatial position during the different radiographic takes. After the above-mentioned endodontic techniques had been performed, the teeth were again filled with Barium sulphate and were also radiographed under the same previously mentioned conditions. The pre- and post-operative digital images were then analyzed in two computerized programs, AutoCAD 2004 and CorelDraw 10, to assess, respectively, the areas and the horizontal alterations which occurred in the internal and external walls of the root canals. The results indicated that although no significant differences among the techniques were shown in the statistical analysis, in a descriptive analysis the Progressive Preparation technique was shown to be more regular, uniform and effective.Objetivou-se comparar, in vitro, através de análise computadorizada de imagens radiográficas digitais, as alterações anatômicas promovidas nas paredes dentinárias de canais mésio-vestibulares com curvatura severa de molares inferiores por três técnicas endodônticas diferentes: Preparo Progressivo

  3. Estudo das Técnicas de Bioengenharia, Motomecanização e a Implantação de Parque Linear na Bacia do Córrego do Limoeiro | A Study of Bioengineering Techniques, Mechanization and Implementation at the Basin of the Limoeiro Stream

    Directory of Open Access Journals (Sweden)

    Diogo Laercio Gonçalves

    2014-05-01

    Full Text Available Normal 0 21 false false false PT-BR X-NONE X-NONE Introduction: The main focus of this study is the application of knowledge concerning technology and techniques of environmental recovery in Permanent Preservation Areas (APP at the basin of the Limoeiro stream, comprising the Balneário da Amizade in the municipalities of Álvares Machado and Presidente Prudente, in the State of São Paulo, particularly in the Residencial Maré Mansa and Parque Imperial neighbour hoods, taking account of the importance of APPs in the life of the urban population. Among the main objectives of this research, is a study of the techniques and technology of soil bioengineering in the recovery of the banks of the stream along with mechanization techniques used by the São Paulo Agricultural Development Company (CODASP at its regional headquarters in Presidente Prudente. It is hoped to elaborate on plans for environmental restoration in the basin area of the Limoeiro stream with research for the betterment of the population, as well as outlining a proposal for a linear park with the objective of incorporating an APP in the district, looking towards a better integration between society and nature. Methodology and Development: The methodological procedures covered in this research include a literary review of such topics as bioengineering, APPs, and environmental legislation, as well as field work with CODASP to identify mechanization techniques used to counter erosion. ALOS Satellite images, available at UNESP, are being used to determine the character of the stream basin, plus the cartographic databases of IGC, CPRM and IBGE, part of the GADIS research group, using ArcGIS and SPRING software. We propose to forward the results of this survey to the relevant bodies such as the municipalities of both cities and the River Basin Committee of Pontal do Paranapanema in the hope that these organs will take action to improve the lives of residents in the basin area. Final

  4. Mass spectrometry for biomarker development

    Energy Technology Data Exchange (ETDEWEB)

    Wu, Chaochao; Liu, Tao; Baker, Erin Shammel; Rodland, Karin D.; Smith, Richard D.

    2015-06-19

    Biomarkers potentially play a crucial role in early disease diagnosis, prognosis and targeted therapy. In the past decade, mass spectrometry based proteomics has become increasingly important in biomarker development due to large advances in technology and associated methods. This chapter mainly focuses on the application of broad (e.g. shotgun) proteomics in biomarker discovery and the utility of targeted proteomics in biomarker verification and validation. A range of mass spectrometry methodologies are discussed emphasizing their efficacy in the different stages in biomarker development, with a particular emphasis on blood biomarker development.

  5. Estudo prospectivo comparativo de duas técnicas cirúrgicas de extração extra-capsular planejada de catarata com implante de lente intra-ocular: incisão limbar e incisão escleral tunelizada Prospective comparative study of two techniques of planned extracapsular cataract extraction: limbal incision and scleral tunnel incision

    Directory of Open Access Journals (Sweden)

    Lincoln Lemes Freitas

    2001-06-01

    Full Text Available Introdução: A catarata é responsável por 50% da cegueira no mundo, com um número estimado de 15 milhões de casos que necessitariam cirurgia. Diferentes técnicas para a extração extra-capsular da catarata com implante de lente intra-ocular foram propostas. Objetivo: Comparar as técnicas para extração extra-capsular de catarata com implante de lente intra-ocular utilizando incisão limbar e incisão escleral tunelizada. Métodos: Foram avaliados, prospectivamente, 59 olhos de 54 pacientes com acompanhamento pós-operatório de 6 meses. Aleatoriamente, os pacientes foram divididos em dois grupos. No Grupo I (n=30, a técnica realizada foi a de extração extra-capsular com implante de lente intra-ocular com incisão limbar e no Grupo II (n=29, com incisão tunelizada. Foram avaliadas as medidas da acuidade visual corrigida, inflamação intra-ocular (células e "flare", tempo de cirurgia, microscopia especular, astigmatismo ceratométrico induzido e paquimetria. Resultados: O tempo de cirurgia, a perda de células endoteliais e o astigmatismo ceratométrico induzido foram estatisticamente maiores no Grupo I que no Grupo II. Não houve diferença estatisticamente significante entre os grupos I e II quanto à acuidade visual, a quantidade de células na câmara anterior, a quantidade de "flare" na câmara anterior e paquimetria. Conclusão: A técnica para extração extra-capsular de catarata com incisão tunelizada apresentou vantagens quanto ao tempo de cirurgia, perda de células endoteliais e astigmatismo induzido em relação à técnica com incisão limbar. Os passos utilizados nessa técnica visam facilitar a extração da catarata, além de treinar o cirurgião para uma transição mais segura para facoemulsificação, sem aumentar o custo da cirurgia.Purpose: Cataract is the main cause of blindness throughout the world, affecting more than 15 million people worldwide. There are different techniques for extracapsular cataract

  6. Comparative study of different Al{sub 2}O{sub 3}:C dosimeters using OSL technique for dosimetry on Volumetric Modulated Arc Radiotherapy Treatment (VMAT); Estudo comparativo de diferentes dosimetros de Al{sub 2}O{sub 3}:C pela tecnica OSL na dosimetria de tratamentos Radioterapicos por Arco Modulado Volumetrico (VMAT)

    Energy Technology Data Exchange (ETDEWEB)

    Villani, Daniel; Campos, LetIcia L., E-mail: dvillani@ipen.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil); Mancini, Anselmo; Haddad, Cecilia M.K. [Hospital Sirio-Libanes, Sao Paulo, SP (Brazil). Centro de Radioterapia

    2016-07-01

    In modern radiotherapy, the VMAT technique has become a successful treatment alternative. Due to its complexity, a quality assurance program must be established by evaluating, among other items, the dosimetric factors. This paper aims to compare the performance between the OSL aluminum oxide (Al{sub 2}O{sub 3}:C) nanoDot™ dosimeters (Inlight™ system) manufactured by Landauer Inc. and TLD-500 Al{sub 2}O{sub 3}:C dosimeters manufactured by Rexon™ for VMAT dosimetry using an anthropomorphic phantom. The results showed that both type of Al{sub 2}O{sub 3}:C dosimeters presented good repeatability and agreement between the doses measured and calculated by planning system. However, the need of sophisticated readers to OSL analysis of the TLD-500, turns it less practical for routine usage, comparing to Inlight™ system. (author)

  7. Effects of two different deep digital flexor tenotomy techniques on distal articular angles of equine cadaver forelimbs Efeito de duas técnicas de tenotomia do flexor digital profundo sobre os ângulos articulares distais dos membros anteriores de equinos: estudo post-mortem

    Directory of Open Access Journals (Sweden)

    Antonio Cezar de Oliveira Dearo

    2012-11-01

    Full Text Available Deep digital flexor (DDF tenotomy is a technique employed for years to treat selected disorders of the musculoskeletal system in horses. Although two different surgical approaches (i.e. mid-metacarpal and pastern have been described for performing the procedure, in vitro quantitative data regarding the modifications induced by either technique on the distal articular angles is lacking. Therefore, the purpose of the study reported here was to investigate the viability of a proposed biomechanical system of induced-traction used to compare the two DDF tenotomy techniques by measuring the distal articular angles of equine cadaver forelimbs. Ten pairs of forelimbs were collected and mounted to a biomechanical system developed to apply traction at the toe level. Dorsal articular angles of the metacarpophalangeal (MP, proximal interphalangeal (PIP and distal interphalangeal (DIP joints were determined by geometric lines on radiographs taken before and after performing each technique. Comparisons between each tenotomy group and its own control, for each joint, and between the two tenotomy groups using as variable the difference between the tenotomy and control groups were tested. Despite the lack of statistical significance, the DDF tenotomy technique at the pastern level produced extension, to a lesser and greater extent, of the PIP and DIP joints, respectively when compared to the mid-metacarpal level. No remarkable differences could be observed for the MP joint. The developed traction-induced biomechanical construct seemed to be effective in producing valuable quantitative estimations of the distal articular angles of equine cadaver forelimbs subjected to different DDF tenotomy techniques.A tenotomia do flexor digital profundo (FDP é uma das técnicas cirúrgicas empregadas para o tratamento de algumas anormalidades osteomusculares, como as deformidades flexurais e a laminite em equinos. Embora diferentes acessos cirúrgicos (i.e. terço médio do

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

    Science.gov (United States)

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

    2017-09-01

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

  9. New possibilities in prompt gamma ray spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Borderie, B; Barrandon, J N [Centre National de la Recherche Scientifique, 45 - Orleans-la-Source (France). Lab. du cyclotron; Pinault, J L [Bureau de Recherches Geologiques et Minieres (BRGM), 45 - Orleans (France)

    1977-01-01

    Prompt gamma ray spectrometry has been used as an analytical tool for many years. The high level of background noise does, however, remain a major problem with this technique. From simple theoretical consideration, conditions (particle, energy) were determined to reduce significantly the background noise under irradiation. Alpha particles of 3.5 MeV were chosen. Some fifty elements were studied, of which 24 gave interesting results. The detection limits obtained for a sample of niobium were as follows: approximately 1 ppm (10/sup -6/g/g) for the light elements Li, B, F and Na, and between 50 ppm and 1% for the others. Numerous applications may be envisaged in the geo- and cosmo-sciences.

  10. Recent development in isotope ratio mass spectrometry

    International Nuclear Information System (INIS)

    Platzner, I.

