WorldWideScience

Sample records for plasma-optic mass separators

  1. Mass Separation by Metamaterials.

    Science.gov (United States)

    Restrepo-Flórez, Juan Manuel; Maldovan, Martin

    2016-02-25

    Being able to manipulate mass flow is critically important in a variety of physical processes in chemical and biomolecular science. For example, separation and catalytic systems, which requires precise control of mass diffusion, are crucial in the manufacturing of chemicals, crystal growth of semiconductors, waste recovery of biological solutes or chemicals, and production of artificial kidneys. Coordinate transformations and metamaterials are powerful methods to achieve precise manipulation of molecular diffusion. Here, we introduce a novel approach to obtain mass separation based on metamaterials that can sort chemical and biomolecular species by cloaking one compound while concentrating the other. A design strategy to realize such metamaterial using homogeneous isotropic materials is proposed. We present a practical case where a mixture of oxygen and nitrogen is manipulated using a metamaterial that cloaks nitrogen and concentrates oxygen. This work lays the foundation for molecular mass separation in biophysical and chemical systems through metamaterial devices.

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

    Science.gov (United States)

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

    2015-07-23

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-07-23

    Graphical abstract: This tutorial review is dedicated to the analysis of organic/hydro-organic matrices by ICP techniques. A state-of-the-art focusing on sample introduction, relevant operating parameters optimization and analytical strategies for elemental quantification is provided. - Highlights: • Practical considerations to perform analyses in organic/hydro-organic matrices. • Description, benefits and drawbacks of recent introduction devices. • Optimization to improve plasma tolerance towards organic/hydro-organic matrices. • Analytical strategies for elemental quantification in organic/hydro-organic matrices. - Abstract: Inductively coupled plasma optical emission spectrometry (ICP-OES) and mass spectrometry (ICP-MS) are increasingly used to carry out analyses in organic/hydro-organic matrices. The introduction of such matrices into ICP sources is particularly challenging and can be the cause of numerous drawbacks. This tutorial review, divided in two parts, explores the rich literature related to the introduction of organic/hydro-organic matrices in ICP sources. Part I provided theoretical considerations associated with the physico-chemical properties of such matrices, in an attempt to understand the induced phenomena. Part II of this tutorial review is dedicated to more practical considerations on instrumentation, instrumental and operating parameters, as well as analytical strategies for elemental quantification in such matrices. Two important issues are addressed in this part: the first concerns the instrumentation and optimization of instrumental and operating parameters, pointing out (i) the description, benefits and drawbacks of different kinds of nebulization and desolvation devices and the impact of more specific instrumental parameters such as the injector characteristics and the material used for the cone; and, (ii) the optimization of operating parameters, for both ICP-OES and ICP-MS. Even if it is at the margin of this tutorial review

  4. Optics of mass separator I

    Energy Technology Data Exchange (ETDEWEB)

    Balestrini, S.J.

    1981-07-01

    The ion optics of an existing mass separator are documented. The elctrostatic and magnetic stages are analyzed theoretically, both separately and in combination, by paying particular attention to the ion trajectories, the linear and angular magnifications, and the dispersion. The possibility of converting the magnet into a tunable unit by means of current-carrying elements in the gap is demonstrated. The feasibility of correction coils constructed from printed circuit board is shown.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-07-23

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

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

    Science.gov (United States)

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

    2015-07-23

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

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

    Science.gov (United States)

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

    2016-09-06

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

  8. SPIRAL2/DESIR high resolution mass separator

    Energy Technology Data Exchange (ETDEWEB)

    Kurtukian-Nieto, T., E-mail: kurtukia@cenbg.in2p3.fr [Centre d’Études Nucléaires de Bordeaux Gradignan, Université Bordeaux 1-CNRS/IN2P3, BP 120, F-33175 Gradignan Cedex (France); Baartman, R. [TRIUMF, 4004 Wesbrook Mall, Vancouver B.C., V6T 2A3 (Canada); Blank, B.; Chiron, T. [Centre d’Études Nucléaires de Bordeaux Gradignan, Université Bordeaux 1-CNRS/IN2P3, BP 120, F-33175 Gradignan Cedex (France); Davids, C. [Physics Division, Argonne National Laboratory, Argonne, IL 60439 (United States); Delalee, F. [Centre d’Études Nucléaires de Bordeaux Gradignan, Université Bordeaux 1-CNRS/IN2P3, BP 120, F-33175 Gradignan Cedex (France); Duval, M. [GANIL, CEA/DSM-CNRS/IN2P3, Bd Henri Becquerel, BP 55027, F-14076 Caen Cedex 5 (France); El Abbeir, S.; Fournier, A. [Centre d’Études Nucléaires de Bordeaux Gradignan, Université Bordeaux 1-CNRS/IN2P3, BP 120, F-33175 Gradignan Cedex (France); Lunney, D. [CSNSM-IN2P3-CNRS, Université de Paris Sud, F-91405 Orsay (France); Méot, F. [BNL, Upton, Long Island, New York (United States); Serani, L. [Centre d’Études Nucléaires de Bordeaux Gradignan, Université Bordeaux 1-CNRS/IN2P3, BP 120, F-33175 Gradignan Cedex (France); Stodel, M.-H.; Varenne, F. [GANIL, CEA/DSM-CNRS/IN2P3, Bd Henri Becquerel, BP 55027, F-14076 Caen Cedex 5 (France); and others

    2013-12-15

    DESIR is the low-energy part of the SPIRAL2 ISOL facility under construction at GANIL. DESIR includes a high-resolution mass separator (HRS) with a designed resolving power m/Δm of 31,000 for a 1 π-mm-mrad beam emittance, obtained using a high-intensity beam cooling device. The proposed design consists of two 90-degree magnetic dipoles, complemented by electrostatic quadrupoles, sextupoles, and a multipole, arranged in a symmetric configuration to minimize aberrations. A detailed description of the design and results of extensive simulations are given.

  9. Rotation and instabilities for isotope and mass separation

    Science.gov (United States)

    Rax, J.-M.; Gueroult, R.

    2016-10-01

    Rotating plasmas have the potential to offer unique capabilities for isotope and mass separation. Among the various electric and magnetic field configurations offering mass separation capabilities, rotating plasmas produced through static or oscillating fields are shown to be a leading candidate for tackling the unsolved problem of large-scale plasma separation. The successful development and deployment of industrial-scale plasma separation technologies could, among many other applications, provide an innovative path towards advanced sustainable nuclear energy. In this context, the potential and versatility of plasma rotation induced by rotating magnetic fields is uncovered and analysed. Analytical stability diagrams are derived from rotating ion orbits as a function of ion mass. Based on these findings, the basic principles of a rotating field plasma separator are then introduced. In light of these results, challenges associated with this original separation process are underlined, and the main directions for a future research program aimed at this important unsolved problem of applied plasma physics are identified.

  10. Application for the On-line Isotope Mass Separator ISOLDE Facility: the Mass Scan

    CERN Document Server

    Sánchez-Conejo, Jorge

    2003-01-01

    The purpose of the Mass Scan Application is to scan the mass of the ion beam that passes through the GPS (General Purpose Separator) on the On-Line Isotope Mass Separator ISOLDE facility. The application has been developed in Java, making use of the Java Development Kit 1.4 and the PS Java environment.

  11. Precise Measurement of Separation Between Two Spherical Source Masses

    Institute of Scientific and Technical Information of China (English)

    陈德才; 罗俊; 胡忠坤; 赵亮

    2004-01-01

    A driving gauge method is performed to determine the separation between two spherical source masses in the measurement of Newtonian gravitational constant G. The experimental result shows that the uncertainty of determining the separation is about 0.35μm, which would contribute an uncertainty of 7.3ppm to the value of G.

  12. Membrane device and process for mass exchange, separation, and filtration

    Science.gov (United States)

    Liu, Wei; Canfield, Nathan L.

    2016-11-15

    A membrane device and processes for fabrication and for using are disclosed. The membrane device may include a number of porous metal membranes that provide a high membrane surface area per unit volume. The membrane device provides various operation modes that enhance throughput and selectivity for mass exchange, mass transfer, separation, and/or filtration applications between feed flow streams and permeate flow streams.

  13. Hybrid ion mobility and mass spectrometry as a separation tool.

    Science.gov (United States)

    Ewing, Michael A; Glover, Matthew S; Clemmer, David E

    2016-03-25

    Ion mobility spectrometry (IMS) coupled to mass spectrometry (MS) has seen spectacular growth over the last two decades. Increasing IMS sensitivity and capacity with improvements in MS instrumentation have driven this growth. As a result, a diverse new set of techniques for separating ions by their mobility have arisen, each with characteristics that make them favorable for some experiments and some mass spectrometers. Ion mobility techniques can be broken down into dispersive and selective techniques based upon whether they pass through all mobilities for later analysis by mass spectrometry or select ions by mobility or a related characteristic. How ion mobility techniques fit within a more complicated separation including mass spectrometry and other techniques such as liquid chromatography is of fundamental interest to separations scientists. In this review we explore the multitude of ion mobility techniques hybridized to different mass spectrometers, detailing current challenges and opportunities for each ion mobility technique and for what experiments one technique might be chosen over another. The underlying principles of ion mobility separations, including: considerations regarding separation capabilities, ion transmission, signal intensity and sensitivity, and the impact that the separation has upon the ion structure (i.e., the possibility of configurational changes due to ion heating) are discussed.

  14. Recent development of plasma optical systems (invited)

    Energy Technology Data Exchange (ETDEWEB)

    Goncharov, A. A., E-mail: gonchar@iop.kiev.ua [Institute of Physics, National Academy of Science, Kiev 03028 (Ukraine)

    2016-02-15

    The article devotes a brief description of the recent development and current status of an ongoing research of plasma optical systems based on the fundamental plasma optical idea magnetic electron isolation, equipotentialization magnetic field lines, and the axi-symmetric cylindrical electrostatic plasma lens (PL) configuration. The experimental, theoretical, and simulation investigations have been carried out over recent years collaboratively between IP NASU (Kiev), LBNL (Berkeley, USA), and HCEI RAS (Tomsk). The crossed electric and magnetic fields inherent the PL configuration that provides the attractive method for establishing a stable plasma discharge at low pressure. Using PL configuration, several high reliability plasma devices were developed. These devices are attractive for many high-tech applications.

  15. Modelling of new generation plasma optical devices

    Directory of Open Access Journals (Sweden)

    Litovko Irina V.

    2016-06-01

    Full Text Available The paper presents new generation plasma optical devices based on the electrostatic plasma lens configuration that opens a novel attractive possibility for effective high-tech practical applications. Original approaches to use of plasma accelerators with closed electron drift and open walls for the creation of a cost-effective low-maintenance plasma lens with positive space charge and possible application for low-cost, low-energy rocket engine are described. The preliminary experimental, theoretical and simulation results are presented. It is noted that the presented plasma devices are attractive for many different applications in the state-of-the-art vacuum-plasma processing.

  16. Quark Mass Correction to Chiral Separation Effect and Pseudoscalar Condensate

    CERN Document Server

    Guo, Er-dong

    2016-01-01

    We derived an analytic structure of the quark mass correction to chiral separation effect (CSE) in small mass regime. We confirmed this structure by a D3/D7 holographic model study in a finite density, finite magnetic field background. The quark mass correction to CSE can be related to correlators of pseudo-scalar condensate, quark number density and quark condensate in static limit. We found scaling relations of these correlators with spatial momentum in the small momentum regime. They characterize medium responses to electric field, inhomogeneous quark mass and chiral shift. Beyond the small momentum regime, we found existence of normalizable mode, which possibly leads to formation of spiral phase. The normalizable mode exists beyond a critical magnetic field, whose magnitude decreases with quark chemical potential.

  17. An Application for the On-Line Isotope Mass Separator ISOLDE facility: the Mass Control

    CERN Document Server

    Ovalle Gonzalez, E

    2003-01-01

    The Mass Control Application will calculate the magnetic field for both the HRS and GPS separators. The calculation will be carry out according to parameters either entered by the user or taken from other sources.

  18. Effect of nebulizer/spray chamber interfaces on simultaneous, axial view inductively coupled plasma optical emission spectrometry for the direct determination of As and Se species separated by ion exchange high-performance liquid chromatography

    Science.gov (United States)

    Gettar, Raquel T.; Smichowski, Patricia; Garavaglia, Ricardo N.; Farías, Silvia; Batistoni, Daniel A.

    2005-06-01

    Different nebulizer/expansion chamber combinations were evaluated to assess their performance for sample introduction in the direct coupling with an axial view inductively coupled plasma multielement spectrometer for on-line determination of As and Se species previously separated by ion exchange-high performance liquid chromatography. The column effluents were injected into the plasma without prior derivatization. The instrument operation software was adapted for data acquisition and processing to allow multi-wavelength recording of the transient chromatographic peaks. After optimization of the chromatographic operating conditions, separation of mixtures of inorganic As and Se species, and of inorganic and two organic As species (monomethylarsonic and dimethylarsinic acids), was achieved with excellent resolution. Species discrimination from mixtures of As and Se oxyanions was further improved by the simultaneous element detection at specific analytical wavelengths. Three nebulizers and three spray chambers, employed in seven combinations, were tested as interfaces. Concentric nebulizers associated to a glass cyclonic chamber appear most suitable regarding sensitivity and signal to noise ratio. Measured element detection limits (3 σ) were around 10 ng ml - 1 for all the species considered, making the method a viable alternative to similar procedures that employ volatile hydride generation previous to sample injection into the plasma. Analytical recoveries both for inorganic and organic species ranged between 92 and 107%. The method was demonstrated to be apt for the analysis of surface waters potentially subjected to natural contamination with arsenic.

  19. Recent developments at the GSI Online Mass Separator

    CERN Document Server

    Schmidt, K; Burkard, K; Döring, J; aGórska, M; Grawe, H; Hüller, W; Janas, Z; Kirchner, R; La Commara, M; Mazzocchi, C; Roeckl, E

    2002-01-01

    The research programme at the GSI Online Mass Separator focuses on the study of exotic nuclei far from the valley of stability. Special emphasis is placed on the investigation of decay properties of isotopes along the N=Z line between the double shell closures at sup 5 sup 6 Ni and sup 1 sup 0 sup 0 Sn. In this contribution, the major recent achievements along with the corresponding experimental methods are reviewed.

  20. Mass selective separation applied to radioisotopes of cesium: Mass selective applied to radioisotopes

    Energy Technology Data Exchange (ETDEWEB)

    Dion, Michael [Pacific Northwest National Laboratory, 902 Battelle Boulevard Richland 99354 WA USA; Eiden, Greg [Pacific Northwest National Laboratory, 902 Battelle Boulevard Richland 99354 WA USA; Farmer, Orville [Pacific Northwest National Laboratory, 902 Battelle Boulevard Richland 99354 WA USA; Finch, Zach [Pacific Northwest National Laboratory, 902 Battelle Boulevard Richland 99354 WA USA; Liezers, Martin [Pacific Northwest National Laboratory, 902 Battelle Boulevard Richland 99354 WA USA

    2016-07-22

    A developed technique that uses the intrinsic mass-based separation capability of a quadrupole mass spectrometer has been used to resolve spectral radiometric interference of two isotopes of the same element. In this work the starting sample was a combination of 137Cs and 134Cs and was (activity) dominated by 137Cs and this methodology separated and “implanted” 134Cs that was later quantified for spectral features and ac- tivity with traditional radiometric techniques. This work demonstrated a 134Cs/137Cs activity ratio enhancement of >4 orders of magnitude and complete removal of 137Cs spectral features from the implanted target mass (i.e., 134).

  1. Attomole quantitation of protein separations with accelerator mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Vogel, J S; Grant, P G; Buccholz, B A; Dingley, K; Turteltaub, K W

    2000-12-15

    Quantification of specific proteins depends on separation by chromatography or electrophoresis followed by chemical detection schemes such as staining and fluorophore adhesion. Chemical exchange of short-lived isotopes, particularly sulfur, is also prevalent despite the inconveniences of counting radioactivity. Physical methods based on isotopic and elemental analyses offer highly sensitive protein quantitation that has linear response over wide dynamic ranges and is independent of protein conformation. Accelerator mass spectrometry quantifies long-lived isotopes such as 14C to sub-attomole sensitivity. We quantified protein interactions with small molecules such as toxins, vitamins, and natural biochemicals at precisions of 1-5% . Micro-proton-induced-xray-emission quantifies elemental abundances in separated metalloprotein samples to nanogram amounts and is capable of quantifying phosphorylated loci in gels. Accelerator-based quantitation is a possible tool for quantifying the genome translation into proteome.

  2. Laser photodissociation and spectroscopy of mass-separated biomolecular ions

    CERN Document Server

    Polfer, Nicolas C

    2014-01-01

    This lecture notes book presents how enhanced structural information of biomolecular ions can be obtained from interaction with photons of specific frequency - laser light. The methods described in the book ""Laser photodissociation and spectroscopy of mass-separated biomolecular ions"" make use of the fact that the discrete energy and fast time scale of photoexcitation can provide more control in ion activation. This activation is the crucial process producing structure-informative product ions that cannot be generated with more conventional heating methods, such as collisional activation. Th

  3. MASS DEFLECTOR APPLICATION FOR CERN’s ON-LINE ISOTOPE SEPARATOR FACILITY 073

    CERN Document Server

    Sánchez-Conejo, J

    2004-01-01

    The mass deflector application for the General Purpose Separator GPS allows splitting a beam of particles, characterized by a central mass, into two particle beams, which are sent to a high-mass and low-mass beam lines.

  4. MASS DEFLECTOR APPLICATION FOR CERN’s ON-LINE ISOTOPE SEPARATOR FACILITY 077

    CERN Document Server

    Sánchez-Conejo, J

    2004-01-01

    The mass deflector application for the General Purpose Separator GPS allows splitting a beam of particles, characterized by a central mass, into two particle beams, which are sent to a high-mass and low-mass beam lines.

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

    Science.gov (United States)

    Oropeza, D.

    2016-12-01

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

  6. Ion reactions for isobar separation in accelerator mass spectrometry

    CERN Document Server

    Litherland, A E; Doupe, J P

    2003-01-01

    The use of resonant and near resonant keV ion reactions for isobar separation in AMS is discussed. It is shown that these and other ionic reactions can be useful provided that the multiple scattering is taken into account.

  7. Radio-frequency ion deflector for mass separation

    Energy Technology Data Exchange (ETDEWEB)

    Schlösser, Magnus, E-mail: magnus.schloesser@googlemail.com; Rudnev, Vitaly; Ureña, Ángel González, E-mail: laseres@pluri.ucm.es [Unidad de Láseres y Haces Moleculares, Instituto Plurisdisciplinar, Universidad Complutense de Madrid, Madrid 28040 (Spain)

    2015-10-15

    Electrostatic cylindrical deflectors act as energy analyzer for ion beams. In this article, we present that by imposing of a radio-frequency modulation on the deflecting electric field, the ion transmission becomes mass dependent. By the choice of the appropriate frequency, amplitude, and phase, the deflector can be used as mass filter. The basic concept of the new instrument as well as simple mathematic relations are described. These calculations and further numerical simulations show that a mass sensitivity is achievable. Furthermore, we demonstrate the proof-of-principle in experimental measurements, compare the results to those of from a 1 m linear time-of-flight spectrometer, and comment on the mass resolution of the method. Finally, some potential applications are indicated.

  8. Penning trap for isobaric mass separation at IGISOL

    CERN Document Server

    Kolhinen, V; Hakala, J; Jokinen, A; Kopecky, S; Rinta-Antila, S; Szerypo, J; Äystö, J

    2003-01-01

    A cylindrical Penning trap has been built at the ion guide isotope separator facility IGISOL of the University of Jyvaeskylae. The main goal of the Penning trap application is to purify low-energy radioactive ion beams. The aim is to make isobarically pure beams. The technical description is presented.

  9. Penning trap for isobaric mass separation at IGISOL

    Energy Technology Data Exchange (ETDEWEB)

    Kolhinen, V.S. E-mail: veli.kolhinen@phys.jyu.fi; Eronen, T.; Hakala, J.; Jokinen, A.; Kopecky, S.; Rinta-Antila, S.; Szerypo, J.; Aeystoe, J

    2003-05-01

    A cylindrical Penning trap has been built at the ion guide isotope separator facility IGISOL of the University of Jyvaeskylae. The main goal of the Penning trap application is to purify low-energy radioactive ion beams. The aim is to make isobarically pure beams. The technical description is presented.

  10. Laser vaporization/ionization interface for coupling microscale separation techniques with mass spectrometry

    Science.gov (United States)

    Yeung, E.S.; Chang, Y.C.

    1999-06-29

    The present invention provides a laser-induced vaporization and ionization interface for directly coupling microscale separation processes to a mass spectrometer. Vaporization and ionization of the separated analytes are facilitated by the addition of a light-absorbing component to the separation buffer or solvent. 8 figs.

  11. Mass analysis of the components separated from printed circuit boards

    Directory of Open Access Journals (Sweden)

    Hana Charvátová

    2010-06-01

    Full Text Available Methods of effective and ecological recycling of printed circuit boards (PCBs are searched all over the world at this time.The material composition and temperature properties of PCB are necessary to be known for an optimal recycling technology. For thispurpose we analyzed weight ratio of the electronic components moulded on the selected kinds of PCBs and next we formulatedmathematic model of temperature field in PCB during a grinding process in that the metal layers are separated from the plasticelements. We present the obtained results in this paper.

  12. On the implications of aerosol liquid water and phase separation for organic aerosol mass

    Data.gov (United States)

    U.S. Environmental Protection Agency — This dataset contains data presented in the figures of the paper "On the implications of aerosol liquid water and phase separation for organic aerosol mass"...

  13. Conventional and Advanced Separations in Mass Spectrometry-Based Metabolomics: Methodologies and Applications

    Energy Technology Data Exchange (ETDEWEB)

    Heyman, Heino M.; Zhang, Xing; Tang, Keqi; Baker, Erin Shammel; Metz, Thomas O.

    2016-02-16

    Metabolomics is the quantitative analysis of all metabolites in a given sample. Due to the chemical complexity of the metabolome, optimal separations are required for comprehensive identification and quantification of sample constituents. This chapter provides an overview of both conventional and advanced separations methods in practice for reducing the complexity of metabolite extracts delivered to the mass spectrometer detector, and covers gas chromatography (GC), liquid chromatography (LC), capillary electrophoresis (CE), supercritical fluid chromatography (SFC) and ion mobility spectrometry (IMS) separation techniques coupled with mass spectrometry (MS) as both uni-dimensional and as multi-dimensional approaches.

  14. Proteolysis in microfluidic droplets: an approach to interface protein separation and peptide mass spectrometry

    OpenAIRE

    Ji, Ji; Nie, Lei; Qiao, Liang; Li, Yixin; Guo, Liping; Liu, Baohong; Yang, Pengyuan; Girault, Hubert H.

    2012-01-01

    A versatile microreactor protocol based on microfluidic droplets has been developed for on-line protein digestion. Proteins separated by liquid chromatography are fractionated in water-in-oil droplets and digested in sequence. The microfluidic reactor acts also as an electrospray ionization emitter for mass spectrometry analysis of the peptides produced in the individual droplets. Each droplet is an enzymatic micro-reaction unit with efficient proteolysis due to rapid mixing, enhanced mass tr...

  15. Intensification of heat and mass transfer by ultrasound: application to heat exchangers and membrane separation processes.

    Science.gov (United States)

    Gondrexon, N; Cheze, L; Jin, Y; Legay, M; Tissot, Q; Hengl, N; Baup, S; Boldo, P; Pignon, F; Talansier, E

    2015-07-01

    This paper aims to illustrate the interest of ultrasound technology as an efficient technique for both heat and mass transfer intensification. It is demonstrated that the use of ultrasound results in an increase of heat exchanger performances and in a possible fouling monitoring in heat exchangers. Mass transfer intensification was observed in the case of cross-flow ultrafiltration. It is shown that the enhancement of the membrane separation process strongly depends on the physico-chemical properties of the filtered suspensions.

  16. Ion exchange separation of chromium from natural water matrix for stable isotope mass spectrometric analysis

    Science.gov (United States)

    Ball, J.W.; Bassett, R.L.

    2000-01-01

    A method has been developed for separating the Cr dissolved in natural water from matrix elements and determination of its stable isotope ratios using solid-source thermal-ionization mass spectrometry (TIMS). The separation method takes advantage of the existence of the oxidized form of Cr as an oxyanion to separate it from interfering cations using anion-exchange chromatography, and of the reduced form of Cr as a positively charged ion to separate it from interfering anions such as sulfate. Subsequent processing of the separated sample eliminates residual organic material for application to a solid source filament. Ratios for 53Cr/52Cr for National Institute of Standards and Technology Standard Reference Material 979 can be measured using the silica gel-boric acid technique with a filament-to-filament standard deviation in the mean 53Cr/52Cr ratio for 50 replicates of 0.00005 or less. (C) 2000 Elsevier Science B.V. All rights reserved.

  17. Rapid separation of phosphopeptides by microchip electrophoresis-electrospray ionization mass spectrometry.

    Science.gov (United States)

    Ollikainen, Elisa; Bonabi, Ashkan; Nordman, Nina; Jokinen, Ville; Kotiaho, Tapio; Kostiainen, Risto; Sikanen, Tiina

    2016-04-01

    Protein phosphorylation is a significant biological process, but separation of phosphorylated peptide isomers is often challenging for many analytical techniques. We developed a microchip electrophoresis (MCE) method for rapid separation of phosphopeptides with on-chip electrospray ionization (ESI) facilitating online sample introduction to the mass spectrometer (MS). With the method, two monophosphorylated positional isomers of insulin receptor peptide (IR1A and IR1B) and a triply phosphorylated insulin receptor peptide (IR3), all with the same amino acid sequence, were separated from the nonphosphorylated peptide (IR0) in less than one minute. For efficient separation of the positional peptide isomers from each other derivatization with 9-fluorenylmethyl reagents (either chloroformate, Fmoc-Cl, or N-succinimidyl carbonate, Fmoc-OSu) was required before the analysis. The derivatization improved not only the separation of the monophosphorylated positional peptide isomers in MCE, but also identification of the phosphorylation site based on MS/MS.

  18. Star-galaxy separation strategies for WISE-2MASS all-sky infrared galaxy catalogues

    Science.gov (United States)

    Kovács, András; Szapudi, István

    2015-04-01

    We combine photometric information of the Wide-Field Infrared Survey Explorer (WISE) and Two Micron All Sky Survey (2MASS) all-sky infrared data bases, and demonstrate how to produce clean and complete galaxy catalogues for future analyses. Adding 2MASS colours to WISE photometry improves star-galaxy separation efficiency substantially at the expense of losing a small fraction of the galaxies. We find that 93 per cent of the WISE objects within W1 training set from the Sloan Digital Sky Survey PhotoObj table with known star-galaxy separation, and determined redshift distribution of our sample from the Galaxy and Mass Assembly spectroscopic survey. Varying the combination of photometric parameters input into our algorithm we show that W1WISE - J2MASS is a simple and effective star-galaxy separator, capable of producing results comparable to the multidimensional SVM classification. We present a detailed description of our star-galaxy separation methods, and characterize the robustness of our tools in terms of contamination, completeness, and accuracy. We explore systematics of the full sky WISE-2MASS galaxy map, such as contamination from moon glow. We show that the homogeneity of the full sky galaxy map is improved by an additional J2MASS galaxy catalogue we present in this paper covers 21 200 deg2 with dusty regions masked out, and has an estimated stellar contamination of 1.2 per cent and completeness of 70.1 per cent among 2.4 million galaxies with zmed ≈ 0.14. WISE-2MASS galaxy maps with well controlled stellar contamination will be useful for spatial statistical analyses, including cross-correlations with other cosmological random fields, such as the cosmic microwave background. The same techniques also yield a statistically controlled sample of stars as well.

  19. Flatland Position-Dependent-Mass: Polar Coordinates, Separability and Exact Solvability

    Directory of Open Access Journals (Sweden)

    Omar Mustafa

    2010-10-01

    Full Text Available The kinetic energy operator with position-dependent-mass in plane polar coordinates is obtained. The separability of the corresponding Schrödinger equation is discussed. A hypothetical toy model is reported and two exactly solvable examples are studied.

  20. Application for the On-line Isotope Mass Separator ISOLDE Facility: the Target Heater

    CERN Document Server

    Sánchez-Conejo, Jorge

    2003-01-01

    The purpose of the Heater Application is to heat and cool the target and line used on the On-Line Isotope Mass Separator ISOLDE facility up to a desired temperature selected by the user. The application has been developed in Java, making use of the Java Development Kit 1.4 and the PS Java environment.

  1. Stimuli-responsive Membranes: Smart Tools for Controllable Mass-transfer and Separation Processes

    Institute of Scientific and Technical Information of China (English)

    褚良银; 谢锐; 巨晓洁

    2011-01-01

    As emerging artificial biomimetic membranes, smart or intelligent membranes that are able to respond to environmental stimuli are attracting ever-increasing interests from various fields. Their permeation properties including hydraulic permeability and diffusional permeability can be dramatically controlled or adjusted self-regulatively in response to small chemical and/or physical stimuli in their environments. Such environmental stimuli-responsive smart membranes could find myriad applications in numerous fields ranging from controlled release to separations. Here the trans-membrane mass-transfer and membrane separation is introduced as the beginning to initiate the requirement of smart membranes, and then bio-inspired design of environmental stimuli-responsive smart membranes and four essential elements for smart membranes are introduced and discussed. Next, smart membrane types and their applications as smart tools for controllable mass-transfer in controlled release and separations are reviewed. The research tooics in the near future are also suggested.

  2. Selective Fluorination and Separation of Metals with NF3 for Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Clark, Richard A.; Barinaga, Charles J.; McNamara, Bruce K.; Schwantes, Jon M.; Ballou, Nathan E.

    2016-03-01

    We report recent progress on the development of a new methodology based on the generation of volatile metal fluorides through the use of nitrogen trifluoride (NF3), and the separation and measurement of these metal fluorides by electron ionization mass spectrometry. Though unreactive under ambient conditions, NF3 reacts selectively at specified temperatures with various metal-containing species to form volatile metal fluorides. Utilizing these species-dependent traits, elements of a sample may be sequentially produced and thus separated on-line. Metals were reacted inside a thermogravimetric analyzer, the gas outlet of which was directly coupled to a quadrupole mass spectrometer with an electron impact ionization source via a molecular leak valve. We present results of this project including the electron ionization mass spectrum of gaseous tellurium hexafluoride.

  3. Mass separation of deuterium and helium with conventional quadrupole mass spectrometer by using varied ionization energy

    Science.gov (United States)

    Yu, Yaowei; Hu, Jiansheng; Wan, Zhao; Wu, Jinhua; Wang, Houyin; Cao, Bin

    2016-03-01

    Deuterium pressure in deuterium-helium mixture gas is successfully measured by a common quadrupole mass spectrometer (model: RGA200) with a resolution of ˜0.5 atomic mass unit (AMU), by using varied ionization energy together with new developed software and dedicated calibration for RGA200. The new software is developed by using MATLAB with the new functions: electron energy (EE) scanning, deuterium partial pressure measurement, and automatic data saving. RGA200 with new software is calibrated in pure deuterium and pure helium 1.0 × 10-6-5.0 × 10-2 Pa, and the relation between pressure and ion current of AMU4 under EE = 25 eV and EE = 70 eV is obtained. From the calibration result and RGA200 scanning with varied ionization energy in deuterium and helium mixture gas, both deuterium partial pressures (PD2) and helium partial pressure (PHe) could be obtained. The result shows that deuterium partial pressure could be measured if PD2 > 10-6 Pa (limited by ultimate pressure of calibration vessel), and helium pressure could be measured only if PHe/PD2 > 0.45, and the measurement error is evaluated as 15%. This method is successfully employed in EAST 2015 summer campaign to monitor deuterium outgassing/desorption during helium discharge cleaning.

  4. Real-time 2D separation by LC × differential ion mobility hyphenated to mass spectrometry.

    Science.gov (United States)

    Varesio, Emmanuel; Le Blanc, J C Yves; Hopfgartner, Gérard

    2012-03-01

    The liquid chromatography-mass spectrometry (LC-MS) analysis of complex samples such as biological fluid extracts is widespread when searching for new biomarkers as in metabolomics. The success of this hyphenation resides in the orthogonality of both separation techniques. However, there are frequent cases where compounds are co-eluting and the resolving power of mass spectrometry (MS) is not sufficient (e.g., isobaric compounds and interfering isotopic clusters). Different strategies are discussed to solve these cases and a mixture of eight compounds (i.e., bromazepam, chlorprothixene, clonapzepam, fendiline, flusilazol, oxfendazole, oxycodone, and pamaquine) with identical nominal mass (i.e., m/z 316) is taken to illustrate them. Among the different approaches, high-resolution mass spectrometry or liquid chromatography (i.e., UHPLC) can easily separate these compounds. Another technique, mostly used with low resolving power MS analyzers, is differential ion mobility spectrometry (DMS), where analytes are gas-phase separated according to their size-to-charge ratio. Detailed investigations of the addition of different polar modifiers (i.e., methanol, ethanol, and isopropanol) into the transport gas (nitrogen) to enhance the peak capacity of the technique were carried out. Finally, a complex urine sample fortified with 36 compounds of various chemical properties was analyzed by real-time 2D separation LC×DMS-MS(/MS). The addition of this orthogonal gas-phase separation technique in the LC-MS(/MS) hyphenation greatly improved data quality by resolving composite MS/MS spectra, which is mandatory in metabolomics when performing database generation and search.

  5. BINARY CEPHEIDS: SEPARATIONS AND MASS RATIOS IN 5 M {sub ☉} BINARIES

    Energy Technology Data Exchange (ETDEWEB)

    Evans, Nancy Remage; Karovska, Margarita; Tingle, Evan [Smithsonian Astrophysical Observatory, MS 4, 60 Garden Street, Cambridge, MA 02138 (United States); Bond, Howard E. [Department of Astronomy and Astrophysics, Pennsylvania State University, University Park, PA 16802 (United States); Schaefer, Gail H. [The CHARA Array, Georgia State University, P.O. Box 3965, Atlanta, GA 30302-3965 (United States); Mason, Brian D., E-mail: nevans@cfa.harvard.edu, E-mail: heb11@psu.edu, E-mail: schaefer@chara-array.org [US Naval Observatory, 3450 Massachusetts Avenue, NW, Washington, DC 20392-5420 (United States)

    2013-10-01

    Deriving the distribution of binary parameters for a particular class of stars over the full range of orbital separations usually requires the combination of results from many different observing techniques (radial velocities, interferometry, astrometry, photometry, direct imaging), each with selection biases. However, Cepheids—cool, evolved stars of ∼5 M {sub ☉}—are a special case because ultraviolet (UV) spectra will immediately reveal any companion star hotter than early type A, regardless of the orbital separation. We have used International Ultraviolet Explorer UV spectra of a complete sample of all 76 Cepheids brighter than V = 8 to create a list of all 18 Cepheids with companions more massive than 2.0 M {sub ☉}. Orbital periods of many of these binaries are available from radial-velocity studies, or can be estimated for longer-period systems from detected velocity variability. In an imaging survey with the Hubble Space Telescope Wide Field Camera 3, we resolved three of the companions (those of η Aql, S Nor, and V659 Cen), allowing us to make estimates of the periods out to the long-period end of the distribution. Combining these separations with orbital data in the literature, we derive an unbiased distribution of binary separations, orbital periods, and mass ratios. The distribution of orbital periods shows that the 5 M {sub ☉} binaries have systematically shorter periods than do 1 M {sub ☉} stars. Our data also suggest that the distribution of mass ratios depends on both binary separation and system multiplicity. The distribution of mass ratios as a function of orbital separation, however, does not depend on whether a system is a binary or a triple.

  6. Multidimensional Separation of Natural Products Using Liquid Chromatography Coupled to Hadamard Transform Ion Mobility Mass Spectrometry

    Science.gov (United States)

    Liu, Wenjie; Zhang, Xing; Knochenmuss, Richard; Siems, William F.; Hill, Herbert H.

    2016-05-01

    A high performance liquid chromatograph (HPLC)was interfaced to an atmospheric drift tube ion mobility time of flight mass spectrometry. The power of multidimensional separation was demonstrated using chili pepper extracts. The ambient pressure drift tube ion mobility provided high resolving powers up to 166 for the HPLC eluent. With implementation of Hadamard transform (HT), the duty cycle for the ion mobility drift tube was increased from less than 1% to 50%, and the ion transmission efficiency was improved by over 200 times compared with pulsed mode, improving signal to noise ratio 10 times. HT ion mobility and TOF mass spectrometry provide an additional dimension of separation for complex samples without increasing the analysis time compared with conventional HPLC.

  7. 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.

  8. Aerosol generation of As and Se hydrides using a new Flow Blurring® multiple nebulizer for sample introduction in inductively coupled plasma optical emission spectrometry

    OpenAIRE

    Pereira, Catarinie D.; Aguirre Pastor, Miguel Ángel; NÓBREGA, Joaquim A.; Hidalgo Núñez, Montserrat; Canals Hernández, Antonio

    2014-01-01

    A new Flow Blurring® multiple nebulizer (FBMN) has been used for the efficient generation of As and Se hydrides directly into the aerosol formed inside the spray chamber before detection by inductively coupled plasma optical emission spectrometry (ICP OES). The FBMN allowed the hydride generation directly into the spray chamber without using any additional device either for solution and gas control or for gas phase separation. Synthetic solutions containing As and Se plus Ca, Mg and K were us...

  9. Separation Techniques for Uranium and Plutonium at Trace Levels for the Thermal Ionization Mass Spectrometric Determination

    Energy Technology Data Exchange (ETDEWEB)

    Suh, M. Y.; Han, S. H.; Kim, J. G.; Park, Y. J.; Kim, W. H

    2005-12-15

    This report describes the state of the art and the progress of the chemical separation and purification techniques required for the thermal ionization mass spectrometric determination of uranium and plutonium in environmental samples at trace or ultratrace levels. Various techniques, such as precipitation, solvent extraction, extraction chromatography, and ion exchange chromatography, for separation of uranium and plutonium were evaluated. Sample preparation methods and dissolution techniques for environmental samples were also discussed. Especially, both extraction chromatographic and anion exchange chromatographic procedures for uranium and plutonium in environmental samples, such as soil, sediment, plant, seawater, urine, and bone ash were reviewed in detail in order to propose some suitable methods for the separation and purification of uranium and plutonium from the safeguards environmental or swipe samples. A survey of the IAEA strengthened safeguards system, the clean room facility of IAEA's NWAL(Network of Analytical Laboratories), and the analytical techniques for safeguards environmental samples was also discussed here.

  10. Two-dimensional liquid separations-mass mapping of proteins from human cancer cell lysates.

    Science.gov (United States)

    Lubman, David M; Kachman, Maureen T; Wang, Haixing; Gong, Siyuan; Yan, Fang; Hamler, Rick L; O'Neil, Kimberly A; Zhu, Kan; Buchanan, Nathan S; Barder, Timothy J

    2002-12-25

    A review of two-dimensional (2D) liquid separation methods used in our laboratory to map the protein content of human cancer cells is presented herein. The methods discussed include various means of fractionating proteins according to isoelectric point (pI) in the first dimension. The proteins in each pI fraction are subsequently separated using nonporous (NPS) reversed-phase high-performance liquid chromatography (RP-HPLC). The liquid eluent of the RP-HPLC separation is directed on-line into an electrospray ionization time-of-flight (ESI-TOF) mass spectrometer where an accurate value of the protein intact M(r) can be obtained. The result is a 2D map of pI versus M(r) analogous to 2D gel electrophoresis; however the highly accurate and reproducible M(r) serves as the basis for interlysate comparisons. In addition, the use of liquid separations allows for the collection of hundreds of purified proteins in the liquid phase for further analysis via peptide mass mapping using matrix assisted laser desorption ionization TOF MS. A description of the methodology used and its applications to analysis of several types of human cancer cell lines is described. The potential of the method for differential proteomic analysis for the identification of biomarkers of disease is discussed.

  11. Proteolysis in microfluidic droplets: an approach to interface protein separation and peptide mass spectrometry.

    Science.gov (United States)

    Ji, Ji; Nie, Lei; Qiao, Liang; Li, Yixin; Guo, Liping; Liu, Baohong; Yang, Pengyuan; Girault, Hubert H

    2012-08-07

    A versatile microreactor protocol based on microfluidic droplets has been developed for on-line protein digestion. Proteins separated by liquid chromatography are fractionated in water-in-oil droplets and digested in sequence. The microfluidic reactor acts also as an electrospray ionization emitter for mass spectrometry analysis of the peptides produced in the individual droplets. Each droplet is an enzymatic micro-reaction unit with efficient proteolysis due to rapid mixing, enhanced mass transfer and automated handling. This droplet approach eliminates sample loss, cross-contamination, non-specific absorption and memory effect. A protein mixture was successfully identified using the droplet-based micro-reactor as interface between reverse phase liquid chromatography and mass spectrometry.

  12. Mass, charge, and energy separation by selective acceleration with a traveling potential hill

    Science.gov (United States)

    Tung, L. Schwager; Barr, W. L.; Lowder, R. S.; Post, R. F.

    1996-10-01

    A traveling electric potential hill has been used to generate an ion beam with an energy distribution that is mass dependent from a monoenergetic ion beam of mixed masses. This effect can be utilized as a novel method for mass separation applied to identification or enrichment of ions (e.g., of elements, isotopes, or molecules). This theory for mass-selective acceleration is presented here and is shown to be confirmed by experiment and by a time-dependent particle-in-cell computer simulation. Results show that monoenergetic ions with the particular mass of choice are accelerated by controlling the hill potential and the hill velocity. The hill velocity is typically 20%-30% faster than the ions to be accelerated. The ability of the hill to pickup a particular mass uses the fact that small kinetic energy differences in the lab frame appear much larger in the moving hill frame. Ions will gain energy from the approaching hill if their relative energy in the moving hill frame is less than the peak potential of the hill. The final energy of these accelerated ions can be several times the source energy, which facilitates energy filtering for mass purification or identification. If the hill potential is chosen to accelerate multiple masses, the heaviest mass will have the greatest final energy. Hence, choosing the appropriate hill potential and collector retarding voltage will isolate ions with the lightest, heaviest, or intermediate mass. In the experimental device, called a Solitron, purified 20Ne and 22Ne are extracted from a ribbon beam of neon that is originally composed of 20Ne:22Ne in the natural ratio of 91:9. The isotopic content of the processed beam is determined by measuring the energy distribution of the detected current. These results agree with the theory. In addition to mass selectivity, our theory can also be applied to the filtration of an ion beam according to charge state or energy. Because of this variety of properties, the Solitron is envisioned to

  13. Review of zero-net-mass-flux jet and its application in separation flow control

    Institute of Scientific and Technical Information of China (English)

    2008-01-01

    Since the zero-net-mass-flux (ZNMF) jet was first used as a laboratory flow control method in 1990’s, it has attracted much attention. The ZNMF jet has unique features such as compact actuator, no requirement for external air supply, complex piping, etc., and becomes a hot topic research subject in fluid mechanics. This review introduces the state of the art in the development of ZNMF jet in the quiescent fluid, the interaction of the ZNMF jet with the cross flow and its application in the separation flow control. The evolution of the vortex ring/pair and the spacial flow structure of the ZNMF in quicent fluid or cross flow are presented, as well as the key parameter effects. At last, the applications of ZNMF jet in the wake control of the circular cylinder, the separation control on the airfoil and the aerodynamic force or moment control on MAV/UAV are presented.

  14. Review of zero-net-mass-flux jet and its application in separation flow control

    Institute of Scientific and Technical Information of China (English)

    ZHANG PanFeng; WANG JinJun; FENG LiHao

    2008-01-01

    Since the zero-net-mass-flux (ZNMF) jet was first used as a laboratory flow control method in 1990's, it has attracted much attention. The ZNMF jet has unique features such as compact actuator, no requirement for external air supply, complex piping, etc., and becomes a hot topic research subject in fluid mechanics. This review introduces the state of the art in the development of ZNMF jet in the quiescent fluid, the interaction of the ZNMF jet with the cross flow and its application in the separation flow control. The evolution of the vortex ring/pair and the spacial flow structure of the ZNMF in quicent fluid or cross flow are presented, as well as the key parameter effects. At last, the applications of ZNMF jet in the wake control of the circular cylinder, the separation control on the airfoil and the aerodynamic force or moment control on MAV/UAV are presented.

  15. Base flow separation: A comparison of analytical and mass balance methods

    Science.gov (United States)

    Lott, Darline A.; Stewart, Mark T.

    2016-04-01

    Base flow is the ground water contribution to stream flow. Many activities, such as water resource management, calibrating hydrological and climate models, and studies of basin hydrology, require good estimates of base flow. The base flow component of stream flow is usually determined by separating a stream hydrograph into two components, base flow and runoff. Analytical methods, mathematical functions or algorithms used to calculate base flow directly from discharge, are the most widely used base flow separation methods and are often used without calibration to basin or gage-specific parameters other than basin area. In this study, six analytical methods are compared to a mass balance method, the conductivity mass-balance (CMB) method. The base flow index (BFI) values for 35 stream gages are obtained from each of the seven methods with each gage having at least two consecutive years of specific conductance data and 30 years of continuous discharge data. BFI is cumulative base flow divided by cumulative total discharge over the period of record of analysis. The BFI value is dimensionless, and always varies from 0 to 1. Areas of basins used in this study range from 27 km2 to 68,117 km2. BFI was first determined for the uncalibrated analytical methods. The parameters of each analytical method were then calibrated to produce BFI values as close to the CMB derived BFI values as possible. One of the methods, the power function (aQb + cQ) method, is inherently calibrated and was not recalibrated. The uncalibrated analytical methods have an average correlation coefficient of 0.43 when compared to CMB-derived values, and an average correlation coefficient of 0.93 when calibrated with the CMB method. Once calibrated, the analytical methods can closely reproduce the base flow values of a mass balance method. Therefore, it is recommended that analytical methods be calibrated against tracer or mass balance methods.

  16. Analysis of Protein Glycosylation and Phosphorylation Using Liquid Phase Separation, Protein Microarray Technology, and Mass Spectrometry

    Science.gov (United States)

    Zhao, Jia; Patwa, Tasneem H.; Pal, Manoj; Qiu, Weilian; Lubman, David M.

    2010-01-01

    Summary Protein glycosylation and phosphorylation are very common posttranslational modifications. The alteration of these modifications in cancer cells is closely related to the onset and progression of cancer and other disease states. In this protocol, strategies for monitoring the changes in protein glycosylation and phosphorylation in serum or tissue cells on a global scale and specifically characterizing these alterations are included. The technique is based on lectin affinity enrichment for glycoproteins, all liquid-phase two-dimensional fractionation, protein microarray, and mass spectrometry technology. Proteins are separated based on pI in the first dimension using chromatofocusing (CF) or liquid isoelectric focusing (IEF) followed by the second-dimension separation using nonporous silica RP-HPLC. Five lectins with different binding specificities to glycan structures are used for screening glycosylation patterns in human serum through a biotin–streptavidin system. Fluorescent phosphodyes and phosphospecific antibodies are employed to detect specific phosphorylated proteins in cell lines or human tissues. The purified proteins of interest are identified by peptide sequencing. Their modifications including glycosylation and phosphorylation could be further characterized by mass-spectrometry-based approaches. These strategies can be used in biological samples for large-scale glycoproteome/phosphoproteome screening as well as for individual protein modification analysis. PMID:19241043

  17. Extension of the two-dimensional mass channel cluster plot method to fast separations utilizing low thermal mass gas chromatography with time-of-flight mass spectrometry.

    Science.gov (United States)

    Fitz, Brian D; Synovec, Robert E

    2016-03-24

    Implementation of a data reduction and visualization method for use with high-speed gas chromatography and time-of-flight mass spectrometry (GC-TOFMS) is reported. The method, called the "2D m/z cluster method" facilitates analyte detection, deconvolution, and identification, by accurately measuring peak widths and retention times using a fast TOFMS sampling frequency (500 Hz). Characteristics and requirements for high speed GC are taken into consideration: fast separations with narrow peak widths and high peak capacity, rapid data collection rate, and effective peak deconvolution. Transitioning from standard GC (10-60+ minute separations) to fast GC (1-10 min separations) required consideration of how to properly analyze the data. This report validates use of the 2D m/z cluster method with newly developed GC technology that produces ultra-fast separations (∼1 min) with narrow analyte peak widths. Low thermal mass gas chromatography (LTM-GC) operated at a heating rate of 250 °C/min coupled to a LECO Pegasus III TOFMS analyzed a 115 component test mixture in 120 s with peak widths-at-base, wb (4σ), of 350 ms (average) to produce a separation with a high peak capacity, nc ∼ 340 (at unit resolution Rs = 1). The 2D m/z cluster method is shown to separate overlapped analytes to a limiting Rs ∼ 0.03, so the effective peak capacity was increased nearly 30-fold to nc ∼10,000 in the 120 s separation. The method, when coupled with LTM-GC-TOFMS, is demonstrated to provide unambiguous peak rank (i.e. the number of analytes per overlapped peak in the total ion current (TIC)), by visualizing locations of pure and chromatographically overlapped m/z. Hence, peak deconvolution and identification using MCR-ALS (multivariate curve resolution - alternating least squares) is demonstrated.

  18. Americium and plutonium separation by extraction chromatography for determination by accelerator mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Kazi, Zakir H. [Department of Earth Science, University of Ottawa, 140 Louis Pasteur Avenue, Ottawa K1N 6N5 (Canada); Cornett, Jack R., E-mail: jack.cornett@uottawa.ca [Department of Earth Science, University of Ottawa, 140 Louis Pasteur Avenue, Ottawa K1N 6N5 (Canada); Zhao, Xaiolei; Kieser, Liam [Department of Physics, University of Ottawa, 140 Louis Pasteur Avenue, Ottawa K1N 6N5 (Canada)

    2014-06-01

    Highlights: • Am and Pu were adsorbed and separated using a single extraction chromatography DGA column. • Pu was eluted from the column completely using on-column reduction of Pu(IV) to Pu(III). • ²⁴¹Am and 239,240Pu measurements by accelerator mass spectrometry (AMS) agree with the certified values in two SRMs. Abstract: A simple method was developed to separate Pu and Am using single column extraction chromatography employing N,N,N',N'-tetra-n-octyldiglycolamide (DGA) resin. Isotope dilution measurements of Am and Pu were performed using accelerator mass spectrometry (AMS) and alpha spectrometry. For maximum adsorption Pu was stabilized in the tetra valent oxidation state in 8 M HNO₃ with 0.05 M NaNO₂ before loading the sample onto the resin. Am(III) was adsorbed also onto the resin from concentrated HNO₃, and desorbed with 0.1 M HCl while keeping the Pu adsorbed. The on-column reduction of Pu(IV) to Pu(III) with 0.02 M TiCl₃ facilitated the complete desorption of Pu. Interferences (e.g. Ca²⁺, Fe³⁺) were washed off from the resin bed with excess HNO₃. Using NdF₃, micro-precipitates of the separated isotopes were prepared for analysis by both AMS and alpha spectrometry. The recovery was 97.7 ± 5.3% and 95.5 ± 4.6% for ²⁴¹Am and ²⁴²Pu respectively in reagents without a matrix. The recoveries of the same isotopes were 99.1 ± 6.0 and 96.8 ± 5.3% respectively in garden soil. The robustness of the method was validated using certified reference materials (IAEA 384 and IAEA 385). The measurements agree with the certified values over a range of about 1–100 Bq kg⁻¹. The single column separation of Pu and Am saves reagents, separation time, and cost.

  19. Americium and plutonium separation by extraction chromatography for determination by accelerator mass spectrometry.

    Science.gov (United States)

    Kazi, Zakir H; Cornett, Jack R; Zhao, Xaiolei; Kieser, Liam

    2014-06-04

    A simple method was developed to separate Pu and Am using single column extraction chromatography employing N,N,N',N'-tetra-n-octyldiglycolamide (DGA) resin. Isotope dilution measurements of Am and Pu were performed using accelerator mass spectrometry (AMS) and alpha spectrometry. For maximum adsorption Pu was stabilized in the tetra valent oxidation state in 8M HNO3 with 0.05 M NaNO2 before loading the sample onto the resin. Am(III) was adsorbed also onto the resin from concentrated HNO3, and desorbed with 0.1 M HCl while keeping the Pu adsorbed. The on-column reduction of Pu(IV) to Pu(III) with 0.02 M TiCl3 facilitated the complete desorption of Pu. Interferences (e.g. Ca(2+), Fe(3+)) were washed off from the resin bed with excess HNO3. Using NdF3, micro-precipitates of the separated isotopes were prepared for analysis by both AMS and alpha spectrometry. The recovery was 97.7±5.3% and 95.5±4.6% for (241)Am and (242)Pu respectively in reagents without a matrix. The recoveries of the same isotopes were 99.1±6.0 and 96.8±5.3% respectively in garden soil. The robustness of the method was validated using certified reference materials (IAEA 384 and IAEA 385). The measurements agree with the certified values over a range of about 1-100 Bq kg(-1). The single column separation of Pu and Am saves reagents, separation time, and cost.

  20. Separation and identification of neuropeptide Y, two of its fragments and their degradation products using capillary electrophoresis mass spectrometry

    NARCIS (Netherlands)

    Ensing, K; de Boer, Theo; Schreuder, N; de Zeeuw, RA

    1999-01-01

    This paper describes the development of an analytical method for the separation and identification of neuropeptide Y (NPY) and two important NPY fragments by capillary electrophoresis (CE) arid mass spectrometry (MS). A satisfactory separation and the highest sensitivity were obtained with formic ac

  1. Photon Scattering from the Stable Even-Mass Mo Isotopes Below the Neutron-Separation Energy

    Science.gov (United States)

    Rusev, G.; Hutcheson, A.; Kwan, E.; Tonchev, A. P.; Tornow, W.; Angell, C.; Hammond, S.; Karwowski, H. J.; Kelley, J. H.; Schwengner, R.; Dönau, F.; Wagner, A.

    2008-10-01

    We present results from photon-scattering experiments on the stable even-mass molybdenum isotopes below the neutron-separation energy carried out with bremsstrahlung at the superconducting electron accelerator ELBE at the Research Center Dresden-Rossendorf in Germany, and with monoenergetic photon beams at the HIγS facility at TUNL. We applied statistical methods in order to correct for the branching and cascade transitions and to determine the photoabsorption cross section. The obtained results allowed us to extend the tail of the Giant Dipole Resonance below the (,) threshold down to 4 MeV. The photoabsorption cross sections deduced from the present experiments show that the dipole strength increases with the neutron number of the Mo isotopes. The experimental results are discussed in the frame of Quasiparticle-Random-Phase-Approximation in a deformed basis which describe the increasing strength as a result of the deformation.

  2. Hollow fiber apparatus and use thereof for fluids separations and heat and mass transfers

    Science.gov (United States)

    Bikson, Benjamin; Etter, Stephen; Ching, Nathaniel

    2014-06-10

    A hollow fiber device includes a hollow fiber bundle, comprising a plurality of hollow fibers, a first tubesheet and a second tubesheet encapsulating respective distal ends of the hollow fiber bundle. The tubesheets have boreholes in fluid communication with bores of the hollow fibers. In at least one of the tubesheets, the boreholes are formed radially. The hollow fiber device can be utilized in heat exchange, in gas/gas, liquid/liquid and gas/liquid heat transfer, in combined heat and mass transfer and in fluid separation assemblies and processes. The design disclosed herein is light weight and compact and is particularly advantageous when the pressure of a first fluid introduced into the bores of hollow fibers is higher than the pressure on the shell side of the device.

  3. Advanced Multidimensional Separations in Mass Spectrometry: Navigating the Big Data Deluge

    Science.gov (United States)

    May, Jody C.; McLean, John A.

    2016-06-01

    Hybrid analytical instrumentation constructed around mass spectrometry (MS) is becoming the preferred technique for addressing many grand challenges in science and medicine. From the omics sciences to drug discovery and synthetic biology, multidimensional separations based on MS provide the high peak capacity and high measurement throughput necessary to obtain large-scale measurements used to infer systems-level information. In this article, we describe multidimensional MS configurations as technologies that are big data drivers and review some new and emerging strategies for mining information from large-scale datasets. We discuss the information content that can be obtained from individual dimensions, as well as the unique information that can be derived by comparing different levels of data. Finally, we summarize some emerging data visualization strategies that seek to make highly dimensional datasets both accessible and comprehensible.

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

    Energy Technology Data Exchange (ETDEWEB)

    Matos, Wladiana O. [Grupo de Analise Instrumental Aplicada, Universidade Federal de Sao Carlos, Sao Carlos SP (Brazil); Grupo de Analise Instrumental Aplicada, Embrapa Pecuaria Sudeste, Sao Carlos, SP (Brazil)], E-mail: wladianamatos@yahoo.com.br; Menezes, Eveline A. [Grupo de Analise Instrumental Aplicada, Universidade Federal de Sao Carlos, Sao Carlos SP (Brazil); Grupo de Analise Instrumental Aplicada, Embrapa Pecuaria Sudeste, Sao Carlos, SP (Brazil); Gonzalez, Mario H. [Grupo de Analise Instrumental Aplicada, Universidade Federal de Sao Carlos, Sao Carlos SP (Brazil); Costa, Leticia M. [Departamento de Quimica-ICEx, Universidade Federal de Minas Gerais, Belo Horizonte MG (Brazil); Trevizan, Lilian C. [Centro de Energia Nuclear na Agricultura, Universidade de Sao Paulo, Piracicaba SP (Brazil); Nogueira, Ana Rita A. [Grupo de Analise Instrumental Aplicada, Embrapa Pecuaria Sudeste, Sao Carlos, SP (Brazil)

    2009-06-15

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

  5. Identifying Gel-Separated Proteins Using In-Gel Digestion, Mass Spectrometry, and Database Searching: Consider the Chemistry

    Science.gov (United States)

    Albright, Jessica C.; Dassenko, David J.; Mohamed, Essa A.; Beussman, Douglas J.

    2009-01-01

    Matrix-assisted laser desorption/ionization (MALDI) mass spectrometry is an important bioanalytical technique in drug discovery, proteomics, and research at the biology-chemistry interface. This is an especially powerful tool when combined with gel separation of proteins and database mining using the mass spectral data. Currently, few hands-on…

  6. Identifying Gel-Separated Proteins Using In-Gel Digestion, Mass Spectrometry, and Database Searching: Consider the Chemistry

    Science.gov (United States)

    Albright, Jessica C.; Dassenko, David J.; Mohamed, Essa A.; Beussman, Douglas J.

    2009-01-01

    Matrix-assisted laser desorption/ionization (MALDI) mass spectrometry is an important bioanalytical technique in drug discovery, proteomics, and research at the biology-chemistry interface. This is an especially powerful tool when combined with gel separation of proteins and database mining using the mass spectral data. Currently, few hands-on…

  7. Experimental heat and mass transfer of the separated and coupled rotating desiccant wheel and heat wheel

    Energy Technology Data Exchange (ETDEWEB)

    Enteria, Napoleon; Yoshino, Hiroshi; Mochida, Akashi; Takaki, Rie [Graduate School of Engineering, Tohoku University, Sendai 980-8579 (Japan); Satake, Akira [Technical Research Institute, Maeda Corporation, Tokyo 179-8914 (Japan); Yoshie, Ryuichiro [Faculty of Engineering, Tokyo Polytechnic University, Atsugi 243-0297 (Japan); Mitamura, Tiruaki [Faculty of Engineering, Ashikaga Institute of Technology, Ashikaga 326-8558 (Japan); Baba, Seizo [Earth Clean Tohoku Co., Ltd., Sendai 984-0038 (Japan)

    2010-07-15

    The experimental evaluation of the separated and coupled rotating desiccant wheel and heat wheel is reported. The study aims to investigate the performance of the desiccant wheel and of the heat wheel both when operated separately and jointly. The performance evaluation of the desiccant wheel is based on its moisture removal capacity (MRC), moisture removal regeneration (MRR), and moisture mass balance (MMB). In addition, the study used the total energy balance (TEB), sensible coefficient of performance (COP{sub Sensible}), latent coefficient of performance (COP{sub Latent}) and, total coefficient of performance (COP{sub Total}). The performance of the heat wheel is based on its effectiveness. The COP{sub Sensible}, COP{sub Latent} and, COP{sub Total} are used in the performance evaluation of the coupled desiccant wheel and heat wheel. The general results of the study show that the MRC, MRR and MMB coupled with the TEB, COP{sub Latent}, COP{sub Sensible} and COP{sub Total} predict adequately the performance of the desiccant wheel. In addition, the coupled operation of the desiccant wheel and heat wheel, contributed to the reduction of the external thermal energy requirement for the regeneration of the desiccant wheel. This study can be applied in other researches seeking evaluation of the desiccant wheel, heat wheel, and their combined operation. Moreover, the data presented here are significant for the desiccant wheel benchmarking and for evaluation of the desiccant wheel models. (author)

  8. First laser ions at an off-line mass separator of the ISAC facility at TRIUMF

    CERN Document Server

    Rauth, C; Horn, R; Lassen, J; Bricault, P; Wendt, K; 10.1016/j.nimb.2003.08.029

    2004-01-01

    For efficient and in particular for selective production of radioactive ion beams at on-line mass separator facilities the technique of resonance ionization laser ion sources (RILlS) has become the most powerful tool. In facilities like ISOLDE at CERN they nowadays represent the most commonly used type of ion source for rare short-lived isotopes, delivering highest suppression of isobaric contaminations. For a first off-line demonstration preparing the development and installation of such a laser ion source at the new ISAC facility at TRIUMF in Vancouver (Canada), an all solid state laser system developed at the University of Mainz (Germany), was transferred and tested there at an off-line test separator. The laser system consists of three tunable titanium:sapphire lasers with a repetition rate of 12 kHz, pulse length of ~30 ns, up to 2.5 W output power in the infrared to red spectral region and features additional frequency doubling units. With this system first RILIS studies were performed in a number of el...

  9. Separation and Analysis of Boron Isotope in High Plant by Thermal Ionization Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Qingcai Xu

    2015-01-01

    Full Text Available Knowledge of boron and its isotope in plants is useful to better understand the transposition and translocation of boron within plant, the geochemical behavior in the interface between soil and plant, and the biogeochemical cycle of boron. It is critical to develop a useful method to separate boron from the plant for the geochemical application of boron and its isotope. A method was developed for the extraction of boron in plant sample, whose isotope was determined by thermal ionization mass spectrometry. The results indicated that this method of dry ashing coupled with two-step ion-exchange chromatography is powerful for the separation of boron in plant sample with large amounts of organic matters completely. The ratios of boron isotope composition in those plant tissue samples ranged from -19.45‰ to +28.13‰ (total range: 47.58‰ with a mean value of 2.61±11.76‰ SD. The stem and root isotopic compositions were lower than those in flower and leaf. The molecular mechanism of boron isotope may be responsible for the observed variation of boron isotopic composition and are considered as a useful tool for the better understanding of boron cycling process in the environment and for the signature of living systems.

  10. Liquid electrode plasma-optical emission spectrometry combined with solid-phase preconcentration for on-site analysis of lead.

    Science.gov (United States)

    Barua, Suman; Rahman, Ismail M M; Alam, Iftakharul; Miyaguchi, Maho; Sawai, Hikaru; Maki, Teruya; Hasegawa, Hiroshi

    2017-08-15

    A relatively rapid and precise method is presented for the determination of lead in aqueous matrix. The method consists of analyte quantitation using the liquid electrode plasma-optical emission spectrometry (LEP-OES) coupled with selective separation/preconcentration by solid-phase extraction (SPE). The impact of operating variables on the retention of lead in SPEs such as pH, flow rate of the sample solution; type, volume, flow rate of the eluent; and matrix effects were investigated. Selective SPE-separation/preconcentration minimized the interfering effect due to manganese in solution and limitations in lead-detection in low-concentration samples by LEP-OES. The LEP-OES operating parameters such as the electrical conductivity of sample solution; applied voltage; on-time, off-time, pulse count for applied voltage; number of measurements; and matrix effects have also been optimized to obtain a distinct peak for the lead at λmax=405.8nm. The limit of detection (3σ) and the limit of quantification (10σ) for lead determination using the technique were found as 1.9 and 6.5ng mL(-1), respectively. The precision, as relative standard deviation, was lower than 5% at 0.1μg mL(-1) Pb, and the preconcentration factor was found to be 187. The proposed method was applied to the analysis of lead contents in the natural aqueous matrix (recovery rate:>95%). The method accuracy was verified using certified reference material of wastewaters: SPS-WW1 and ERM-CA713. The results from LEP-OES were in good agreement with inductively coupled plasma optical emission spectrometry measurements of the same samples. The application of the method is rapid (≤5min, without preconcentration) with a reliable detection limit at trace levels. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Separation Of Uranium And Plutonium Isotopes For Measurement By Multi Collector Inductively Coupled Plasma Mass Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-03-29

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

  12. Mass spectrometric analysis of electrophoretically separated allergens and proteases in grass pollen diffusates

    Directory of Open Access Journals (Sweden)

    Geczy Carolyn L

    2003-09-01

    Full Text Available Abstract Background Pollens are important triggers for allergic asthma and seasonal rhinitis, and proteases released by major allergenic pollens can injure airway epithelial cells in vitro. Disruption of mucosal epithelial integrity by proteases released by inhaled pollens could promote allergic sensitisation. Methods Pollen diffusates from Kentucky blue grass (Poa pratensis, rye grass (Lolium perenne and Bermuda grass (Cynodon dactylon were assessed for peptidase activity using a fluorogenic substrate, as well as by gelatin zymography. Following one- or two-dimensional gel electrophoresis, Coomassie-stained individual bands/spots were excised, subjected to tryptic digestion and analysed by mass spectrometry, either MALDI reflectron TOF or microcapillary liquid chromatography MS-MS. Database searches were used to identify allergens and other plant proteins in pollen diffusates. Results All pollen diffusates tested exhibited peptidase activity. Gelatin zymography revealed high Mr proteolytic activity at ~ 95,000 in all diffusates and additional proteolytic bands in rye and Bermuda grass diffusates, which appeared to be serine proteases on the basis of inhibition studies. A proteolytic band at Mr ~ 35,000 in Bermuda grass diffusate, which corresponded to an intense band detected by Western blotting using a monoclonal antibody to the timothy grass (Phleum pratense group 1 allergen Phl p 1, was identified by mass spectrometric analysis as the group 1 allergen Cyn d 1. Two-dimensional analysis similarly demonstrated proteolytic activity corresponding to protein spots identified as Cyn d 1. Conclusion One- and two-dimensional electrophoretic separation, combined with analysis by mass spectrometry, is useful for rapid determination of the identities of pollen proteins. A component of the proteolytic activity in Bermuda grass diffusate is likely to be related to the allergen Cyn d 1.

  13. Enhanced Mixture Separations of Metal Adducted Tetrasaccharides Using Frequency Encoded Ion Mobility Separations and Tandem Mass Spectrometry

    Science.gov (United States)

    Morrison, Kelsey A.; Bendiak, Brad K.; Clowers, Brian H.

    2016-10-01

    Using five isomeric tetrasaccharides in combination with seven multivalent metals, the impact on mobility separations and resulting CID spectra were examined using a hybrid ion mobility atmospheric pressure drift tube system coupled with a linear ion trap. By enhancing the duty cycle of the drift tube system using a linearly chirped frequency, the collision-induced dissociation spectra were encoded in the mobility domain according to the drift times of each glycan isomer precursor. Differential fragmentation patterns correlated with precursor drift times ensured direct assignment of fragments with precursor structure whether as individual standards or in a mixture of isomers. In addition to certain metal ions providing higher degrees of separation than others, in select cases more than one arrival time distribution was observed for a single pure carbohydrate isomer. These observations suggest the existence of alternative coordination sites within a single monomeric species, but more interesting was the observation of different fragmentation ion yields for carbohydrate dimers formed through metal adduction. Positive-ion data were also compared with negative-ion species, where dimer formation did not occur and single peaks were observed for each isomeric tetrasaccharide-alditol. This enhanced analytical power has implications not only for carbohydrate molecules but also for a wide variety of complex mixtures of molecules where dissociation spectra may potentially be derived from combinations of monomeric, homodimeric, and heterodimeric species having identical nominal m/z values.

  14. Enriching and Separating Primary Copper Impurity from Pb-3 Mass Pct Cu Melt by Super-Gravity Technology

    Science.gov (United States)

    Yang, Yuhou; Song, Bo; Song, Gaoyang; Yang, Zhanbing; Xin, Wenbin

    2016-10-01

    In this study, super-gravity technology was introduced in the lead bullion-refining process to investigate the enriching and separating laws of copper impurity from Pb-3 mass pct Cu melt. With the gravity coefficient G = 700 at the cooling rate of ν = 5 K min-1, the entire copper phase gathers at the upper area of the sample, and it is hard to find any copper particles at the bottom area of the sample. The floatation movement of copper phase was greatly intensified by super gravity and the mass pct of copper in tailing lead is up to 8.631 pct, while that in the refined lead is only 0.113 pct. The refining rate of lead bullion reached up to 94.27 pct. Copper-phase impurity can be separated effectively from Pb-3 mass pct Cu melt by filtration method in super-gravity field, and the separation efficiency increased with the increasing gravity coefficient in the range of G ≥ 10. After filtration at 613 K (340 °C) with gravity coefficient G = 100 for 10 minutes, the refined lead, with just 0.157 mass pct copper impurity, was separated to the bottom of the crucible, and the copper dross containing only 23.56 mass pct residual lead was intercepted by the carbon fiber felt, leading to the separation efficiency up to 96.18 pct (meaning a great reduction in metal loss).

  15. Isomer separation and gas-phase configurations of organoruthenium anticancer complexes: ion mobility mass spectrometry and modeling.

