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Sample records for mass separator st

  1. COSY Simulations to Guide Commissioning of the St. George Recoil Mass Separator

    NASA Astrophysics Data System (ADS)

    Schmitt, Jaclyn; Moran, Michael; Seymour, Christopher; Gilardy, Gwenaelle; Meisel, Zach; Couder, Manoel

    2015-10-01

    The goal of St. George (STrong Gradient Electromagnetic Online Recoil separator for capture Gamma ray Experiments) is to measure (α, γ) cross sections relevant to stellar helium burning. Recoil separators such as St. George are able to more closely approach the low astrophysical energies of interest because they collect reaction recoils rather than γ-rays, and thus are not limited by room background. In order to obtain an accurate cross section measurement, a recoil separator must be able to collect all recoils over their full range of expected energy and angular spread. The energy acceptance of St. George is currently being measured, and the angular acceptance will be measured soon. Here we present the results of COSY ion optics simulations and magnetic field analyses which were performed to help guide the commissioning measurements and diagnostic upgrades required to complete those measurements. National Science Foundation Research Experiences for Undergraduates program.

  2. Mass Separation by Metamaterials

    NASA Astrophysics Data System (ADS)

    Restrepo-Flórez, Juan Manuel; Maldovan, Martin

    2016-02-01

    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.

  3. Moving towards first science with the St. George recoil separator

    NASA Astrophysics Data System (ADS)

    Meisel, Zachary; Berg, G. P. A.; Gilardy, G.; Moran, M.; Schmitt, J.; Seymour, C.; Stech, E.; Couder, M.

    2015-10-01

    The St. George recoil mass separator has recently been coupled to the 5MV St. Ana accelerator at the University of Notre Dame's Nuclear Science Lab. St. George is a unique tool designed to measure radiative alpha-capture reactions for nuclei up to A = 40 in inverse kinematics in order to directly obtain cross sections required for astrophysical models of stellar and explosive helium burning. Commissioning of St. George is presently taking place with primary beams of hydrogen, helium, and oxygen. In this presentation, results will be shown for the measured energy acceptance of St. George, which compare favorably to COSY results when employing the calculated optimal ion-optical settings. Additionally, future plans will be discussed, such as assessing the angular acceptance of St. George and the re-integration of HiPPO at the separator target position to provide a dense, windowless helium gas-jet target. The material presented in this work is partially supported by the National Science Foundation Grant No. 1419765.

  4. Optics of mass separator I

    SciTech Connect

    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. Separable quantizations of Stäckel systems

    NASA Astrophysics Data System (ADS)

    Błaszak, Maciej; Marciniak, Krzysztof; Domański, Ziemowit

    2016-08-01

    In this article we prove that many Hamiltonian systems that cannot be separably quantized in the classical approach of Robertson and Eisenhart can be separably quantized if we extend the class of admissible quantizations through a suitable choice of Riemann space adapted to the Poisson geometry of the system. Actually, in this article we prove that for every quadratic in momenta Stäckel system (defined on 2 n dimensional Poisson manifold) for which Stäckel matrix consists of monomials in position coordinates there exist infinitely many quantizations-parametrized by n arbitrary functions-that turn this system into a quantum separable Stäckel system.

  6. Energy acceptance of the St. George recoil separator

    NASA Astrophysics Data System (ADS)

    Meisel, Z.; Moran, M. T.; Gilardy, G.; Schmitt, J.; Seymour, C.; Couder, M.

    2017-04-01

    Radiative alpha-capture, (α , γ) , reactions play a critical role in nucleosynthesis and nuclear energy generation in a variety of astrophysical environments. The St. George recoil separator at the University of Notre Dame's Nuclear Science Laboratory was developed to measure (α , γ) reactions in inverse kinematics via recoil detection in order to obtain nuclear reaction cross sections at the low energies of astrophysical interest, while avoiding the γ-background that plagues traditional measurement techniques. Due to the γ ray produced by the nuclear reaction at the target location, recoil nuclei are produced with a variety of energies and angles, all of which must be accepted by St. George in order to accurately determine the reaction cross section. We demonstrate the energy acceptance of the St. George recoil separator using primary beams of helium, hydrogen, neon, and oxygen, spanning the magnetic and electric rigidity phase space populated by recoils of anticipated (α , γ) reaction measurements. We find the performance of St. George meets the design specifications, demonstrating its suitability for (α , γ) reaction measurements of astrophysical interest.

  7. MASS SEPARATION OF HIGH ENERGY PARTICLES

    DOEpatents

    Marshall, L.

    1962-09-25

    An apparatus and method are described for separating charged, high energy particles of equal momentum forming a beam where the particles differ slightly in masses. Magnetic lenses are utilized to focus the beam and maintain that condition while electrostatic fields located between magnetic lenses are utilized to cause transverse separation of the particles into two beams separated by a sufficient amount to permit an aperture to block one beam. (AEC)

  8. CHARGE BOTTLE FOR A MASS SEPARATOR

    DOEpatents

    Davidson, P.H.