    1992-01-01

    Within the limited of this review the following topics will be briefly discussed: a) Accuracy, precision, internal relative standard deviation (RISD) and external relative standard deviation (RESD) of isotope ratio measurements. With advanced instrumentation and use of standard reference materials, high accuracy and RESD = 0.002% (or better) may be achieved; b) The advantages of modern automatic isotope ratio mass spectrometer are briefly described. Computer controlled operation and data acquisition, and multiple ion collection are the recent important improvement; c) The isotopic fractionation during the course of isotope ratio measurement is considered as a major source of errors in thermal ionization of metallic elements. The phenomenon in strontium, neodymium, uranium, lead and calcium and methods to correct the measured data are discussed; d) Applications of isotope ratio mass spectrometry in atomic weight determinations, the isotope dilution technique, isotope geology, and isotope effects in biological systems are described together with specific applications in various research and technology area. (author)

  11. Radiocarbon positive-ion mass spectrometry

    International Nuclear Information System (INIS)

    Freeman, Stewart P.H.T.; Shanks, Richard P.; Donzel, Xavier; Gaubert, Gabriel

    2015-01-01

    Proof-of-principle of a new mass spectrometric technique for radiocarbon measurement is demonstrated. Interfering nitrogen and hydrocarbon molecules are largely eliminated in a charge-exchange cell operating on non-metallic gas. The positive-to-negative ion conversion is the reverse of that conventionally used in accelerator mass spectrometry (AMS) and is compatible with plasma ion sources that may be significantly more efficient and capable of greater output than are AMS sputter ion sources. The Nanogan electron cyclotron resonance (ECR) ion source employed exhibited no sample memory and the >50 kyrs age range of AMS was reproduced. A bespoke prototype new instrument is now required to optimise the plasma and cell physics and to realise hypothetical performance gains over AMS.

  12. Radiocarbon positive-ion mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Freeman, Stewart P.H.T.; Shanks, Richard P. [Scottish Universities Environmental Research Centre (SUERC), Scottish Enterprise Technology Park, East Kilbride G75 0QF (United Kingdom); Donzel, Xavier; Gaubert, Gabriel [Pantechnik S.A., 13 Rue de la Résistance, 14400 Bayeux (France)

    2015-10-15

    Proof-of-principle of a new mass spectrometric technique for radiocarbon measurement is demonstrated. Interfering nitrogen and hydrocarbon molecules are largely eliminated in a charge-exchange cell operating on non-metallic gas. The positive-to-negative ion conversion is the reverse of that conventionally used in accelerator mass spectrometry (AMS) and is compatible with plasma ion sources that may be significantly more efficient and capable of greater output than are AMS sputter ion sources. The Nanogan electron cyclotron resonance (ECR) ion source employed exhibited no sample memory and the >50 kyrs age range of AMS was reproduced. A bespoke prototype new instrument is now required to optimise the plasma and cell physics and to realise hypothetical performance gains over AMS.

  13. Radiocarbon dating with accelerator mass spectrometry

    International Nuclear Information System (INIS)

    Blake, W. Jr.

    1985-01-01

    Radiocarbon dating by means of accelerator mass spectrometry (AMS) has two great advantages over conventional dating: 1) much smaller samples can be handled and 2) counting time is significantly shorter. Three examples are given for Holocene-age material from east-central Ellesmere Island. The results demonstrate the potential use of this technique as a powerful research tool in studies of Quaternary chronology. Individual fragments of marine shells as small as 0.1 g have been dated successfully at the IsoTrace Laboratory, University of Toronto. In the case of an aquatic moss from a lake sediment core, an increment 0.5 cm thick could be used instead of a 5 cm-thick slice, thus allowing a much more precise estimate of the onset of organic sedimentation

  14. Handbook of laboratory techniques

    International Nuclear Information System (INIS)

    2002-01-01

    The Nuclear Regulatory Authority in Argentina have laboratories of support to regulations functions on radiological and nuclear safety, safeguards and physical protection, that have a surface of 2950 m 2 in the Ezeiza Atomic Center. The manual describes in seven chapters the different techniques developed and applied in the laboratories along four decades of existence. The chapter 1: Dedicated to the treatment of environmental samples, described the procedures associated with the different types of samples: deposits, waters, sediments, vegetables, milk, fish and diet. The chapter 2: Details 48 radiochemical techniques associated to the measurements of americium 241, carbon 16, strontium 90, iodine 129, plutonium, radium 226, radon, uranium, nickel and actinides. The chapter 3: Describes the measurements techniques of alpha and gamma spectrometry. The different techniques of biological and physical dosimetry are described in the chapters 5 and 6 respectively. The final chapter is dedicated the techniques of external and internal contamination. It s important to emphasize that this manual contains the standardized technologies that the Nuclear Regulatory Authority of Argentina submits regularly to international comparisons

  15. Alpha spectrometry without chemistry

    International Nuclear Information System (INIS)

    Murray, A.S.; Heaton, B.

    1983-01-01

    A gridded cylindrical pulse ionization chamber is considered for the simultaneous analysis of natural alpha emitters. Solid sources of up to 0.3 g are deposited after wet grinding as a thin layer on 1.1 m 2 of aluminized plastic film, which acts as the cathode. No chemistry is involved, and thus there is little chance of nuclide fractionation. With a ''weightless'' source the resolution is about 55 keV; 110 keV has been easily achieved at 4.2 MeV with real sources. We conclude that significant information about isotope activities in the natural series is available with only a fraction of the work involved in conventional techniques. (author)

  16. Estudos organizacionais, (descolonialidade e estudos da dependência: as contribuições da Cepal

    Directory of Open Access Journals (Sweden)

    Sergio Wanderley

    Full Text Available O objetivo deste artigo é (revisitar o conceito de dependência como categoria de investigação da (e a partir da América Latina, por meio de uma perspectiva histórica crítica descolonial, a fim de ampliar o espaço de debates em estudos organizacionais e promover alternativas à ordem neoliberal. Este ensaio terá como foco os estudos da dependência realizados pela Comissão Econômica para a América Latina e o Caribe (Cepal durante a década de 1950 e o início dos anos 1960. A perspectiva descolonial é um constructo teórico de autores latino-americanos que se consideram herdeiros da longa tradição do pensamento social crítico da região, na qual a teoria da dependência está inserida. As propostas dos autores da dependência confrontaram as principais teorias ortodoxas do Norte produzidas à época. A partir do conceito de centro-periferia, da denúncia de assimetrias nas relações entre essas regiões, do reconhecimento da interdependência entre desenvolvimento e subdesenvolvimento, o conceito de dependência foi sendo (reelaborado nas décadas de 1950 e 1960 por diversos autores latino-americanos como uma categoria de investigação da realidade da (e a partir da região. Essas investigações tinham por objetivo não somente elaborar constructos teóricos, mas, também, transformar a realidade por meio da criação de diversas organizações e instituições que deveriam servir ao propósito de superar o subdesenvolvimento. A denúncia da historicidade da situação de subdesenvolvimento desnudou o caráter de neutralidade do economicismo das teorias produzidas no Norte e promoveu um encontro teórico entre economia e política que muito tem a contribuir com a área dos estudos organizacionais.

  17. Some analytical aspects of the Moessbauer spectrometry

    International Nuclear Information System (INIS)

    Meisel, W.

    1975-01-01

    Analytical applications of Moessbauer spectrometry are reviewed. Various methods of analysis (qualitative, semiquantitative and quantitative) using the Moessbauer effect are dealt with. Sensitivity and accuracy of Moessbauer spectrometry in analytical applications are discussed. (Z.S.)

  18. Laser ionization mass spectrometry in inorganic trace analysis

    International Nuclear Information System (INIS)

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

    1992-01-01

    Among the different spectrometric techniques for trace analysis Laser Ionization Mass Spectrometry (LIMS) is well established as a trace analytical method. With the LIMS technique the sample material is evaporated and ionized by means of a focused pulsed laser in a laser microplasma, which is formed in the spot area of the irradiated sample. All chemical elements in the sample materials are evaporated and ionized in the laser plasma. The ions formed are separated according to their mass and energy by a time-of-flight, quadrupole or double focusing mass spectrometer. In this review the characteristics and analytical features, some recent developments and applications of laser ionization mass spectrometry in inorganic trace analysis are described. (orig.)

  19. Técnica de separação da membrana de Descemet para transplante de células endoteliais da córnea: estudo experimental em coelhos Technique for separating Descemet membrane for corneal endothelial cells transplantation: experimental study in rabbits

    Directory of Open Access Journals (Sweden)

    Daniel Wasilewski

    2010-02-01

    Full Text Available OBJETIVO: Avaliar a porcentagem de dano endotelial induzido por uma técnica cirúrgica para a separação da membrana de Descemet contendo endotélio sadio, analisar a viabilidade e eficácia desta técnica, e avaliar a porcentagem de dano endotelial causado pela inversão da córnea em câmara anterior artificial. MÉTODOS: As córneas de três grupos de 12 coelhos da linhagem Nova Zelândia foram avaliadas. O grupo 1 foi usado como controle; portanto, as córneas foram analisadas após coletadas e trepanadas. O grupo 2 foi analisado após a inversão da córnea (endotélio para cima na posição convexa, montada em câmara anterior artificial, para o cálculo da porcentagem do dano endotelial induzido por esta inversão. O grupo 3 foi avaliado após a separação entre a membrana de Descemet e o estroma com o uso de substância viscoelástica em córneas invertidas e montadas em câmara anterior artificial. O dano endotelial foi avaliado por meio de fotografias digitais tiradas no microscópio após impregnar o endotélio com vermelho de alizarina. Amostras do grupo 3 foram processadas para avaliação histopatológica. RESULTADOS: O grupo 3 (separação viscoelástica apresentou um índice de lesão celular endotelial de 10,06%, o grupo 2 apresentou um índice de 3,58% e o grupo controle um índice de 0,18% de lesão celular endotelial (pPURPOSE: To evaluate the percentage of endothelial cell damage induced during a surgical technique of Descemet's membrane separation containing healthy endothelium, analyze the viability and efficacy of this technique, and evaluate the percentage of endothelial cell damage caused by inversion of the cornea on an artificial anterior chamber. METHODS: The corneas from three groups of 12 New Zealand rabbits were evaluated. The Group one was used as the control, so the corneas were analyzed after collected and trephinated. The Group two was analyzed after inversion of the cornea (endothelial side up at a convex

  20. Structural level characterization of base oils using advanced analytical techniques

    KAUST Repository

    Hourani, Nadim; Muller, Hendrik; Adam, Frederick M.; Panda, Saroj K.; Witt, Matthias; Al-Hajji, Adnan A.; Sarathy, Mani

    2015-01-01

    cyclotron resonance mass spectrometry (FT-ICR MS) equipped with atmospheric pressure chemical ionization (APCI) and atmospheric pressure photoionization (APPI) sources. First, the capabilities and limitations of each analytical technique were evaluated