    Science.gov (United States)

    Williams, Jonathan P; Bugarcic, Tijana; Habtemariam, Abraha; Giles, Kevin; Campuzano, Iain; Rodger, P Mark; Sadler, Peter J

    2009-06-01

    We have used ion mobility-mass spectrometry combined with molecular modeling for the separation and configurational analysis of three low-molecular-weight isomeric organoruthenium anticancer complexes containing ortho-, meta-, or para-terphenyl arene ligands. The isomers were separated using ion mobility based on traveling-wave technology and the experimentally determined collision cross sections were compared to theoretical calculations. Excellent agreement was observed between the experimentally and theoretically derived measurements.

  16. Mosquito mass rearing technology: a cold-water vortex device for continuous unattended separation of Anopheles arabiensis pupae from larvae.

    Science.gov (United States)

    Balestrino, Fabrizio; Gilles, Jérémie R L; Soliban, Sharon M; Nirschl, Anton; Benedict, Quentin E; Benedict, Mark Q

    2011-09-01

    In mass rearing of anopheline mosquitoes, pupae are usually separated from larvae on a daily basis to prevent unwanted adult emergence from trays. Depending on the device and species, 2 physical characteristics have most often been used for separation: buoyant density and size. In this report, we describe a system for continuous separation of Anopheles arabiensis larvae from pupae based on the natural difference in buoyant density and behavior between the 2 stages. We determined that temperatures 4-15 degrees C caused neither mortality nor reduction in likelihood of pupation or emergence. Separation improved as temperatures decreased down to 4 degrees C. We devised and demonstrated a 15 degrees C water vortex separator that we anticipate can process approximately 1 million larvae and pupae per hour with a < 0.3% pupal contamination rate and which operates unattended.

  17. Characterization of polysorbate 85, a nonionic surfactant, by liquid chromatography vs. ion mobility separation coupled with tandem mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Solak Erdem, Nilüfer; Alawani, Nadrah; Wesdemiotis, Chrys, E-mail: wesdemiotis@uakron.edu

    2014-01-15

    Graphical abstract: -- Highlights: •Liquid chromatography (LC) separates amphiphilic blends according to hydrophobicity. •Ion mobility (IM) spectrometry separates these blends based on molecular size/shape. •LC–MS provides the separation resolution needed for quantifying fatty acid content. •IM–MS enables rapid, solvent-free separation and the detection of trace components. •With either method, tandem MS allows to count the hydrophobic substituents. -- Abstract: Liquid chromatography (LC) and ion mobility (IM) separation have been coupled with mass spectrometry (MS) and tandem mass spectrometry (MS{sup 2}) to characterize a commercially important nonionic surfactant, polysorbate 85. The constituents of this amphiphilic blend contained a sorbitan or isosorbide core that was chain extended with poly(ethylene oxide) (PEO) and partially esterified at the PEO termini with oleic acid or, to a lesser extent, other fatty acids. Using interactive LC in reverse-phase mode, the oligomers of the surfactant were separated according to their hydrophobicity/hydrophilicity balance. On the other hand, IM spectrometry dispersed the surfactant oligomers by their charge and collision cross section (i.e. size/shape). With either separation method, an increased number of fatty ester groups and/or lack of the polar sorbitan (or isosorbide) core led to higher retention/drift times, enabling the separation of isobaric species or species with superimposed isotope patterns, so that their ester content could be conclusively identified by MS{sup 2}. LC–MS and IM–MS permitted the detection of several byproducts besides the major PEO-sorbitan oleate oligomers. LC–MS provides the separation resolution needed for quantitative determination of the degree of esterification. IM–MS, which minimizes analysis time and solvent use, is ideally suitable for a fast, qualitative survey of samples differing in their minor constituents or impurities.

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

    Energy Technology Data Exchange (ETDEWEB)

    Zheng, Xueyun [Earth and Biological Sciences Directorate, Pacific Northwest National Laboratory, Richland, Washington 99352,; Wojcik, Roza [Earth and Biological Sciences Directorate, Pacific Northwest National Laboratory, Richland, Washington 99352,; Zhang, Xing [Skaggs School of Pharmacy and Pharmaceutical Sciences, Anschutz Medical Campus, University of Colorado, Denver, Colorado 80045; Ibrahim, Yehia M. [Earth and Biological Sciences Directorate, Pacific Northwest National Laboratory, Richland, Washington 99352,; Burnum-Johnson, Kristin E. [Earth and Biological Sciences Directorate, Pacific Northwest National Laboratory, Richland, Washington 99352,; Orton, Daniel J. [Earth and Biological Sciences Directorate, Pacific Northwest National Laboratory, Richland, Washington 99352,; Monroe, Matthew E. [Earth and Biological Sciences Directorate, Pacific Northwest National Laboratory, Richland, Washington 99352,; Moore, Ronald J. [Earth and Biological Sciences Directorate, Pacific Northwest National Laboratory, Richland, Washington 99352,; Smith, Richard D. [Earth and Biological Sciences Directorate, Pacific Northwest National Laboratory, Richland, Washington 99352,; Baker, Erin S. [Earth and Biological Sciences Directorate, Pacific Northwest National Laboratory, Richland, Washington 99352,

    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.

  19. Two-dimensional separation of ionic species by hyphenation of capillary ion chromatography × capillary electrophoresis-mass spectrometry.

    Science.gov (United States)

    Beutner, Andrea; Kochmann, Sven; Mark, Jonas Josef Peter; Matysik, Frank-Michael

    2015-03-17

    The separation of complex mixtures such as biological or environmental samples requires high peak capacities, which cannot be established with a single separation technique. Therefore, multidimensional systems are in demand. In this work, we present the hyphenation of the two most important (orthogonal) techniques in ion analysis, namely, ion chromatography (IC) and capillary electrophoresis (CE), in combination with mass spectrometry. A modulator was developed ensuring a well-controlled coupling of IC and CE separations. Proof-of-concept measurements were performed using a model system consisting of nucleotides and cyclic nucleotides. The data are presented in a multidimensional contour plot. Analyte stacking in the CE separation could be exploited on the basis of the fact that the suppressed IC effluent is pure water.

  20. Evaluation of the mineral profile of textile materials using inductively coupled plasma optical emission spectrometry and chemometrics

    Energy Technology Data Exchange (ETDEWEB)

    Menezes, E.A.; Carapelli, R.; Bianchi, S.R. [Grupo de Analise Instrumental Aplicada, Departamento de Quimica, Universidade Federal de Sao Carlos, Sao Carlos, SP (Brazil); Embrapa Pecuaria Sudeste, C.P. 339, Sao Carlos, SP 13560-970 (Brazil); Souza, S.N.P. [Grupo de Analise Instrumental Aplicada, Departamento de Quimica, Universidade Federal de Sao Carlos, Sao Carlos, SP (Brazil); Matos, W.O. [Departamento de Quimica Analitica e Fisico-Quimica, Universidade Federal do Ceara, Fortaleza, CE (Brazil); Pereira-Filho, E.R. [Grupo de Analise Instrumental Aplicada, Departamento de Quimica, Universidade Federal de Sao Carlos, Sao Carlos, SP (Brazil); Nogueira, A.R.A., E-mail: anarita@cppse.embrapa.br [Embrapa Pecuaria Sudeste, C.P. 339, Sao Carlos, SP 13560-970 (Brazil)

    2010-10-15

    The content of Al, Ba, Ca, Cr, Cu, Fe, Ni, P, Zn, Cd and Pb was determined in textile material samples after microwave-assisted decomposition in a cavity oven and extraction with an artificial sweat solution. Radial viewing inductively coupled plasma optical emission spectrometry (ICP OES) was the main detection technique, but Cd and Pb were determined by thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) to increase the sensitivity. Principal components analysis (PCA) was applied to the data sets to characterize the samples with respect to their geographic origin and color difference. The PCA for Brazilian single-color samples showed separation, with one group consisting of blue and green textiles and another with all the other materials evaluated. The geographic origin study showed a clear separation between Brazilian and Chinese textiles. The metals amount extracted with sweat extractable solution were lower than limits values pointed by the International Testing and Certification System for Textiles, Oko Tex Standard 100, in the all considered classes. Recoveries varied from 85 to 112% for additions ranging from 3.0 to 25 mg kg{sup -1} for Ca and from 0.3 to 7.0 mg kg{sup -1} for all other analytes through the microwave-assisted decomposition procedure.

  1. Time-separated oscillatory fields for high-precision mass measurements on short-lived Al and Ca nuclides

    CERN Document Server

    George, S; Blank, B; Blaum, K; Breitenfeldt, M; Hager, U; Herfurth, F; Herlert, A; Kellerbauer, A G; Kluge, H J; Kretzschmar, M; Lunney, D; Savreux, R; Schwarz, S; Schweikhard, L; Yazidjian, C

    2008-01-01

    High-precision Penning trap mass measurements on the stable nuclide $^{27}$Al as well as on the short-lived radionuclides $^{26}$Al and $^{38,39}$Ca have been performed by use of radio-frequency excitation with time-separated oscillatory fields, i.e. Ramsey's method, as recently introduced for the excitation of the ion motion in a Penning trap, was applied. A comparison with the conventional method of a single continuous excitation demonstrates its advantage of up to ten times shorter measurements. The new mass values of $^{26,27}$Al clarify conflicting data in this specific mass region. In addition, the resulting mass values of the superallowed $\\beta$-emitter $^{38}$Ca as well as of the groundstate of the $\\beta$-emitter $^{26}$Al$^{m}$ confirm previous measurements and corresponding theoretical corrections of the ft-values.

  2. Identification of two-dimensional electrophoresis-separated proteins in human hepatoma cell by electrospray ion trap mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    As one of the most important analytical methods in proteome research, mass spectrometry was utilized to identify proteins separated by two-dimensional electrophoresis in the human hepatoma cell line BEL-7404. The protein spots were excised from the gel, followed by in-gel digestion, and the peptide mappings were analyzed by liquid chromatography electrospray ion trap mass spectrometer. Nine proteins were identified via database searching, according to the molecular weights and amino acid sequences of peptides, among which two proteins have not been identified in the other liver-cell database. The sequence coverage was 21%-72%. Furthermore, the relationship between the expressed proteins and the liver carcinoma was discussed.

  3. Mass Balance Reconciliation for Bilinear Systems: A Case Study of a Raw Mill Separator in a Typical Moroccan Cement Plant

    Directory of Open Access Journals (Sweden)

    S. Fellaou

    2016-06-01

    Full Text Available Stream flow rates and their several compositions are measured in a typical cement raw mill separator. In order to simultaneously reconcile flow and composition measurements in this circuit, the component mass balances was included as constraints which contain the products of flow rate and composition variables in the data reconciliation problem. In this paper, the effectiveness of simultaneous procedures for bilinear data reconciliation is established, the numerical problem constraints were coded in MATLAB and a mass balance model is built. Moreover, based on the difference between the measured and reconciled data it was found that it performs optimally.

  4. Separation and identification of Musa acuminate Colla (banana) leaf proteins by two-dimensional gel electrophoresis and mass spectrometry.

    Science.gov (United States)

    Lu, Y; Qi, Y X; Zhang, H; Zhang, H Q; Pu, J J; Xie, Y X

    2013-12-19

    To establish a proteomic reference map of Musa acuminate Colla (banana) leaf, we separated and identified leaf proteins using two-dimensional polyacrylamide gel electrophoresis (2D-PAGE) and mass spectrometry (MS). Tryptic digests of 44 spots were subjected to peptide mass fingerprinting (PMF) by matrix-assisted laser desorption/ionization time-of-flight (MALDI-TOF) MS. Three spots that were not identified by MALDI-TOF MS analysis were identified by searching against the NCBInr, SwissProt, and expressed sequence tag (EST) databases. We identified 41 unique proteins. The majority of the identified leaf proteins were found to be involved in energy metabolism. The results indicate that 2D-PAGE is a sensitive and powerful technique for the separation and identification of Musa leaf proteins. A summary of the identified proteins and their putative functions is discussed.

  5. Heat and mass transfer in porous media phase separation at temperatures below the lambda-point of He-4

    Science.gov (United States)

    Yuan, S. W. K.; Frederking, T. H. K.

    1986-01-01

    Newtonian fluid motion, coupled to heat transfer via latent heat of phase transition, is well known from numerous studies of condensation and boiling. Considerably less knowledge is available for vapor-liquid phase separation in the absence of gravity effect on the transport phenomena. The present studies are focused on heat and mass transfer associated with vapor-liquid phase separation required for long-term storage of the cryogen liquid He II in space vessels. Though space conditions are the dominant mode of interest in advanced equipment, e.g. IR telescopes, the systems may be operated in principle during terrestrial conditions. The latter are considered in the present work. It emphasizes the linear regime including an extrapolation based on variable thermophysical properties. Data taken with a phase separation approach show departures from the linear regime prediction. They agree with a transport equation proposed for the nonlinear, turbulent regime.

  6. Ion Mobility Separations of Isomers based upon Long Path Length Structures for Lossless Ion Manipulations Combined with Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Deng, Liulin [Biological Sciences Division and Environmental Molecular Sciences Laboratory, Pacific Northwest National Laboratory, 902 Battelle Blvd Richland, WA 99352 USA; Ibrahim, Yehia M. [Biological Sciences Division and Environmental Molecular Sciences Laboratory, Pacific Northwest National Laboratory, 902 Battelle Blvd Richland, WA 99352 USA; Baker, Erin S. [Biological Sciences Division and Environmental Molecular Sciences Laboratory, Pacific Northwest National Laboratory, 902 Battelle Blvd Richland, WA 99352 USA; Aly, Noor A. [Biological Sciences Division and Environmental Molecular Sciences Laboratory, Pacific Northwest National Laboratory, 902 Battelle Blvd Richland, WA 99352 USA; Hamid, Ahmed M. [Biological Sciences Division and Environmental Molecular Sciences Laboratory, Pacific Northwest National Laboratory, 902 Battelle Blvd Richland, WA 99352 USA; Zhang, Xing [Biological Sciences Division and Environmental Molecular Sciences Laboratory, Pacific Northwest National Laboratory, 902 Battelle Blvd Richland, WA 99352 USA; Zheng, Xueyun [Biological Sciences Division and Environmental Molecular Sciences Laboratory, Pacific Northwest National Laboratory, 902 Battelle Blvd Richland, WA 99352 USA; Garimella, Sandilya V. B. [Biological Sciences Division and Environmental Molecular Sciences Laboratory, Pacific Northwest National Laboratory, 902 Battelle Blvd Richland, WA 99352 USA; Webb, Ian K. [Biological Sciences Division and Environmental Molecular Sciences Laboratory, Pacific Northwest National Laboratory, 902 Battelle Blvd Richland, WA 99352 USA; Prost, Spencer A. [Biological Sciences Division and Environmental Molecular Sciences Laboratory, Pacific Northwest National Laboratory, 902 Battelle Blvd Richland, WA 99352 USA; Sandoval, Jeremy A. [Biological Sciences Division and Environmental Molecular Sciences Laboratory, Pacific Northwest National Laboratory, 902 Battelle Blvd Richland, WA 99352 USA; Norheim, Randolph V. [Biological Sciences Division and Environmental Molecular Sciences Laboratory, Pacific Northwest National Laboratory, 902 Battelle Blvd Richland, WA 99352 USA; Anderson, Gordon A. [Biological Sciences Division and Environmental Molecular Sciences Laboratory, Pacific Northwest National Laboratory, 902 Battelle Blvd Richland, WA 99352 USA; Tolmachev, Aleksey V. [Biological Sciences Division and Environmental Molecular Sciences Laboratory, Pacific Northwest National Laboratory, 902 Battelle Blvd Richland, WA 99352 USA; Smith, Richard D. [Biological Sciences Division and Environmental Molecular Sciences Laboratory, Pacific Northwest National Laboratory, 902 Battelle Blvd Richland, WA 99352 USA

    2016-07-01

    Mass spectrometry (MS)-based multi-omic measurements, including proteomics, metabolomics, lipidomics, and glycomics, are increasingly transforming our ability to characterize and understand biological systems, but, presently have limitations due to the chemical diversity and range of abundances of biomolecules in complex samples. Advances addressing these challenges increasingly are based upon the ability to quickly separate, react and otherwise manipulate sample components for analysis by MS. Here we report on a new approach using Structures for Lossless Ion Manipulations (SLIM) to enable long serpentine path ion mobility spectrometry (IMS) separations followed by MS analyses. This approach provides previously unachieved mobility biomolecule isomer separations for biomolecular species, in conjunction with more effective ion utilization, and producing a basis for the improved characterization of very small samples.

  7. Heat and mass transfer in porous media phase separation at temperatures below the lambda-point of He-4

    Science.gov (United States)

    Yuan, S. W. K.; Frederking, T. H. K.

    1986-01-01

    Newtonian fluid motion, coupled to heat transfer via latent heat of phase transition, is well known from numerous studies of condensation and boiling. Considerably less knowledge is available for vapor-liquid phase separation in the absence of gravity effect on the transport phenomena. The present studies are focused on heat and mass transfer associated with vapor-liquid phase separation required for long-term storage of the cryogen liquid He II in space vessels. Though space conditions are the dominant mode of interest in advanced equipment, e.g. IR telescopes, the systems may be operated in principle during terrestrial conditions. The latter are considered in the present work. It emphasizes the linear regime including an extrapolation based on variable thermophysical properties. Data taken with a phase separation approach show departures from the linear regime prediction. They agree with a transport equation proposed for the nonlinear, turbulent regime.

  8. Rapid, high-purity chemical separation of molybdenum from iron meteorites for isotopic analysis by using thermal ionization mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Qi-Lu; Masuda, Akimasa (Tokyo Univ. (Japan). Dept. of Chemistry)

    1992-05-01

    A chemical procedure has been developed, which combines both solvent extraction and anion exchange, so that microgram amounts of Mo can be cleanly, rapidly and efficiently separated from gram amounts of iron meteorites. Particular attention was directed to the complete separation of Mo from Zr and Ru. The isotopic abundance ratios of Mo can subsequently be determined with high accuracy by using thermal ionization mass spectrometry. The experiments indicate that the behaviour of Mo during solvent extraction and anion exchange is considerably different from that reported previously. In particular, it was found that there is a very narrow range of HCl concentrations within which it is possible to separate Mo from Fe by solvent extraction. The reproducibility and recovery of the method were examined by using inductively coupled plasma atomic emission spectrometry. (Author).

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

    CSIR Research Space (South Africa)

    Archer, M

    2003-12-01

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

  10. Normal phase liquid chromatography coupled to quadrupole time of flight atmospheric pressure chemical ionization mass spectrometry for separation, detection and mass spectrometric profiling of neutral sphingolipids and cholesterol.

    Science.gov (United States)

    Farwanah, Hany; Wirtz, Jennifer; Kolter, Thomas; Raith, Klaus; Neubert, Reinhard H H; Sandhoff, Konrad

    2009-10-01

    Many lipidomic approaches focus on investigating aspects of sphingolipid metabolism. Special emphasis is put on neutral sphingolipids and cholesterol and their interaction. Such an interest is attributed to the fact that those lipids are altered in a series of serious disorders including various sphingolipidoses. High performance thin-layer chromatography (HPTLC) has become a widely used technique for lipid analysis. However, mass spectrometric profiling is irreplaceable for gaining an overview about the various molecular species within a lipid class. In this work we have developed a sensitive method based on a gradient normal phase high performance liquid chromatography (HPLC) coupled to quadrupole time of flight (QTOF) atmospheric pressure chemical ionization mass spectrometry (APCI-MS) in positive mode, which for the first time enables separation, on-line detection, and mass spectrometric profiling of multiple neutral sphingolipids including ceramide, glucosylceramide, lactosylceramide, globotriaosylceramide, globotetraosylceramide, sphingomyelin as well as cholesterol within less than 15min. An important advantage of the presented HPLC/APCI-MS approach is that the separation pattern emulates the one obtained by an optimized HPTLC method with a multiple stage development. Thus, the lipid classes previously separated and quantified by HPTLC can be easily screened regarding their mass spectrometric profiles by HPLC/APCI-MS. In addition, the selected ionization conditions enable in-source fragmentation providing useful structural information. The methods (HPLC/APCI-MS and the optimized HPTLC) were applied for the analysis of the mentioned lipids in human fibroblasts. This approach is aimed basically at investigators who perform studies based on genetic modifications or treatment with pharmacological agents leading to changes in the biochemical pathways of neutral sphingolipids and cholesterol. In addition, it can be of interest for research on disorders related to

  11. A mass-balance model to separate and quantify colloidal and solute redistributions in soil

    Science.gov (United States)

    Bern, C.R.; Chadwick, O.A.; Hartshorn, A.S.; Khomo, L.M.; Chorover, J.

    2011-01-01

    Studies of weathering and pedogenesis have long used calculations based upon low solubility index elements to determine mass gains and losses in open systems. One of the questions currently unanswered in these settings is the degree to which mass is transferred in solution (solutes) versus suspension (colloids). Here we show that differential mobility of the low solubility, high field strength (HFS) elements Ti and Zr can trace colloidal redistribution, and we present a model for distinguishing between mass transfer in suspension and solution. The model is tested on a well-differentiated granitic catena located in Kruger National Park, South Africa. Ti and Zr ratios from parent material, soil and colloidal material are substituted into a mixing equation to quantify colloidal movement. The results show zones of both colloid removal and augmentation along the catena. Colloidal losses of 110kgm-2 (-5% relative to parent material) are calculated for one eluviated soil profile. A downslope illuviated profile has gained 169kgm-2 (10%) colloidal material. Elemental losses by mobilization in true solution are ubiquitous across the catena, even in zones of colloidal accumulation, and range from 1418kgm-2 (-46%) for an eluviated profile to 195kgm-2 (-23%) at the bottom of the catena. Quantification of simultaneous mass transfers in solution and suspension provide greater specificity on processes within soils and across hillslopes. Additionally, because colloids include both HFS and other elements, the ability to quantify their redistribution has implications for standard calculations of soil mass balances using such index elements. ?? 2011.

  12. First on-line applications of multi-reflection time-of-flight mass separator at ISOLTRAP and the mass measurement of $^{82}$Zn

    CERN Document Server

    Wolf, Robert

    This thesis describes the implementation and first on-line application of a multi-reflection time-of-flight (MR-ToF) mass analyzer for high-resolution mass separation at the ISOLTRAP mass spectrometer at ISOLDE/CERN. On the one hand, the major objective was to improve ISOLTRAPs mass-measurement capabilities with respect to the ratio of delivered contaminating ions to ions of interest. On the other hand, the time necessary to purify wanted from unwanted species should be reduced as much as possible to enable access to even more exotic nuclei. The device has been set up, optimized and tested at the University of Greifswald before its move to ISOLTRAP. The achieved performance comprises mass resolving powers of up to 200000 reached at observation times of 30ms and a contamination suppression of about four orders of magnitude by use of a Bradbury-Nielsen gate. With the characteristics, it outperforms clearly the so far state-of-the-art purification method of a gas-filled Penning trap. To improve the utilization o...

  13. Separation of VX, RVX and GB Enantiomers Using Liquid ChromatographyTime-of-Flight Mass Spectrometry

    Science.gov (United States)

    2016-02-01

    a bandwidth of 4 nm) was referenced to a wavelength of 360 nm. An Agilent series 1200 fraction collector (Agilent Technologies; Santa Clara, CA) was...phosphorus compounds have four  bonds arranged through sp3 hybrid orbitals as occurs in tetrahedral carbon compounds. The first enantiomeric phosphorus...1200 Infinity series fraction collector was configured using the peak- time-based collection protocol, and the separated enantiomers were combined into

  14. Diffusion induced phase separation with crystallizable nylons. I. Mass transfer processes for nylon 4,6

    NARCIS (Netherlands)

    Bulte, A.M.W.; Bulte, A.M.W.; Mulder, M.H.V.; Smolders, C.A.; Smolders, C.A.; Strathmann, H.

    1996-01-01

    Mass transfer during membrane formation by means of phase inversion for a polymeric system with both a solid-liquid and a liquid-liquid equilibrium was studied on the basis of the theory developed by Reuvers and Smolders. During the first moments of immersion in the coagulation bath, the concentrati

  15. First spatial separation of a heavy ion isomeric beam with a multiple-reflection time-of-flight mass spectrometer

    Directory of Open Access Journals (Sweden)

    T. Dickel

    2015-05-01

    Full Text Available 211Po ions in the ground and isomeric states were produced via 238U projectile fragmentation at 1000 MeV/u. The 211Po ions were spatially separated in flight from the primary beam and other reaction products by the fragment separator FRS. The ions were energy-bunched, slowed-down and thermalized in a gas-filled cryogenic stopping cell (CSC. They were then extracted from the CSC and injected into a high-resolution multiple-reflection time-of-flight mass spectrometer (MR-TOF-MS. The excitation energy of the isomer and, for the first time, the isomeric-to-ground state ratio were determined from the measured mass spectrum. In the subsequent experimental step, the isomers were spatially separated from the ions in the ground state by an ion deflector and finally collected with a silicon detector for decay spectroscopy. This pioneering experimental result opens up unique perspectives for isomer-resolved studies. With this versatile experimental method new isomers with half-lives longer than a few milliseconds can be discovered and their decay properties can be measured with highest sensitivity and selectivity. These experiments can be extended to studies with isomeric beams in nuclear reactions.

  16. First spatial separation of a heavy ion isomeric beam with a multiple-reflection time-of-flight mass spectrometer

    Energy Technology Data Exchange (ETDEWEB)

    Dickel, T. [II. Physikalisches Institut, Justus-Liebig-Universität Gießen, 35392 Gießen (Germany); GSI Helmholtzzentrum für Schwerionenforschung GmbH, 64291 Darmstadt (Germany); Plaß, W.R., E-mail: Wolfgang.R.Plass@exp2.physik.uni-giessen.de [II. Physikalisches Institut, Justus-Liebig-Universität Gießen, 35392 Gießen (Germany); GSI Helmholtzzentrum für Schwerionenforschung GmbH, 64291 Darmstadt (Germany); Ayet San Andres, S. [GSI Helmholtzzentrum für Schwerionenforschung GmbH, 64291 Darmstadt (Germany); Ebert, J. [II. Physikalisches Institut, Justus-Liebig-Universität Gießen, 35392 Gießen (Germany); Geissel, H.; Haettner, E. [II. Physikalisches Institut, Justus-Liebig-Universität Gießen, 35392 Gießen (Germany); GSI Helmholtzzentrum für Schwerionenforschung GmbH, 64291 Darmstadt (Germany); Hornung, C. [II. Physikalisches Institut, Justus-Liebig-Universität Gießen, 35392 Gießen (Germany); Miskun, I. [II. Physikalisches Institut, Justus-Liebig-Universität Gießen, 35392 Gießen (Germany); GSI Helmholtzzentrum für Schwerionenforschung GmbH, 64291 Darmstadt (Germany); Pietri, S.; Purushothaman, S. [GSI Helmholtzzentrum für Schwerionenforschung GmbH, 64291 Darmstadt (Germany); and others

    2015-05-11

    {sup 211}Po ions in the ground and isomeric states were produced via {sup 238}U projectile fragmentation at 1000 MeV/u. The {sup 211}Po ions were spatially separated in flight from the primary beam and other reaction products by the fragment separator FRS. The ions were energy-bunched, slowed-down and thermalized in a gas-filled cryogenic stopping cell (CSC). They were then extracted from the CSC and injected into a high-resolution multiple-reflection time-of-flight mass spectrometer (MR-TOF-MS). The excitation energy of the isomer and, for the first time, the isomeric-to-ground state ratio were determined from the measured mass spectrum. In the subsequent experimental step, the isomers were spatially separated from the ions in the ground state by an ion deflector and finally collected with a silicon detector for decay spectroscopy. This pioneering experimental result opens up unique perspectives for isomer-resolved studies. With this versatile experimental method new isomers with half-lives longer than a few milliseconds can be discovered and their decay properties can be measured with highest sensitivity and selectivity. These experiments can be extended to studies with isomeric beams in nuclear reactions.

  17. Energy-Resolved Ion Mobility-Mass Spectrometry—A Concept to Improve the Separation of Isomeric Carbohydrates

    Science.gov (United States)

    Hoffmann, Waldemar; Hofmann, Johanna; Pagel, Kevin

    2014-03-01

    Recent works using ion mobility-mass spectrometry (IM-MS) have highlighted the power of this instrumental configuration to tackle one of the greatest challenges in glycomics and glycoproteomics: the existence of isobaric isomers. For a successful separation of species with identical mass but different structure via IM-MS, it is crucial to have sufficient IM resolution. In commercially available IM-MS instruments, however, this resolution is limited by the design of the instrument and usually cannot be increased at-will without extensive modifications. Here, we present a systematic approach to improve the resolving capability of IM-MS instruments using so-called energy-resolved ion mobility-mass spectrometry. The technique utilizes the fact that individual components in an isobaric mixture fragment at considerably different energies when activated in the gas phase via collision-induced dissociation (CID). As a result, certain components can be suppressed selectively at increased CID activation energy. Using a mixture of four isobaric carbohydrates, we show that each of the individual sugars can be resolved and unambiguously identified even when their drift times differ by as little as 3 %. However, the presented results also indicate that a certain difference in the gas-phase stability of the individual components is crucial for a successful separation via energy-resolved IM-MS.

  18. Energy-resolved ion mobility-mass spectrometry--a concept to improve the separation of isomeric carbohydrates.

    Science.gov (United States)

    Hoffmann, Waldemar; Hofmann, Johanna; Pagel, Kevin

    2014-03-01

    Recent works using ion mobility-mass spectrometry (IM-MS) have highlighted the power of this instrumental configuration to tackle one of the greatest challenges in glycomics and glycoproteomics: the existence of isobaric isomers. For a successful separation of species with identical mass but different structure via IM-MS, it is crucial to have sufficient IM resolution. In commercially available IM-MS instruments, however, this resolution is limited by the design of the instrument and usually cannot be increased at-will without extensive modifications. Here, we present a systematic approach to improve the resolving capability of IM-MS instruments using so-called energy-resolved ion mobility-mass spectrometry. The technique utilizes the fact that individual components in an isobaric mixture fragment at considerably different energies when activated in the gas phase via collision-induced dissociation (CID). As a result, certain components can be suppressed selectively at increased CID activation energy. Using a mixture of four isobaric carbohydrates, we show that each of the individual sugars can be resolved and unambiguously identified even when their drift times differ by as little as 3%. However, the presented results also indicate that a certain difference in the gas-phase stability of the individual components is crucial for a successful separation via energy-resolved IM-MS.

  19. Searching for Scatterers: High-Contrast Imaging of Young Stars Hosting Wide-Separation Planetary-Mass Companions

    CERN Document Server

    Bryan, Marta L; Knutson, Heather A; Kraus, Adam L; Hinkley, Sasha; Mawet, Dimitri; Nielsen, Eric L; Blunt, Sarah C

    2016-01-01

    We have conducted an angular differential imaging survey with NIRC2 at Keck in search of close-in substellar companions to a sample of seven systems with confirmed planetary-mass companions (PMCs) on wide orbits (>50 AU). These wide-separation PMCs pose significant challenges to all three possible formation mechanisms: core accretion plus scattering, disk instability, and turbulent fragmentation. We explore the possibility that these companions formed closer in and were scattered out to their present-day locations by searching for other massive bodies at smaller separations. The typical sensitivity for this survey is \\Delta K ~ 12.5 at 1". We identify eight candidate companions, whose masses would reach as low as one Jupiter mass if gravitationally bound. From our multi-epoch astrometry we determine that seven of these are conclusively background objects, while the eighth near DH Tau is ambiguous and requires additional monitoring. We rule out the presence of >7 M$_{\\rm Jup}$ bodies in these systems down to 1...

  20. A miniature system for separating aerosol particles and measuring mass concentrations.

    Science.gov (United States)

    Liang, Dao; Shih, Wen-Pin; Chen, Chuin-Shan; Dai, Chi-An

    2010-01-01

    We designed and fabricated a new sensing system which consists of two virtual impactors and two quartz-crystal microbalance (QCM) sensors for measuring particle mass concentration and size distribution. The virtual impactors utilized different inertial forces of particles in air flow to classify different particle sizes. They were designed to classify particle diameter, d, into three different ranges: d3.20 μm. The QCM sensors were coated with a hydrogel, which was found to be a reliable adhesive for capturing aerosol particles. The QCM sensor coated with hydrogel was used to measure the mass loading of particles by utilizing its characteristic of resonant frequency shift. An integrated system has been demonstrated.

  1. A Miniature System for Separating Aerosol Particles and Measuring Mass Concentrations

    Directory of Open Access Journals (Sweden)

    Dao Liang

    2010-04-01

    Full Text Available We designed and fabricated a new sensing system which consists of two virtual impactors and two quartz-crystal microbalance (QCM sensors for measuring particle mass concentration and size distribution. The virtual impactors utilized different inertial forces of particles in air flow to classify different particle sizes. They were designed to classify particle diameter, d, into three different ranges: d < 2.28 μm, 2.28 μm ≤ d ≤ 3.20 μm, d > 3.20 μm. The QCM sensors were coated with a hydrogel, which was found to be a reliable adhesive for capturing aerosol particles. The QCM sensor coated with hydrogel was used to measure the mass loading of particles by utilizing its characteristic of resonant frequency shift. An integrated system has been demonstrated.

  2. Isotope-Dilution Mass Spectrometry for Quantification of Urinary Active Androgens Separated by Gas Chromatography

    OpenAIRE

    Su Hyeon Lee; Man Ho Choi; Won-Yong Lee; Bong Chul Chung

    2010-01-01

    Cross reacting antibodies can cause an overestimation of the results of immunoassays. Therefore, alternative methodsare needed for the accurate quantification of steroids. Gas chromatography combined with isotope-dilution mass spectrometry(GC-IDMS) is developed to quantify urinary active androgens, testosterone, epitestosterone and dihydrotestosterone, which areclinically relevant androgens to both hair-loss and prostate diseases. The method devised involves enzymatic hydrolysis with β-glucur...

  3. The control system of the CERN-ISOLDE on-line mass-separator facility

    Energy Technology Data Exchange (ETDEWEB)

    Jonsson, O.C.; Bret, A.; Catherall, R.; Deloose, I.; Focker, G.J.; Forkel, D.; Kugler, E.; Olesen, G.; Pace, A.; Ravn, H.L.; Shering, G.; Tengblad, O. (CERN, Geneva (Switzerland)); Borch, O. (Aalborg Univ. (Denmark). Inst. of Electronic Systems); Richard-Serre, C. (IN2P3, 75 - Paris (France)); Torgersen, H.J. (Oslo Univ. (Norway). Dept. of Chemistry); ISOLDE Collaboration

    1992-08-01

    With the move of the ISOLDE facility to the PS-Booster from the now closed Synchro-Cyclotron at CERN, a new control system will be implented for the two separators. Personal computers, based on the Intel 80386 microprocessor running under MS-DOS and Microsoft Windows, are used. Network-wide distributed front end computers, which access the hardware for controls and measurements, are controlled by PC-consoles via a local area network with a PC file server used as a database. (orig.).

  4. The control system of the CERN-ISOLDE on-line mass-separator facility

    Science.gov (United States)

    Jonsson, O. C.; Borch, O.; Bret, A.; Catherall, R.; Deloose, I.; Focker, G. J.; Forkel, D.; Kugler, E.; Olesen, G.; Pace, A.; Ravn, H. L.; Richard-Serre, C.; Shering, G.; Tengblad, O.; Torgersen, H. J.; Isolde Collaboration

    1992-08-01

    With the move of the ISOLDE facility to the PS-Booster from the now closed Synchro-Cyclotron at CERN, a new control system will be implemented for the two separators. Personal computers, based on the Intel 80386 microprocessor running under MS-DOS and Microsoft Windows, are used. Network-wide distributed front end computers, which access the hardware for controls and measurements, are controlled by PC-consoles via a local area network with a PC file server used as a database.

  5. Ion Mobility Separations of Isomers based upon Long Path Length Structures for Lossless Ion Manipulations Combined with Mass Spectrometry.

    Science.gov (United States)

    Deng, Liulin; Ibrahim, Yehia M; Baker, Erin S; Aly, Noor A; Hamid, Ahmed M; Zhang, Xing; Zheng, Xueyun; Garimella, Sandilya V B; Webb, Ian K; Prost, Spencer A; Sandoval, Jeremy A; Norheim, Randolph V; Anderson, Gordon A; Tolmachev, Aleksey V; Smith, Richard D

    2016-07-01

    Mass spectrometry (MS)-based multi-omic measurements, including proteomics, metabolomics, lipidomics, and glycomics, are increasingly transforming our ability to characterize and understand biological systems. Multi-omic analyses and the desire for comprehensive measurement coverage presently have limitations due to the chemical diversity and range of abundances of biomolecules in complex samples. Advances addressing these challenges increasingly are based upon the ability to quickly separate, react and otherwise manipulate sample components for analysis by MS. Here we report on a new approach using Structures for Lossless Ion Manipulations (SLIM) to enable long serpentine path ion mobility spectrometry (IMS) separations followed by MS analyses. This approach provides previously unachieved resolution for biomolecular species, in conjunction with more effective ion utilization, and a basis for greatly improved characterization of very small sample sizes.

  6. Formation of residual nuclei with medium mass number in the reaction of protons with separated tin isotopes

    CERN Document Server

    Aleksandryan, V E; Balabekyan, A R; Danagulyan, A S; Kalinnikov, V G; Musulmanbekov, G; Rodionov, V K; Stegailov, V I; Frana, J

    2000-01-01

    The mechanism of formation of residual nuclei in the mass region 42<=A<=81 in the reactions of protons with separated tin isotopes at three protons energies 0.66, 1.0 and 8.1 GeV was investigated. The absolute cross-sections of the residual nuclei were compared with the theoretical ones calculated by the standard cascade-evaporation and the intranuclear cascad plus statistical multifragmentation models (INC+SMM). It was shown that at E sub p =8.1 GeV these nuclei may arise both from disintegration of the nucleus and as partners of several fragments.

  7. Enhancement of biological mass spectrometry by using separations based on changes in ion mobility (FAIMS and DMS).

    Science.gov (United States)

    Purves, Randy W

    2013-01-01

    Analysis of complex biological samples for low-level analytes by liquid chromatography-tandem mass spectrometry (LC-MS/MS) often requires additional selectivity. Differential mobility techniques (FAIMS and DMS) have been shown to enhance LC-MS/MS analyses by separating ions in the gas-phase on a millisecond timescale by use of a mechanism that is complementary to both liquid chromatography and mass spectrometry. In this overview, a simplified description of the operation of these devices is given and an example presented that illustrates the utility of FAIMS (DMS) for solving a challenging analytical assay. Important recent advances in the field, including work with gas modifiers, are presented, along with an outlook for the technology.

  8. Broad Separation of Isomeric Lipids by High-Resolution Differential Ion Mobility Spectrometry with Tandem Mass Spectrometry

    Science.gov (United States)

    Bowman, Andrew P.; Abzalimov, Rinat R.; Shvartsburg, Alexandre A.

    2017-08-01

    Maturation of metabolomics has brought a deeper appreciation for the importance of isomeric identity of lipids to their biological role, mirroring that for proteoforms in proteomics. However, full characterization of the lipid isomerism has been thwarted by paucity of rapid and effective analytical tools. A novel approach is ion mobility spectrometry (IMS) and particularly differential or field asymmetric waveform IMS (FAIMS) at high electric fields, which is more orthogonal to mass spectrometry. Here we broadly explore the power of FAIMS to separate lipid isomers, and find a 75% success rate across the four major types of glycero- and phospho- lipids ( sn, chain length, double bond position, and cis/ trans). The resolved isomers were identified using standards, and (for the first two types) tandem mass spectrometry. These results demonstrate the general merit of incorporating high-resolution FAIMS into lipidomic analyses.

  9. Electrophoretic separation techniques and their hyphenation to mass spectrometry in biological inorganic chemistry.

    Science.gov (United States)

    Holtkamp, Hannah; Grabmann, Gerlinde; Hartinger, Christian G

    2016-04-01

    Electrophoretic methods have been widely applied in research on the roles of metal complexes in biological systems. In particular, CE, often hyphenated to a sensitive MS detector, has provided valuable information on the modes of action of metal-based pharmaceuticals, and more recently new methods have been added to the electrophoretic toolbox. The range of applications continues to expand as a result of enhanced CE-to-MS interfacing, with sensitivity often at picomolar level, and evolved separation modes allowing for innovative sample analysis. This article is a followup to previous reviews about CE methods in metallodrug research (Electrophoresis, 2003, 24, 2023-2037; Electrophoresis, 2007, 28, 3436-3446; Electrophoresis, 2012, 33, 622-634), also providing a comprehensive overview of metal species studied by electrophoretic methods hyphenated to MS. It highlights the latest CE developments, takes a sneak peek into gel electrophoresis, traces biomolecule labeling, and focuses on the importance of early-stage drug development.

  10. On the implications of aerosol liquid water and phase separation for organic aerosol mass

    Science.gov (United States)

    Pye, Havala O. T.; Murphy, Benjamin N.; Xu, Lu; Ng, Nga L.; Carlton, Annmarie G.; Guo, Hongyu; Weber, Rodney; Vasilakos, Petros; Wyat Appel, K.; Hapsari Budisulistiorini, Sri; Surratt, Jason D.; Nenes, Athanasios; Hu, Weiwei; Jimenez, Jose L.; Isaacman-VanWertz, Gabriel; Misztal, Pawel K.; Goldstein, Allen H.

    2017-01-01

    Organic compounds and liquid water are major aerosol constituents in the southeast United States (SE US). Water associated with inorganic constituents (inorganic water) can contribute to the partitioning medium for organic aerosol when relative humidities or organic matter to organic carbon (OM / OC) ratios are high such that separation relative humidities (SRH) are below the ambient relative humidity (RH). As OM / OC ratios in the SE US are often between 1.8 and 2.2, organic aerosol experiences both mixing with inorganic water and separation from it. Regional chemical transport model simulations including inorganic water (but excluding water uptake by organic compounds) in the partitioning medium for secondary organic aerosol (SOA) when RH > SRH led to increased SOA concentrations, particularly at night. Water uptake to the organic phase resulted in even greater SOA concentrations as a result of a positive feedback in which water uptake increased SOA, which further increased aerosol water and organic aerosol. Aerosol properties, such as the OM / OC and hygroscopicity parameter (κorg), were captured well by the model compared with measurements during the Southern Oxidant and Aerosol Study (SOAS) 2013. Organic nitrates from monoterpene oxidation were predicted to be the least water-soluble semivolatile species in the model, but most biogenically derived semivolatile species in the Community Multiscale Air Quality (CMAQ) model were highly water soluble and expected to contribute to water-soluble organic carbon (WSOC). Organic aerosol and SOA precursors were abundant at night, but additional improvements in daytime organic aerosol are needed to close the model-measurement gap. When taking into account deviations from ideality, including both inorganic (when RH > SRH) and organic water in the organic partitioning medium reduced the mean bias in SOA for routine monitoring networks and improved model performance compared to observations from SOAS. Property updates from

  11. Potential of Solid Sampling Electrothermal Vaporization for solving spectral interference in Inductively Coupled Plasma Optical Emission Spectrometry

    Science.gov (United States)

    Asfaw, Alemayehu; Wibetoe, Grethe

    2009-05-01

    Spectral interference is one of the main causes of erroneous results in Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES). This paper describes some cases of spectral interferences with conventional nebulization ICP-OES and the potential of solving them utilizing electrothermal vaporization for volatility-based separation. The cases studied were, the well-known spectral overlap between the As and Cd lines at 228.8 nm that are only 10 pm apart, and the interference of Fe on the main emission lines of As, Cd and Pb. The spectral interferences were studied by monitoring the typical signals of solutions that contain the analytes and the potential interferent, by studying the spectra and calculating Background Equivalent Concentration (BEC)-values. A three step temperature program was developed to be used for direct analysis of solid soil samples by Electrothermal Vaporization (ETV)-ICP-OES: step 1 (760 °C, 40 s), step 2 (1620 °C, 20 s) and a cleaning step (2250 °C, 10 s) where Cd vaporizes in step 1, As, Pb and part of Fe in step 2 and the major part of Fe in the cleaning step. Because As and Cd were time-separated using this program, their prominent lines at 228.8 nm, could be used for determination of each element by ETV-ICP-OES, in spite of the serious wavelength overlap. Selective vaporization was also shown to reduce or eliminate the Fe background emission on As, Cd and Pb lines. To confirm the applicability of the method, a solid soil certified reference materials was analyzed directly without any sample treatment. Good or reasonable accuracy was obtained for the three elements.

  12. Inductively Coupled Plasma Optical-Emission Spectroscopy Determination of Major and Minor Elements in Vinegar

    Directory of Open Access Journals (Sweden)

    Arzu AKPINAR-BAYIZIT

    2010-12-01

    Full Text Available This study characterizes the mineral content of vinegar samples. The concentrations of Na, K, Ca, Mg and P (major elements as well as Fe, Mn, Sn, Cu, Ni, Zn, Pb and Cd (minor elements were determined in 35 commercial vinegar samples using inductively coupled plasma optical-emission spectrometry (ICP-OES. The elements with the highest concentrations were K, Na, Ca, Mg and P. The concentrations of heavy metals in the vinegar samples, including Cd, Ni, Sn and Pb, were not considered a health risk.

  13. Ricin as a weapon of mass terror--separating fact from fiction.

    Science.gov (United States)

    Schep, Leo J; Temple, Wayne A; Butt, Grant A; Beasley, Michael D

    2009-11-01

    In recent years there has been an increased concern regarding the potential use of chemical and biological weapons for mass urban terror. In particular, there are concerns that ricin could be employed as such an agent. This has been reinforced by recent high profile cases involving ricin, and its use during the cold war to assassinate a high profile communist dissident. Nevertheless, despite these events, does it deserve such a reputation? Ricin is clearly toxic, though its level of risk depends on the route of entry. By ingestion, the pathology of ricin is largely restricted to the gastrointestinal tract where it may cause mucosal injuries; with appropriate treatment, most patients will make a full recovery. As an agent of terror, it could be used to contaminate an urban water supply, with the intent of causing lethality in a large urban population. However, a substantial mass of pure ricin powder would be required. Such an exercise would be impossible to achieve covertly and would not guarantee success due to variables such as reticulation management, chlorination, mixing, bacterial degradation and ultra-violet light. By injection, ricin is lethal; however, while parenteral delivery is an ideal route for assassination, it is not realistic for an urban population. Dermal absorption of ricin has not been demonstrated. Ricin is also lethal by inhalation. Low doses can lead to progressive and diffuse pulmonary oedema with associated inflammation and necrosis of the alveolar pneumocytes. However, the risk of toxicity is dependent on the aerodynamic equivalent diameter (AED) of the ricin particles. The AED, which is an indicator of the aerodynamic behaviour of a particle, must be of sufficiently low micron size as to target the human alveoli and thereby cause major toxic effects. To target a large population would also necessitate a quantity of powder in excess of several metric tons. The technical and logistical skills required to formulate such a mass of powder to

  14. Analytical methods for proteome data obtained from SDS-PAGE multi-dimensional separation and mass spectrometry

    Directory of Open Access Journals (Sweden)

    Gun Wook Park

    2010-03-01

    Full Text Available For proteome analysis, various experimental protocols using mass spectrometry have been developed over thelast decade. The different protocols have differing performances and degrees of accuracy. Furthermore, the “best”protocol for a proteomic analysis of a sample depends on the purpose of the analysis, especially in connection withdisease proteomics, including biomarker discovery and therapeutics analyses of human serum or plasma. Theprotein complexity and the wide dynamic range of blood samples require high-dimensional separation technology.In this article, we review proteome analysis protocols in which both Sodium Dodecyl Sulfate-Polyacryl Amide GelElectrophoresis(SDS-PAGE and liquid chromatography are used for peptide and protein separations. Multidimensionalseparation technology supplies a high-quality dataset of tandem mass spectra and reveals signals fromlow-abundance proteins, although it can be time-consuming and laborious work. We survey shotgun proteomicsprotocols using SDS-PAGE and liquid chromatography and introduce bioinformatics tools for the analysis ofproteomics data. We also review efforts toward the biological interpretation of the proteome.

  15. Design of a single magnet separator with mass resolving power m/Δm ≈ 20, 000

    Science.gov (United States)

    Breitenfeldt, Martin; Augustin, Mathieu; Catherall, Richard; Giles, Tim; Schoerling, Daniel; Tveten, Gry M.

    2016-06-01

    ISOLDE at CERN is a leading radioactive ion beam facility. With its upgrade, the HIE-ISOLDE project, an increase in primary beam intensity and energy is envisaged and the aim is a significant increase in intensity of the exotic beams. The high resolution separator (HRS) after the upgrade is required to suppress contaminations almost completely when the masses differ to the beam of interest by Δm / m > 1 / 20, 000 . Here a 120° magnet with a bending radius of 1.25 m has been chosen. The magnetic rigidity is 0.625 Tm (B-field of 0.5 T) to allow for separation of molecules of up to a mass of 300 u. The magnet comprises a yoke in wedged H-type configuration for stability and precision and pole face conductors for focusing and compensation of aberrations. The concept was derived analytically, refined with the OPERA 2D software and tested with the ray-tracing module of OPERA 3D.

  16. Proteomic analysis of estrogen response of premalignant human breast cells using a 2-D liquid separation/mass mapping technique.

    Science.gov (United States)

    Zhao, Jia; Zhu, Kan; Lubman, David M; Miller, Fred R; Shekhar, Malthy P V; Gerard, Brigitte; Barder, Timothy J

    2006-07-01

    A 2-D liquid-phase separation method based on chromatofocusing and nonporous silica RP-HPLC followed by ESI-TOF-MS was used to analyze proteins in whole cell lysates from estrogen-treated and untreated premalignant, estrogen-responsive cell line MCF10AT1 cells. 2-D mass maps in the pH range 4.6-6.0 were generated with good correlation to theoretical M(r) values for intact proteins. Proteins were identified based on intact M(r), pI and PMF, or MS/MS sequencing. About 300 unique proteins were identified and 120 proteins in mass range 5-75 kDa were quantified upon treatment of estrogen. Around 40 proteins were found to be more highly expressed (>four-fold) and 17 were down-regulated (>four-fold) in treated cells. In our study, we found that many altered proteins have characteristics consistent with the development of a malignant phenotype. Some of them have a role in the ras pathway or play an important role in signal pathways. These changed proteins might be essential in the estrogen regulation mechanism. Our study highlights the use of the MCF10AT1 cell line to examine estrogen-induced changes in premalignant breast cells and the ability of the 2-D mass mapping technique to quantitatively study protein expression changes on a proteomic scale.

  17. Design and commissioning of a timestamp-based data acquisition system for the DRAGON recoil mass separator

    CERN Document Server

    Christian, G; Connolly, D; Fallis, J; Hutcheon, D; Olchanski, K; Ruiz, C

    2014-01-01

    The DRAGON recoil mass separator at TRIUMF exists to study radiative proton and alpha capture reactions, which are important in a variety of astrophysical scenarios. DRAGON experiments require a data acquisition system that can be triggered on either reaction product ($\\gamma$ ray or heavy ion), with the additional requirement of being able to promptly recognize coincidence events in an online environment. To this end, we have designed and implemented a new data acquisition system for DRAGON which consists of two independently triggered readouts. Events from both systems are recorded with timestamps from a $20$ MHz clock that are used to tag coincidences in the earliest possible stage of the data analysis. Here we report on the design, implementation, and commissioning of the new DRAGON data acquisition system, including the hardware, trigger logic, coincidence reconstruction algorithm, and live time considerations. We also discuss the results of an experiment commissioning the new system, which measured the ...

  18. Comprehensive ultra-performance liquid chromatographic separation and mass spectrometric analysis of eicosanoid metabolites in human samples.

    Science.gov (United States)

    Wang, Yan; Armando, Aaron M; Quehenberger, Oswald; Yan, Chao; Dennis, Edward A

    2014-09-12

    Over the past decade, the number of known eicosanoids has expanded immensely and we have now developed an ultra-performance liquid chromatography-electrospray ionization triple quadrupole mass spectrometric (UPLC-QTRAP/MS/MS) method to monitor and quantify numerous eicosanoids. The UPLC-QTRAP/MS/MS approach utilizes scheduled multiple reaction monitoring (MRM) to optimize sensitivity, number of metabolites that can be analyzed and the time requirement of the analysis. A total of 184 eicosanoids including 26 deuterated internal standards can be separated and monitored in a single 5min UPLC run. To demonstrate a practical application, human plasma samples were analyzed following solid-phase extraction (SPE) and the recovery rate and matrix effects were determined for the 26 deuterated internal standards added to the plasma. The method was validated and shown to be sensitive with the limit of quantitation at pg levels for most compounds, accurate with recovery rates of 70-120%, and precise with a CVeicosanoids.

  19. Quantitative Mass spectrometric Analysis of Ropivacaine and Bupivacaine in Authentic, Pharmaceutical and Spiked Human Plasma without Chromatographic Separation

    Directory of Open Access Journals (Sweden)

    Nahla N. Salama

    2009-01-01

    Full Text Available The present study employs time of flight mass spectrometry for quantitative analysis of the local anesthetic drugs ropivacaine and bupivacaine in authentic, pharmaceutical and spiked human plasma as well as in the presence of their impurities 2,6-dimethylaniline and alkaline degradation product. The method is based on time of flight electron spray ionization mass spectrometry technique without preliminary chromatographic separation and makes use of bupivacaine as internal standard for ropivacaine, which is used as internal standard for bupivacaine. A linear relationship between drug concentrations and the peak intensity ratio of ions of the analyzed substances is established. The method is linear from 23.8 to 2380.0 ng mL-1 for both drugs. The correlation coefficient was ≥0.996 in authentic and spiked human plasma. The average percentage recoveries in the ranges of 95.39%–102.75% was obtained. The method is accurate (% RE < 5% and reproducible with intra- and inter-assay precision (RSD% < 8.0%. The quantification limit is 23.8 ng mL-1 for both drugs. The method is not only highly sensitive and selective, but also simple and effective for determination or identification of both drugs in authentic and biological fluids. The method can be applied in purity testing, quality control and stability monitoring for the studied drugs.

  20. Solvent Separating Secondary Metabolites Directly from Biosynthetic Tissue for Surface-Assisted Laser Desorption Ionisation Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    David Rudd

    2015-03-01

    Full Text Available Marine bioactive metabolites are often heterogeneously expressed in tissues both spatially and over time. Therefore, traditional solvent extraction methods benefit from an understanding of the in situ sites of biosynthesis and storage to deal with heterogeneity and maximize yield. Recently, surface-assisted mass spectrometry (MS methods namely nanostructure-assisted laser desorption ionisation (NALDI and desorption ionisation on porous silicon (DIOS surfaces have been developed to enable the direct detection of low molecular weight metabolites. Since direct tissue NALDI-MS or DIOS-MS produce complex spectra due to the wide variety of other metabolites and fragments present in the low mass range, we report here the use of “on surface” solvent separation directly from mollusc tissue onto nanostructured surfaces for MS analysis, as a mechanism for simplifying data annotation and detecting possible artefacts from compound delocalization during the preparative steps. Water, ethanol, chloroform and hexane selectively extracted a range of choline esters, brominated indoles and lipids from Dicathais orbita hypobranchial tissue imprints. These compounds could be quantified on the nanostructured surfaces by comparison to standard curves generated from the pure compounds. Surface-assisted MS could have broad utility for detecting a broad range of secondary metabolites in complex marine tissue samples.

  1. Optimal hydrograph separation using a recursive digital filter constrained by chemical mass balance, with application to selected Chesapeake Bay watersheds

    Science.gov (United States)

    Raffensperger, Jeff P.; Baker, Anna C.; Blomquist, Joel D.; Hopple, Jessica A.

    2017-06-26

    Quantitative estimates of base flow are necessary to address questions concerning the vulnerability and response of the Nation’s water supply to natural and human-induced change in environmental conditions. An objective of the U.S. Geological Survey National Water-Quality Assessment Project is to determine how hydrologic systems are affected by watershed characteristics, including land use, land cover, water use, climate, and natural characteristics (geology, soil type, and topography). An important component of any hydrologic system is base flow, generally described as the part of streamflow that is sustained between precipitation events, fed to stream channels by delayed (usually subsurface) pathways, and more specifically as the volumetric discharge of water, estimated at a measurement site or gage at the watershed scale, which represents groundwater that discharges directly or indirectly to stream reaches and is then routed to the measurement point.Hydrograph separation using a recursive digital filter was applied to 225 sites in the Chesapeake Bay watershed. The recursive digital filter was chosen for the following reasons: it is based in part on the assumption that groundwater acts as a linear reservoir, and so has a physical basis; it has only two adjustable parameters (alpha, obtained directly from recession analysis, and beta, the maximum value of the base-flow index that can be modeled by the filter), which can be determined objectively and with the same physical basis of groundwater reservoir linearity, or that can be optimized by applying a chemical-mass-balance constraint. Base-flow estimates from the recursive digital filter were compared with those from five other hydrograph-separation methods with respect to two metrics: the long-term average fraction of streamflow that is base flow, or base-flow index, and the fraction of days where streamflow is entirely base flow. There was generally good correlation between the methods, with some biased

  2. Trace elemental composition of curry by inductively coupled plasma optical emission spectrometry (ICP-OES).

    Science.gov (United States)

    Gonzálvez, A; Armenta, S; De La Guardia, M

    2008-01-01

    A methodology based on inductively coupled plasma optical emission spectrometry (ICP-OES) after microwave-assisted acid digestion was developed to determine the content of traces elements in curry samples from the Spanish market. The methodology was validated in terms of accuracy by the analysis of citrus and tomato leaf reference materials achieving comparable results with the certified values. The trace metal content of curry samples was compared with data available from previously published reports concerning Indian samples, especially in terms of heavy metal composition, in order to guarantee the quality of the commercially available spices in the European countries. Values found for the analysis of arsenic, lead and cadmium were significantly lower than the maximum limit allowed by European Union statutory limits for heavy metals and lower than those obtained for Indian curry leaves reported by Indian research teams by using neutron activation and γ-ray analysis.

  3. Inductively coupled plasma optical emission spectroscopy determination of trace element composition of argan oil.

    Science.gov (United States)

    Gonzálvez, A; Ghanjaoui, M E; El Rhazi, M; de la Guardia, M

    2010-02-01

    A methodology based on inductively coupled plasma optical emission spectroscopy (ICP-OES) after microwave assisted acid digestion has been developed to determine the trace element content of Moroccan argan oil. Limit of detection values equal or lower than few mg/kg were obtained for all elements under study. To assure the accuracy of the whole procedure, recovery studies were carried out on argan oil samples spiked at different concentration levels from 10 to 200 µg/L. Quantitative average recovery values were obtained for all elements evaluated, demonstrating the suitability of this methodology for the determination of trace elements in argan oil samples. Aluminum, calcium, chromium, iron, potassium, lithium, magnesium, sodium, vanadium and zinc were quantitatively determined in Moroccan argan oils being found that their concentration is different of that found in other edible oils thus offering a way for authentication and for the evaluation of possible adulterations.

  4. Relativistic plasma optics enabled by near-critical density nanostructured material

    CERN Document Server

    Bin, J H; Wang, H Y; Streeter, M J V; Kreuzer, C; Kiefer, D; Yeung, M; Cousens, S; Foster, P S; Dromey, B; Yan, X Q; Meyer-ter-Vehn, J; Zepf, M; Schreiber, J

    2014-01-01

    The nonlinear optical properties of a plasma due to the relativistic electron motion in an intense laser field are of fundamental importance for current research and the generation of brilliant laser-driven sources of particles and photons1-15. Yet, one of the most interesting regimes, where the frequency of the laser becomes resonant with the plasma, has remained experimentally hard to access. We overcome this limitation by utilizing ultrathin carbon nanotube foam16 (CNF) targets allowing the strong relativistic nonlinearities at near- critical density (NCD) to be exploited for the first time. We report on the experimental realization of relativistic plasma optics to spatio-temporally compress the laser pulse within a few micrometers of propagation, while maintaining about half its energy. We also apply the enhanced laser pulses to substantially improve the properties of an ion bunch accelerated from a secondary target. Our results provide first insights into the rich physics of NCD plasmas and the opportuni...

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

    Science.gov (United States)

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

    2014-01-01

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

  6. Automatically Detecting and Tracking Coronal Mass Ejections. I. Separation of Dynamic and Quiescent Components in Coronagraph Images

    Science.gov (United States)

    Morgan, Huw; Byrne, Jason P.; Habbal, Shadia Rifai

    2012-06-01

    Automated techniques for detecting and tracking coronal mass ejections (CMEs) in coronagraph data are of ever increasing importance for space weather monitoring and forecasting. They serve to remove the biases and tedium of human interpretation, and provide the robust analysis necessary for statistical studies across large numbers of observations. An important requirement in their operation is that they satisfactorily distinguish the CME structure from the background quiescent coronal structure (streamers, coronal holes). Many studies resort to some form of time differencing to achieve this, despite the errors inherent in such an approach—notably spatiotemporal crosstalk. This article describes a new deconvolution technique that separates coronagraph images into quiescent and dynamic components. A set of synthetic observations made from a sophisticated model corona and CME demonstrates the validity and effectiveness of the technique in isolating the CME signal. Applied to observations by the LASCO C2 and C3 coronagraphs, the structure of a faint CME is revealed in detail despite the presence of background streamers that are several times brighter than the CME. The technique is also demonstrated to work on SECCHI/COR2 data, and new possibilities for estimating the three-dimensional structure of CMEs using the multiple viewing angles are discussed. Although quiescent coronal structures and CMEs are intrinsically linked, and although their interaction is an unavoidable source of error in any separation process, we show in a companion paper that the deconvolution approach outlined here is a robust and accurate method for rigorous CME analysis. Such an approach is a prerequisite to the higher-level detection and classification of CME structure and kinematics.

  7. Conception of PIPERADE: A high-capacity Penning-trap mass separator for high isobaric contamination at DESIR

    Energy Technology Data Exchange (ETDEWEB)

    Minaya Ramirez, E., E-mail: minaya@ipno.in2p3.fr [Max-Planck-Institut für Kernphysik, 69117 Heidelberg (Germany); Alfaurt, P.; Aouadi, M.; Ascher, P.; Blank, B. [Centre d’Etudes Nucléaires de Bordeaux-Gradignan (France); Blaum, K. [Max-Planck-Institut für Kernphysik, 69117 Heidelberg (Germany); Cam, J.-F. [Laboratoire de Physique Corpusculaire, Caen (France); Chauveau, P. [Grand Accélérateur National d’Ions Lourds CEA/DSM-CNRS-IN2P3, Caen (France); Daudin, L. [Centre d’Etudes Nucléaires de Bordeaux-Gradignan (France); Delahaye, P. [Grand Accélérateur National d’Ions Lourds CEA/DSM-CNRS-IN2P3, Caen (France); Delalee, F. [Centre d’Etudes Nucléaires de Bordeaux-Gradignan (France); Dupré, P. [Centre de Sciences Nucléaires et de Sciences de la Matière, Orsay (France); El Abbeir, S.; Gerbaux, M.; Grévy, S.; Guérin, H. [Centre d’Etudes Nucléaires de Bordeaux-Gradignan (France); Lunney, D. [Centre de Sciences Nucléaires et de Sciences de la Matière, Orsay (France); Metz, F. [Max-Planck-Institut für Kernphysik, 69117 Heidelberg (Germany); Naimi, S. [Riken, 2-1 Hirosawa, Wako, Saitama 351-0198 (Japan); Perrot, L. [Institut de Physique Nucléaire, Orsay (France); and others

    2016-06-01

    The DESIR (decay, excitation and storage of radioactive ions) facility at GANIL-SPIRAL2 will receive a large variety of exotic nuclei at low energy (up to 60 keV) with high intensities. However, the production methods of radioactive beams are non selective, limiting the purity of the beams of interest. Moreover, the high precision needed for nuclear structure and astrophysics studies using beta decay spectroscopy, laser spectroscopy and trap-based experiments at DESIR requires highly pure samples of exotic nuclei. The aim of the double-Pennig-trap mass separator PIPERADE is to deliver large and very pure samples of exotic nuclei to the different experiments in DESIR. New excitation schemes and a large inner diameter of the first trap will mitigate space charge effects to attempt trapping of up to 10{sup 5} ions per pulse. The purification cycle will be performed in a few milliseconds so that short-lived nuclei can be purified. To extract the nuclides of interest from the large amount of isobaric contaminants, a resolving power of 10{sup 5} is mandatory. Afterwards the ions of interest will be accumulated in the second trap until they constitute a sufficiently pure sample for the measurements. The status of the project is presented.

  8. Enhancing glycan isomer separations with metal ions and positive and negative polarity ion mobility spectrometry-mass spectrometry analyses

    Energy Technology Data Exchange (ETDEWEB)

    Zheng, Xueyun; Zhang, Xing; Schocker, Nathaniel S.; Renslow, Ryan S.; Orton, Daniel J.; Khamsi, Jamal; Ashmus, Roger A.; Almeida, Igor C.; Tang, Keqi; Costello, Catherine E.; Smith, Richard D.; Michael, Katja; Baker, Erin S.

    2016-09-07

    Glycomics has become an increasingly important field of research since glycans play critical roles in biology processes ranging from molecular recognition and signaling to cellular communication. Glycans often conjugate with other biomolecules such as proteins and lipids, and alter their properties and functions, so understanding the effect glycans have on cellular systems is essential. However the analysis of glycans is extremely difficult due to their complexity and structural diversity (i.e., the number and identity of monomer units, and configuration of their glycosidic linkages and connectivities). In this work, we coupled ion mobility spectrometry with mass spectrometry (IMS-MS) to characterize glycan standards and biologically important isomers of synthetic αGal-containing O-glycans including glycotopes of the protozoan parasite Trypanosoma cruzi, which is the causative agent of Chagas disease. IMS-MS results showed significant differences for the glycan structural isomers when analyzed in positive and negative polarity and complexed with different metal cations. These results suggest specific metal ions or ion polarities could be used to target and baseline separate glycan isomers of interest with IMS-MS.

  9. Combined Reversed Phase HPLC, Mass Spectrometry, and NMR Spectroscopy for a Fast Separation and Efficient Identification of Phosphatidylcholines

    Directory of Open Access Journals (Sweden)

    Jan Willmann

    2011-01-01

    Full Text Available In respect of the manifold involvement of lipids in biochemical processes, the analysis of intact and underivatised lipids of body fluids as well as cell and tissue extracts is still a challenging task, if detailed molecular information is required. Therefore, the advantage of combined use of high-pressure liquid chromatography (HPLC, mass spectrometry (MS, and nuclear magnetic resonance (NMR spectroscopy will be shown analyzing three different types of extracts of the ubiquitous membrane component phosphatidylcholine. At first, different reversed phase modifications were tested on phosphatidylcholines (PC with the same effective carbon number (ECN for their applicability in lipid analysis. The results were taken to improve the separation of three natural PC extract types and a new reversed phase (RP-HPLC method was developed. The individual species were characterized by one- and two-dimensional NMR and positive or negative ion mode quadrupole time of flight (q-TOF-MS as well as MS/MS techniques. Furthermore, ion suppression effects during electrospray ionisation (ESI, difficulties, limits, and advantages of the individual analytical techniques are addressed.

  10. Direct determination of melamine in dairy products by gas chromatography/mass spectrometry with coupled column separation

    Energy Technology Data Exchange (ETDEWEB)

    Xu Xiaomin [Department of Chemistry, Xixi Campus, Zhejiang University, Hangzhou, 310028 (China); Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou, 310051 (China); Ren Yiping [Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou, 310051 (China); Zhu Yun [Xinjiang Uygur Autonomous Region Center for Disease Control and Prevention, Urumchi, 830002 (China); Cai Zengxuan; Han Jianlong; Huang Baifen [Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou, 310051 (China); Zhu Yan, E-mail: zhuyan@zju.edu.cn [Department of Chemistry, Xixi Campus, Zhejiang University, Hangzhou, 310028 (China)

    2009-09-14

    A coupled capillary column system was developed for the qualitative and quantitative determination of melamine with isotope internal standard in dairy products by gas chromatography/mass spectrometry (GC/MS) without derivatization. A 30 m of DB-5ms ((5%-phenyl)-methylpolysiloxane, 0.25 mm i.d., 0.25 {mu}m df) coupled with a 1.5 m of Innowax (polyethylene glycol, 0.32 mm i.d., 0.25 {mu}m df) by a quartz capillary column connector was introduced as separation column. Three advantages were discussed for the coupled system. The sample was fortified with a ring-labeled {sup 13}C{sub 3}{sup 15}N{sub 3}-melamine as an isotope internal standard and extracted by 1% of trichloroacetic acid aqueous solution. 2.2% of lead acetate solution was then added to deposit protein in the sample matrix. After purification by cation exchange cartridge, the sample solution was directly injected and detected by GC/MS. A six-point calibration curve ranging from 0.05 to 2 mg kg{sup -1} of melamine in sample was used to establish instrument response. The recovery was 93.9-102% with relative standard deviation from 3.1 to 8.7% when isotope internal standard used. The calculated method detection limit was 0.01 mg kg{sup -1}.

  11. Design and commissioning of a timestamp-based data acquisition system for the DRAGON recoil mass separator

    Energy Technology Data Exchange (ETDEWEB)

    Christian, G.; Fallis, J.; Hutcheon, D.; Olchanski, K.; Ruiz, C. [TRIUMF, Vancouver (Canada); Akers, C. [TRIUMF, Vancouver (Canada); University of York, Department of Physics, Heslington, York (United Kingdom); Connolly, D. [Colorado School of Mines, Department of Physics, Golden, CO (United States)

    2014-04-15

    The DRAGON recoil mass separator at TRIUMF exists to study radiative proton and alpha capture reactions, which are important in a variety of astrophysical scenarios. DRAGON experiments require a data acquisition system that can be triggered on either reaction product (γ-ray or heavy ion), with the additional requirement of being able to promptly recognize coincidence events in an online environment. To this end, we have designed and implemented a new data acquisition system for DRAGON, which consists of two independently triggered readouts. Events from both systems are recorded with timestamps from a 20 MHz clock that are used to tag coincidences in the earliest possible stage of the data analysis. Here we report on the design, implementation, and commissioning of the new DRAGON data acquisition system, including the hardware, trigger logic, coincidence reconstruction algorithm, and live time considerations. We also discuss the results of an experiment commissioning the new system, which measured the strength of the E{sub c.m.} = 1113 keV resonance in the {sup 20} Ne(p, γ){sup 21} Na radiative proton capture reaction. (orig.)