    1959-07-01

    Improved mass separator charge bottles are described for containing a dense charge of a chemical compound of copper, nickel, lead or other useful substance which is to be vaporized, and to the method of utilizing such improvcd charge bottles so that the chemical compound is vaporized from the under surface of the charge and thus permits the non-volatile portion thereof to fall to the bottom of the charge bottle where it does not form an obstacle to further evaporation. The charge bottle comprises a vertically disposed cylindrical portion, an inner re-entrant cylindrical portion extending axially and downwardly into the same from the upper end thereof, and evaporative source material in the form of a chemical compound compacted within the upper annular pontion of the charge bottle formed by the re-entrant cylindrical portion, whereby vapor from the chemical compound will pass outwardly from the charge bottle through an apertured closure.

  9. Advances and problems in plasma-optical mass-separation

    SciTech Connect

    Bardakov, V. M.; Ivanov, S. D.; Strokin, N. A.

    2014-03-15

    This paper presents a short review of plasma-optical mass-separation and defines the fields for its possible application. During theoretical studies, numerical simulations, and experiments, the effect of the azimuthator finite size and of the vacuum conditions on the mass separator characteristics was revealed, as well as the quality of different-mass ion separation. The problems, solving which may lead to a successful end of the mass-separation plasma-optical technique implementation, were specified.

  10. Plasma mass filtering for separation of actinides from lanthanides

    NASA Astrophysics Data System (ADS)

    Gueroult, R.; Fisch, N. J.

    2014-06-01

    Separating lanthanides from actinides is a key process in reprocessing nuclear spent fuel. Plasma mass filters, which operate on dissociated elements, offer conceptual advantages for such a task as compared with conventional chemical methods. The capabilities of a specific plasma mass filter concept, called the magnetic centrifugal mass filter, are analyzed within this particular context. Numerical simulations indicate separation of americium ions from a mixture of lanthanides ions for plasma densities of the order of 1012 cm-3, and ion temperatures of about 10 eV. In light of collision considerations, separating small fractions of heavy elements from a larger volume of lighter ones is shown to enhance the separation capabilities.

  11. Rotation and instabilities for isotope and mass separation

    NASA Astrophysics Data System (ADS)

    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.

  12. Compact ExB mass separator for heavy ion beams

    SciTech Connect

    Wada, M.; Hashino, T.; Hirata, F.; Kasuya, T.; Sakamoto, Y.; Nishiura, M.

    2008-02-15

    A compact ExB mass separator that deflects beam by 30 deg. has been designed and built to prove its principle of operation. The main part of the separator is contained in a shielding box of 11 cm long, 9 cm wide, and 1.5 cm high. An electromagnet of 7 cm pole diameter produced variable magnetic field in the mass separation region instead of a couple of permanent magnets which is to be used in the final design. The experimental result agreed well with the theoretical prediction, and larger mass ions is bent with less magnetic field with the aid of the deflection electric field. The reduction in resolving power for mass separation due to the deflection electric field has been investigated experimentally.

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

    DOEpatents

    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.

  14. Mass transfer apparatus and method for separation of gases

    DOEpatents

    Blount, Gerald C.

    2015-10-13

    A process and apparatus for separating components of a source gas is provided in which more soluble components of the source gas are dissolved in an aqueous solvent at high pressure. The system can utilize hydrostatic pressure to increase solubility of the components of the source gas. The apparatus includes gas recycle throughout multiple mass transfer stages to improve mass transfer of the targeted components from the liquid to gas phase. Separated components can be recovered for use in a value added application or can be processed for long-term storage, for instance in an underwater reservoir.

  15. Mass Transport Separation via Grace: Anthropogenic and Natural Change

    NASA Astrophysics Data System (ADS)

    Dickey, J. O.; de Viron, O.

    2011-12-01

    The GRACE satellite has been monitoring the change in the mass distribution at the Earth surface for nearly 10 years. This becomes enough to study long-term mass change, and to separate interannual variations from trends. Up to now, many studies have shown a fast (and non-linear) loss of mass in many glaciers and ice sheets. They all have been attributed to global warming, though part of the mass variation is also associated with the classical long-term climate variation. Using climatic data as well as the GRACE mascon solution, we can separate the part associated to the anthropogenic part from the non-anthropogenic part, in order to better estimate those contributions. Results and implications from our analyses will be presented.

  16. Assessment of the capabilities of the tICA and stICA methods for geophysical signal separation in GRACE data

    NASA Astrophysics Data System (ADS)

    Börgens, Eva; Rangelova, Elena; Sideris, Michael; Kusche, Jürgen

    2013-04-01

    We investigate the potential of the tICA and stICA methods for separating geophysical signals in GRACE gravity data. Since the start of the Gravity Recovery and Climate Experiment (GRACE) satellite mission in 2002, GRACE has provided us with global gravity data with a spatial resolution of a few hundred kilometers and a temporal resolution of one month, 10 days or even a week. These data represent the total, integrated gravity change inducing by mass signals related to hydrological processes, post glacial rebound (PGR), ice mass change and others. Isolating a particular mass signal may be accomplished by removing all others using geophysical background models, but these are usually not perfect. Therefore methods are required for separating data into the different geophysical signals on the basis of their statistical properties. To this end, we assess the potential of temporal Independent Component Analysis (tICA) and spatio-temporal Independent Component Analysis (stICA). The tICA method is based on the assumption of statistical independence of signals in the temporal domain and thus separates the GRACE-observed mass changes into maximal independent source signals. In comparison, stICA maximizes both the temporal and spatial independence. These two ICA methods are compared to the conventional Principle Component Analysis (PCA). We test them on GRACE data with respect to their ability to separate the hydrology signal from a trend signal not induced by hydrological processes, such as post glacial rebound (PGR). In addition, we investigate whether they are capable of separating the hydrological signal in annual and semi-annual components. We analyze both simulated and CSR GRACE water mass anomalies (January 2003 -December 2010). The simulated mass anomalies are composed of outputs of hydrologic, PGR, ice loss and ocean bottom pressure models. The two ICA methods are capable of separating the trend and annual hydrology signals both on a global and regional scale (North