  1. Estudo da função simpático-adrenal em crianças submetidas a cirurgia cardíaca com hipotermia de superfície, perfusão limitada e parada circulatória Simpathoadrenal function during cardiac surgery in infants using the technique of surface cooling, limited cardiopulmonary bypass and circulatory arrest

    Directory of Open Access Journals (Sweden)

    Richard K Firmin

    1988-04-01

    Full Text Available Os níveis de catecolamina plasmática foram medidos em 20 crianças (idade média de 6,00 ± 5,86 meses; peso médio 5,3 ± 1,82 kg, durante a correção de defeitos cardíacos congênitos, usando-se a hipotermia de superfície (26ºC, perfusão cardiopulmonar limitada e parada circulatória (15ºC. Adrenalina e noradrenalina plasmática foram dosadas em amostras sangüíneas arteriais seriadas, usando-se a cromatografia. A hipotermia de superfície produziu um significante aumento de ambas as catecolaminas. Durante o resfriamento central, os níveis caíram devido à hemodiluição. Após o período de parada circulatória (23/64 minutos, média de 41,3, ocorreu um aumento das catecolaminas plasmáticas, que persistiu durante o reaquecimento. Após o reaquecimento, as catecolaminas plasmáticas permaneceram elevadas até o final do ato cirúrgico. Nossos resultados mostram que a técnica de hipotermia de superfície, perfusão cardiopulmonar limitada e parada circulatória, sob as nossas condições de anestesia, produziu significante aumento da concentração de adrenalina e noradrenalina plasmática, porém o significado biológico é, ainda, inseguro.Plasma catecholamine levels were measured in 20 infants (mean age 6.0 ± 5.86 months; mean weigh 5.3 ± 1.82 Kg, undergoing correction of congenital heart defects using surface cooling (26ºC, limited cardiopulmonary bypass and circulatory arrest (15ºC. Plasma adrenaline and noradrenaline were assayed in serial arterial blood samples using cromatography and electrochemical techniques. Surface cooling produced a significant rise in adrenaline and noradrenaline: the levels of both catecholamines fell, however, during core-cooling on cardiopulmonary bypass. Following the period of circulatory arrest (23/64 min, mean 41.3 min, there was a further increase in plasma catecholamines, which persisted during rewarming. Following rewarming, plasma catecholamines remained elevated untill the end of the

  2. X-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    Vries, J.L. de.

    1976-01-01

    The seventh edition of Philips' Review of Literature on x-ray fluorescence spectrometry starts with a list of conference proceedings on the subject, organised by the Philips organisation at regular intervals in various European countries. It is followed by a list of bulletins. The bibliography is subdivided according to spectra, equipment, applications and absorption analysis

  3. Mass spectrometry in epigenetic research

    DEFF Research Database (Denmark)

    Beck, Hans Christian

    2010-01-01

    cancers has gained tremendous interest in recent years, and many of these inhibitors are currently undergoing clinical trials. Despite intense research, however, the exact molecular mechanisms of action of these molecules remain, to a wide extent, unclear. The recent application of mass spectrometry...

  4. X-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    Ray, N.B.

    1977-01-01

    The principle, instrument and procedure of X-ray fluorescence spectrometry are described. It is a rapid, simple and sensitive method for the trace analysis of elements from sodium to uranium in powder, liquid or metal samples. (M.G.B.)

  5. Mass spectrometry of large molecules

    International Nuclear Information System (INIS)

    Facchetti, S.

    1985-01-01

    The lectures in this volume were given at a course on mass spectrometry of large molecules, organized within the framework of the Training and Education programme of the Joint Research Centre of the European Communities. Although first presented in 1983, most of the lectures have since been updated by their authors. (orig.)

  6. Mass spectrometry with particle accelerator

    International Nuclear Information System (INIS)

    Anon.

    1983-01-01

    The heavy ion accelerator use is renewing the ultrasensitive mass spectrometry in extending the detection limits. These new devices allow the measurement of rare isotope ratio, as 10 Be, 14 C, 26 Al, 36 Cl or 41 Ca, from the earth natural reservoirs [fr

  7. Eleventh ISMAS workshop on mass spectrometry

    International Nuclear Information System (INIS)

    Aggarwal, S.K.; Jaison, P.G.

    2004-10-01

    This volume deals with the latest developments in this field, exposing the innumerable applications of mass spectrometry. The topics covered include basic fundamentals of mass spectrometry, qualitative and quantitative aspects and data interpretation, maintenance of mass spectrometers, selection of a mass spectrometer, its applications in various branches of science as well as recent advances in mass spectrometry. Emphasis is also laid on the practical aspects of mass spectrometry. Papers relevant to INIS are indexed separately

  8. Doping control analysis of anabolic steroids in equine urine by gas chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Wong, April S Y; Leung, Gary N W; Leung, David K K; Wan, Terence S M

    2017-09-01

    Anabolic steroids are banned substances in equine sports. Gas chromatography-mass spectrometry (GC-MS) has been the traditional technique for doping control analysis of anabolic steroids in biological samples. Although liquid chromatography-mass spectrometry (LC/MS) has become an important technique in doping control, the detection of saturated hydroxysteroids by LC-MS remains a problem due to their low ionization efficiency under electrospray. The recent development in fast-scanning gas-chromatography-triple-quadrupole mass spectrometry (GC-MS/MS) has provided a better alternative with a significant reduction in chemical noise by means of selective reaction monitoring. Herein, we present a sensitive and selective method for the screening of over 50 anabolic steroids in equine urine using gas chromatography-tandem mass spectrometry (GC-MS/MS). Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  9. Aplicação de técnicas eletroquímicas no estudo da dissolução oxidativa da covelita (CuS por Thiobacillus ferrooxidans Electrochemical techniques applied to study the oxidative dissolution of the covellite: CuS by Thiobacillus ferrooxidans

    Directory of Open Access Journals (Sweden)

    Christiane Medina Teixeira

    2002-02-01

    Full Text Available Among the copper sulphides, chalcopyrite (CuFeS2, covellite (CuS and chalcocite (Cu2S are the most important source of minerals for copper mining industry. The acknowledge of behaviour of these sulphides related with bacterial leaching process are essential for optimization procedures. Despite of its importance, covellite has not deserved much interest of researchers regarding this matter. In this work it was studied the oxidation of covellite by the chemolithotrophic bacterium Thiobacillus ferrooxidans by using electrochemical techniques, such as open circuit potentials with the time and cyclic voltammetry. The experiments were carried out in acid medium (pH 1.8, containing or not Fe2+ as additional energy source, and in different periods of incubation; chemical controls were run in parallel. The results showed that a sulphur layer is formed spontaneously due the acid attack, covering the sulphide in the initial phase of incubation, blocking the sulphide oxidation. However, the bacterium was capable to oxidize this sulphur layer. In the presence of Fe2+ as supplemental energy source, the corrosion process was facilitated, because ocurred an indirect oxidation of covellite by Fe3+, which was produced by T. ferrooxidans oxidation of the Fe2+ added in the medium.

  10. Proteômica na sepse: estudo piloto Proteomics in sepsis: a pilot study

    Directory of Open Access Journals (Sweden)

    Rita Azevedo de Paiva

    2010-12-01

    processes are expressed by proteins. This study was aimed to advance the insight into the molecular foundations of sepsis. It employed proteomic techniques to identify and analyze differential serum protein expressions taken from a patient throughout the stages of sepsis (sepsis, severe sepsis and septic shock. Serum samples were collected at each stage of sepsis and submitted to one-dimensional electrophoresis, on gradient strips of immobilized pH, followed by two-dimensional 12.5% polyacrylamide gel electrophoresis. The gels obtained were stained, scanned and analyzed by the ImageMasterPlatinum program. Proteins that were differentially expressed in the gels were excised, digested with trypsin and identified through mass spectrometry. Fourteen differentially expressed proteins were identified throughout the stages of sepsis, as well as a protein that was not expressed in all stages, suggesting the potential existence of a biomarker. The differentially expressed proteins identified were: serum amyloid A, apolipoprotein A-1 (2 isoforms, zinc finger protein 222, human albumin, PRO 2619, immunoglobulin kappa light chain VLJ region, monoclonal immunoglobulin M cold agglutinin, 7 proteinase inhibitors - alpha-1 antitrypsin. The findings of this pilot study demonstrate the involvement of the complement and coagulation pathways, of the lipid metabolism and of genetic information in sepsis. The vast majority of proteins identified are involved in the immune system and the proteinase inhibitor proteins are predominant.

  11. Mass spectrometry with ionization induced by 252Cf fission fragments

    International Nuclear Information System (INIS)

    Sysoev, A.A.; Artaev, V.B.

    1991-01-01

    The review deals with mass-spectrometry with ionization induced by 252 Cf fission fragments. Equipment and technique of the analysis, analytic possibilities of the method are considered. The method permits to determine molecular masses of large nonvolatile biological molecules. The method is practically nondestructive, it possesses a high resolution over the depth and surface, which permits to use it for the analysis of surface of semiconductors, dielectrics, catalysts, for the study of formation kinetics of complex unstable molecules on the surface

  12. Mass spectrometry of submicrogram quantities of lead and cadmium

    International Nuclear Information System (INIS)

    Moraes, Noemia M.P. de; Kakazu, M.H.; Iyer, S.S.

    1980-01-01

    Isotope analyses of submicrogram quantities of lead and cadmium are carried out by single filament solid source mass spectrometry. Thermionic emission of Pb and Cd is enhanced using silica gel as an emitter. Details of the chemical and mass spectrometric techniques are described. The low blank levels are maintained by extra purification of the reagents. The applications of isotope ratios of Pb and Cd in environmental sciences and geochemistry are discussed. (Author) [pt

  13. Gamma spectrometry analysis of fertilizers used in Costa Rica

    International Nuclear Information System (INIS)

    Loria, L.G.; Jimenez, R.; Badilla, M.

    2002-01-01

    Using the low level gamma spectrometry technique, the specific activity of natural and artificial isotopes present in national consumption fertilizers, supplied by local dealers, was quantified. The most outstanding isotope found in some of the fertilizers is U 235 , with an specific activity higher than the expected in this kind of product, which might mean that this isotope comes from imported raw material. (Author) [es

  14. Unidade de Estudos de Mastites em Pequenos Ruminantes - estudos em ovinos de regime extensivo

    OpenAIRE

    Queiroga, Cristina; Potes, Maria Eduarda; Duarte, Elsa Maria; Marinho, Artur; Bettencourt, Carlos Manuel; Matos, Claudino; Belo, Carlos Carmona; Ribeiro, José Manuel; Vilela, Cristina Lobo

    2007-01-01

    A “Unidade de Estudo de Mastites em Pequenos Ruminantes”, formalmente constituída no âmbito do Programa Nacional de Re-equipamento Científico, da Fundação para a Ciência e a Tecnologia, vem dar corpo ao trabalho de colaboração de diversas equipas de investigação que se têm debruçado sobre a problemática das infecções intramamárias em pequenos ruminantes, nos seus aspectos de saúde animal, saúde pública veterinária e qualidade e segurança alimentar. Tem como principal objectivo criar condições...