  12. Enantiomeric separation of free L- and D-amino acids in hydrolyzed protein fertilizers by capillary electrophoresis tandem mass spectrometry.

    Science.gov (United States)

    Sánchez-Hernández, Laura; Serra, Nuria Sierras; Marina, María Luisa; Crego, Antonio L

    2013-05-29

    Two capillary electrophoresis-tandem mass spectrometry (CE-MS(2)) methods were optimized in this work using cyclodextrins (CDs) as chiral selectors in order to determine the degree of racemization of the free amino acids contained in different hydrolyzed protein fertilizers used as plant biostimulants. The methodologies developed were characterized by the specificity of MS(2) experiments enabling the identification of all protein amino acids, except for cysteine. The enantiomeric separation of up to 14 amino acids was achieved with resolutions above 1.0 and limits of detection between 0.02 and 0.8 μM. The methods were applied to the analysis of complex samples such as hydrolyzed protein fertilizers to evaluate the presence of d-amino acids after different kinds of hydrolysis treatments. The results corroborated the absence or almost negligible presence of enantiomeric conversions of the L-amino acids into D-amino acids in the case of fertilizers obtained by enzymatic hydrolysis, as well as the high racemization rate for those obtained through a chemical hydrolysis.

  13. HPLC separation and GC-MS identification of the polar components of coal liquids. [High pressure liquid chromatography, gas chromatography-mass spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Satoh, M.; Tanabe, K.; Uchino, H.; Yokoyama, S.; Sanada, Y.

    1984-01-01

    The polar components in the 200-400 C fraction of Akabira coal liquids were separated by high pressure liquid chromatography using an amine-based column. By varying the CHCl/sub 3/ concentration in the solvent, basic, neutral and acid fractions were obtained. These were then investigated separately using infrared spectroscopy, flame ionization detection-gas chromatography and gas chromatography-mass spectroscopy. The basic fraction contained alkyltetrahydroquinolines, the neutral fraction, alkylphenols and alkylcarbazoles; and the acid fraction, alkylphenols. 15 references.

  14. Proteomic profiling of amniotic fluid in premature labor using two-dimensional liquid separation and mass spectrometry

    Science.gov (United States)

    Bujold, Emmanuel; Romero, Roberto; Kusanovic, Juan Pedro; Erez, Offer; Gotsch, Francesca; Chaiworapongsa, Tinnakorn; Gomez, Ricardo; Espinoza, Jimmy; Vaisbuch, Edi; Kim, Yeon Mee; Edwin, Samuel; Pisano, Mike; Allen, Beth; Podust, Vladimir N.; Dalmasso, Enrique A.; Rutherford, Jennifer; Rogers, Wade; Moser, Allan; Yoon, Bo Hyun; Barder, Tim

    2011-01-01

    Objective Simultaneous analysis of the protein composition of biological fluids is now possible. Such an approach can be used to identify biological markers of disease and to understand the pathophysiology of disorders that have eluded classification, diagnosis, and treatment. The purpose of this study was to analyze the differences in protein composition in amniotic fluid of patients in preterm labor. Study Design Amniotic fluid was obtained by amniocenteses from three groups of women with preterm labor and intact membranes: (1) women without intra-amniotic infection/inflammation (IAI) who delivered at term; (2) women without intra-amniotic IAI who delivered a preterm neonate; and (3) women with IAI. Intra-amniotic infection was defined as a positive amniotic fluid culture for microorganisms. Intra-amniotic inflammation was defined as an elevated amniotic fluid interleukin (IL)-6 (≥2.3 ng/mL). Two-dimensional (2D) chromatography was used for analysis. The first dimension separated proteins by isoelectric point, while the second, by the degree of hydrophobicity. 2D protein maps were generated using different experimental conditions (reducing agents as well as protein concentration). The maps were used to discern subsets of isoelectric point/hydrophobicity containing differentially expressed proteins. Protein identification of differentially expressed fractions was conducted with mass spectrometry. ELISA immunoassays as well as surface-enhanced laser desorption/ionization time-of-flight mass spectrometry (SELDI-TOF MS)--based on-chip antibody capture immunoassay were also used for confirmation of a specific protein that was differentially expressed. Results 1) Amniotic fluid protein composition can be analyzed using a combination of 2D liquid chromatography and mass spectrometry for the identification of proteins differentially expressed in patients in preterm labor; 2) While total insulin-like growth factor-binding protein-1 (IGFBP-1) concentration did not change

  15. Proteomic profiling of amniotic fluid in preterm labor using two-dimensional liquid separation and mass spectrometry.

    Science.gov (United States)

    Bujold, Emmanuel; Romero, Roberto; Kusanovic, Juan Pedro; Erez, Offer; Gotsch, Francesca; Chaiworapongsa, Tinnakorn; Gomez, Ricardo; Espinoza, Jimmy; Vaisbuch, Edi; Mee Kim, Yeon; Edwin, Samuel; Pisano, Mike; Allen, Beth; Podust, Vladimir N; Dalmasso, Enrique A; Rutherford, Jennifer; Rogers, Wade; Moser, Allan; Yoon, Bo Hyun; Barder, Tim

    2008-10-01

    Simultaneous analysis of the protein composition of biological fluids is now possible. Such an approach can be used to identify biological markers of disease and to understand the pathophysiology of disorders that have eluded classification, diagnosis, and treatment. The purpose of this study was to analyze the differences in protein composition of the amniotic fluid of patients in preterm labor. Amniotic fluid was obtained by amniocentesis from three groups of women with preterm labor and intact membranes: (1) women without intra-amniotic infection/inflammation (IAI) who delivered at term, (2) women without IAI who delivered a preterm neonate, and (3) women with IAI. Intra-amniotic infection was defined as a positive amniotic fluid culture for microorganisms. Intra-amniotic inflammation was defined as an elevated amniotic fluid interleukin (IL)-6 (> or =2.3 ng/mL). Two-dimensional (2D) chromatography was used for analysis. The first dimension separated proteins by isoelectric point, while the second, by the degree of hydrophobicity. 2D protein maps were generated using different experimental conditions (reducing agents as well as protein concentration). The maps were used to discern subsets of isoelectric point/hydrophobicity containing differentially expressed proteins. Protein identification of differentially expressed fractions was conducted with mass spectrometry. Enzyme-linked immunosorbent assays (ELISA) as well as surface-enhanced laser desorption/ionization time-of-flight mass spectrometry (SELDI-TOF MS)-based on-chip antibody capture immunoassays were also used for confirmation of a specific protein that was differentially expressed. (1) Amniotic fluid protein composition can be analyzed using a combination of 2D liquid chromatography and mass spectrometry for the identification of proteins differentially expressed in patients in preterm labor. (2) While total insulin-like growth factor-binding protein-1 (IGFBP-1) concentration did not change, IGFBP-1

  16. Sequential cloud point extraction for the speciation of mercury in seafood by inductively coupled plasma optical emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Li Yingjie [Department of Chemistry, Wuhan University, Wuhan 430072 (China); Hu Bin [Department of Chemistry, Wuhan University, Wuhan 430072 (China)], E-mail: binhu@whu.edu.cn

    2007-10-15

    A novel nonchromatographic speciation technique for the speciation of mercury by sequential cloud point extraction (CPE) combined with inductively coupled plasma optical emission spectrometry (ICP-OES) was developed. The method based on Hg{sup 2+} was complexed with I{sup -} to form HgI{sub 4}{sup 2-}, and the HgI{sub 4}{sup 2-} reacted with the methyl green (MG) cation to form hydrophobic ion-associated complex, and the ion-associated complex was then extracted into the surfactant-rich phase of the non-ionic surfactant octylphenoxypolyethoxyethanol (Triton X-114), which are subsequently separated from methylmercury (MeHg{sup +}) in the initial solution by centrifugation. The surfactant-rich phase containing Hg(II) was diluted with 0.5 mol L{sup -1} HNO{sub 3} for ICP-OES determination. The supernatant is also subjected to the similar CPE procedure for the preconcentration of MeHg{sup +} by the addition of a chelating agent, ammonium pyrrolidine dithiocarbamate (APDC), in order to form water-insolvable complex with MeHg{sup +}. The MeHg{sup +} in the micelles was directly analyzed after disposal as describe above. Under the optimized conditions, the extraction efficiency was 93.5% for Hg(II) and 51.5% for MeHg{sup +} with the enrichment factor of 18.7 for Hg(II) and 10.3 for MeHg{sup +}, respectively. The limits of detection (LODs) were 56.3 ng L{sup -1} for Hg(II) and 94.6 ng L{sup -1} for MeHg{sup +} (as Hg) with the relative standard deviations (RSDs) of 3.6% for Hg(II) and 4.5% for MeHg{sup +} (C = 10 {mu}g L{sup -1}, n = 7), respectively. The developed technique was applied to the speciation of mercury in real seafood samples and the recoveries for spiked samples were found to be in the range of 93.2-108.7%. For validation, a certified reference material of DORM-2 (dogfish muscle) was analyzed and the determined values are in good agreement with the certified values.

  17. Sequential cloud point extraction for the speciation of mercury in seafood by inductively coupled plasma optical emission spectrometry

    Science.gov (United States)

    Li, Yingjie; Hu, Bin

    2007-10-01

    A novel nonchromatographic speciation technique for the speciation of mercury by sequential cloud point extraction (CPE) combined with inductively coupled plasma optical emission spectrometry (ICP-OES) was developed. The method based on Hg 2+ was complexed with I - to form HgI 42-, and the HgI 42- reacted with the methyl green (MG) cation to form hydrophobic ion-associated complex, and the ion-associated complex was then extracted into the surfactant-rich phase of the non-ionic surfactant octylphenoxypolyethoxyethanol (Triton X-114), which are subsequently separated from methylmercury (MeHg +) in the initial solution by centrifugation. The surfactant-rich phase containing Hg(II) was diluted with 0.5 mol L - 1 HNO 3 for ICP-OES determination. The supernatant is also subjected to the similar CPE procedure for the preconcentration of MeHg + by the addition of a chelating agent, ammonium pyrrolidine dithiocarbamate (APDC), in order to form water-insolvable complex with MeHg +. The MeHg + in the micelles was directly analyzed after disposal as describe above. Under the optimized conditions, the extraction efficiency was 93.5% for Hg(II) and 51.5% for MeHg + with the enrichment factor of 18.7 for Hg(II) and 10.3 for MeHg +, respectively. The limits of detection (LODs) were 56.3 ng L - 1 for Hg(II) and 94.6 ng L - 1 for MeHg + (as Hg) with the relative standard deviations (RSDs) of 3.6% for Hg(II) and 4.5% for MeHg + ( C = 10 μg L -1, n = 7), respectively. The developed technique was applied to the speciation of mercury in real seafood samples and the recoveries for spiked samples were found to be in the range of 93.2-108.7%. For validation, a certified reference material of DORM-2 (dogfish muscle) was analyzed and the determined values are in good agreement with the certified values.

  18. Oxygen bomb combustion of biological samples for inductively coupled plasma optical emission spectrometry

    Science.gov (United States)

    Souza, Gilberto B.; Carrilho, Elma Neide V. M.; Oliveira, Camila V.; Nogueira, Ana Rita A.; Nóbrega, Joaquim A.

    2002-12-01

    A rapid sample preparation method is proposed for decomposition of milk powder, corn bran, bovine and fish tissues, containing certified contents of the analytes. The procedure involves sample combustion in a commercial stainless steel oxygen bomb operating at 25 bar. Most of the samples were decomposed within 5 min. Diluted nitric acid or water-soluble tertiary amines 10% v/v were used as absorption solutions. Calcium, Cu, K, Mg, Na, P, S and Zn were recovered with the bomb washings and determined by inductively coupled plasma optical emission spectrometry (ICP-OES). Ethanol mixed with paraffin was used as a combustion aid to allow complete combustion. A cooling step prior releasing of the bomb valve was employed to increase the efficiency of sample combustion. Iodine was also determined in milk samples spiked with potassium iodide to evaluate the volatilization and collection of iodine in amine CFA-C medium and the feasibility of its determination by ICP-OES with axial view configuration. Most of the element recoveries in the samples were between 91 and 105% and the certified and found contents exhibited a fair agreement at a 95% confidence level.

  19. Depletion-mode carrier-plasma optical modulator in zero-change advanced CMOS.

    Science.gov (United States)

    Shainline, Jeffrey M; Orcutt, Jason S; Wade, Mark T; Nammari, Kareem; Moss, Benjamin; Georgas, Michael; Sun, Chen; Ram, Rajeev J; Stojanović, Vladimir; Popović, Miloš A

    2013-08-01

    We demonstrate the first (to the best of our knowledge) depletion-mode carrier-plasma optical modulator fabricated in a standard advanced complementary metal-oxide-semiconductor (CMOS) logic process (45 nm node SOI CMOS) with no process modifications. The zero-change CMOS photonics approach enables this device to be monolithically integrated into state-of-the-art microprocessors and advanced electronics. Because these processes support lateral p-n junctions but not efficient ridge waveguides, we accommodate these constraints with a new type of resonant modulator. It is based on a hybrid microring/disk cavity formed entirely in the sub-90 nm thick monocrystalline silicon transistor body layer. Electrical contact of both polarities is made along the inner radius of the multimode ring cavity via an array of silicon spokes. The spokes connect to p and n regions formed using transistor well implants, which form radially extending lateral junctions that provide index modulation. We show 5 Gbps data modulation at 1265 nm wavelength with 5.2 dB extinction ratio and an estimated 40 fJ/bit energy consumption. Broad thermal tuning is demonstrated across 3.2 THz (18 nm) with an efficiency of 291 GHz/mW. A single postprocessing step to remove the silicon handle wafer was necessary to support low-loss optical confinement in the device layer. This modulator is an important step toward monolithically integrated CMOS photonic interconnects.

  20. Separate and combined associations of body-mass index and abdominal adiposity with cardiovascular disease : collaborative analysis of 58 prospective studies

    NARCIS (Netherlands)

    Wormser, David; Kaptoge, Stephen; Di Angelantonio, Emanuele; Wood, Angela M.; Pennells, Lisa; Thompson, Alex; Sarwar, Nadeem; Kizer, Jorge R.; Lawlor, Debbie A.; Nordestgaard, Borge G.; Ridker, Paul; Salomaa, Veikko; Stevens, June; Woodward, Mark; Sattar, Naveed; Collins, Rory; Thompson, Simon G.; Whitlock, Gary; Danesh, John

    2011-01-01

    Background Guidelines differ about the value of assessment of adiposity measures for cardiovascular disease risk prediction when information is available for other risk factors. We studied the separate and combined associations of body-mass index (BMI), waist circumference, and waist-to-hip ratio wi

  1. Separate and combined associations of body-mass index and abdominal adiposity with cardiovascular disease: collaborative analysis of 58 prospective studies

    DEFF Research Database (Denmark)

    Wormser, David; Kaptoge, Stephen; Di Angelantonio, Emanuele

    2011-01-01

    Guidelines differ about the value of assessment of adiposity measures for cardiovascular disease risk prediction when information is available for other risk factors. We studied the separate and combined associations of body-mass index (BMI), waist circumference, and waist-to-hip ratio with risk...

  2. High resolution LC-ESI-TOF-mass spectrometry method for fast separation, identification, and quantification of 12 isoflavones in soybeans and soybean products.

    Science.gov (United States)

    Lee, Mi Jin; Chung, Ill-Min; Kim, Hunjung; Jung, Mun Yhung

    2015-06-01

    A high resolution LC-ESI-TOF-MS analytical method was established for the rapid isolation, identification, and quantification of 12 isoflavones in soybean and soybean products. Individual isoflavones were identified on the basis of the accurate mass data of their respective protonated mass ions, Na or K adduct ions, fragment ions, and isotope ion patterns. The protonated mass ions of isoflavones were extracted for their quantification in soybean products. Twelve different isoflavones in the soybean products were fully separated, identified and quantified within 12min separation time. The established LC-TOF/MS was an effective analytical method for the simultaneous characterization and quantification of isoflavones with exceptionally short analytical time, high selectivity, a high linearity (r(2)>0.992) in a wide range, low LOD and LOQ, high precision, inter-and intra-day repeatability, and no significant matrix effect. Furthermore, it requires simple sample preparation procedure (solvent extraction, dilution, and syringe filtration).

  3. PSYM-WIDE: A Survey for Large-separation Planetary-mass Companions to Late Spectral Type Members of Young Moving Groups

    Science.gov (United States)

    Naud, Marie-Eve; Artigau, Étienne; Doyon, René; Malo, Lison; Gagné, Jonathan; Lafrenière, David; Wolf, Christian; Magnier, Eugene A.

    2017-09-01

    We present the results of a direct imaging survey for very large separation (>100 au), low-mass companions around 95 nearby young K5–L5 stars and brown dwarfs. They are high-likelihood candidates or confirmed members of the young (≲150 Myr) β Pictoris and AB Doradus moving groups (ABDMG) and the TW Hya, Tucana–Horologium, Columba, Carina, and Argus associations. Images in i\\prime and z\\prime filters were obtained with the Gemini Multi-Object Spectrograph (GMOS) on Gemini South to search for companions down to an apparent magnitude of z\\prime ∼ 22–24 at separations ≳20″ from the targets and in the remainder of the wide 5.‧5 × 5.‧5 GMOS field of view. This allowed us to probe the most distant region where planetary-mass companions could be gravitationally bound to the targets. This region was left largely unstudied by past high-contrast imaging surveys, which probed much closer-in separations. This survey led to the discovery of a planetary-mass (9–13 {M}{Jup}) companion at 2000 au from the M3V star GU Psc, a highly probable member of ABDMG. No other substellar companions were identified. These results allowed us to constrain the frequency of distant planetary-mass companions (5–13 {M}{Jup}) to {0.84}-0.66+6.73% (95% confidence) at semimajor axes between 500 and 5000 au around young K5–L5 stars and brown dwarfs. This is consistent with other studies suggesting that gravitationally bound planetary-mass companions at wide separations from low-mass stars are relatively rare.

  4. Development of the helium-jet fed on-line mass separator RAMA and its application to studies of T/sub z/ = -2 nuclei

    Energy Technology Data Exchange (ETDEWEB)

    Moltz, D.M.

    1979-10-01

    The study of nuclei far from beta stability is hampered greatly when the nuclide of interest decays in a manner identical to that of a nuclide produced in greater yield in the same bombardment. One solution to this problem is through the use of an on-line mass separator. Development of the Berkelely helium-jet fed on-line mass separator RAMA is discussed as applied to studies of the A = 4n, T/sub z/ = -2 nuclides. RAMA (Recoil Atom Mass Analyzer) has typical efficiencies of 0.1% for approx. 75 elements with melting points less than or equal to 2000/sup 0/C. This efficiency permits decay studies to be readily performed on nuclei with production cross sections greater than or equal to 500 ..mu..b for ..gamma..-ray spectroscopy and greater than or equal to 1 ..mu..b for discrete energy charged particle spectroscopy. The mass range on the normalized RAMA focal plane is +- 10%. The quoted efficiency is for a mass resolution of M/..delta..M approx. 300. RAMA has been used to observe two members of the A = 4n, T/sub z/ = -2 series of beta-delayed proton emitters, /sup 20/Mg and /sup 24/Si. Observation of beta-delayed protons from a mass-separated sample of /sup 20/Mg(t/sub 1/2/ approx. 95 ms) establishes the mass-excess of the lowest T = 2 (0/sup +/) state in /sup 20/Na (13.42 +- .05 MeV), thereby completing the mass twenty isospin quintet. A similar measurement of the decay of /sup 24/Si (t/sub 1/2/ approx. 100 ms) establishes the mass-excess of the lowest T = 2 (0/sup +/) state in /sup 24/Al (5.903 +- 0.009 MeV). The mass 24 isospin quintet is incomplete because the mass of /sup 24/Si remains unknown. In both cases, excellent agreement is obtained using only the quadratic form of the isobaric multiplet mass equation (IMME). 79 references.

  5. Separation of small molecular peptides with the same amino acid composition but different sequences by high performance liquid chromatography-electrospray ionization-mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    2009-01-01

    Peptidomics has emerged as a new discipline in recent years. Mass spectrometry (MS) is the most universal and efficient tool for structure identification of proteins and peptides. However,there is a limitation for the identification of peptides with the same amino acid composition but different se-quences because these peptides have identical mass spectra of molecular ions. This paper presents a high performance liquid chromatography-electrospray ionization-mass spectrometry (HPLC-ESI-MS) method for the separation of small molecular peptides with the same amino acid composition but dif-ferent sequences. Two tripeptides of Gly-Ser-Phe and Gly-Phe-Ser were used as a model sample. The separation behavior has been investigated and the separation conditions have been optimized. Under the optimum conditions,good repeatability was achieved. The developed method could provide a helpful reference for the separation of other peptides with the same amino acid composition but different sequences in the study of proteomics and peptidomics.

  6. Copper Determination in Gunshot Residue by Cyclic Voltammetric and Inductive Coupled Plasma-Optical Emission Spectroscopy

    Directory of Open Access Journals (Sweden)

    Mohd Hashim Nurul’Afiqah Hashimah

    2016-01-01

    Full Text Available Analysis of gunshot residue (GSR is a crucial evidences for a forensic analyst in the fastest way. GSR analysis insists a suitable method provides a relatively simple, rapid and precise information on the spot at the crime scene. Therefore, the analysis of Cu(II in GSR using cyclic voltammetry (CV on screen printed carbon electrode (SPCE is a better choice compared to previous alternative methods such as Inductive Coupled Plasma-Optical Emission Spectroscopy (ICP-OES those required a long time for analysis. SPCE is specially designed to handle with microvolumes of sample such as GSR sample. It gives advantages for identification of copper in GSR on-site preliminary test to prevent the sample loss on the process to be analyzed in the laboratory. SPCE was swabbed directly on the shooter’s arm immediately after firing and acetate buffer was dropped on SPCE before CV analysis. For ICP-OES analysis, cotton that had been soaked in 0.5 M nitric acid was swabbed on the shooter’s arm immediately after firing and kept in a tightly closed sampling tube. Gold coated SPCE that had been through nanoparticles modification exhibits excellent performance on voltammograms. The calibration was linear from 1 to 50 ppm of copper, the limit of detection for copper was 0.3 ppm and a relative standard deviation was 6.1 %. The method was successfully applied to the determination of copper in GSR. The Cu determination on SPCE was compared and validated by ICP-OES method with 94 % accuracy.

  7. Multielemental inductively coupled plasma optical emission spectrometry analysis of nickeliferous minerals.

    Science.gov (United States)

    Abad-Peña, Elizabet; Larrea-Marín, María Teresa; Villanueva-Tagle, Margarita Edelia; Pomares-Alfonso, Mario Simeón

    2014-06-01

    An inductively coupled plasma optical emission spectrometry method for the quantitative simultaneous determination of Al, Ca, Co, Cu, Cr, Fe, K, Mg, Mn, Na, Ni, P and Zn in Cuban laterite and serpentine minerals has been developed. Additionally, V and Ti can be quantitatively determined in laterite mineral; Li, Sr, and Zr can be detected in both mineral types and Pb can be detected just in laterite mineral. The microwave-assisted total acid digestion of samples was achieved with HCl+HNO3+HF and HNO3+HClO4+HF acid mixtures for laterite and serpentine samples, respectively. In non-robust plasma operating conditions, the matrix effect characteristics of the laterite sample were dictated by the principal component Fe; while the character of the Mg principal component matrix effect was some how modified by the concomitants Fe and Ni in serpentine sample. The selection of robust conditions decreased the matrix effect. Additionally, the simulation of the matrix samples by introducing the principal component Fe or Mg, correspondingly, in calibration dissolutions was needed to overcome completely the matrix effect over the analysis accuracy. Precision of analysis was very near or lower than 10% for most elements, except Sr (15%) in L-1; and K (15%) and Li (15%) in SNi sample. Accuracy of analysis was around or lowers than 10% for most elements, except K (15%), Na (19%), P (19%) and V (19%) in L-1 sample; and Ca (14%) and P (20%) in SNi sample. Copyright © 2014 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

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

    2016-05-01

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

  9. Separating the Chaff from the Oats: Evidence for a Conceptual Distinction between Count Noun and Mass Noun Aggregates

    Science.gov (United States)

    Middleton, Erica L.; Wisniewski, Edward J.; Trindel, Kelly A.; Imai, Mutsumi

    2004-01-01

    The English language makes a grammatical distinction between count nouns and mass nouns. For example, count nouns but not mass nouns can be pluralized and can appear with the indefinite article. Some scholars dismiss the distinction as an arbitrary convention of language whereas others suggest that it is conceptually based. The present studies…

  10. Solid-state Marx based two-switch voltage modulator for the On-Line Isotope Mass Separator accelerator at the European Organization for Nuclear Research.

    Science.gov (United States)

    Redondo, L M; Silva, J Fernando; Canacsinh, H; Ferrão, N; Mendes, C; Soares, R; Schipper, J; Fowler, A

    2010-07-01

    A new circuit topology is proposed to replace the actual pulse transformer and thyratron based resonant modulator that supplies the 60 kV target potential for the ion acceleration of the On-Line Isotope Mass Separator accelerator, the stability of which is critical for the mass resolution downstream separator, at the European Organization for Nuclear Research. The improved modulator uses two solid-state switches working together, each one based on the Marx generator concept, operating as series and parallel switches, reducing the stress on the series stacked semiconductors, and also as auxiliary pulse generator in order to fulfill the target requirements. Preliminary results of a 10 kV prototype, using 1200 V insulated gate bipolar transistors and capacitors in the solid-state Marx circuits, ten stages each, with an electrical equivalent circuit of the target, are presented, demonstrating both the improved voltage stability and pulse flexibility potential wanted for this new modulator.

  11. Optimization of the operating conditions of solid sampling electrothermal vaporization coupled to inductively coupled plasma optical emission spectrometry for the sensitive direct analysis of powdered rice.

    Science.gov (United States)

    Sadiq, Nausheen; Beauchemin, Diane

    2014-12-03

    Two different approaches were used to improve the capabilities of solid sampling (SS) electrothermal vaporization (ETV) coupled to inductively coupled plasma optical emission spectrometry (ICP-OES) for the direct analysis of powdered rice. Firstly, a cooling step immediately before and after the vaporization step in the ETV temperature program resulted in a much sharper analyte signal peak. Secondly, point-by-point internal standardization with an Ar emission line significantly improved the linearity of calibration curves obtained with an increasing amount of rice flour certified reference material (CRM). Under the optimized conditions, detection limits ranged from 0.01 to 6ngg(-1) in the solid, depending on the element and wavelength selected. The method was validated through the quantitative analysis of corn bran and wheat flour CRMs. Application of the method to the multi-elemental analysis of 4-mg aliquots of real organic long grain rice (white and brown) also gave results for Al, As, Co, Cu, Fe, Mg, Se, Pb and Zn in agreement with those obtained by inductively coupled plasma mass spectrometry following acid digestion of 0.2-g aliquots. As the analysis takes roughly 5min per sample (2.5min for grinding, 0.5-1min for weighing a 4-mg aliquot and 87s for the ETV program), this approach shows great promise for fast screening of food samples.

  12. Ultra high performance liquid chromatography with tandem mass spectrometry for rapid separation and identification of main constituents in Chinese herbal formula Xuan Hu Suo San.

    Science.gov (United States)

    Tang, Huaqi; Zhang, Xinyue; Luo, Shilin; Shang, Fei; Chen, Jianping; Wang, Jinghong; Duan, Xiaojie; Gao, Xiaoyan; Sun, Yikun

    2017-02-15

    Xuan Hu Suo San (XHSS) is a traditional Chinese medicine that has been extensively applied in the treatment of osteoarthritis for many years, however, its chemical composition has not yet been elucidated. Thus, a rapid, efficient, and precise method based on ultra high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry was applied in both positive- and negative-ion modes to rapidly separate and identify the main chemical ingredients in XHSS for the first time. Finally, with the optimised separation and detection method, a total of 57 compounds were simultaneously separated within 13 min, among which 14 compounds were confirmed by comparing retention time and MS data with reference standards and others were tentatively identified by comparing with reference literatures. This rapid and sensitive approach is highly useful for the identification and characterisation of chemical constituents, and provides fundamental and extensive information supporting further metabolic and pharmacokinetic studies of XHSS.

  13. Laser ablation inductively coupled plasma optical emission spectrometry for analysis of pellets of plant materials

    Energy Technology Data Exchange (ETDEWEB)

    Gomes, Marcos S. [Departamento de Química, Universidade Federal de São Carlos, Rod. Washington Luís, km 235, 13565-905 São Carlos, SP (Brazil); Centro de Energia Nuclear na Agricultura, Universidade de São Paulo, Av. Centenário 303, 13416-000 Piracicaba, SP (Brazil); Schenk, Emily R. [Department of Chemistry and Biochemistry, Florida International University, Miami, FL (United States); International Forensic Research Institute, Florida International University, Miami, FL (United States); Santos, Dário [Departamento de Ciências Exatas e da Terra, Universidade Federal de São Paulo, Rua Professor Arthur Riedel 275, Diadema, SP (Brazil); Krug, Francisco José [Centro de Energia Nuclear na Agricultura, Universidade de São Paulo, Av. Centenário 303, 13416-000 Piracicaba, SP (Brazil); Almirall, José R., E-mail: almirall@fiu.edu [Department of Chemistry and Biochemistry, Florida International University, Miami, FL (United States); International Forensic Research Institute, Florida International University, Miami, FL (United States)

    2014-04-01

    An evaluation of laser ablation inductively coupled plasma optical emission spectroscopy (LAICP OES) for the direct analysis of pelleted plant material is reported. Ground leaves of orange citrus, soy and sugarcane were comminuted using a high-speed ball mill, pressed into pellets and sampled directly with laser ablation and analyzed by ICP OES. The limits of detection (LODs) for the method ranged from as low as 0.1 mg kg{sup −1} for Zn to as high as 94 mg kg{sup −1} for K but were generally below 6 mg kg{sup −1} for most of the elements of interest. A certified reference material consisting of a similar matrix (NIST SRM 1547 peach leaves) was used to check the accuracy of the calibration and the reported method resulted in an average bias of ∼ 5% for all the elements of interest. The precision for the reported method ranged from as low as 4% relative standard deviation (RSD) for Mn to as high as 17% RSD for Zn but averaged ∼ 6.5% RSD for all the elements (n = 10). The proposed method was tested for the determination of Ca, Mg, P, K, Fe, Mn, Zn and B, and the results were in good agreement with those obtained for the corresponding acid digests by ICP-OES, no differences being observed by applying a paired t-test at the 95% confidence level. The reported direct solid sampling method provides a fast alternative to acid digestion that results in similar and appropriate analytical figures of merit with regard to sensitivity, accuracy and precision for plant material analysis. - Highlights: • An evaluation of LA-ICP-OES for the direct analysis of pelleted plant material is reported. • Orange citrus, soy and sugarcane plants were pressed into pellets and sampled directly. • The element menu consisted of Ca, Mg, P, K, Fe, Mn, Zn and B. • LODs for the method ranged from 0.1 mg kg{sup −1} for Zn to 94 mg kg{sup −1} for K. • The precision ranged from 4% RSD for Mn to 17% RSD for Zn (∼ 6.5% RSD average)

  14. Effect of bend separation distance on the mass transfer in back-to-back pipe bends arranged in a 180° configuration

    Science.gov (United States)

    Chen, X.; Le, T.; Ewing, D.; Ching, C. Y.

    2016-12-01

    The mass transfer to turbulent flow through back-to-back pipe bends arranged in a 180° configuration with different lengths of pipe between the bends was measured using a dissolving gypsum test section in water. The measurements were performed for bends with a radius of curvature of 1.5 times the pipe diameter ( D) at a Reynolds numbers of 70,000 and Schmidt number of 1280. The maximum mass transfer in the bends decreased from approximately 1.8 times the mass transfer in the upstream pipe when there was no separation distance between the bends to 1.7 times when there was a 1 D or 5 D length of pipe between the bends. The location of the maximum mass transfer was on the inner sidewall downstream of the second bend when there was no separation distance between the bends. This location changed to the inner wall at the beginning of the second bend when there was a 1 D long pipe between the bends, and to the inner sidewall at the end of the first bend when there was a 5 D long pipe between the bends.

  15. Quantitative separation of the influence of copper (II) chloride mass migration on the chemo-responsive shape memory effect in polyurethane shape memory polymer

    Science.gov (United States)

    Lu, Haibao; Lu, Chunrui; Huang, Wei Min; Leng, Jinsong

    2016-10-01

    Chemo-responsive shape memory effect in polyurethane shape memory polymer (SMP) composite triggered by mass migration of copper (II) chloride (CuCl2) has been experimentally demonstrated. In this study, we present a comprehensive study on quantitative separation of the effect of CuCl2 particle mass migration on the chemo-responsive shape recovery behavior of polyurethane SMP composites with different concentrations of CuCl2 particles. It is found that the SMP is featured with a critical release rate of the mechanical energy storage associated with the shape recovery behavior due to mass migration of the CuCl2 particle. A sequence of molecular interactions among CuCl2 particles, polyurethane macromolecules and water molecules, i.e., assembly of the CuCl2 particle with polyurethane macromolecules, and then disassembly and dissolution of the CuCl2 particle in water, results in an acceleration of water-induced shape recovery of polyurethane SMP. This study focuses on the quantitative separation of the influence of mass migration on the chemo-responsive shape recovery behavior of polyurethane SMP in response to water. It is expected to promote and achieve the actuation of chemo-responsive SMPs in a fully controllable manner.

  16. Mechanical coupling between two innovative theories on erosion, transportation and phase-separation: Solving some long-standing problems in mass flows

    Science.gov (United States)

    Pudasaini, Shiva P.; Fischer, Jan-Thomas; Mergili, Martin

    2017-04-01

    Debris flows are gravity driven mixture flows of soil, sand, rock and water. The solid particles and viscous fluid governs the rheological properties, and their coupling significantly influences the dynamics. For example, debris flows can dramatically increase their volume and destructive potential, and become exceptionally mobile by entraining bed material. The mixture composition can evolve to strikingly change the spatial distribution of particles and fluid, and thus frictional and viscous resistance. So, erosion-deposition and phase-separation between solid and fluid, which strongly depend on material composition, play a critical role in debris flow dynamics. Proper understanding of these complex physical processes is very important in accurate description of impact forces, inundation areas, landscape evolution and developing reliable mitigation plans. Predicting the underlying processes of erosion, phase-separation and deposition in debris flow are long-standing challenges. However, due to lack of data and suitable models, there exists no runout prediction method that includes observed processes of erosion of dry and saturated beds, entrainment and diffusion of eroded material, grain sorting, phase-separation, levee/lobe formation and evolution of deposition patterns. Based on innovative mechanical models for erosion-deposition (Pudasaini and Fischer, 2016a) and phase-separation (Pudasaini and Fischer, 2016b) that explicitly consider changes in local flow compositions, and their basic/potential validations, we present a novel, unified, efficient and fully coupled solution method to these true multi-phase, three-dimensional mass flow problems. As debris flows are better described by a three-phase mixture that include viscous fluid, and fine and coarse grains as compared to often used single-phase models, we propose model extensions that consists of three-phases including yield strength. Thus, we present an advanced mass flow simulation model aiming to

  17. Topographical and Chemical Imaging of a Phase Separated Polymer Using a Combined Atomic Force Microscopy/Infrared Spectroscopy/Mass Spectrometry Platform.

    Science.gov (United States)

    Tai, Tamin; Karácsony, Orsolya; Bocharova, Vera; Van Berkel, Gary J; Kertesz, Vilmos

    2016-03-01

    In this paper, the use of a hybrid atomic force microscopy/infrared spectroscopy/mass spectrometry imaging platform was demonstrated for the acquisition and correlation of nanoscale sample surface topography and chemical images based on infrared spectroscopy and mass spectrometry. The infrared chemical imaging component of the system utilized photothermal expansion of the sample at the tip of the atomic force microscopy probe recorded at infrared wave numbers specific to the different surface constituents. The mass spectrometry-based chemical imaging component of the system utilized nanothermal analysis probes for thermolytic surface sampling followed by atmospheric pressure chemical ionization of the gas phase species produced with subsequent mass analysis. The basic instrumental setup, operation, and image correlation procedures are discussed, and the multimodal imaging capability and utility are demonstrated using a phase separated poly(2-vinylpyridine)/poly(methyl methacrylate) polymer thin film. The topography and both the infrared and mass spectral chemical images showed that the valley regions of the thin film surface were comprised primarily of poly(2-vinylpyridine) and hill or plateau regions were primarily poly(methyl methacrylate). The spatial resolution of the mass spectral chemical images was estimated to be 1.6 μm based on the ability to distinguish surface features in those images that were also observed in the topography and infrared images of the same surface.

  18. GPS Separator

    CERN Multimedia

    2016-01-01

    Footage of the 70 degree ISOLDE GPS separator magnet MAG70 as well as the switchyard for the Central Mass and GLM (GPS Low Mass) and GHM (GPS High Mass) beamlines in the GPS separator zone. In the GPS20 vacuum sector equipment such as the long GPS scanner 482 / 483 unit, faraday cup FC 490, vacuum valves and wiregrid piston WG210 and WG475 and radiation monitors can also be seen. Also the RILIS laser guidance and trajectory can be seen, the GPS main beamgate switch box and the actual GLM, GHM and Central Beamline beamgates in the beamlines as well as the first electrostatic quadrupoles for the GPS lines. Close up of the GHM deflector plates motor and connections and the inspection glass at the GHM side of the switchyard.

  19. Uncertainty Estimation of Metals and Semimetals Determination in Wastewater by Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES)

    Science.gov (United States)

    Marques, J. R.; Villa-Soares, S. M.; Stellato, T. B.; Silva, T. B. S. C.; Faustino, M. G.; Monteiro, L. R.; Pires, M. A. F.; Cotrim, M. E. B.

    2016-07-01

    The measurement uncertainty is a parameter that represents the dispersion of the results obtained by a method of analysis. The estimation of measurement uncertainty in the determination of metals and semimetals is important to compare the results with limits defined by environmental legislation and conclude if the analytes are meeting the requirements. Therefore, the aim of this paper is present all the steps followed to estimate the uncertainty of the determination of amount of metals and semimetals in wastewater by Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES). Measurement uncertainty obtained was between 4.6 and 12.2% in the concentration range of mg.L-1.

  20. Monolithic Superhydrophobic Polymer Layer with Photopatterned Virtual Channel for the Separation of Peptides Using Two-Dimensional Thin Layer Chromatography-Desorption Electrospray Ionization Mass Spectrometry

    Science.gov (United States)

    Han, Yehua; Levkin, Pavel; Abarientos, Irene; Liu, Huwei; Svec, Frantisek; Fréchet, Jean M.J.

    2010-01-01

    Superhydrophobic monolithic porous polymer layers with a photopatterned hydrophilic channel have been prepared. These layers were used for two-dimensional thin layer chromatography of peptides. The 50 μm thin poly(butyl methacrylate-co-ethylene dimethacrylate) layers supported onto 4.0 × 3.3 cm glass plates were prepared using UV-initiated polymerization in a simple glass mold. Photografting of a mixture of 2-acrylamido-2-methyl-1-propanesulfonic acid and 2-hydroxyethyl methacrylate carried out through a mask afforded a 600 μm wide virtual channel along one side of the layer. This channel, which contains ionizable functionalities, enabled the first dimension separation in ion exchange mode. The aqueous mobile phase migrates only through the channel due to the large difference in surface tension at the interface of the hydrophilic channel and the superhydrophobic monolith. The unmodified part of the layer featuring hydrophobic chemistry was then used for the reversed phase separation in the orthogonal second dimension. Practical application of our technique was demonstrated with a rapid 2D separation of a mixture of model peptides differing in hydrophobicity and isoelectric point using a combination of ion-exchange and reversed phase modes. In the former mode, the peptides migrated 11 mm in less than 1 min. Detection of fluorescently labeled peptides was achieved through UV light visualization. Separation of the native peptides was monitored directly using a desorption electrospray ionization (DESI) source coupled to a mass spectrometer. Unidirectional surface scanning with the DESI source was found suitable to determine both the location of each separated peptide and its molecular mass. PMID:20151661

  1. Determination of ultra-low level 129I in vegetation using pyrolysis for iodine separation and accelerator mass spectrometry measurements

    DEFF Research Database (Denmark)

    Hou, Xiaolin; Wang, Yanyun

    2016-01-01

    Radioactive isotopes of iodine are the most common radiological toxins from nuclear accidents due to their high release and high enrichment in human thyroid. Among the radioactive isotopes, long-lived 129I can not only be used for the estimation of the radioactive risk of short-lived radioactive...... isotopes of iodine to humans and ecosystems, but also for the investigation of the biogeochemical cycle and environmental behavior of iodine. Accurate determination of 129I in various environmental and biological samples is the key issue for these purposes. Due to its beta decay, low specific activity...... and ultra-low concentration in normal environmental and biological samples, it is important to efficiently separate iodine from the sample matrix and sensitively measure 129I. However, the complicated chemical properties of iodine and high organic content in biological samples make efficient separation...

  2. Cull sow knife-separable lean content evaluation at harvest and lean mass content prediction equation development.

    Science.gov (United States)

    Abell, Caitlyn E; Stalder, Kenneth J; Hendricks, Haven B; Fitzgerald, Robert F

    2012-07-01

    The objectives of this study were to develop a prediction equation for carcass knife-separable lean within and across USDA cull sow market weight classes (MWC) and to determine carcass and individual primal cut knife separable lean content from cull sows. There were significant percent lean and fat differences in the primal cuts across USDA MWC. The two lighter USDA MWC had a greater percent carcass lean and lower percent fat compared to the two heavier MWC. In general, hot carcass weight explained the majority of carcass lean variation. Additionally, backfat was a significant variation source when predicting cull sow carcass lean. The findings support using a single lean prediction equation across MWC to assist processors when making cull sow purchasing decisions and determine the mix of animals from various USDA MWC that will meet their needs when making pork products with defined lean:fat content.

  3. Characterization of gel-separated glycoproteins using two-step proteolytic digestion combined with sequential microcolumns and mass spectrometry

    DEFF Research Database (Denmark)

    Larsen, Martin Røssel; Højrup, Peter; Roepstorff, Peter

    2005-01-01

    Protein glycosylation can be vital for changing the function or physiochemical properties of a protein. Abnormal glycosylation can lead to protein malfunction, resulting in severe diseases. Therefore, it is important to develop techniques for characterization of such modifications in proteins...... present a new technique that allows characterization of low amounts of glycoproteins separated by gel electrophoresis. The method takes advantage of sequential specific and nonspecific enzymatic treatment followed by selective purification and characterization of the glycopeptides using graphite powder...

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

    Science.gov (United States)

    Zhang, Gai; Tian, Min

    2015-04-01

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

  5. Modeling of mass transfer of Phospholipids in separation process with supercritical CO2 fluid by RBF artificial neural networks

    Science.gov (United States)

    An artificial Radial Basis Function (RBF) neural network model was developed for the prediction of mass transfer of the phospholipids from canola meal in supercritical CO2 fluid. The RBF kind of artificial neural networks (ANN) with orthogonal least squares (OLS) learning algorithm were used for mod...

  6. Photo-ionisation mass spectrometry as detection method for gas chromatography. Optical selectivity and multidimensional comprehensive separations.

    Science.gov (United States)

    Zimmermann, Ralf; Welthagen, Werner; Gröger, Thomas

    2008-03-14

    Mass spectrometry (MS) with soft ionisation techniques (i.e. ionisation without fragmentation of the analyte molecules) for gaseous samples exhibits interesting analytical properties for direct analysis applications (i.e. direct inlet mass spectrometric on-line monitoring) as well as mass spectrometric detection method for gas chromatography (GC-MS). Commonly either chemical ionisation (CI) or field ionisation (FI) is applied as soft ionisation technology for GC-MS. An interesting alternative to the CI and FI technologies methods are photo-ionisation (PI) methods. PI overcomes some of the limitations of CI and FI and furthermore add some unique analytical properties. The resonance enhanced multi-photon ionisation (REMPI) method uses intense UV-laser pulses (wavelength range approximately 350-193 nm) for highly selective, sensitive and soft ionisation of predominately aromatic compounds. The single photon ionisation (SPI) method utilises VUV light (from lamps or laser sources, wavelengths range approximately 150-110 nm) can be used for a universal soft ionisation of organic molecules. In this article the historical development as well as the current status and concepts of gas chromatography hyphenated to photo-ionisation mass spectrometry are reviewed.

  7. Determination of plutonium isotopes (238Pu, 239Pu, 240Pu, 241Pu) in environmental samples using radiochemical separation combined with radiometric and mass spectrometric measurements.

    Science.gov (United States)

    Xu, Yihong; Qiao, Jixin; Hou, Xiaolin; Pan, Shaoming; Roos, Per

    2014-02-01

    This paper reports an analytical method for the determination of plutonium isotopes ((238)Pu, (239)Pu, (240)Pu, (241)Pu) in environmental samples using anion exchange chromatography in combination with extraction chromatography for chemical separation of Pu. Both radiometric methods (liquid scintillation counting and alpha spectrometry) and inductively coupled plasma mass spectrometry (ICP-MS) were applied for the measurement of plutonium isotopes. The decontamination factors for uranium were significantly improved up to 7.5 × 10(5) for 20 g soil compared to the level reported in the literature, this is critical for the measurement of plutonium isotopes using mass spectrometric technique. Although the chemical yield of Pu in the entire procedure is about 55%, the analytical results of IAEA soil 6 and IAEA-367 in this work are in a good agreement with the values reported in the literature or reference values, revealing that the developed method for plutonium determination in environmental samples is reliable. The measurement results of (239+240)Pu by alpha spectrometry agreed very well with the sum of (239)Pu and (240)Pu measured by ICP-MS. ICP-MS can not only measure (239)Pu and (240)Pu separately but also (241)Pu. However, it is impossible to measure (238)Pu using ICP-MS in environmental samples even a decontamination factor as high as 10(6) for uranium was obtained by chemical separation.

  8. Separation of polar mushroom toxins by mixed-mode hydrophilic and ionic interaction liquid chromatography-electrospray ionization-mass spectrometry.

    Science.gov (United States)

    Chung, Wai-cheung; Tso, Sau-ching; Sze, Sai-tim

    2007-02-01

    Reversed-phase liquid chromatography (RPLC) is commonly used to analyze nonvolatile contaminants and naturally occurring toxins in foods. However, polar compounds, such as hydrophilic polypeptides and quaternary ammonium salts, are often not satisfactorily separated by RPLC and present a challenge for analytical scientists. In this study, hydrophilic interaction liquid chromatography (HILIC), on an amide-based stationary phase in combination with electrospray ionization (ESI) tandem mass spectrometry (MS-MS), is successfully employed to simultaneously separate polar mushroom toxins, including amanitins and phallotoxins, which are cyclic oligopeptides and muscarine, a quaternary ammonium compound, in mushrooms. The sensitivity of different ionization modes is studied, and the positive ionization mode is found to provide a more sensitive and effective tool for the unambiguous identification of the concerned polar toxins because of their characteristic fragmentation patterns. The properties of the mobile phase are also found to have significant impacts on the separation. At a high acetonitrile (ACN) concentration, hydrophilic interaction dominates, and all analytes under study demonstrate a much higher affinity with the stationary phase. The addition of methanol (MeOH) as a modifier could further enhance the HILIC separation for amanitins, phallotoxins, and muscarine. Valley-to-valley separation is achieved upon the optimatizatiqn of the mobile phase (comprising of ACN, MeOH, and ammonium formate buffer at pH approximately 3.5) and the solvent gradient. HILIC coupled with ESI-MS-MS is demonstrated to be a novel technique for the simultaneous separation and confirmatory analysis of the concerned polar toxins by providing an environment of solubility and retention that could not be achieved through the use of RPLC.

  9. Toward 'omic scale metabolite profiling: a dual separation-mass spectrometry approach for coverage of lipid and central carbon metabolism.

    Science.gov (United States)

    Ivanisevic, Julijana; Zhu, Zheng-Jiang; Plate, Lars; Tautenhahn, Ralf; Chen, Stephen; O'Brien, Peter J; Johnson, Caroline H; Marletta, Michael A; Patti, Gary J; Siuzdak, Gary

    2013-07-16

    Although the objective of any 'omic science is broad measurement of its constituents, such coverage has been challenging in metabolomics because the metabolome is comprised of a chemically diverse set of small molecules with variable physical properties. While extensive studies have been performed to identify metabolite isolation and separation methods, these strategies introduce bias toward lipophilic or water-soluble metabolites depending on whether reversed-phase (RP) or hydrophilic interaction liquid chromatography (HILIC) is used, respectively. Here we extend our consideration of metabolome isolation and separation procedures to integrate RPLC/MS and HILIC/MS profiling. An aminopropyl-based HILIC/MS method was optimized on the basis of mobile-phase additives and pH, followed by evaluation of reproducibility. When applied to the untargeted study of perturbed bacterial metabolomes, the HILIC method enabled the accurate assessment of key, dysregulated metabolites in central carbon pathways (e.g., amino acids, organic acids, phosphorylated sugars, energy currency metabolites), which could not be retained by RPLC. To demonstrate the value of the integrative approach, bacterial cells, human plasma, and cancer cells were analyzed by combined RPLC/HILIC separation coupled to ESI positive/negative MS detection. The combined approach resulted in the observation of metabolites associated with lipid and central carbon metabolism from a single biological extract, using 80% organic solvent (ACN:MeOH:H2O 2:2:1). It enabled the detection of more than 30,000 features from each sample type, with the highest number of uniquely detected features by RPLC in ESI positive mode and by HILIC in ESI negative mode. Therefore, we conclude that when time and sample are limited, the maximum amount of biological information related to lipid and central carbon metabolism can be acquired by combining RPLC ESI positive and HILIC ESI negative mode analysis.

  10. Aluminum and phosphorus separation: application to preparation of target from brain tissue for {sup 26}Al determination by accelerator mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Brauer, Russell D.; Robertson, J. David; Sharma, Pankaj; Yokel, Robert A. E-mail: ryokel1@pop.uky.edu

    1999-04-01

    Acid digested brain containing 4 mg added {sup 27}Al was ashed at 1000 deg. C to prepare an Al{sub 2}O{sub 3} target for accelerator mass spectrometry (AMS) analysis of {sup 26}Al. A glass-like material usually resulted which was thought to be aluminum (Al) oxyphosphate. The separation of Al and phosphate was investigated. Al, but not phosphate, was bound by a cation exchange resin (AG 50-X8). Hydrofluoric acid eluted the Al from the resin. Removal of phosphate from acid digested brain by this method produced an amorphous material after ashing that was easier to recover from the porcelain crucible and had a higher AMS beam current. This procedure to separate Al from phosphate may have utility in other applications.

  11. IgY14 and SuperMix immunoaffinity separations coupled with liquid chromatography-mass spectrometry for human plasma proteomic biomarker discovery

    Energy Technology Data Exchange (ETDEWEB)

    Shi, Tujin; Zhou, Jianying; Gritsenko, Marina A.; Hossain, Mahmud; Camp, David G.; Smith, Richard D.; Qian, Weijun

    2012-02-01

    Interest in the application of advanced proteomics technologies to human blood plasma- or serum-based clinical samples for the purpose of discovering disease biomarkers continues to grow; however, the enormous dynamic range of protein concentrations in these types of samples (often >10 orders of magnitude) represents a significant analytical challenge, particularly for detecting low-abundance candidate biomarkers. In response, immunoaffinity separation methods for depleting multiple high- and moderate-abundance proteins have become key tools for enriching low-abundance proteins and enhancing detection of these proteins in plasma proteomics. Herein, we describe IgY14 and tandem IgY14-Supermix separation methods for removing 14 high-abundance and up to 60 moderate-abundance proteins, respectively, from human blood plasma and highlight their utility when combined with liquid chromatography-tandem mass spectrometry for interrogating the human plasma proteome.

  12. IgY14 and SuperMix immunoaffinity separations coupled with liquid chromatography-mass spectrometry for human plasma proteomics biomarker discovery.

    Science.gov (United States)

    Shi, Tujin; Zhou, Jian-Ying; Gritsenko, Marina A; Hossain, Mahmud; Camp, David G; Smith, Richard D; Qian, Wei-Jun

    2012-02-01

    Interest in the application of advanced proteomics technologies to human blood plasma- or serum-based clinical samples for the purpose of discovering disease biomarkers continues to grow; however, the enormous dynamic range of protein concentrations in these types of samples (often >10 orders of magnitude) represents a significant analytical challenge, particularly for detecting low-abundance candidate biomarkers. In response, immunoaffinity separation methods for depleting multiple high- and moderate-abundance proteins have become key tools for enriching low-abundance proteins and enhancing detection of these proteins in plasma proteomics. Herein, we describe IgY14 and tandem IgY14-Supermix separation methods for removing 14 high-abundance and up to 60 moderate-abundance proteins, respectively, from human blood plasma and highlight their utility when combined with liquid chromatography-tandem mass spectrometry for interrogating the human plasma proteome.

  13. Radiochemical Separation and Measurement by Mass Spectrometry with Magnetic Sector with Inductively Coupled Plasma source (ICP-SFMS of Plutonium Isotopes in Soil Samples

    Directory of Open Access Journals (Sweden)

    C. O. Torres-Cortés

    2016-08-01

    Full Text Available The aim of this work is twofold: to optimize the radiochemical separation of Plutonium (Pu from soil samples, and to measure the Pu concentration. Soil samples were prepared using acid digestion assisted by microwaves; then, Pu purification was carried out with Pu AG1X8 resin. Pu isotopes were measured using Mass Spectrometry with Magnetic Sector with Inductively Coupled Plasma source (ICP-SFMS. In order to reduce the interference due to the presence of 238UH+ in the samples a desolvation system (Apex was used. The limit of detection (LOD of Pu was determined. The efficiency of Pu recovery from soil samples varies from 70 to 93%.

  14. Determination of Ultralow Level 129I/127I in Natural Samples by Separation of Microgram Carrier Free Iodine and Accelerator Mass Spectrometry Detection

    DEFF Research Database (Denmark)

    Hou, Xiaolin; Zhou, Weijian; Chen, Ning;

    2010-01-01

    a carrier free method using coprecipitation of AgI with AgCl for preparing micrograms of iodine target, associated with combustion using a tube furnace for separating iodine from solid samples and anion exchange chromatography for preconcentrating iodine from a large volume of water. An accelerator mass...... of 129I/127I, and a detection limit of this method for 129I is calculated to be 105 atoms. This will allow us to accurately determine 129I in prenuclear geological samples of low iodine concentration with 129I/127I of 10−12, such as loess, soil, coral, rock, sediment, and groundwater. Some samples...

  15. Separation and characterization of phenolic compounds in fennel (Foeniculum vulgare) using liquid chromatography-negative electrospray ionization tandem mass spectrometry.

    Science.gov (United States)

    Parejo, Irene; Jauregui, Olga; Sánchez-Rabaneda, Ferran; Viladomat, Francesc; Bastida, Jaume; Codina, Carles

    2004-06-16

    Liquid chromatography (LC) diode array detection (DAD) coupled to negative electrospray ionization (ESI) tandem mass spectrometry (MS/MS) was used for the rapid and sensitive identification of water-soluble phenolic compounds in fennel waste. The plant material was first extracted and then chromatographed on Sephadex LH-20 to afford seven fractions, each of them being subjected to LC-MS analysis. Identification of the compounds was carried out by interpretation of UV, MS, and MS/MS spectra. Forty-two phenolic substances were identified, 27 of which had not previously been reported in fennel, including hydroxycinnamic acid derivatives, flavonoid glycosides, and flavonoid aglycons.

  16. A fast and sensitive method for the separation of carotenoids using ultra-high performance supercritical fluid chromatography-mass spectrometry.

    Science.gov (United States)

    Jumaah, Firas; Plaza, Merichel; Abrahamsson, Victor; Turner, Charlotta; Sandahl, Margareta

    2016-08-01

    In this study, a rapid and sensitive ultra-high performance supercritical fluid chromatography-mass spectrometry (UHPSFC-MS) method has been developed and partially validated for the separation of carotenoids within less than 6 min. Six columns of orthogonal selectivity were examined, and the best separation was obtained by using a 1-aminoanthracene (1-AA) column. The length of polyene chain as well as the number of hydroxyl groups in the structure of the studied carotenoids determines their differences in the physiochemical properties and thus the separation that is achieved on this column. All of the investigated carotenoids were baseline separated with resolution values greater than 1.5. The effects of gradient program, back pressure, and column temperature were studied with respect to chromatographic properties such as retention and selectivity. Electrospray ionization (ESI) and atmospheric pressure chemical ionization (APCI) were compared in both positive and negative mode, using both direct infusion and hyphenated with UHPSFC. The ESI in positive mode provided the highest response. The coefficient of determination (R (2)) for all calibration curves were greater than 0.998. Limit of detection (LOD) was in the range of 2.6 and 25.2 ng/mL for α-carotene and astaxanthin, respectively, whereas limit of quantification (LOQ) was in the range of 7.8 and 58.0 ng/mL for α-carotene and astaxanthin, respectively. Repeatability and intermediate precision of the developed UHPSFC-MS method were determined and found to be RSD supercritical fluid extracts of microalgae and rosehip. Graphical Abstract Ultra-high performance supercritical fluid chromatography-a rapid separation method for the analysis of carotenoids in rosehip and microalgae samples.

  17. Separating climate-induced mass transfers and instrumental effects from tectonic signal in repeated absolute gravity measurements

    Science.gov (United States)

    Van Camp, M.; Viron, O.; Avouac, J. P.

    2016-05-01

    We estimate the signature of the climate-induced mass transfers in repeated absolute gravity measurements based on satellite gravimetric measurements from the Gravity Recovery and Climate Experiment (GRACE) mission. We show results at the globe scale and compare them with repeated absolute gravity (AG) time behavior in three zones where AG surveys have been published: Northwestern Europe, Canada, and Tibet. For 10 yearly campaigns, the uncertainties affecting the determination of a linear gravity rate of change range 3-4 nm/s2/a in most cases, in the absence of instrumental artifacts. The results are consistent with what is observed for long-term repeated campaigns. We also discuss the possible artifact that can result from using short AG survey to determine the tectonic effects in a zone of high hydrological variability. We call into question the tectonic interpretation of several gravity changes reported from stations in Tibet, in particular the variation observed prior to the 2015 Gorkha earthquake.

  18. Biodegradation testing of chemicals with high Henry’s constants – separating mass and effective concentration reveals higher rate constants

    DEFF Research Database (Denmark)

    Birch, Heidi; Andersen, Henrik Rasmus; Comber, Mike

    During simulation-type biodegradation tests, volatile chemicals will continuously partition between water phase and headspace. This study addressed how (1) this partitioning affects biodegradation test results and (2) it can be accounted for by combining mass balance and dynamic biodegradation...... Microextraction (HS-SPME) was applied directly on the test systems to measure substrate depletion by biodegradation relative to abiotic controls. HS-SPME was also applied to determine air to water partitioning ratios. Water phase biodegradation rate constants, kwater, were up to 72 times higher than test system...... biodegradation rate constants, ksystem. True water phase degradation rate constants facilitate extrapolation to other air-water systems and are more suitable input parameters for aquatic exposure and fate models. As such, they should be considered more appropriate for risk assessments than test system rate...

  19. Selective separation, detection of zotepine and mass spectral characterization of degradants by LC-MS/MS/QTOF

    Institute of Scientific and Technical Information of China (English)

    M.V.N. Kumar Talluri; Naveen Reddy Kandimalla; Raju Bandu; Divya Chundi; Ramesh Marupaka; Ragampeta Srinivas

    2014-01-01

    A simple, precise, accurate stability-indicating gradient reversed-phase high-performance liquid chromatographic (RP-HPLC) method was developed for the quantitative determination of zotepine (ZTP) in bulk and pharmaceutical dosage forms in the presence of its degradation products (DPs). The method was developed using Phenomenex C18 column (250 mm ~ 4.6 mm i.d., 5 mm) with a mobile phase containing a gradient mixture of solvents, A (0.05%trifluoroacetic acid (TFA), pH ¼ 3.0) and B (acetonitrile). The eluted compounds were monitored at 254 nm;the run time was within 20.0 min, in which ZTP and its DPs were well separated, with a resolution of 41.5. The stress testing of ZTP was carried out under acidic, alkaline, neutral hydrolysis, oxidative, photolytic and thermal stress conditions. ZTP was found to degrade significantly in acidic, photolytic, thermal and oxidative stress conditions and remain stable in basic and neutral conditions. The developed method was validated with respect to specificity, linearity, limit of detection, limit of quantification, accuracy, precision and robustness as per ICH guidelines. This method was also suitable for the assay determination of ZTP in pharmaceutical dosage forms. The DPs were characterized by LC-MS/MS and their fragmentation pathways were proposed.

  20. Selective separation, detection of zotepine and mass spectral characterization of degradants by LC–MS/MS/QTOF

    Directory of Open Access Journals (Sweden)

    M.V.N. Kumar Talluri

    2014-04-01

    Full Text Available A simple, precise, accurate stability-indicating gradient reversed-phase high-performance liquid chromatographic (RP–HPLC method was developed for the quantitative determination of zotepine (ZTP in bulk and pharmaceutical dosage forms in the presence of its degradation products (DPs. The method was developed using Phenomenex C18 column (250 mm×4.6 mm i.d., 5 µm with a mobile phase containing a gradient mixture of solvents, A (0.05% trifluoroacetic acid (TFA, pH=3.0 and B (acetonitrile. The eluted compounds were monitored at 254 nm; the run time was within 20.0 min, in which ZTP and its DPs were well separated, with a resolution of >1.5. The stress testing of ZTP was carried out under acidic, alkaline, neutral hydrolysis, oxidative, photolytic and thermal stress conditions. ZTP was found to degrade significantly in acidic, photolytic, thermal and oxidative stress conditions and remain stable in basic and neutral conditions. The developed method was validated with respect to specificity, linearity, limit of detection, limit of quantification, accuracy, precision and robustness as per ICH guidelines. This method was also suitable for the assay determination of ZTP in pharmaceutical dosage forms. The DPs were characterized by LC–MS/MS and their fragmentation pathways were proposed.

  1. Rapid chiral separation of atenolol, metoprolol, propranolol and the zwitterionic metoprolol acid using supercritical fluid chromatography-tandem mass spectrometry - Application to wetland microcosms.

    Science.gov (United States)

    Svan, Alfred; Hedeland, Mikael; Arvidsson, Torbjörn; Jasper, Justin T; Sedlak, David L; Pettersson, Curt E

    2015-08-28

    A method for enantiomeric separation of the three β-blocking agents atenolol, metoprolol, propranolol and the zwitterionic metoprolol acid, a major metabolite of both metoprolol and in environmental matrices also atenolol, has been developed. By use of supercritical fluid chromatography and the polysaccharide-based Chiralpak(®) IB-3, all four compounds were simultaneously enantiomerically separated (Rs>1.5) within 8min. Detection was performed using tandem mass spectrometry, and to avoid isobaric interference between the co-eluting metoprolol and metoprolol acid, the achiral column Acquity(®) UPC(2) BEH 2-EP was attached ahead of to the chiral column. Carbon dioxide with 18% methanol containing 0.5% (v/v) of the additives trifluoroacetic acid and ammonia in a 2:1 molar ratio were used as mobile phase. A post column make-up flow (0.3mL/min) of methanol containing 0.1% (v/v) formic acid was used to enhance the positive electrospray ionization. Detection was carried out using a triple quadrupole mass spectrometer operating in the selected reaction monitoring mode, using one transition per analyte and internal standard. The method was successfully applied for monitoring the enantiomeric fraction change over time in a laboratory scale wetland degradation study. It showed good precision, recovery, sensitivity and low effect of the sample matrix.

  2. Detection of activity and mass spectrometric identification of mouse liver carboxylesterase and aldehyde dehydrogenase separated by non-denaturing two-dimensional electrophoresis after extraction with detergents.

    Science.gov (United States)

    Shimazaki, Youji; Manabe, Takashi

    2005-05-20

    To examine the activities and identity of enzymes associated with organelles such as microsomes and mitochondria, proteins from mouse liver were extracted using the non-ionic detergents Nonidet P-40 (NP-40), polyoxyethylene sorbitan monooleate (Tween 80), polyoxyethylene isooctylphenyl ester (Triton X), n-octyl beta-D-glucoside (octyl glycoside) or anionic detergent sodium dodecylsulfate (SDS) after the removal of cytosolic proteins. The proteins extracted by detergents were separated by non-denaturing two-dimensional electrophoresis (2-DE). The activities of esterase and aldehyde dehydrogenase were retained by non-denaturing 2-DE after treatment with each non-ionic detergent, but the activities were reduced or lost when the proteins were extracted with more than 0.5% SDS. For proteomic analysis of the organelle-associated proteins in mouse liver, proteins were separated by non-denaturing 2-DE and were identified using electrospray ionization tandem mass spectrometry (ESI-MS/MS) after the proteins were solubilized by octyl glycoside, NP-40 and 0.1% SDS. Several organelle-associated proteins such as carboxylesterase, aldehyde dehydrogenase, glucose regulated protein and HSP60 were identified. These results indicate that the activities and identity of detergent-soluble enzymes can be examined by this non-denaturing 2-DE and mass spectrometry.

  3. Indirect chiral separation of new recreational drugs by gas chromatography-mass spectrometry using trifluoroacetyl-L-prolyl chloride as chiral derivatization reagent.

    Science.gov (United States)

    Weiß, Jennifer A; Mohr, Stefan; Schmid, Martin G

    2015-03-01

    New recreational drugs such as amphetamine-, cathinone, and benzofury derivatives gained high popularity on the drug market in recent years. They can be purchased via the Internet from different providers and online portals. Most of these compounds are chiral, which makes the development of chiral separation methods necessary. Besides this, it is useful to find out if the compounds were sold as racemic mixtures. Also, it is important to check whether the new psychoactive compounds contain further ingredients or impurities. The aim of this research was the continuation of the application of a method for indirect chiral separation of 24 new psychoactive compounds recently purchased via the Internet. After derivatization with the chiral derivatization reagent trifluoroacetyl-L-prolyl chloride, chromatographic separation of diastereomers was achieved using a 30 m HP5-MS capillary column. As carrier gas, helium was used with a constant flow of 1.0 ml/min. Three different column temperature programs were tested. Under optimum conditions 13 out of 24 compounds were successfully resolved into their enantiomers obtaining Rs values up to 7.0. The use of a single quadrupole mass spectrometer as the detector allowed the identification of the compounds in multicomponent samples.

  4. Rapid and Green Separation of Mono- and Diesters of Monochloropropanediols by Ultrahigh Performance Supercritical Fluid Chromatography-Mass Spectrometry Using Neat Carbon Dioxide as a Mobile Phase.

    Science.gov (United States)

    Jumaah, Firas; Jędrkiewicz, Renata; Gromadzka, Justyna; Namieśnik, Jacek; Essén, Sofia; Turner, Charlotta; Sandahl, Margareta

    2017-09-20

    This study demonstrates the effect of column selectivity and density of supercritical carbon dioxide (SC-CO2) on the separation of monochloropropanediol (MCPD) esters, known as food toxicants, using SC-CO2 without addition of cosolvent in ultrahigh performance supercritical fluid chromatography-mass spectrometry (UHPSFC-MS). This study shows that over 20 2-monochloropropanediol (2-MCPD) and 3-monochloropropanediol (3-MCPD) mono- and diesters are separated on a 2-picolylamine column in less than 12 min. The presence and position of a hydroxyl group in the structure, the number of unsaturated bonds, and the acyl chain length play a significant role in the separation of MCPD esters. The flow rate, backpressure, and column oven temperature, which affect the density of the mobile phase, were shown to have a substantial impact on retention, efficiency, and selectivity. The developed method was successfully applied for the determination of MCPD esters in refined oils and showed a close to excellent green analysis score using the Analytical Eco-Scale.

  5. Gadolinium speciation with Tetradentate, N-donor extractants for minor actinide/lanthanide separation: an XRD, mass spectrometry and EPR study

    Energy Technology Data Exchange (ETDEWEB)

    Whittaker, D.M. [School of Chemistry, The University of Manchester, Oxford Road, Manchester, M13 9PL (United Kingdom); Sharrad, C.A. [School of Chemical Engineering and Analytical Science, The University of Manchester, Oxford Road, Manchester M13 9PL (United Kingdom); Research Centre for Radwaste and Decommissioning, Dalton Nuclear Institute, The University of Manchester, Oxford Road, Manchester M13 9PL (United Kingdom); Sproules, S. [Photon Science Institute, The University of Manchester, Oxford Road, Manchester M13 9PL (United Kingdom); WestCHEM, School of Chemistry, University of Glasgow, Glasgow G12 8QQ (United Kingdom)

    2013-07-01

    The hydrophobic organic molecules CyMe{sub 4}-BTPhen (1) and CyMe{sub 4}-BTBP (2) have been developed and tuned over many years to be able to separate the trivalent actinides from the trivalent lanthanides (Ln) selectively in bi-phasic solvent extraction processes for the separation of the long-lived radio-toxic minor actinides from spent nuclear fuel. The ability of these N-donor ligands to perform this separation is poorly understood, as is their speciation with the metal ions when extracted into the organic phase. Our previous work has shown Ln{sup 3+} speciation to be largely 1:2 Ln:L in nature with another small molecule, either water or nitrate, occupying a cavity between the tetradentate bound N-donor ligands. The identity of the small molecule changes across the lanthanide series, and here we continue investigations into this speciation. Complexes of these N-donor ligands with Gd{sup 3+} have been synthesised and characterised by X-ray crystallography, mass spectrometry and EPR spectroscopy. We show that the N-donor ligands have no effect on the electronic configuration of Gd{sup 3+} and that the lanthanide contraction with the steric rigidity of the N-donor ligand appears to determine the size of the cavity between the coordinated ligands. This in turn appears to control the identity of the small molecule on the ninth site in the 1:2 Gd:L species. (authors)

  6. Target-guided separation of Bougainvillea glabra betacyanins by direct coupling of preparative ion-pair high-speed countercurrent chromatography and electrospray ionization mass-spectrometry.