  17. Quark mass correction to chiral separation effect and pseudoscalar condensate

    NASA Astrophysics Data System (ADS)

    Guo, Er-dong; Lin, Shu

    2017-01-01

    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.

  18. Ion optics system incorporating radio frequency mass separation

    NASA Technical Reports Server (NTRS)

    Anderson, John R.; Carruth, M. R., Jr.

    1990-01-01

    Results of an experimental study are presented. They show that an RF mass discriminator, based on a Bennett mass spectrometer concept, can be used to discriminate between two species of ions with about a 2-to-1 charge-to-mass ratio. Such a device would be useful for separating monatomic and diatomic oxygen ions in a system designed to simulate the environment that spacecraft encounter in low earth orbit. The influence of changing mass discriminator parameters - such as the spacing of its grids, the amplitude and frequency of RF voltage signals applied to it and the current density of ions incident upon it - on its species discrimination capabilities is discussed. Experimental results are also compared to the results of a simple theoretical model to gain insight into the processes occurring in the discriminator. These results are shown to be in good agreement.

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

    SciTech Connect

    Dion, Michael; Eiden, Greg; Farmer, Orville; Finch, Zach; Liezers, Martin

    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).

  20. Is the Binary Mass Ratio Distribution Separation-Dependent?

    NASA Astrophysics Data System (ADS)

    Gullikson, Kevin; Kraus, Adam L.

    2016-01-01

    Recent discoveries of planets orbiting retired A-stars on close orbits and young A-stars on very wide orbits have renewed interest in the properties of nearby intermediate-mass stars. Especially interesting are the young stars because directly-imaged planets orbiting them may be bright enough for characterization (e.g. HR 8799, Beta Pictoris, etc). However, intermediate-mass stars and especially young intermediate mass stars are part of multiple systems more often than not. Close stellar companions may affect the formation and orbital evolution of any planets, and the properties of the companions can help constrain the binary formation mechanism. The mass ratio distribution of a population of binary stars, especially if the distribution for close companions is significantly different from that of wide companions, is helpful to distinguish companions that were born in or affected by the circumstellar disk from those which formed through fragmentation of the molecular core. Previous imaging surveys have found that binary systems with A-type primary stars tend to have cool companions with extreme mass ratios. There are hints at a much flatter mass ratio distribution for close companions, but strong completeness effects complicate the picture. We have conducted a spectroscopic survey of ~400 nearby main sequence A- and B-type stars, aimed at detecting stellar companions as late as M4 for all orbital separations <100 AU. We have searched for companions to the stars by cross-correlating the spectra against model templates for F-M type stars; a significant peak in the cross-correlation function indicates a detection. Our cross-correlation technique can detect low-mass companions with orbits that are too wide to detect with radial velocity monitoring and too small to detect with imaging techniques, making it complementary to work already done. We will present results from our survey and compare the mass ratio distribution we measure to the corresponding distribution for

  1. Combined heat and mass transfer device for improving separation process

    DOEpatents

    Tran, Thanh Nhon

    1999-01-01

    A two-phase small channel heat exchange matrix simultaneously provides for heat transfer and mass transfer between the liquid and vapor phases of a multi-component mixture at a single, predetermined location within a separation column, significantly improving the thermodynamic efficiency of the separation process. The small channel heat exchange matrix is composed of a series of channels having a hydraulic diameter no greater than 5.0 millimeters for conducting a two-phase coolant. In operation, the matrix provides the liquid-vapor contacting surfaces within the separation column, such that heat and mass are transferred simultaneously between the liquid and vapor phases. The two-phase coolant allows for a uniform heat transfer coefficient to be maintained along the length of the channels and across the surface of the matrix. Preferably, a perforated, concave sheet connects each channel to an adjacent channel to facilitate the flow of the liquid and vapor phases within the column and to increase the liquid-vapor contacting surface area.

  2. Combined heat and mass transfer device for improving separation process

    DOEpatents

    Tran, T.N.

    1999-08-24

    A two-phase small channel heat exchange matrix simultaneously provides for heat transfer and mass transfer between the liquid and vapor phases of a multi-component mixture at a single, predetermined location within a separation column, significantly improving the thermodynamic efficiency of the separation process. The small channel heat exchange matrix is composed of a series of channels having a hydraulic diameter no greater than 5.0 millimeters for conducting a two-phase coolant. In operation, the matrix provides the liquid-vapor contacting surfaces within the separation column, such that heat and mass are transferred simultaneously between the liquid and vapor phases. The two-phase coolant allows for a uniform heat transfer coefficient to be maintained along the length of the channels and across the surface of the matrix. Preferably, a perforated, concave sheet connects each channel to an adjacent channel to facilitate the flow of the liquid and vapor phases within the column and to increase the liquid-vapor contacting surface area. 12 figs.