  15. Secondary Ion Mass Spectrometry SIMS XI

    Science.gov (United States)

    Gillen, G.; Lareau, R.; Bennett, J.; Stevie, F.

    2003-05-01

    This volume contains 252 contributions presented as plenary, invited and contributed poster and oral presentations at the 11th International Conference on Secondary Ion Mass Spectrometry (SIMS XI) held at the Hilton Hotel, Walt Disney World Village, Orlando, Florida, 7 12 September, 1997. The book covers a diverse range of research, reflecting the rapid growth in advanced semiconductor characterization, ultra shallow depth profiling, TOF-SIMS and the new areas in which SIMS techniques are being used, for example in biological sciences and organic surface characterization. Papers are presented under the following categories: Isotopic SIMS Biological SIMS Semiconductor Characterization Techniques and Applications Ultra Shallow Depth Profiling Depth Profiling Fundamental/Modelling and Diffusion Sputter-Induced Topography Fundamentals of Molecular Desorption Organic Materials Practical TOF-SIMS Polyatomic Primary Ions Materials/Surface Analysis Postionization Instrumentation Geological SIMS Imaging Fundamentals of Sputtering Ion Formation and Cluster Formation Quantitative Analysis Environmental/Particle Characterization Related Techniques These proceedings provide an invaluable source of reference for both newcomers to the field and experienced SIMS users.

  16. Mass spectrometry in structural biology and biophysics architecture, dynamics, and interaction of biomolecules

    CERN Document Server

    Kaltashov, Igor A; Desiderio, Dominic M; Nibbering, Nico M

    2012-01-01

    The definitive guide to mass spectrometry techniques in biology and biophysics The use of mass spectrometry (MS) to study the architecture and dynamics of proteins is increasingly common within the biophysical community, and Mass Spectrometry in Structural Biology and Biophysics: Architecture, Dynamics, and Interaction of Biomolecules, Second Edition provides readers with detailed, systematic coverage of the current state of the art. Offering an unrivalled overview of modern MS-based armamentarium that can be used to solve the most challenging problems in biophysics, structural biol

  17. Quantitative radiological characterization of waste. Integration of gamma spectrometry and passive/active neutron assay

    Energy Technology Data Exchange (ETDEWEB)

    Simone, Gianluca; Mauro, Egidio; Gagliardi, Filippo; Gorello, Edoardo [Nucleco S.p.A., Rome (Italy)

    2016-06-15

    The radiological characterization of drums through Non-Destructive Assay (NDA) techniques commonly relies on gamma spectrometry. This paper introduces the procedure developed in Nucleco for the NDA radiological characterization of drums when the presence of Special Nuclear Material (SNM) is expected/observed. The procedure is based on the integration of a gamma spectrometry in SGS mode (Segmented Gamma Scanner) and a passive/active neutron assay. The application of this procedure is discussed on a real case of drums. The extension of the integration procedure to other gamma spectrometry systems is also discussed.

  18. Comparison of 15N analysis by optical emission spectrometry and mass spectrometry for clinical studies during total parenteral nutrition

    International Nuclear Information System (INIS)

    Ragon, A.; Reynier, J.P.; Guiraud, G.

    1985-01-01

    During total and stable parenteral nutrition, a branched chain amino acid enriched solution containing [ 15 N]leucine was infused into a patient to determine the fate of the nitrogen administered through this formulation. Measurements of 15 N isotopic enrichments were performed on the same biological samples (urinary urea, total plasma proteins and albumin) by optical emission spectrometry (OES) and mass spectrometry (MS) to determine if OES with its specific advantages (cost, handling maintenance) constituted even with low enrichments a useful alternative technique to MS considered as the reference method. The results show that OES constituted a very useful analytical technique to obtain reliable information in clinical metabolic studies when low 15 N enrichments must be determined. (Auth.)

  19. Contribuição ao estudo da microinfiltração in vitro de lesões cervicais não cariosas restauradas com diferentes materiais adesivos e técnicas In vitro evaluation of microleakage of noncarious cervical lesions restored with different adhesive materials and techniques

    Directory of Open Access Journals (Sweden)

    Adriana Bona MATOS

    1997-01-01

    Full Text Available A restauração de lesões cervicais não cariosas é um procedimento comum na clínica diária, havendo uma alta incidência de casos de perda da restauração, descoloração marginal e recidiva de cárie. A etiologia desse tipo de lesão é considerada multifatorial. Neste trabalho, avaliou-se a microinfiltração diante das seguintes variáveis: tipo de material utilizado (dois adesivos de quarta geração utilizados em conjunto com duas resinas compostas de tipos diferentes, ©microfillª e híbrida, dois métodos de polimerização dos sistemas adesivos (foto e dual e duas técnicas restauradoras (incremental e do incremento único. Na metodologia deste trabalho, utilizaram-se ciclagem térmica e mecânica, técnica de infiltração com nitrato de prata, cortes seriados e leitura dos resultados através de escala de escores. A microinfiltração foi menor quando se utilizou uma resina composta híbrida comparada à resina ©microfillª. Ao se utilizar o método de polimerização dual do sistema adesivo, a microinfiltração foi menor do que com o método somente fotopolimerizável. A técnica restauradora não exerceu influência sobre o padrão de microinfiltração encontrado nas restaurações de lesões cervicais não cariosasRestoration of noncarious cervical lesions is a usual clinical procedure, and there is a high incidence of restoration loss, marginal discoloration, and recurrent caries. All the factors that play an important role in this process have to be considered when studying this kind of lesion of complex multifactorial etiology. Microleakage was evaluated related to the type of material used (two fourth generation bonding systems used with two types of composite resins: hybrid and microfill, two polymerization methods for bonding systems (photo and dual cure and two restorative techniques (incremental and bulk. This study used thermal and mechanical cycling procedures, infiltration tests with silver nitrate solution

  20. Uma ferramenta para planejamento de estudos para concursos

    Directory of Open Access Journals (Sweden)

    Leonardo Pimentel

    2015-11-01

    Full Text Available De acordo com a constituição brasileira, a única forma de se tornar um empregado do governo é passar em um concurso público. O exame de conhecimento do cargo é um dos componentes mais importantes de um concurso. Estudar para esse exame é uma tarefa que requer planejamento. Um meio de obter um bom planejamento é construir uma grade de horários que relacione as matérias a serem estudadas com os respectivos horários disponíveis para o estudo. Esse tipo de problema se assemelha bastante à gerência de projetos, em que se procura estabelecer a distribuição das atividades ao longo do tempo disponível. Assim, torna-se interessante explorar a dinâmica de estudos para concursos como um projeto. O presente trabalho apresenta a ferramenta de apoio ao estudos - Passe-me, baseada no ciclo PDCA (do inglês, Plan-Do-Check-Act. Por se tratar de uma ferramenta web, o tempo de resposta para produzir uma grade de estudos é fundamental. A ferramenta faz uso de algoritmo genético para calcular a grade de horários priorizando a velocidade de resposta. A ferramenta foi avaliada em diferentes cenários de uso e obteve desempenho satisfatório durante a produção da grade de estudos.

  1. Electronic sputtering of large organic molecules and its application in bio molecular mass spectrometry

    International Nuclear Information System (INIS)

    Sundqvist, B.U.R.

    1992-01-01

    This is a review of research which has its origin in the discovery of Plasma Desorption Mass Spectrometry (PDMS). Two main fields of research have developed, namely fundamental studies of the ejection process at fast ion impact and studies of applications of the new mass spectrometric technique. In this review the emphasis will be on the process of electronic sputtering of organic solids but also applications of this process in bio molecular mass spectrometry will be discussed. (author)

  2. Non-conventional measurement techniques for the determination of some long-lived radionuclides produced in nuclear fuel

    International Nuclear Information System (INIS)

    Rosenberg, R.J.

    1992-04-01

    The results of a literature survey on non-radiometric analytical techniques for the determination of long-lived radionuclides are described. The methods which have been considered are accelerator mass spectrometry, inductively coupled plasma mass spectrometry, thermal ionization mass spectrometry, resonance ionization spectrometry, resonance ionization mass spectrometry and neutron activation analysis. Neutron activation analysis has been commonly used for the determination of 129 I and 237 Np in environmental samples. Inductively coupled mass spectrometry seems likely to become the method of choice for the determination of 99 Tc, 237 Np and Pu-isotopes. The methods are discussed and the chemical separation methods described. (orig.)

  3. Positioning of the femoral tunnel for arthroscopic reconstruction of the anterior cruciate ligament: comparative study of 2 techniques Posicionamento do túnel femoral na reconstrução artroscópica do LCA: estudo comparativo de duas técnicas

    Directory of Open Access Journals (Sweden)

    Roberto Freire da Mota Albuquerque

    2007-01-01

    Full Text Available OBJECTIVE: To compare the accuracy of positioning of the femoral tunnel in reconstructing the anterior cruciate ligament by means of 2 techniques: tibial tunnel and anteromedial portal. METHOD: Femoral tunnels were drilled in 20 knees from human cadavers by means of arthroscopy. Group I had the femoral tunnel drilled via a trans-tibial tunnel, and Group II via the anteromedial portal. Four variables were measured: A posterior wall thickness; B tunnel positioning at the notch; C tunnel inclination in relation to the femoral axis; and D distance between the wire guide exit and the lateral epicondyle. RESULTS: As above, respectively, A 2.23 mm for group I and 2.36 mm for group II (P =.54; B 25.5° for group I and 30.0° for group II (P =.23; C 23.9° for group I and 32.0° for group II (P =.02; D 7.8 cm for group I and 3.9 cm for group II (P OBJETIVO: Comparar a acurácia do posicionamento do túnel femoral na reconstrução do ligamento cruzado anterior através de duas vias: túnel tibial e portal ântero - medial. MÉTODO: Foram perfurados túneis femorais em vinte joelhos de cadáveres humanos por via artroscópica. Grupo I: túnel femoral por acesso trans túnel tibial. Grupo II: via portal ântero-medial. Quatro variáveis foram estudadas: A espessura da parede posterior; B posicionamento do túnel no intercôndilo; C angulação do túnel em relação ao eixo do fêmur; D distância entre a saída do fio guia e o epicôndilo lateral. RESULTADO: A grupo I: 2,23 mm, grupo II: 2,36 mm (p=0,543; B grupo I: 25,5º, grupo II: 30º (p=0,226; C grupo I: 23,9º, grupo II: 32º (p= 0,014; D grupo I: 7,8 cm, grupo II 3,9 cm (p<0,001. CONCLUSÃO: As duas técnicas obteveram o posicionamento desejado da entrada do túnel femoral e espessura adequada da cortical posterior. A perfuração via portal ântero-medial pode propiciar maior proteção contra rotura da parede posterior.