    Science.gov (United States)

    Jerz, Gerold; Wybraniec, Sławomir; Gebers, Nadine; Winterhalter, Peter

    2010-07-02

    In this study, preparative ion-pair high-speed countercurrent chromatography was directly coupled to an electrospray ionization mass-spectrometry device (IP-HSCCC/ESI-MS-MS) for target-guided fractionation of high molecular weight acyl-oligosaccharide linked betacyanins from purple bracts of Bougainvillea glabra (Nyctaginaceae). The direct identification of six principal acyl-oligosaccharide linked betacyanins in the mass range between m/z 859 and m/z 1359 was achieved by positive ESI-MS ionization and gave access to the genuine pigment profile already during the proceeding of the preparative separation. Inclusively, all MS/MS-fragmentation data were provided during the chromatographic run for a complete analysis of substitution pattern. On-line purity evaluation of the recovered fractions is of high value in target-guided screening procedures and for immediate decisions about suitable fractions used for further structural analysis. The applied preparative hyphenation was shown to be a versatile screening method for on-line monitoring of countercurrent chromatographic separations of polar crude pigment extracts and also traced some minor concentrated compounds. For the separation of 760mg crude pigment extract the biphasic solvent system tert.-butylmethylether/n-butanol/acetonitrile/water 2:2:1:5 (v/v/v/v) was used with addition of ion-pair forming reagent trifluoroacetic acid. The preparative HSCCC-eluate had to be modified by post-column addition of a make-up solvent stream containing formic acid to reduce ion-suppression caused by trifluoroacetic acid and later significantly maximized response of ESI-MS/MS detection of target substances. A variable low-pressure split-unit guided a micro-eluate to the ESI-MS-interface for sensitive and direct on-line detection, and the major volume of the effluent stream was directed to the fraction collector for preparative sample recovery. The applied make-up solvent mixture significantly improved smoothness of the continuously

  7. Associations of adult separation anxiety disorder with conflict-related trauma, ongoing adversity, and the psychosocial disruptions of mass conflict among West Papuan refugees.

    Science.gov (United States)

    Tay, Alvin Kuowei; Rees, Susan; Kareth, Moses; Silove, Derrick

    2016-03-01

    Refugees commonly experience traumatic events that threaten the self and close others, suggesting the possibility that they may experience overlapping symptoms of posttraumatic stress disorder (PTSD) and separation anxiety disorder (SAD). We examine this possibility among West Papua refugees (n = 230) displaced to Port Moresby, Papua New Guinea. We also examine associations between the combined PTSD-SAD construct and indices of past trauma exposure, ongoing adversity, and the psychosocial disruptions caused by mass conflict and displacement. We applied culturally adapted interview modules to assess symptoms of PTSD, SAD, traumatic events (TEs), ongoing adversity, and 5 psychosocial dimensions. Latent class analysis identified a PTSD class (23%), a posttraumatic (PT) SAD class (22%), and a low-symptom class (55%). Compared with the low-symptom class, both the PTSD and PT-SAD classes endorsed higher levels of exposure to all domains of TEs (conflict-related trauma, witnessing murder, childhood related adversities, traumatic losses, and health stress) and ongoing adversity (access to health care, displacement/separation, safety in the community, and access to basic needs), but the 2 comorbid groups did not differ on these indices. The PT-SAD class alone scored higher than the low-symptom reference class in relation to disruptions to the psychosocial domains (safety/security, bonds/network, access to justice, roles/identities, existential meaning) and higher than the PTSD class on safety/security, justice and roles/identities. Our findings suggest that the PT-SAD pattern may represent a response to the most severe forms of psychosocial disruptions of mass conflict among refugees. A focus on separation anxiety may enhance psychotherapies designed to treat PTSD in refugees. (PsycINFO Database Record

  8. Biodegradation testing of chemicals with high Henry's constants - Separating mass and effective concentration reveals higher rate constants.

    Science.gov (United States)

    Birch, Heidi; Andersen, Henrik R; Comber, Mike; Mayer, Philipp

    2017-05-01

    During simulation-type biodegradation tests, volatile chemicals will continuously partition between water phase and headspace. This study addressed how (1) this partitioning affects test results and (2) can be accounted for by combining equilibrium partition and dynamic biodegradation models. An aqueous mixture of 9 (semi)volatile chemicals was first generated using passive dosing and then diluted with environmental surface water producing concentrations in the ng/L to μg/L range. After incubation for 2 h to 4 weeks, automated Headspace Solid Phase Microextraction (HS-SPME) was applied directly on the test systems to measure substrate depletion by biodegradation relatively to abiotic controls. HS-SPME was also applied to determine air to water partitioning ratios. Biodegradation rate constants relating to the chemical in the water phase, kwater, were generally a factor 1 to 11 times higher than biodegradation rate constants relating to the total mass of chemical in the test system, ksystem, with one exceptional factor of 72 times for a long chain alkane. True water phase degradation rate constants were found (i) more appropriate for risk assessment than test system rate constants, (ii) to facilitate extrapolation to other air-water systems and (iii) to be better defined input parameters for aquatic exposure and fate models.

  9. [Fast separation and identification of nine carcinogenic dyes in textiles using liquid chromatography-electrospray tandem mass spectrometry].

    Science.gov (United States)

    Ding, Youchao; Cao, Xizhong; Wu, Lina; Zhang, Qian

    2008-09-01

    A qualitative method of the identification of nine carcinogenic dyes prohibited in textiles was developed using high performance liquid chromatography-tandem mass spectrometry interfaced with electro-spray ionization (HPLC-ESI-MS/MS) in the selective reaction monitoring (SRM) mode. The dyes were extracted from textiles composed of natural or chemical fibers by methanol under ultrasounication, and then eluted with gradient by acetonitrile and 5 mmol/L ammonium acetate from an RP-C18 column with two segments in effluents. The first effluents accommodated Acid Red 26, Direct Blue 6, Direct Black 38 and Direct Red 28 with negative ionization mode, while the second accommodated Basic Red 9, Basic Violet 14, Disperse Blue 1, Disperse Orange 11 and Disperse Yellow 3 with positive ionization mode. Thus the investigated compounds could be identified simultaneously with single-run analysis no matter which type of the fibre the sample was and no matter which category of the dye the analyte was. The established method was successfully applied to identify the carcinogenic dyes in textile samples through comparing the chromatographic retention time and the relative abundance of characteristic product ions with the standards.

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

    DEFF Research Database (Denmark)

    Hansen, Elo Harald; Wang, Jianhua

    2002-01-01

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

  11. Separating Autotrophic and Heterotrophic Contributions to Soil Respiration in Maize-Based Agroecosystems Using Stable Carbon Isotope Ratio Mass Spectrometry.

    Science.gov (United States)

    Amos, B.; Walters, D. T.; Madhavan, S.; Arkebauer, T. J.; Scoby, D. L.

    2005-12-01

    Any effort to establish a carbon budget for a growing crop by means of a thorough accounting of all C sources and sinks will require the ability to discriminate between autotrophic and heterotrophic contributions to soil surface CO2 flux. Autotrophic soil respiration (Ra) is defined as combined root respiration and the respiration of soil microorganisms residing in the rhizosphere and using root-derived carbohydrates as an energy source, while heterotrophic respiration (Rh) is defined as the respiration of soil microorganisms and macroorganisms not directly under the influence of the live root system and using SOM as an energy source. We partition soil surface CO2 flux into its autotrophic and heterotrophic components by combining root exclusion with stable carbon isotope techniques in production scale (~65 ha) maize-based agroecosystems. After flux measurements, small chambers are placed on collars in both root excluded shields and in non-root excluded soil, ambient headspace CO2 is removed using a soda lime trap, and soil-respired C is allowed to collect in the chambers. Soil respiration samples are then collected in 12mL evacuated exetainers and analyzed for δ13C by means of a Finnigan Delta-S isotope ratio mass spectrometer interfaced with a Thermo Finnigan GasBench II and a cryogenic trap to increase CO2 concentration. These δ13C measurements were made throughout the 2005 growing season in maize fields representing three agroecosystems: irrigated continuous maize, irrigated maize-soybean rotation, and rainfed maize soybean rotation. Estimates of autotrophic and heterotrophic soil respiration along with other results of this study will be presented.

  12. Determination of Silicon in Gasoline by Directly Measuring under Organic Phase Using Inductively Coupled Plasma Optical Emission Spectroscopy.

    Science.gov (United States)

    Zhang, Wen-mei; Wen, Huan; Lü, Huan-ming; Liu, Hui-qin; Lin, Zhi-sheng; Wang, Rong-hua

    2015-03-01

    A simple and accurate method was developed for determining silicon in gasoline using inductively coupled plasma optical emission spectroscopy (ICP-OES). For sample inroduction a Burgener nubulizer and a Cyclonic spray chamber were used. A gasoline sample was diluted with isooctane and then introduced into the cooled spray chamber of the ICP-OES. Good linearity was achieved in the silicon concentration range 0.1 - 10.0 mg x kg(-1), and the correlation coefficient was 0.999 96. The detection limit for silicon was 0.012 mg x kg(-1) and the silicon recoveries from gasoline samples were 95.8% - 98.4%, with relative standard deviations of less than 3.0% The method was proved to be simple, reliable and highly sensitive, and suitable for determining silicon in samples of motor gasoline, ethanol-gasoline and methanol-gasoline fuel mixtures those containing not more than 15% (V/V) oxygenates.

  13. Nuclear magnetic resonance and liquid chromatography-mass spectrometry combined with an incompleted separation strategy for identifying the natural products in crude extract

    Energy Technology Data Exchange (ETDEWEB)

    Dai Dongmei; He Jiuming [Key Laboratory of Bioactive Substances and Resource Utilization of Chinese Herbal Medicine, Ministry of Education, Institute of Materia Medica, Chinese Academy of Medical Sciences and Peking Union Medical College, 1 Xian Nong Tan Street, Beijing 100050 (China); Sun Ruixiang [Institute of Computing Technology, Chinese Academy of Sciences, Beijing 100080 (China); Zhang Ruiping [Key Laboratory of Bioactive Substances and Resource Utilization of Chinese Herbal Medicine, Ministry of Education, Institute of Materia Medica, Chinese Academy of Medical Sciences and Peking Union Medical College, 1 Xian Nong Tan Street, Beijing 100050 (China); Aisa, Haji Akber [Xinjiang Technological Institute of Physics and Chemistry, Chinese Academy of Sciences, Urumqi 830011 (China); Abliz, Zeper [Key Laboratory of Bioactive Substances and Resource Utilization of Chinese Herbal Medicine, Ministry of Education, Institute of Materia Medica, Chinese Academy of Medical Sciences and Peking Union Medical College, 1 Xian Nong Tan Street, Beijing 100050 (China)], E-mail: zeper@imm.ac.cn

    2009-01-26

    NMR and LC-MS combined with an incompleted separation strategy were proposed to the simultaneous structure identification of natural products in crude extracts, and a novel method termed as NMR/LC-MS parallel dynamic spectroscopy (NMR/LC-MS PDS) was developed to discover the intrinsic correlation between retention time (Rt), mass/charge (m/z) and chemical shift ({delta}) data of the same constituent from mixture spectra by the co-analysis of parallelly visualized multispectroscopic datasets from LC-MS and {sup 1}H NMR. The extracted ion chromatogram (XIC) and {sup 1}H NMR signals deriving from the same individual constituent were correlated through fraction ranges and intensity changing profiles in NMR/LC-MS PDS spectrum due to the signal amplitude co-variation resulted from the concentration variation of constituents in a series of incompletely separated fractions. NMR/LC-MS PDS was applied to identify 12 constituents in an active herbal extract including flavonol glycosides, which was separated into a series of fractions by flash column chromatography. The complementary spectral information of the same individual constituent in the crude extract was discovered simultaneously from mixture spectra. Especially, two groups of co-eluted isomers were identified successfully. The results demonstrated that NMR/LC-MS PDS combined with the incompleted separation strategy achieved the similar function of on-line LC-NMR-MS analysis in off-line mode and had the potential for simplifying and accelerating the analytical routes for structure identification of constituents in herbs or their active extracts.

  14. Antioxidant activity guided separation of major polyphenols of marjoram (Origanum majorana L.) using flash chromatography and their identification by liquid chromatography coupled with electrospray ionization tandem mass spectrometry.

    Science.gov (United States)

    Hossain, Mohammad B; Camphuis, Gabriel; Aguiló-Aguayo, Ingrid; Gangopadhyay, Nirupama; Rai, Dilip K

    2014-11-01

    Marjoram extracts have been separated into polar and nonpolar parts using liquid-liquid extraction. Both polar and nonpolar parts of the extracts were further fractionated by flash chromatography. The obtained fractions (90 polar and 45 nonpolar fractions) were investigated for their antioxidant activities by 2,2-diphenylpicrylhydrazyl and ferric ion reducing antioxidant power assays. A direct, positive, and linear relationship between antioxidant activity and total phenolic content of the fractions was observed. Based on antioxidant and total phenolic content data, the three fractions with the high antioxidant activities from polar and nonpolar part of the extract were analyzed for their constituent polyphenols by liquid chromatography coupled with electrospray ionization tandem mass spectrometry. Compounds were identified by matching the mass spectral data and retention time with those of authentic standards. Identification of the compounds for which there were no "in-house" standards available was carried out by accurate mass measurement of the precursor ions and product ions generated from collision-induced dissociation. Rosmarinic acid was found to be the strongest antioxidant polyphenol conferring the highest antioxidant activity to fractions 47 and 17 of polar and nonpolar part of the extract, respectively. The identification of the rosmarinic acid was further confirmed by (1) H NMR spectroscopy.

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

    Science.gov (United States)

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

    2014-06-01

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

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

    DEFF Research Database (Denmark)

    Hansen, Elo Harald; Wang, Jianhua

    2002-01-01

    Various preconditioning procedures encomprising appropriate separation/preconcentration schemes in order to obtain optimal sensitivity and selectivity characteristics when using electrothermal atomic absorption spectrometry (ETAAS) and inductively coupled plasma mass spectrometry (ICPMS) are pres......Various preconditioning procedures encomprising appropriate separation/preconcentration schemes in order to obtain optimal sensitivity and selectivity characteristics when using electrothermal atomic absorption spectrometry (ETAAS) and inductively coupled plasma mass spectrometry (ICPMS...... prior to detection are effected in a microconduit placed on top of an SI selection valve....

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

    Science.gov (United States)

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

    2008-09-15

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

  18. Separating refractory and non-refractory particulate chloride and estimating chloride depletion by aerosol mass spectrometry in a marine environment

    Directory of Open Access Journals (Sweden)

    I. Nuaaman

    2015-01-01

    Full Text Available Aerosol composition and concentration measurements along the coast of California were obtained using an Aerodyne high-resolution time-of-flight aerosol mass spectrometer (HR-AMS onboard the research vessel Atlantis during the CalNex study in 2010. This paper focuses on the measurement of aerosol chloride using the HR-AMS that can be ambiguous in regions with significant quantities of sea salt aerosols. This ambiguity arises due to large differences in the sensitivity of the HR-AMS to refractory chloride species (i.e., NaCl and non refractory chloride species (i.e., NH4Cl, HCl, etc.. Using the HR-AMS, the aerosol chloride signal is typically quantified using ion signals for 35Cl+, H35Cl+, 37Cl+ and H37Cl+ (HxCl+. During this study, the highest aerosol chloride signal was observed during sea sweep experiments when the source of the aerosol chloride was NaCl present in artificially generated sea salt aerosols even though the HR-AMS has significantly lower sensitivity to such refractory species. Other prominent ion signals that arise from NaCl salt were also observed at m/z 22.99 for Na+ and m/z 57.96 for Na35Cl+ during both sea sweep experiments and during periods of ambient measurements. Thus, refractory NaCl contributes significantly to the HxCl+ signal, interfering with attempts to quantify non sea salt chloride (nssCl. It was found that during ambient aerosol measurements, the interference in the HxCl+ signal from sea salt chloride (ssCl was as high as 89%, but with a study wide average of 10%. The Na35Cl+ ion signal was found to be a good tracer for NaCl. We outline a method to establish nssCl in the ambient aerosols by subtracting the sea salt chloride (ssCl signal from the HxCl+ signal. The ssCl signal is derived from the Na35Cl+ ion tracer signal and the HxCl+ to Na35Cl+ ratio established from the sea sweep experiments. Ambient submicron concentrations of ssCl were also established using the

  19. A THERMAL INFRARED IMAGING STUDY OF VERY LOW MASS, WIDE-SEPARATION BROWN DWARF COMPANIONS TO UPPER SCORPIUS STARS: CONSTRAINING CIRCUMSTELLAR ENVIRONMENTS

    Energy Technology Data Exchange (ETDEWEB)

    Bailey, Vanessa; Hinz, Philip M.; Su, Kate Y. L.; Hoffmann, William F.; Rieke, George; Rodigas, Timothy; Skemer, Andrew; Vaitheeswaran, Vidhya [Steward Observatory, University of Arizona, 933 N. Cherry Ave., Tucson, AZ 85721 (United States); Currie, Thayne [Department of Astronomy and Astrophysics, University of Toronto, 50 St. George Street, Toronto, ON M5S 3H4 (Canada); Esposito, Simone; Pinna, Enrico; Puglisi, Alfio [Osservatorio Astrofisico di Arcetri, Largo Enrico Fermi 5, I-50125 Firenze (Italy); Hill, John M. [Large Binocular Telescope Observatory, University of Arizona, 933 N. Cherry Ave., Tucson, AZ 85721 (United States); Jones, Terry [School of Physics and Astronomy, University of Minnesota, 116 Church St. SE, Minneapolis, MN 55455 (United States); Kim, Jihun [College of Optical Sciences, University of Arizona, 1630 E. University Blvd., Tucson, AZ 85721 (United States); Leisenring, Jarron; Meyer, Michael [Institut fuer Angewandte Physik, Eidgenoessische Technische Hochschule-Zuerich, CH-8093 (Switzerland); Murray-Clay, Ruth; Skrutskie, Michael F. [Harvard-Smithsonian Center for Astrophysics, Harvard University, 60 Garden St., Cambridge, MA 02138 (United States); Nelson, Matthew J., E-mail: vbailey@as.arizona.edu [Department of Astronomy, University of Virginia, Charlottesville, VA 22904 (United States); and others

    2013-04-10

    We present a 3-5 {mu}m LBT/MMT adaptive optics imaging study of three Upper Scorpius stars with brown dwarf (BD) companions with very low masses/mass ratios (M{sub BD} <25 M{sub Jup}; M{sub BD}/M{sub *} Almost-Equal-To 1%-2%) and wide separations (300-700 AU): GSC 06214, 1RXS 1609, and HIP 78530. We combine these new thermal IR data with existing 1-4 {mu}m and 24 {mu}m photometry to constrain the properties of the BDs and identify evidence for circumprimary/circumsecondary disks in these unusual systems. We confirm that GSC 06214B is surrounded by a disk, further showing that this disk produces a broadband IR excess due to small dust near the dust sublimation radius. An unresolved 24 {mu}m excess in the system may be explained by the contribution from this disk. 1RXS 1609B exhibits no 3-4 {mu}m excess, nor does its primary; however, the system as a whole has a modest 24 {mu}m excess, which may come from warm dust around the primary and/or BD. Neither object in the HIP 78530 system exhibits near- to mid-IR excesses. We additionally find that the 1-4 {mu}m colors of HIP 78530B match a spectral type of M3 {+-} 2, inconsistent with the M8 spectral type assigned based on its near-IR spectrum, indicating that it may be a low-mass star rather than a BD. We present new upper limits on additional low-mass companions in the system (<5 M{sub Jup} beyond 175 AU). Finally, we examine the utility of circumsecondary disks as probes of the formation histories of wide BD companions, finding that the presence of a disk may disfavor BD formation near the primary with subsequent outward scattering.

  20. Improvements to the on-line mass separator, RAMA, and the beta-delayed charged-particle emission of proton-rich sd shell nuclei

    Energy Technology Data Exchange (ETDEWEB)

    Ognibene, Theodore Joseph [Lawrence Berkeley National Lab., CA (United States). Nuclear Science Div.

    1996-03-01

    To overcome the extreme difficulties encountered in the experimental decay studies of proton drip line nuclei, several techniques have been utilized, including a helium-jet transport system, particle identification detectors and mass separation. Improvements to the ion source/extraction region of the He-jet coupled on-line Recoil Atom Mass Analyzer (RAMA) and its target/ion source coupling resulted in significant increases in RAMA efficiencies and its mass resolution, as well as reductions in the overall transit time. At the 88-Inch Cyclotron at LBNL, the decays of 31Cl, 27P and 28P, with half-lives of 150 msec, 260 msec and 270.3 msec, respectively, were examined using a he-jet and low-energy gas ΔE-gas ΔE-silicon E detector telescopes. Total beta-delayed proton branches of 0.3% and 0.07% in 31Cl and 27P, respectively, were estimated. Several proton peaks that had been previously assigned to the decay of 31Cl were shown to be from the decay of 25Si. In 27P, two proton groups at 459 ± 14 keV and 610 ± 11 keV, with intensities of 7 ± 3% and 92 ± 4% relative to the main (100%) group were discovered. The Gamow-Teller component of the preceding beta-decay of each observed proton transition was compared to results from shell model calculations. Finally, a new proton transition was identified, following the β-decay of 28P, at 1,444 ± 12 keV with a 1.7 ± 0.5% relative intensity to the 100% group. Using similar low-energy detector telescopes and the mass separator TISOL at TRIUMF, the 109 msec and 173 msec activities, 17Ne and 33Ar, were studied. A new proton group with energy 729 ± 15 keV was observed following the beta-decay of 17Ne. Several discrepancies between earlier works as to the energies, intensities and assignments of several proton transitions from 17Ne and 33Ar were resolved.

  1. Improvements to the on-line mass separator, RAMA, and the beta-delayed charged-particle emission of proton-rich sd shell nuclei

    Energy Technology Data Exchange (ETDEWEB)

    Ognibene, T.J. [Lawrence Berkeley National Lab., CA (United States). Nuclear Science Div.

    1996-03-01

    To overcome the extreme difficulties encountered in the experimental decay studies of proton drip line nuclei, several techniques have been utilized, including a helium-jet transport system, particle identification detectors and mass separation. Improvements to the ion source/extraction region of the He-jet coupled on-line Recoil Atom Mass Analyzer (RAMA) and its target/ion source coupling resulted in significant increases in RAMA efficiencies and its mass resolution, as well as reductions in the overall transit time. At the 88-Inch Cyclotron at LBNL, the decays of {sup 31}Cl, {sup 27}P and {sup 28}P, with half-lives of 150 msec, 260 msec and 270.3 msec, respectively, were examined using a he-jet and low-energy gas {Delta}E-gas {Delta}E-silicon E detector telescopes. Total beta-delayed proton branches of 0.3% and 0.07% in {sup 31}Cl and {sub 27}P, respectively, were estimated. Several proton peaks that had been previously assigned to the decay of {sup 31}Cl were shown to be from the decay of {sup 25}Si. In {sup 27}P, two proton groups at 459 {+-} 14 keV and 610 {+-} 11 keV, with intensities of 7 {+-} 3% and 92 {+-} 4% relative to the main (100%) group were discovered. The Gamow-Teller component of the preceding beta-decay of each observed proton transition was compared to results from shell model calculations. Finally, a new proton transition was identified, following the {beta}-decay of {sup 28}P, at 1,444 {+-} 12 keV with a 1.7 {+-} 0.5% relative intensity to the 100% group. Using similar low-energy detector telescopes and the mass separator TISOL at TRIUMF, the 109 msec and 173 msec activities, {sup 17}Ne and {sup 33}Ar, were studied. A new proton group with energy 729 {+-} 15 keV was observed following the beta-decay of {sup 17}Ne. Several discrepancies between earlier works as to the energies, intensities and assignments of several proton transitions from {sup 17}Ne and {sup 33}Ar were resolved.

  2. Using GPS and absolute gravity observations to separate the effects of present-day and Pleistocene ice-mass changes in South East Greenland

    Science.gov (United States)

    van Dam, T.; Francis, O.; Wahr, J.; Khan, S. A.; Bevis, M.; van den Broeke, M. R.

    2017-02-01

    Measurements of vertical crustal uplift from bedrock sites around the edge of the Greenland ice sheet (GrIS) can be used to constrain present day mass loss. Interpreting any observed crustal displacement around the GrIS in terms of present day changes in ice is complicated, however, by the glacial isostatic adjustment (GIA) signal. With GPS observations alone, it is impossible to separate the uplift driven by present day mass changes from that due to ice mass changes in the past. Wahr et al. (1995) demonstrated that viscoelastic surface displacements were related to the viscoelastic gravity changes through a proportionality constant that is nearly independent of the choice of Earth viscosity or ice history model. Thus, by making measurements of both gravity and surface motion at a bedrock site, the viscoelastic effects could be removed from the observations and we would be able to constrain present day ice mass changes. Alternatively, we could use the same observations of surface displacements and gravity to determine the GIA signal. In this paper, we extend the theory of Wahr et al. (1995) by introducing a constant, Z, that represents the ratio between the elastic changes in gravity and elastic uplift at a particular site due to present day mass changes. Further, we combine 20 yrs of GPS observations of uplift with eight absolute gravity observations over the same period to determine the GIA signal near Kulusuk, a site on the southeastern side of the GrIS, to experimentally demonstrate the theory. We estimate that the GIA signal in the region is 4.49 ± 1.44mm/yr and is inconsistent with most previously reported model predictions that demonstrate that the GIA signal here is negative. However, as there is very little in situ data to constrain the GIA rate in this part of Greenland, the Earth model or the ice history reconstructions could be inaccurate (Khan et al., 2016). Improving the estimate of GIA in this region of Greenland will allow us to better determine

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

    Energy Technology Data Exchange (ETDEWEB)

    Hanley, Traci A.; Saadawi, Ryan; Zhang, Peng; Caruso, Joseph A., E-mail: joseph.caruso@uc.edu; Landero-Figueroa, Julio

    2014-10-01

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

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

    Science.gov (United States)

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

    2014-10-01

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

  5. Detection and quantification of some plant growth regulators in a seaweed-based foliar spray employing a mass spectrometric technique sans chromatographic separation.

    Science.gov (United States)

    Prasad, Kamalesh; Das, Arun Kumar; Oza, Mihir Deepak; Brahmbhatt, Harshad; Siddhanta, Arup Kumar; Meena, Ramavatar; Eswaran, Karuppanan; Rajyaguru, Mahesh Rameshchandra; Ghosh, Pushpito Kumar

    2010-04-28

    The sap expelled from the fresh harvest of Kappaphycus alvarezii , a red seaweed growing in tropical waters, has been reported to be a potent foliar spray. Tandem mass spectrometry of various organic extracts of the sap confirmed the presence of the plant growth regulators (PGRs) indole 3-acetic acid, gibberellin GA(3), kinetin, and zeatin. These PGRs were quantified in fresh state and after 1 year of storage by ESI-MS without recourse to chromatographic separation. Quantification was validated against HPLC data. The results may be useful in correlating with the efficacy of the sap. The methodology was extended to two other seaweeds. The method developed is convenient and precise and may find application in other agricultural formulations containing these growth hormones.

  6. Direct Separation of Pregabalin Enantiomers Using a Zwitterionic Chiral Selector by High Performance Liquid Chromatography Coupled to Mass Spectrometry and Ultraviolet Detection

    Directory of Open Access Journals (Sweden)

    Lakshmi Narayana Chennuru

    2016-11-01

    Full Text Available The chromatographic resolution of pregabalin enantiomers has been often achieved by derivatization of the molecule, in order to reach enough sensitivity at low concentrations of the minor enantiomer present in the active principle. In the present article, the development and optimization of two liquid chromatographic methods are presented for the direct resolution of pregabalin enantiomers on a chiral stationary phase (CSP containing a zwitterionic selector derived from cinchona alkaloid and sulfonic acid (CHIRALPAK ZWIX. The key parameters for the separation as well as the compatibility of chromatographic conditions with different detection modes (ultraviolet and mass spectrometry were investigated. The resulting methods were found to be selective, of high performance and low limits of detection (2 µg/mL by UV and 1 ng/mL by MS, respectively and quantification (6 µg/mL by UV and 5 ng/mL by MS, respectively for the minor enantiomer which is considered as a chiral impurity.

  7. Enhanced capabilities for imaging gangliosides in murine brain with matrix-assisted laser desorption/ionization and desorption electrospray ionization mass spectrometry coupled to ion mobility separation.

    Science.gov (United States)

    Škrášková, Karolina; Claude, Emmanuelle; Jones, Emrys A; Towers, Mark; Ellis, Shane R; Heeren, Ron M A

    2016-07-15

    The increased interest in lipidomics calls for improved yet simplified methods of lipid analysis. Over the past two decades, mass spectrometry imaging (MSI) has been established as a powerful technique for the analysis of molecular distribution of a variety of compounds across tissue surfaces. Matrix-assisted laser desorption/ionization (MALDI) MSI is widely used to study the spatial distribution of common lipids. However, a thorough sample preparation and necessity of vacuum for efficient ionization might hamper its use for high-throughput lipid analysis. Desorption electrospray ionization (DESI) is a relatively young MS technique. In DESI, ionization of molecules occurs under ambient conditions, which alleviates sample preparation. Moreover, DESI does not require the application of an external matrix, making the detection of low mass species more feasible due to the lack of chemical matrix background. However, irrespective of the ionization method, the final information obtained during an MSI experiment is very complex and its analysis becomes challenging. It was shown that coupling MSI to ion mobility separation (IMS) simplifies imaging data interpretation. Here we employed DESI and MALDI MSI for a lipidomic analysis of the murine brain using the same IMS-enabled instrument. We report for the first time on the DESI IMS-MSI of multiply sialylated ganglioside species, as well as their acetylated versions, which we detected directly from the murine brain tissue. We show that poly-sialylated gangliosides can be imaged as multiply charged ions using DESI, while they are clearly separated from the rest of the lipid classes based on their charge state using ion mobility. This represents a major improvement in MSI of intact fragile lipid species. We additionally show that complementary lipid information is reached under particular conditions when DESI is compared to MALDI MSI.

  8. A novel phosphoprotein analysis scheme for assessing changes in premalignant and malignant breast cell lines using 2D liquid separations, protein microarrays and tandem mass spectrometry.

    Science.gov (United States)

    Patwa, Tasneem H; Wang, Yanfei; Miller, Fred R; Goodison, Steve; Pennathur, Subramaniam; Barder, Timothy J; Lubman, David M

    2008-01-01

    An analysis of phosphorylation changes that occur during cancer progression would provide insights into the molecular pathways responsible for a malignant phenotype. In this study we employed a novel coupling of 2D-liquid separations and protein microarray technology to reveal changes in phosphoprotein status between premalignant (AT1) and malignant (CA1a) cell lines derived from the human MCF10A breast cell lines. Intact proteins were first separated according to their isoelectric point and hydrophobicities, then arrayed on SuperAmine glass slides. Phosphoproteins were detected using the universal, inorganic phospho-sensor dye, ProQ Diamond. Using this dye, out of 140 spots that were positive for phosphorylation, a total of 85 differentially expressed spots were detected over a pH range of 7.2 to 4.0. Proteins were identified and their peptides sequenced by mass spectrometry. The strategy enabled the identification of 75 differentially expressed phosphoproteins, from which 51 phosphorylation sites in 27 unique proteins were confirmed. Interestingly, the majority of differentially expressed phosphorylated proteins observed were nuclear proteins. Three regulators of apoptosis, Bad, Bax and Acinus, were also differentially phosphorylated in the two cell lines. Further development of this strategy will facilitate an understanding of the mechanisms involved in malignancy progression and other disease-related phenotypes.

  9. Nanoliter-volume protein enrichment, tryptic digestion, and partial separation based on isoelectric points by CE for MALDI mass spectral analysis.

    Science.gov (United States)

    Nesbitt, Chandra A; Jurcic, Kristina; Yeung, Ken K-C

    2008-01-01

    Sequence-specific proteolysis is an important part of protein identification by MS. Digestion of protein is commonly performed in-solution, in sample vials with volumes ranging from milli- to microliters. When digestion is performed with a sample volume below 1 microL, handling of solution and potential sample loss via adsorption become significant issues. In this report, a proof of concept for the digestion of a small volume protein solution inside a capillary was demonstrated using a discontinuous buffer system previously studied (Nesbitt, C. A., et al. J. Chromatogr. A 2005, 1073, 175-180). Upon voltage application, a pH junction was created by the discontinuous buffer. Using myoglobin as an example, the protein molecules were enriched at the junction with an estimated volume of a few nanoliters. A protease, trypsin, was then introduced to myoglobin at the junction by coenrichment to induce in-capillary digestion. The voltage application was then suspended to provide the necessary time (2 h) for the proteolysis to proceed. When completed, voltage application was resumed, and the discontinuous buffer reconcentrated the peptides formed from digestion. Importantly, the refocused peptides appeared to roughly elute according to their pIs, resulting in a partial separation. Direct sample deposition from capillary was performed to facilitate mass spectral analysis by MALDI. The partial separation, according to pI, offered the potential benefits of MALDI MS signal enhancement and provided supplementary pI information for peptide identity assignment.

  10. Determination of ultralow level 129I/127I in natural samples by separation of microgram carrier free iodine and accelerator mass spectrometry detection.

    Science.gov (United States)

    Hou, Xiaolin; Zhou, Weijian; Chen, Ning; Zhang, Luyuan; Liu, Qi; Luo, Maoyi; Fan, Yukun; Liang, Wangguo; Fu, Yunchong

    2010-09-15

    Separation of carrier free iodine from low iodine level samples and accurate measurement of ultralow level (129)I in micrograms of iodine target are essential but a bottleneck in geological dating of terrestrial system and tracer research using naturally produced (129)I. In this work, we present a carrier free method using coprecipitation of AgI with AgCl for preparing micrograms of iodine target, associated with combustion using a tube furnace for separating iodine from solid samples and anion exchange chromatography for preconcentrating iodine from a large volume of water. An accelerator mass spectrometry was used to measure ultralow level (129)I in micrograms of iodine target. The recovery of iodine in the entire separation procedure is higher than 80% and 65% for solid and water samples, respectively. One microgram iodine in the target (AgI-AgCl) can produce a stable (127)I signal for AMS measurement of (129)I/(127)I, and a detection limit of this method for (129)I is calculated to be 10(5) atoms. This will allow us to accurately determine (129)I in prenuclear geological samples of low iodine concentration with (129)I/(127)I of 10(-12), such as loess, soil, coral, rock, sediment, and groundwater. Some samples with low iodine content have been successfully analyzed, and the lowest value of the (129)I/(127)I ratio of 2 × 10(-11) was observed in 23.5 and 63.5 m loess samples collected in the Loess Plateau, China. The developed method sheds light on a wide application in earth science.

  11. Detection of bacteria from biological mixtures using immunomagnetic separation combined with matrix-assisted laser desorption/ionization time-of-flight mass spectrometry

    Science.gov (United States)

    Madonna, A.J.; Basile, F.; Furlong, E.; Voorhees, K.J.

    2001-01-01

    A rapid method for identifying specific bacteria from complex biological mixtures using immunomagnetic separation coupled to matrix-assisted laser desorption/ionization time-of-flight mass spectrometry has been developed. The technique employs commercially available magnetic beads coated with polycolonal antibodies raised against specific bacteria and whole cell analysis by MALDI-MS. A suspension of a bacterial mixture is mixed with the immunomagnetic beads specific for the target microorganism. After a short incubation period (20 mins) the bacteria captured by the beads are washed, resuspended in deionized H2O and directly applied onto a MALDI probe. Liquid suspensions containing bacterial mixtures can be screened within 1 h total analysis time. Positive tests result in the production of a fingerprint mass spectrum primarily consisting of protein biomarkers characteristic of the targeted microorganism. Using this procedure, Salmonella choleraesuis was isolated and detected from standard bacterial mixtures and spiked samples of river water, human urine, and chicken blood. Copyright ?? 2001 John Wiley & Sons, Ltd.

  12. Chromatographic enrichment and subsequent separation of nickel and vanadyl porphyrins from natural seeps and molecular characterization by positive electrospray ionization FT-ICR mass spectrometry.

    Science.gov (United States)

    Putman, Jonathan C; Rowland, Steven M; Corilo, Yuri E; McKenna, Amy M

    2014-11-04

    We report a novel chromatographic method to enrich and separate nickel and vanadyl porphyrins from a natural seep sample and combine molecular level characterization by positive-ion electrospray ionization Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS). Vanadyl and nickel porphyrin model compound elution from primary secondary amine (PSA) stationary phase combined with UV-vis spectroscopy confirms enrichment and subsequent fractionation of nickel and vanadyl porphyrins into polarity-based subfractions. A more than 100-fold increase in signal-to-noise ratio for nickel porphyrins enables unequivocal elemental composition assignment confirmed by isotopic fine structure for all isotopes >1% relative abundance, and the first mass spectral identification of (61)Ni porphyrin isotopologues derived from natural seeps. Oxygen-containing vanadyl porphyrins and sulfur-containing vanadyl porphyrins are isolated in the same fraction simultaneously from the same sample. We provide the first chromatographic evidence of carboxylic acid functionalities peripheral to the porphyrin core, in agreement with previous studies.

  13. A Thermal Infrared Imaging Study of Very Low-Mass, Wide Separation Brown Dwarf Companions to Upper Scorpius Stars: Constraining Circumstellar Environments

    CERN Document Server

    Bailey, Vanessa; Currie, Thayne; Su, Kate Y L; Esposito, Simone; Hill, John M; Hoffmann, William F; Jones, Terry; Kim, Jihun; Leisenring, Jarron; Meyer, Michael; Murray-Clay, Ruth; Nelson, Matthew J; Pinna, Enrico; Puglisi, Alfio; Rieke, George; Rodigas, Timothy; Skemer, Andrew; Skrutskie, Michael F; Vaitheeswaran, Vidhya; Wilson, John C

    2013-01-01

    We present a 3-5um LBT/MMT adaptive optics imaging study of three Upper Scorpius stars with brown dwarf (BD) companions with very low-masses/mass ratios (M_BD < 25M_Jup; M_BD / M_star ~ 1-2%), and wide separations (300-700 AU): GSC 06214, 1RXS 1609, and HIP 78530. We combine these new thermal IR data with existing 1-4um and 24um photometry to constrain the properties of the BDs and identify evidence for circumprimary/secondary disks in these unusual systems. We confirm that GSC 06214B is surrounded by a disk, further showing this disk produces a broadband IR excess due to small dust near the dust sublimation radius. An unresolved 24um excess in the system may be explained by the contribution from this disk. 1RXS 1609B exhibits no 3-4um excess, nor does its primary; however, the system as a whole has a modest 24um excess, which may come from warm dust around the primary and/or BD. Neither object in the HIP 78530 system exhibits near- to mid-IR excesses. We additionally find that the 1-4um colors of HIP 7853...

  14. Simultaneous determination of 3-monochloropropane-1,2-diol and acrylamide in food by gas chromatography-triple quadrupole mass spectrometry with coupled column separation.

    Science.gov (United States)

    Xu, Xiao-min; He, Hua-li; Zhu, Yan; Feng, Liang; Ying, Ying; Huang, Bai-fen; Shen, Hai-tao; Han, Jian-long; Ren, Yi-ping

    2013-01-14

    Both 3-monochloropropane-1,2-diol (3-MCPD) and acrylamide are contaminants found in heat-processed foods and their related products. A quantitative method was developed for the simultaneous determination of both contaminants in food by gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS). The analytes were purified and extracted by the matrix solid-phase dispersion extraction (MSPDE) technique with Extrelut NT. A coupled column (a 3 m Innowax combined with a 30 m DB-5 ms) was developed to separate both compounds efficiently without derivatization. Triple quadrupole mass spectrometry in multiple reaction monitoring mode (MRM) was applied to suppress matrix interference and obtain good sensitivity in the determination of both analytes. The limit of detection (LOD) in the sample matrix was 5 μg kg(-1) for 3-MCPD or acrylamide. The average recoveries for 3-MCPD and acrylamide in different food matrices were 90.5-107% and 81.9-95.7%, respectively, with the intraday relative standard deviations (RSDs) of 5.6-13.5% and 5.3-13.4%, respectively. The interday RSDs were 6.1-12.6% for 3-MCPD and were 5.0-12.8% for acrylamide. Both contaminants were found in samples of bread, fried chips, fried instant noodles, soy sauce, and instant noodle flavoring. Neither 3-MCPD nor acrylamide was detected in the samples of dairy products (solid or liquid samples) and non-fried instant noodles. Copyright © 2012 Elsevier B.V. All rights reserved.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-06-01

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

  16. Simultaneous preconcentration of copper, zinc, cadmium, and nickel in water samples by cloud point extraction using 4-(2-pyridylazo)-resorcinol and their determination by inductively coupled plasma optic emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Silva, Edson Luiz, E-mail: edsonqmc@hotmail.com [Centro de Energia Nuclear na Agricultura, Universidade de Sao Paulo, Av. Centenario, 303, CP 96, 13416-000 Piracicaba, SP (Brazil); Santos Roldan, Paulo dos [Universidade Federal de Alagoas, Campus A.C. Simoes, Av. Lourival Melo Mota, Tabuleiro do Martins, CEP: 57072-970 AL (Brazil); Gine, Maria Fernanda [Centro de Energia Nuclear na Agricultura, Universidade de Sao Paulo, Av. Centenario, 303, CP 96, 13416-000 Piracicaba, SP (Brazil)

    2009-11-15

    A procedure for simultaneous separation/preconcentration of copper, zinc, cadmium, and nickel in water samples, based on cloud point extraction (CPE) as a prior step to their determination by inductively coupled plasma optic emission spectrometry (ICP-OES), has been developed. The analytes reacted with 4-(2-pyridylazo)-resorcinol (PAR) at pH 5 to form hydrophobic chelates, which were separated and preconcentrated in a surfactant-rich phase of octylphenoxypolyethoxyethanol (Triton X-114). The parameters affecting the extraction efficiency of the proposed method, such as sample pH, complexing agent concentration, buffer amount, surfactant concentration, temperature, kinetics of complexation reaction, and incubation time were optimized and their respective values were 5, 0.6 mmol L{sup -1}, 0.3 mL, 0.15% (w/v), 50 deg. C, 40 min, and 10 min for 15 mL of preconcentrated solution. The method presented precision (R.S.D.) between 1.3% and 2.6% (n = 9). The concentration factors with and without dilution of the surfactant-rich phase for the analytes ranged from 9.4 to 10.1 and from 94.0 to 100.1, respectively. The limits of detection (L.O.D.) obtained for copper, zinc, cadmium, and nickel were 1.2, 1.1, 1.0, and 6.3 {mu}g L{sup -1}, respectively. The accuracy of the procedure was evaluated through recovery experiments on aqueous samples.

  17. Simultaneous preconcentration of copper, zinc, cadmium, and nickel in water samples by cloud point extraction using 4-(2-pyridylazo)-resorcinol and their determination by inductively coupled plasma optic emission spectrometry.

    Science.gov (United States)

    Silva, Edson Luiz; Roldan, Paulo dos Santos; Giné, Maria Fernanda

    2009-11-15

    A procedure for simultaneous separation/preconcentration of copper, zinc, cadmium, and nickel in water samples, based on cloud point extraction (CPE) as a prior step to their determination by inductively coupled plasma optic emission spectrometry (ICP-OES), has been developed. The analytes reacted with 4-(2-pyridylazo)-resorcinol (PAR) at pH 5 to form hydrophobic chelates, which were separated and preconcentrated in a surfactant-rich phase of octylphenoxypolyethoxyethanol (Triton X-114). The parameters affecting the extraction efficiency of the proposed method, such as sample pH, complexing agent concentration, buffer amount, surfactant concentration, temperature, kinetics of complexation reaction, and incubation time were optimized and their respective values were 5, 0.6 mmol L(-1), 0.3 mL, 0.15% (w/v), 50 degrees C, 40 min, and 10 min for 15 mL of preconcentrated solution. The method presented precision (R.S.D.) between 1.3% and 2.6% (n=9). The concentration factors with and without dilution of the surfactant-rich phase for the analytes ranged from 9.4 to 10.1 and from 94.0 to 100.1, respectively. The limits of detection (L.O.D.) obtained for copper, zinc, cadmium, and nickel were 1.2, 1.1, 1.0, and 6.3 microg L(-1), respectively. The accuracy of the procedure was evaluated through recovery experiments on aqueous samples.

  18. Ultrasound- and microwave-assisted extractions followed by hydride generation inductively coupled plasma optical emission spectrometry for lead determination in geological samples.

    Science.gov (United States)

    Welna, Maja; Borkowska-Burnecka, Jolanta; Popko, Malgorzata

    2015-11-01

    Followed the current idea of simplified sample pretratmet before analysis we evaluated the procedure for the determination of Pb in calcium-rich materials such as dolomites after ultrasound- or microwave- assisted extraction with diluted acids using hydride generation inductively coupled plasma optical emission spectrometry (HG-ICP-OES). Corresponding Pb hydride was generated in the reaction of an acidified sample solution with NaBH4 after pre-oxidation of Pb(II) to Pb(IV) by K3[Fe(CN)6]. Several chemical (acidic media: HCl, HNO3 or CH3COOH, concentration of the reductant as well as type and concentration of oxidazing agents) and physical (reagents flow rates, reaction coil length) parameters affecting the efficiency of plumbane formation were optimized in order to improve the detectability of Pb using HG-ICP-OES. Limitation of the method derived from the matrix effects was pointed out. Employing Pb separation by HG technique allows the significant reduction of interferences caused by sample matrix constituents (mainly Ca and Mg), nevertheless they could not be overcame at all, hence calibration based on the standard addition method was recommended for Pb quantification in dolomites. Under the selected conditions, i.e. 0.3 mol L(-1) HCl, HNO3 or CH3COOH, 1.5% NaBH4 and 3.0% K3[Fe(CN)6] the limits of detection (LODs) between 2.3-5.6 μg L(-1) (3.4-6.8 μg L(-1) considering matrix effects) and the precision below 5% were achieved. The accuracy of the procedure was verified by analysis of certified reference materials (NCS DC70308 (Carbonate Rock) and NIST 14000 (Bone Ash)) and recovery test with satisfactory results of Pb recoveries ranging between 94-108% (CRMs analysis) and 92-114% (standard addition method). The applicability of the proposed method was demonstrated by the determination of Pb in dolomites used by different fertiliser factories.

  19. Separation of isomeric short-chain acyl-CoAs in plant matrices using ultra-performance liquid chromatography coupled with tandem mass spectrometry.

    Science.gov (United States)

    Purves, Randy W; Ambrose, Stephen J; Clark, Shawn M; Stout, Jake M; Page, Jonathan E

    2015-02-01

    Acyl coenzyme A (acyl-CoA) thioesters are important intermediates in cellular metabolism and being able to distinguish among them is critical to fully understanding metabolic pathways in plants. Although significant advances have been made in the identification and quantification of acyl-CoAs using liquid chromatography tandem mass spectrometry (LC-MS/MS), separation of isomeric species such as isobutyryl- and n-butyrl-CoA has remained elusive. Here we report an ultra-performance liquid chromatography (UPLC)-MS/MS method for quantifying short-chain acyl-CoAs including isomeric species n-butyryl-CoA and isobutyryl-CoA as well as n-valeryl-CoA and isovaleryl-CoA. The method was applied to the analysis of extracts of hop (Humulus lupulus) and provided strong evidence for the existence of an additional structural isomer of valeryl-CoA, 2-methylbutyryl-CoA, as well as an unexpected isomer of hexanoyl-CoA. The results showed differences in the acyl-CoA composition among varieties of Humulus lupulus, both in glandular trichomes and cone tissues. When compared with the analysis of hemp (Cannabis sativa) extracts, the contribution of isobutyryl-CoAs in hop was greater as would be expected based on the downstream polyketide products. Surprisingly, branched chain valeryl-CoAs (isovaleryl-CoA and 2-methylbutyryl-CoA) were the dominant form of valeryl-CoAs in both hop and hemp. The capability to separate these isomeric forms will help to understand biochemical pathways leading to specialized metabolites in plants.

  20. The non-Newtonian heat and mass transport of He 2 in porous media used for vapor-liquid phase separation. Ph.D. Thesis

    Science.gov (United States)

    Yuan, S. W. K.

    1985-01-01

    This investigation of vapor-liquid phase separation (VLPS) of He 2 is related to long-term storage of cryogenic liquid. The VLPS system utilizes porous plugs in order to generate thermomechanical (thermo-osmotic) force which in turn prevents liquid from flowing out of the cryo-vessel (e.g., Infrared Astronomical Satellite). An apparatus was built and VLPS data were collected for a 2 and a 10 micrometer sintered stainless steel plug and a 5 to 15 micrometer sintered bronze plug. The VLPS data obtained at high temperature were in the nonlinear turbulent regime. At low temperature, the Stokes regime was approached. A turbulent flow model was developed, which provides a phenomenological description of the VLPS data. According to the model, most of the phase separation data are in the turbulent regime. The model is based on concepts of the Gorter-Mellink transport involving the mutual friction known from the zero net mass flow (ZNMF) studies. The latter had to be modified to obtain agreement with the present experimental VLPS evidence. In contrast to the well-known ZNMF mode, the VLPS results require a geometry dependent constant (Gorter-Mellink constant). A theoretical interpretation of the phenomenological equation for the VLPS data obtained, is based on modelling of the dynamics of quantized vortices proposed by Vinen. In extending Vinen's model to the VLPS transport of He 2 in porous media, a correlation between the K*(GM) and K(p) was obtained which permits an interpretation of the present findings. As K(p) is crucial, various methods were introduced to measure the permeability of the porous media at low temperatures. Good agreement was found between the room temperature and the low temperature K(p)-value of the plugs.

  1. Characterizing Low Molecular Weight Organic Matter in Arctic Polygonal Tundra Soils to Identify Biogeochemical Hotspots Using a Dual-Separation, High-Resolution Mass Spectrometry Approach

    Science.gov (United States)

    Ladd, M.; Wullschleger, S. D.; Iversen, C. M.; Hettich, R.

    2016-12-01

    Reliably modeling biogeochemical processes (e.g. decomposition, plant-microbial competition for nutrients) across spatial or temporal scales requires elucidating the chemical composition of low molecular weight (LMW) dissolved soil organic matter (DOM). Our understanding is limited, however, by the wide-ranging physicochemical properties and high fluxes of these compounds, posing major challenges in detection, isolation, and quantification. Here, we developed and evaluated a sensitive, non-targeted approach to characterize LMW DOM in the Arctic, a unique system that is warming at a rate twice that of the global average and may have significant feedbacks to global C and N cycles. Soil cores were collected from a continuous permafrost, polygonal tundra landscape near Barrow, Alaska (71° 16' N) and sectioned into 5 cm increments. Water and salt extracts from each section were filtered and injected onto C18 reversed-phase or zwitterionic-type hydrophilic interaction chromatography (ZIC-pHILIC) columns for separation. LMW DOM profiles were obtained using high-resolution mass spectrometry (HRMS), and unique features, known and unknown, were characterized by LC retention time, accurate mass (m/z), and molecular fragmentation pattern. Coupling two orthogonal chromatographic separations with HRMS enabled the characterization of hundreds of analytes in a single measurement providing enhanced, high-throughput coverage of LMW DOM from soil extracts. The complexity and relative/absolute intensities of LMW DOM features (e.g. organic acids, amino sugars, peptides) varied across polygon type (high- or low-centered), extract condition, and with depth, providing an information-rich, molecular signal of LMW DOM availability across scales. Comprehensively profiling this complex mixture of small molecules of both biotic and abiotic origin provides a chemical signature of biological function, allowing for more reliable predictions of how discrete, molecular-scale processes may control

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

    Energy Technology Data Exchange (ETDEWEB)

    Bezerra, Marcos A. [Universidade Federal da Bahia, Instituto de Quimica, Grupo de Pesquisa em Quimica Analitica, Campus Universitario de Ondina, Salvador, Bahia 40170-290 (Brazil); Universidade Estadual do Sudoeste da Bahia, Laboratorio de Quimica Analitica, Campus de Jequie, Jequie, Bahia 45206-190 (Brazil); Santos, Walter N.L. dos [Departamento de Ciencias Exatas e da Terra, Universidade do Estado da Bahia, R. Silveira Martins, 2555, Salvador, Bahia 41195-001 (Brazil); Lemos, Valfredo A. [Universidade Estadual do Sudoeste da Bahia, Laboratorio de Quimica Analitica, Campus de Jequie, Jequie, Bahia 45206-190 (Brazil)], E-mail: vlemos@uesb.br; Korn, Maria das Gracas A.; Ferreira, Sergio L.C. [Universidade Federal da Bahia, Instituto de Quimica, Grupo de Pesquisa em Quimica Analitica, Campus Universitario de Ondina, Salvador, Bahia 40170-290 (Brazil)

    2007-09-05

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

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

    Directory of Open Access Journals (Sweden)

    Nikolaya Velitchkova

    2013-01-01

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

  4. Solid-Sampling Electrothermal Vaporization Inductively Coupled Plasma Optical Emission Spectrometry for Direct Determination of Total Oxygen in Coal.

    Science.gov (United States)

    Vogt, Thomas; Bauer, Daniela; Nennstiel, David; Otto, Matthias

    2015-10-20

    A new analytical method for direct determination of total oxygen contents in eight coal samples of the Argonne Premium Coal (APC) series and in the NIST SRM 1632d is presented. The development of a suitable calibration procedure, optimization of measurement conditions, and the application of a tailored data processing for handling of plasma effects and high blanks enable the quantification of oxygen simultaneously with other trace, minor, or major elements in whole coal samples by means of electrothermal vaporization inductively coupled plasma optical emission spectrometry (ETV-ICP OES). For comparison, the oxygen contents were determined by a direct oxygen analyzer. The obtained oxygen values of the APC and the reference material NIST SRM 1632d were compared to data in the literature. The precision of the ETV-ICP OES was within ±3.5%, and the recovery better than 92%. With this good accuracy, the developed direct solid sampling method ETV-ICP OES is well suited for the fast determination of oxygen in coals, varying in rank from lignite to semianthracite, in a content range of about 100 ppm up to 27% using 1.5 mg sample weight. This direct analysis method represents an accurate, advantageous alternative to currently used methods for estimation of total oxygen contents in coals.

  5. Direct determination of impurities in high purity silicon carbide by inductively coupled plasma optical emission spectrometry using slurry nebulization technique.

    Science.gov (United States)

    Wang, Zheng; Qiu, Deren; Ni, Zheming; Tao, Guangyi; Yang, Pengyuan

    2006-09-08

    A novel method for the determination of Al, Ca, Cr, Cu, Fe, Mg, Mn, Ni and Ti in high purity silicon carbide (SiC) using slurry introduction axial viewed inductively coupled plasma optical emission spectrometry (ICP-OES) was described. The various sizes of SiC slurry were dispersed by adding dispersant polyethylene imine (PEI). The stability of slurry was characterized by zeta potential measurement, SEM observation and signal stability testing. The optimal concentration of PEI was found to be 0.5 wt% for the SiC slurry. Analytical results of sub-mum size SiC by the slurry introduction were in good accordance with those by the alkaline fusion method which verified that determination could be calibrated by aqueous standards. For mum size SiC, results of most elements have a negative deviation and should be calibrated by the Certified Reference Material slurry. Owing to a rather low contamination in the sample preparation and stability of the slurry, the limits of detection (LODs), which are in the range of 40-2000 ng g(-1), superior to those of the conventional nebulization technique by ICP-OES or ICP-MS.

  6. Separation and analysis of trace volatile formaldehyde in aquatic products by a MoO₃/polypyrrole intercalative sampling adsorbent with thermal desorption gas chromatography and mass spectrometry.

    Science.gov (United States)

    Ma, Yunjian; Zhao, Cheng; Zhan, Yisen; Li, Jianbin; Zhang, Zhuomin; Li, Gongke

    2015-05-01

    An in situ embedded synthesis strategy was developed for the preparation of a MoO3 /polypyrrole intercalative sampling adsorbent for the separation and analysis of trace volatile formaldehyde in aquatic products. Structural and morphological characteristics of the MoO3 /polypyrrole intercalative adsorbent were investigated by a series of characterization methods. The MoO3 /polypyrrole sampling adsorbent possessed a higher sampling capacity and selectivity for polar formaldehyde than commonly used commercial adsorbent Tenax TA. Finally, the MoO3 /polypyrrole adsorbent was packed in the thermal desorption tube that was directly coupled to gas chromatography with mass spectrometry for the analysis of trace volatile formaldehyde in aquatic products. Trace volatile formaldehyde from real aquatic products could be selectively sampled and quantified to be 0.43-6.6 mg/kg. The detection limit was achieved as 0.004 μg/L by this method. Good recoveries for spiked aquatic products were achieved in range of 75.0-108% with relative standard deviations of 1.2-9.0%. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. A supersonic jet target for the cross section measurement of the 12C(α, γ)16O reaction with the recoil mass separator ERNA

    Science.gov (United States)

    Rapagnani, D.; Buompane, R.; Di Leva, A.; Gialanella, L.; Busso, M.; De Cesare, M.; De Stefano, G.; Duarte, J. G.; Gasques, L. R.; Morales Gallegos, L.; Palmerini, S.; Romoli, M.; Tufariello, F.

    2017-09-01

    12C(α, γ)16O cross section plays a key-role in the stellar evolution and nucleosynthesis of massive stars. Hence, it must be determined with the precision of about 10% at the relevant Gamow energy of 300 keV. The ERNA (European Recoil mass separator for Nuclear Astrophysics) collaboration measured, for the first time, the total cross section of 12C(α, γ)16O by means of the direct detection of the 16O ions produced in the reaction down to an energy of Ecm = 1.9 MeV. To extend the measurement at lower energy, it is necessary to limit the extension of the He gas target. This can be achieved using a supersonic jet, where the oblique shock waves and expansion fans formed at its boundaries confine the gas, which can be efficiently collected using a catcher. A test version of such a system has been designed, constructed and experimentally characterized as a bench mark for a full numerical simulation using FV (Finite Volume) methods. The results of the commissioning of the jet test version and the design of the new system that will be used in combination with ERNA are presented and discussed.

  8. High performance liquid chromatography/ion-trap mass spectrometry for separation and simultaneous determination of ethynylestradiol, gestodene, levonorgestrel, cyproterone acetate and desogestrel.

    Science.gov (United States)

    Matejícek, David; Kubán, Vlastimil

    2007-04-11

    A fast and highly sensitive high performance liquid chromatographic/ion-trap mass spectrometric method (LC/MS) has been developed for simultaneous determination of ethynylestradiol (EE2), gestodene (GES), levonorgestrel (LNG), cyproterone acetate (CPA) and desogestrel (DES). Among three types of sorbents tested (C8, C18 and phenyl) from two suppliers, the best separation was achieved on reverse phase Zorbax SB-Phenyl column using aqueous methanol as a mobile phase. A linear gradient profile from 70 up to 100% (v/v) in 7th min, kept constant at 100% up to 10th min and followed by a negative gradient to 70% of methanol up to 12th min was used for elution. Applicability of electrospray ionization (ESI) and atmospheric pressure chemical ionization (APCI) and influence of the mobile phase composition, its flow rate, capillary/vaporizer temperature of API source and in-source fragmentor voltage ionization are discussed. The on-column limits of quantification (10S/N) were 300 pg of EE2, 14 pg of GES and LNG, 4 pg of CPA and 960 pg of DES per injection (1 microL) using APCI with data collection in selected ion monitoring (SIM) mode. The analytical performance of the method was evaluated using the determination of EE2, GES, LNG, CPA and DES in contraceptives and river water samples.

  9. The transesterification of rapeseed and waste sunflower oils: Mass-transfer and kinetics in a laboratory batch reactor and in an industrial-scale reactor/separator setup.

    Science.gov (United States)

    Klofutar, B; Golob, J; Likozar, B; Klofutar, C; Zagar, E; Poljansek, I

    2010-05-01

    We have investigated the transesterification of rapeseed (RO) and waste sunflower (SO) oils with methanol in the presence of potassium hydroxide as a catalyst. The transesterification of tri-acylglycerols was first conducted in a batch reactor. The effect of the temperature on the reaction rates was studied at a constant molar ratio of the alcohol to tri-acylglycerols (6:1) and for a constant concentration of the catalyst (1.0wt%). Size-exclusion chromatography and (1)H NMR spectroscopy were used to quantitatively monitor the transesterification reaction. The mass-transfer coefficients of the tri-acylglycerols during the initial transesterification stage were found to be 0.2-1.2x10(-5)mmin(-1), depending on the type of oil and the temperature. Calculated activation energies implied that at higher temperatures the formation of mono-acylglycerols and glycerole was favored for the SO (93kJ/mol for the forward and 48kJ/mol for the backward reaction) and the RO (47kJ/mol for the forward and 36kJ/mol for the backward reaction), respectively. For the continuous industrial reactor/separator setup, the optimum methanol recycle ratio was established as 0.0550.

  10. Dispersive liquid–liquid microextraction combined with laser-induced breakdown spectrometry and inductively coupled plasma optical emission spectrometry to elemental analysis

    OpenAIRE

    Gaubeur, Ivanise; Aguirre Pastor, Miguel Ángel; Kovachev, Nikolay; Hidalgo Núñez, Montserrat; Canals Hernández, Antonio

    2015-01-01

    In this paper, two analytical methodologies based on the combination of dispersive liquid–liquid microextraction with inductively coupled plasma optical emission spectrometry and laser-induced breakdown spectrometry, respectively, were evaluated for simultaneous preconcentration and detection of Cd, Co, Ni, Pb and Zn. The microextraction procedure was based on the injection of appropriate quantities of 1-undecanol and methanol into the sample solution containing the complexes formed between m...

  11. The determination of trace element concentrations in fly ash samples using ultrasound-assisted digestion followed with inductively coupled plasma optical emission spectrometry

    OpenAIRE

    Ilander, Aki; Väisänen, Ari

    2009-01-01

    A method of ultrasound-assisted digestion followed by inductively coupled plasma optical emission spectrometry (ICP-OES) used for the determination of trace element (chromium, copper, lead, nickel, vanadium and zinc) concentrations in fly ash samples was developed. All the measurements were performed in robust plasma conditions. Ultrasound-assisted digestion procedures using digestion solutions of aqua regia and hydrofluoric acid (HF) resulted in recovery rates of over 80% for all the analyte...

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

    OpenAIRE

    Ilander, Aki; Väisänen, Ari

    2007-01-01

    method of ultrasound-assisted digestion followed by inductively coupled plasma optical emission spectrometry (ICP-OES) used for the determination of toxic element concentrations (arsenic, barium, cobalt, copper, lead, nickel, strontium, vanadium and zinc) in ash samples was developed. All the measurements were performed in robust plasma conditions which were tested by measuring the Mg(II) 280.270 nm/Mg(I) 285.213 nm line intensity ratios. The highest line intensity ratios were observed when a...

  13. A Geochemical Mass-Balance Method for Base-Flow Separation, Upper Hillsborough River Watershed, West-Central Florida, 2003-2005 and 2009

    Science.gov (United States)

    Kish, G.R.; Stringer, C.E.; Stewart, M.T.; Rains, M.C.; Torres, A.E.

    2010-01-01

    Geochemical mass-balance (GMB) and conductivity mass-balance (CMB) methods for hydrograph separation were used to determine the contribution of base flow to total stormflow at two sites in the upper Hillsborough River watershed in west-central Florida from 2003-2005 and at one site in 2009. The chemical and isotopic composition of streamflow and precipitation was measured during selected local and frontal low- and high-intensity storm events and compared to the geochemical and isotopic composition of groundwater. Input for the GMB method included cation, anion, and stable isotope concentrations of surface water and groundwater, whereas input for the CMB method included continuous or point-sample measurement of specific conductance. The surface water is a calcium-bicarbonate type water, which closely resembles groundwater geochemically, indicating that much of the surface water in the upper Hillsborough River basin is derived from local groundwater discharge. This discharge into the Hillsborough River at State Road 39 and at Hillsborough River State Park becomes diluted by precipitation and runoff during the wet season, but retains the calcium-bicarbonate characteristics of Upper Floridan aquifer water. Field conditions limited the application of the GMB method to low-intensity storms but the CMB method was applied to both low-intensity and high-intensity storms. The average contribution of base flow to total discharge for all storms ranged from 31 to 100 percent, whereas the contribution of base flow to total discharge during peak discharge periods ranged from less than 10 percent to 100 percent. Although calcium, magnesium, and silica were consistent markers of Upper Floridan aquifer chemistry, their use in calculating base flow by the GMB method was limited because the frequency of point data collected in this study was not sufficient to capture the complete hydrograph from pre-event base-flow to post-event base-flow concentrations. In this study, pre-event water

  14. Development of a direct hydride generation nebulizer for the determination of selenium by inductively coupled plasma optical emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Carrion, Nereida E-mail: ncarrion@strix.ciens.ucv.ve; Murillo, Miguel; Montiel, Edie; Diaz, Dorfe

    2003-08-15

    A study was conducted to evaluate the performance of a new direct hydride generation nebulizer system for determination of hydride forming elements by inductively coupled plasma optical emission spectroscopy. This system was designed and optimized to obtain the highest sensitivity. Several experimental designs were used for these purposes. To optimize the individual parameters of the system, and to study the interaction between these parameters for both direct hydride generation nebulizers, a central composite orthogonal design with eight factors was set up. Significant behavioral differences were observed in the two direct hydride generation nebulizers studied. Finally, a 70 {mu}m gas orifice nebulizer exhibits a better detection limit than the 120 {mu}m nebulizer. Generally, for determination of selenium, this new direct hydride generation nebulizer system exhibits a linear dynamic range and detection limit (3{sigma}b) of 3 orders of magnitude and 0.2 {mu}g l{sup -1} for selenium, respectively. This new hydride generator is much simpler system that conventional hydride generation systems, which does not need to be changed to work in normal mode with the inductively coupled plasma, since this system may be used for hydride forming elements and those that do not form them. It produces a rapid response with low memory effect. It reduces the interference level of Ni, Co and Cu to 600, 500 and 5 mg l{sup -1}, respectively. The accuracy of the system was verified by the determination of selenium in several standard reference materials of ambient, food and clinical sample matrices. No statistically significant differences (95 confidence level) were obtained between our method and the reference values.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2008-02-15

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

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

    Directory of Open Access Journals (Sweden)

    Petrović Sanja M.

    2016-01-01

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

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

    Science.gov (United States)

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

    2014-11-01

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

  18. Slurry micro-sampling technique for use in argon-helium microwave induced plasma optical emission spectrometry.

    Science.gov (United States)

    Ślachciński, Mariusz

    2016-12-01

    The Flow Focusing Pneumatic Nebulizer (FFPN) working at low liquid flow rates was evaluated for the elemental analysis in slurried samples by argon-helium microwave induced plasma optical emission spectrometry (MIP-OES). The obtained results achieved were compared with commercially available V-groove Babington type nebulizer (VBPN). A univariate approach and the simplex optimization procedure were used to achieve optimized conditions and derive analytical figures of merit. Analytical performance of the micro nebulization system was characterized by a determination of the limits of detection (LODs), the precision (RSDs) and the wash-out times for Ba, Ca, Cd, Cu, Fe, Mg, Mn, Pb and Sr. The experimental concentration detection limits for simultaneous determination, calculated as the concentration giving a signal equal to three times of the standard deviation of the blank (LOD, 3σblank criterion, peak height) were 0.9, 0.2, 0.3, 0.2, 0.3, 0.1, 0.2, 0.4, 0.4 and 0.3ngmL(-1) for Ba, Ca, Cd, Cu, Fe, Mg, Mn, Pb and Sr, respectively. The method offers relatively good precision (RSD ranged from 5% to 8%) for micro-slurry sampling analysis. Analyses of the certified reference materials (NRCC DOLT-2, GBW 07302 and SRM 2710) were performed in order to determine the accuracy available with the presented nebulization systems. The measured contents of elements in the reference materials were in satisfactory agreement with the certified values. In addition, these elements were determined in two real samples. Slurry concentration up to 3% m/v (particles technique. An ultrasonic probe was used to homogenize the slurry in the polypropylene bottle just before its introduction into the nebulizer. The nebulizers exhibited no clogging problems. Copyright © 2016 Elsevier B.V. All rights reserved.

  19. Determination of metals in coal fly ashes using ultrasound-assisted digestion followed by inductively coupled plasma optical emission spectrometry.

    Science.gov (United States)

    Pontes, Fernanda V M; Mendes, Bruna A de O; de Souza, Evelyn M F; Ferreira, Fernanda N; da Silva, Lílian I D; Carneiro, Manuel C; Monteiro, Maria I C; de Almeida, Marcelo D; Neto, Arnaldo A; Vaitsman, Delmo S

    2010-02-05

    A method for determination of Co, Cr, Cu, Fe, Mn, Ni, Ti, V and Zn in coal fly ash samples using ultrasound-assisted digestion followed by inductively coupled plasma optical emission spectrometry (ICP-OES) is proposed. The digestion procedure consisted in the sonication of the previously dried sample with hydrofluoric acid and aqua regia at 80 degrees C for 30 min, elimination of fluorides by heating until dryness for about 1h and dissolution of the residue with nitric acid solution. A classical digestion method, used as comparative method, consisted in the addition of HCl, HNO(3) and HF to 1 g of sample, and heating on a hot plate until dryness for about 6h. The proposed method presents several advantages: it requires lower amounts of sample and reagents, and it is faster. It is also advantageous when compared to the published methods, which also use ultrasound-assisted digestion procedure: lower detection limits for Co, Cu, Ni, V and Zn, and it does not require shaking during the digestion. The detection limits (microg g(-1)) for Co, Cr, Cu, Fe, Mn, Ni, Ti, V and Zn were 0.06, 0.37, 1.0, 25, 0.93, 0.45, 4.0, 1.7 and 4.3, respectively. The results were in good agreement with those obtained by the classical method and reference values. The exception was Cr, which presented low recoveries in classical and proposed methods (83 and 87%, respectively). Also, the concentration for Cu obtained by the proposed method was significantly different from the reference value, in spite of the good recovery (91+/-1%).