  3. Attomole quantitation of protein separations with accelerator mass spectrometry

    SciTech Connect

    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.

  4. Chemical separations by bubble-assisted interphase mass-transfer.

    PubMed

    Boyd, David A; Adleman, James R; Goodwin, David G; Psaltis, Demetri

    2008-04-01

    We show that when a small amount of heat is added close to a liquid-vapor interface of a captive gas bubble in a microchannel, interphase mass-transfer through the bubble can occur in a controlled manner with only a slight change in the temperature of the fluid. We demonstrate that this method, which we refer to as bubble-assisted interphase mass-transfer (BAIM), can be applied to interphase chemical separations, e.g., simple distillation, without the need for high temperatures, vacuum, or active cooling. Although any source of localized heating could be used, we illustrate BAIM with an all-optical technique that makes use of the plasmon resonance in an array of nanoscale metal structures that are incorporated into the channel to produce localized heating of the fluid when illuminated by a stationary low-power laser.

  5. Widest Separation and the Lowest Mass Objects among Planetary-mass Companion Candidates around Young Stars

    NASA Astrophysics Data System (ADS)

    Oh, D.

    2014-08-01

    Two substellar companion candidates with planetary mass, around a T-Tauri star in the ρ Ophiuchi star-forming region, are discovered by results of near-infrared imaging. Candidates are separated by 1454AU, candi 1 for short, and 542AU, candi 2 for short. There are high possibilities that both candidates are physically related to its primary star from their common proper motions, colors and statistics of YSOs in star forming region. candi 2 is identified as an extremely low-mass object, 0.0070.002 ⊙, and this is the lowest mass among planetary-mass companion(PMC) candidates imaged to date. In addition, separation from its primary star of candi 1, 0.014 ± 0.002 ⊙, is the widest among PMC candidates imaged to date. Formation of these extremely wide separated, > 100AU, PMCs, like candi 1 and c, is not fully explained by current planet formation theories, core accretion or gravitational instability. This discovery may suggest that PMCs separated by > 100AU form via extreme mass ratio case of cloud core fragmentation for multiple stars. Apologies : Because of our team policy, we cannot present the name and details of this target currently.

  6. Sub-barrier reactions measured using a recoil mass separator

    SciTech Connect

    Betts, R.R.

    1988-01-01

    Few data exist in the sub-barrier region for reaction channels other than fusion. In particular, our experimental knowledge of quasi-elastic transfer reactions is sparse, despite the belief that this particular channel may be dominant in determining some features of the sub-barrier fusion enhancement. Transfer reactions are governed primarily by the closet approach of the colliding nuclei which, at low energies, results in a strong backward peaking of the angular distribution in the center-of-mass frame. For situations where the projectile has a significant fraction of the target mass, as is so in most cases of interest, the backscattered projectile-like fragment has such low energy that the usual techniques of measurement and identification become invalid. Here, we report on a solution to this problem which allows a systematic study of many aspects of transfer reactions in the energy regime of interest. We exploit the fact that associated with the low-energy backscattered projectile-like fragment is a complementary target-like fragment which recoils to forward angles with a large fraction of the incident beam energy. These target-like fragments were detected and identified using the Daresbury Recoil Mass Separator thus allowing the measurement of quasi-elastic transfer over hitherto inaccessible energy range from the vicinity of the barrier to several tens of MeV below. The experiments described here used VYNi beams of energies ranging from 180 to 260 MeV provided by the Daresbury Laboratory Nuclear Structure Facility tandem accelerator. Data on sub-barrier transfer for targets of /sup 116,118,120,122,124/Sn and /sup 144,148,150,152,154/Sm were obtained. 16 refs., 10 figs., 2 tabs.

  7. An examination of possible mass burials in Pensacola, Florida's historic St. Michael's Cemetery

    NASA Astrophysics Data System (ADS)

    Rosenberg Marshall, Nicole Marie

    St. Michael's Cemetery is the oldest extant cemetery in Pensacola, Florida. St. Michael's Cemetery is also one of the two oldest cemeteries in Florida (the other being located in St. Augustine). Since 2000, the University of West Florida (UWF) has been engaged in ongoing research at the cemetery. Historical records indicate that a significant unmarked burial population may be present within the cemetery. In 2007 and 2008, a systematic Ground Penetrating Radar (GPR) survey identified 3,915 sub-surface anomalies that may represent unmarked burials. Some of these anomalies are significantly larger than would be expected for single interments and potentially represent mass burials from colonial and post-colonial period epidemic events. To test this hypothesis, excavations were conducted at three of the five large anomalies during 2009, 2010, and 2011. The goals of these investigations were to determine whether the sub-surface anomalies represent mass interments and to determine the chronology and ethnicity of any individual burials encountered using grave attributes and associated artifacts. While none of the anomalies excavated were mass graves, several individual unmarked burials were exposed and documented. This thesis summarizes the methods, results, and conclusions of the research conducted in St. Michael's Cemetery while contextualizing them within previous research.