  4. Studies on survival, biological activities and behavior of Biomphalaria glabrata, the host snail of Schistosomiasis, submitted to increased hydrostatic pressure: a technique Estudos sobre a sobrevivência, atividades biológicas e comportamento de Biomphalaria glabrata, hospedeiro intermediário da esquistossomose, submetido a aumento da pressão hidrostática: uma técnica

    Directory of Open Access Journals (Sweden)

    P. Jurberg

    1988-03-01

    Full Text Available To study changes in survival, in biological activities and behavior of planorbids submitted to increased hydrostatic pressure, we developed a technique using two transparent chambers and a hydraulic piston. The apparatus permitted renewal of the liquid medium without substantial variations in pressure, thus eliminating excretion products and maintaining the desired O2 level and thereby permitting us to evaluate the effects of pressure independently of the occurrence of anoxia. Pressure was maintained without any contact of the liquid medium with compressed air, a situation which reproduced with relative fidelity what occurs in nature and assured the presence of the same amounts of gases in the two observation chambers (Control and Experimental. Biomphalaria glabrata was found to be able to survive at least 48 hours when submitted to 49.02 x 10**4 Pa (equivalent to a water depth of 48.8 m, continuing to day egg masses and showing few behavioral changes when compared with the control group.Para estudar mudanças na sobrevivência, atividades biológicas e comportamento de planorbídeos submetidos a aumento de pressão hidrostática, desenvolvemos uma técnica que utiliza duas câmaras transparentes e um pistão hidráulico. O aparelho permitiu a renovação do meio líquido sem variações substanciais na pressão, eliminando assim os produtos de excreção e mantendo o nível de O2 disseolvido desejado, e desse modo permitido-nos avaliar o efeito da pressão independente da ocorrência de anoxia. A pressão foi mantida sem nenhum contato do meio líquido com o ar comprimido, situação que produziu com relativa fidelildade o que ocorre na natureza, e assegurou a presença da mesma quantidade de gases nas duas câmaras de observação. Biomphalaria glabrata foi capaz de sobreviver pelo menos 48 horas quando submetida a 49,02 x 10 Pa (equivalente a 48 m de profundidade continuando a pôr massas ovíferas, e mostrando poucas modifica

  5. Chromatography and mass spectrometry of chemical warfare agents, toxins and related compounds: state of the art and future prospects

    NARCIS (Netherlands)

    Kientz, C.E.

    1998-01-01

    Methods for the identification of chemical warfare agents, toxins, bioregulators and related products are frequently reported in literature. These methods are often based on instrumental analysis using chromatography (gas and liquid) and mass spectrometry. Here, these instrumental techniques are

  6. ISMAS international discussion meet on elemental mass spectrometry in health and environmental sciences

    International Nuclear Information System (INIS)

    Aggarwal, S.K.; Jaison, P.G.; Telmore, V.M.

    2011-04-01

    Mass spectrometry is an indispensable analytical tool associated with almost all branches of science including biology, chemistry, earth sciences, nuclear science, physics, etc. The technique holds tremendous potential owing to its high sensitivity, selectivity and its ability to measure small changes in the isotopic abundances of different elements. Innovations in mass spectrometry instrumentation are further widening the scope by making it possible to handle very large bio-molecules and polymers. New techniques for mass analysis, novel designs for ionization and developments in electronic accessories have contributed to elevate mass spectrometry to a position of prime importance in research. Development in mass spectrometry has revolutionized the study of micro-nutrient metabolism, of biologically active compounds and for drug discovery in pharmaceutical research. Elemental mass spectrometry is making major contributions to food toxicology, food forensics, and study of metabolism of nutrient minerals including Fe, Zn, Ca, Cu and Se. The area of speciation analysis using hyphenated techniques as well as electro-spray ionization have undergone a phenomenal evolution and development in the recent past. Impressive progress in mass spectrometry towards lower detection limits, higher resolution and molecule-specific detection at trace levels in complex matrices allows new frontiers to be crossed. Papers relevant to INIS are indexed separately

  7. Ninth ISMAS workshop on mass spectrometry

    International Nuclear Information System (INIS)

    Aggarwal, S.K.

    2000-12-01

    Mass spectrometry has wide-ranging applications in such diverse areas as nuclear industry, agriculture, drugs, environment, petroleum and lentils. There is an urgent need to absorb and assimilate state-of-the-art technological developments in the field. Emerging trends in atomic mass spectrometry, advances in organic mass spectrometry, qualitative and quantitative analyses by mass spectrometry and mass spectrometry in oceanography are some of the areas that need to be expeditiously examined and are covered in this volume. Papers relevant to INIS are indexed separately

  8. Alpha spectrometry and the secondary ion mass spectrometry of thorium

    International Nuclear Information System (INIS)

    Strisovska, J.; Kuruc, J.; Galanda, D.; Matel, L.; Aranyosiova, M.; Velic, D.

    2009-01-01

    The main objective of this master thesis was preparation of samples with thorium content on the steel discs by electrodeposition for determination of natural thorium isotope by alpha spectrometry and the secondary ion mass spectrometry and finding out their possible linear correlation between these methods. The samples with electrolytically excluded isotope of 232 Th were prepared by electrodeposition from solution Th(NO 3 ) 4 ·12 H2 O on steel discs in electrodeposition cell with use of solutions Na 2 SO 4 , NaHSO 4 , KOH and (NH 4 ) 2 (C 2 O 4 ) by electric current 0.75 A. Discs were measured by alpha spectrometer. Activity was calculated from the registered impulses for 232 Th and surface's weight. After alpha spectrometry measurements discs were analyzed by TOF-SIMS IV which is installed in the International Laser Centre in Bratislava. Intensities of isotope of 232 Th and ions of ThO + , ThOH + , ThO 2 H + , Th 2 O 4 H + , ThO 2 - , ThO 3 H - , ThH 3 O 3 - and ThN 2 O 5 H - were identified. The linear correlation is between surface's weights of Th and intensities of ions of Th + from SIMS, however the correlation coefficient has relatively low value. We found out with SIMS method that oxidized and hydride forms of thorium are significantly represented in samples with electroplated thorium. (authors)

  9. Use of the helium-3 proportional counter for neutron spectrometry

    International Nuclear Information System (INIS)

    Vialettes, H.; Le Thanh, P.

    1967-01-01

    Up to now, two methods have been mainly used for neutron spectrometry near nuclear installations: - photographic emulsion spectrometry - the so-called, 'multisphere' technique spectrometry. The first method, which is fairly difficult to apply, has a threshold energy of about 500 keV; this is a big disadvantage for an apparatus which has to be used for spectrometry around nuclear installations where the neutron radiation is very much degraded energetically. The second method does not suffer from this disadvantage but the results which it yields are only approximate. In order to extend the energy range of the neutron spectra studied with sufficient accuracy the use of a helium-3 proportional counter has been considered. This report presents the principles of operation of the helium-3 spectrometer, and the calculation methods which make it possible to take into account the two main effects tending to deform the spectra obtained: - energy absorption by the walls of the counter, - energy loss of the incident neutrons due to elastic collisions with helium-3 nuclei. As an example of the application, the shape of the neutron spectrum emitted by a polonium-lithium source is given; the results obtained are in excellent agreement with theoretical predictions. (authors) [fr

  10. Direct Analysis of Samples of Various Origin and Composition Using Specific Types of Mass Spectrometry.

    Science.gov (United States)

    Byliński, Hubert; Gębicki, Jacek; Dymerski, Tomasz; Namieśnik, Jacek

    2017-07-04

    One of the major sources of error that occur during chemical analysis utilizing the more conventional and established analytical techniques is the possibility of losing part of the analytes during the sample preparation stage. Unfortunately, this sample preparation stage is required to improve analytical sensitivity and precision. Direct techniques have helped to shorten or even bypass the sample preparation stage; and in this review, we comment of some of the new direct techniques that are mass-spectrometry based. The study presents information about the measurement techniques using mass spectrometry, which allow direct sample analysis, without sample preparation or limiting some pre-concentration steps. MALDI - MS, PTR - MS, SIFT - MS, DESI - MS techniques are discussed. These solutions have numerous applications in different fields of human activity due to their interesting properties. The advantages and disadvantages of these techniques are presented. The trends in development of direct analysis using the aforementioned techniques are also presented.

  11. Applications of ambient mass spectrometry in high-throughput screening.

    Science.gov (United States)

    Li, Li-Ping; Feng, Bao-Sheng; Yang, Jian-Wang; Chang, Cui-Lan; Bai, Yu; Liu, Hu-Wei

    2013-06-07

    The development of rapid screening and identification techniques is of great importance for drug discovery, doping control, forensic identification, food safety and quality control. Ambient mass spectrometry (AMS) allows rapid and direct analysis of various samples in open air with little sample preparation. Recently, its applications in high-throughput screening have been in rapid progress. During the past decade, various ambient ionization techniques have been developed and applied in high-throughput screening. This review discusses typical applications of AMS, including DESI (desorption electrospray ionization), DART (direct analysis in real time), EESI (extractive electrospray ionization), etc., in high-throughput screening (HTS).

  12. Electrospray mass spectrometry for actinides and lanthanide speciation

    International Nuclear Information System (INIS)

    Moulin, C.; Amekraz, B.; Colette, S.; Doizi, D.; Jacopin, C.; Lamouroux, C.; Plancque, G.

    2006-01-01

    Electrospray mass spectrometry (ES-MS) is a new speciation technique that has the great interest to be able to probe the element, the ligand and the complex in order to reach the speciation. This paper will focus on the use of ES-MS for the speciation of actinides/lanthanides on several systems of interest in various fields such as the interaction between DTPA (decorporant) and europium, HEBP and uranium, BTP (new extracting agent) and lanthanides with comparison with known chemistry as well as whenever possible with other speciation techniques

  13. Application of accelerator mass spectrometry in aluminum metabolism studies

    International Nuclear Information System (INIS)

    Meirav, O.; Vetterli, D.; Johnson, R.R.; Sutton, R.A.L.; Walker, V.R.; Halabe, A.; Fink, D.; Middleton, R.; Klein, J.