  20. Laser-ablation electrospray ionization mass spectrometry with ion mobility separation reveals metabolites in the symbiotic interactions of soybean roots and rhizobia

    Energy Technology Data Exchange (ETDEWEB)

    Stopka, Sylwia A. [Department of Chemistry, W. M. Keck Institute for Proteomics Technology and Applications, The George Washington University, Washington DC 20052 USA; Agtuca, Beverly J. [Divisions of Plant Sciences and Biochemistry, C. S. Bond Life Sciences Center, University of Missouri, Columbia MO 65211 USA; Koppenaal, David W. [Environmental Molecular Sciences Laboratory, Earth and Biological Sciences Directorate, Pacific Northwest National Laboratory, 902 Battelle Boulevard Richland WA 99354 USA; Paša-Tolić, Ljiljana [Environmental Molecular Sciences Laboratory, Earth and Biological Sciences Directorate, Pacific Northwest National Laboratory, 902 Battelle Boulevard Richland WA 99354 USA; Stacey, Gary [Divisions of Plant Sciences and Biochemistry, C. S. Bond Life Sciences Center, University of Missouri, Columbia MO 65211 USA; Vertes, Akos [Department of Chemistry, W. M. Keck Institute for Proteomics Technology and Applications, The George Washington University, Washington DC 20052 USA; Anderton, Christopher R. [Environmental Molecular Sciences Laboratory, Earth and Biological Sciences Directorate, Pacific Northwest National Laboratory, 902 Battelle Boulevard Richland WA 99354 USA

    2017-05-23

    Technologies enabling in situ metabolic profiling of living plant systems are invaluable for understanding physiological processes and could be used for rapid phenotypic screening (e.g., to produce plants with superior biological nitrogen fixing ability). The symbiotic interaction between legumes and nitrogen-fixing soil bacteria results in a specialized plant organ (i.e., root nodule), where the exchange of nutrients between host and endosymbiont occurs. Laser ablation electrospray ionization mass spectrometry (LAESI-MS) is a method that can be performed under ambient conditions requiring minimal sample preparation. Here, we employed LAESI-MS to explore the well-characterized symbiosis between soybean (Glycine max L. Merr.) and its compatible symbiont, Bradyrhizobium japonicum. The utilization of ion mobility separation (IMS) improved the molecular coverage, selectivity, and identification of the detected biomolecules. Specifically, incorporation of IMS resulted in an increase of 153 detected metabolites in the nodule samples. The data presented demonstrates the advantages of using LAESI-IMS-MS for the rapid analysis of intact root nodules, uninfected root segments, and free-living rhizobia. Untargeted pathway analysis revealed several metabolic processes within the nodule (e.g., zeatin, riboflavin, and purine synthesis). Compounds specific to the uninfected root and bacteria were also detected. Lastly, we performed depth-profiling of intact nodules to reveal the location of metabolites to the cortex and inside the infected region, and lateral profiling of sectioned nodules confirmed these molecular distributions. Our results established the feasibility of LAESI-IMS-MS for the analysis and spatial mapping of plant tissues, with its specific demonstration to improve our understanding of the soybean-rhizobial symbiosis.

  1. Mathematical modeling of separated two-phase turbulent reactive flows using a filtered mass density function approach for large eddy simulation

    Science.gov (United States)

    Carrara, Mark David

    2006-04-01

    The overall objective of this dissertation is the development of a modeling and simulation approach for turbulent two-phase chemically reacting flows. A new full velocity-scalar filtered mass density function (FMDF) formulation for large eddy simulation (LES) of a separated two-phase flow is developed. In this formulation several terms require modeling that include important conditionally averaged phase-coupling terms (PCT). To close the PCT a new derivation of the local instantaneous two-phase equations is presented and important identities are derived relating the PCT to surface averages. The formulation is then applied for two particle laden flow cases and solved using a full particle based Monte-Carlo numerical solution procedure. The first case is a temporally developing counter-current mixing layer dilutely seeded with evaporating water droplets. Validation studies reveal excellent agreement of the full particle method to previous hybrid FDF studies and direct numerical simulations for single-phase flows. One-way coupled simulations reveal that the overall dispersion is maximized with unity Stokes number droplets. Two-way coupled simulations reveal the advantages of two FDF approaches where the subgrid variation of droplet properties are explicitly taken into account. Comparisons of the fully-coupled FDF approach are compared to more approximate means of determining phase-coupling based on filtered properties and local and compounded global errors are assessed. The second case considered is the combustion aluminum particles. A new mechanistic model for the ignition and combustion of aluminum particulate is developed that accounts for unsteady heating, melting, heterogeneous surface reactions (HSR) and quasi-steady burning. Results of this model agree well with experimental data for overall burn rates and ignition times. Two-phase simulations of aluminum particulate seeded mixing layer reveal the variations in flame radius resulting in local extinguishment

  2. Comprehensive two-dimensional liquid chromatography: Ion chromatography × reversed-phase liquid chromatography for separation of low-molar-mass organic acids

    NARCIS (Netherlands)

    S.S. Brudin; R.A. Shellie; P.R. Haddad; P.J. Schoenmakers

    2010-01-01

    In the work presented here a novel approach to comprehensive two-dimensional liquid chromatography is evaluated. Ion chromatography is chosen for the first-dimension separation and reversed-phase liquid chromatography is chosen for the second-dimension separation mode. The coupling of these modes is

  3. Rapid chemical separations

    CERN Document Server

    Trautmann, N

    1976-01-01

    A survey is given on the progress of fast chemical separation procedures during the last few years. Fast, discontinuous separation techniques are illustrated by a procedure for niobium. The use of such techniques for the chemical characterization of the heaviest known elements is described. Other rapid separation methods from aqueous solutions are summarized. The application of the high speed liquid chromatography to the separation of chemically similar elements is outlined. The use of the gas jet recoil transport method for nuclear reaction products and its combination with a continuous solvent extraction technique and with a thermochromatographic separation is presented. Different separation methods in the gas phase are briefly discussed and the attachment of a thermochromatographic technique to an on-line mass separator is shown. (45 refs).

  4. Chemical Characterisation of Bulk and Melt-spun Ribbons of NiMnIn Alloy using Inductively Coupled Plasma Optical Emission Spectrometry

    Directory of Open Access Journals (Sweden)

    S.S. Kalyan Kamal

    2011-05-01

    Full Text Available Method development for the analysis of NiMnIn, a new magnetocaloric effect (MCE material using inductively-coupled plasma optical emission spectrometry (ICPOES is discussed. Spectral interference of Ni and Mn on the analysis of In were studied. The process of method validation was carried out using various analytical techniques like conventional wet chemical techniques and instrumental techniques such as atomic absorption spectrometry. All the techniques show a close agreement in values, thus this method could be applied for regular analysis of NiMnIn alloys. A comparative chemical analysis of bulk and melt-spun ribbons of this alloy is also discussed.

  5. A novel phosphoprotein analysis scheme for assessing changes in premalignant and malignant breast cell lines using 2D liquid separations, protein microarrays and tandem mass spectrometry

    OpenAIRE

    Patwa, Tasneem H; Wang, Yanfei; Miller, Fred R.; Goodison, Steve; Pennathur, Subramaniam; Timothy J Barder; David M Lubman

    2008-01-01

    An analysis of phosphorylation changes that occur during cancer progression would provide insights into the molecular pathways responsible for a malignant phenotype. In this study we employed a novel coupling of 2D-liquid separations and protein microarray technology to reveal changes in phosphoprotein status between premalignant (AT1) and malignant (CA1a) cell lines derived from the human MCF10A breast cell lines. Intact proteins were first separated according to their isoelectric point and ...

  6. Separation and identification of polyphenols in apple pomace by high-speed counter-current chromatography and high-performance liquid chromatography coupled with mass spectrometry.

    Science.gov (United States)

    Cao, Xueli; Wang, Cong; Pei, Hairun; Sun, Baoguo

    2009-05-01

    Apple pomace, a by-product in the processing of apple juice, was investigated as a potential source of polyphenols. Two methods of separation and purification of polyphenols from apple pomace extract were established by combination of gel chromatography with high-speed counter-current chromatography (HSCCC) and solvent extraction with HSCCC, respectively. The optimal separation was performed on a Sephadex LH-20 column using gradient aqueous ethanol as eluting solvent from 0% to 100% in increments of 10%. HPLC analysis indicated that main polyphenols existed in fractions eluted between 40% and 50% aqueous ethanol. The fractions of interest from column were separated by HSCCC with the solvent system hexane-ethyl acetate-1% aqueous acetic acid (0.5:9.5:10, v/v/v). Ethyl acetate fractionation of the apple pomace extract followed by direct HSCCC separation by the same solvent system in the volume ratio of 1:9:10 also produced a good separation of the main polyphenols of interest. Six high-purity polyphenols were achieved tentatively and identified by HPLC/MS: chlorogenic acid (1, m/z 354), quercetin-3-glucoside/quercetin-3-glacaside (2, m/z 464), quercetin-3-xyloside (3, m/z 434), phloridzin (4, m/z 436), quercetin-3-arabinoside (5, m/z 434), and quercetin-3-rhamnoside (6, m/z 448). These results provided a preliminary foundation for further development and exploration of apple pomace.

  7. Separation and identification of moxifloxacin impurities in drug substance by high-performance liquid chromatography coupled with ultraviolet detection and Fourier transform ion cyclotron resonance mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    Cai Sheng Wu; Zhi Xin Jia; Bao Ming Ning; Jin Lan Zhang; Song Wu

    2012-01-01

    In this paper,a high-performance liquid chromatography coupled with ultraviolet detection and Fourier transform-ion cyclotron resonance mass spectrometry (HPLC-UV/FTICRMS) method was described for the investigation of impurity profile in moxifloxacin (MOX) drug substance and chemical reference substance.Ten impurities were detected by HPLC-UV,while eight impurities were identified by using the high accurate molecular mass combined with multiple-stage mass spectrometric data and fragmentation rules.In addition,to our knowledge,five impurities were founded for the first time in MOX drug substance.

  8. A gas chromatograph/mass spectrometry method for determining isotopic distributions in organic compounds used in the chemical approach to stable isotope separation

    Energy Technology Data Exchange (ETDEWEB)

    Martinez, A.M.; Spall, W.D.; Smith, B.F.

    1990-01-01

    A variety of gas chromatograph/mass spectrometry (GC/MS) methods have been developed to resolve benzene, benzophenone, anthracene, fluorenone, and their respective stable isotope analogs from other components by gas chromatography. The ratio of stable isotope-labeled material to natural isotopic abundance compounds is determined from the mass spectra averaged across the chromatographic peak. Both total ion and selective ion chromatographic approaches were used for relative data and comparison. 9 refs., 11 tabs.

  9. Electroextraction separation of dyestuffs

    Energy Technology Data Exchange (ETDEWEB)

    Luo, G.S.; Yu, M.J.; Jiang, W.B.; Zhu, S.L.; Dai, Y.Y. [Tsinghua Univ., Beijing (China). Dept. of Chemical Engineering

    1999-03-01

    Electroseparation technologies have prospects for significant growth well into the next century. Electroextraction, a coupled separation technique of solvent extraction with electrophoresis, was used to remove dyestuffs from their aqueous stream. A study on the characteristics of the separation technique was carried out with n-butanol/acid-chrom blue K/water and n-butanol/methyl blue/water as working systems. A continuous separation equipment was designed and sued in this work. The influences of two-phase flow, field strength, and concentration of the feed on the recovery of solute were studied. The results showed that much higher recovery of solute with less solvent consumption could be achieved by using this technique to remove dyes from their aqueous streams, especially for the separation of the dilute solution. When the field strength is increased, the recovery and mass flux increase. When the feed flow rate and the initial solute concentration are increased, the recovery decreases and the mass flux increases.

  10. Oligosaccharide mapping of heparinase I-treated heparins by hydrophilic interaction liquid chromatography separation and online fluorescence detection and electrospray ionization-mass spectrometry characterization.

    Science.gov (United States)

    Galeotti, Fabio; Volpi, Nicola

    2016-05-06

    Oligosaccharide mapping based on enzyme cleavage provides a useful molecular fingerprint of the heparin structure revealing detailed structural information regarding its sequence and the content of part of the ATIII-binding region. This approach is performed by strong-anion exchange (SAX)-HPLC separation which is incompatible with MS requiring purification of oligosaccharides for their conclusive identification. We report a novel oligosaccharide mapping strategy based on the HILIC separation of the main heparin disaccharides/oligosaccharides released by heparinase I, fluorotagged with 2-aminoacridone and on-line detected by a fluorescence detector and characterized by ESI-MS. The application of a polar solvent having a high pH with acetonitrile avoided desulfation enabling a simple and accurate structural oligosaccharide assignment. Oligosaccharide mapping, or merely complete disaccharide composition, may be performed on nanogram-scale by the fluorescence detector vs micrograms useful for classical SAX-HPLC. Additionally, only widely commercially available heparin lyase I is necessary, without the use of expensive heparinases II and III. Contrary to SAX-HPLC, this novel HILIC approach is able to separate and identify the saturated trisulfated disaccharide belonging to the non-reducing end of heparin chains. Finally, the content of 3-O-sulfo groups of the ATIII-binding region is determined.

  11. Separation Logic

    DEFF Research Database (Denmark)

    Reynolds, John C.

    2002-01-01

    expressions) for accessing and modifying shared structures, and for explicit allocation and deallocation of storage. Assertions are extended by introducing a "separating conjunction" that asserts that its sub-formulas hold for disjoint parts of the heap, and a closely related "separating implication". Coupled......, dynamically allocated arrays, and recursive procedures. We will also discuss promising future directions....

  12. Separation of parent homopolymers from poly(ethylene oxide) and polystyrene-based block copolymers by liquid chromatography under limiting conditions of desorption--1. Determination of the suitable molar mass range and optimization of chromatographic conditions.

    Science.gov (United States)

    Rollet, Marion; Pelletier, Bérengère; Altounian, Anaïs; Berek, Dusan; Maria, Sébastien; Phan, Trang N T; Gigmes, Didier

    2015-05-01

    We studied molar mass limits for the LC LCD separation of parent polystyrene (PS) and poly(ethylene oxide) (PEO) homopolymers from PEO/PS based block copolymers and we identified optimized chromatographic conditions. Time delays between barriers and sample injections were 0-2-3'10. Eluent was composed of dimethylformamide (DMF) 40 wt.% and 1-chlorobutane (CLB) 60 wt.%; Barrier 1 (B1), which retained block copolymer, was composed of 100 wt.% CLB and Barrier 2 (B2), which retained PEO, was a mixture of DMF and CLB, which proportions were adjusted to studied block copolymers. With B2 composed of DMF 23 wt.% and CLB 77 wt.%, we obtained successful separation of PS23K-b-PEO35K-b-PS23K (56.5 wt.% of PS, the subscripts indicate the molar mass in kg mol(-1) of each polymer part in the block copolymer) from its parent homopolymers. With B2 adjusted to DMF 30 wt.% and CLB 70 wt.%, PS2.3K-b-PEO3.1K (42.6 wt.% of PS) was also efficiently separated from its parent homopolymers.

  13. The Separation and Quantitation of Peptides with and without Oxidation of Methionine and Deamidation of Asparagine Using Hydrophilic Interaction Liquid Chromatography with Mass Spectrometry (HILIC-MS)

    Science.gov (United States)

    Badgett, Majors J.; Boyes, Barry; Orlando, Ron

    2017-01-01

    Peptides with deamidated asparagine residues and oxidized methionine residues are often not resolved sufficiently to allow quantitation of their native and modified forms using reversed phase (RP) chromatography. The accurate quantitation of these modifications is vital in protein biotherapeutic analysis because they can affect a protein's function, activity, and stability. We demonstrate here that hydrophilic interaction liquid chromatography (HILIC) adequately and predictably separates peptides with these modifications from their native counterparts. Furthermore, coefficients describing the extent of the hydrophilicity of these modifications have been derived and were incorporated into a previously made peptide retention prediction model that is capable of predicting the retention times of peptides with and without these modifications.

  14. CENTRIFUGAL SEPARATORS

    Science.gov (United States)

    Skarstrom, C.

    1959-03-10

    A centrifugal separator is described for separating gaseous mixtures where the temperature gradients both longitudinally and radially of the centrifuge may be controlled effectively to produce a maximum separation of the process gases flowing through. Tbe invention provides for the balancing of increases and decreases in temperature in various zones of the centrifuge chamber as the result of compression and expansions respectively, of process gases and may be employed effectively both to neutralize harmful temperature gradients and to utilize beneficial temperaturc gradients within the centrifuge.

  15. Characterization of Low-mass, Wide-separation Substellar Companions to Stars in Upper Scorpius: Near-infrared Photometry and Spectroscopy

    CERN Document Server

    Lachapelle, François-René; Gagné, Jonathan; Jayawardhana, Ray; Janson, Markus; Helling, Christiane; Witte, Soeren

    2015-01-01

    We present new 0.9-2.45 $\\mu$m spectroscopy ($R \\sim 1000$), and $Y$, $J$, $H$, $K_s$, $L^\\prime$ photometry, obtained at Gemini North, of three low-mass brown dwarf companions on wide orbits around young stars of the Upper Scorpius OB association: HIP 78530 B, [PGZ2001] J161031.9-191305 B, and GSC 06214-00210 B. We use these data to assess the companions' spectral type, temperature, surface gravity and mass, as well as the ability of the BT-Settl and Drift-Phoenix atmosphere models to reproduce the spectral features of young substellar objects. For completeness, we also analyze the archival spectroscopy and photometry of the Upper Scorpius planetary mass companion 1RXS J160929.1-210524 b. Based on a comparison with model spectra we find that the companions, in the above order, have effective temperatures of 2700, 2500, 2300 and 1700 K. These temperatures are consistent with our inferred spectral types, respectively M7 $\\beta$, M9 $\\gamma$, M9 $\\gamma$, and L4 $\\gamma$. From bolometric luminosities estimated ...

  16. Chemical Characterisation of Bulk and Melt-spun Ribbons of NiMnIn alloy using Inductively Coupled Plasma Optical Emission Spectrometry

    Directory of Open Access Journals (Sweden)

    S.S. Kalyan Kamal

    2011-04-01

    Full Text Available Method development for the analysis of NiMnIn, a new magnetocaloric effect (MCE material using inductively coupled plasma optical emission spectrometry (ICPOES is discussed. Spectral interference of Ni and Mn on the analysis of In were studied. The process of method validation was carried out using various analytical techniques like conventional wet chemical techniques and instrumental techniques such as atomic absorption spectrometry. All the techniques show a close agreement in values, thus this method could be applied for regular analysis of NiMnIn alloys. A comparative chemical analysis of bulk and melt-spun ribbons of this alloy is also discussed.Defence Science Journal, 2011, 61(3, pp.270-274, DOI:http://dx.doi.org/10.14429/dsj.61.397

  17. Direct determination of sulfur species in coals from the Argonne premium sample program by solid sampling electrothermal vaporization inductively coupled plasma optical emission spectrometry.

    Science.gov (United States)

    Bauer, Daniela; Vogt, Thomas; Klinger, Mathias; Masset, Patrick Joseph; Otto, Matthias

    2014-10-21

    A new direct solid sampling method for speciation of sulfur in coals by electrothermal vaporization inductively coupled plasma optical emission spectrometry (ETV-ICP OES) is presented. On the basis of the controlled thermal decomposition of coal in an argon atmosphere, it is possible to determine the different sulfur species in addition to elemental sulfur in coals. For the assignment of the obtained peaks from the sulfur transient emission signal, several analytical techniques (reflected light microscopy, scanning electron microscopy with energy dispersive X-ray spectroscopy and X-ray diffraction) were used. The developed direct solid sampling method enables a good accuracy (relative standard deviation ≤ 6%), precision and was applied to determine the sulfur forms in the Argonne premium coals, varying in rank. The generated method is time- and cost-effective and well suited for the fast characterization of sulfur species in coal. It can be automated to a large extent and is applicable for process-accompanying analyses.

  18. [Determination of nine hazardous elements in textiles by inductively coupled plasma optical emission spectrometer after microwave-assisted dilute nitric acid extraction].

    Science.gov (United States)

    Chen, Fei; Xu, Dian-dou; Tang, Xiao-ping; Cao, Jing; Liu, Ya-ting; Deng, Jian

    2012-01-01

    Textiles are easily contaminated by heavy metals in the course of processing. In order to monitor the quality of textiles, a new method was developed for simultaneous determination of arsenic, antimony, lead, cadmium, chromium, cobalt, copper, nickel and mercury in textiles by inductively coupled plasma optical emission spectrometry (ICP-OES) after microwave-assisted dilute nitric acid extraction. After optimizing extraction conditions, we ultimately selected 5% nitric acid as extractant and 5 min as extraction time with the extraction temperature of 120 degrees C and instrument power of 400W in the microwave-assisted extraction procedure. Nine hazardous elements were detected sequentially by ICP-OES. The results showed that the detection limits were 0.3-15 microg x L(-1) and the recoveries 73.6%-105% with the RSDs (n = 3) of 0.1%-3%. The proposed method was successfully used to determine nine elements in cotton, wool, terylene and acrylic.

  19. Separation and characterisation of beta2-microglobulin folding conformers by ion-exchange liquid chromatography and ion-exchange liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Bertoletti, Laura; Regazzoni, Luca; Aldini, Giancarlo; Colombo, Raffaella; Abballe, Franco; Caccialanza, Gabriele; De Lorenzi, Ersilia

    2013-04-10

    In this work we present for the first time the use of ion-exchange liquid chromatography to separate the native form and a partially structured intermediate of the folding of the amyloidogenic protein beta2-microglobulin. Using a strong anion-exchange column that accounts for the differences in charge exposure of the two conformers, a LC-UV method is initially optimised in terms of mobile phase pH, composition and temperature. The preferred mobile phase conditions that afford useful information were found to be 35 mM ammonium formate, pH 7.4 at 25°C. The dynamic equilibrium of the two species is demonstrated upon increasing the concentration of acetonitrile in the protein sample. Then, the chromatographic method is transferred to MS detection and the respective charge state distributions of the separated conformers are identified. The LC-MS results demonstrate that one of the conformers is partially unfolded, compared with the native and more compact species. The correspondence with previous results obtained in free solution by capillary electrophoresis suggest that strong ion exchange LC-MS does not alter beta2-microglobulin conformation and maintains the dynamic equilibrium already observed between the native protein and its folding intermediate.

  20. Development of an on-line flow injection Sr/matrix separation method for accurate, high-throughput determination of Sr isotope ratios by multiple collector-inductively coupled plasma-mass spectrometry.

    Science.gov (United States)

    Galler, Patrick; Limbeck, Andreas; Boulyga, Sergei F; Stingeder, Gerhard; Hirata, Takafumi; Prohaska, Thomas

    2007-07-01

    This work introduces a newly developed on-line flow injection (FI) Sr/Rb separation method as an alternative to the common, manual Sr/matrix batch separation procedure, since total analysis time is often limited by sample preparation despite the fast rate of data acquisition possible by inductively coupled plasma-mass spectrometers (ICPMS). Separation columns containing approximately 100 muL of Sr-specific resin were used for on-line FI Sr/matrix separation with subsequent determination of (87)Sr/(86)Sr isotope ratios by multiple collector ICPMS. The occurrence of memory effects exhibited by the Sr-specific resin, a major restriction to the repetitive use of this costly material, could successfully be overcome. The method was fully validated by means of certified reference materials. A set of two biological and six geological Sr- and Rb-bearing samples was successfully characterized for its (87)Sr/(86)Sr isotope ratios with precisions of 0.01-0.04% 2 RSD (n = 5-10). Based on our measurements we suggest (87)Sr/(86)Sr isotope ratios of 0.713 15 +/- 0.000 16 (2 SD) and 0.709 31 +/- 0.000 06 (2 SD) for the NIST SRM 1400 bone ash and the NIST SRM 1486 bone meal, respectively. Measured (87)Sr/(86)Sr isotope ratios for five basalt samples are in excellent agreement with published data with deviations from the published value ranging from 0 to 0.03%. A mica sample with a Rb/Sr ratio of approximately 1 was successfully characterized for its (87)Sr/(86)Sr isotope signature to be 0.718 24 +/- 0.000 29 (2 SD) by the proposed method. Synthetic samples with Rb/Sr ratios of up to 10/1 could successfully be measured without significant interferences on mass 87, which would otherwise bias the accuracy and uncertainty of the obtained data.

  1. Separation and analysis of phenolic acids from Salvia miltiorrhiza and its related preparations by off-line two-dimensional hydrophilic interaction chromatography×reversed-phase liquid chromatography coupled with ion trap time-of-flight mass spectrometry.

    Science.gov (United States)

    Sun, Wanyang; Tong, Ling; Miao, Jingzhuo; Huang, Jingyi; Li, Dongxiang; Li, Yunfei; Xiao, Hongting; Sun, Henry; Bi, Kaishun

    2016-01-29

    Salvia miltiorrhiza (SM) is one of the most widely used Traditional Chinese Medicine. Active constituents of SM mainly contain hydrophilic phenolic acids (PAs) and lipophilic tanshinones. However, due to the existing of multiple ester bonds and unsaturated bonds in the structures, PAs have numerous chemical conversion products. Many of them are so low-abundant that hard to be separated using conventional methods. In this study, an off-line two-dimensional liquid chromatography (2D-LC) method was developed to separate PAs in SM and its related preparations. In the first dimension, samples were fractionated by hydrophilic interaction chromatography (HILIC) (Acchrom×Amide, 4.6×250mm, 5μm) mainly based on the hydrogen bonding effects. The fractions were then separated on reversed-phase liquid chromatography (RP-LC) (Acquity HSS T3, 2.1×50mm, 1.7μm) according to hydrophobicity. For the selective identification of PAs, diode array detector (DAD) and electrospray ionization tandem ion trap time-of-flight mass spectrometry (ESI-IT-TOF-MS) were employed. Practical and effective peak capacities of all the samples were greater than 2046 and 1130, respectively, with the orthogonalities ranged from 69.7% to 92.8%, which indicated the high efficiency and versatility of this method. By utilizing the data post-processing techniques, including mass defect filter, neutral loss filter and product ion filter, a total of 265 compounds comprising 196 potentially new PAs were tentatively characterized. Twelve kinds of derivatives, mainly including glycosylated compounds, O-alkylated compounds, condensed compounds and hydrolyzed compounds, constituted the novelty of the newly identified PAs. The HILIC×RP-LC/TOF-MS system expanded our understanding on PAs of S. miltiorrhiza and its related preparations, which could also benefit the separation and characterization of polar constituents in complicated herbal extracts.

  2. GPS Separator HD

    CERN Multimedia

    2016-01-01

    Footage of the 70 degree ISOLDE GPS separator magnet MAG70 as well as the switchyard for the Central Mass and GLM (GPS Low Mass) and GHM (GPS High Mass) beamlines in the GPS separator zone. In the GPS20 vacuum sector equipment such as the long GPS scanner 482 / 483 unit, faraday cup FC 490, vacuum valves and wiregrid piston WG210 and WG475 and radiation monitors can also be seen. Also the RILIS laser guidance and trajectory can be seen, the GPS main beamgate switch box and the actual GLM, GHM and Central Beamline beamgates in the beamlines as well as the first electrostatic quadrupoles for the GPS lines. Close up of the GHM deflector plates motor and connections and the inspection glass at the GHM side of the switchyard.

  3. A compact electron beam ion source with integrated Wien filter providing mass and charge state separated beams of highly charged ions.

    Science.gov (United States)

    Schmidt, M; Peng, H; Zschornack, G; Sykora, S

    2009-06-01

    A Wien filter was designed for and tested with a room temperature electron beam ion source (EBIS). Xenon charge state spectra up to the charge state Xe46+ were resolved as well as the isotopes of krypton using apertures of different sizes. The complete setup consisting of an EBIS and a Wien filter has a length of less than 1 m substituting a complete classical beamline setup. The Wien filter is equipped with removable permanent magnets. Hence total beam current measurements are possible via simple removal of the permanent magnets. In dependence on the needs of resolution a weak (0.2 T) or a strong (0.5 T) magnets setup can be used. In this paper the principle of operation and the design of the Wien filter meeting the requirements of an EBIS are briefly discussed. The first ion beam extraction and separation experiments with a Dresden EBIS are presented.

  4. The Separation and Quantitation of Peptides with and without Oxidation of Methionine and Deamidation of Asparagine Using Hydrophilic Interaction Liquid Chromatography with Mass Spectrometry (HILIC-MS).

    Science.gov (United States)

    Badgett, Majors J; Boyes, Barry; Orlando, Ron

    2017-01-03

    Peptides with deamidated asparagine residues and oxidized methionine residues are often not resolved sufficiently to allow quantitation of their native and modified forms using reversed phase (RP) chromatography. The accurate quantitation of these modifications is vital in protein biotherapeutic analysis because they can affect a protein's function, activity, and stability. We demonstrate here that hydrophilic interaction liquid chromatography (HILIC) adequately and predictably separates peptides with these modifications from their native counterparts. Furthermore, coefficients describing the extent of the hydrophilicity of these modifications have been derived and were incorporated into a previously made peptide retention prediction model that is capable of predicting the retention times of peptides with and without these modifications. Graphical Abstract ᅟ.

  5. Accelerated Analyte Uptake on Single Beads in Microliter-scale Batch Separations using Acoustic Streaming: Plutonium Uptake by Anion Exchange for Analysis by Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Paxton, Walter F.; O' Hara, Matthew J.; Peper, Shane M.; Petersen, Steven L.; Grate, Jay W.

    2008-06-01

    The use of acoustic streaming as a non-contact mixing platform to accelerate mass transport-limited diffusion processes in small volume heterogeneous reactions has been investigated. Single bead anion exchange of plutonium at nanomolar and sub-picomolar concentrations in 20 microliter liquid volumes was used to demonstrate the effect of acoustic mixing. Pu uptake rates on individual ~760 micrometer diameter AG 1x4 anion exchange resin beads were determined using acoustic mixing and compared with Pu uptake rates achieved by static diffusion alone. An 82 MHz surface acoustic wave (SAW) device was placed in contact with the underside of a 384-well microplate containing flat-bottomed semiconical wells. Acoustic energy was coupled into the solution in the well, inducing acoustic streaming. Pu uptake rates were determined by the plutonium remaining in solution after specific elapsed time intervals, using liquid scintillation counting (LSC) for nanomolar concentrations and thermal ionization mass spectrometry (TIMS) analysis for the sub-picomolar concentration experiments. It was found that this small batch uptake reaction could be accelerated by a factor of about five-fold or more, depending on the acoustic power applied.

  6. Trace amounts of rare earth elements in high purity samarium oxide by sector field inductively coupled plasma mass spectrometry after separation by HPLC

    Energy Technology Data Exchange (ETDEWEB)

    Pedreira, W.R. [Instituto de Geociencias, Universidade de Brasilia (UnB), 70910-900 Brasilia, DF (Brazil) and Fundacao Jorge Duprat Figueiredo de Seguranca e Medicina do Trabalho (FUNDACENTRO), 05409-002 Sao Paulo, SP (Brazil)]. E-mail: walter.pedreira@fundacentro.gov.br; Queiroz, C.A. [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), 05508-900 Sao Paulo, SP (Brazil); Abrao, A. [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), 05508-900 Sao Paulo, SP (Brazil); Rocha, S.M. [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), 05508-900 Sao Paulo, SP (Brazil); Vasconcellos, M.E. de [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), 05508-900 Sao Paulo, SP (Brazil); Boaventura, G.R. [Instituto de Geociencias, Universidade de Brasilia (UnB), 70910-900 Brasilia, DF (Brazil); Pimentel, M.M. [Instituto de Geociencias, Universidade de Brasilia (UnB), 70910-900 Brasilia, DF (Brazil)

    2006-07-20

    Today there is an increasing need for high purity rare earth compounds in various fields, the optical, the electronics, the ceramic, the nuclear and geochemistry. Samarium oxide has special uses in glass, phosphors, lasers and thermoelectric devices. Calcium chloride crystals treated with samarium have been employed in lasers, which produce light beams intense enough to burn metal. In general, the inductively coupled plasma mass spectrometry (ICP-MS) presents some advantages for trace element analysis, due to high sensitivity and resolution, when compared with other analytical techniques such as ICP optical emission spectrometry (ICP-OES). In this work, sector field inductively coupled plasma mass spectrometry was used. Sixteen elements (Sc, Y and 14 lanthanides) were determined selectively with the ICP-MS system using a concentration gradient method. The detection limits with the ICP-MS system were about 0.2 (La) pg mL{sup -1} to 8 (Gd) pg mL{sup -1}. The %R.S.D. of the methods varying between 0.9 and 1.5% for a set of five (n = 5) replicates was found for the IPEN's material and for the certificate reference sample. Determination of trace REEs in two high pure samarium oxides samples (IPEN and JMC) was performed. IPEN's material is highly pure (>99.99%) and was successfully analyzed without spectral interference (MO{sup +} and MOH{sup +})

  7. Classification of organic aerosol in the atmosphere over Seoul based on chemical group separation using two dimensional gas chromatography-time of flight mass spectrometry (GC×GC TOFMS) data

    Science.gov (United States)

    Jeon, S.; Lim, H. B.; Choi, N.; Lee, J.; Ahn, Y. K.; Kim, Y. P.

    2016-12-01

    Organic aerosols contain thousands of organic compounds and contribute to 20-90% of the total fine aerosol mass. For analyzing organic aerosols, a wide range of analytical techniques have been used such as gas chromatography mass spectrometer (GC/MS), liquid chromatography mass spectrometer (LC/MS), aerosol mass spectrometer (AMS), etc. Among them, comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometer (GCxGC/TOF-MS) can provide higher chemical resolution than AMS and analyze more mass fractions of organic aerosols than GC/MS. In this study, we suggest a new data processing method using GCxGC/TOF-MS data for analyzing organic compounds in the ambient aerosols. TSP samples were collected on the roof of the Asan engineering building, Ewha Womans University, Seoul, South Korea (37.56 °N, 126.94 °E, 20 m above ground level). A total of 67 samples were obtained during summer (August 2013) and winter (January and February 2014) with a PUF sampler (Tisch, TE-1000) on quartz fiber filter. Filters were extracted using accelerated solvent extractor with a mixture of dichloromethane and methanol (3:1, v/v). Total extracts were blown down to 0.5 mL using a nitrogen evaporator (Turbo Vap Ⅱ, caliper Life Sciences). Organic compounds in the TSP samples were separated into 6 chemical groups, depending on their retention time in two dimensions for their volatility and polarity. All area of peaks in each group was summed and variance of total area in each group was compared depending on season and diurnal cycle.

  8. [Non-equilibrium thermodynamic separation theory of nonlinear chromatography. II. The 0-1 model for nonlinear-mass transfer kinetic processes].

    Science.gov (United States)

    Liang, Heng; Jia, Zhenbin

    2007-11-01

    In the optimal design and control of preparative chromatographic processes, the obstacles appear when one tries to link the Wilson' s framework of chromatographic theories based on partial differential equations (PDEs) with the Eulerian presentation to optimal control approaches based on discrete time states, such as Markov decision processes (MDP) or Model predictive control (MPC). In this paper, the 0-1 model is presented to overcome the obstacles for nonlinear transport chromatography (NTC). With the Lagrangian-Eulerian description (L-ED), one solute cell unit is split into two solute cells, one (SCm) in the mobile phase with the linear velocity of the mobile phase, and the other (SCs) in the stationary phase with zero-velocity. The thermodynamic state vector, S(k), which comprises four vector components, i.e., the sequence number, the position and the local solute concentrations in both SCms and SCses, is introduced to describe the local thermodynamic path (LTP) and the macroscopical thermodynamic path (MTP). For the NTC, the LTP is designed for a solute zone to evolve from the state, S(k), to the virtual migration state, S(M), undergoing the virtual net migration sub-process, and then to the state, S(k+1), undergoing the virtual net inter phase mass transfer sub-process in a short time interval. Complete thermodynamic state iterations with the Markov characteristics are derived by using the local equilibrium isotherm and the local lumped mass transfer coefficient. When the local thermodynamic equilibrium is retained, excellent properties, such as consistency, stability, conservation, accuracy, etc., of the numerical solution of the 0-1 model are observed in the theoretical analysis and in the numerical experiments of the nonlinear ideal chromatography. It is found that the 0-1 model could properly link up with the MDP or optimal control approaches based on discrete time states.

  9. Mass spectrometric peptide analysis of 2DE-separated mouse spinal cord and rat hippocampus proteins suggests an NGxG motif of importance for in vivo deamidation.

    Science.gov (United States)

    Mikkat, Stefan; Kischstein, Timo; Kreutzer, Michael; Glocker, Michael O

    2013-06-01

    Asparagine deamidation is a common nonenzymatic post-translational modification comprising the conversion of asparaginyl residues to aspartyl and isoaspartyl residues, respectively. As a result an additional negative charge is introduced that can affect the tertiary structure as well as the biological activity of a protein. Since deamidation reduces the protein's pI value, differentially deamidated forms of a protein can be separated in 2D gels. We have analyzed a dataset of 430 protein spots from 2D gels that contained mouse spinal cord proteins and estimated that roughly 10% of the spots in a Coomassie-stained gel derive from in vivo deamidation at particular asparaginyl residues. Several of the deamidated protein forms, e.g. tropomodulin-2, V-type proton ATPase subunit B, and protein disulfide-isomerase A3 were also found in 2D gels of proteins extracted from rat hippocampus. All identified deamidation sites contained a glycine residue on the carboxyl side of the asparaginyl residue. Strikingly, a second glycine residue at the +3 position was found in the majority of the deamidated peptides. We propose that the NGxG motif confers exceptional susceptibility to in vivo asparagine deamidation.

  10. Separation of intact proteins on γ-ray-induced polymethacrylate monolithic columns: A highly permeable stationary phase with high peak capacity for capillary high-performance liquid chromatography with high-resolution mass spectrometry.

    Science.gov (United States)

    Simone, Patrizia; Pierri, Giuseppe; Foglia, Patrizia; Gasparrini, Francesca; Mazzoccanti, Giulia; Capriotti, Anna Laura; Ursini, Ornella; Ciogli, Alessia; Laganà, Aldo

    2016-01-01

    Polymethacrylate-based monolithic capillary columns, prepared by γ-radiation-induced polymerization, were used to optimize the experimental conditions (nature of the organic modifiers, the content of trifluoroacetic acid and the column temperature) in the separation of nine standard proteins with different hydrophobicities and a wide range of molecular weights. Because of the excellent permeability of the monolithic columns, an ion-pair reversed-phase capillary liquid chromatography with high-resolution mass spectrometry method has been developed by coupling the column directly to the mass spectrometer without a flow-split and using a standard electrospray interface. Additionally, the high working flow and concomitant high efficiency of these columns allowed us to employ a longer column (up to 50 cm) and achieve a peak capacity value superior to 1000. This work is motivated by the need to develop new materials for high-resolution chromatographic separation that combine chemical stability at elevated temperatures (up to 75°C) and a broad pH range, with a high peak capacity value. The advantage of the γ-ray-induced monolithic column lies in the batch-to-batch reproducibility and long-term high-temperature stability. Their proven high loading capacity, recovery, good selectivity and high permeability, moreover, compared well with that of a commercially available poly(styrene-divinylbenzene) monolithic column, which confirms that such monolithic supports might facilitate analysis in proteomics.

  11. Orthogonal separation and identification of long-chain peptides from scorpion Buthus martensi Karsch venom by using two-dimensional mixed-mode reversed phase-reversed phase chromatography coupled to tandem mass spectrometry.

    Science.gov (United States)

    Xu, Junyan; Zhang, Xiuli; Guo, Zhimou; Yan, Jingyu; Yu, Long; Li, Xiuling; Xue, Xingya; Liang, Xinmiao

    2013-03-21

    Peptide components of scorpion venom have been employed as useful pharmacological tools in the study of ion channel function. The isolation of individual components is necessary for determination of their biological significance. Here, we have described a novel reversed phase (RP)/ion exchange stationary phase, Click oligo ethylene glycol (Click OEG), and the chromatographic efficiency of its mixed-mode sorbent in peptide separation experiments. The Click OEG presents a mixed-mode RP/weak anion-exchange type stationary phase at pH 3.5 and mixed-mode RP/weak cation-exchange type stationary phase at pH 6.0, and it was suitable for separation of long-chain peptides in scorpion venom. Subsequently, a two dimensional mixed-mode RP-RP system based Click OEG and C18 with different pH values in two dimensions was developed for orthogonal separation of scorpion venom. Furthermore, two fractions were analyzed in depth, and 11 long-chain peptides were purified and sequences were identified by using tandem mass spectrometry incorporating the tryptic approach. Among these, we isolated six novel peptides including one peptide with a new sequence and five transcript-level peptides, and speculated on their possible bioactivities.

  12. Separation and characterization of phenolic compounds and triterpenoid saponins in licorice (Glycyrrhiza uralensis) using mobile phase-dependent reversed-phase×reversed-phase comprehensive two-dimensional liquid chromatography coupled with mass spectrometry.

    Science.gov (United States)

    Qiao, Xue; Song, Wei; Ji, Shuai; Wang, Qi; Guo, De-an; Ye, Min

    2015-07-10

    Licorice is one of the most popular herbal medicines worldwide. It contains a big array of phenolic compounds (flavonoids, coumarins, and diphenylethanones). Due to high structural diversity, low abundance, and co-elution with licorice saponins, these phenolic compounds are difficult to be separated by conventional chromatography. In this study, a mobile phase-dependent reversed-phase×reversed phase comprehensive two-dimensional liquid chromatography (RP×RP 2DLC) method was established to separate phenolic compounds in licorice (the roots of Glycyrrhiza uralensis). Organic solvents in the mobile phase were optimized to improve orthogonality of the first and second dimensions, and a synchronized gradient mode was used to improve chromatographic resolution. Finally, licorice extracts were eluted with methanol/water/formic acid in the first dimension (Acquity CSH C18 column), and acetonitrile/water/formic acid in the second dimension (Poroshell Phenyl-Hexyl column). By using this 2DLC system, a total of 311 compounds were detected within 40min. The practical and effective peak capacity was 1329 and 524, respectively, and the orthogonality was 79.8%. The structures of 21 selected unknown compounds were tentatively characterized by mass spectrometry, and 8 of them were discovered from G. uralensis for the first time. The mobile phase-dependent 2DLC/MS system could benefit the separation and characterization of natural products in complicated herbal extracts.

  13. Stability of arsenic peptides in plant extracts: off-line versus on-line parallel elemental and molecular mass spectrometric detection for liquid chromatographic separation.

    Science.gov (United States)

    Bluemlein, Katharina; Raab, Andrea; Feldmann, Jörg

    2009-01-01

    The instability of metal and metalloid complexes during analytical processes has always been an issue of an uncertainty regarding their speciation in plant extracts. Two different speciation protocols were compared regarding the analysis of arsenic phytochelatin (As(III)PC) complexes in fresh plant material. As the final step for separation/detection both methods used RP-HPLC simultaneously coupled to ICP-MS and ES-MS. However, one method was the often used off-line approach using two-dimensional separation, i.e. a pre-cleaning step using size-exclusion chromatography with subsequent fraction collection and freeze-drying prior to the analysis using RP-HPLC-ICP-MS and/or ES-MS. This approach revealed that less than 2% of the total arsenic was bound to peptides such as phytochelatins in the root extract of an arsenate exposed Thunbergia alata, whereas the direct on-line method showed that 83% of arsenic was bound to peptides, mainly as As(III)PC(3) and (GS)As(III)PC(2). Key analytical factors were identified which destabilise the As(III)PCs. The low pH of the mobile phase (0.1% formic acid) using RP-HPLC-ICP-MS/ES-MS stabilises the arsenic peptide complexes in the plant extract as well as the free peptide concentration, as shown by the kinetic disintegration study of the model compound As(III)(GS)(3) at pH 2.2 and 3.8. But only short half-lives of only a few hours were determined for the arsenic glutathione complex. Although As(III)PC(3) showed a ten times higher half-life (23 h) in a plant extract, the pre-cleaning step with subsequent fractionation in a mobile phase of pH 5.6 contributes to the destabilisation of the arsenic peptides in the off-line method. Furthermore, it was found that during a freeze-drying process more than 90% of an As(III)PC(3) complex and smaller free peptides such as PC(2) and PC(3) can be lost. Although the two-dimensional off-line method has been used successfully for other metal complexes, it is concluded here that the fractionation and

  14. Geologic interpretations of seismic data Route 128 (Northern Circumferential Highway) cut, and Hopkins Street grade separation stations 1-18 in Wakefield, Mass.

    Science.gov (United States)

    May, James E.; Lineham, Rev. Daniel

    1950-01-01

    The completion of a segment of the Northern Circumferential Highway, Route 126, in Wakefield, Mass., requires an underpass bridge at Hopkins Street, Station 5+50. The plan of the project shows approximately 1800 feet if approach cuts between stations 1 and 18. In October 1945 a preliminary seismic study was made of a segment of this cut between stations 6+50 and 13+30. Four profiles were made at this time and a report was submitted by Newton E. Chute and Rev. Daniel Linhan (file report of January 15). This work showed a relatively shallow (in general, 6 to 12 feet in depth) somewhat irregular bedrock surface between stations 6+50 and 13+50. That data indicated that much of this segment of the cut will be in bedrock. In order to obtain more complete data for the preparation of detailed estimates on the amount of bedrock to be excavated for this segment of the cut, and also to obtain sufficient data for the unexplored segment of the cut, 21 additional seismic traverses were made in September 1949. The present report contains only the results obtained from this later work. The work was performed as a part of a cooperative program of the Massachusetts Department of Public Works and the United States Geological Survey.

  15. Direct coupling of thin-layer chromatography-bioautography with electrostatic field induced spray ionization-mass spectrometry for separation and identification of lipase inhibitors in lotus leaves.

    Science.gov (United States)

    Zhang, Lei; Shi, Jiyao; Tang, Jihe; Cheng, Zhihong; Lu, Xiaohui; Kong, Yao; Wu, Tao

    2017-05-15

    In situ profiling compounds in complex matrices is important technology to develop in analytic chemistry. The aim of this study is to develop a direct coupling method of thin layer chromatography (TLC) to mass spectrometry (MS) via electrostatic field induced spray ionization (EFISI). We proposed a surface treatment method of normal-phase thin layer chromatography (TLC) plates with dimethyl silicone oil coating which successfully allowed TLC to couple to MS via EFISI. Different parameters affecting the ionization efficiency were investigated and optimized, including silicone oil concentrations, air-drying times, applied voltages, and TLC plate types. This optimized TLC-EFISI-MS method was successfully applied to examine lipase inhibitory components present in lotus leaves. Six active alkaloids including three aporphines and three benzylisoquinolines were profiled with their MS(n) (n = 4) data, or with a comparison with reference substances. This is the first report on the coupling EFISI-MS to TLC or TLC bioautography for in situ identification of active natural products. Copyright © 2017 Elsevier B.V. All rights reserved.

  16. Core shell stationary phases for a novel separation of triglycerides in plant oils by high performance liquid chromatography with electrospray-quadrupole-time of flight mass spectrometer.

    Science.gov (United States)

    La Nasa, Jacopo; Ghelardi, Elisa; Degano, Ilaria; Modugno, Francesca; Colombini, Maria Perla

    2013-09-20

    A new method for the analysis of triglycerides (TAGs) in vegetable oils was developed using a Poroshell 120 EC-C18 column (3.0 mm×50 mm, 2.7 μm) with a high resolution ESI-Q-ToF tandem mass spectrometer as detection system. We used an Agilent Poroshell column, which is characterized by a recently developed stationary phase based on non-porous core particles. The results highlighted the advantages of this column in terms of the dramatic improvement in the number of theoretical plates and in low column backpressure. The developed method enabled us to analyze complex mixtures of more than 40 TAGs within less than 25 min and with a low backpressure (lower than 100 bar), and represents the first application of a core-shell stationary phase in reverse phase HPLC using an ESI-Q-ToF as detection system. The method was optimized on standards of TAGs, validated and applied to several plant oils. By a quantitative point of view, the method showed a very good linearity (r(2)>0.999) in the range 0.1-2.4 μg/g; high intra- and inter-day precision both in terms of retention times (RSD%<0.04%) and peak areas (RSD%<0.3%). Limits of detection and quantitation were lower than 0.03 μg/g and 0.10 μg/g, respectively.

  17. Separate Ways: The Mass-Metallicity Relation Does Not Strongly Correlate with Star Formation Rate in SDSS-IV MaNGA Galaxies

    Science.gov (United States)

    Barrera-Ballesteros, J. K.; Sánchez, S. F.; Heckman, T.; Blanc, G. A.; The MaNGA Team

    2017-07-01

    We present the integrated stellar mass-metallicity relation (MZR) for more than 1700 galaxies included in the integral field area SDSS-IV MaNGA survey. The spatially resolved data allow us to determine the metallicity at the same physical scale (effective radius, R eff) using a heterogeneous set of 10 abundance calibrators. In addition to scale factors, the shape of the MZR is similar for all calibrators, consistent with those reported previously using single-fiber and integral field spectroscopy. We compare the residuals of this relation against the star formation rate (SFR) and specific SFR (sSFR). We do not find a strong secondary relation of the MZR with either SFR or sSFR for any of the calibrators, in contrast with previous single-fiber spectroscopic studies. Our results agree with a scenario in which metal enrichment happens at local scales, with global outflows playing a secondary role in shaping the chemistry of galaxies and cold-gas inflows regulating the stellar formation.

  18. The simultaneous separation and determination of chloropropanols in soy sauce and other flavoring with gas chromatography-mass spectrometry in negative chemical and electron impact ionization modes.

    Science.gov (United States)

    Xu, Xiaomin; Ren, Yiping; Wu, Pinggu; Han, Jianlong; Shen, Xianghong

    2006-02-01

    Both gas chromatography-mass spectrometry in electron ionization (GC-MS-EI) and negative chemical ionization (GC-MS-NCI) modes are reported in this paper for the simultaneous determination of 1,3-dichloropropan-2-ol (1,3-DCP), 2,3-dichloropropan-1-ol (2,3-DCP), 3-chloropropane-1,2-diol (3-MCPD) and 2-chloropropane-1,3-diol (2-MCPD) in soy sauce and other flavoring. D(5)-3-MCPD (for 3-MCPD and 2-MCPD) and d(5)-1,3-DCP (for 1,3-DCP and 2,3-DCP) were used as the deuterium isotopic labelled internal standards. The feasibility of using heptafluorobutyric anhydride modified with triethylamine (HFBA-Et(3)N) as a new derivatization reagent to replace heptafluorobutyrylimidazole (HFBI) is proposed. Liquid/liquid extraction with hexane was introduced for high lipid content samples. A small survey was carried out of soy sauces (103 samples) and instant noodles (45 samples) and the applicability of GC-MS-NCI and GC-MS-EI was assessed in these different matrices.

  19. Post-polymerization photografting on methacrylate-based monoliths for separation of intact proteins and protein digests with comprehensive two-dimensional liquid chromatography hyphenated with high-resolution mass spectrometry.

    Science.gov (United States)

    Vonk, Rudy J; Wouters, Sam; Barcaru, Andrei; Vivó-Truyols, Gabriel; Eeltink, Sebastiaan; de Koning, Leo J; Schoenmakers, Peter J

    2015-05-01

    Post-polymerization photografting is a versatile tool to alter the surface chemistry of organic-based monoliths so as to obtain desired stationary phase properties. In this study, 2-acrylamido-2-methyl-1-propanesulfonic acid was grafted to a hydrophobic poly(butyl methacrylate-co-ethylene glycol dimethacrylate) monolith to create a strong cation exchange stationary phase. Both single-step and two-step photografting were addressed, and the effects of grafting conditions were assessed. An experimental design has been applied in an attempt to optimize three of the key parameters of the two-step photografting chemistry, i.e. the grafting time of the initiator, the monomer concentration and the monomer irradiation time. The photografted columns were implemented in a comprehensive two-dimensional column liquid chromatography ( (t) LC ×  (t) LC) workflow and applied for the separation of intact proteins and peptides. A baseline separation of 11 intact proteins was obtained within 20 min by implementing a gradient across a limited RP composition window in the second dimension. (t) LC ×  (t) LC with UV detection was used for the separation of cytochrome c digest, bovine serum insulin digest and a digest of a complex protein mixture. A semi-quantitative estimation of the occupation of separation space, the orthogonality, of the (t) LC ×  (t) LC system yielded 75%. The (t) LC ×  (t) LC setup was hyphenated to a high-resolution Fourier transform ion cyclotron resonance mass spectrometer instrument to identify the bovine serum insulin tryptic peptides and to demonstrate the compatibility with MS analysis.

  20. Impact of the nature and composition of the mobile phase on the mass transfer mechanism in chiral reversed phase liquid chromatography. Application to the minimization of the solvent cost in chiral separations.

    Science.gov (United States)

    Gritti, Fabrice; Guiochon, Georges

    2014-01-31

    The mechanism of mass transfer was studied on a cellulose-based chiral stationary phase (CSP, Lux Cellulose-1) using aqueous mixtures of acetonitrile (50/50-90/10, v/v) or methanol (90/10 and 100/0, v/v) as the mobile phase. An experimental protocol validated in RPLC and HILIC chromatography and recently extended to chiral RPLC was applied. The five mass-transfer contributions (longitudinal diffusion, short-range and long-range eddy dispersion, solid-liquid mass transfer resistances due to finite intra-particle diffusivity and slow adsorption-desorption) to the reduced height equivalent to a theoretical plate (HETP) were measured. The experimental results show that the adsorption rate constants kads of trans-stilbene enantiomers onto the CSP are three times larger with acetonitrile than with methanol as the organic modifier. This is correlated to the decrease of enantioselectivity from 1.4 (in methanol) to only 1.1 (in acetonitrile). The amount of solvent needed to achieve a separation factor of exactly 2.0 was determined. This showed that analysis cost could be reduced seven times by selecting pure methanol as the eluent for a 5cm long column rather than an acetonitrile-water mixture for a longer (20-45cm) column.

  1. HRS Separator

    CERN Multimedia

    2016-01-01

    Footage of the 90 and 60 degree ISOLDE HRS separator magnets in the HRS separator zone. In the two vacuum sectors HRS20 and HRS30 equipment such as the HRS slits SL240, the HRS faraday cup FC300 and wiregrid WG210 can be spotted. Vacuum valves, turbo pumps, beamlines, quadrupoles, water and compressed air connections, DC and signal cabling can be seen throughout the video. The HRS main and user beamgate in the beamline between MAG90 and MAG60 and its switchboxes as well as all vacuum bellows and flanges are shown. Instrumentation such as the HRS scanner unit 482 / 483, the HRS WG470 wiregrid and slits piston can be seen. The different quadrupoles and supports are shown as well as the RILIS guidance tubes and installation at the magnets and the different radiation monitors.

  2. Separation of Two Distinct O-Glycoforms of Human IgA1 by Serial Lectin Chromatography Followed by Mass Spectrometry O-Glycan Analysis.

    Science.gov (United States)

    Lehoux, S; Ju, T

    2017-01-01

    Human immunoglobulin A1 (IgA1), which carries four to six mucin-type O-glycans (O-glycans) on its hinge region (HR), is the most abundant O-glycoprotein in plasma or serum. While normal O-glycans from hematopoietic-originated cells are core 1-based complex structures, many reports showed that the IgA1 from patients with IgA nephropathy (IgAN) carries undergalactosylated or truncated O-glycans such as the Tn antigen and its sialylated version the SialylTn (STn) antigen on the HR. Yet, there is still a debate whether Tn/STn on the HR of IgA1 is specific to the IgA1 from patients with IgAN since these antigens have also been seen in serum IgA1 of healthy individuals. An additional question is whether the O-glycans at all sites on the two HRs of one IgA1 molecule are homogeneous (either all normal or all Tn/STn) or heterogeneous (both normal and Tn/STn O-glycans). To address these questions, we conducted a systematic study on the O-glycans of plasma IgA1 from both IgAN patients and healthy controls using serial HPA and PNA lectin chromatography followed by western blotting and further analysis of O-glycans from HPA-bound and PNA-bound IgA1 fractions by mass spectrometry. Unexpectedly, we found that a variable minor fraction of IgA1 from both IgAN patients and healthy controls had Tn/STn antigens, and that the O-glycoprotein IgA1 molecules from most samples had only two distinct O-glycoforms: one major glycoform with homogeneous normal core 1-based O-glycans and one minor glycoform with homogeneous Tn/STn antigens. These results raised a serious question about the role of Tn/STn antigens on IgA1 in pathogenesis of IgAN, and there is a demand for a practical methodology that any laboratory can utilize to analyze the O-glycans of IgA1. Herein, we describe the methodology we developed in more detail. The method could also be applied to the analysis of any other O-glycosylated proteins.

  3. Development of an enantioselective assay for simultaneous separation of venlafaxine and O-desmethylvenlafaxine by micellar electrokinetic chromatography-tandem mass spectrometry: Application to the analysis of drug-drug interaction.

    Science.gov (United States)

    Liu, Yijin; Jann, Michael; Vandenberg, Chad; Eap, Chin B; Shamsi, Shahab A

    2015-11-13

    To-date, there has been no effective chiral capillary electrophoresis-mass spectrometry (CE-MS) method reported for the simultaneous enantioseparation of the antidepressant drug, venlafaxine (VX) and its structurally-similar major metabolite, O-desmethylvenlafaxine (O-DVX). This is mainly due to the difficulty of identifying MS compatible chiral selector, which could provide both high enantioselectivity and sensitive MS detection. In this work, poly-sodium N-undecenoyl-L,L-leucylalaninate (poly-L,L-SULA) was employed as a chiral selector after screening several dipeptide polymeric chiral surfactants. Baseline separation of both O-DVX and VX enantiomers was achieved in 15 min after optimizing the buffer pH, poly-L,L-SULA concentration, nebulizer pressure and separation voltage. Calibration curves in spiked plasma (recoveries higher than 80%) were linear over the concentration range 150-5000 ng/mL for both VX and O-DVX. The limit of detection (LOD) was found to be as low as 30 ng/mL and 21 ng/mL for O-DVX and VX, respectively. This method was successfully applied to measure the plasma concentrations of human volunteers receiving VX or O-DVX orally when co-administered without and with indinivar therapy. The results suggest that micellar electrokinetic chromatography electrospray ionization-tandem mass spectrometry (MEKC-ESI-MS/MS) is an effective low cost alternative technique for the pharmacokinetics and pharmacodynamics studies of both O-DVX and VX enantiomers. The technique has potential to identify drug-drug interaction involving VX and O-DVX enantiomers while administering indinivar therapy.

  4. Use of factorial design for evaluation of plasma conditions and comparison of two liquid sample introduction systems for an axially viewed inductively coupled plasma optical emission spectrometer

    Energy Technology Data Exchange (ETDEWEB)

    Trevizan, Lilian C. [Grupo de Analise Instrumental Aplicada, Departamento de Quimica, Universidade Federal de Sao Carlos, Caixa Postal 676, Sao Carlos, SP, 13650-970 (Brazil); Vieira, Edivan C. [Grupo de Analise Instrumental Aplicada, Departamento de Quimica, Universidade Federal de Sao Carlos, Caixa Postal 676, Sao Carlos, SP, 13650-970 (Brazil); Embrapa Pecuaria Sudeste, Sao Carlos, SP (Brazil); Nogueira, Ana Rita A. [Embrapa Pecuaria Sudeste, Sao Carlos, SP (Brazil); Nobrega, Joaquim A. [Grupo de Analise Instrumental Aplicada, Departamento de Quimica, Universidade Federal de Sao Carlos, Caixa Postal 676, Sao Carlos, SP, 13650-970 (Brazil)]. E-mail: djan@terra.com.br

    2005-06-30

    A factorial design was applied to evaluate plasma conditions employing the Mg II 280/Mg I 285 nm intensity ratio in an axially viewed inductively coupled plasma optical emission spectrometer using different sample introduction devices: a concentric or a V-groove nebulizer and a cyclonic or a Sturman-Masters spray chamber. Effects of nebulizer gas flow-rate on Mg II/Mg I ratio were different in each introduction system. Robust conditions were obtained at low nebulizer gas flow-rate when using concentric nebulizer with a cyclonic spray chamber or a concentric nebulizer and a Sturman-Masters spray chamber. However, when using a V-groove nebulizer with a Sturman-Masters spray chamber, Mg II/Mg I ratio increased at high nebulizer gas flow-rates. Recovery experiments for a milk standard reference material diluted in water-soluble tertiary amines in both robust and non-robust conditions indicated that the robust condition was reached at higher nebulizer gas flow-rates and led to better accuracy and precision when using a V-groove nebulizer.

  5. Investigation of the direct hydride generation nebulizer for the determination of arsenic, antimony and selenium in inductively coupled plasma optical emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Rojas, Illiana; Murillo, Miguel; Carrion, Nereida; Chirinos, Jose [Centro de Quimica Analitica, Escuela de Quimica, Facultad de Ciencias, Universidad Central de Venezuela, P.O. Box 47102, 1041a, Caracas (Venezuela)

    2003-05-01

    A direct hydride generation nebulizer (DHGN) was explored for introduction of the sample in inductively coupled plasma-optical emission spectrometry (ICP-OES) using radially viewed mode. This simple hydride generation system was constructed in our laboratory and requires similar plasma operating conditions to conventional nebulizer-spray-chamber arrangements. This work was focused on the optimization of the operating conditions for hydride generation and evaluation of the main analytical figures of merit for the determination of As, Sb and Se. The excitation conditions of the ICP-OES instrument operated with the DHGN were also explored. Results showed that the analytical performance of the new system for the determination of As, Sb and Se was superior to that of conventional nebulization systems. The DHGN also enabled the determination of elements that do not form volatile hydrides, but with less sensitivity than conventional nebulization systems. Evaluation of the plasma robustness showed that gases generated in hydride generation do not significantly affects the plasma discharge. Similar to conventional hydride generation techniques, analysis with DHGN was susceptible to non-spectroscopic interferences produced by transition metals. Finally, the utility of the DHGN in practical ICP-OES studies was demonstrated in the determination of trace elements in an oyster tissue standard reference material. (orig.)

  6. Determination of Se in biological samples by axial view inductively coupled plasma optical emission spectrometry after digestion with aqua regia and on-line chemical vapor generation

    Energy Technology Data Exchange (ETDEWEB)

    Santos, Eder Jose dos [Instituto de Tecnologia do Parana (TECPAR), 81350-010 Curitiba, PR (Brazil)], E-mail: eder@tecpar.br; Herrmann, Amanda Beatriz; Kulik de Caires, Suzete [Instituto de Tecnologia do Parana (TECPAR), 81350-010 Curitiba, PR (Brazil); Azzolin Frescura, Vera Lucia; Curtius, Adilson Jose [Departamento de Quimica, Universidade Federal de Santa Catarina (UFSC), 880400-900 Florianopolis, SC (Brazil)

    2009-06-15

    A simple and fast method for the determination of Se in biological samples, including food, by axial view inductively coupled plasma optical emission spectrometry using on-line chemical vapor generation (CVG-ICP OES) is proposed. The concentrations of HCl and NaBH{sub 4}, used in the chemical vapor generation were optimized by factorial analysis. Six certified materials (non-fat milk powder, lobster hepatopancreas, human hair, whole egg powder, oyster tissue, and lyophilised pig kidney) were treated with 10 mL of aqua regia in a microwave system under reflux for 15 min followed by additional 15 min in an ultrasonic bath. The solutions were transferred to a 100 mL volumetric flask and the final volume was made up with water. The Se was determined directly in these solutions by CVG-ICP OES, using the analytical line at 196.026 nm. Calibration against aqueous standards in 10% v/v aqua regia in the concentration range of 0.5-10.0 {mu}g L{sup -} {sup 1} Se(IV) was used for the analysis. The quantification limit, considering a 0.5 g sample weight in a final volume of 100 mL{sup -} {sup 1} was 0.10 {mu}g g{sup -} {sup 1}. The obtained concentration values were in agreement with the total certified concentrations, according to the t-test for a 95% confidence level.

  7. Speciation of inorganic selenium in environmental water samples by inductively coupled plasma optical emission spectrometry after preconcentration by using a mesoporous zirconia coating on coal cinder.

    Science.gov (United States)

    Wei, Xiao-Shu; Wu, Yi-Wei; Han, Li-Juan; Guo, Jing; Sun, Hong-Li

    2014-08-01

    A simple, novel, and selective flow-injection solid-phase extraction with inductively coupled plasma optical emission spectrometry method was developed for the speciation of inorganic selenium in environmental water samples. A mesoporous zirconia film was simply introduced to coat coal cinder by means of the sol-gel technique, and the adsorptive performance of the coated material for Se(IV)/Se(VI) was investigated in different media. Both Se(IV) and Se(VI) can be retained quantitatively by the material in HCl/NaOH (pH 1.0-9.0) media, while only Se(IV) was adsorbed quantitatively in sodium acetate buffer (pH 3.5-6.0). Thus, the assay of Se(VI) is based on subtracting Se(IV) from total selenium by controlling different adsorptive media without employing any redox procedure. Under the optimum conditions, the detection limit of Se(IV) is 9.0 ng/L with an enrichment factor of 100, and the relative standard deviation is 3.6% (n = 9, C = 5.0 ng/mL). The developed method was successfully applied to the speciation of inorganic selenium in environmental water samples with satisfactory results. In order to further verify the accuracy of the developed method, it was applied to analysis of total selenium in GSBZ 50031-94 certified reference environmental water, and the determined values coincided with the certified values very well.

  8. Optimization of an open-focused microwave oven digestion procedure for determination of metals in diesel oil by inductively coupled plasma optical emission spectrometry.

    Science.gov (United States)

    Sant'Ana, Flavio W; Santelli, Ricardo E; Cassella, Alessandra R; Cassella, Ricardo J

    2007-10-01

    This work reports the optimization of a focused microwave assisted procedure for the wet acid dissolution of diesel oil in order to allow the determination of metals in the samples by inductively coupled plasma optical emission spectrometry (ICP-OES). The dissolution process was monitored by measuring residual carbon content (RCC), also by ICP-OES, in the final solutions obtained after application of digestion program. All experimental work was performed using a commercial sample of diesel oil containing 85.74+/-0.13% of carbon. The initial dissolution program comprised three steps: (i) carbonization with H(2)SO(4); (ii) oxidation with HNO(3) and (iii) final oxidation with H(2)O(2). During work it was verified that the first step played an important role on the dissolution process of this kind of sample. It is therefore, necessary to give a detailed optimization of such step. Employing the optimized conditions it was possible to digest 2.5 g of diesel oil with a 40 min-heating program. At these conditions, residual carbon content was always lower than 5%. Optimized methodology was applied in the determination of metals in three diesel oil samples by ICP-OES. Recovery tests were also performed by adding 10 microg of metals, as organic standards, to the samples before digestion. Recovery percentages always higher than 90% were obtained for the metals of interest (Al, Cu, Fe and Ni), except for Zn, which presented recoveries between 70 and 78%.

  9. Determination of arsenic, cadmium, cobalt, chromium, lead, molybdenum, nickel, and selenium in fertilizers by microwave digestion and inductively coupled plasma-optical emission spectrometry detection: collaborative study.

    Science.gov (United States)

    Kane, Peter F; Hall, William L

    2006-01-01

    There is increasing regulatory interest in the non-nutritive metals content of fertilizer materials, but at present there is no consensus analytical method for acid digestion and instrument detection of those elements in fertilizer matrixes. This lack of method standardization has resulted in unacceptable variability of results between fertilizer laboratories performing metals analysis. A method has been developed using microwave digestion with nitric acid at 200 degrees C, followed by inductively coupled plasma-optical emission spectrometry instrument detection, for the elements arsenic, cadmium, cobalt, chromium, molybdenum, nickel, lead, and selenium. The method has been collaboratively studied, and statistical results are here reported. Fourteen collaborators were sent 62 sample materials in a blind duplicate design. Materials represented a broad cross section of fertilizer types, including phosphate ore, manufactured phosphate products, N-P-K blends, organic fertilizers, and micro-nutrient materials. As much as possible within the limit of the number of samples, materials were selected from different regions of the United States and the world. Limit of detection (LOD) was determined using synthetic fertilizers consisting of reagent grade chemicals with near zero levels of the non-nutritive elements, analyzed blindly. Samples with high iron content caused the most variability between laboratories. Most samples reasonably above LOD gave HorRat values within the range 0.5 to 2.0, indicating acceptable method performance according to AOAC guidelines for analyses in the mg/kg range. The method is recommended for AOAC Official First Action status.

  10. The determination of trace element concentrations in fly ash samples using ultrasound-assisted digestion followed with inductively coupled plasma optical emission spectrometry.