  8. Binary Cepheids: Separations and Mass Ratios in 5 Solar Mass Binaries

    DTIC Science & Technology

    2013-10-01

    material: color figures 1. INTRODUCTION Binary-star studies are valuable for what they provide directly (e.g., stellar masses), as well as for the...the high stellar density in the cluster, this could be a chance alignment. 3.2.2. Approximate Orbital Periods We used the angular separations in Table...subsequent evolution of the system will be drastically altered. For Cepheids we have a good estimation of where this effect sets in. Z Lac—not in our sample

  9. Spectral Measurements of Plasma Rotation and Mass Separation in the Archimedes Plasma Mass Filter

    NASA Astrophysics Data System (ADS)

    Umstadter, K. R.; Anderegg, F.; Cluggish, B. P.; Freeman, R. L.; Gilleland, J.; Isler, R. C.; Lee, W. D.; Litvak, A.; Mavrin, V.; Miller, R. L.; Ohkawa, T.; Putvinski, S.

    2003-10-01

    The Archimedes Demonstration Unit (ADU), a full scale experiment based upon the Plasma Mass Filter^1 technology, began plasma operations early this year. The Filter is a cylindrical device with an axial magnetic field that utilizes end electrodes to generate a radial electric field in a noble gas plasma of density ˜10^18 m-3. In addition to microwave interferometry, bolometry, videography and Langmuir probe diagnostics, high-resolution and survey spectroscopy is utilized to monitor the plasma emission. This is accomplished through the use of several in-vacuum optical arrays which have collimated views parallel and perpendicular to the magnetic axis. Optical measurements are compared to other diagnostics and electrode currents. Doppler shifts, linewidths and line ratios have been measured to determine rotation speed, temperature and separation in noble gas plasmas. ^1T. Ohkawa, "Plasma Mass Filter", U.S. Patent 6,096,220, August 1, 2000.

  10. Isobar Separation in a Multiple-Reflection Time-of-Flight Mass Spectrometer by Mass-Selective Re-Trapping

    NASA Astrophysics Data System (ADS)

    Dickel, Timo; Plaß, Wolfgang R.; Lippert, Wayne; Lang, Johannes; Yavor, Mikhail I.; Geissel, Hans; Scheidenberger, Christoph

    2017-03-01

    A novel method for (ultra-)high-resolution spatial mass separation in time-of-flight mass spectrometers is presented. Ions are injected into a time-of-flight analyzer from a radio frequency (rf) trap, dispersed in time-of-flight according to their mass-to-charge ratios and then re-trapped dynamically in the same rf trap. This re-trapping technique is highly mass-selective and after sufficiently long flight times can provide even isobaric separation. A theoretical treatment of the method is presented and the conditions for optimum performance of the method are derived. The method has been implemented in a multiple-reflection time-of-flight mass spectrometer and mass separation powers (FWHM) in excess of 70,000, and re-trapping efficiencies of up to 35% have been obtained for the protonated molecular ion of caffeine. The isobars glutamine and lysine (relative mass difference of 1/4000) have been separated after a flight time of 0.2 ms only. Higher mass separation powers can be achieved using longer flight times. The method will have important applications, including isobar separation in nuclear physics and (ultra-)high-resolution precursor ion selection in multiple-stage tandem mass spectrometry.

  11. Isobar Separation in a Multiple-Reflection Time-of-Flight Mass Spectrometer by Mass-Selective Re-Trapping.

    PubMed

    Dickel, Timo; Plaß, Wolfgang R; Lippert, Wayne; Lang, Johannes; Yavor, Mikhail I; Geissel, Hans; Scheidenberger, Christoph

    2017-03-15

    A novel method for (ultra-)high-resolution spatial mass separation in time-of-flight mass spectrometers is presented. Ions are injected into a time-of-flight analyzer from a radio frequency (rf) trap, dispersed in time-of-flight according to their mass-to-charge ratios and then re-trapped dynamically in the same rf trap. This re-trapping technique is highly mass-selective and after sufficiently long flight times can provide even isobaric separation. A theoretical treatment of the method is presented and the conditions for optimum performance of the method are derived. The method has been implemented in a multiple-reflection time-of-flight mass spectrometer and mass separation powers (FWHM) in excess of 70,000, and re-trapping efficiencies of up to 35% have been obtained for the protonated molecular ion of caffeine. The isobars glutamine and lysine (relative mass difference of 1/4000) have been separated after a flight time of 0.2 ms only. Higher mass separation powers can be achieved using longer flight times. The method will have important applications, including isobar separation in nuclear physics and (ultra-)high-resolution precursor ion selection in multiple-stage tandem mass spectrometry. Graphical Abstract ᅟ.

  12. Relationships involving fine-particle mass, fine-particle sulfur, and ozone during episodic periods at sites in and around St. Louis, Missouri

    SciTech Connect

    Altshuller, A.P.