    1990-06-01

    The recent recognition that aluminum causes toxicity in uremic patients and may be associated with Alzheimer's disease has stimulated many studies of its biochemical effects. However, such studies were hampered by the lack of a suitable tracer. In a novel experiment, we have applied the new technique of accelerator mass spectrometry to investigate aluminum kinetics in rats, using as a marker the long-lived isotope 26 Al. We present the first aluminum kinetic model for a biological system. The results clearly demonstrate the advantage this technique holds for isotope tracer studies in animals as well as humans. (Author) (24 refs., 3 figs.)

  14. Application of accelerator mass spectrometry in aluminum metabolism studies

    Energy Technology Data Exchange (ETDEWEB)

    Meirav, O; Vetterli, D; Johnson, R R [British Columbia Univ., Vancouver, BC (Canada). Dept. of Physics; Sutton, R A.L.; Walker, V R; Halabe, A [British Columbia U.iv., Vancouver, BC (Canada). Dept. of Medicine; Fink, D; Middleton, R; Klein, J [Pennsylvania Univ., Philadelphia, PA (United States). Dept. of Physics

    1990-06-01

    The recent recognition that aluminum causes toxicity in uremic patients and may be associated with Alzheimer`s disease has stimulated many studies of its biochemical effects. However, such studies were hampered by the lack of a suitable tracer. In a novel experiment, we have applied the new technique of accelerator mass spectrometry to investigate aluminum kinetics in rats, using as a marker the long-lived isotope {sup 26}Al. We present the first aluminum kinetic model for a biological system. The results clearly demonstrate the advantage this technique holds for isotope tracer studies in animals as well as humans. (Author) (24 refs., 3 figs.).

  15. Abordagem Exploratória do Emprego das Técnicas de Análise de Regressão e Análise Conjunta em Estudos do Comportamento do ConsumidorExploratory Approach to the use of Techniques of Regression Analysis and Pooled Analysis in Studies of Consumer BehaviorEstudio Exploratorio sobre la Utilización de Técnicas de Análisis de Regresión y de Análisis Conjunto en los Estudios del Comportamiento del Consumidor

    Directory of Open Access Journals (Sweden)

    GOUVÊA, Maria Aparecida

    2010-09-01

    Full Text Available RESUMOEste artigo faz parte de um amplo estudo de avaliação da adequação no uso de técnicas estatísticas multivariadas em teses e dissertações de algumas instituições de ensino superior na área de marketing na temática do comportamento do consumidor entre 1997 e 2006. Neste artigo são focalizadas as técnicas de análise de regressão e análise conjunta, duas técnicas com grande potencial de uso em estudos de marketing. Foi objetivo desse trabalho a análise da adequação do emprego destas técnicas às necessidades dos problemas de pesquisa apresentados nas teses e dissertações e a aferição do nível de acerto no atendimento de suas premissas. De forma geral, os resultados sugerem a necessidade de um aumento do comprometimento dos pesquisadores na verificação de todos os preceitos teóricos de aplicação destas técnicas classificadas na categoria de investigação de dependência entre variáveis.ABSTRACTThis paper is part of a large study to assess the adequacy of the use of multivariate statistical techniques in theses and dissertations of some higher education institutions in the area of marketing with theme of consumer behavior from 1997 to 2006. The regression and conjoint analysis are focused on in this paper, two techniques with great potential of use in marketing studies. The objective of this study was to analyze whether the employment of these techniques suits the needs of the research problem presented in as well as to evaluate the level of success in meeting their premisses. Overall, the results suggest the need for more involvement of researchers in the verification of all the theoretical precepts of application of the techniques classified in the category of investigation of dependence among variables.RESUMENEste artículo forma parte de un amplio estudio que evalúa la adecuación del uso de técnicas estadísticas multivariantes en las tesis y disertaciones de algunas instituciones de educación superior

  16. Automatic gamma spectrometry analytical apparatus

    International Nuclear Information System (INIS)

    Lamargot, J.-P.; Wanin, Maurice.

    1980-01-01

    This invention falls within the area of quantitative or semi-quantitative analysis by gamma spectrometry and particularly refers to a device for bringing the samples into the counting position. The purpose of this invention is precisely to provide an automatic apparatus specifically adapted to the analysis of hard gamma radiations. To this effect, the invention relates to a gamma spectrometry analytical device comprising a lead containment, a detector of which the sensitive part is located inside the containment and additionally comprising a transfer system for bringing the analyzed samples in succession to a counting position inside the containment above the detector. A feed compartment enables the samples to be brought in turn one by one on to the transfer system through a duct connecting the compartment to the transfer system. Sequential systems for the coordinated forward feed of the samples in the compartment and the transfer system complete this device [fr

  17. Mass Spectrometry Instrumentation in Proteomics

    DEFF Research Database (Denmark)

    Sprenger, Richard Remko; Roepstorff, Peter

    2012-01-01

    Mass spectrometry has evolved into a crucial technology for the field of proteomics, enabling the comprehensive study of proteins in biological systems. Innovative developments have yielded flexible and versatile mass spectrometric tools, including quadrupole time-of-flight, linear ion trap......, Orbitrap and ion mobility instruments. Together they offer various and complementary capabilities in terms of ionization, sensitivity, speed, resolution, mass accuracy, dynamic range and methods of fragmentation. Mass spectrometers can acquire qualitative and quantitative information on a large scale...

  18. The history of radiation spectrometry

    International Nuclear Information System (INIS)

    Mori, Kunishiro

    2007-01-01

    Recently combination of charge sensitive amplifier, pulse shape amplifier and multi-channel PHA (MCA) is regarded as standard configuration of radiation spectrometry. PHA history shows various kinds of MCA devices before we have obtained original digital ADC technology based MCA in 1960s. Those MCAs include interesting ones such as photographic type, which still keep fresh ideas even today. Room temperature preamplifiers are classified to low, medium range, and large capacitance (over 10000pF) detectors keeping ultra low noise. (author)

  19. Dismantling techniques

    International Nuclear Information System (INIS)

    Wiese, E.

    1998-01-01

    Most of the dismantling techniques used in a Decontamination and Dismantlement (D and D) project are taken from conventional demolition practices. Some modifications to the techniques are made to limit exposure to the workers or to lessen the spread of contamination to the work area. When working on a D and D project, it is best to keep the dismantling techniques and tools as simple as possible. The workers will be more efficient and safer using techniques that are familiar to them. Prior experience with the technique or use of mock-ups is the best way to keep workers safe and to keep the project on schedule

  20. Dismantling techniques

    Energy Technology Data Exchange (ETDEWEB)

    Wiese, E.

    1998-03-13

    Most of the dismantling techniques used in a Decontamination and Dismantlement (D and D) project are taken from conventional demolition practices. Some modifications to the techniques are made to limit exposure to the workers or to lessen the spread of contamination to the work area. When working on a D and D project, it is best to keep the dismantling techniques and tools as simple as possible. The workers will be more efficient and safer using techniques that are familiar to them. Prior experience with the technique or use of mock-ups is the best way to keep workers safe and to keep the project on schedule.

  1. Instrumentation for mass spectrometry: 1997

    Energy Technology Data Exchange (ETDEWEB)

    McLuckey, S.A.

    1997-08-01

    All mass spectrometry experiments involve the manipulation of material, an interface with the mass spectrometer, ionization, ion manipulation/analysis, detection and data collection/reduction. Each of these elements involve instrumentation. The wide range of species now amenable to mass spectrometry and the diverse areas of physical science in which it plays a role have led to a seemingly unlimited array of instrumental combinations. However, only a limited number of mass analyzers, and their combinations, dominate. The dominant analyzers include time-of-flight, Fourier transform ion cyclotron resonance, the Paul trap, the mass filter, and the sector mass spectrometer. Why there are so few (or so many, depending upon one`s point of view) can be understood upon consideration of a set of mass analyzer figures of merit. These include mass resolution, mass accuracy, mass range, dynamic range, abundance sensitivity, precision, efficiency, speed, MS{sup n} capability, compatibility with the ionizer, cost, and size. The most appropriate form of mass spectrometry is determined by the priorities of the particular measurement placed on the various mass analyzer characteristics and the relative strengths of the analyzers in meeting the requirements. Each of the analyzer types has a unique set of figures of merit that makes it optimally suited for particular applications. This paper discusses these figures of merit, provides data illustrating recent developments for each analyzer type, and gives the figures of merit of each type of analyzer as they stand in 1997. 101 refs., 24 figs.

  2. Urban gamma spectrometry. Report 2

    Energy Technology Data Exchange (ETDEWEB)

    Aage, H.K. (Technical Univ. of Denmark, Kgs. Lyngby (Denmark)); Kuukankorpi, S.; Moring, M.; Smolander, P.; Toivonen, H. (Radiation and Nuclear Safety Authority, Helsinki (Finland))

    2009-06-15

    Urban gamma spectrometry has been given only minor attention with the focus being on rural gamma spectrometry. However, in recent years the Nordic emergency management authorities have turned focus towards border control and lost or stolen sources. Gamma spectra measured in urban areas are characterized by a wide variety of spectrum shapes and very fast changes in environmental background. In 2004 a Danish CGS (Carborne Gamma Spectrometry) survey took place in Copenhagen. It was found that gamma spectrometry in urban areas is far more complicated to interpret than had previously been thought and a new method 'Fitting with Spectral Components', FSC, based on NASVD, was tested with some success. In Finland, a database 'LINSSI' has been developed for spectral data management. In CGS search mode a 'peak hypothesis test' is applied to the measured spectra. This system was tested during the Helsinki 2005 Athletics World Championship and it provides fast and reliable automated alarms for intermediate and high level signals. In Sweden mobile detector systems are used for border controls and problems are encountered when making measurement in harbour, container areas. The methods for handling data and for interpretation of urban gamma spectrometry measurements were compared and tested on the same data sets from Copenhagen and Helsinki. Software tools were developed for converting data between the Finnish LINSSI database and the binary file formats used in Denmark and Sweden. The Processing methods used at DTU and STUK have different goals. The ASSS and FSC methods are designed to optimize the overall detection capability of the system, while sacrificing speed, usability and to a certain level robustness. These methods cannot always be used for real time analysis. The Peak Significance method is designed to give robust alarms in real time, while sacrificing some of the detection capability. Thus these methods are not interchangeable, but rather

  3. Urban gamma spectrometry. Report 2

    International Nuclear Information System (INIS)

    Aage, H.K.; Kuukankorpi, S.; Moring, M.; Smolander, P.; Toivonen, H.