    Science.gov (United States)

    Ilander, Aki; Väisänen, Ari

    2009-08-01

    A method of ultrasound-assisted digestion followed by inductively coupled plasma optical emission spectrometry (ICP-OES) used for the determination of trace element (chromium, copper, lead, nickel, vanadium and zinc) concentrations in fly ash samples was developed. All the measurements were performed in robust plasma conditions. Ultrasound-assisted digestion procedures using digestion solutions of aqua regia and hydrofluoric acid (HF) resulted in recovery rates of over 80% for all the analyte elements. Ultrasound-assisted two-step digestion with digestion solutions of 6mL of HNO(3) (Step 1) and 3mL of HNO(3)+3mL of HF (Step 2) resulted in recovery rates of over 92% for all the analyte elements with one exception, chromium, which had a recovery of about 85%. The analysis of SRM 1633b showed that the two-step ultrasound-assisted digestion method developed resulted in chromium, copper, nickel and zinc concentrations higher than the microwave digestion method standardized by the United States Environmental Protection Agency (USEPA method 3052). This is the very first time when a digestion method using ultrasound resulted in higher efficiency than microwave (USEPA method 3052) for chromium and nickel in very hard to dissolve samples. The major advantages of the ultrasound-assisted digestion over microwave digestion is the high treatment rate (about 30 samples simultaneously with a sonication time of 18min) and the possibility to use new sample vessels without a significant increase in costs.

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

    Science.gov (United States)

    Ilander, Aki; Väisänen, Ari

    2007-10-29

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-12-01

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

  13. Determination of heavy metals and their speciation in street dusts by inductively coupled plasma-optical emission spectrometry after a Community Bureau of Reference sequential extraction procedure.

    Science.gov (United States)

    Altundag, Huseyin; Imamoglu, Mustafa; Doganci, Secil; Baysal, Erkan; Albayrak, Sinem; Tuzen, Mustafa

    2013-01-01

    Sequential selective extraction techniques are commonly used to fractionate the solid-phase forms of metals in soils. This procedure provides measurements of extractable metals from media, such as acetic acid (0.11 M), hydroxyl ammonium chloride (0.1 M), hydrogen peroxide (8.8 M) plus ammonium acetate (1 M), and aqua regia stages of the sequential extraction procedure. In this work, the extractable Pb, Cu, Mn, Sr, Ni, V, Fe, Zn, and Cr were evaluated in street dust samples from Sakarya, Turkey, between May and October 2009 using the three-step sequential extraction procedure described by the Community Bureau of Reference (BCR, now the Standards, Measurements, and Testing Programme) of the European Union. The sampling sites were divided into 10 categories; a total of 50 street dusts were analyzed. The determination of multielements in the samples was performed by inductively coupled plasma-optical emission spectrometry. Validation of the proposed method was performed using BCR 701 certified reference material. The results showed good agreement between the obtained and the certified values for the metals analyzed.

  14. Simultaneous extraction and preconcentration of uranium and thorium in aqueous samples by new modified mesoporous silica prior to inductively coupled plasma optical emission spectrometry determination.

    Science.gov (United States)

    Yousefi, Seyed Reza; Ahmadi, Seyed Javad; Shemirani, Farzaneh; Jamali, Mohammad Reza; Salavati-Niasari, Masoud

    2009-11-15

    A new synthesized modified mesoporous silica (MCM-41) using 5-nitro-2-furaldehyde (fural) was applied as an effective sorbent for the solid phase extraction of uranium(VI) and thorium(IV) ions from aqueous solution for the measurement by inductively coupled plasma optical emission spectrometry (ICP OES). The influences of some analytical parameters on the quantitative recoveries of the analyte ions were investigated in batch method. Under optimal conditions, the analyte ions were sorbed by the sorbent at pH 5.5 and then eluted with 1.0 mL of 1.0 mol L(-1) HNO(3). The preconcentration factor was 100 for a 100mL sample volume. The limits of detection (LOD) obtained for uranium(VI) and thorium(IV) were 0.3 microg L(-1). The maximum sorption capacity of the modified MCM-41 was found to be 47 and 49 mg g(-1) for uranium(VI) and thorium(IV), respectively. The sorbent exhibited good stability, reusability, high adsorption capacity and fast rate of equilibrium for sorption/desorption of uranium and thorium ions. The applicability of the synthesized sorbent was examined using CRM and real water samples.

  15. Determination of rare earth elements in waters by inductively coupled plasma optical emission spectrometry after preconcentration with 6-(2-thienyl)-2-pyridinecarboxaldehyde functionalized Amberlite XAD-4 resin.

    Science.gov (United States)

    Karadaş, Cennet; Kara, Derya

    2014-01-01

    A new method has been developed for the determination of rare earth elements (REEs) (Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu) in water samples based on preconcentration with a mini-column packed with 6-(2-thienyl)-2-pyridinecarboxaldehyde functionalized Amberlite XAD-4 resin prior to their determination using inductively coupled plasma optical emission spectrometry (ICP-OES). The optimum experimental parameters for preconcentration of REEs, such as pH of the sample, sample and eluent flow rates and sample volume, were investigated. The optimum pH values for quantitative (90-110%) sorption of the REE ions were between 6.0 and 8.0. The elution process was carried out using 2 mL of 1.0 mol L(-1) HNO3 solution. Under the optimum conditions, detection limits between 0.032 and 0.963 μg L(-1) for a 10 mL sample volume and 0.006 and 0.193 μg L(-1) for a 50 mL sample volume were determined. The proposed method was successfully applied to the determination of REEs in water samples with recoveries in the range of 90.1-110.5%.

  16. Direct High-Precision Measurements of the (87)Sr/(86)Sr Isotope Ratio in Natural Water without Chemical Separation Using Thermal Ionization Mass Spectrometry Equipped with 10(12) Ω Resistors.

    Science.gov (United States)

    Li, Chao-Feng; Guo, Jing-Hui; Chu, Zhu-Yin; Feng, Lian-Jun; Wang, Xuan-Ce

    2015-07-21

    Thermal ionization mass spectrometry (TIMS) allows excellent precision for determining Sr isotope ratios in natural water samples. Traditionally, a chemical separation procedure using cation exchange resin has been employed to obtain a high purity Sr fraction from natural water, which makes sample preparation time-consuming. In this study, we present a rapid and precise method for the direct determination of the Sr isotope ratio of natural water using TIMS equipped with amplifiers with two 10(12) Ω resistors. To eliminate the (87)Rb isobaric interference, Re ribbons are used as filaments, providing a significant advantage over W ribbons in the inhibition of Rb(+) emission, based on systematically examining a series of NIST SRM987 standard doping with various amounts of Rb using Re and W ribbons. To validate the applicability of our method, twenty-two natural water samples, including different water types (rain, snow, river, lake and drinking water), that show a large range in Sr content variations (2.54-922.8 ppb), were collected and analyzed from North and South China. Analytical results show good precision (0.003-0.005%, 2 RSE) and the method was further validated by comparative analysis of the same water with and without chemical separation. The method is simple and rapid, eliminates sample preparation time, and prevents potential contamination during complicated sample-preparation procedures. Therefore, a high sample throughput inherent to the TIMS can be fully utilized.

  17. Redox speciation of final repository relevant elements using separation methods in combination with ICP mass spectrometry; Redoxspeziation von endlagerrelevanten Elementen mit Hilfe von Trennmethoden gekoppelt an ein Massenspektrometer mit induktiv gekoppeltem Plasma

    Energy Technology Data Exchange (ETDEWEB)

    Graser, Carl-Heinrich

    2015-12-18

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

  18. Multivariate optimization by exploratory analysis applied to the determination of microelements in fruit juice by inductively coupled plasma optical emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Santos Froes, Roberta Eliane; Borges Neto, Waldomiro [Departamento de Quimica, Universidade Federal de Minas Gerais, Campus Pampulha, Cx Postal 702, Belo Horizonte, MG, 31270-901 (Brazil); Oliveira Couto e Silva, Nilton; Lopes Pereira Naveira, Rita [Fundacao Ezequiel Diaz, FUNED, Belo Horizonte, MG (Brazil); Nascentes, Clesia Cristina [Departamento de Quimica, Universidade Federal de Minas Gerais, Campus Pampulha, Cx Postal 702, Belo Horizonte, MG, 31270-901 (Brazil)], E-mail: clesia@qui.ufmg.br; Bento Borba da Silva, Jose [Departamento de Quimica, Universidade Federal de Minas Gerais, Campus Pampulha, Cx Postal 702, Belo Horizonte, MG, 31270-901 (Brazil)

    2009-06-15

    A method for the direct determination (without sample pre-digestion) of microelements in fruit juice by inductively coupled plasma optical emission spectrometry has been developed. The method has been optimized by a 2{sup 3} factorial design, which evaluated the plasma conditions (nebulization gas flow rate, applied power, and sample flow rate). A 1:1 diluted juice sample with 2% HNO{sub 3} (Tetra Packed, peach flavor) and spiked with 0.5 mg L{sup - 1} of Al, Ba, Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, Sb, Sn, and Zn was employed in the optimization. The results of the factorial design were evaluated by exploratory analysis (Hierarchical Cluster Analysis, HCA, and Principal Component Analysis, PCA) to determine the optimum analytical conditions for all elements. Central point condition differentiation (0.75 L min{sup - 1}, 1.3 kW, and 1.25 mL min{sup - 1}) was observed for both methods, Principal Component Analysis and Hierarchical Cluster Analysis, with higher analytical signal values, suggesting that these are the optimal analytical conditions. F and t-student tests were used to compare the slopes of the calibration curves for aqueous and matrix-matched standards. No significant differences were observed at 95% confidence level. The correlation coefficient was higher than 0.99 for all the elements evaluated. The limits of quantification were: Al 253, Cu 3.6, Fe 84, Mn 0.4, Zn 71, Ni 67, Cd 69, Pb 129, Sn 206, Cr 79, Co 24, and Ba 2.1 {mu}g L{sup - 1}. The spiking experiments with fruit juice samples resulted in recoveries between 80 and 120%, except for Co and Sn. Al, Cd, Pb, Sn and Cr could not be quantified in any of the samples investigated. The method was applied to the determination of several elements in fruit juice samples commercialized in Brazil.

  19. Multivariate optimization by exploratory analysis applied to the determination of microelements in fruit juice by inductively coupled plasma optical emission spectrometry

    Science.gov (United States)

    Froes, Roberta Eliane Santos; Neto, Waldomiro Borges; Silva, Nilton Oliveira Couto e.; Naveira, Rita Lopes Pereira; Nascentes, Clésia Cristina; da Silva, José Bento Borba

    2009-06-01

    A method for the direct determination (without sample pre-digestion) of microelements in fruit juice by inductively coupled plasma optical emission spectrometry has been developed. The method has been optimized by a 2 3 factorial design, which evaluated the plasma conditions (nebulization gas flow rate, applied power, and sample flow rate). A 1:1 diluted juice sample with 2% HNO 3 (Tetra Packed, peach flavor) and spiked with 0.5 mg L - 1 of Al, Ba, Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, Sb, Sn, and Zn was employed in the optimization. The results of the factorial design were evaluated by exploratory analysis (Hierarchical Cluster Analysis, HCA, and Principal Component Analysis, PCA) to determine the optimum analytical conditions for all elements. Central point condition differentiation (0.75 L min - 1 , 1.3 kW, and 1.25 mL min - 1 ) was observed for both methods, Principal Component Analysis and Hierarchical Cluster Analysis, with higher analytical signal values, suggesting that these are the optimal analytical conditions. F and t-student tests were used to compare the slopes of the calibration curves for aqueous and matrix-matched standards. No significant differences were observed at 95% confidence level. The correlation coefficient was higher than 0.99 for all the elements evaluated. The limits of quantification were: Al 253, Cu 3.6, Fe 84, Mn 0.4, Zn 71, Ni 67, Cd 69, Pb 129, Sn 206, Cr 79, Co 24, and Ba 2.1 µg L - 1 . The spiking experiments with fruit juice samples resulted in recoveries between 80 and 120%, except for Co and Sn. Al, Cd, Pb, Sn and Cr could not be quantified in any of the samples investigated. The method was applied to the determination of several elements in fruit juice samples commercialized in Brazil.

  20. An evaluation of microwave-assisted fusion and microwave-assisted acid digestion methods for determining elemental impurities in carbon nanostructures using inductively coupled plasma optical emission spectrometry

    KAUST Repository

    Patole, Shashikant P.

    2015-10-21

    It is common for as-prepared carbon nanotube (CNT) and graphene samples to contain remnants of the transition metals used to catalyze their growth; contamination may also leave other trace elemental impurities in the samples. Although a full quantification of impurities in as-prepared samples of carbon nanostructures is difficult, particularly when trace elements are intercalated or encapsulated within a protective layer of graphitic carbon, reliable information is essential for reasons such as quantifying the adulteration of physico-chemical properties of the materials and for evaluating environmental issues. Here, we introduce a microwave-based fusion method to degrade single- and double-walled CNTs and graphene nanoplatelets into a fusion flux thereby thoroughly leaching all metallic impurities. Subsequent dissolution of the fusion product in diluted hydrochloric and nitric acid allowed us to identify their trace elemental impurities using inductively coupled plasma optical emission spectrometry. Comparisons of the results from the proposed microwave-assisted fusion method against those of a more classical microwave-assisted acid digestion approach suggest complementarity between the two that ultimately could lead to a more reliable and less costly determination of trace elemental impurities in carbon nanostructured materials. Graphical abstract A method for the complete digestion of carbon nanostructures has been demonstrated. Photographs (on the left side) show zirconium crucibles containing SWCNTs with flux of Na2CO3 and K2CO3, before and after microwave fusion; (on the right side) the appearance of the final solutions containing dissolved samples, from microwave-assisted fusion and microwave-assisted acid digestion. These solutions were used for determining the trace elemental impurities by ICP‒OES.

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

    Science.gov (United States)

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

    2017-04-01

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

  2. Sensitive determination of mercury in tap water by cloud point extraction pre-concentration and flow injection-cold vapor-inductively coupled plasma optical emission spectrometry

    Science.gov (United States)

    de Wuilloud, Jorgelina C. A.; Wuilloud, Rodolfo G.; Silva, María. F.; Olsina, Roberto A.; Martinez, Luis D.

    2002-02-01

    A pre-concentration and determination methodology for mercury at trace levels in water samples was developed. Cloud point extraction was successfully employed for the pre-concentration of mercury prior to inductively coupled plasma optical emission spectrometry coupled to a flow injection with cold vapor generation system. The mercury was extracted as mercury-2-(5-bromo-2-pyridylazo)-5-diethylaminophenol [Hg(II)-(5-Br-PADAP)] complex, at pH 9.2 mediated by micelles of the non-ionic surfactant polyethyleneglycolmono- p-nonylphenylether (PONPE 5). Cold vapor generation was developed from 100 μl of the extracted surfactant-rich phase by means of a stannous chloride (SnCl 2) solution as reluctant. An exhaustive study of the variables affecting the cloud point extraction with PONPE 5 and cold vapor mercury generation from the surfactant phase was performed. The 50-ml sample solution pre-concentration allowed us to raise an enrichment factor of 200-fold. The lower limit of detection obtained under the optimal conditions was 4 ng l -1. The precision for 10 replicate determinations at the 0.5-μg l -1 Hg level was 3.4% relative standard deviation (R.S.D.), calculated with the peak heights. The calibration graph using the pre-concentration system for mercury was linear with a correlation coefficient of 0.9998 at levels near the detection limits up to at least 50 μg l -1. The method was successfully applied to the determination of mercury in tap water samples.

  3. Straightforward way to enhance robustness in ultrasonic nebulization-axial view inductively coupled plasma optical emission spectrometry via an additional N2 gas stream

    Science.gov (United States)

    Scheffler, Guilherme Luiz; Pozebon, Dirce

    2015-11-01

    In the present study a low flow of N2 is mixed with the aerosol produced by ultrasonic nebulization (USN) prior analysis using inductively coupled plasma optical emission spectrometry (ICP OES). The foreign gas is added for improving plasma characteristics in axially-viewed ICP. By computing the Mg ionic to atomic ratio (plasma robustness) it was concluded that N2 dissociates closer to the load coil when USN is used as sample introduction system. The maximum emission intensity of Mg(II) for pneumatic nebulization (PN) was observed at 11 mm from the load coil while it was 8 mm for USN, indicating earlier aerosol desolvation, atomization and excitation processes in the ICP. Emission profiles of Ar(I) 415.861 nm, Ba(II) 486.601 nm and Ba(II) 233.527 nm indicated that metastable Ar species are overpopulated in the ICP under the N2 flow. Copper and manganese ionic lines with energy close to 16 eV (Ar ionization) were monitored to evaluate spatially dependent charge-transfer reaction along the ICP axis in the presence and absence of the N2 flow. The Cu(II) signal profiles indicated abundance of Ar+ species at low distances from the load coil when N2 was added. On the other hand, differences were not observed at longer distances from the load coil for both plasmas (mixed-gas and pure Ar-ICP). The calculated limits of detection (LODs) for both plasmas had the same order of magnitude. Analysis of certified reference samples demonstrated that the accuracy was preserved by adding the low flow of N2. It was concluded that adding a low flow of N2 to the aerosol produced by USN is a simple way to increase plasma robustness, which is usually lower than that achieved using conventional PN.

  4. Determination of phosphorus and potassium in commercial inorganic fertilizers by inductively coupled plasma-optical emission spectrometry: single-laboratory validation.

    Science.gov (United States)

    Bartos, James M; Boggs, Barton L; Falls, J Harold; Siegel, Sanford A

    2014-01-01

    A two-part single-laboratory validation study was conducted for determination of the P and K content in commercial fertilizer materials by inductively coupled plasma-optical emission spectrometry (ICP-OES). While several methods exist for determination of P and K in fertilizer products, the main focus of this study was on ICP-OES determination, which offers several unique advantages. Fertilizer samples with consensus P and K values from the Magruder and Association of Fertilizer and Phosphate Chemists (AFPC) check sample programs were selected for this study. Validation materials ranging from 4.4 to 52.4% P205 (1.7 to 22.7% P) and 3 to 62% K20 (2.5 to 51.5% K) were utilized. Because all P and K compounds contained in fertilizer materials are not "available" for plants to use, this study was conducted in two parts. Part A focused on ammonium citrate-disodium EDTA as the extraction solvent, as it estimates the pool of fertilizer P and K that is considered available to plants. Part B focused on hydrochloric acid as the digestion solvent, as it estimates the total P and K content of the fertilizer product. Selectivity studies indicated that this method can have a high bias for fertilizer products containing sources of phosphite or organic P compared to gravimetric or colorimetric methods that measure just orthophosphate. Provided the analytical challenges outlined in this study are addressed, this method offers the potential for a quick, accurate, and safe alternative for determining the P and K content of commercial inorganic fertilizer materials.

  5. 植物花青苷液质联用方法的分析鉴定%Golden rules of separation and characterization of plant anthocyanins by high pressure liquid chromatography-tandem mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    张洁; 李崇晖; 王亮生; 陈峰

    2013-01-01

      花青苷(anthocyanins)是植物中广泛存在的水溶性色素,在食品加工业中具有重要的地位。花青苷与人体健康密切相关,具有较强的抗氧化、抗炎症、抗微生物、抑制血小板凝聚和抗肿瘤等功效,已作为重要的功能因子而受到广泛的关注。花青苷成分的分析鉴定是花青苷生物活性研究的基础。然而,花青苷种类繁多,结构修饰多样,同时易受环境条件的影响,难以分离鉴定。高压液相色谱-二极管阵列检测-质谱联用技术(HPLC-DAD-MS)是花青苷分析最常规的手段。本文综述了如何利用HPLC-DAD-MS快速有效分离花青苷以及结构解析的一般规律及经验,以期为高附加值资源筛选以及花青苷构效关系的进一步揭示提供重要的化学基础。%  Anthocyanins are important water-soluble pigments, which have significant influence in food processing industry. Anthocyanins have anti-oxidant, anti-inflammatory, anti-antimicrobial, inhibition of platelet aggregation and anticancer activity, and have been the focus as important functional ingredients. Separation and identification of anthocyanins are the base for studying their bioactive effects. However, the complexity and va-riety of anthocyanins make it difficult to characterize the composition of anthocyanins. High pressure liquid chromatography (HPLC) coupled with mass spectrometry has become the standard and most powerful method for routine anthocyanin analysis. This paper reviewed the golden rules for separation and identification of anthocya-nins by high pressure liquid chromatography-tandem mass spectrometry (HPLC-DAD-MS), which might provide the chemical evidence for clarification of structure-activity relationship and screening for high value-added re-sources.

  6. Isogeometric shape optimization of magnetic density separators

    NARCIS (Netherlands)

    Dang Manh, N.; Evgrafov, A.; Gravesen, J.; Lahaye, D.

    2013-01-01

    Purpose: The waste recycling industry increasingly relies on magnetic density separators. These devices generate an upward magnetic force in ferro-fluids allowing to separate the immersed particles according to their mass density. Recently a new separator design that significantly reduces the requir

  7. Atomic lithium vapor laser isotope separation

    CERN Document Server

    Olivares, I E

    2002-01-01

    An atomic vapor laser isotope separation in lithium was performed using tunable diode lasers. The method permits also the separation of the isotopes between the sup 6 LiD sub 2 and the sup 7 LiD sub 1 lines using a self-made mass separator which includes a magnetic sector and an ion beam designed for lithium. (Author)

  8. [Separation and identification of beta-casein from Chinese human milk by ion exchange chromatography-matrix-assisted laser desorption/ionization time of flight/time of flight mass spectrometry].

    Science.gov (United States)

    Huang, Yu; Ren, Haowei; Liu, Biao; Liu, Ning; Li, Meng; Wang, Dongmao

    2013-05-01

    The selective precipitation of whole casein from skimmed milk was achieved by the addition of calcium salt under acidic pH. The effects of pH, centrifugal force and final concentration of CaCl2 on the separation of casein were studied by measuring the purity of final products using sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE). The results showed that casein with the highest purity could be obtained with the pH of 4.3, the centrifugal force of 10 400 g and the final concentration of CaCl2 of 60 mmol/L. The casein was processed with DEAE anion exchange chromatography and three peaks were obtained. Then the third peak (peak III) was identified with Western-Blot method and matrix-assisted laser desorption/ionization time of flight/time of flight mass spectrometry (MALDI-TOF/TOF MS). The identification of Western-Blot showed that peak III can combine with the specificity of human milk beta-casein antibody, and it is proved to be human milk beta-casein. The fingerprints of peak III were nalyzed by Mascot searching, and the sequence coverage was 50%, further supporting it is human milk beta-casein. In conclusion, an effective method to obtain human milk beta-casein from milk samples through DEAE anion exchange chromatography was established, and it is suitable for the proteomics research requirements of the beta-casein from human milk.

  9. 关于传质分离技术课程项目化教学改革探索%Project Teaching Reform on Mass Transfer Separation Technology Curriculum

    Institute of Scientific and Technical Information of China (English)

    李洪林

    2013-01-01

      课程改革是当前高职教学改革的核心任务。依据工学结合理念开发的项目化导向的《传质分离技术》课程,突出了高职教学特色。该课程对课程体系、教学内容、教学方法、教学手段、考核评价方式等方面进行了全方位改革,并按项目化教学要求改进了实训条件,采用“任务驱动、项目导向”的方法,实现了“教、学、做”一体化,收到了良好的教学效果。%The curriculum reform is the core task of teaching reform in vocational colleges. Based on the combination of learning with working, we developed the project-oriented Mass Transfer Separation Technology curriculum which highlighted the characteristics of higher vocational education. It reformed the curriculum system, teaching content, teaching method, teaching mean, and examination method etc., and improved training conditions; it used the teaching methodology of "task-driven" and "project-oriented", realized the integration of teaching, learning and doing, and received a good teaching effect.

  10. Testing Orions Fairing Separation System

    Science.gov (United States)

    Martinez, Henry; Cloutier, Chris; Lemmon, Heber; Rakes, Daniel; Oldham, Joe; Schlagel, Keith

    2014-01-01

    Traditional fairing systems are designed to fully encapsulate and protect their payload from the harsh ascent environment including acoustic vibrations, aerodynamic forces and heating. The Orion fairing separation system performs this function and more by also sharing approximately half of the vehicle structural load during ascent. This load-share condition through launch and during jettison allows for a substantial increase in mass to orbit. A series of component-level development tests were completed to evaluate and characterize each component within Orion's unique fairing separation system. Two full-scale separation tests were performed to verify system-level functionality and provide verification data. This paper summarizes the fairing spring, Pyramidal Separation Mechanism and forward seal system component-level development tests, system-level separation tests, and lessons learned.

  11. Selective Iron(III ion uptake using CuO-TiO2 nanostructure by inductively coupled plasma-optical emission spectrometry

    Directory of Open Access Journals (Sweden)

    Rahman Mohammed M

    2012-12-01

    Full Text Available Abstract Background CuO-TiO2 nanosheets (NSs, a kind of nanomaterials is one of the most attracting class of transition doped semiconductor materials due to its interesting and important optical, electrical, and structural properties and has many technical applications, such as in metal ions detection, photocatalysis, Chemi-sensors, bio-sensors, solar cells and so on. In this paper the synthesis of CuO-TiO2 nanosheets by the wet-chemically technique is reported. Methods CuO-TiO2 NSs were prepared by a wet-chemical process using reducing agents in alkaline medium and characterized by UV/vis., FT-IR spectroscopy, X-ray photoelectron spectroscopy (XPS, powder X-ray diffraction (XRD, and field-emission scanning electron microscopy (FE-SEM etc. Results The structural and optical evaluation of synthesized NSs were measured by XRD pattern, Fourier transform infrared (FT-IR and UV–vis spectroscopy, respectively which confirmed that the obtained NSs are well-crystalline CuO-TiO2 and possessing good optical properties. The morphological analysis of CuO-TiO2 NSs was executed by FE-SEM, which confirmed that the doped products were sheet-shaped and growth in large quantity. Here, the analytical efficiency of the NSs was applied for a selective adsorption of iron(III ion prior to detection by inductively coupled plasma-optical emission spectrometry (ICP-OES. The selectivity of NSs towards various metal ions, including Au(III, Cd(II, Co(II, Cr(III, Fe(III, Pd(II, and Zn(II was analyzed. Conclusions Based on the selectivity study, it was confirmed that the selectivity of doped NSs phase was the most towards Fe(III ion. The static adsorption capacity for Fe(III was calculated to be 110.06 mgg−1. Results from adsorption isotherm also verified that the adsorption process was mainly monolayer-adsorption onto a surface containing a finite number of CuO-TiO2 NSs adsorption sites.

  12. Total sulfur determination in gasoline, kerosene and diesel fuel using inductively coupled plasma optical emission spectrometry after direct sample introduction as detergent emulsions

    Energy Technology Data Exchange (ETDEWEB)

    Santelli, Ricardo Erthal [Departamento de Geoquimica, Universidade Federal Fluminense, Outeiro Sao Joao Batista s/n, Centro, Niteroi/RJ, 24020-150 (Brazil)], E-mail: santelli@geoq.uff.br; Padua Oliveira, Eliane [Departamento de Geoquimica, Universidade Federal Fluminense, Outeiro Sao Joao Batista s/n, Centro, Niteroi/RJ, 24020-150 (Brazil); Departamento de Engenharia Quimica e de Petroleo, Universidade Federal Fluminense, Rua Passos da Patria 156, Sao Domingos, Niteroi/RJ, 24210-230 (Brazil); Batista de Carvalho, Maria de Fatima [Centro de Pesquisas e Desenvolvimento da PETROBRAS, Avaliacao e Monitoramento Ambiental, Av. Horacio Macedo, 950, Cidade Universitaria, Rio de Janeiro/RJ, 21941-598 (Brazil); Almeida Bezerra, Marcos [Departamento de Geoquimica, Universidade Federal Fluminense, Outeiro Sao Joao Batista s/n, Centro, Niteroi/RJ, 24020-150 (Brazil); Universidade Estadual do Sudoeste da Bahia, Laboratorio de Quimica Analitica, Rua Jose Moreira Sobrinho s/n, Jequiezinho, Jequie/BA, 45206-190 (Brazil); Soares Freire, Aline [Departamento de Geoquimica, Universidade Federal Fluminense, Outeiro Sao Joao Batista s/n, Centro, Niteroi/RJ, 24020-150 (Brazil)

    2008-07-15

    Herein, we present the development of a procedure for the determination of total sulfur in petroleum-derived products (gasoline, kerosene and diesel fuel) employing inductively coupled plasma optical emission spectrometry (ICP OES). For this procedure, samples were prepared as emulsions that were made using concentrated nitric acid, Triton X-100, sample, and ultra pure water in proportions of 5/10/7/78% (v/v), respectively. Sample volumes were weighed because of the density differences, and oxygen was added to the sheat gas entrance of the ICP OES in order to decrease carbon deposition in the torch and to minimize background effects. A Doehlert design was applied as an experimental matrix to investigate the flow ratios of argon (sheat and plasma gas) and oxygen in relation to the signal-to-background ratio. A comparative study among the slopes of the analytical curves built in aqueous media, surfactant/HNO{sub 3}, and by spike addition for several sample emulsions indicates that a unique solution of surfactant in acidic media can be employed to perform the external calibration for analysis of the emulsions. The developed procedure allows for the determination of the total sulfur content in petroleum derivatives with a limit of detection (LOD) and limit of quantification (LOQ) of 0.72 and 2.4 {mu}g g{sup -1}, respectively. Precision values, expressed as the relative standard deviations (% RSD, n = 10) for 12 and 400 {mu}g g{sup -1}, were 2.2% and 1.3%, respectively. The proposed procedure was applied toward the determination of total sulfur in samples of gasoline, kerosene, and diesel fuel commercialized in the city of Niteroi/RJ, Brazil. The accuracy of the proposed method was evaluated by the determination of the total sulfur in three different standard reference materials (SRM): NIST 2723a (sulfur in diesel fuel oil), NIST 1616b (sulfur in kerosene), and NIST 2298 (sulfur in gasoline). The data indicate that the methodology can be successfully applied to these

  13. A methodology for quantifying trace elements in the exoskeletons of Florida stone crab (Menippe mercenaria) larvae using inductively coupled plasma optical emission spectrometry (ICP–OES)

    Science.gov (United States)

    Gravinese, Philip M.; Flannery, Jennifer A.; Toth, Lauren T.

    2016-11-23

    The larvae of the Florida stone crab, Menippe mercenaria, migrate through a variety of habitats as they develop and, therefore, experience a broad range of environmental conditions through ontogeny. Environmental variability experienced by the larvae may result in distinct elemental signatures within the exoskeletons, which could provide a tool for tracking the environmental history of larval stone crab populations. A method was developed to examine trace-element ratios, specifically magnesium-to-calcium (Mg/Ca) and strontium-to-calcium (Sr/Ca) ratios, in the exoskeletons of M. mercenaria larvae. Two developmental stages of stone crab larvae were analyzed—stage III and stage V. Specimens were reared in a laboratory environment under stable conditions to quantify the average ratios of Mg/Ca and Sr/Ca of larval stone crab exoskeletons and to determine if the ratios differed through ontogeny. The elemental compositions (Ca, Mg, and Sr) in samples of stage III larvae (n = 50 per sample) from 11 different broods (mean Sr/Ca = 5.916 ± 0.161 millimole per mole [mmol mol−1]; mean Mg/Ca = 218.275 ± 59.957 mmol mol−1) and stage V larvae (n = 10 per sample) from 12 different broods (mean Sr/Ca = 6.110 ± 0.300 mmol mol−1; mean Mg/Ca = 267.081 ± 67.211 mmol mol–1) were measured using inductively coupled plasma optical emission spectrometry (ICP–OES). The ratio of Sr/Ca significantly increased from stage III to stage V larvae, suggesting an ontogenic shift in Sr/Ca ratios between larval stages. The ratio of Mg/Ca did not change significantly between larval stages, but variability among broods was high. The method used to examine the trace-element ratios provided robust, highly reproducible estimates of Sr/Ca and Mg/Ca ratios in the larvae of M. mercenaria, demonstrating that ICP–OES can be used to determine the trace-element composition of chitinous organisms like the Florida stone crab.

  14. Laser Induced Breakdown Spectroscopy compared with conventional plasma optical emission techniques for the analysis of metals - A review of applications and analytical performance

    Science.gov (United States)

    Bengtson, A.

    2017-08-01

    This review is focused on a comparison of LIBS with the two most common plasma Optical Emission Spectroscopy (OES) techniques for analysis of metals; spark OES and glow discharge (GD) OES. It is shown that these two techniques have only minor differences in analytical performance. An important part of the paper reviews a direct comparison of the analytical figures of merit for bulk analysis of steels using spark and LIBS sources. The comparison was carried out using one instrument with interchangeable sources, eliminating differences related to the optical system and detectors. It was found that the spark provides slightly better analytical figures of merit. The spark analysis is considerably faster, the simple design of the spark stand has enabled complete automation, both properties of great importance in the metallurgical industry for routine analysis. The analysis of non-metallic inclusions (NMI) with spark and LIBS is presented, in the case of the spark this has become known as Pulse Distribution Analysis (PDA). A very significant difference between the techniques is that the electrical spark typically evaporates 100 times more material than a single laser pulse, resulting in complete evaporation of an NMI present in the evaporated metal. The major advantage of LIBS is that it is localised with very good lateral resolution. The major advantages of spark is that it is much faster (can be done simultaneous with the bulk analysis) and easier to quantify. Compositional Depth Profiling (CDP) is compared for GD-OES and LIBS. It is shown that for applications where GD-OES is well suited, e.g. coated metallic sheet, GD-OES still performs slightly better than LIBS. Similar to the case of NMI analysis, the major advantage of LIBS is the great lateral resolution. This allows elemental surface mapping, as well as CDP of very small areas on μm scale. One further advantage of LIBS is that samples of almost any material, shape and size can be analysed, whereas GD-OES has

  15. Environmental biomonitoring of essential and toxic elements in human scalp hair using accelerated microwave-assisted sample digestion and inductively coupled plasma optical emission spectroscopy.

    Science.gov (United States)

    Kumakli, Hope; Duncan, A'ja V; McDaniel, Kiara; Mehari, Tsdale F; Stephenson, Jamira; Maple, Lareisha; Crawford, Zaria; Macemore, Calvin L; Babyak, Carol M; Fakayode, Sayo O

    2017-05-01

    Human scalp hair samples were collected and used to assess exposure to toxic elements and essential elements in the state of North Carolina, USA using accelerated microwave assisted acid digestion and inductively coupled plasma optical emission spectroscopy (ICP-OES). The figures-of-merit of the ICP-OES were appropriate for elemental analysis in scalp hair with detection limits as low as 0.0001 mg/L for Cd, good linearity (R(2) > 0.9978), and percent recoveries that ranged from 96 to 106% for laboratory-fortified-blanks and 88-112% for sample spike recovery study. The concentrations of essential elements in scalp hair were larger than those of toxic elements, with Ca having the highest average concentration (3080 μg/g, s = 14,500, n = 194). Some of the maximum concentrations observed for As (65 μg/g), Ni (331 μg/g), Cd (2.96 μg/g), and Cr (84.6 μg/g) in individual samples were concerning, however. Samples were statistically analyzed to determine the influence of race, gender, smoking habits, or age on the elemental concentrations in scalp hair. Higher concentrations of essential elements were observed in the scalp hair of Caucasians, females, and non-smokers, and the differences were often significant at a 90% confidence level. Several pairs of essential elements, for example Ca-K, Ca-Mg, and Ca-Zn, were strongly correlated in Caucasian hair but uncorrelated in African-American hair. Similarly, essential elements were strongly correlated in female hair but weakly correlated in male hair. Toxic element pairs (As-Cd, As-Se, Pb-As, and Se-Cd) were strongly correlated in the hair of smokers but uncorrelated in that of non-smokers, suggesting that cigarette smoke is a common source of toxic elements in humans. Published by Elsevier Ltd.

  16. Determination of metallic elements in natural and waste water by inductively coupled plasma-optical emission spectrometry (Icp-OES); Determinazione di specie metalliche in acque naturali e reflue mediante spettroscopia di emissione in sorgente al plasma (ICP-OES)

    Energy Technology Data Exchange (ETDEWEB)

    Petruzzelli, D. [Consiglio Nazionale delle Ricerche, Bari (Italy). Ist. di Ricerca sulle Acque; Bettinelli, M.; Spezia, S. [ENEL UML, Piacenza (Italy); Mastroianni, D.; Capri, S.; Pettine, M. [Consiglio Nazionale delle Ricerche, Rome (Italy). Ist. di Ricerca sulle Acque

    1998-12-31

    A method is described for multielement determination of 33 elements in liquids samples by inductively coupled plasma-optical emission spectrometry (Icp-OES). In this method the intensity of the light emitted at specific wavelengths from excited atoms and ions of a sample is measured and used to determine the concentrations of the element of interest. [Italiano] Viene descritto un metodo per la determinazione multielementare di 33 elementi in campioni liquidi basato sull`uso del plasma ottico. In questo metodo si misura l`intensita` della radiazione elettromagnetica emessa dagli atomi e ioni eccitati delle specie presenti nel campione.

  17. 色谱纯化和质谱分析法研究牛骨源咸味肽%Separation, Purification and Analysis of Salty Peptides Derived from Bovine Bone by Chromatography and Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    李迎楠; 刘文营; 张顺亮; 成晓瑜

    2016-01-01

    以牛骨为研究对象,通过中空纤维超滤装置、Sephadex G-25凝胶色谱柱对相对分子质量小于5000的酶解产物进行初步分离,选用制备型及分析型高效液相色谱分析仪对咸味肽进行纯化、收集及分析。结果表明:收集得到牛骨源咸味肽为单一组分;用基质辅助激光解析电离-飞行时间质谱仪对咸味肽进行分析,得到其为相对分子质量均小于1000的短肽,其呈现咸味的物质质荷比值可能为679.5109。%The enzymatic hydrolysate of bovine bone with relative molecular weight < 5 000 was separated by hollow fiber ultrafiltration and Sephadex G-25 column chromatography. Two salty peptide fractions from the hydrolysate were purified by preparative high performance liquid chromatography (HPLC) and the pooled samples were analyzed by HPLC. The two fractions were found to consist of a single homogenous component. As analyzed by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF/MS), both peptide fractions had a relative molecular weight less than 1000, the salty taste compound of which was m/z 679.510 9.

  18. Isobar separator for radioactive nuclear beams project

    Energy Technology Data Exchange (ETDEWEB)

    Davids, C.N.; Nolen, J.A.

    1995-08-01

    In order to produce pure beams of radioactive products emanating from the production target/ion source system, both mass and isobar separation is required. A preliminary mass separation with a resolution {triangle}M/M of approximately 10{sup -3} will select the proper mass beam. An isobar separator is needed because the masses of adjacent isobars are usually quite close, especially for beams near stability. In general, a mass resolution of 5 x 10{sup -5} is needed for isobar separation in the A < 120 region, while a resolution of 3 x 10{sup -5} or better is needed for heavier masses. Magnets are used to obtain mass separation. However, in addition to having mass dispersion properties, magnets also have an equal energy dispersion. This means that an energy variation in the beam cannot be distinguished from a mass difference. This is important because ions emerge from the ion source having a small ({approximately} 10{sup -5} - 10{sup -4}) energy spread. In order to make the system respond only to mass differences, it must be made energy dispersion. This is normally accomplished by using a combination of electric and magnetic fields. The most convenient way of doing this is to use an electric deflection following the magnet separator. A preliminary isobar separator which achieves a mass resolution of 2.7 x 10{sup -5} is shown in Figure I-38. It uses two large 60{degrees} bending magnets to obtain a mass dispersion of 140 mm/%, and four electric dipoles with bending angles of 39{degrees} to cancel the energy dispersion. Sextupole and octupole correction elements are used to reduce the geometrical aberrations.

  19. DESIR high resolution separator at GANIL, France

    Directory of Open Access Journals (Sweden)

    Toprek Dragan

    2012-01-01

    Full Text Available A high-resolution separator for the SPIRAL2/DESIR project at GANIL has been designed. The extracted isotopes from SPIRAL2 will be transported to and cooled in a RFQ cooler yielding beams with very low transverse emittance and energy spread. These beams will then be accelerated to 60 keV and sent to a high-resolution mass separator where a specific isotope will be selected. The good beam properties extracted from the RFQ cooler will allow one to obtain a mass resolution of č26000 with the high-resolution mass separator.

  20. Fictional Separation Logic

    DEFF Research Database (Denmark)

    Jensen, Jonas Buhrkal; Birkedal, Lars

    2012-01-01

    , separation means physical separation. In this paper, we introduce \\emph{fictional separation logic}, which includes more general forms of fictional separating conjunctions P * Q, where "*" does not require physical separation, but may also be used in situations where the memory resources described by P and Q...

  1. Separation Anxiety (For Parents)

    Science.gov (United States)

    ... Kids to Be Smart About Social Media Separation Anxiety KidsHealth > For Parents > Separation Anxiety Print A A ... both of you get through it. About Separation Anxiety Babies adapt pretty well to other caregivers. Parents ...

  2. Separation Anxiety (For Parents)

    Science.gov (United States)

    ... Feeding Your 1- to 2-Year-Old Separation Anxiety KidsHealth > For Parents > Separation Anxiety A A A ... both of you get through it. About Separation Anxiety Babies adapt pretty well to other caregivers. Parents ...

  3. Isogeometric shape optimization of magnetic density separators

    OpenAIRE

    2013-01-01

    Purpose: The waste recycling industry increasingly relies on magnetic density separators. These devices generate an upward magnetic force in ferro-fluids allowing to separate the immersed particles according to their mass density. Recently a new separator design that significantly reduces the required amount of permanent magnet material has been proposed. The purpose of this paper is to alleviate the undesired end-effects in this design by altering the shape of the ferromagnetic covers of the...

  4. Controlling Separation in Turbomachines

    Science.gov (United States)

    Evans, Simon; Himmel, Christoph; Power, Bronwyn; Wakelam, Christian; Xu, Liping; Hynes, Tom; Hodson, Howard

    2010-01-01

    Four examples of flow control: 1) Passive control of LP turbine blades (Laminar separation control). 2) Aspiration of a conventional axial compressor blade (Turbulent separation control). 3) Compressor blade designed for aspiration (Turbulent separation control). 4.Control of intakes in crosswinds (Turbulent separation control).

  5. A novel method for fast enrichment and monitoring of hexavalent and trivalent chromium at the ppt level with modified silica MCM-41 and its determination by inductively coupled plasma optical emission spectrometry

    Directory of Open Access Journals (Sweden)

    Ganjali Mohammad Reza

    2006-01-01

    Full Text Available Chromium(III at the ng L-1 level was extracted using partially silylated MCM-41 modified by a tetraazamacrocyclic compound (TAMC and determined by inductively coupled plasma optical emision spectrometry (ICP OES. The extraction time and efficiency, pH and flow rate, type and minimum amount of stripping acid, and break- through volume were investigated. The method's enrichment factor and detection limit are 300 and 45.5 pg mL-1, respectively. The maximum capacity of the 10 mg of modified silylated MCM-41 was found to be 400.5?4.7 µg for Cr(III. The method was applied to the determination of Cr(III and Cr(VI in the wastewater of the chromium electroplating industry and in environmental and biological samples (black tea, hot and black pepper.

  6. Determination of plutonium isotopes (238Pu, 239Pu, 240Pu, 241Pu) in environmental samples using radiochemical separation combined with radiometric and mass spectrometric measurements

    DEFF Research Database (Denmark)

    Xu, Yihong; Qiao, Jixin; Hou, Xiaolin

    2014-01-01

    This paper reports an analytical method for the determination of plutonium isotopes (238Pu, 239Pu, 240Pu, 241Pu) in environmental samples using anion exchange chromatography in combination with extraction chromatography for chemical separation of Pu. Both radiometric methods (liquid scintillation...

  7. Improved tryptic digestion assisted with an acid-labile anionic surfactant for the separation and characterization of glycopeptide glycoforms of a proteolytic-resistant glycoprotein by capillary electrophoresis time-of-flight mass spectrometry.

    Science.gov (United States)

    Barroso, Albert; Giménez, Estela; Benavente, Fernando; Barbosa, José; Sanz-Nebot, Victoria

    2016-04-01

    Certain glycoproteins are rather difficult to digest due to compacted tertiary or quaternary structures. In a previous study, a capillary LC coupled to TOF-MS (μLC-TOF-MS) method was developed for the detection and characterization of the glycopeptide glycoforms of human transferrin (Tf), a proteolytic resistant glycoprotein, in serum samples. After immunoaffinity purification, Tf was digested with trypsin in the presence of RapiGest(®) and μLC-TOF-MS analyses permitted to detect the N413 and N611 glycopeptide glycoforms. Conversely, the use of this surfactant, albeit mandatory to quantitatively digest the isolated Tf, proved detrimental to CE-TOF-MS analysis due to its interaction with the inner surface of the silica capillary walls. As CE is usually regarded as an interesting alternative to other separation techniques (low consumption of reagents, excellent separation efficiency, and reduced analysis times), in this work, the undesirable interferences of the surfactant have been removed to allow the correct separation and detection of Tf glycoforms by CE-TOF-MS. Moreover, the digestion protocol described by the RapiGest(®) manufacturer has been modified to minimize desialylation of Tf glycopeptide glycoforms. The new developed CE-TOF-MS methodology has been then compared with the former μLC-TOF-MS by means of sensitivity and separation efficiency of Tf glycopeptide glycoforms in the standard glycoprotein. Additionally, Tf glycopeptide glycoforms from serum of healthy volunteers and patients with congenital disorders of glycosylation have also been analyzed following the developed methodology.

  8. 亲和毛细管电泳、环糊精-电动色谱、毛细管电泳-质谱用于对映体分离的研究进展%Method Development of Enantiomer Separations by Affinity Capillary Electrophoresis,Cyclodextrin Electrokinetic Chromatography and Capillary Electrophoresis-Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    Capillary electrophoresis (CE) has become a powerful tool for enantiomer separat ions during the last decade. Since 1993, the author has investigated enantiomer separations by affinity capillary electrophoresis (affinity CE) with some prote ins and by cyclodextrin electrokinetic chromatography (CDEKC) with some charged cyclodextrins (CDs). Many successful enantiomer separations are demonstrated f rom our study in this review article. In the enantiomer separations by affinit y CE, the deterioration of detection sensitivity was observed under high concent ration of the protein in running solutions. The partial filling technique was practically useful to solve the serious problem. It allowed operation at high protein concentrations, such as 500 μmol/L, without the detection problem. Cha rged CDs had several advantages for the enantiomer separations over neutral ones . Strong electrostatic interactions between a charged CD and oppositely charged analytes should be effective for the formation of the complex. A large differen ce in electrophoretic mobility between the free analyte and the inclusion comple x should also enhance the enantiomeric resolution. In CEmass spectrometry (CE MS), the partial filling technique was applied to avoid the introduction of no nvolatile chiral selectors into the CEMS interface. By replacing the nonvolat ile electrolytes in the running buffer by volatile ones, the separation conditio ns employed in CE with the UV detection method could be transferred to CEMS.

  9. Separation anxiety in children

    Science.gov (United States)

    ... page: //medlineplus.gov/ency/article/001542.htm Separation anxiety in children To use the sharing features on this page, please enable JavaScript. Separation anxiety in children is a developmental stage in which ...

  10. Ionene membrane battery separator

    Science.gov (United States)

    Moacanin, J.; Tom, H. Y.

    1969-01-01

    Ionic transport characteristics of ionenes, insoluble membranes from soluble polyelectrolyte compositions, are studied for possible application in a battery separator. Effectiveness of the thin film of separator membrane essentially determines battery lifetime.

  11. Magnetic separation of algae

    Energy Technology Data Exchange (ETDEWEB)

    Nath, Pulak; Twary, Scott N.

    2016-04-26

    Described herein are methods and systems for harvesting, collecting, separating and/or dewatering algae using iron based salts combined with a magnetic field gradient to separate algae from an aqueous solution.

  12. Separation of seven arsenic compounds by high-performance liquid chromatography with on-line detection by hydrogen–argon flame atomic absorption spectrometry and inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Hansen, S. H.; Larsen, E. H.; Pritzl, G.

    1992-01-01

    Seven molecular forms of arsenic were separated by anion- and cation-exchange high-performance liquid chromatography (HPLC) with on-line detection by flame atomic absorption spectrometry (FAAS). The interfacing was established by a vented poly(tetrafluoroethylene) capillary tubing connecting...... the HPLC column to the nebulizer of the atomic absorption spectrometer. Arsenite, arsenate, monomethylarsonate (MMA) and dimethylarsinate (DMA) were separated from each other and from the co-injected cationic arsenic compounds, arsenobetaine (AsB), arsenocholine (AsC) and the tetramethylarsonium ion (TMAs......-to-noise ratio of the on-line AAS detector was optimized. This involved the use of the hydrogen-argon-entrained air flame, a slotted tube atom trap in the flame for signal enhancement, electronic noise damping and a high-intensity light source. The detection limits in mu-g cm-3, using 100 mm3 injections...

  13. Separation of seven arsenic compounds by high performance liquid chromatography with on-line detection by hydrogen-argon flame atomic absorption spectrometry and inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Hansen, S. H.; Larsen, Erik Huusfeldt; Pritzl, G.

    1992-01-01

    Seven molecular forms of arsenic were separated by anion- and cation-exchange high-performance liquid chromatography (HPLC) with on-line detection by flame atomic absorption spectrometry (FAAS). The interfacing was established by a vented poly(tetrafluoroethylene) capillary tubing connecting......-to-noise ratio of the on-line AAS detector was optimized. This involved the use of the hydrogen-argon-entrained air flame, a slotted tube atom trap in the flame for signal enhancement, electronic noise damping and a high-intensity light source. The detection limits in mu-g cm-3, using 100 mm3 injections...... the HPLC column to the nebulizer of the atomic absorption spectrometer. Arsenite, arsenate, monomethylarsonate (MMA) and dimethylarsinate (DMA) were separated from each other and from the co-injected cationic arsenic compounds, arsenobetaine (AsB), arsenocholine (AsC) and the tetramethylarsonium ion (TMAs...

  14. Kinetic Gravity Separation

    NARCIS (Netherlands)

    Van Kooy, L.; Mooij, M.; Rem, P.

    2004-01-01

    Separations by density, such as the separation of non-ferrous scrap into light and heavy alloys, are often realized by means of heavy media. In principle, kinetic gravity separations in water can be faster and cheaper, because they do not rely on suspensions or salt solutions of which the density

  15. Acoustofluidic bacteria separation

    Science.gov (United States)

    Li, Sixing; Ma, Fen; Bachman, Hunter; Cameron, Craig E.; Zeng, Xiangqun; Huang, Tony Jun

    2017-01-01

    Bacterial separation from human blood samples can help with the identification of pathogenic bacteria for sepsis diagnosis. In this work, we report an acoustofluidic device for label-free bacterial separation from human blood samples. In particular, we exploit the acoustic radiation force generated from a tilted-angle standing surface acoustic wave (taSSAW) field to separate Escherichia coli from human blood cells based on their size difference. Flow cytometry analysis of the E. coli separated from red blood cells shows a purity of more than 96%. Moreover, the label-free electrochemical detection of the separated E. coli displays reduced non-specific signals due to the removal of blood cells. Our acoustofluidic bacterial separation platform has advantages such as label-free separation, high biocompatibility, flexibility, low cost, miniaturization, automation, and ease of in-line integration. The platform can be incorporated with an on-chip sensor to realize a point-of-care sepsis diagnostic device.

  16. Rapid Identification of Bacteria Directly from Positive Blood Cultures by Use of a Serum Separator Tube, Smudge Plate Preparation, and Matrix-Assisted Laser Desorption Ionization-Time of Flight Mass Spectrometry.

    Science.gov (United States)

    Chen, Yan; Porter, Vanessa; Mubareka, Samira; Kotowich, Leona; Simor, Andrew E

    2015-10-01

    We analyzed the matrix-assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF MS) of smudge plate growth for bacterial identification from 400 blood cultures. Ninety-seven percent of Gram-negative bacilli and 85% of Gram-positive organisms were correctly identified within 4 h; only eight isolates (2.0%) were misidentified. This method provided rapid and accurate microbial identification from positive blood cultures.

  17. Fragment separator momentum compression schemes

    Energy Technology Data Exchange (ETDEWEB)

    Bandura, Laura, E-mail: bandura@anl.gov [Facility for Rare Isotope Beams (FRIB), 1 Cyclotron, East Lansing, MI 48824-1321 (United States); National Superconducting Cyclotron Lab, Michigan State University, 1 Cyclotron, East Lansing, MI 48824-1321 (United States); Erdelyi, Bela [Argonne National Laboratory, Argonne, IL 60439 (United States); Northern Illinois University, DeKalb, IL 60115 (United States); Hausmann, Marc [Facility for Rare Isotope Beams (FRIB), 1 Cyclotron, East Lansing, MI 48824-1321 (United States); Kubo, Toshiyuki [RIKEN Nishina Center, RIKEN, Wako (Japan); Nolen, Jerry [Argonne National Laboratory, Argonne, IL 60439 (United States); Portillo, Mauricio [Facility for Rare Isotope Beams (FRIB), 1 Cyclotron, East Lansing, MI 48824-1321 (United States); Sherrill, Bradley M. [National Superconducting Cyclotron Lab, Michigan State University, 1 Cyclotron, East Lansing, MI 48824-1321 (United States)

    2011-07-21

    We present a scheme to use a fragment separator and profiled energy degraders to transfer longitudinal phase space into transverse phase space while maintaining achromatic beam transport. The first order beam optics theory of the method is presented and the consequent enlargement of the transverse phase space is discussed. An interesting consequence of the technique is that the first order mass resolving power of the system is determined by the first dispersive section up to the energy degrader, independent of whether or not momentum compression is used. The fragment separator at the Facility for Rare Isotope Beams is a specific application of this technique and is described along with simulations by the code COSY INFINITY.

  18. Fragment separator momentum compression schemes.

    Energy Technology Data Exchange (ETDEWEB)

    Bandura, L.; Erdelyi, B.; Hausmann, M.; Kubo, T.; Nolen, J.; Portillo, M.; Sherrill, B.M. (Physics); (MSU); (Northern Illinois Univ.); (RIKEN)

    2011-07-21

    We present a scheme to use a fragment separator and profiled energy degraders to transfer longitudinal phase space into transverse phase space while maintaining achromatic beam transport. The first order beam optics theory of the method is presented and the consequent enlargement of the transverse phase space is discussed. An interesting consequence of the technique is that the first order mass resolving power of the system is determined by the first dispersive section up to the energy degrader, independent of whether or not momentum compression is used. The fragment separator at the Facility for Rare Isotope Beams is a specific application of this technique and is described along with simulations by the code COSY INFINITY.

  19. Magnetic Separator Enhances Treatment Possibilities

    Science.gov (United States)

    2008-01-01

    Since the earliest missions in space, NASA specialists have performed experiments in low gravity. Protein crystal growth, cell and tissue cultures, and separation technologies such as electrophoresis and magnetophoresis have been studied on Apollo 14, Apollo 16, STS-107, and many other missions. Electrophoresis and magnetophoresis, respectively, are processes that separate substances based on the electrical charge and magnetic field of a molecule or particle. Electrophoresis has been studied on over a dozen space shuttle flights, leading to developments in electrokinetics, which analyzes the effects of electric fields on mass transport (atoms, molecules, and particles) in fluids. Further studies in microgravity will continue to improve these techniques, which researchers use to extract cells for various medical treatments and research.

  20. Simultaneous screening for lipophilic and hydrophilic toxins in marine harmful algae using a serially coupled reversed-phase and hydrophilic interaction liquid chromatography separation system with high-resolution mass spectrometry.

    Science.gov (United States)

    Chen, Junhui; Gao, Liyuan; Li, Zhaoyong; Wang, Shuai; Li, Jingxi; Cao, Wei; Sun, Chengjun; Zheng, Li; Wang, Xiaoru

    2016-03-31

    The presence of toxins in harmful algal blooms (HABs) poses considerable concerns because of their potential adverse effects on ecological environments and human health. When marine HABs occur, efficient screening and identification of toxins in different kinds of HAB algae remains a challenge. In this study, the applicability of serial coupling of reversed-phase liquid chromatography (RPLC) and hydrophilic interaction chromatography (HILIC) combined with high resolution mass spectrometry (HR-MS) for the simultaneous screening and identification of various kinds of known lipophilic and hydrophilic toxins in HAB algae was investigated for the first time. Ultrasound-assisted extraction (UAE) was explored to extract both lipophilic and hydrophilic toxins in algae simultaneously. As in most cases, toxin standards were not available; therefore, an identification procedure based on accurate mass data and chromatographic behavior was proposed. According to this procedure, eight known lipophilic toxins and 11 hydrophilic toxins were successfully detected in a single injection, and the proposed method was validated. Satisfactory sensitivity, repeatability (RSD marine algal toxins in a single run. Using this method, several known toxins in different marine toxigenic algae including Alexandrium tamarense, Alexandrium minutum and Prorocentrum lima were successfully observed and identified. This work demonstrates that RPLC/HILIC-HR-MS combined with an accurate mass list of known marine algal toxins may be used as a powerful tool for screening of different classes of known toxins in marine harmful algae. Copyright © 2016 Elsevier B.V. All rights reserved.

  1. A validated liquid chromatographic method for the determination of polycyclic aromatic hydrocarbons in honey after homogeneous liquid-liquid extraction using hydrophilic acetonitrile and sodium chloride as mass separating agent.

    Science.gov (United States)

    Koltsakidou, Anastasia; Zacharis, Constantinos K; Fytianos, Konstantinos

    2015-01-16

    In the present report, a simple and cost-effective method for the determination of twelve US EPA priority polycyclic aromatic hydrocarbons (PAHs) in honey samples after salting-assisted liquid-liquid extraction and UHPLC with fluorescence detection is proposed. The sample treatment is based on the usage of hydrophilic acetonitrile as extraction solvent and its phase separation under high salinity conditions. Due to the high sugar content of the samples the phase separation is promoted effortlessly. Several parameters affecting the extraction efficiency and method sensitivity including the concentration of the honey samples, the type and volume of the extraction solvent, the type and quantity of the inorganic salt, extraction time and centrifugation time was systematically investigated. The method was validated in-house according to the Commission Decision 2002/657/EC guidelines. The limit of detection (LOD) of the method lay between 0.02 and 0.04ngmL(-1) (corresponding to 0.08 and 0.16ngg(-1)) which are close to the quality criteria established by European Regulation (EC) 836/2011 concerning the PAHs in foodstuffs. The mean analytical bias (expressed as relative recoveries) in all spiking levels was acceptable being in the range of 54-118% while the relative standard deviation (RSD) was lower than 19%. The proposed method has been satisfactorily applied for the analysis of the selected PAHs residues in various honey samples obtained from Greek region.

  2. The Point Mass Concept

    Directory of Open Access Journals (Sweden)

    Lehnert B.

    2011-04-01

    Full Text Available A point-mass concept has been elaborated from the equations of the gravitational field. One application of these deductions results in a black hole configuration of the Schwarzschild type, having no electric charge and no angular momentum. The critical mass of a gravitational collapse with respect to the nuclear binding energy is found to be in the range of 0.4 to 90 solar masses. A second application is connected with the spec- ulation about an extended symmetric law of gravitation, based on the options of positive and negative mass for a particle at given positive energy. This would make masses of equal polarity attract each other, while masses of opposite polarity repel each other. Matter and antimatter are further proposed to be associated with the states of positive and negative mass. Under fully symmetric conditions this could provide a mechanism for the separation of antimatter from matter at an early stage of the universe.

  3. [Separation anxiety in children].

    Science.gov (United States)

    Purper-Ouakil, Diane; Franc, Nathalie

    2010-06-20

    Separation anxiety disorder can be differentiated from developmental anxiety because of its intensity, persistence and negative impact on adaptive functioning. This disorder is closely linked to other anxiety and mood disorders and can also be associated with externalizing psychopathology in children and adolescents. Severe separation anxiety can result in school refusal and intra-familial violence. Cognitive behavioral therapies have the best evidence-based support for the treatment of separation anxiety disorder in children and adolescents. In addition, it is important to detect factors associated with persistence of anxiety such as systematic avoidance of separation and parental overprotection. The role of pediatricians and general practitioners in recognizing clinical separation anxiety and encouraging appropriate care and positive parental attitudes is essential, as separation anxiety is often associated with a variety of somatic symptoms.

  4. Structural characterization of antibody drug conjugate by a combination of intact, middle-up and bottom-up techniques using sheathless capillary electrophoresis - Tandem mass spectrometry as nanoESI infusion platform and separation method.

    Science.gov (United States)

    Said, Nassur; Gahoual, Rabah; Kuhn, Lauriane; Beck, Alain; François, Yannis-Nicolas; Leize-Wagner, Emmanuelle

    2016-04-28

    Antibody-drug conjugates (ADCs) represent a fast growing class of biotherapeutic products. Their production leads to a distribution of species exhibiting different number of conjugated drugs overlaying the inherent complexity resulting from the monoclonal antibody format, such as glycoforms. ADCs require an additional level of characterization compared to first generation of biotherapeutics obtained through multiple analytical techniques for complete structure assessment. We report the development of complementary approaches implementing sheathless capillary electrophoresis-mass spectrometry (sheathless CE-MS) to characterize the different aspects defining the structure of brentuximab vedotin. Native MS using sheathless CE-MS instrument as a nanoESI infusion platform enabled accurate mass measurements and estimation of the average drug to antibody ratio alongside to drug load distribution. Middle-up analysis performed after limited IdeS proteolysis allowed to study independently the light chain, Fab and F(ab')2 subunits incorporating 1, 0 to 4 and 0 to 8 payloads respectively. Finally, a CZE-ESI-MS/MS methodology was developed in order to be compatible with hydrophobic drug composing ADCs. From a single injection, complete sequence coverage could be achieved. Using the same dataset, glycosylation and drug-loaded peptides could be simultaneously identified revealing robust information regarding their respective localization and abundance. Drug-loaded peptide fragmentation mass spectra study demonstrated drug specific fragments reinforcing identification confidence, undescribed so far. Results reveal the method ability to characterize ADCs primary structure in a comprehensive manner while reducing tremendously the number of experiments required. Data generated showed that sheathless CZE-ESI-MS/MS characteristics position the methodology developed as a relevant alternative for comprehensive multilevel characterization of these complex biomolecules. Copyright © 2016

  5. 安非他明类毒品的手性对映体气相色谱-质谱分析%Enantiomer Separation and Determination of Amphetamines with Chiral Derivatization by Gas Chromatography-Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    孟品佳

    2001-01-01

    采用手性衍生化试剂:(S)(-)N-三氟乙酰-1-脯胺酰氯(TPC)和(R)(+)-α-甲氯基-α-三氟甲基苯乙酸(MTPA)与安非他明类对映体反应生成非对映体衍生化产物,通过常规的GC/MS方法将其分离。本文较系统地考察了这两种手性试剂衍生化反应中溶剂、手性试剂用量、加热温度、反应时间等因素对安非他明类对映体衍生化结果的影响。实现了Am、MAm、MDA、MDMA、MDEA、MBDB等几种毒品对映体间的良好分离。%Most drugs of amphetamines contain chiral centers, which form different optical isomers, or enantiomers. Because different enantiomers have different pharmcological effect and have different machnism of metabolism. Besides, the ratio of the two eanatiomers could reflect the route and method used in the synthesis of the drugs. So the separation and determination of these eanantiomers for seizured samples or for biological samples became very important in the sence of forensic science.The paper used two chiral reagents: N-trifluroacetylprolyl chloride (TPC) and ( R )-( + )-α-methoxy-α-(trifluormethyl)phenylacetic acid (MTPA) to reach the purpose. They reacted with amphetamine enantiomers to form diasteromeric pairs, which possess some diffeences in physical and chemical natures and could be separated by GC/MS. The paper examined in detail some fectors such as the solvents, chiral reagent amounts, reaction time,temperature,etc. on the effect of chiral derivatization. Some enantiomers of amphetamine (Am),N-methylamphetamine(MAm),3,4-methylenedioxyamphetamin (MDA), 3,4-methylenedioxy-N-methylamphetamine (MDMA), 3, 4-methylenedioxy-N-ethylamphetamine ( MDEA ) and N-methyl-1-( 3, 4-methylenedioxy )-2-butanamine (MBDB) were well separated each other.

  6. [Separation anxiety. Theoretical considerations].

    Science.gov (United States)

    Blandin, N; Parquet, P J; Bailly, D

    1994-01-01

    The interest in separation anxiety is nowadays increasing: this disorder appearing during childhood may predispose to the occurrence of anxiety disorders (such as panic disorder and agoraphobia) and major depression into adulthood. Psychoanalytic theories differ on the nature of separation anxiety and its place in child development. For some authors, separation anxiety must be understood as resulting from the unconscious internal conflicts inherent in the individuation process and gradual attainment of autonomy. From this point of view, the fear of loss of mother by separation is not regarded as resulting from a real danger. However, Freud considers the primary experience of separation from protecting mother as the prototype situation of anxiety and compares the situations generating fear to separation experiences. For him, anxiety originates from two factors: the physiological fact is initiated at the time of birth but the primary traumatic situation is the separation from mother. This point of view may be compared with behavioral theories. Behavioral theories suggest that separation anxiety may be conditioned or learned from innate fears. In Freud's theory, the primary situation of anxiety resulting from the separation from mother plays a role comparable to innate fears. Grappling with the problem of separation anxiety, Bowlby emphasizes then the importance of the child's attachment to one person (mother or primary caregiver) and the fact that this attachment is instinctive. This point of view, based on the watch of infants, is akin to ethological theories on behaviour of non human primates. Bowlby especially shows that the reactions of infant separated from mother evolve on three stages: the phase of protestation which may constitute the prototype of adulthood anxiety, the phase of desperation which may be the prototype of depression, and the phase of detachment. He emphasizes so the role of early separations in the development of vulnerability to depression

  7. Separation of flow

    CERN Document Server

    Chang, Paul K

    2014-01-01

    Interdisciplinary and Advanced Topics in Science and Engineering, Volume 3: Separation of Flow presents the problem of the separation of fluid flow. This book provides information covering the fields of basic physical processes, analyses, and experiments concerning flow separation.Organized into 12 chapters, this volume begins with an overview of the flow separation on the body surface as discusses in various classical examples. This text then examines the analytical and experimental results of the laminar boundary layer of steady, two-dimensional flows in the subsonic speed range. Other chapt

  8. Ultra-high performance liquid chromatography with linear ion trap-Orbitrap hybrid mass spectrometry combined with a systematic strategy based on fragment ions for the rapid separation and characterization of components in Stellera chamaejasme extracts.

    Science.gov (United States)

    Wang, Zhixin; Qu, Yang; Wang, Li; Zhang, Xiaozhe; Xiao, Hongbin

    2016-04-01

    Stellera chamaejasme, a famous toxic herb, has been used in traditional Chinese medicine to treat various diseases. For decades, increasing attention in modern pharmacological studies has been drawn to S. chamaejasme because of its potential anti-tumor, anti-virus, and anti-fungus activities. However, due to the intrinsic complexity of chemical constitutes, hardly any investigations formed an overall recognition for the chemical profiles of this herb. In this study, a rapid and sensitive ultra-high performance liquid chromatography coupled with linear ion trap-Orbitrap mass spectrometry method was developed to characterize the chemical components of S. chamaejasme extracts. Based on optimized ultra-high performance liquid chromatography and mass spectrometry conditions and systematic fragment ions-based strategy, a total of 47 components including flavones, diterpenes, coumarins, and lignans were simultaneously detected and identified or tentatively identified for the first time. The MS(n) fragmentation patterns of all the characterized compounds in positive or negative electrospray ionization modes were also explored and summarized. These results provided essential data for further pharmacological research on S. chamaejasme. Moreover, the method was demonstrated to be an efficient tool for rapid qualitative analysis of secondary metabolites from natural resources.

  9. The separation of adult separation anxiety disorder.

    Science.gov (United States)

    Baldwin, David S; Gordon, Robert; Abelli, Marianna; Pini, Stefano

    2016-08-01

    The Diagnostic and Statistical Manual of Mental Disorders, Fifth Edition (DSM-5) categorization of mental disorders places "separation anxiety disorder" within the broad group of anxiety disorders, and its diagnosis no longer rests on establishing an onset during childhood or adolescence. In previous editions of DSM, it was included within the disorders usually first diagnosed in infancy, childhood, or adolescence, with the requirement for an onset of symptoms before the age of 18 years: symptomatic adults could only receive a retrospective diagnosis, based on establishing this early onset. The new position of separation anxiety disorder is based upon the findings of epidemiological studies that revealed the unexpectedly high prevalence of the condition in adults, often in individuals with an onset of symptoms after the teenage years; its prominent place within the DSM-5 group of anxiety disorders should encourage further research into its epidemiology, etiology, and treatment. This review examines the clinical features and boundaries of the condition, and offers guidance on how it can be distinguished from other anxiety disorders and other mental disorders in which "separation anxiety" may be apparent.

  10. Gas-filled separators - An overview

    CERN Document Server

    Leino, M

    2003-01-01

    Gas-filled recoil separators have been used in nuclear physics studies since the early fifties. Most notably, they have found use in the separation of evaporation residues of heavy and very heavy elements from unwanted background. Gas-filled separators, alone or coupled to a detector array, offer an efficient, fast, compact and relatively inexpensive solution for nuclear structure studies. A new application is the use of a gas-filled device as a pre-separator in the study of chemical properties of the heaviest elements. Other uses include systematic study of fusion evaporation cross sections and accelerator mass spectrometry. In this contribution, an overview on gas-filled recoil separators, their characteristics, fields of application and possible future developments is given.

  11. Working with Separation

    Science.gov (United States)

    Krugman, Dorothy C.

    1971-01-01

    Discusses the role of the caseworker in providing support to children experiencing separation from their families and emphasizes the need to recognize that there are differences between those separation experiences dictated by the needs of children and those dictated by arbitrary or noncasework factors. (AJ)

  12. Separation anxiety disorder

    NARCIS (Netherlands)

    Nauta, M.H.; Emmelkamp, P.M.G.; Sturmey, P.; Hersen, M.

    2012-01-01

    Separation anxiety disorder (SAD) is the only anxiety disorder that is specific to childhood; however, SAD has hardly ever been addressed as a separate disorder in clinical trials investigating treatment outcome. So far, only parent training has been developed specifically for SAD. This particular t

  13. Social Separation in Monkeys.

    Science.gov (United States)

    Mineka, Susan; Suomi, Stephen J.