    1985-01-01

    A number of investigations have been published on relationships involving particulate sulfate over regions of North America. Elevated concentrations of sulfate and ozone have been identified as occurring during the same periods in the summer months of the year in the United States. Particle sulfur and particle mass measurements obtained from the regional monitoring stations (RAMS) in and around St. Louis, Missouri, during the Regional Air Pollution Study (RAPS) have been discussed previously. Ozone measurements made in the RAPS study have received separate consideration. The large extended series of concurrent measurements of fine-particle sulfur, fine-particle mass, and ozone at both urban and nonurban locations in the St. Louis area provides an opportunity to examine relationships among these species in detail. The emphasis here is on the patterns of concentration of these species particularly during periods of especially high concentrations, episodic periods.

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

    DOEpatents

    Yeung, Edward S.; Chang, Yu-chen

    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.

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

    DOEpatents

    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.

  15. Still Separate, Still Unequal: Social Determinants of Playground Safety and Proximity Disparities in St. Louis.

    PubMed

    Arroyo-Johnson, Cassandra; Woodward, Krista; Milam, Laurel; Ackermann, Nicole; Komaie, Goldie; Goodman, Melody S; Hipp, J Aaron

    2016-08-01

    Physical activity among youth is shaped by the natural and built environment within which they live; however, few studies have focused on assessing playground safety and proximity in detail as part of the built environment for youth physical activity. We analyzed data on 100 publicly accessible playgrounds from Play Across St. Louis, a community-partnered study of the built environment for youth physical activity. Outcomes included overall playground safety, maintenance, and construction scores; distance to nearest playground; and distance to nearest top playground. Independent variables included neighborhood % youth, % black residents, % owner-occupied units, and % vacant units. Playgrounds in the city have varying degrees of safety and proximity. Mean overall playground safety score was 67.0 % (CI = 63.5, 70.4). Neighborhood % youth and % black residents were inversely associated with overall playground safety (p = 0.03 and p < 0.01) and maintenance (p < 0.01 and p < 0.0001). Mean distance to nearest playground was 638.1 and 1488.3 m to nearest top playground. Clusters of low safety scores were found in the northern and central areas while all high safety score clusters were found in the southern part of St. Louis. Public playground safety and proximity vary across St. Louis neighborhoods, especially by neighborhood demographics. Disparities in playground safety and proximity reveal an opportunity to develop community-wide interventions focused on playgrounds for youth activity. Further work is needed to examine the association between playground safety, proximity, and use and youth physical activity and weight.

  16. Mid-Pleistocene climate transition drives net mass loss from rapidly uplifting St. Elias Mountains, Alaska.

    PubMed

    Gulick, Sean P S; Jaeger, John M; Mix, Alan C; Asahi, Hirofumi; Bahlburg, Heinrich; Belanger, Christina L; Berbel, Glaucia B B; Childress, Laurel; Cowan, Ellen; Drab, Laureen; Forwick, Matthias; Fukumura, Akemi; Ge, Shulan; Gupta, Shyam; Kioka, Arata; Konno, Susumu; LeVay, Leah J; März, Christian; Matsuzaki, Kenji M; McClymont, Erin L; Moy, Chris; Müller, Juliane; Nakamura, Atsunori; Ojima, Takanori; Ribeiro, Fabiana R; Ridgway, Kenneth D; Romero, Oscar E; Slagle, Angela L; Stoner, Joseph S; St-Onge, Guillaume; Suto, Itsuki; Walczak, Maureen D; Worthington, Lindsay L; Bailey, Ian; Enkelmann, Eva; Reece, Robert; Swartz, John M

    2015-12-08

    Erosion, sediment production, and routing on a tectonically active continental margin reflect both tectonic and climatic processes; partitioning the relative importance of these processes remains controversial. Gulf of Alaska contains a preserved sedimentary record of the Yakutat Terrane collision with North America. Because tectonic convergence in the coastal St. Elias orogen has been roughly constant for 6 My, variations in its eroded sediments preserved in the offshore Surveyor Fan constrain a budget of tectonic material influx, erosion, and sediment output. Seismically imaged sediment volumes calibrated with chronologies derived from Integrated Ocean Drilling Program boreholes show that erosion accelerated in response to Northern Hemisphere glacial intensification (∼ 2.7 Ma) and that the 900-km-long Surveyor Channel inception appears to correlate with this event. However, tectonic influx exceeded integrated sediment efflux over the interval 2.8-1.2 Ma. Volumetric erosion accelerated following the onset of quasi-periodic (∼ 100-ky) glacial cycles in the mid-Pleistocene climate transition (1.2-0.7 Ma). Since then, erosion and transport of material out of the orogen has outpaced tectonic influx by 50-80%. Such a rapid net mass loss explains apparent increases in exhumation rates inferred onshore from exposure dates and mapped out-of-sequence fault patterns. The 1.2-My mass budget imbalance must relax back toward equilibrium in balance with tectonic influx over the timescale of orogenic wedge response (millions of years). The St. Elias Range provides a key example of how active orogenic systems respond to transient mass fluxes, and of the possible influence of climate-driven erosive processes that diverge from equilibrium on the million-year scale.