    2009-06-01

    Urban gamma spectrometry has been given only minor attention with the focus being on rural gamma spectrometry. However, in recent years the Nordic emergency management authorities have turned focus towards border control and lost or stolen sources. Gamma spectra measured in urban areas are characterized by a wide variety of spectrum shapes and very fast changes in environmental background. In 2004 a Danish CGS (Carborne Gamma Spectrometry) survey took place in Copenhagen. It was found that gamma spectrometry in urban areas is far more complicated to interpret than had previously been thought and a new method 'Fitting with Spectral Components', FSC, based on NASVD, was tested with some success. In Finland, a database 'LINSSI' has been developed for spectral data management. In CGS search mode a 'peak hypothesis test' is applied to the measured spectra. This system was tested during the Helsinki 2005 Athletics World Championship and it provides fast and reliable automated alarms for intermediate and high level signals. In Sweden mobile detector systems are used for border controls and problems are encountered when making measurement in harbour, container areas. The methods for handling data and for interpretation of urban gamma spectrometry measurements were compared and tested on the same data sets from Copenhagen and Helsinki. Software tools were developed for converting data between the Finnish LINSSI database and the binary file formats used in Denmark and Sweden. The Processing methods used at DTU and STUK have different goals. The ASSS and FSC methods are designed to optimize the overall detection capability of the system, while sacrificing speed, usability and to a certain level robustness. These methods cannot always be used for real time analysis. The Peak Significance method is designed to give robust alarms in real time, while sacrificing some of the detection capability. Thus these methods are not interchangeable, but rather complementary. An ideal system

  4. Nuclear analysis techniques and environmental sciences

    International Nuclear Information System (INIS)

    1997-10-01

    31 theses are collected in this book. It introduced molecular activation analysis micro-PIXE and micro-probe analysis, x-ray fluorescence analysis and accelerator mass spectrometry. The applications about these nuclear analysis techniques are presented and reviewed for environmental sciences

  5. A decade of plant proteomics and mass spectrometry: Translation of technical advancements to food security and safety issues

    NARCIS (Netherlands)

    Agrawal, G.; Sarkar, A.; Righetti, P.; Pedreschi Plasencia, R.P.

    2013-01-01

    Tremendous progress in plant proteomics driven by mass spectrometry (MS) techniques has been made since 2000 when few proteomics reports were published and plant proteomics was in its infancy. These achievements include the refinement of existing techniques and the search for new techniques to

  6. Analysis of organic compounds by secondary neutral mass spectrometry (SNMS) and secondary ion mass spectrometry (SIMS)

    International Nuclear Information System (INIS)

    Ewinger, H.P.

    1993-05-01

    This study is about the use of secondary neutral mass spectrometry (SNMS) and secondary ion mass spectrometry (SIMS) as analytical techniques with depth resolution in determining organic components in environmental solid microparticles. The first application of plasma SNMS to organic compounds revealed the spectra to be composed mainly of signals from the atoms of all participating elements, such as C, H, O, N, S, P, and Cl. In addition, signals produced by multi-atomic clusters can be detected, such as CH, C 2 , CH 2 , C 2 H, and C 3 , as well as signals indicating the presence of organic compounds with hetero elements, such as OH, NH, and CN. Their intensity decreases very markedly with increasing numbers of atoms. Among the signals from bi-atomic clusters, those coming from elements with large mass differences are most intense. The use of plasma SNMS with organic compounds has shown that, except for spurious chemical reactions induced by ion bombardment and photodesorption by the photons of the plasma, it is possible to analyze with resolution in depth, elements of organic solids. A more detailed molecular characterization of organic compounds is possible by means of SIMS on the basis of multi-atomic fragments and by comparison with suitable signal patterns. (orig./BBR) [de

  7. Pragmatismo e os pragmáticos nos estudos organizacionais

    Directory of Open Access Journals (Sweden)

    Francis Kanashiro Meneghetti

    Full Text Available O objetivo central deste ensaio teórico é avaliar as contribuições do pragmatismo nos Estudos Organizacionais e, os específicos, avaliar se as contribuições teóricas de Charles Peirce e John Dewey possibilitam afirmar o pragmatismo como senso comum, ciência ou teoria do conhecimento; analisar as contribuições - possibilidadese limites - do pragmatismo como conhecimento científico; compreender os percursos do pragmatismo nos Estudos Organizacionais. Chaga-se a conclusão de que ser pragmático é diferente de conceber estudos articulados no campo epistemológico do pragmatismo. O sujeito pragmático vê na sua utilidade e na necessidade deação, o ponto de tensão que coloca em dúvida a veracidade dos pressupostos do pragmatismo como ciência. O que ocorre nos Estudos Organizacionais éa conversão do pragmatismo como conhecimento científico emsubordinação irracional à utilidade e à ação prática, sobretudo, no campo da economia, da política, da ciência, da cultura, da educação, e assim por diante.

  8. ACREDITAÇÃO HOSPITALAR: UM ESTUDO DE CASO

    Directory of Open Access Journals (Sweden)

    Felipe Antunes

    2005-06-01

    Full Text Available Este artigo aborda a qualidade e acreditação hospitalar através do Manual das Organizações Prestadoras de Serviços Hospitalares, desenvolvido pela Organização Nacional de Acreditação (ONA. O objetivo geral deste trabalho é avaliar o processo de acreditação, identificando dificuldades e benefícios advindos da implantação deste  Manual. Após a realização de uma revisão bibliográfica sobre qualidade em hospitais e normas da qualidade aplicáveis a hospitais, é feita uma análise crítica teórica do Manual das Organizações Prestadoras de Serviços Hospitalares. Tal análise crítica inclui um estudo comparativo entre os requisitos do Manual e da norma NBR ISO 9001/2000. A seguir, a análise teórica é complementada através de um estudo de caso contemplando a implantação do Manual junto a um hospital de grande porte. Finalmente, são apresentadas as conclusões, baseadas tanto no estudo teórico como no estudo prático.

  9. Direct analysis of traditional Chinese medicines by mass spectrometry.

    Science.gov (United States)

    Wong, Melody Yee-Man; So, Pui-Kin; Yao, Zhong-Ping

    2016-07-15

    Analysis of traditional Chinese medicines (TCMs) plays important roles in quality control of TCMs and understanding their pharmacological effects. Mass spectrometry (MS) is a technique of choice for analysis of TCMs due to its superiority in speed, sensitivity and specificity. However, conventional MS analysis of TCMs typically requires extensive sample pretreatment and chromatographic separation, which could be time-consuming and laborious, prior to the analysis. The expanding usage of TCMs worldwide demands development of rapid, cost-effective and reliable methods for analysis of TCMs. In recent years, new sample preparation and ionization techniques have been developed to enable direct analysis of TCMs by MS, significantly reducing the analysis time and cost. In this review, various MS-based techniques, mainly including ambient ionization-MS and MALDI-MS based techniques, applied for direct analysis of TCMs are summarized and their applicability and future prospects are discussed. Copyright © 2015 Elsevier B.V. All rights reserved.

  10. Translation Techniques

    OpenAIRE

    Marcia Pinheiro

    2015-01-01

    In this paper, we discuss three translation techniques: literal, cultural, and artistic. Literal translation is a well-known technique, which means that it is quite easy to find sources on the topic. Cultural and artistic translation may be new terms. Whilst cultural translation focuses on matching contexts, artistic translation focuses on matching reactions. Because literal translation matches only words, it is not hard to find situations in which we should not use this technique.  Because a...

  11. Native Mass Spectrometry in Fragment-Based Drug Discovery

    Directory of Open Access Journals (Sweden)

    Liliana Pedro

    2016-07-01

    Full Text Available The advent of native mass spectrometry (MS in 1990 led to the development of new mass spectrometry instrumentation and methodologies for the analysis of noncovalent protein–ligand complexes. Native MS has matured to become a fast, simple, highly sensitive and automatable technique with well-established utility for fragment-based drug discovery (FBDD. Native MS has the capability to directly detect weak ligand binding to proteins, to determine stoichiometry, relative or absolute binding affinities and specificities. Native MS can be used to delineate ligand-binding sites, to elucidate mechanisms of cooperativity and to study the thermodynamics of binding. This review highlights key attributes of native MS for FBDD campaigns.

  12. Inorganic trace analysis by laser ionization mass spectrometry

    International Nuclear Information System (INIS)

    Becker, S.; Dietze, H.J.

    1991-01-01

    Among the different spectrometric techniques for trace analysis Laser Ionization Mass Spectrometry (LIMS) is well established as a trace analytic method with a wide coverage. In the LIMS the sample material is evaporated and ionized by means of a focused pulsed laser beam in a laser microplasma, which is formed in the spot area of the irradiated sample. All chemical elements in the sample materials are evaporated and ionized in the laser plasma. The formed ions are separated according to mass and energy by a time-of-flight, quadrupole or double focusing mass spectrometer. In this review the characteristics and analytical features, some recent developments, and applications of laser ionization mass spectrometry in inorganic trace analysis are described. (orig.)

  13. Identifying modifications in RNA by MALDI mass spectrometry

    DEFF Research Database (Denmark)

    Douthwaite, Stephen; Kirpekar, Finn

    2007-01-01

    as RNA modifications added in cell-free in vitro systems. MALDI-MS is particularly useful in cases in which other techniques such as those involving primer extension or chromatographic analyses are not practicable. To date, MALDI-MS has been used to localize rRNA modifications that are involved......Posttranscriptional modifications on the base or sugar of ribonucleosides generally result in mass increases that can be measured by mass spectrometry. Matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) is a direct and accurate means of determining the masses of RNAs. Mass...... spectra produced by MALDI are relatively straightforward to interpret, because they are dominated by singly charged ions, making it possible to analyze complex mixtures of RNA oligonucleotides ranging from trinucleotides up to 20-mers. Analysis of modifications within much longer RNAs, such as ribosomal...