    1978-01-01

    Reviews phenomena associated with social separation from attachment objects in nonhuman primates. Evaluates four theoretical treatments of separation in light of existing data: Bowlby's attachment-object-loss theory, Kaufman's conservation-withdrawal theory, Seligman's learned helplessness theory, and Solomon and Corbit's opponent-process theory.…

  14. Nonterminal Separating Macro Grammars

    NARCIS (Netherlands)

    Hogendorp, Jan Anne; Asveld, P.R.J.; Nijholt, A.; Verbeek, Leo A.M.

    1987-01-01

    We extend the concept of nonterminal separating (or NTS) context-free grammar to nonterminal separating $m$-macro grammar where the mode of derivation $m$ is equal to "unrestricted". "outside-in' or "inside-out". Then we show some (partial) characterization results for these NTS $m$-macro grammars.

  15. Optimization of an accelerated solvent extraction dispersive liquid-liquid microextraction method for the separation and determination of essential oil from Ligusticum chuanxiong Hort by gas chromatography with mass spectrometry.

    Science.gov (United States)

    Yang, Guang; Sun, Qiushi; Hu, Zhiyan; Liu, Hua; Zhou, Tingting; Fan, Guorong

    2015-10-01

    In this study, an accelerated solvent extraction dispersive liquid-liquid microextraction coupled with gas chromatography and mass spectrometry was established and employed for the extraction, concentration and analysis of essential oil constituents from Ligusticum chuanxiong Hort. Response surface methodology was performed to optimize the key parameters in accelerated solvent extraction on the extraction efficiency, and key parameters in dispersive liquid-liquid microextraction were discussed as well. Two representative constituents in Ligusticum chuanxiong Hort, (Z)-ligustilide and n-butylphthalide, were quantitatively analyzed. It was shown that the qualitative result of the accelerated solvent extraction dispersive liquid-liquid microextraction approach was in good agreement with that of hydro-distillation, whereas the proposed approach took far less extraction time (30 min), consumed less plant material (usually extraction and analysis of essential oil.

  16. Spiral microfluidic nanoparticle separators

    Science.gov (United States)

    Bhagat, Ali Asgar S.; Kuntaegowdanahalli, Sathyakumar S.; Dionysiou, Dionysios D.; Papautsky, Ian

    2008-02-01

    Nanoparticles have potential applications in many areas such as consumer products, health care, electronics, energy and other industries. As the use of nanoparticles in manufacturing increases, we anticipate a growing need to detect and measure particles of nanometer scale dimensions in fluids to control emissions of possible toxic nanoparticles. At present most particle separation techniques are based on membrane assisted filtering schemes. Unfortunately their efficiency is limited by the membrane pore size, making them inefficient for separating a wide range of sizes. In this paper, we propose a passive spiral microfluidic geometry for momentum-based particle separations. The proposed design is versatile and is capable of separating particulate mixtures over a wide dynamic range and we expect it will enable a variety of environmental, medical, or manufacturing applications that involve rapid separation of nanoparticles in real-world samples with a wide range of particle components.

  17. Lithium loss in the solid electrolyte interphase: Lithium quantification of aged lithium ion battery graphite electrodes by means of laser ablation inductively coupled plasma mass spectrometry and inductively coupled plasma optical emission spectroscopy

    Science.gov (United States)

    Schwieters, Timo; Evertz, Marco; Mense, Maximilian; Winter, Martin; Nowak, Sascha

    2017-07-01

    In this work we present a new method using LA-ICP-MS to quantitatively determine the lithium content in aged graphite electrodes of a lithium ion battery (LIB) by performing total depth profiling. Matrix matched solid external standards are prepared using a solid doping approach to avoid elemental fractionation effects during the measurement. The results are compared and matched to the established ICP-OES technique for bulk quantification after performing a microwave assisted acid digestion. The method is applied to aged graphite electrodes in order to determine the lithium immobilization (= ;Li loss;) in the solid electrolyte interphase after the first cycle of formation. For this, different samples including a reference sample are created to obtain varying thicknesses of the SEI covering the electrode particles. By applying defined charging voltages, an initial lithiation process is performed to obtain specific graphite intercalation compounds (GICs, with target stoichiometries of LiC30, LiC18, LiC12 and LiC6). Afterwards, the graphite electrode is completely discharged to obtain samples without mobile, thus active lithium in its lattice. Taking the amount of lithium into account which originates from the residues of the LiPF6 (dissolved in the carbon components containing electrolyte), it is possible to subtract the amount of lithium in the SEI.

  18. Internal standardization for the determination of cadmium, cobalt, chromium and manganese in saline produced water from petroleum industry by inductively coupled plasma optical emission spectrometry after cloud point extraction

    Energy Technology Data Exchange (ETDEWEB)

    Almeida Bezerra, Marcos [Departamento de Geoquimica, Universidade Federal Fluminense, Outeiro Sao Joao Batista s/n, Centro, Niteroi/RJ, 24020-150 (Brazil); Universidade Estadual do Sudoeste da Bahia, Departamento de Quimica e Exatas, Rua Jose Moreira Sobrinho s/n, Jequiezinho, Jequie/BA, 45206-190 (Brazil)], E-mail: mbezerra@uesb.br; Mitihiro do Nascimento Maeda, Sergio; Padua Oliveira, Eliane [Departamento de Geoquimica, Universidade Federal Fluminense, Outeiro Sao Joao Batista s/n, Centro, Niteroi/RJ, 24020-150 (Brazil); Fatima Batista de Carvalho, Maria de [Centro de Pesquisas e Desenvolvimento da PETROBRAS, Avaliacao e Monitoramento Ambiental, Av. Jequitiba, 950, Cidade Universitaria, Rio de Janeiro/RJ, 21941-598 (Brazil); Erthal Santelli, Ricardo [Departamento de Geoquimica, Universidade Federal Fluminense, Outeiro Sao Joao Batista s/n, Centro, Niteroi/RJ, 24020-150 (Brazil)

    2007-09-15

    In the present paper a procedure is proposed for the determination of traces of Cd, Co, Mn and Cr in petroleum industry produced water by inductively coupled plasma optical emission spectrometry. The procedure is based on cloud point extraction of these metals, as their dithizonate complexes, into the surfactant-rich phase of octylphenoxypolyethoxyethanol surfactant (Triton X-114). Extractions were carried out in solutions with salinities between 10 per mille and 70 per mille. Since residual salinity in the surfactant-rich phase caused differences in its transport to the plasma, yttrium was used as an internal standard to correct for this effect. The simultaneous metal extraction procedure was optimized by response surface methodology using a Doehlert design and desirability function. Enhancement factors of 21, 21, 9 and 19, along with limits of quantification of 0.093, 0.20, 0.73 and 1.2 {mu}g L{sup -1}, and precision expressed as relative standard deviation (n = 8, 20.0 {mu}g L{sup -1}) of 5.8, 1.2, 1.7 and 5.7% were obtained for Cd, Co, Mn and Cr, respectively. The accuracy was evaluated by spike recovery tests on the high salinity water samples with salinity of 40 and 63 per mille.

  19. Chemometric evaluation of Cd, Co, Cr, Cu, Ni (inductively coupled plasma optical emission spectrometry) and Pb (graphite furnace atomic absorption spectrometry) concentrations in lipstick samples intended to be used by adults and children.

    Science.gov (United States)

    Batista, Érica Ferreira; Augusto, Amanda dos Santos; Pereira-Filho, Edenir Rodrigues

    2016-04-01

    A method was developed for determining the concentrations of Cd, Co, Cr, Cu, Ni and Pb in lipstick samples intended to be used by adults and children using inductively coupled plasma optical emission spectrometry (ICP OES) and graphite furnace atomic absorption spectrometry (GF AAS) after treatment with dilute HNO3 and hot block. The combination of fractional factorial design and Desirability function was used to evaluate the ICP OES operational parameters and the regression models using Central Composite and Doehlert designs were calculated to stablish the best working condition for all analytes. Seventeen lipstick samples manufactured in different countries with different colors and brands were analyzed. Some samples contained high concentrations of toxic elements, such as Cr and Pb, which are carcinogenic and cause allergic and eczematous dermatitis. The maximum concentration detected was higher than the permissible safe limits for human use, and the samples containing these high metal concentrations were intended for use by children. Principal component analysis (PCA) was used as a chemometrics tool for exploratory analysis to observe the similarities between samples relative to the metal concentrations (a correlation between Cd and Pb was observed). Copyright © 2015 Elsevier B.V. All rights reserved.

  20. Internal standardization for the determination of cadmium, cobalt, chromium and manganese in saline produced water from petroleum industry by inductively coupled plasma optical emission spectrometry after cloud point extraction

    Science.gov (United States)

    Bezerra, Marcos Almeida; Mitihiro do Nascimento Maêda, Sérgio; Oliveira, Eliane Padua; de Fátima Batista de Carvalho, Maria; Santelli, Ricardo Erthal

    2007-09-01

    In the present paper a procedure is proposed for the determination of traces of Cd, Co, Mn and Cr in petroleum industry produced water by inductively coupled plasma optical emission spectrometry. The procedure is based on cloud point extraction of these metals, as their dithizonate complexes, into the surfactant-rich phase of octylphenoxypolyethoxyethanol surfactant (Triton X-114). Extractions were carried out in solutions with salinities between 10‰ and 70‰. Since residual salinity in the surfactant-rich phase caused differences in its transport to the plasma, yttrium was used as an internal standard to correct for this effect. The simultaneous metal extraction procedure was optimized by response surface methodology using a Doehlert design and desirability function. Enhancement factors of 21, 21, 9 and 19, along with limits of quantification of 0.093, 0.20, 0.73 and 1.2 μg L - 1 , and precision expressed as relative standard deviation ( n = 8, 20.0 μg L - 1 ) of 5.8, 1.2, 1.7 and 5.7% were obtained for Cd, Co, Mn and Cr, respectively. The accuracy was evaluated by spike recovery tests on the high salinity water samples with salinity of 40 and 63‰.

  1. Cloud point extraction with/without chelating agent on-line coupled with inductively coupled plasma optical emission spectrometry for the determination of trace rare earth elements in biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Li Yingjie [Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072 (China); Hu Bin, E-mail: binhu@whu.edu.cn [Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072 (China)

    2010-02-15

    The on-line incorporation of cloud point extraction (CPE) with/without 8-hydroxyquinoline (8-Ox) as chelating agent into flow injection analysis associated with inductively coupled plasma optical emission spectrometry (ICP-OES) for determining trace rare earth elements (REEs) is presented and evaluated. The significant parameters affecting on-line cloud point extraction of REEs such as sample pH, flow rate, 8-Ox concentration, Triton X-114 concentration were systematically studied. Under the optimized conditions, with the consumption of 3.0 mL sample solution, the limits of detection (3{sigma}) were ranged from 41.4 pg mL{sup -1} (Yb) to 448 pg mL{sup -1} (Gd) with relative standard deviations (RSDs) of 1.0% (Eu)-5.9% (Sm) for on-line CPE-ICP-OES with 8-Ox as chelating agent, and 69.0 pg mL{sup -1} (Sc) to 509.5 pg mL{sup -1} (Sm) with RSDs of 2.9% (Yb)-7.5% (Ho) for on-line CPE-ICP-OES without 8-Ox as chelating agent, respectively. The sample throughput of 17 samples h{sup -1} was obtained for both systems. The developed methods of on-line CPE-ICP-OES were validated by the analysis of certified reference material (GBW07605, tea leaves) and real biological samples of pig liver, Auricularia auricula and mushroom.

  2. Restricted accessed material-copper(II) ion imprinted polymer solid phase extraction combined with inductively coupled plasma-optical emission spectrometry for the determination of free Cu(II) in urine and serum samples.

    Science.gov (United States)

    Cui, Chao; He, Man; Chen, Beibei; Hu, Bin

    2013-11-15

    A novel restricted accessed material (RAM)-Cu(II) ion imprinted polymer (IIP) was synthesized by the surface imprinted-emulsion method, and possessed a high selectivity to Cu(II) and good macromolecules exclusion property. And a novel method of RAM-IIP packed microcolumn solid phase extraction (SPE) combined with inductively coupled plasma-optical emission spectrometry (ICP-OES) was developed for the determination of trace free Cu(II) in human body fluids. Under the optimized conditions, the adsorption capacity of RAM-IIP for Cu(II) was 15.9 mg g(-1). With a preconcentration factor of 30, the limit of detection was 0.17 µg L(-1), and the relative standard deviation was 2.2% (n=7, c=1 µg L(-1)). The developed method was validated by the analysis of two Certified Reference Materials, and the determined values were in good agreement with the certified values. This method was also successfully applied for the direct analysis of free Cu(II) in human urine and serum samples. While the total Cu can be determined by the proposed method after microwave digestion. The concentrations of free Cu(II) were much lower than that of total Cu, indicating that Cu is mainly coordinated with macromolecules in these biological samples. From this point of view, the developed method exhibits application potential in speciation of free metal ions and metallic complex molecules in biological samples. © 2013 Elsevier B.V. All rights reserved.

  3. Analysis of organic compounds of water-in-crude oil emulsions separated by microwave heating using comprehensive two-dimensional gas chromatography and time-of-flight mass spectrometry.

    Science.gov (United States)

    Freitas, Lisiane S; Von Mühlen, Carin; Bortoluzzi, Janaína H; Zini, Claudia A; Fortuny, Montserrat; Dariva, Claudio; Coutinho, Raquel C C; Santos, Alexandre F; Caramão, Elina B

    2009-04-03

    In this work the higher peak capacity and resolution of comprehensive two-dimensional gas chromatography (GCxGC) has been successfully applied, for the first time, to tentatively identify several polar organic compounds of organic extracts of aqueous phases resulting from microwave demulsification process of water-in-crude oil emulsions. Results have shown that higher temperatures and longer exposure time to microwave irradiation produced water phases with a wider variety of polar organic compounds. The microwave process showed to be suitable for the extraction of several polar compounds classes of petroleum. The proposed microwave extraction method and GCxGC identification of polar compounds of petroleum samples are of practical interest for the petrochemical industry due to corrosion and related problems associated with these polar compounds in refinery equipments. The GCxGC/time-of-flight MS technique shows to be very important in the total separation of different classes of compounds and allows the identification of many compounds in these classes.

  4. LISA propulsion module separation study

    Energy Technology Data Exchange (ETDEWEB)

    Merkowitz, S M [NASA Goddard Space Flight Center, Greenbelt, MD 20771 (United States); Ahmad, A [NASA Goddard Space Flight Center, Greenbelt, MD 20771 (United States); Hyde, T T [NASA Goddard Space Flight Center, Greenbelt, MD 20771 (United States); Sweetser, T [Jet Propulsion Laboratory, California Institute of Technology, Pasadena, CA 91109 (United States); Ziemer, J [Jet Propulsion Laboratory, California Institute of Technology, Pasadena, CA 91109 (United States); Conkey, S [Swales Aerospace, 5050 Powder Mill Road, Beltsville, MD 20705 (United States); III, W Kelly [Swales Aerospace, 5050 Powder Mill Road, Beltsville, MD 20705 (United States); Shirgur, B [Swales Aerospace, 5050 Powder Mill Road, Beltsville, MD 20705 (United States)

    2005-05-21

    The Laser Interferometer Space Antenna (LISA) mission is a space-borne gravitational wave detector consisting of three sciencecraft in heliocentric orbit. Each sciencecraft is delivered to its operational orbit by a propulsion module. Because of the strict thermal and mass balancing requirements of LISA, the baseline mission concept requires that the propulsion module separate from the sciencecraft after delivery. The only propulsion system currently included in the sciencecraft design are micronewton level thrusters, such as field emission electric propulsion (FEEP) or colloid thrusters, that are used to balance the 30-40 {mu}N of solar radiation pressure and provide the drag-free and attitude control of the sciencecraft. Due to these thrusters' limited authority, the separation of the propulsion module from the sciencecraft must be well controlled to not induce a large tip-off rotation of the sciencecraft. We present here the results of a study of the propulsion module separation system requirements that are necessary to safely deliver the three LISA sciencecraft to their final operational orbits.

  5. On-line complexation/cloud point preconcentration for the sensitive determination of dysprosium in urine by flow injection inductively coupled plasma-optical emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Ortega, Claudia; Cerutti, Soledad; Silva, Maria F. [Departamento de Quimica Analitica, Facultad de Quimica, Bioquimica y Farmacia, Universidad Nacional de San Luis, Chacabuco y Pedernera, 5700, San Luis (Argentina); Olsina, Roberto A.; Martinez, Luis D. [Departamento de Quimica Analitica, Facultad de Quimica, Bioquimica y Farmacia, Universidad Nacional de San Luis, Chacabuco y Pedernera, 5700, San Luis (Argentina); Consejo Nacional de Investigaciones Cientificas y Tecnicas (CONICET), Avda. Rivadavia 1917, CP C1033AAJJ, Buenos Aires (Argentina)

    2003-01-01

    An on-line dysprosium preconcentration and determination system based on the hyphenation of cloud point extraction (CPE) to flow injection analysis (FIA) associated with ICP-OES was studied. For the preconcentration of dysprosium, a Dy(III)-2-(5-bromo-2-pyridylazo)-5-diethylaminophenol complex was formed on-line at pH 9.22 in the presence of nonionic micelles of PONPE-7.5. The micellar system containing the complex was thermostated at 30 C in order to promote phase separation, and the surfactant-rich phase was retained in a microcolumn packed with cotton at pH 9.2. The surfactant-rich phase was eluted with 4 mol L{sup -1} nitric acid at a flow rate of 1.5 mL min{sup -1}, directly in the nebulizer of the plasma. An enhancement factor of 50 was obtained for the preconcentration of 50 mL of sample solution. The detection limit value for the preconcentration of 50 mL of aqueous solution of Dy was 0.03 {mu}g L{sup -1}. The precision for 10 replicate determinations at the 2.0 {mu}g L{sup -1}Dy level was 2.2% relative standard deviation (RSD), calculated from the peak heights obtained. The calibration graph using the preconcentration system for dysprosium was linear with a correlation coefficient of 0.9994 at levels near the detection limits up to at least 100 {mu}g L {sup -1}. The method was successfully applied to the determination of dysprosium in urine. (orig.)

  6. Rest mass or inertial mass?

    OpenAIRE

    Khrapko, R. I.

    2001-01-01

    Rest mass takes the place of inertial mass in modern physics textbooks. It seems to be wrong. But this phenomenon is hidden away by the facts that rest mass adherents busily call rest mass "mass", not rest mass, and the word "mass" is associated with a measure of inertia. This topic has been considered by the author in the article "What is mass?" [1, 2, 3]. Additional arguments to a confirmation of such a thesis are presented here.

  7. Preparation of Fe3O4@PPy magnetic nanoparticles as solid-phase extraction sorbents for preconcentration and separation of phthalic acid esters in water by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Zhao, Hongyan; Huang, Manyan; Wu, Jianrong; Wang, Li; He, Hua

    2016-02-01

    The purpose of this paper is to introduce a solid-phase extraction method of separating and determining of phthalic acid esters (PAEs) by PPy-coated Fe3O4 magnetic nanoparticles (Fe3O4@PPy MNPs). In the process, nanoparticles were served as sorbents and the optimal conditions of the extraction have been explored. The composite was synthesized through the chemical oxidation method, combining pyrrole monomer with Fe3O4 magnetic ball in the form of aggregation state and the coated nanoparticles possessed core-shell construction. The PPy-coated Fe3O4 magnetic microspheres have been extensively characterized by transmission electron microscopy, Fourier transform infrared spectroscopy and vibrating sample magnetometry. The optimum conditions were investigated by orthogonal experimental design, which was used to testing the influence of main factors and the interactions among them. The orthoplan is famous for the merit that it can study the whole experiments comprehensively through minimal tests. Under the optimal extraction conditions: 20mg of modified magnetite nanoparticles, eluting with acetic ester of 2mL, 40min of MSPE, eluting in 1h and 20mL of sample volume, good linearity (r(2)>0.9912) of all calibration curves was obtained in validation experiments. And the limits of detection (LODs) were from 0.006 to 0.021ng/mL. The recoveries in different sample matrices were in the range from 80.4% to 108.2% with relative standard deviations less than 12.8%. The present work demonstrates the applicability of the developed method for the determination of PAEs in water sample and the results justified that it can be applied successfully to the selective isolation and enrichment of PAEs in real water samples.

  8. Bioequivalence study between a fixed-dose single-pill formulation of nebivolol plus hydrochlorothiazide and separate formulations in healthy subjects using high-performance liquid chromatography coupled to tandem mass spectrometry.

    Science.gov (United States)

    Vespasiano, Celso Francisco Pimentel; Laurito, Tiago Luders; Iwamoto, Renan Donomae; Moreno, Ronilson Agnaldo; Mendes, Gustavo D; De Nucci, Gilberto

    2016-11-03

    Systemic arterial hypertension is a major risk factor for cerebrovascular disease. Therefore, adequate control of blood pressure is of enormous importance. One of the many fixed-dose single-pill antihypertensive formulations available on the market is the combination of nebivolol and hydrochlorothiazide. The objective of this study was to develop two distinct high-performance liquid chromatography coupled to tandem mass spectrometry methods to simultaneously quantify nebivolol and hydrochlorothiazide in human plasma. The methods were employed in a bioequivalence study, the first assay involving a nebivolol fixed-dose single-pill formulation based on healthy Brazilian volunteers. Nebilet HCT™ (nebivolol 5 mg + hydrochlorothiazide 12.5 mg tablet, manufactured by Menarini) was the test formulation. The reference formulations were Nebilet™ (nebivolol 5 mg tablet, manufactured by Menarini) and Clorana™ (hydrochlorothiazide 25 mg tablet, manufactured by Sanofi). For both analytes, liquid-liquid extraction was employed for sample preparation and the chromatographic run time was 3.5 min. The limits of quantification validated were 0.02 ng/mL for nebivolol and 1 ng/mL for hydrochlorothiazide. Since the 90% CI for Cmax , AUC(0-last) and AUC(0-inf) individual test/reference ratios were within the 80-125% interval indicative of bioequivalence, it was concluded that Nebilet HCT™ is bioequivalent to Nebilet™ and Clorana™.

  9. Spatial separation of molecular conformers and clusters.

    Science.gov (United States)

    Horke, Daniel; Trippel, Sebastian; Chang, Yuan-Pin; Stern, Stephan; Mullins, Terry; Kierspel, Thomas; Küpper, Jochen

    2014-01-09

    Gas-phase molecular physics and physical chemistry experiments commonly use supersonic expansions through pulsed valves for the production of cold molecular beams. However, these beams often contain multiple conformers and clusters, even at low rotational temperatures. We present an experimental methodology that allows the spatial separation of these constituent parts of a molecular beam expansion. Using an electric deflector the beam is separated by its mass-to-dipole moment ratio, analogous to a bender or an electric sector mass spectrometer spatially dispersing charged molecules on the basis of their mass-to-charge ratio. This deflector exploits the Stark effect in an inhomogeneous electric field and allows the separation of individual species of polar neutral molecules and clusters. It furthermore allows the selection of the coldest part of a molecular beam, as low-energy rotational quantum states generally experience the largest deflection. Different structural isomers (conformers) of a species can be separated due to the different arrangement of functional groups, which leads to distinct dipole moments. These are exploited by the electrostatic deflector for the production of a conformationally pure sample from a molecular beam. Similarly, specific cluster stoichiometries can be selected, as the mass and dipole moment of a given cluster depends on the degree of solvation around the parent molecule. This allows experiments on specific cluster sizes and structures, enabling the systematic study of solvation of neutral molecules.

  10. Radiochemical separation of Cobalt

    NARCIS (Netherlands)

    Erkelens, P.C. van

    1961-01-01

    A method is described for the radiochemical separation of cobalt based on the extraordinary stability of cobalt diethyldithiocarbamate. Interferences are few; only very small amounts of zinc and iron accompany cobalt, which is important in neutron-activation analysis.

  11. On Separate Universes

    CERN Document Server

    Dai, Liang; Schmidt, Fabian

    2015-01-01

    The separate universe conjecture states that in General Relativity a density perturbation behaves locally (i.e. on scales much smaller than the wavelength of the mode) as a separate universe with different background density and curvature. We prove this conjecture for a spherical compensated tophat density perturbation of arbitrary amplitude and radius in $\\Lambda$CDM. We then use Conformal Fermi Coordinates to generalize this result to scalar perturbations of arbitrary configuration and scale in a general cosmology with a mixture of fluids, but to linear order in perturbations. In this case, the separate universe conjecture holds for the isotropic part of the perturbations. The anisotropic part on the other hand is exactly captured by a tidal field in the Newtonian form. We show that the separate universe picture is restricted to scales larger than the sound horizons of all fluid components. We then derive an expression for the locally measured matter bispectrum induced by a long-wavelength mode of arbitrary...

  12. Shoulder separation - aftercare

    Science.gov (United States)

    ... and top of your shoulder blade A severe shoulder separation You may need surgery right away if you have: Numbness in your fingers Cold fingers Muscle weakness in your arm Severe deformity of the joint

  13. Radiochemical separation of Cobalt

    NARCIS (Netherlands)

    Erkelens, P.C. van

    1961-01-01

    A method is described for the radiochemical separation of cobalt based on the extraordinary stability of cobalt diethyldithiocarbamate. Interferences are few; only very small amounts of zinc and iron accompany cobalt, which is important in neutron-activation analysis.

  14. Safe Separators for Treewidth

    NARCIS (Netherlands)

    Bodlaender, H.L.; Koster, A.M.C.A.

    2003-01-01

    A set of vertices S Í V is called a safe separator for treewidth, if S is a separator of G, and the treewidth of G equals the maximum of the treewidth over all connected components W of G - S of the graph, obtained by making S a clique in the subgraph of G, induced by W È S. We show that such safe s

  15. Hydrogen separation process

    Science.gov (United States)

    Mundschau, Michael [Longmont, CO; Xie, Xiaobing [Foster City, CA; Evenson, IV, Carl; Grimmer, Paul [Longmont, CO; Wright, Harold [Longmont, CO

    2011-05-24

    A method for separating a hydrogen-rich product stream from a feed stream comprising hydrogen and at least one carbon-containing gas, comprising feeding the feed stream, at an inlet pressure greater than atmospheric pressure and a temperature greater than 200.degree. C., to a hydrogen separation membrane system comprising a membrane that is selectively permeable to hydrogen, and producing a hydrogen-rich permeate product stream on the permeate side of the membrane and a carbon dioxide-rich product raffinate stream on the raffinate side of the membrane. A method for separating a hydrogen-rich product stream from a feed stream comprising hydrogen and at least one carbon-containing gas, comprising feeding the feed stream, at an inlet pressure greater than atmospheric pressure and a temperature greater than 200.degree. C., to an integrated water gas shift/hydrogen separation membrane system wherein the hydrogen separation membrane system comprises a membrane that is selectively permeable to hydrogen, and producing a hydrogen-rich permeate product stream on the permeate side of the membrane and a carbon dioxide-rich product raffinate stream on the raffinate side of the membrane. A method for pretreating a membrane, comprising: heating the membrane to a desired operating temperature and desired feed pressure in a flow of inert gas for a sufficient time to cause the membrane to mechanically deform; decreasing the feed pressure to approximately ambient pressure; and optionally, flowing an oxidizing agent across the membrane before, during, or after deformation of the membrane. A method of supporting a hydrogen separation membrane system comprising selecting a hydrogen separation membrane system comprising one or more catalyst outer layers deposited on a hydrogen transport membrane layer and sealing the hydrogen separation membrane system to a porous support.

  16. Separation techniques: Chromatography

    OpenAIRE

    Coskun, Ozlem

    2016-01-01

    Chromatography is an important biophysical technique that enables the separation, identification, and purification of the components of a mixture for qualitative and quantitative analysis. Proteins can be purified based on characteristics such as size and shape, total charge, hydrophobic groups present on the surface, and binding capacity with the stationary phase. Four separation techniques based on molecular characteristics and interaction type use mechanisms of ion exchange, surface adsorp...

  17. Distal humeral epiphyseal separation.

    Science.gov (United States)

    Moucha, Calin S; Mason, Dan E

    2003-10-01

    Distal humeral epiphyseal separation is an uncommon injury that is often misdiagnosed upon initial presentation. To make a timely, correct diagnosis, the treating physician must have a thorough understanding of basic anatomical relationships and an awareness of the existence of this injury. This is a case of a child who sustained a separation of the distal humeral epiphysis, as well as multiple other bony injuries, secondary to child abuse.

  18. The role of macrocyclic compounds in the extraction and possible separation of platinum and rhodium from chloride solutions

    Science.gov (United States)

    Jyothi, Rajesh Kumar; Lee, Jin-Young

    2016-06-01

    Macrocyclic compounds (crown ethers), specifically 18-crown-6 (18-C-6), benzo-15-crown-5 (B-15-C-5), di-benzo-18-crown-6 (DB-18-C-6) and di-cyclohexano-18-crown-6 (DC-18C-6), are used as extractants as well as synergists with amine-group extractants. Platinum and rhodium belong to platinum-group metals (PGMs) and have very similar ionic radii and similar properties. The separation of PGMs is most useful for the preparation of functional materials. Macrocyclic compounds are tested for platinum and rhodium separation and are found to achieve marginal separation. Amines (used as extractants) are paired with macrocyclic compounds (used as synergists), and the separation factor between platinum and rhodium is increased with synergistic enhancement from a chloride solution. The present study discusses extraction chemistry, separation factors and the synergy between platinum and rhodium from chloride solutions. To ensure accurate data, the aqueous samples in this study are analyzed using an inductively coupled plasma optical emission spectrometer (ICP-OES).

  19. High-accuracy determination of iron in seawater by isotope dilution multiple collector inductively coupled plasma mass spectrometry (ID-MC-ICP-MS) using nitrilotriacetic acid chelating resin for pre-concentration and matrix separation

    Energy Technology Data Exchange (ETDEWEB)

    Jong, Jeroen de [Universite Libre de Bruxelles (ULB), Departement des Sciences de la Terre et de l' Environnement (DSTE), Unite Isotopes: Petrologie et Environnement - IPE CP 160/02, Avenue F.D. Roosevelt 50, B-1050 Brussels (Belgium)], E-mail: jdejong@ulb.ac.be; Schoemann, Veronique [Universite Libre de Bruxelles (ULB), Ecologie des Systemes Aquatiques (ESA) CP 221, Avenue F.D. Roosevelt 50, B-1050 Brussels (Belgium); Lannuzel, Delphine [Universite Libre de Bruxelles (ULB), Departement des Sciences de la Terre et de l' Environnement (DSTE), Laboratoire d' Oceanographie Chimique et Geochimie des Eaux - LOCGE CP 208, Avenue F.D. Roosevelt 50, B-1050 Brussels (Belgium); Tison, Jean-Louis [Universite Libre de Bruxelles (ULB), Departement des Sciences de la Terre et de l' Environnement (DSTE), Laboratoire de Glaciologie - GLACIOL CP 160/03, Avenue F.D. Roosevelt 50, B-1050 Brussels (Belgium); Mattielli, Nadine [Universite Libre de Bruxelles (ULB), Departement des Sciences de la Terre et de l' Environnement (DSTE), Unite Isotopes: Petrologie et Environnement - IPE CP 160/02, Avenue F.D. Roosevelt 50, B-1050 Brussels (Belgium)

    2008-08-15

    In the present paper we describe a robust and simple method to measure dissolved iron (DFe) concentrations in seawater down to <0.1 nmol L{sup -1} level, by isotope dilution multiple collector inductively coupled plasma mass spectrometry (ID-MC-ICP-MS) using a {sup 54}Fe spike and measuring the {sup 57}Fe/{sup 54}Fe ratio. The method provides for a pre-concentration step (100:1) by micro-columns filled with the resin NTA Superflow of 50 mL seawater samples acidified to pH 1.9. NTA Superflow is demonstrated to quantitatively extract Fe from acidified seawater samples at this pH. Blanks are kept low (grand mean 0.045 {+-} 0.020 nmol L{sup -1}, n = 21, 3x S.D. limit of detection per session 0.020-0.069 nmol L{sup -1} range), as no buffer is required to adjust the sample pH for optimal extraction, and no other reagents are needed than ultrapure nitric acid, 12 mM H{sub 2}O{sub 2}, and acidified (pH 1.9) ultra-high purity (UHP) water. We measured SAFe (sampling and analysis of Fe) reference seawater samples Surface-1 (0.097 {+-} 0.043 nmol L{sup -1}) and Deep-2 (0.91 {+-} 0.17 nmol L{sup -1}) and obtained results that were in excellent agreement with their DFe consensus values: 0.118 {+-} 0.028 nmol L{sup -1} (n = 7) for Surface-1 and 0.932 {+-} 0.059 nmol L{sup -1} (n = 9) for Deep-2. We also present a vertical DFe profile from the western Weddell Sea collected during the Ice Station Polarstern (ISPOL) ice drift experiment (ANT XXII-2, RV Polarstern) in November 2004-January 2005. The profile shows near-surface DFe concentrations of {approx}0.6 nmol L{sup -1} and bottom water enrichment up to 23 nmol L{sup -1} DFe.

  20. Separable approximation method for two-body relativistic scattering

    Energy Technology Data Exchange (ETDEWEB)

    Tandy, P.C.; Thaler, R.M.

    1988-03-01

    A method for defining a separable approximation to a given interaction within a two-body relativistic equation, such as the Bethe-Salpeter equation, is presented. The rank-N separable representation given here permits exact reproduction of the T matrix on the mass shell and half off the mass shell at N selected bound state and/or continuum values of the invariant mass. The method employed is a four-space generalization of the separable representation developed for Schroedinger interactions by Ernst, Shakin, and Thaler, supplemented by procedures for dealing with the relativistic spin structure in the case of Dirac particles.

  1. Separable approximation method for two-body relativistic scattering

    Science.gov (United States)

    Tandy, P. C.; Thaler, R. M.

    1988-03-01

    A method for defining a separable approximation to a given interaction within a two-body relativistic equation, such as the Bethe-Salpeter equation, is presented. The rank-N separable representation given here permits exact reproduction of the T matrix on the mass shell and half off the mass shell at N selected bound state and/or continuum values of the invariant mass. The method employed is a four-space generalization of the separable representation developed for Schrödinger interactions by Ernst, Shakin, and Thaler, supplemented by procedures for dealing with the relativistic spin structure in the case of Dirac particles.

  2. 分子蒸馏技术拆分独活油及GC-MS分析%Gas chromatography/Mass Spectrometry (GC-MS) Analysis of the Essential Oil from Angelica Pubescens Maxim. by Molecular Distillation Separation

    Institute of Scientific and Technical Information of China (English)

    侯召华; 邹飞雪

    2015-01-01

    The essential oil was extracted from Angelica pubescens Maxim. by steam distillation and fractionated by molecular distillation ( MD ) . The crude essential oil was used as the feed for two molecular distillation processes. One residue ( RF2 ) and two distillate ( DF1 and DF2 ) fractions were prepared by MD. Three fractions were obtained under the operation parameters of 30 ℃,5. 0mbar;and 60℃, 5. 0mbar, respectively. The chemical components of different fractions were analyzed by Gas chromatography/mass spectrometry ( GC-MS) . Results:The yields of distilled fractions ( DF1 ,and DF2 ) and residued fractions (RF2)were 33. 65%,61. 39%,and 3. 88% (w/w),respectively. GC-MS results revealed that 21 ingredients were detected in the essential oil, including (+)-Limonene,α-Pinene,β-Pinene, Terpinen-4-ol, Eucalyptol, Terpinolene, and (-)-Carveol et. Concentrations and compositions of chemical components in different factions were significantly different. In conclusion, the technology of molecular distillation is a feasible separaction method for essential oil.%独活原油由水蒸汽蒸馏法得到,经过分子蒸馏拆分,得到不同馏分,进行气相色谱-质谱( GC-MS)分析。分子蒸馏为二级,一级条件:蒸发温度30℃、真空度500 Pa、刮膜转速150 r/min;二级条件:蒸发温度60℃、真空度500 Pa、刮膜转速200 r/min;两级进样温度30℃、冷凝水温度10℃。两级分子蒸馏共得到3部分,总上样量336.17 g,回收得到332.51 g,回收率98.92%;一级轻组分(DF1)113.12 g(33.65%);二级轻组分(DF2)206.36 g (61.39%);二级重组分(RF2)13.03 g,所占质量比3.88%。原油和馏分物中共确定21种化合物,主要是右旋萜二烯、α-蒎烯、4-异丙基甲苯、萜品烯、月桂烯等;三部分馏分物( DF1,DF2和RF2)和原油中组分数量分别为8、10、17和6种;且不同组分中成分数量及浓度差异显著。分子蒸馏是一种有效的分离纯化技术,可应用于挥发油的加工利用。

  3. Deconstructed Transverse Mass Variables

    CERN Document Server

    Ismail, Ahmed; Virzi, Joseph S; Walker, Devin G E

    2014-01-01

    Traditional searches for R-parity conserving natural supersymmetry (SUSY) require large transverse mass and missing energy cuts to separate the signal from large backgrounds. SUSY models with compressed spectra inherently produce signal events with small amounts of missing energy that are hard to explore. We use this difficulty to motivate the construction of "deconstructed" transverse mass variables which are designed preserve information on both the norm and direction of the missing momentum. We demonstrate the effectiveness of these variables in searches for the pair production of supersymmetric top-quark partners which subsequently decay into a final state with an isolated lepton, jets and missing energy. We show that the use of deconstructed transverse mass variables extends the accessible compressed spectra parameter space beyond the region probed by traditional methods. The parameter space can further be expanded to neutralino masses that are larger than the difference between the stop and top masses. ...

  4. Organic Separation Test Results

    Energy Technology Data Exchange (ETDEWEB)

    Russell, Renee L.; Rinehart, Donald E.; Peterson, Reid A.

    2014-09-22

    Separable organics have been defined as “those organic compounds of very limited solubility in the bulk waste and that can form a separate liquid phase or layer” (Smalley and Nguyen 2013), and result from three main solvent extraction processes: U Plant Uranium Recovery Process, B Plant Waste Fractionation Process, and Plutonium Uranium Extraction (PUREX) Process. The primary organic solvents associated with tank solids are TBP, D2EHPA, and NPH. There is concern that, while this organic material is bound to the sludge particles as it is stored in the tanks, waste feed delivery activities, specifically transfer pump and mixer pump operations, could cause the organics to form a separated layer in the tank farms feed tank. Therefore, Washington River Protection Solutions (WRPS) is experimentally evaluating the potential of organic solvents separating from the tank solids (sludge) during waste feed delivery activities, specifically the waste mixing and transfer processes. Given the Hanford Tank Waste Treatment and Immobilization Plant (WTP) waste acceptance criteria per the Waste Feed Acceptance Criteria document (24590-WTP-RPT-MGT-11-014) that there is to be “no visible layer” of separable organics in the waste feed, this would result in the batch being unacceptable to transfer to WTP. This study is of particular importance to WRPS because of these WTP requirements.

  5. Gulf stream separation dynamics

    Science.gov (United States)

    Schoonover, Joseph

    Climate models currently struggle with the more traditional, coarse ( O(100 km) ) representation of the ocean. In these coarse ocean simulations, western boundary currents are notoriously difficult to model accurately. The modeled Gulf Stream is typically seen exhibiting a mean pathway that is north of observations, and is linked to a warm sea-surface temperature bias in the Mid-Atlantic Bight. Although increased resolution ( O(10 km) ) improves the modeled Gulf Stream position, there is no clean recipe for obtaining the proper pathway. The 70 year history of literature on the Gulf Stream separation suggests that we have not reached a resolution on the dynamics that control the current's pathway just south of the Mid-Atlantic Bight. Without a concrete knowledge on the separation dynamics, we cannot provide a clean recipe for accurately modeling the Gulf Stream at increased resolutions. Further, any reliable parameterization that yields a realistic Gulf Stream path must express the proper physics of separation. The goal of this dissertation is to determine what controls the Gulf Stream separation. To do so, we examine the results of a model intercomparison study and a set of numerical regional terraforming experiments. It is argued that the separation is governed by local dynamics that are most sensitive to the steepening of the continental shelf, consistent with the topographic wave arrest hypothesis of Stern (1998). A linear extension of Stern's theory is provided, which illustrates that wave arrest is possible for a continuously stratified fluid.

  6. Separably injective Banach spaces

    CERN Document Server

    Avilés, Antonio; Castillo, Jesús M F; González, Manuel; Moreno, Yolanda

    2016-01-01

    This monograph contains a detailed exposition of the up-to-date theory of separably injective spaces: new and old results are put into perspective with concrete examples (such as l∞/c0 and C(K) spaces, where K is a finite height compact space or an F-space, ultrapowers of L∞ spaces and spaces of universal disposition). It is no exaggeration to say that the theory of separably injective Banach spaces is strikingly different from that of injective spaces. For instance, separably injective Banach spaces are not necessarily isometric to, or complemented subspaces of, spaces of continuous functions on a compact space. Moreover, in contrast to the scarcity of examples and general results concerning injective spaces, we know of many different types of separably injective spaces and there is a rich theory around them. The monograph is completed with a preparatory chapter on injective spaces, a chapter on higher cardinal versions of separable injectivity and a lively discussion of open problems and further lines o...

  7. Investigations on the use of pneumatic cross-flow nebulizers with dual solution loading including the correction of matrix effects in elemental determinations by inductively coupled plasma optical emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Bauer, Mathieu [Institute for Inorganic and Applied Chemistry, University of Hamburg, Martin-Luther-King-Platz 6, D-20146 Hamburg (Germany); Broekaert, Jose A.C. [Institute for Inorganic and Applied Chemistry, University of Hamburg, Martin-Luther-King-Platz 6, D-20146 Hamburg (Germany)], E-mail: jose.broekaert@chemie.uni-hamburg.de

    2007-02-15

    The use of a so-called trihedral and a T-shaped cross-flow pneumatic nebulizer with dual solution loading for inductively coupled plasma optical emission spectrometry has been studied. By these devices analyte clouds from two solutions can be mixed during the aerosol generation step. For both nebulizers the correction of matrix effects using internal standardization and standard addition calibration in an on-line way was investigated and compared to elemental determinations using a conventional cross-flow nebulizer and calibration with synthetic standard solutions without matrix matching. A significant improvement of accuracy, both for calibration with internal standardization and standard addition, was obtained in the case of four synthetic solutions containing each 40 mmol L{sup -1} Na, K, Rb and Ba as matrix elements and 300 {mu}g L{sup -1} Cd, Co, Cr, Cu, Fe, Mn, Ni and Pb as analytes. Calibration by standard addition in the case of dual solution loading has been shown to be very useful in the determination of elements at minor and trace levels in steel and alumina reference materials. The results of analysis for minor concentrations of Cr, Cu and Ni in steel as well as for Ca, Fe, Ga, Li, Mg, Mn, Na, Si and Zn in alumina powder certified reference materials subsequent to sample dissolution were found to be in good agreement with the certificates. Limits of detection were found to be only slightly above those for a conventional cross-flow nebulizer and a precision better than 3% was realized with both novel nebulizers.

  8. Analysis of metals and phosphorus in biodiesel B100 from different feedstock using a Flow Blurring® multinebulizer in inductively coupled plasma-optical emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Avila Orozco, Francisco D. [Lab. FIA, Sección Química Analítica, INQUISUR (UNS-CONICET), Universidad Nacional del Sur, Avenida Alem 1253, B8000CPB, Bahía Blanca (Argentina); Kovachev, Nikolay; Aguirre Pastor, Miguel Ángel [Dpto. Química Analítica, Nutrición y Bromatología e Instituto Universitario de Materiales, Facultad de Ciencias, Universidad de Alicante, Apdo. 99, Alicante (Spain); Domini, Claudia E.; Fernández Band, Beatriz S. [Lab. FIA, Sección Química Analítica, INQUISUR (UNS-CONICET), Universidad Nacional del Sur, Avenida Alem 1253, B8000CPB, Bahía Blanca (Argentina); Canals Hernández, Antonio, E-mail: a.canals@ua.es [Dpto. Química Analítica, Nutrición y Bromatología e Instituto Universitario de Materiales, Facultad de Ciencias, Universidad de Alicante, Apdo. 99, Alicante (Spain)

    2014-05-01

    Highlights: • The elemental analysis of biodiesel by the proposed method is simple and fast. • Two-nozzles Flow Blurring® nebulizer allow to reduce the spectral interferences. • Two-nozzles Flow Blurring® nebulizer avoid the formation of carbon deposits. • The analysis may be carried out without any sample pretreatment. Abstract: A simple and fast method for determining the content of Na, K, Ca, Mg, P, and 20 heavy metals in biodiesel samples with inductively coupled plasma optical emission spectrometry (ICP OES) using a two-nozzle Flow Blurring® multinebulizer prototype and on-line internal standard calibration, are proposed. The biodiesel samples were produced from different feedstock such as sunflower, corn, soybean and grape seed oils, via a base catalyst transesterification. The analysis was carried out without any sample pretreatment. The standards and samples were introduced through one of the multinebulizer nozzles, while the aqueous solution containing yttrium as an internal standard was introduced through the second nozzle. Thus, the spectral interferences were compensated and the formation of carbon deposits on the ICP torch was prevented. The determination coefficients (R²) were greater than 0.99 for the studied analytes, in the range 0.21–14.75 mg kg⁻¹. Short-term and long-term precisions were estimated as relative standard deviation. These were acceptable, their values being lower than 10%. The LOQ for major components such as Ca, K, Mg, Na, and P, were within a range between 4.9 ng g⁻¹ for Mg (279.553 nm) and 531.1 ng g⁻¹ for Na (588.995 nm), and for the other 20 minor components they were within a range between 1.1 ng g⁻¹ for Ba (455.403 nm) and 2913.9 ng g⁻¹ for Pb (220.353 nm). Recovery values ranged between 95% and 106%.

  9. Understanding the effects of potassium ferricyanide on lead hydride formation in tetrahydroborate system and its application for determination of lead in milk using hydride generation inductively coupled plasma optical emission spectrometry.

    Science.gov (United States)

    Deng, Biyang; Xu, Xiangshu; Xiao, Yan; Zhu, Pingchuan; Wang, Yingzi

    2015-01-01

    To understand the formation of plumbane in the Pb(II)-NaBH4-K3Fe(CN)6 system, the intermediate products produced in the reaction of lead(II) and NaBH4 in the presence of K3Fe(CN)6 were studied. The produced plumbane and elemental lead were measured through continuous flow hydride generation (HG)-inductively coupled plasma optical emission spectrometry (ICP OES) and X-ray diffraction spectrometry techniques, respectively. Based on the experimental results, the explanations can be depicted in the following steps: (1) plumbane and black lead sediment (black Pb) are formed in the reaction of lead(II) and NaBH4; (2) the black Pb is oxidized by K3Fe(CN)6 to form Pb2[Fe(CN)6], which further reacts with NaBH4 to form more plumbane and black Pb; and (3) another round starts in which the produced black Pb from the step 2 is then oxidized continuously by K3Fe(CN)6 to form more Pb2[Fe(CN)6] complex, which would produce more plumbane. In short, the black Pb and Pb2[Fe(CN)6] complex are the key intermediate products for the formation of plumbane in the Pb(II)-NaBH4-K3Fe(CN)6 system. Based on the enhancement effect of potassium ferricyanide and potassium ferrocyanide, a method was developed to analyze lead in milk with HG-ICP OES technique. The detection limit of the method was observed as 0.081 μg L(-1). The linearity range of lead was found between 0.3 and 50,000 μg L(-1) with correlation coefficient of 0.9993. The recovery of lead was determined as 97.6% (n=5) for adding 10 μg L(-1) lead into the milk sample.

  10. Phaco slice and separate.

    Science.gov (United States)

    Arshinoff, S A

    1999-04-01

    Phaco slice and separate retains the advantages of the chopping techniques of Nagahara, Koch, and Fukasaku but replaces chopping or snapping with slicing across the center of the phaco-tip-stabilized nucleus using a Nagahara chopper and then repositioning the chopper to optimally separate the divided lens halves. As the lens is rotated in the capsular bag, small pieces of the nuclear pie are sliced off, separated, emulsified, and aspirated. Emulsification and aspiration can alternatively be left until most or all the slices have been made. This technique works with a broader range of lens densities than other chopping techniques and uses no sculpting and very little phaco time. The phaco time required for this technique is relatively independent of nuclear density compared with a sculpting technique.

  11. Membrane separation of hydrocarbons

    Science.gov (United States)

    Chang, Y. Alice; Kulkarni, Sudhir S.; Funk, Edward W.

    1986-01-01

    Mixtures of heavy oils and light hydrocarbons may be separated by passing the mixture through a polymeric membrane. The membrane which is utilized to effect the separation comprises a polymer which is capable of maintaining its integrity in the presence of hydrocarbon compounds and which has been modified by being subjected to the action of a sulfonating agent. Sulfonating agents which may be employed will include fuming sulfuric acid, chlorosulfonic acid, sulfur trioxide, etc., the surface or bulk modified polymer will contain a degree of sulfonation ranging from about 15 to about 50%. The separation process is effected at temperatures ranging from about ambient to about 100.degree. C. and pressures ranging from about 50 to about 1000 psig.

  12. Gas separation membranes

    Science.gov (United States)

    Schell, William J.

    1979-01-01

    A dry, fabric supported, polymeric gas separation membrane, such as cellulose acetate, is prepared by casting a solution of the polymer onto a shrinkable fabric preferably formed of synthetic polymers such as polyester or polyamide filaments before washing, stretching or calendering (so called griege goods). The supported membrane is then subjected to gelling, annealing, and drying by solvent exchange. During the processing steps, both the fabric support and the membrane shrink a preselected, controlled amount which prevents curling, wrinkling or cracking of the membrane in flat form or when spirally wound into a gas separation element.

  13. Separation membrane development

    Energy Technology Data Exchange (ETDEWEB)

    Lee, M.W. [Savannah River Technology Center, Aiken, SC (United States)

    1998-08-01

    A ceramic membrane has been developed to separate hydrogen from other gases. The method used is a sol-gel process. A thin layer of dense ceramic material is coated on a coarse ceramic filter substrate. The pore size distribution in the thin layer is controlled by a densification of the coating materials by heat treatment. The membrane has been tested by permeation measurement of the hydrogen and other gases. Selectivity of the membrane has been achieved to separate hydrogen from carbon monoxide. The permeation rate of hydrogen through the ceramic membrane was about 20 times larger than Pd-Ag membrane.

  14. Separation techniques: Chromatography

    Science.gov (United States)

    Coskun, Ozlem

    2016-01-01

    Chromatography is an important biophysical technique that enables the separation, identification, and purification of the components of a mixture for qualitative and quantitative analysis. Proteins can be purified based on characteristics such as size and shape, total charge, hydrophobic groups present on the surface, and binding capacity with the stationary phase. Four separation techniques based on molecular characteristics and interaction type use mechanisms of ion exchange, surface adsorption, partition, and size exclusion. Other chromatography techniques are based on the stationary bed, including column, thin layer, and paper chromatography. Column chromatography is one of the most common methods of protein purification. PMID:28058406

  15. Learning Isometric Separation Maps

    CERN Document Server

    Vasiloglou, Nikolaos; Anderson, David V

    2008-01-01

    Maximum Variance Unfolding (MVU) and its variants have been very successful in embedding data-manifolds in lower dimensionality spaces, often revealing the true intrinsic dimensions. In this paper we show how to also incorporate supervised class information into an MVU-like method without breaking its convexity. We call this method the Isometric Separation Map and we show that the resulting kernel matrix can be used for a binary/multiclass Support Vector Machine in a semi-supervised (transductive) framework. We also show that the method always finds a kernel matrix that linearly separates the training data exactly without projecting them in infinite dimensional spaces.

  16. Separators for electrochemical cells

    Science.gov (United States)

    Carlson, Steven Allen; Anakor, Ifenna Kingsley

    2014-11-11

    Provided are separators for use in an electrochemical cell comprising (a) an inorganic oxide and (b) an organic polymer, wherein the inorganic oxide comprises organic substituents. Preferably, the inorganic oxide comprises an hydrated aluminum oxide of the formula Al.sub.2O.sub.3.xH.sub.2O, wherein x is less than 1.0, and wherein the hydrated aluminum oxide comprises organic substituents, preferably comprising a reaction product of a multifunctional monomer and/or organic carbonate with an aluminum oxide, such as pseudo-boehmite and an aluminum oxide. Also provided are electrochemical cells comprising such separators.

  17. Digital Imaging Mass Spectrometry

    CERN Document Server

    Bamberger, Casimir; Bamberger, Andreas

    2011-01-01

    Methods to visualize the two-dimensional distribution of molecules by mass spectrometric imaging evolve rapidly and yield novel applications in biology, medicine, and material surface sciences. Most mass spectrometric imagers acquire high mass resolution spectra spot-by-spot and thereby scan the object's surface. Thus, imaging is slow and image reconstruction remains cumbersome. Here we describe an imaging mass spectrometer that exploits the true imaging capabilities by ion optical means for the time of flight mass separation. The mass spectrometer is equipped with the ASIC Timepix chip as an array detector to acquire the position, mass, and intensity of ions that are imaged by MALDI directly from the target sample onto the detector. This imaging mass spectrometer has a spatial resolving power at the specimen of (84\\pm35) \\mu m with a mass resolution of 45 and locates atoms or organic compounds on a surface area up to ~2 cm2. Extended laser spots of ~5 mm2 on structured specimens allowed parallel imaging of s...

  18. Separation, preconcentration and inductively coupled plasma-mass spectrometric (ICP-MS) determination of thorium(IV), titanium(IV), iron(III), lead(II) and chromium(III) on 2-nitroso-1-naphthol impregnated MCI GEL CHP20P resin

    Energy Technology Data Exchange (ETDEWEB)

    Aydin, Funda Armagan [Erciyes University, Faculty of Art and Science, Department of Chemistry, 38039 Kayseri (Turkey); General Directorate of State Hydraulic Works, Technical Research and Quality Control Department, 06100 Ankara (Turkey); Soylak, Mustafa, E-mail: soylak@erciyes.edu.tr [Erciyes University, Faculty of Art and Science, Department of Chemistry, 38039 Kayseri (Turkey)

    2010-01-15

    A simple and effective method is presented for the separation and preconcentration of Th(IV), Ti(IV), Fe(III), Pb(II) and Cr(III) by solid phase extraction on 2-nitroso-1-naphthol impregnated MCI GEL CHP20P resin prior to their inductively coupled plasma-mass spectrometric determinations. The influence of analytical parameters including pH of the aqueous solution, flow rates of sample and eluent solutions and sample volume on the quantitative recoveries of analyte ions was investigated. Matrix effects caused by the presence of alkali, earth alkali and some metal ions in the analyzed solutions were investigated. The presented solid phase extraction method was applied to BCR-144R Sewage Sludge (domestic origin), BCR-141R Calcareous Loam Soil, NIST 1568a Rice Flour and NIST 1577b Bovine Liver certified reference materials (CRMs) for the determination of analyte ions and the results were in good agreement with the certified values. The separation procedure presented was also applied to the various natural water samples collected from Turkey with satisfactory results.

  19. Separation, preconcentration and inductively coupled plasma-mass spectrometric (ICP-MS) determination of thorium(IV), titanium(IV), iron(III), lead(II) and chromium(III) on 2-nitroso-1-naphthol impregnated MCI GEL CHP20P resin.

    Science.gov (United States)

    Aydin, Funda Armagan; Soylak, Mustafa

    2010-01-15

    A simple and effective method is presented for the separation and preconcentration of Th(IV), Ti(IV), Fe(III), Pb(II) and Cr(III) by solid phase extraction on 2-nitroso-1-naphthol impregnated MCI GEL CHP20P resin prior to their inductively coupled plasma-mass spectrometric determinations. The influence of analytical parameters including pH of the aqueous solution, flow rates of sample and eluent solutions and sample volume on the quantitative recoveries of analyte ions was investigated. Matrix effects caused by the presence of alkali, earth alkali and some metal ions in the analyzed solutions were investigated. The presented solid phase extraction method was applied to BCR-144R Sewage Sludge (domestic origin), BCR-141R Calcareous Loam Soil, NIST 1568a Rice Flour and NIST 1577b Bovine Liver certified reference materials (CRMs) for the determination of analyte ions and the results were in good agreement with the certified values. The separation procedure presented was also applied to the various natural water samples collected from Turkey with satisfactory results.

  20. diffusive phase separation

    Directory of Open Access Journals (Sweden)

    Nobuyuki Kenmochi

    1996-01-01

    w is constrained to have double obstacles σ*≤w≤σ* (i.e., σ* and σ* are the threshold values of w. The objective of this paper is to discuss the semigroup {S(t} associated with the phase separation model, and construct its global attractor.

  1. Phase separation micro molding

    NARCIS (Netherlands)

    Vogelaar, Laura

    2005-01-01

    The research described in this thesis concerns the development of a new microfabrication method, Phase Separation Micro Molding (PSμM). While microfabrication is still best known from semiconductor industry, where it is used to integrate electrical components on a chip, the scope has immensely expan

  2. Fathering After Marital Separation

    Science.gov (United States)

    Keshet, Harry Finkelstein; Rosenthal, Kristine M.

    1978-01-01

    Deals with experiences of a group of separated or divorced fathers who chose to remain fully involved in the upbringing of their children. As they underwent transition from married parenthood to single fatherhood, these men learned that meeting demands of child care contributed to personal stability and growth. (Author)

  3. Isotope hydrograph separation

    Energy Technology Data Exchange (ETDEWEB)

    Fritz, P. [UFZ-Umweltforschungszentrum, Centre of Environmental Research Leipzig-Halle, Leipzig (Germany)

    2000-07-01

    Storm-runoff thus reflects the complex hydraulic behaviour of drainage basins and water-links of such systems. Water of different origin may participate in the events and in this lecture, the application of isotope techniques to separate storm hydrographs into different components will be presented.

  4. Unity Through Separation

    DEFF Research Database (Denmark)

    Dabelsteen, Hans B.

    This PhD thesis asks how we can conceptualize the current separation doctrine of religion and politics in a country like Denmark, where the structure of the established church and peoplehood overlap. In order to answer this question, Hans Bruun Dabelsteen maps the current discussion of secularism...

  5. Acromioclavicular Joint Separations

    Science.gov (United States)

    2013-01-01

    Published online: 16 December 2012 # Springer Science+Business Media New York 2012 Abstract Acromioclavicular (AC) joint separations are common...injuries. The sports most likely to cause AC joint dislocations are football, soccer , hockey, rugby, and skiing, among others [9, 28, 29]. The major cause

  6. Pre-Separation Guide

    Science.gov (United States)

    1992-03-04

    SEPARATEES Defense Outplacement Referral System (DORS) Since most of us are not independently wealthy, we will need a job after separation. DORS is...Job Assistance SPOUSES OF ALL SEPARATEES As a spouse you may take advantage of preparing Standard Form 17 1’s and resu- the outplacement services

  7. Separation of Powers.

    Science.gov (United States)

    Bill of Rights in Action, 1987

    1987-01-01

    The dimensions of the separation of powers principle are explored through three lessons in the subject areas of U.S. history, U.S. government, and world history. In 1748, a French nobleman, Baron de Montesquieu, wrote a book called "The Spirit of the Laws," in which he argued that there could be no liberty when all government power was…

  8. Axino mass

    CERN Document Server

    Kim, Jihn E

    2012-01-01

    I will talk on my recent works. Axino, related to the SUSY transformation of axion, can mix with Goldstino in principle. In this short talk, I would like to explain what is the axino mass and its plausible mass range. The axino mass is known to have a hierarchical mass structure depending on accidental symmetries. With only one axino, if G_A=0 where G=K+ 2ln|W|, we obtain axino mass= gravitino mass. For G_A nonzero, the axino mass depends on the details of the Kaehler potential. I also comment on the usefulness of a new parametrization of the CKM matrix.

  9. Novel PEFC Application for Deuterium Isotope Separation

    Directory of Open Access Journals (Sweden)

    Hisayoshi Matsushima

    2017-03-01

    Full Text Available The use of a polymer electrolyte fuel cell (PEFC with a Nafion membrane for isotopic separation of deuterium (D was investigated. Mass analysis at the cathode side indicated that D diffused through the membrane and participated in an isotope exchange reaction. The exchange of D with protium (H in H2O was facilitated by a Pt catalyst. The anodic data showed that the separation efficiency was dependent on the D concentration in the source gas, whereby the water produced during the operation of the PEFC was more enriched in D as the D concentration of the source gas was increased.

  10. Microgravity Passive Phase Separator

    Science.gov (United States)

    Paragano, Matthew; Indoe, William; Darmetko, Jeffrey

    2012-01-01

    A new invention disclosure discusses a structure and process for separating gas from liquids in microgravity. The Microgravity Passive Phase Separator consists of two concentric, pleated, woven stainless- steel screens (25-micrometer nominal pore) with an axial inlet, and an annular outlet between both screens (see figure). Water enters at one end of the center screen at high velocity, eventually passing through the inner screen and out through the annular exit. As gas is introduced into the flow stream, the drag force exerted on the bubble pushes it downstream until flow stagnation or until it reaches an equilibrium point between the surface tension holding bubble to the screen and the drag force. Gas bubbles of a given size will form a front that is moved further down the length of the inner screen with increasing velocity. As more bubbles are added, the front location will remain fixed, but additional bubbles will move to the end of the unit, eventually coming to rest in the large cavity between the unit housing and the outer screen (storage area). Owing to the small size of the pores and the hydrophilic nature of the screen material, gas does not pass through the screen and is retained within the unit for emptying during ground processing. If debris is picked up on the screen, the area closest to the inlet will become clogged, so high-velocity flow will persist farther down the length of the center screen, pushing the bubble front further from the inlet of the inner screen. It is desired to keep the velocity high enough so that, for any bubble size, an area of clean screen exists between the bubbles and the debris. The primary benefits of this innovation are the lack of any need for additional power, strip gas, or location for venting the separated gas. As the unit contains no membrane, the transport fluid will not be lost due to evaporation in the process of gas separation. Separation is performed with relatively low pressure drop based on the large surface

  11. Plasma optical modulators for intense lasers

    Science.gov (United States)

    Yu, Lu-Le; Zhao, Yao; Qian, Lie-Jia; Chen, Min; Weng, Su-Ming; Sheng, Zheng-Ming; Jaroszynski, D. A.; Mori, W. B.; Zhang, Jie

    2016-06-01

    Optical modulators can have high modulation speed and broad bandwidth, while being compact. However, these optical modulators usually work for low-intensity light beams. Here we present an ultrafast, plasma-based optical modulator, which can directly modulate high-power lasers with intensity up to 1016 W cm-2 to produce an extremely broad spectrum with a fractional bandwidth over 100%, extending to the mid-infrared regime in the low-frequency side. This concept relies on two co-propagating laser pulses in a sub-millimetre-scale underdense plasma, where a drive laser pulse first excites an electron plasma wave in its wake while a following carrier laser pulse is modulated by the plasma wave. The laser and plasma parameters suitable for the modulator to work are based on numerical simulations.

  12. Plasma optical modulators for intense lasers

    CERN Document Server

    Yu, Lu-Le; Qian, Lie-Jia; Chen, Min; Weng, Su-Ming; Sheng, Zheng-Ming; Jaroszynski, D A; Mori, W B; Zhang, Jie

    2016-01-01

    Optical modulators can be made nowadays with high modulation speed, broad bandwidth, while being compact, owing to the recent advance in material science and microfabrication technology. However, these optical modulators usually work for low intensity light beams. Here, we present an ultrafast, plasma-based optical modulator, which can directly modulate high power lasers with intensity up to 10^16 W/cm^2 level to produce an extremely broad spectrum with a fractional bandwidth over 100%, extending to the mid-infrared regime in the low-frequency side. This concept relies on two co-propagating laser beams in a sub-mm-scale underdense plasma, where a drive laser pulse first excites an electron plasma wave in its wake while a following carrier laser beam is modulated by the plasma wave. The laser and plasma parameters suitable for the modulator to work are presented. Such optical modulators may enable new applications in the high field physics.

  13. A mechanical model for phase-separation in debris flow

    CERN Document Server

    Pudasaini, Shiva P

    2016-01-01

    Understanding the physics of phase-separation between solid and fluid phases as a mixture mass moves down slope is a long-standing challenge. Here, we propose an extension of the two phase mass flow model (Pudasaini, 2012) by including a new mechanism, called separation-flux, that leads to strong phase-separation in avalanche and debris flows while balancing the enhanced solid flux with the reduced fluid flux. The separation flux mechanism is capable of describing the dynamically evolving phase-separation and levee formation in a multi-phase, geometrically three-dimensional debris flow. These are often observed phenomena in natural debris flows and industrial processes that involve the transportation of particulate solid-fluid mixture material. The novel separation-flux model includes several dominant physical and mechanical aspects such as pressure gradients, volume fractions of solid and fluid phases and their gradients, shear-rates, flow depth, material friction, viscosity, material densities, topographic ...

  14. HRS Separator HD

    CERN Multimedia

    2016-01-01

    Footage of the 90 and 60 degree ISOLDE HRS separator magnets in the HRS separator zone. In the two vacuum sectors HRS20 and HRS30 equipment such as the HRS slits SL240, the HRS faraday cup FC300 and wiregrid WG210 can be spotted. Vacuum valves, turbo pumps, beamlines, quadrupoles, water and compressed air connections, DC and signal cabling can be seen throughout the video. The HRS main and user beamgate in the beamline between MAG90 and MAG60 and its switchboxes as well as all vacuum bellows and flanges are shown. Instrumentation such as the HRS scanner unit 482 / 483, the HRS WG470 wiregrid and slits piston can be seen. The different quadrupoles and supports are shown as well as the RILIS guidance tubes and installation at the magnets and the different radiation monitors.

  15. Nylon separators. [thermal degradation

    Science.gov (United States)

    Lim, H. S.

    1977-01-01

    A nylon separator was placed in a flooded condition in K0H solution and heated at various high temperatures ranging from 60 C to 110 C. The weight decrease was measured and the molecular weight and decomposition product were analyzed to determine: (1) the effect of K0H concentration on the hydrolysis rate; (2) the effect of K0H concentration on nylon degradation; (3) the activation energy at different K0H concentrations; and (4) the effect of oxygen on nylon degradation. The nylon hydrolysis rate is shown to increase as K0H concentration is decreased 34%, giving a maximum rate at about 16%. Separator hydrolysis is confirmed by molecular weight decrease in age of the batteries, and the reaction of nylon with molecular oxygen is probably negligible, compared to hydrolysis. The extrapolated rate value from the high temperature experiment correlates well with experimental values at 35 degrees.

  16. Battery separator manufacturing process

    Energy Technology Data Exchange (ETDEWEB)

    Palmer, N.I.; Sugarman, N.

    1974-12-27

    A battery with a positive plate, a negative plate, and a separator of polymeric resin having a degree of undesirable hydrophobia, solid below 180/sup 0/F, extrudable as a hot melt, and resistant to degradation by at least either acids or alkalies positioned between the plates is described. The separator comprises a nonwoven mat of fibers, the fibers being comprised of the polymeric resin and a wetting agent in an amount of 0.5 to 20 percent by weight based on the weight of the resin with the amount being incompatible with the resin below the melting point of the resin such that the wetting agent will bloom over a period of time at ambient temperatures in a battery, yet being compatible with the resin at the extrusion temperature and bringing about blooming to the surface of the fibers when the fibers are subjected to heat and pressure.

  17. Unity Through Separation

    DEFF Research Database (Denmark)

    Dabelsteen, Hans B.

    analysis, Dabelsteen study Danish secularism as an ideological concept. He finds that the conceptual structure of Danish secularism holds separation-as-principled distance at its core. Institutionally this particularly pertains to the establishment arrangement, and in practice it translates...... and proposes two conceptual expansions. The first is to include modest establishment in a framework of secularism defensible by political liberalism, and the second is to consider secularism in close connection to a theory of peoplehood. Methodologically positioned between interpretive realism and policy...... into the principle of treating everybody equally (with religious freedom, equality and Danish peoplehood as the most important principles adjacent to secularism). In a study of the historical roots of the separation doctrine and two current policy cases (same-sex marriage and reforms of church governance...

  18. Acoustophoresis separation method

    Science.gov (United States)

    Heyman, Joseph S. (Inventor)

    1993-01-01

    A method and apparatus are provided for acoustophoresis, i.e., the separation of species via acoustic waves. An ultrasonic transducer applies an acoustic wave to one end of a sample container containing at least two species having different acoustic absorptions. The wave has a frequency tuned to or harmonized with the point of resonance of the species to be separated. This wave causes the species to be driven to an opposite end of the sample container for removal. A second ultrasonic transducer may be provided to apply a second, oppositely directed acoustic wave to prevent undesired streaming. In addition, a radio frequency tuned to the mechanical resonance and coupled with a magnetic field can serve to identify a species in a medium comprising species with similar absorption coefficients, whereby an acoustic wave having a frequency corresponding to this gyrational rate can then be applied to sweep the identified species to one end of the container for removal.

  19. Separation of enantiomers

    CERN Document Server

    Todd , Matthew H

    2014-01-01

    In one handy volume this handbook summarizes the most common synthetic methods for the separation of racemic mixtures, allowing an easy comparison of the different strategies described in the literature.Alongside classical methods, the authors also consider kinetic resolutions, dynamic kinetic resolutions, divergent reactions of a racemic mixture, and a number of ""neglected"" cases not covered elsewhere, such as the use of circularly polarized light, polymerizations, ""ripening"" processes, dynamic combinatorial chemistry, and several thermodynamic processes. The result is a thorough introdu

  20. Separation Logic and Concurrency

    Science.gov (United States)

    Bornat, Richard

    Concurrent separation logic is a development of Hoare logic adapted to deal with pointers and concurrency. Since its inception, it has been enhanced with a treatment of permissions to enable sharing of data between threads, and a treatment of variables as resource alongside heap cells as resource. An introduction to the logic is given with several examples of proofs, culminating in a treatment of Simpson's 4-slot algorithm, an instance of racy non-blocking concurrency.