  17. Mid-Pleistocene climate transition drives net mass loss from rapidly uplifting St. Elias Mountains, Alaska

    PubMed Central

    Jaeger, John M.; Mix, Alan C.; Asahi, Hirofumi; Bahlburg, Heinrich; Belanger, Christina L.; Berbel, Glaucia B. B.; Childress, Laurel; Cowan, Ellen; Drab, Laureen; Forwick, Matthias; Fukumura, Akemi; Ge, Shulan; Gupta, Shyam; Konno, Susumu; LeVay, Leah J.; März, Christian; McClymont, Erin L.; Moy, Chris; Müller, Juliane; Nakamura, Atsunori; Ojima, Takanori; Ribeiro, Fabiana R.; Ridgway, Kenneth D.; Romero, Oscar E.; Slagle, Angela L.; Stoner, Joseph S.; St-Onge, Guillaume; Suto, Itsuki; Walczak, Maureen D.; Worthington, Lindsay L.; Bailey, Ian; Enkelmann, Eva; Reece, Robert; Swartz, John M.

    2015-01-01

    Erosion, sediment production, and routing on a tectonically active continental margin reflect both tectonic and climatic processes; partitioning the relative importance of these processes remains controversial. Gulf of Alaska contains a preserved sedimentary record of the Yakutat Terrane collision with North America. Because tectonic convergence in the coastal St. Elias orogen has been roughly constant for 6 My, variations in its eroded sediments preserved in the offshore Surveyor Fan constrain a budget of tectonic material influx, erosion, and sediment output. Seismically imaged sediment volumes calibrated with chronologies derived from Integrated Ocean Drilling Program boreholes show that erosion accelerated in response to Northern Hemisphere glacial intensification (∼2.7 Ma) and that the 900-km-long Surveyor Channel inception appears to correlate with this event. However, tectonic influx exceeded integrated sediment efflux over the interval 2.8–1.2 Ma. Volumetric erosion accelerated following the onset of quasi-periodic (∼100-ky) glacial cycles in the mid-Pleistocene climate transition (1.2–0.7 Ma). Since then, erosion and transport of material out of the orogen has outpaced tectonic influx by 50–80%. Such a rapid net mass loss explains apparent increases in exhumation rates inferred onshore from exposure dates and mapped out-of-sequence fault patterns. The 1.2-My mass budget imbalance must relax back toward equilibrium in balance with tectonic influx over the timescale of orogenic wedge response (millions of years). The St. Elias Range provides a key example of how active orogenic systems respond to transient mass fluxes, and of the possible influence of climate-driven erosive processes that diverge from equilibrium on the million-year scale. PMID:26598689

  18. Optical spectroscopy using mass-separated beams: Nuclear properties of unstable indium and tin isotopes

    NASA Astrophysics Data System (ADS)

    Kuehl, T.; Kirchner, R.; Klepper, O.; Marx, D.; Dinger, U.; Eberz, J.; Huber, G.; Lochmann, H.; Menges, R.; Ulm, G.

    1987-05-01

    Collinear fast-beam laser-spectroscopy has been used to measure the hyperfine structure and isotope shift of several indium and tin isotopes. The related experimental techniques are described, including the preparation of mass-separated beams of neutron-deficient indium and tin isotopes at the GSI on-line mass separator following fusion-evaporation reactions. The deviation of the observed dependence of the charge radii upon the neutron number from the expected behaviour is briefly discussed.

  19. Atmospheric Pressure Surface Sampling/Ionization Techniques for Direct Coupling of Planar Separations with Mass Spectrometry

    SciTech Connect

    Pasilis, Sofie P; Van Berkel, Gary J

    2010-01-01

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

  20. Mass Intrusion at Mount St. Helens (WA) From Temporal Gravity Variations

    NASA Astrophysics Data System (ADS)

    Battaglia, M.; Lisowski, M.; Dzurisin, D.; Poland, M. P.; Schilling, S. P.; Diefenbach, A. K.; Wynn, J.

    2015-12-01

    Repeated high-precision gravity measurements made at Mount St. Helens (WA) have revealed systematic temporal variations in the gravity field several years after the end of the 2004-2008 dome-building eruption. Changes in gravity with respect to a stable reference station 36 km NW of the volcano were measured at 10 sites on the volcanic edifice and at 4 sites far afield (10 to 36 km) from the summit in August 2010, August 2012 and August 2014. After simulating and removing the gravity signal associated with changes in mass of the crater glacier, the local hydrothermal aquifer, and vertical deformation, the residual gravity field observed at sites near the volcano's summit significantly increased with respect to the stable reference site during 2010-2012 (maximum change 48 ± 15 mgal). No significant change was measured during 2012-2014. The pattern of gravity increase is radially symmetrical, with a half-width of about 2.5 km and a point of maximum change centered at the 2004-2008 lava dome. Forward modeling of residual gravity data using the same source geometry, depth, and location as that inferred from geodetic data (a spheroidal source centered 7.5 km beneath the 2004-2008 dome) indicates a mass increase rate of the order of 1011 kg/year. For a reasonable magma density (~2250 kg/m3), the volume rate of magma intrusion beneath the summit region inferred from gravity (~ 0.1 km3/yr) greatly exceeds the volume inferred from inversion of geodetic data (0.001 km3/yr between 2008-2011), suggesting that either magma compressibility or other processes are important aspects of magma storage at Mount St. Helens, or that the data argue for a different source.

  1. A mass balance of genotoxicity in the St. Lawrence River (Montreal) based on SOS chromotest results

    SciTech Connect

    White, P.A.; Rasmussen, J.B.