  14. Determination of {sup 135}Cs by accelerator mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    MacDonald, C.M.; Charles, C.R.J. [Andre. E. Lalonde AMS Laboratory, University of Ottawa, 150 Louis Pasteur, Ottawa, ON K1N 6N5 (Canada); Department of Earth Sciences, University of Ottawa, 150 Louis Pasteur, Ottawa, ON K1N 6N5 (Canada); Zhao, X.-L.; Kieser, W.E. [Andre. E. Lalonde AMS Laboratory, University of Ottawa, 150 Louis Pasteur, Ottawa, ON K1N 6N5 (Canada); Department of Physics, University of Ottawa, 150 Louis Pasteur, Ottawa, ON K1N 6N5 (Canada); Cornett, R.J. [Andre. E. Lalonde AMS Laboratory, University of Ottawa, 150 Louis Pasteur, Ottawa, ON K1N 6N5 (Canada); Department of Earth Sciences, University of Ottawa, 150 Louis Pasteur, Ottawa, ON K1N 6N5 (Canada); Litherland, A.E. [IsoTrace Laboratory, University of Toronto, 60 St. George St., Toronto, ON M5S 1A7 (Canada)

    2015-10-15

    The ratio of anthropogenic {sup 135}Cs and {sup 137}Cs isotopes is characteristic of a uranium fission source. This research evaluates the technique of isotope dilution (yield tracing) for the purpose of quantifying {sup 135}Cs by accelerator mass spectrometry with on-line isobar separation. Interferences from Ba, Zn{sub 2}, and isotopes of equal mass to charge ratios were successfully suppressed. However, some sample crosstalk from source contamination remains. The transmission and di-fluoride ionization efficiencies of Cs isotopes were found to be 8 × 10{sup −3} and 1.7 × 10{sup −7} respectively. This quantification of {sup 135}Cs using yield tracing by accelerator mass spectrometry shows promise for future environmental sample analysis once the issues of sample crosstalk and low efficiency can be resolved.

  15. Simultaneous determination of U and Pu isotopes by alpha spectrometry

    International Nuclear Information System (INIS)

    Equillor, H.E.; Campos, J.M.

    2011-01-01

    Determination of actinides by alpha spectrometry is usually carried out after full separation of each of the components of the sample. The procedure presented in this paper permits U and Pu isotopes to be measured together allowing faster sample processing and measurement. The method consists in the extraction with tributyl phosphate of U and Pu isotopes from the rest of the matrix, followed by a cathodic electrodeposition to obtain alpha spectrometry suitable pieces. It can be applied to various environmental samples, such as water, filters and soil (about 0.5 g of solid sample for the described conditions). High-quality electroplated discs are essential for simultaneous processing, so a technique to achieve this requirement is also explained. (authors) [es

  16. Desorption and ionization processes in laser mass spectrometry

    International Nuclear Information System (INIS)

    Peyl, G.J.Q. van der.

    1984-01-01

    In this thesis results are reported from a study on the desorption- and ionization process initiated by infra-red laser irradiation (LDMS) or ion bombardment (SIMS) of thin organic sample layers. The study is especially focused on the formation of quasimolecular ions under these conditions. Results of these investigations can be used for a better optimization of the LDMS and SIMS techniques in organic mass spectrometry. First, an overview is given of laser desorption mass spectrometry. Next, the coupling of the laser energy into the organic sample layer is investigated. It is concluded that the laser energy is primarily absorbed by the substrate material and not by the organic overlayer. The formation of quasi-molecular ions, either in the gas phase or in the substrate surface is investigated. The final section reports kinetic energy distributions for ions sputtered from organic solids and liquids. (Auth.)

  17. Sharing and community curation of mass spectrometry data with GNPS

    Science.gov (United States)

    Nguyen, Don Duy; Watrous, Jeramie; Kapono, Clifford A; Luzzatto-Knaan, Tal; Porto, Carla; Bouslimani, Amina; Melnik, Alexey V; Meehan, Michael J; Liu, Wei-Ting; Crüsemann, Max; Boudreau, Paul D; Esquenazi, Eduardo; Sandoval-Calderón, Mario; Kersten, Roland D; Pace, Laura A; Quinn, Robert A; Duncan, Katherine R; Hsu, Cheng-Chih; Floros, Dimitrios J; Gavilan, Ronnie G; Kleigrewe, Karin; Northen, Trent; Dutton, Rachel J; Parrot, Delphine; Carlson, Erin E; Aigle, Bertrand; Michelsen, Charlotte F; Jelsbak, Lars; Sohlenkamp, Christian; Pevzner, Pavel; Edlund, Anna; McLean, Jeffrey; Piel, Jörn; Murphy, Brian T; Gerwick, Lena; Liaw, Chih-Chuang; Yang, Yu-Liang; Humpf, Hans-Ulrich; Maansson, Maria; Keyzers, Robert A; Sims, Amy C; Johnson, Andrew R.; Sidebottom, Ashley M; Sedio, Brian E; Klitgaard, Andreas; Larson, Charles B; P., Cristopher A Boya; Torres-Mendoza, Daniel; Gonzalez, David J; Silva, Denise B; Marques, Lucas M; Demarque, Daniel P; Pociute, Egle; O'Neill, Ellis C; Briand, Enora; Helfrich, Eric J. N.; Granatosky, Eve A; Glukhov, Evgenia; Ryffel, Florian; Houson, Hailey; Mohimani, Hosein; Kharbush, Jenan J; Zeng, Yi; Vorholt, Julia A; Kurita, Kenji L; Charusanti, Pep; McPhail, Kerry L; Nielsen, Kristian Fog; Vuong, Lisa; Elfeki, Maryam; Traxler, Matthew F; Engene, Niclas; Koyama, Nobuhiro; Vining, Oliver B; Baric, Ralph; Silva, Ricardo R; Mascuch, Samantha J; Tomasi, Sophie; Jenkins, Stefan; Macherla, Venkat; Hoffman, Thomas; Agarwal, Vinayak; Williams, Philip G; Dai, Jingqui; Neupane, Ram; Gurr, Joshua; Rodríguez, Andrés M. C.; Lamsa, Anne; Zhang, Chen; Dorrestein, Kathleen; Duggan, Brendan M; Almaliti, Jehad; Allard, Pierre-Marie; Phapale, Prasad; Nothias, Louis-Felix; Alexandrov, Theodore; Litaudon, Marc; Wolfender, Jean-Luc; Kyle, Jennifer E; Metz, Thomas O; Peryea, Tyler; Nguyen, Dac-Trung; VanLeer, Danielle; Shinn, Paul; Jadhav, Ajit; Müller, Rolf; Waters, Katrina M; Shi, Wenyuan; Liu, Xueting; Zhang, Lixin; Knight, Rob; Jensen, Paul R; Palsson, Bernhard O; Pogliano, Kit; Linington, Roger G; Gutiérrez, Marcelino; Lopes, Norberto P; Gerwick, William H; Moore, Bradley S; Dorrestein, Pieter C; Bandeira, Nuno

    2017-01-01

    The potential of the diverse chemistries present in natural products (NP) for biotechnology and medicine remains untapped because NP databases are not searchable with raw data and the NP community has no way to share data other than in published papers. Although mass spectrometry techniques are well-suited to high-throughput characterization of natural products, there is a pressing need for an infrastructure to enable sharing and curation of data. We present Global Natural Products Social molecular networking (GNPS, http://gnps.ucsd.edu), an open-access knowledge base for community wide organization and sharing of raw, processed or identified tandem mass (MS/MS) spectrometry data. In GNPS crowdsourced curation of freely available community-wide reference MS libraries will underpin improved annotations. Data-driven social-networking should facilitate identification of spectra and foster collaborations. We also introduce the concept of ‘living data’ through continuous reanalysis of deposited data. PMID:27504778

  18. Time-of-flight scattering and recoiling spectrometry

    International Nuclear Information System (INIS)

    Rabalais, J.W.

    1991-01-01

    Ion scattering and recoiling spectrometry consists of directing a collimated beam of monoenergetic ions towards a surface and measuring the flux of scattered and recoiled particles from this surface. When the neutral plus ion flux is velocity selected by measuring the flight times from the sample to the detector, the technique is called time-of-flight scattering and recoiling spectrometry (TOF-SARS). TOF-SARS is capable of (1) surface elemental analysis by applying classical mechanics to the velocities of the particles, (2) surface structural analysis by monitoring the angular anisotropies in the particle flux, and (3) ion-surface electron exchange probabilities by analysis of the ion/neutral fractions in the particle flux. Examples of these three areas are presented herein

  19. On the expression 'external calibration' in atomic spectrometry

    International Nuclear Information System (INIS)

    Kantor, Tibor

    2008-01-01

    The expressions 'calibration' and 'external calibration' appear together in the present literature of atomic spectrometry resulting in a dilemma of understanding and correct use. It is examined how the IUPAC can provide a guidance to the solution of this problem by recalling the definitions of related terms of optical, mass and X-ray atomic spectrometry techniques. The introduction and definition of these expressions in widely used text books are investigated and statistically evaluated for the articles published during the last 30 years in the periodical Spectrochimica Acta Part B. For the elimination of the literary difficulties with the use of the term 'calibration', attributes are proposed to express the degree of matrix matching of standards and samples

  20. GESTÃO DO VOLUNTARIADO: Um Panorama dos Estudos Realizados no Brasil.

    Directory of Open Access Journals (Sweden)

    Sheila Patrícia Ramos

    2016-08-01

    Full Text Available Um novo padrão de voluntariado iniciou a partir de 1990 no Brasil, foram criados centros de referência que tinham por objetivo organizar, capacitar e direcionar o trabalho voluntário. A presente pesquisa tem como objetivo analisar os estudos publicados no Brasil sobre o tema gestão do voluntariado e com isso pretende-se mapear estudos teóricos e empíricos nacionais. Para tanto, foi realizada uma pesquisa bibliométrica, de caráter exploratório-descritiva, em dados secundários. Os resultados foram dispostos em forma de tabela. A amostra foi composta por quinze estudos, sendo artigos científicos publicados em revistas e eventos. A média de autores identificados nos artigos foram de 2,4. Predominam as pesquisas práticas e qualitativas com uso da técnica de entrevista apoiado pelo uso de documentos e/ou observação.  80% das pesquisas são qualitativas e 20% de natureza quali/quanti. 80% dos estudos identificados são práticos, 60% foram publicados em fontes classificadas pela CAPES como “B” e 40% “A”.    A new voluntary standard started from 1990 in Brazil, the reference centers have been created that aimed to organize, train and direct volunteer work. This research aims to analyze the studies published in Brazil the problem of volunteer management and aims to map theoretical and empirical national. For this, a bibliometric, descriptive and exploratory research was conducted on secondary data. The results were arranged in a table. The sample consisted of fifteen scientific studies and articles published in magazines and events. The average number of authors identified in Articles 2.4. Predominance of practice and qualitative research using the interview technique with the support of the use of documents and / or observation. 80% of research is qualitative and 20% qualitative / quantitative nature. 80% of the identified studies are practical, 60% were published in classified by CAPES as "B" and 40% "A" sources.