  1. Multimodal separation and multistage mass spectrometry of synthetic polymers

    NARCIS (Netherlands)

    Song, J.

    2011-01-01

    Synthetic polymers and polymer-based materials are essential and indispensable in many aspects of our life. An increasing demand of polymers with tailor-made properties has led to an extraordinary range of new materials. Most of the methods for characterisation of polymers only produce results on an

  2. At the target station of the SC ISOLDE mass separator

    CERN Multimedia

    1974-01-01

    The ISOLDE target is hidden behind the HT shielding box. The tunnel leads to the spent proton-beam absorber (beam dump). Stig Sundell stands on the left. At the time of the picture (upgrade period) the beam line leading to target was not (yet) installed.

  3. A LASER ION-SOURCE FOR ONLINE MASS SEPARATION

    NARCIS (Netherlands)

    VANDUPPEN, P; DENDOOVEN, P; HUYSE, M; VERMEEREN, L; QAMHIEH, ZN; SILVERANS, RE; VANDEWEERT, E

    1992-01-01

    A laser ion source based on resonance photo ionization in a gas cell is proposed. The gas cell, filled with helium, consists of a target chamber in which the recoil products are stopped and neutralized, and an ionization chamber where the atoms of interest are selectively ionized by the laser light.

  4. Multimodal separation and multistage mass spectrometry of synthetic polymers

    NARCIS (Netherlands)

    Song, J.

    2011-01-01

    Synthetic polymers and polymer-based materials are essential and indispensable in many aspects of our life. An increasing demand of polymers with tailor-made properties has led to an extraordinary range of new materials. Most of the methods for characterisation of polymers only produce results on an

  5. Realistic Safe-Separation Distance Determination for Mass Fire Hazards

    Science.gov (United States)

    2013-03-25

    amidships tossed the upper decks back, curled and flattened like a banana peel as indicated in Figure 5. Sections of the Liberte were hurled outward...clad frame and sheet metal roof. For the preceding six weeks the temperature in this area of Finland had been relatively high with 30°C being...flaming debris set sheets of cellulose nitrate on fire, feeding an even greater conflagration. Six hours after the explosion, flames were still burning

  6. Are binary separations related to their system mass?

    Directory of Open Access Journals (Sweden)

    Michael F. Sterzik

    2004-01-01

    Full Text Available Listamos los datos m as recientes sobre la fracci on de multiplicidad y la distribuci on de separaciones de binarias para distintas masas de la primaria, incluyendo primarias de muy baja masa y enanas marrones, y las comparamos con modelos din amicos de disoluci on de c umulos con N peque~no. Las predicciones de los modelos est an basadas en c alculos num ericos detallados de la din amica interna de los c umulos as como en m etodos tipo Monte Carlo. Tanto las observaciones como los modelos muestran las mismas tendencias: (1 La fracci on de multiplicidad aumenta con la masa de la primaria. (2 La separaci on media de las binarias aumenta con la masa del sistema, de tal forma que las binarias de muy baja masa tienen separaciones medias del orden de 4 AU, mientras que la separaci on de las binarias de una masa solar tiene un m aximo alrededor de 40 AU. Las binarias de tipo M pueblan preferentemente las separaciones intermedias. Esta tendencia puede quiz as explicarse si la energ a espec ca al momento de formarse el c umulo es similar para c umulos de distintas masas.

  7. Innovative Separations Technologies

    Energy Technology Data Exchange (ETDEWEB)

    J. Tripp; N. Soelberg; R. Wigeland

    2011-05-01

    Reprocessing used nuclear fuel (UNF) is a multi-faceted problem involving chemistry, material properties, and engineering. Technology options are available to meet a variety of processing goals. A decision about which reprocessing method is best depends significantly on the process attributes considered to be a priority. New methods of reprocessing that could provide advantages over the aqueous Plutonium Uranium Reduction Extraction (PUREX) and Uranium Extraction + (UREX+) processes, electrochemical, and other approaches are under investigation in the Fuel Cycle Research and Development (FCR&D) Separations Campaign. In an attempt to develop a revolutionary approach to UNF recycle that may have more favorable characteristics than existing technologies, five innovative separations projects have been initiated. These include: (1) Nitrogen Trifluoride for UNF Processing; (2) Reactive Fluoride Gas (SF6) for UNF Processing; (3) Dry Head-end Nitration Processing; (4) Chlorination Processing of UNF; and (5) Enhanced Oxidation/Chlorination Processing of UNF. This report provides a description of the proposed processes, explores how they fit into the Modified Open Cycle (MOC) and Full Recycle (FR) fuel cycles, and identifies performance differences when compared to 'reference' advanced aqueous and fluoride volatility separations cases. To be able to highlight the key changes to the reference case, general background on advanced aqueous solvent extraction, advanced oxidative processes (e.g., volumetric oxidation, or 'voloxidation,' which is high temperature reaction of oxide UNF with oxygen, or modified using other oxidizing and reducing gases), and fluorination and chlorination processes is provided.

  8. Colour Separation and Aversion

    Directory of Open Access Journals (Sweden)

    Sarah M Haigh

    2012-05-01

    Full Text Available Aversion to achromatic patterns is well documented but relatively little is known about discomfort from chromatic patterns. Large colour differences are uncommon in the natural environment and deviation from natural statistics makes images uncomfortable (Fernandez and Wilkins 2008, Perception, 37(7, 1098–113; Juricevic et al 2010, Perception, 39(7, 884–899. We report twelve studies documenting a linear increase in aversion to chromatic square-wave gratings as a function of the separation in UCS chromaticity between the component bars, independent of their luminance contrast. Two possible explanations for the aversion were investigated: (1 accommodative response, or (2 cortical metabolic demand. We found no correlation between chromaticity separation and accommodative lag or variance in lag, measured using an open-field autorefractor. However, near infrared spectroscopy of the occipital cortex revealed a larger oxyhaemoglobin response to patterns with large chromaticity separation. The aversion may be cortical in origin and does not appear to be due to accommodation.

  9. Plasma Mass Filters For Nuclear Waste Reprocessing

    Energy Technology Data Exchange (ETDEWEB)

    Fetterman, Abraham J. [Princeton Plasma Physics Lab. (PPPL), Princeton, NJ (United States); Fisch, Nathaniel J. [Princeton Plasma Physics Lab. (PPPL), Princeton, NJ (United States)

    2011-05-01

    Practical disposal of nuclear waste requires high-throughput separation techniques. The most dangerous part of nuclear waste is the fission product, which contains the most active and mobile radioisotopes and produces most of the heat. We suggest that the fission products could be separated as a group from nuclear waste using plasma mass filters. Plasmabased processes are well suited to separating nuclear waste, because mass rather than chemical properties are used for separation. A single plasma stage can replace several stages of chemical separation, producing separate streams of bulk elements, fission products, and actinoids. The plasma mass filters may have lower cost and produce less auxiliary waste than chemical processing plants. Three rotating plasma configurations are considered that act as mass filters: the plasma centrifuge, the Ohkawa filter, and the asymmetric centrifugal trap.

  10. Plasma Mass Filters For Nuclear Waste Reprocessing

    Energy Technology Data Exchange (ETDEWEB)

    Abraham J. Fetterman and Nathaniel J. Fisch

    2011-05-26

    Practical disposal of nuclear waste requires high-throughput separation techniques. The most dangerous part of nuclear waste is the fission product, which contains the most active and mobile radioisotopes and produces most of the heat. We suggest that the fission products could be separated as a group from nuclear waste using plasma mass filters. Plasmabased processes are well suited to separating nuclear waste, because mass rather than chemical properties are used for separation. A single plasma stage can replace several stages of chemical separation, producing separate streams of bulk elements, fission products, and actinoids. The plasma mass filters may have lower cost and produce less auxiliary waste than chemical processing plants. Three rotating plasma configurations are considered that act as mass filters: the plasma centrifuge, the Ohkawa filter, and the asymmetric centrifugal trap.

  11. Iso-geometric shape optimization of magnetic density separators

    OpenAIRE

    2014-01-01

    PurposeThe waste recycling industry increasingly relies on magnetic density separators. These devices generate an upward magnetic force in ferro-fluids allowing to separate the immersed particles according to their mass density. Recently, a new separator design has been proposed that significantly reduces the required amount of permanent magnet material. The purpose of this paper is to alleviate the undesired end-effects in this design by altering the shape of the ferromagnetic covers of the ...

  12. Quintessential Scale Dependence from Separate Universe Simulations

    CERN Document Server

    Chiang, Chi-Ting; Hu, Wayne; LoVerde, Marilena

    2016-01-01

    By absorbing fluctuations into a local background, separate universe simulations provide a powerful technique to characterize the response of small-scale observables to the long-wavelength density fluctuations, for example those of the power spectrum and halo mass function which lead to the squeezed-limit $n$-point function and halo bias, respectively. Using quintessence dark energy as the paradigmatic example, we extend these simulation techniques to cases where non-gravitational forces in other sectors establish a Jeans scale across which the growth of density fluctuations becomes scale dependent. By characterizing the separate universes with matching background expansion histories, we show that the power spectrum and mass function responses depend on whether the long-wavelength mode is above or below the Jeans scale. Correspondingly, the squeezed bispectrum and halo bias also become scale dependent. Models of bias that are effectively local in the density field at a single epoch, initial or observed, canno...

  13. Simultaneous determination of 11 trace elements in coal by inductively coupled plasma-optical emission spectrometry%ICP-OES法同时测定煤中11种微量元素

    Institute of Scientific and Technical Information of China (English)

    吕鑫磊

    2015-01-01

    To quickly determine microelements of coal in batch,the coal sample was ashed first at high temperature,then the product was dissolved by the mixture of HCl,HF and HClO4 ,the third step was to extract the microelements with HCl. The microelements which were Ga,Th,V,P,Cu,Co,Ni,Zn,Pb,Cr,Cd were determined with ICP-OES (Inductively Coupled Plasma-Optical Emission Spectrometry). With reasonable sample dissolution methods,radio-frequency power,analytical spectral line and experimental data,the influence of spec-tral interference on determination was eliminated by off-peak background deduction method, meanwhile, the 11 kinds of microelements could be determined by ICP-OES at the same time. The detection limits for the elements was 0. 03~1. 17 μg/g. The method was applied to the determination of 11 microelements in Soil National Standard Reference Materials and the results were in agreement with certified val-ues with precision of 0. 32% ~3. 19% RSD (n=11).%为实现煤中多种微量元素的批量快速测定,煤样经高温灰化、盐酸-氢氟酸-高氯酸三元体系溶解、盐酸提取后,使用电感耦合等离子体发射光谱( ICP-OES )同时测定煤中镓钍钒磷铜钴镍锌铅铬镉11种微量元素. 在对样品分解方法、射频功率、分析谱线和积分点数合理选择的基础上,通过离峰扣背景法消除了各种光谱干扰对测定的影响,建立了采用ICP-OES同时测定煤中镓钍钒磷铜钴镍锌铅铬镉 11 种微量元素的实验方法. 方法检出限为 0. 03 ~1. 17 μg/g,方法精密度( n=11 ) 0. 32% ~3. 19%,土壤国家标准物质的分析测定值与标准值吻合较好. 与传统化学方法相比,该方法快速准确,提高了分析效率,满足煤质分析的一般要求.

  14. Abdominal mass

    Science.gov (United States)

    Mass in the abdomen ... care provider make a diagnosis. For example, the abdomen can be divided into four areas: Right-upper ... pain or masses include: Epigastric -- center of the abdomen just below the rib cage Periumbilical -- area around ...

  15. Eddy current separation apparatus, separation module, separation method and method for adjusting an eddy current separation apparatus

    NARCIS (Netherlands)

    Rem, P.C.; Bakker, M.C.M.; Berkhout, S.P.M.; Rahman, M.A.

    2012-01-01

    Eddy current separation apparatus (1) for separating particles (20) from a particle stream (w), wherein the apparatus (1) comprises a separator drum (4) adapted to create a first particle fraction (21) and a second particle fraction (23), a feeding device (2) upstream of the separator drum (4) for s

  16. SEPARATION OF PLUTONIUM

    Science.gov (United States)

    Maddock, A.G.; Smith, F.

    1959-08-25

    A method is described for separating plutonium from uranium and fission products by treating a nitrate solution of fission products, uranium, and hexavalent plutonium with a relatively water-insoluble fluoride to adsorb fission products on the fluoride, treating the residual solution with a reducing agent for plutonium to reduce its valence to four and less, treating the reduced plutonium solution with a relatively insoluble fluoride to adsorb the plutonium on the fluoride, removing the solution, and subsequently treating the fluoride with its adsorbed plutonium with a concentrated aqueous solution of at least one of a group consisting of aluminum nitrate, ferric nitrate, and manganous nitrate to remove the plutonium from the fluoride.

  17. POLONIUM SEPARATION PROCESS

    Science.gov (United States)

    Karraker, D.G.

    1959-07-14

    A liquid-liquid extraction process is presented for the recovery of polonium from lead and bismuth. According to the invention an acidic aqueous chloride phase containing the polonium, lead, and bismuth values is contacted with a tributyl phosphate ether phase. The polonium preferentially enters the organic phase which is then separated and washed with an aqueous hydrochloric solution to remove any lead or bismuth which may also have been extracted. The now highly purified polonium in the organic phase may be transferred to an aqueous solution by extraction with aqueous nitric acid.

  18. PLUTONIUM SEPARATION METHOD

    Science.gov (United States)

    Beaufait, L.J. Jr.; Stevenson, F.R.; Rollefson, G.K.

    1958-11-18

    The recovery of plutonium ions from neutron irradiated uranium can be accomplished by bufferlng an aqueous solutlon of the irradiated materials containing tetravalent plutonium to a pH of 4 to 7, adding sufficient acetate to the solution to complex the uranyl present, adding ferric nitrate to form a colloid of ferric hydroxide, plutonlum, and associated fission products, removing and dissolving the colloid in aqueous nitric acid, oxldizlng the plutonium to the hexavalent state by adding permanganate or dichromate, treating the resultant solution with ferric nitrate to form a colloid of ferric hydroxide and associated fission products, and separating the colloid from the plutonlum left in solution.

  19. Hydrogen Exchange Mass Spectrometry.

    Science.gov (United States)

    Mayne, Leland

    2016-01-01

    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.

  20. Printed Spacecraft Separation System

    Energy Technology Data Exchange (ETDEWEB)

    Holmans, Walter [Planetary Systems Corporation, Silver Springs, MD (United States); Dehoff, Ryan [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

    2016-10-01

    In this project Planetary Systems Corporation proposed utilizing additive manufacturing (3D printing) to manufacture a titanium spacecraft separation system for commercial and US government customers to realize a 90% reduction in the cost and energy. These savings were demonstrated via “printing-in” many of the parts and sub-assemblies into one part, thus greatly reducing the labor associated with design, procurement, assembly and calibration of mechanisms. Planetary Systems Corporation redesigned several of the components of the separation system based on additive manufacturing principles including geometric flexibility and the ability to fabricate complex designs, ability to combine multiple parts of an assembly into a single component, and the ability to optimize design for specific mechanical property targets. Shock absorption was specifically targeted and requirements were established to attenuate damage to the Lightband system from shock of initiation. Planetary Systems Corporation redesigned components based on these requirements and sent the designs to Oak Ridge National Laboratory to be printed. ORNL printed the parts using the Arcam electron beam melting technology based on the desire for the parts to be fabricated from Ti-6Al-4V based on the weight and mechanical performance of the material. A second set of components was fabricated from stainless steel material on the Renishaw laser powder bed technology due to the improved geometric accuracy, surface finish, and wear resistance of the material. Planetary Systems Corporation evaluated these components and determined that 3D printing is potentially a viable method for achieving significant cost and savings metrics.

  1. Virus separation using membranes.

    Science.gov (United States)

    Grein, Tanja A; Michalsky, Ronald; Czermak, Peter

    2014-01-01

    Industrial manufacturing of cell culture-derived viruses or virus-like particles for gene therapy or vaccine production are complex multistep processes. In addition to the bioreactor, such processes require a multitude of downstream unit operations for product separation, concentration, or purification. Similarly, before a biopharmaceutical product can enter the market, removal or inactivation of potential viral contamination has to be demonstrated. Given the complexity of biological solutions and the high standards on composition and purity of biopharmaceuticals, downstream processing is the bottleneck in many biotechnological production trains. Membrane-based filtration can be an economically attractive and efficient technology for virus separation. Viral clearance, for instance, of up to seven orders of magnitude has been reported for state of the art polymeric membranes under best conditions.This chapter summarizes the fundamentals of virus ultrafiltration, diafiltration, or purification with adsorptive membranes. In lieu of an impractical universally applicable protocol for virus filtration, application of these principles is demonstrated with two examples. The chapter provides detailed methods for production, concentration, purification, and removal of a rod-shaped baculovirus (Autographa californica M nucleopolyhedrovirus, about 40 × 300 nm in size, a potential vector for gene therapy, and an industrially important protein expression system) or a spherical parvovirus (minute virus of mice, 22-26 nm in size, a model virus for virus clearance validation studies).

  2. Neutrino Masses

    CERN Document Server

    Weinheimer, Christian

    2013-01-01

    The various experiments on neutrino oscillation evidenced that neutrinos have indeed non-zero masses but cannot tell us the absolute neutrino mass scale. This scale of neutrino masses is very important for understanding the evolution and the structure formation of the universe as well as for nuclear and particle physics beyond the present Standard Model. Complementary to deducing constraints on the sum of all neutrino masses from cosmological observations two different methods to determine the neutrino mass scale in the laboratory are pursued: the search for neutrinoless double $\\beta$-decay and the direct neutrino mass search by investigating single $\\beta$-decays or electron captures. The former method is not only sensitive to neutrino masses but also probes the Majorana character of neutrinos and thus lepton number violation with high sensitivity. Currently quite a few experiments with different techniques are being constructed, commissioned or are even running, which aim for a sensitivity on the neutrino ...

  3. The Use of Gas Chromatography and Mass Spectrometry to Introduce General Chemistry Students to Percent Mass and Atomic Mass Calculations

    Science.gov (United States)

    Pfennig, Brian W.; Schaefer, Amy K.

    2011-01-01

    A general chemistry laboratory experiment is described that introduces students to instrumental analysis using gas chromatography-mass spectrometry (GC-MS), while simultaneously reinforcing the concepts of mass percent and the calculation of atomic mass. Working in small groups, students use the GC to separate and quantify the percent composition…

  4. The Use of Gas Chromatography and Mass Spectrometry to Introduce General Chemistry Students to Percent Mass and Atomic Mass Calculations

    Science.gov (United States)

    Pfennig, Brian W.; Schaefer, Amy K.

    2011-01-01

    A general chemistry laboratory experiment is described that introduces students to instrumental analysis using gas chromatography-mass spectrometry (GC-MS), while simultaneously reinforcing the concepts of mass percent and the calculation of atomic mass. Working in small groups, students use the GC to separate and quantify the percent composition…

  5. Plasma separation: physical separation at the molecular level

    Science.gov (United States)

    Gueroult, Renaud; Rax, Jean-Marcel; Fisch, Nathaniel J.

    2016-09-01

    Separation techniques are usually divided in two categories depending on the nature of the discriminating property: chemical or physical. Further to this difference, physical and chemical techniques differ in that chemical separation typically occurs at the molecular level, while physical separation techniques commonly operate at the macroscopic scale. Separation based on physical properties can in principle be realized at the molecular or even atomic scale by ionizing the mixture. This is in essence plasma based separation. Due to this fundamental difference, plasma based separation stands out from other separation techniques, and features unique properties. In particular, plasma separation allows separating different elements or chemical compounds based on physical properties. This could prove extremely valuable to separate macroscopically homogeneous mixtures made of substances of similar chemical formulation. Yet, the realization of plasma separation techniques' full potential requires identifying and controlling basic mechanisms in complex plasmas which exhibit suitable separation properties. In this paper, we uncover the potential of plasma separation for various applications, and identify the key physics mechanisms upon which hinges the development of these techniques.

  6. Particle separator scroll vanes

    Energy Technology Data Exchange (ETDEWEB)

    Lastrina, F. A.; Mayer, J. C.; Pommer, L. M.

    1985-07-09

    An inlet particle separator for a gas turbine engine is provided with unique vanes distributed around an entrance to a particle collection chamber. The vanes are uniquely constructed to direct extraneous particles that enter the engine into the collection chamber and prevent the particles from rebounding back into the engine's air flow stream. The vanes are provided with several features to accomplish this function, including upstream faces that are sharply angled towards air flow stream direction to cause particles to bounce towards the collection chamber. In addition, throat regions between the vanes cause a localized air flow acceleration and a focusing of the particles that aid in directing the particles in a proper direction.

  7. Nebulized therapy. SEPAR year.

    Science.gov (United States)

    Olveira, Casilda; Muñoz, Ana; Domenech, Adolfo

    2014-12-01

    Inhaled drugs are deposited directly in the respiratory tract. They therefore achieve higher concentrations with faster onset of action and fewer side effects than when used systemically. Nebulized drugs are mainly recommended for patients that require high doses of bronchodilators, when they need to inhale drugs that only exist in this form (antibiotics or dornase alfa) or when they are unable to use other inhalation devices. Technological development in recent years has led to new devices that optimize pulmonary deposits and reduce the time needed for treatment. In this review we focus solely on drugs currently used, or under investigation, for nebulization in adult patients; basically bronchodilators, inhaled steroids, antibiotics, antifungals, mucolytics and others such as anticoagulants, prostanoids and lidocaine. Copyright © 2014 SEPAR. Published by Elsevier Espana. All rights reserved.

  8. Block copolymer battery separator

    Energy Technology Data Exchange (ETDEWEB)

    Wong, David; Balsara, Nitash Pervez

    2016-04-26

    The invention herein described is the use of a block copolymer/homopolymer blend for creating nanoporous materials for transport applications. Specifically, this is demonstrated by using the block copolymer poly(styrene-block-ethylene-block-styrene) (SES) and blending it with homopolymer polystyrene (PS). After blending the polymers, a film is cast, and the film is submerged in tetrahydrofuran, which removes the PS. This creates a nanoporous polymer film, whereby the holes are lined with PS. Control of morphology of the system is achieved by manipulating the amount of PS added and the relative size of the PS added. The porous nature of these films was demonstrated by measuring the ionic conductivity in a traditional battery electrolyte, 1M LiPF.sub.6 in EC/DEC (1:1 v/v) using AC impedance spectroscopy and comparing these results to commercially available battery separators.

  9. Block copolymer battery separator

    Science.gov (United States)

    Wong, David; Balsara, Nitash Pervez

    2016-04-26

    The invention herein described is the use of a block copolymer/homopolymer blend for creating nanoporous materials for transport applications. Specifically, this is demonstrated by using the block copolymer poly(styrene-block-ethylene-block-styrene) (SES) and blending it with homopolymer polystyrene (PS). After blending the polymers, a film is cast, and the film is submerged in tetrahydrofuran, which removes the PS. This creates a nanoporous polymer film, whereby the holes are lined with PS. Control of morphology of the system is achieved by manipulating the amount of PS added and the relative size of the PS added. The porous nature of these films was demonstrated by measuring the ionic conductivity in a traditional battery electrolyte, 1M LiPF.sub.6 in EC/DEC (1:1 v/v) using AC impedance spectroscopy and comparing these results to commercially available battery separators.

  10. Device for separation of vortex gas-dynamic energy

    Science.gov (United States)

    Leontiev, A. I.; Burtsev, S. A.

    2015-10-01

    A device for separation of vortex gas-dynamic energy, which combines the mechanism of separation of vortex energy used in the Ranque-Hilsch tubes and the mechanism of separation of gas-dynamic energy, is proposed for supersonic flows. A method of calculation of this device is developed. A comparison is made that showed that, when working with natural gas, the cooling depth of half of the mass flow rate proves to be 1.3 times higher than that for the vortex tube and three times higher than that for the device for separation of the gas-dynamic energy.

  11. Gravity separation for oil wastewater treatment

    OpenAIRE

    Golomeova, Mirjana; Zendelska, Afrodita; Krstev, Boris; Krstev, Aleksandar

    2010-01-01

    In this paper, the applications of gravity separation for oil wastewater treatment are presented. Described is operation on conventional gravity separation and parallel plate separation. Key words: gravity separation, oil, conventional gravity separation, parallel plate separation.

  12. Gravity separation for oil wastewater treatment

    OpenAIRE

    Golomeova, Mirjana; Zendelska, Afrodita; Krstev, Boris; Krstev, Aleksandar

    2010-01-01

    In this paper, the applications of gravity separation for oil wastewater treatment are presented. Described is operation on conventional gravity separation and parallel plate separation. Key words: gravity separation, oil, conventional gravity separation, parallel plate separation.

  13. Separation of polychlorinated dibenzo-p-dioxins/furans, non-ortho/mono/di/tri/tetra-ortho-polychlorinated biphenyls, and polybrominated diphenyl ethers groups of compounds prior to their determination with large volume injection gas chromatography-Quadrupole ion storage tandem mass spectrometry.

    Science.gov (United States)

    Roszko, Marek; Szymczyk, Krystyna; Jędrzejczak, Renata

    2013-10-17

    Polychlorinated dibenzo-p-dioxins/furans (PCDD/Fs), polychlorinated biphenyls (PCBs) and polybrominated diphenyl ethers (PBDEs) are important environmental contaminants. Their maximum legally allowable levels in food and environment are in the low pg g(-1) range. Therefore some highly selective and sensitive analytical methods must be used to determine them. Prior to final determination by GC/MS the cleaned-up samples have to be split into some fractions in view of large differences in concentrations of various analytes and existence of numerous chromatographic co-elutions (which in any case cannot be fully avoided). The aim of this study was to: (i) develop a robust, time-saving analytical method to isolate, clean-up and fractionate PCBs, PBDEs and PCDD/Fs prior to their determination with gas chromatography/ion trap mass spectrometry; (ii) assess method performance using laboratory validation data and some certified reference materials; (iii) use the developed method to assess PCB/PBDE/PCDD/F levels in samples of commercially available food. A combination of alumina, florisil, modified silica gel and two carbon columns were used for sample cleanup and fractionation. Separate fractions containing dioxins/furans, PBDE, non-ortho, mono-ortho and di-/tri-/tetra-ortho PCBs were obtained. The method statistical parameters were compatible with 1883/2006 EC Regulation (80-120%, RSD below 15%). The method performance was successfully used to evaluation of some real life food samples. Copyright © 2013 Elsevier B.V. All rights reserved.

  14. MASS SPECTROMETER

    Science.gov (United States)

    White, F.A.

    1960-08-23

    A mass spectrometer is designed with a first adjustable magnetic field for resolving an ion beam into beams of selected masses, a second adjustable magnetic field for further resolving the ion beam from the first field into beams of selected masses, a thin foil disposed in the path of the beam between the first and second magnets to dissociate molecular ions incident thereon, an electrostatic field for further resolving the ion beam from the second field into beams of selected masses, and a detector disposed adjacent to the electrostatic field to receive the ion beam.

  15. Dynamical Self-mass for Massive Quarks

    CERN Document Server

    Huang, Z; Huang, Zheng

    1992-01-01

    We examine dynamical mass generation in QCD with large current mass quarks. A renormalization group analysis is performed to separate fermion self-mass into a dynamical and a kinematical part. It is shown that the energy scale og the Schwinger-Dyson (SD) equation and the effective gauge coupling are fixed by the current mass. The dynamical self-mass satisfies a homogeneous SD equation which has a trivial solution when the current mass exceeds a critical value. We therefore suggest that the quark condensate, as the function of the current mass, observes a local minimum around 2.7\\Lambda_(QCD).

  16. Selectivity in capillary electrokinetic separations

    NARCIS (Netherlands)

    de Zeeuw, R.A; de Jong, G.J.; Ensing, K

    1999-01-01

    This review gives a survey of selectivity modes in capillary electrophoresis separations in pharmaceutical analysis and bioanalysis. Despite the high efficiencies of these separation techniques, good selectivity is required to allow quantitation or identification of a Chemistry and Toxicology, parti

  17. Physical Separation in the Workplace

    DEFF Research Database (Denmark)

    Stea, Diego; Foss, Nicolai Juul; Holdt Christensen, Peter

    2015-01-01

    Physical separation is pervasive in organizations, and has powerful effects on employee motivation and organizational behaviors. However, research shows that workplace separation is characterized by a variety of tradeoffs, tensions, and challenges that lead to both positive and negative outcomes...

  18. Understanding the effects of potassium ferricyanide on lead hydride formation in tetrahydroborate system and its application for determination of lead in milk using hydride generation inductively coupled plasma optical emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Deng, Biyang, E-mail: dengby16@163.com; Xu, Xiangshu; Xiao, Yan; Zhu, Pingchuan; Wang, Yingzi

    2015-01-01

    Highlights: • Proposed a novel explanation for plumbane generation. • Expounded the role of K{sub 3}Fe(CN){sub 6} in plumbane generation. • Clarified the controversial aspects in the mechanism of K{sub 3}Fe(CN){sub 6} enhancement. • Used X-ray diffractometry to analyze the intermediates. • Developed a method to analyze lead in milk using K{sub 3}Fe(CN){sub 6} and K{sub 4}Fe(CN){sub 6} as new additives. - Absract: To understand the formation of plumbane in the Pb{sup II}-NaBH{sub 4}-K{sub 3}Fe(CN){sub 6} system, the intermediate products produced in the reaction of lead(II) and NaBH{sub 4} in the presence of K{sub 3}Fe(CN){sub 6} were studied. The produced plumbane and elemental lead were measured through continuous flow hydride generation (HG)-inductively coupled plasma optical emission spectrometry (ICP OES) and X-ray diffraction spectrometry techniques, respectively. Based on the experimental results, the explanations can be depicted in the following steps: (1) plumbane and black lead sediment (black Pb) are formed in the reaction of lead(II) and NaBH{sub 4}; (2) the black Pb is oxidized by K{sub 3}Fe(CN){sub 6} to form Pb{sub 2}[Fe(CN){sub 6}], which further reacts with NaBH{sub 4} to form more plumbane and black Pb; and (3) another round starts in which the produced black Pb from the step 2 is then oxidized continuously by K{sub 3}Fe(CN){sub 6} to form more Pb{sub 2}[Fe(CN){sub 6}] complex, which would produce more plumbane. In short, the black Pb and Pb{sub 2}[Fe(CN){sub 6}] complex are the key intermediate products for the formation of plumbane in the Pb{sup II}-NaBH{sub 4}-K{sub 3}Fe(CN){sub 6} system. Based on the enhancement effect of potassium ferricyanide and potassium ferrocyanide, a method was developed to analyze lead in milk with HG-ICP OES technique. The detection limit of the method was observed as 0.081 μg L{sup −1}. The linearity range of lead was found between 0.3 and 50,000 μg L{sup −1} with correlation coefficient of 0

  19. Determine separations process strategy decision

    Energy Technology Data Exchange (ETDEWEB)

    Slaathaug, E.J.

    1996-01-01

    This study provides a summary level comparative analysis of selected, top-level, waste treatment strategies. These strategies include No Separations, Separations (high-level/low-level separations), and Deferred Separations of the tank waste. These three strategies encompass the full range of viable processing alternatives based upon full retrieval of the tank wastes. The assumption of full retrieval of the tank wastes is a predecessor decision and will not be revisited in this study.

  20. High Mass Accuracy and High Mass Resolving Power FT-ICR Secondary Ion Mass Spectrometry for Biological Tissue Imaging

    CERN Document Server

    Smith, Donald F; Leach, Franklin E; Robinson, Errol W; Paša-Tolić, Ljiljana; Heeren, Ron M A

    2013-01-01

    Biological tissue imaging by secondary ion mass spectrometry has seen rapid development with the commercial availability of polyatomic primary ion sources. Endogenous lipids and other small bio-molecules can now be routinely mapped on the sub-micrometer scale. Such experiments are typically performed on time-of-flight mass spectrometers for high sensitivity and high repetition rate imaging. However, such mass analyzers lack the mass resolving power to ensure separation of isobaric ions and the mass accuracy for elemental formula assignment based on exact mass measurement. We have recently reported a secondary ion mass spectrometer with the combination of a C60 primary ion gun with a Fourier transform ion cyclotron resonance mass spectrometer (FT-ICR MS) for high mass resolving power, high mass measurement accuracy and tandem mass spectrometry capabilities. In this work, high specificity and high sensitivity secondary ion FT-ICR MS was applied to chemical imaging of biological tissue. An entire rat brain tissu...

  1. Composite separators and redox flow batteries based on porous separators

    Science.gov (United States)

    Li, Bin; Wei, Xiaoliang; Luo, Qingtao; Nie, Zimin; Wang, Wei; Sprenkle, Vincent L.

    2016-01-12

    Composite separators having a porous structure and including acid-stable, hydrophilic, inorganic particles enmeshed in a substantially fully fluorinated polyolefin matrix can be utilized in a number of applications. The inorganic particles can provide hydrophilic characteristics. The pores of the separator result in good selectivity and electrical conductivity. The fluorinated polymeric backbone can result in high chemical stability. Accordingly, one application of the composite separators is in redox flow batteries as low cost membranes. In such applications, the composite separator can also enable additional property-enhancing features compared to ion-exchange membranes. For example, simple capacity control can be achieved through hydraulic pressure by balancing the volumes of electrolyte on each side of the separator. While a porous separator can also allow for volume and pressure regulation, in RFBs that utilize corrosive and/or oxidizing compounds, the composite separators described herein are preferable for their robustness in the presence of such compounds.

  2. Separating Underdetermined Convolutive Speech Mixtures

    DEFF Research Database (Denmark)

    Pedersen, Michael Syskind; Wang, DeLiang; Larsen, Jan

    2006-01-01

    a method for underdetermined blind source separation of convolutive mixtures. The proposed framework is applicable for separation of instantaneous as well as convolutive speech mixtures. It is possible to iteratively extract each speech signal from the mixture by combining blind source separation...

  3. General Motors sidestream separator

    Energy Technology Data Exchange (ETDEWEB)

    Tessier, R.J.

    1981-01-01

    On February 15, 1980, the United States Environmental Protection Agency, acting pursuant to Paragraph 113(D) (4) of the Clean Air Act, issued to General Motors an innovative technology order covering fifteen coal-fired spreader-stoker boilers located at six General Motors plants in Ohio. The purpose and effect of this order was to permit General Motors time to develop a new, innovative technique for controlling particulate emissions from the specified boilers before compliance with the federally approved Ohio particulate control regulation was required. This new technology was christened, The Sidestream Separator, by General Motors. It provides a highly cost effective means of reducing particulate emissions below levels currently obtainable with conventionally used high efficiency mechanical collectors. These improvements could prove to be of substantial benefit to many industrial facilities with spreader-stoker coal-fired boilers that cannot be brought into compliance with applicble air pollution regulations except by application of far more expensive and unwieldly electrostatic precipitators (ESP's) or fabric filters (baghouses).

  4. PARAFFIN SEPARATION VACUUM DISTILLATION

    Directory of Open Access Journals (Sweden)

    Zaid A. Abdulrahman

    2013-05-01

    Full Text Available Simulated column performance curves were constructed for existing paraffin separation vacuum distillation column in LAB plant (Arab Detergent Company/Baiji-Iraq. The variables considered in this study are the thermodynamic model option, top vacuum pressure, top and bottom temperatures, feed temperature, feed composition & reflux ratio. Also simulated columns profiles for the temperature, vapor & liquid flow rates composition were constructed. Four different thermodynamic model options (SRK, TSRK, PR, and ESSO were used, affecting the results within 1-25% variation for the most cases.The simulated results show that about 2% to 8 % of paraffin (C10, C11, C12, & C13 present at the bottom stream which may cause a problem in the LAB plant. The major variations were noticed for the top temperature & the  paraffin weight fractions at bottom section with top vacuum pressure. The bottom temperature above 240 oC is not recommended because the total bottom flow rate decreases sharply, where as  the weight fraction of paraffins decrease slightly. The study gives evidence about a successful simulation with CHEMCAD

  5. Separation and identification of phospholipid peroxidation products.

    Science.gov (United States)

    Milne, G L; Porter, N A

    2001-11-01

    The molecular species in mixtures of phospholipid hydroperoxides are difficult to separate and identify by typical chromatographic and mass spectrometric techniques. As reported by Havrilla and coworkers, silver ion coordination ion-spray mass spectrometry (CIS-MS) has proven to be a powerful technique for the identification of mixtures of hydroperoxides. This ionization technique, which involves the formation of Ag+ adducts of the hydroperoxides, provides valuable, unambiguous structural information about the hydroperoxides. Herein, we report a method for the analysis and identification of phospholipid hydroperoxides using CIS-MS. We also report an improved method for the separation of phospholipid hydroperoxides by reversed-phase high-performance liquid chromatography (RP-HPLC), which, for the first time, separates some of the hydroperoxide isomers. CIS-MS can be coupled with this RP-HPLC method by the addition of AgBF4 to the mobile phase or to the HPLC effluent postcolumn, thus allowing powerful HPLC-MS techniques to be used to identify complex mixtures of phospholipid hydroperoxides.

  6. Iso-geometric shape optimization of magnetic density separators

    DEFF Research Database (Denmark)

    Dang Manh, Nguyen; Evgrafov, Anton; Gravesen, Jens

    2014-01-01

    Purpose The waste recycling industry increasingly relies on magnetic density separators. These devices generate an upward magnetic force in ferro-fluids allowing to separate the immersed particles according to their mass density. Recently, a new separator design has been proposed that significantly...... is obtained at the cost of a pole cover shape that differs per pole. This limitation has negligible impact on the manufacturing of the separator. The new pole cover shapes therefore lead to improved performance of the density separation. Practical implications Due to the larger uniformity the generated field......, these shapes should enable larger amounts of waste to be processed than the previous design. Originality/value This paper treats the shapes optimization of magnetic density separators systematically and presents new shapes for the ferromagnetic poles covers....

  7. TITAN's multiple-reflection time-of-flight isobar separator

    Science.gov (United States)

    Reiter, Moritz Pascal; Titan Collaboration

    2016-09-01

    At the ISAC facility located at TRIUMF exotic nuclei are produced by the ISOL method. Exotic nuclei are separated by a magnetic separator and transported to TRIUMF's Ion Trap for Atomic and Nuclear science (TITAN). TITAN is a system of multiple ion traps for high precision mass measurements and in-trap decay spectroscopy. Although ISAC can deliver some of the highest yields for even many of the most exotic species many measurements suffer from a strong isobaric background. This background often prevents the high precision measurement of the species of interest. To overcome this limitation an additional isobar separator based on the Multiple-Reflection Time-Of-Flight Mass Spectrometry (MR-TOF-MS) technique has been developed for TITAN. Mass selection is achieved using dynamic re-trapping of the species of interest after a time-of-flight analysis in an electrostatic isochronous reflector system. Additionally the MR-TOF-MS will, on its own, enable mass measurements of very short-lived nuclides that are weakly produced. Being able to measure all isobars of a given mass number at the same time the MR-TOF-MS can be used for beam diagnostics or determination of beam compositions. Results from the offline commissioning showing mass resolving power and separation power will be presented.

  8. Archimedes Mass Filter Vaporizer

    Science.gov (United States)

    Putvinski, S.; Agnew, A. F.; Cluggish, B. P.; Ohkawa, T.; Sevier, L.; Umstadter, K. R.; Dresvin, S. V.; Kuteev, B. V.; Feygenson, O. N.; Ivanov, D. V.; Zverev, S. G.; Miroshnikov, I. V.; Egorov, S. M.; Kiesewetter, D. V.; Maliugin, V. I.

    2001-10-01

    Archimedes Technology Group, Inc., is developing a plasma mass separator called the Archimedes Filter that separates waste oxide mixtures ion by ion into two mass groups: light and heavy. Since high-level waste at Hanford has 99.9its radioactivity associated with heavy elements, the Archimedes Filter can effectively decontaminate over three-quarters of that waste. The Filter process involves some preprocessing followed by volatilization and separation by the magnetic and electric fields of the main plasma. This presentation describes the approach to volatilization of the waste oxy-hydroxide mixture by means of a very high heat flux (q > 10 MW/m2). Such a high heat flux is required to ensure congruent evaporation of the complex oxy-hydroxide mixture and is achieved by injection of small droplets of molten waste into an inductively coupled plasma (ICP) torch. This presentation further addresses different issues related to evaporation of the waste including modeling of droplet evaporation, estimates of parameters of plasma torch, and 2D modeling of the plasma. The experimental test bed for oxide vaporization and results of the initial experiments on oxide evaporation in 60 kW ICP torch will also be described.

  9. Activated Carbon Composites for Air Separation

    Energy Technology Data Exchange (ETDEWEB)

    Contescu, Cristian I [ORNL; Baker, Frederick S [ORNL; Tsouris, Costas [ORNL; McFarlane, Joanna [ORNL

    2008-03-01

    In continuation of the development of composite materials for air separation based on molecular sieving properties and magnetic fields effects, several molecular sieve materials were tested in a flow system, and the effects of temperature, flow conditions, and magnetic fields were investigated. New carbon materials adsorbents, with and without pre-loaded super-paramagnetic nanoparticles of Fe3O4 were synthesized; all materials were packed in chromatographic type columns which were placed between the poles of a high intensity, water-cooled, magnet (1.5 Tesla). In order to verify the existence of magnetodesorption effect, separation tests were conducted by injecting controlled volumes of air in a flow of inert gas, while the magnetic field was switched on and off. Gas composition downstream the column was analyzed by gas chromatography and by mass spectrometry. Under the conditions employed, the tests confirmed that N2 - O2 separation occurred at various degrees, depending on material's intrinsic properties, temperature and flow rate. The effect of magnetic fields, reported previously for static conditions, was not confirmed in the flow system. The best separation was obtained for zeolite 13X at sub-ambient temperatures. Future directions for the project include evaluation of a combined system, comprising carbon and zeolite molecular sieves, and testing the effect of stronger magnetic fields produced by cryogenic magnets.

  10. Selective Ion Transporting Polymerized Ionic Liquid Membrane Separator for Enhancing Cycle Stability and Durability in Secondary Zinc-Air Battery Systems.

    Science.gov (United States)

    Hwang, Ho Jung; Chi, Won Seok; Kwon, Ohchan; Lee, Jin Goo; Kim, Jong Hak; Shul, Yong-Gun

    2016-10-05

    Rechargeable secondary zinc-air batteries with superior cyclic stability were developed using commercial polypropylene (PP) membrane coated with polymerized ionic liquid as separators. The anionic exchange polymer was synthesized copolymerizing 1-[(4-ethenylphenyl)methyl]-3-butylimidazolium hydroxide (EBIH) and butyl methacrylate (BMA) monomers by free radical polymerization for both functionality and structural integrity. The ionic liquid induced copolymer was coated on a commercially available PP membrane (Celguard 5550). The coat allows anionic transfer through the separator and minimizes the migration of zincate ions to the cathode compartment, which reduces electrolyte conductivity and may deteriorate catalytic activity by the formation of zinc oxide on the surface of the catalyst layer. Energy dispersive X-ray spectroscopy (EDS) data revealed the copolymer-coated separator showed less zinc element in the cathode, indicating lower zinc crossover through the membrane. Ion coupled plasma optical emission spectroscopy (ICP-OES) analysis confirmed over 96% of zincate ion crossover was reduced. In our charge/discharge setup, the constructed cell with the ionic liquid induced copolymer casted separator exhibited drastically improved durability as the battery life increased more than 281% compared to the pure commercial PP membrane. Electrochemical impedance spectroscopy (EIS) during the cycle process elucidated the premature failure of cells due to the zinc crossover for the untreated cell and revealed a substantial importance must be placed in zincate control.

  11. 反相超效液相色谱-质谱联用分离分析食用油中的甘油三酯%Separation of Triacylglycerols in Edible Oil by Reversed Phase Ultra Performance Liquid Chromatography-Mass Spectroscopy

    Institute of Scientific and Technical Information of China (English)

    何榕; 山晓琳; 董方圆; 许旭

    2015-01-01

    采用反相超效液相色谱-质谱联用的方法分离分析食用油中的甘油三酯。使用总长40 cm的串联超效C18色谱柱(10 cm+15 cm+15 cm),以乙腈-异丙醇(50:50, V/V)为流动相,流速0.2 mL/min,柱温25℃,在大约74 MPa的高柱压下分离,APCI离子化-质谱检测。食用油以异丙醇溶解后直接进样。实现了对食用油中甘油三酯组分的更精细区分,获得了玉米油、大豆油、花生油、葵花籽油、稻米油、橄榄油和芝麻油等市售食用油中甘油三酯组成的谱图。结果显示,甘油三酯在相同食用油中的组成相似,而在不同食用油中的组成存在差异。采用本方法,通过差异的色谱峰可直接识别出大豆油中掺入的5%猪油。本方法为识别掺假食用油提供了有价值的途径。%A reversed phase ultra performance liquid chromatography-mass spectrometric method was developed for the separation and analysis of triglycerides in edible oils. The samples were separated by using three ultra performance C18 columns in series with a total length of 40 cm (10 cm + 15 cm + 15 cm) at high pressure with acetonitrile-isopropanol (50:50, V/V) as mobile phase at a flow rate of 0. 2 mL/min and at col-umn temperature of 25℃, and detected by APCI ionization-mass spectrometry. The edible oil sample was dis-solved in isopropanol and injected in LC-MS directly. The triglycerides in edible oils were distinguished to their better fine components which included corn oil, peanut oil, sunflower seed oil, rice oil, olive oil, sesa-me oil and soybean oil. The chromatograms of different edible oils showed that the same kind of edible oil was composed of similar triglyceride composition and content, while the different kind of edible oils differed. The experimental result showed that the method could be use for identifying 5% lard adulterated in soybean oil. The method suggests a significant research way for identifying adulteration in edible oil.

  12. Treatise on the measurement of molecular masses with ion mobility spectrometry.

    Science.gov (United States)

    Valentine, Stephen J; Clemmer, David E

    2009-07-15

    The ability to separate isotopes by high-resolution ion mobility spectrometry techniques is considered as a direct means for determining mass at ambient pressures. Calculations of peak shapes from the transport equation show that it should be possible to separate isotopes for low-mass ions (ion mobility analyzers. The mass accuracy associated with this isotopic separation approach based on ion mobility separation is considered. Finally, we predict several isotopes that should be separable.

  13. The new vacuum-mode recoil separator MARA at JYFL

    Science.gov (United States)

    Sarén, J.; Uusitalo, J.; Leino, M.; Greenlees, P. T.; Jakobsson, U.; Jones, P.; Julin, R.; Juutinen, S.; Ketelhut, S.; Nyman, M.; Peura, P.; Rahkila, P.; Scholey, C.; Sorri, J.

    2008-10-01

    A new vacuum-mode recoil separator MARA (Mass Analysing Recoil Apparatus) is under design and construction at the Department of Physics in the University of Jyväskylä. The separator is intended to separate reaction products from the primary beam in mass region below A = 150 . The ion-optical configuration of the separator will be QQQDEDM, where a magnetic quadrupole (Q) triplet is followed by an electrostatic deflector (DE) and a magnetic dipole (DM). The total length of MARA will be less than 7.0 m and the first order resolving power more than 250 for a beam spot size of 2 mm. In this contribution the main properties of MARA are given and results from simulations are shown.

  14. Separators - Technology review: Ceramic based separators for secondary batteries

    Science.gov (United States)

    Nestler, Tina; Schmid, Robert; Münchgesang, Wolfram; Bazhenov, Vasilii; Schilm, Jochen; Leisegang, Tilmann; Meyer, Dirk C.

    2014-06-01

    Besides a continuous increase of the worldwide use of electricity, the electric energy storage technology market is a growing sector. At the latest since the German energy transition ("Energiewende") was announced, technological solutions for the storage of renewable energy have been intensively studied. Storage technologies in various forms are commercially available. A widespread technology is the electrochemical cell. Here the cost per kWh, e. g. determined by energy density, production process and cycle life, is of main interest. Commonly, an electrochemical cell consists of an anode and a cathode that are separated by an ion permeable or ion conductive membrane - the separator - as one of the main components. Many applications use polymeric separators whose pores are filled with liquid electrolyte, providing high power densities. However, problems arise from different failure mechanisms during cell operation, which can affect the integrity and functionality of these separators. In the case of excessive heating or mechanical damage, the polymeric separators become an incalculable security risk. Furthermore, the growth of metallic dendrites between the electrodes leads to unwanted short circuits. In order to minimize these risks, temperature stable and non-flammable ceramic particles can be added, forming so-called composite separators. Full ceramic separators, in turn, are currently commercially used only for high-temperature operation systems, due to their comparably low ion conductivity at room temperature. However, as security and lifetime demands increase, these materials turn into focus also for future room temperature applications. Hence, growing research effort is being spent on the improvement of the ion conductivity of these ceramic solid electrolyte materials, acting as separator and electrolyte at the same time. Starting with a short overview of available separator technologies and the separator market, this review focuses on ceramic-based separators

  15. Mathematical modelling of membrane separation

    DEFF Research Database (Denmark)

    Vinther, Frank

    This thesis concerns mathematical modelling of membrane separation. The thesis consists of introductory theory on membrane separation, equations of motion, and properties of dextran, which will be the solute species throughout the thesis. Furthermore, the thesis consist of three separate mathemat......This thesis concerns mathematical modelling of membrane separation. The thesis consists of introductory theory on membrane separation, equations of motion, and properties of dextran, which will be the solute species throughout the thesis. Furthermore, the thesis consist of three separate....... It is found that the probability of entering the pore is highest when the largest of the radii in the ellipse is equal to half the radius of the pore, in case of molecules with circular radius less than the pore radius. The results are directly related to the macroscopic distribution coefficient...

  16. Capillary Separation: Micellar Electrokinetic Chromatography

    Science.gov (United States)

    Terabe, Shigeru

    2009-07-01

    Micellar electrokinetic chromatography (MEKC), a separation mode of capillary electrophoresis (CE), has enabled the separation of electrically neutral analytes. MEKC can be performed by adding an ionic micelle to the running solution of CE without modifying the instrument. Its separation principle is based on the differential migration of the ionic micelles and the bulk running buffer under electrophoresis conditions and on the interaction between the analyte and the micelle. Hence, MEKC's separation principle is similar to that of chromatography. MEKC is a useful technique particularly for the separation of small molecules, both neutral and charged, and yields high-efficiency separation in a short time with minimum amounts of sample and reagents. To improve the concentration sensitivity of detection, several on-line sample preconcentration techniques such as sweeping have been developed.

  17. Separable programming theory and methods

    CERN Document Server

    Stefanov, Stefan M

    2001-01-01

    In this book, the author considers separable programming and, in particular, one of its important cases - convex separable programming Some general results are presented, techniques of approximating the separable problem by linear programming and dynamic programming are considered Convex separable programs subject to inequality equality constraint(s) and bounds on variables are also studied and iterative algorithms of polynomial complexity are proposed As an application, these algorithms are used in the implementation of stochastic quasigradient methods to some separable stochastic programs Numerical approximation with respect to I1 and I4 norms, as a convex separable nonsmooth unconstrained minimization problem, is considered as well Audience Advanced undergraduate and graduate students, mathematical programming operations research specialists

  18. Separation process using microchannel technology

    Science.gov (United States)

    Tonkovich, Anna Lee; Perry, Steven T.; Arora, Ravi; Qiu, Dongming; Lamont, Michael Jay; Burwell, Deanna; Dritz, Terence Andrew; McDaniel, Jeffrey S.; Rogers, Jr.; William A.; Silva, Laura J.; Weidert, Daniel J.; Simmons, Wayne W.; Chadwell, G. Bradley

    2009-03-24

    The disclosed invention relates to a process and apparatus for separating a first fluid from a fluid mixture comprising the first fluid. The process comprises: (A) flowing the fluid mixture into a microchannel separator in contact with a sorption medium, the fluid mixture being maintained in the microchannel separator until at least part of the first fluid is sorbed by the sorption medium, removing non-sorbed parts of the fluid mixture from the microchannel separator; and (B) desorbing first fluid from the sorption medium and removing desorbed first fluid from the microchannel separator. The process and apparatus are suitable for separating nitrogen or methane from a fluid mixture comprising nitrogen and methane. The process and apparatus may be used for rejecting nitrogen in the upgrading of sub-quality methane.

  19. Wastewater treatment with acoustic separator

    Science.gov (United States)

    Kambayashi, Takuya; Saeki, Tomonori; Buchanan, Ian

    2017-07-01

    Acoustic separation is a filter-free wastewater treatment method based on the forces generated in ultrasonic standing waves. In this report, a batch-system separator based on acoustic separation was demonstrated using a small-scale prototype acoustic separator to remove suspended solids from oil sand process-affected water (OSPW). By applying an acoustic separator to the batch use OSPW treatment, the required settling time, which was the time that the chemical oxygen demand (COD) decreased to the environmental criterion (<200 mg/L), could be shortened from 10 to 1 min. Moreover, for a 10 min settling time, the acoustic separator could reduce the FeCl3 dose as coagulant in OSPW treatment from 500 to 160 mg/L.

  20. Separation of proteins by simulated moving bed chromatography

    OpenAIRE

    Houwing, J.

    2003-01-01

    This thesis describes the use of simulated moving bed (SMB) chromatography for separation of proteins. The underlying aim is the increase of the efficiency of process chromatography in terms of a reduction of the sorbent and buffer consumption in comparison to fixed bed chromatography. Both size exclusion and ion exchange separations of synthetic mixtures of proteins are considered. The main topics covered are the selection of the liquid to sorbent flow rate ratios, mass transfer effects and ...

  1. Mass Spectrometry in Polymer Chemistry

    CERN Document Server

    Barner-Kowollik, Christopher; Falkenhagen, Jana; Weidner, Steffen

    2011-01-01

    Combining an up-to-date insight into mass-spectrometric polymer analysis beyond MALDI with application details of the instrumentation, this is a balanced and thorough presentation of the most important and widely used mass-spectrometric methods.Written by the world's most proficient experts in the field, the book focuses on the latest developments, covering such technologies and applications as ionization protocols, tandem and liquid chromatography mass spectrometry, gas-phase ion-separation techniques and automated data processing. Chapters on sample preparation, polymer degradation and the u

  2. Hereditary separability in Hausdorff continua

    Directory of Open Access Journals (Sweden)

    D. Daniel

    2012-04-01

    Full Text Available We consider those Hausdorff continua S such that each separable subspace of S is hereditarily separable. Due to results of Ostaszewski and Rudin, respectively, all monotonically normal spaces and therefore all continuous Hausdorff images of ordered compacta also have this property. Our study focuses on the structure of such spaces that also possess one of various rim properties, with emphasis given to rim-separability. In so doing we obtain analogues of results of M. Tuncali and I. Loncar, respectively.

  3. Binary Cepheids: Separations and Mass Ratios in 5 Solar Mass Binaries

    Science.gov (United States)

    2013-10-01

    cfa.harvard.edu 2 Department of Astronomy & Astrophysics, Pennsylvania State University, University Park, PA 16802, USA; heb11@psu.edu 3 Space...Telescope Science Institute. STScI is operated by the Association of Universities for Research in Astronomy , Inc., under NASA contract NAS5-26555. 6...spectroscopic binary. We have tested this by comparing two seasons of accurate data from the same group (Moscow Table 2 Cepheids with Resolved Companions

  4. 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

  5. Column-coupling strategies for multidimensional electrophoretic separation techniques.

    Science.gov (United States)

    Kler, Pablo A; Sydes, Daniel; Huhn, Carolin

    2015-01-01

    Multidimensional electrophoretic separations represent one of the most common strategies for dealing with the analysis of complex samples. In recent years we have been witnessing the explosive growth of separation techniques for the analysis of complex samples in applications ranging from life sciences to industry. In this sense, electrophoretic separations offer several strategic advantages such as excellent separation efficiency, different methods with a broad range of separation mechanisms, and low liquid consumption generating less waste effluents and lower costs per analysis, among others. Despite their impressive separation efficiency, multidimensional electrophoretic separations present some drawbacks that have delayed their extensive use: the volumes of the columns, and consequently of the injected sample, are significantly smaller compared to other analytical techniques, thus the coupling interfaces between two separations components must be very efficient in terms of providing geometrical precision with low dead volume. Likewise, very sensitive detection systems are required. Additionally, in electrophoretic separation techniques, the surface properties of the columns play a fundamental role for electroosmosis as well as the unwanted adsorption of proteins or other complex biomolecules. In this sense the requirements for an efficient coupling for electrophoretic separation techniques involve several aspects related to microfluidics and physicochemical interactions of the electrolyte solutions and the solid capillary walls. It is interesting to see how these multidimensional electrophoretic separation techniques have been used jointly with different detection techniques, for intermediate detection as well as for final identification and quantification, particularly important in the case of mass spectrometry. In this work we present a critical review about the different strategies for coupling two or more electrophoretic separation techniques and the

  6. Centrifugal separation for miscible solutions: Fundamentals and applications to separation of molten salt nuclear material

    Science.gov (United States)

    Li, Ning; Camassa, Roberto; Ecke, Robert E.; Venneri, Francesco

    1995-09-01

    We report on the physical separation of dilute solutions using centrifugal techniques. We use numerical simulations of the diffusion and sedimentation dynamics of centrifugation to model the approach to an equilibrium concentration profile. We verify experimentally the equilibrium profiles for aqueous solutions of different salts under rotation at 25000 rpm corresponding to centrifugal accelerations of about 57,000 g and 75,000 g in two different commercial centrifuges. These measurements provide ratios of sedimentation and diffusion coefficients. We show experimental results for the dynamics of separation that confirm the predictions of the theoretical model. We also measure the mass diffusion coefficient for several solutions. Although the relaxation to equilibrium is long, we have determined a method for efficiently extracting enriched components from a ternary mixture based on fast dynamics at early times. These dynamics are modeled in numerical simulations with realistic fluid parameters. Based on these studies we show that a multistage centrifugal separation process could provide efficient physical separation of actinides and fission products from a molten-salt solution in proposed transmutation/energy-production systems. We consider technical issues in the design of such a separation system.

  7. On Poor Separation in Magnetically Driven Shock Tube

    DEFF Research Database (Denmark)

    Chang, C.T.

    1973-01-01

    Observations made at steady-state running conditions in a magnetically driven shock tube, with parallel-plate electrodes, showed that for a given discharge voltage, sufficient separation between the shock and the current-sheet occurred only at relatively high discharge pressures. As a comparison......, poor separations were also noted in conventional diaphragm-type shock tubes running at low initial pressures. It is demonstrated that the observed poor separation can be explained by a mass leakage, instead of through the wall boundary layer, but through the current-sheet itself....

  8. Mass metrology

    CERN Document Server

    Gupta, S V

    2012-01-01

    This book presents the practical aspects of mass measurements. Concepts of gravitational, inertial and conventional mass and details of the variation of acceleration of gravity are described. The Metric Convention and International Prototype Kilogram and BIPM standards are described. The effect of change of gravity on the indication of electronic balances is derived with respect of latitude, altitude and earth topography. The classification of weights by OIML is discussed. Maximum permissible errors in different categories of weights prescribed by national and international organizations are p

  9. Parental separation and pediatric cancer

    DEFF Research Database (Denmark)

    Grant, Sally; Carlsen, Kathrine; Bidstrup, Pernille Envold Hansen

    2012-01-01

    The purpose of this study was to determine the risk for separation (ending cohabitation) of the parents of a child with a diagnosis of cancer.......The purpose of this study was to determine the risk for separation (ending cohabitation) of the parents of a child with a diagnosis of cancer....

  10. Fast Monaural Separation of Speech

    DEFF Research Database (Denmark)

    Pontoppidan, Niels Henrik; Dyrholm, Mads

    2003-01-01

    a Factorial Hidden Markov Model, with non-stationary assumptions on the source autocorrelations modelled through the Factorial Hidden Markov Model, leads to separation in the monaural case. By extending Hansens work we find that Roweis' assumptions are necessary for monaural speech separation. Furthermore we...

  11. Metals Separation by Liquid Extraction.

    Science.gov (United States)

    Malmary, G.; And Others

    1984-01-01

    As part of a project focusing on techniques in industrial chemistry, students carry out experiments on separating copper from cobalt in chloride-containing aqueous solution by liquid extraction with triisoctylamine solvent and search the literature on the separation process of these metals. These experiments and the literature research are…

  12. Vision 2020: 2000 Separations Roadmap

    Energy Technology Data Exchange (ETDEWEB)

    Adler, Stephen [Center for Waster Reduction Technologies; Beaver, Earl [Practical Sustainability; Bryan, Paul [Massachusetts Inst. of Technology (MIT), Cambridge, MA (United States); Robinson, Sharon [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Watson, Jack [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

    2000-01-01

    This report documents the results of four workshops on the technology barriers, research needs, and priorities of the chemical, agricultural, petroleum, and pharmaceutical industries as they relate to separation technologies utilizing adsorbents, crystallization, distillation, extraction, membranes, separative reactors, ion exchange, bioseparations, and dilute solutions.

  13. Electrostatically enhanced core separator system

    Energy Technology Data Exchange (ETDEWEB)

    Easom, B.H.; Smolensky, L.A.; Altman, R.F. [LSR Technologies, Inc., Acton, MA (United States)

    1997-12-31

    The Electrostatically Enhanced Core Separator (EECS) system employs the same design principles as the mechanical Core Separator system plus an electrostatic separation enhancing technique. The EECS system contains a special type of separator, the EECS element, a conventional solids collector and means for flow recirculation. In the EECS system solids separation and collection are accomplished in two different components. The EECS element acts as a separator, not as a collector so particles are not collected on its walls. This eliminates or at least mitigates the problems associated with reentrainment (due to high or low dust resistivity), seepage (due to gas flow below the precipitator plates and over the hoppers), sneakage (due to gas flow both above and below the precipitator plates), and rapping reentrainment. If the EECS separation efficiency is high enough, particles cannot leave the system with the process stream. They recirculate until they are extracted by the collector. As a result, the separation efficiency of the EECS element determines the efficiency of the system, even if the collector efficiency is relatively low. 8 refs., 3 figs.

  14. Relational Parametricity and Separation Logic

    DEFF Research Database (Denmark)

    Birkedal, Lars; Yang, Hongseok

    2008-01-01

    Separation logic is a recent extension of Hoare logic for reasoning about programs with references to shared mutable data structures. In this paper, we provide a new interpretation of the logic for a programming language with higher types. Our interpretation is based on Reynolds's relational...... parametricity, and it provides a formal connection between separation logic and data abstraction. Udgivelsesdato: 2008...

  15. Electrophoresis-mass spectrometry probe

    Science.gov (United States)

    Andresen, Brian D.; Fought, Eric R.

    1987-01-01

    The invention involves a new technique for the separation of complex mixtures of chemicals, which utilizes a unique interface probe for conventional mass spectrometers which allows the electrophoretically separated compounds to be analyzed in real-time by a mass spectrometer. This new chemical analysis interface, which couples electrophoresis with mass spectrometry, allows complex mixtures to be analyzed very rapidly, with much greater specificity, and with greater sensitivity. The interface or probe provides a means whereby large and/or polar molecules in complex mixtures to be completely characterized. The preferred embodiment of the probe utilizes a double capillary tip which allows the probe tip to be continually wetted by the buffer, which provides for increased heat dissipation, and results in a continually operating interface which is more durable and electronically stable than the illustrated single capillary tip probe interface.

  16. Quintessential scale dependence from separate universe simulations

    Science.gov (United States)

    Chiang, Chi-Ting; Li, Yin; Hu, Wayne; LoVerde, Marilena

    2016-12-01

    By absorbing fluctuations into a local background, separate universe simulations provide a powerful technique to characterize the response of small-scale observables to the long-wavelength density fluctuations, for example those of the power spectrum and halo mass function which lead to the squeezed-limit n -point function and halo bias, respectively. Using quintessence dark energy as the paradigmatic example, we extend these simulation techniques to cases where non-gravitational forces in other sectors establish a Jeans scale across which the growth of density fluctuations becomes scale dependent. By characterizing the separate universes with matching background expansion histories, we show that the power spectrum and mass function responses depend on whether the long-wavelength mode is above or below the Jeans scale. Correspondingly, the squeezed bispectrum and halo bias also become scale dependent. Models of bias that are effectively local in the density field at a single epoch, initial or observed, cannot describe this effect which highlights the importance of temporal nonlocality in structure formation. Validated by these quintessence tests, our techniques are applicable to a wide range of models where the complex dynamics of additional fields affect the clustering of matter in the linear regime and it would otherwise be difficult to simulate their impact in the nonlinear regime.

  17. Chromatographic Separations of Enantiomers and Underivatized Oligosaccharides

    Energy Technology Data Exchange (ETDEWEB)

    Ying Liu

    2004-12-19

    My graduate research has focused on separation science and bioanalytical analysis, which emphasized in method development. It includes three major areas: enantiomeric separations using high performance liquid chromatography (HPLC), Super/subcritical fluid chromatography (SFC), and capillary electrophoresis (CE); drug-protein binding behavior studies using CE; and carbohydrate analysis using liquid chromatograph-electrospray ionization mass spectrometry (LC-ESI-MS). Enantiomeric separations continue to be extremely important in the pharmaceutical industry. An in-depth evaluation of the enantiomeric separation capabilities of macrocyclic glycopeptides CSPs with SFC mobile phases was investigated using a set of over 100 chiral compounds. It was found that the macrocyclic based CSPs were able to separate enantiomers of various compounds with different polarities and functionalities. Seventy percent of all separations were achieved in less than 4 min due to the high flow rate (4.0 ml/min) that can be used in SFC. Drug-protein binding is an important process in determining the activity and fate of a drug once it enters the body. Two drug/protein systems have been studied using frontal analysis CE method. More sensitive fluorescence detection was introduced in this assay, which overcame the problem of low sensitivity that is common when using UV detection for drug-protein studies. In addition, the first usage of an argon ion laser with 257 nm beam coupled with CCD camera as a frontal analysis detection method enabled the simultaneous observation of drug fluorescence as well as the protein fluorescence. LC-ESI-MS was used for the separation and characterization of underivatized oligosaccharide mixtures. With the limits of detection as low as 50 picograms, all individual components of oligosaccharide mixtures (up to 11 glucose-units long) were baseline resolved on a Cyclobond I 2000 column and detected using ESI-MS. This system is characterized by high chromatographic

  18. Chromatographic Separations of Enantiomers and Underivatized Oligosaccharides

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Ying [Iowa State Univ., Ames, IA (United States)

    2004-01-01

    My graduate research has focused on separation science and bioanalytical analysis, which emphasized in method development. It includes three major areas: enantiomeric separations using high performance liquid chromatography (HPLC), Super/subcritical fluid chromatography (SFC), and capillary electrophoresis (CE); drug-protein binding behavior studies using CE; and carbohydrate analysis using liquid chromatograph-electrospray ionization mass spectrometry (LC-ESI-MS). Enantiomeric separations continue to be extremely important in the pharmaceutical industry. An in-depth evaluation of the enantiomeric separation capabilities of macrocyclic glycopeptides CSPs with SFC mobile phases was investigated using a set of over 100 chiral compounds. It was found that the macrocyclic based CSPs were able to separate enantiomers of various compounds with different polarities and functionalities. Seventy percent of all separations were achieved in less than 4 min due to the high flow rate (4.0 ml/min) that can be used in SFC. Drug-protein binding is an important process in determining the activity and fate of a drug once it enters the body. Two drug/protein systems have been studied using frontal analysis CE method. More sensitive fluorescence detection was introduced in this assay, which overcame the problem of low sensitivity that is common when using UV detection for drug-protein studies. In addition, the first usage of an argon ion laser with 257 nm beam coupled with CCD camera as a frontal analysis detection method enabled the simultaneous observation of drug fluorescence as well as the protein fluorescence. LC-ESI-MS was used for the separation and characterization of underivatized oligosaccharide mixtures. With the limits of detection as low as 50 picograms, all individual components of oligosaccharide mixtures (up to 11 glucose-units long) were baseline resolved on a Cyclobond I 2000 column and detected using ESI-MS. This system is characterized by high chromatographic

  19. Análise de suspensões de argilas por espectrometria de emissão óptica com plasma induzido com configuração axial Clay slurries analysis using inductively coupled plasma optical emission spectrometry with axial view configuration

    Directory of Open Access Journals (Sweden)

    Cíntia S. Silva

    2002-12-01

    Full Text Available The goal of this study was to evaluate the feasibility of direct introduction of clay slurries in an inductively coupled plasma optical emission spectrometer with axial view configuration. Calibration was performed using a certified reference material with a mean particle size of 13 µm (IPT-42 and the analytical curve was applied for quantification of two others reference materials (IPT-28 and IPT-32 and four samples. It was demonstrated that the analytical curve thus obtained was not completely suitable for IPT-28 and samples due to different mineralogical phases determined by X-ray diffraction. After considering this effect, it was possible for most elements to obtain results in agreement with certified values or with values obtained by a conventional technique at a 95% confidence level. It was demonstrated that the ICP-OES with axial view configuration did not present any incompatibility with the direct introduction of a complex inorganic suspension.

  20. Decomposição de argilas em forno de microondas e determinação simultânea dos seus constituintes principais por espectrometria de emissão óptica em plasma indutivamente acoplado Analysis of clays by inductively coupled plasma optical emission spectrometry after closed-vessel microwave-assisted acid decomposition

    Directory of Open Access Journals (Sweden)

    Claudineia R. Silva

    2005-02-01

    Full Text Available In this work a closed-vessel microwave-assisted acid decomposition procedure for clays was developed. Aluminum, Ca, Fe, K, Mg, Na, Si, and Ti were determined in clay digestates by inductively coupled plasma optical emission spectrometry. The most critical parameter for total decomposition of clays was the composition of the reagent mixture. The applied power and the heating time exerted a less critical influence. Best decomposition conditions were attained using a reagent mixture containing 4 mL aqua regia plus 3 mL HF and the heating program was implemented in 12 min. The accuracy of the results was demonstrated using two standard reference materials and a paired t-test showed a good agreement between determined and certified values at a 95% confidence level.