    1995-12-31

    Mass balance models are frequently used to track contaminants in aquatic ecosystems. To the authors knowledge no mass balance has ever been constructed using only bioassay results for complex mixtures. They have used surface water SOS Chromotest results from Langevin et al (1992) and industrial effluent SOS Chromotest results from White et al (1996) to determine the steady state concentration of genotoxins in the surface waters of the St. Lawrence river around Montreal. The results of Langevin et al indicate that the St. Lawrence River west of Montreal is contributing 446 ng benzo(a)pyrene equivalents per L, while the Ottawa River is contributing 166 ng benzo(a)pyrene equivalents per L. The data of While et al indicate that industrial emissions in the Montreal area are contributing an additional 68 ng benzo(a)pyrene equivalents per L. The latter value is based on the genotoxic potency of final effluents from 13 priority industries, their daily discharge and the mean (n = 35 years) river discharge at Lasalle. Assuming that the industrial effluents do not alter the river discharge, the expected surface water concentration of genotoxins in the Montreal area is 680 ng benzo(a)pyrene equivalents per L. This value is extremely close to the mean of actual surface water measurements published by Langevin et al. (701 ng benzo(a)pyrene equivalents per L). The extremely short water residence time (< 2 days) and rapid current ({approx}1 m/sec) indicate that losses from sedimentation and decay between Valleyfield and Varennes are negligible. The results indicate that municipal wastewater discharges account for over 95% of the Montreal area contribution.

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

    SciTech Connect

    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.

  3. Delayed bunching for multi-reflection time-of-flight mass separation

    SciTech Connect

    Rosenbusch, M.; Marx, G.; Schweikhard, L.; Wienholtz, F.; Chauveau, P.; Delahaye, P.

    2015-06-29

    Many experiments are handicapped when the ion sources do not only deliver the ions of interest but also contaminations, i.e., unwanted ions of similar mass. In the recent years, multi-reflection time-of-flight mass separation has become a promising method to isolate the ions of interest from the contaminants, in particular for measurements with low-energy short-lived nuclides. To further improve the performance of multi-reflection mass separators with respect to the limitations by space-charge effects, the simultaneously trapped ions are spatially widely distributed in the apparatus. Thus, the ions can propagate with reduced Coulomb interactions until, finally, they are bunched by a change in the trapping conditions for high-resolution mass separation. Proof-of-principle measurements are presented.

  4. MASS SEPARATORS

    DOEpatents

    Oppenheimer, F.; Bell, J.W.

    1959-02-17

    An improvement in the mounting arrangement for the ion source within the vacuum tank of a calutron is presented. The entire source is supported by the vacuum envelope through the medium of a bracket secured to a removable face plate. The bracket forms a supporting platform that is generally transverse to the magnetic field. The ion generator is mounted on a pedestal-type insulator supported on the bracket, and the hot leads are brought into the vacuum envelope through a tubular elbow connected to the vacuum envelope, having the axis of its outer opening aligned with the magnetic field at which point a bushing-type insulator is employed. With this arrangement thc ion source is maintained at a positive potential with respect to the vacuum tank and the problem of electron bombardment of the insulator is considerably reduced.

  5. The Outcome of Supernovae in Massive Binaries; Removed Mass, and its Separation Dependence

    NASA Astrophysics Data System (ADS)

    Hirai, Ryosuke; Sawai, Hidetomo; Yamada, Shoichi

    2014-09-01

    The majority of massive stars are formed in binary systems. It is hence reasonable to expect that most core-collapse supernovae (CCSNe) take place in binaries and the existence of a companion star may leave some imprints in observed features. Having this in mind, we have conducted two-dimensional hydrodynamical simulations of the collisions of CCSNe ejecta with the companion star in an almost-equal-mass (~10 M ⊙) binary to find out possible consequences of such events. In particular we pay attention to the amount of mass removed and its dependence on the binary separation. In contrast to the previous surmise, we find that the companion mass is stripped not by momentum transfer but by shock heating. Up to 25% of the original mass can be removed for the closest separations and the removed mass decreases as M ubvpropa -4.3 with the binary separation a. By performing some experimental computations with artificially modified densities of incident ejecta, we show that if the velocity of ejecta is fixed, the density of incident ejecta is the single important parameter that actually determines the removed mass as Mub \\propto ρ ej 1.4. On the other hand, another set of simulations with modified velocities of incident ejecta demonstrate that the strength of the forward shock, which heats up the stellar material and causes the mass loss of the companion star, is actually the key parameter for the removed mass.

  6. A membrane-separator interface for mass-spectrometric analysis of blood plasma

    NASA Astrophysics Data System (ADS)

    Elizarov, A. Yu.; Gerasimov, D. G.

    2014-09-01

    We demonstrate the possibility of rapid mass-spectrometric determination of the content of anesthetic agents in blood plasma with the aid of a membrane-separator interface. The interface employs a hydrophobic selective membrane that is capable of separating various anesthetic drugs (including inhalation anesthetic sevofluran, noninhalation anesthetic thiopental, hypnotic propofol, and opioid analgesic fentanyl) from the blood plasma and introducing samples into a mass spectrometer. Analysis of the blood plasma was not accompanied by the memory effect and did not lead to membrane degradation. Results of clinical investigation of the concentration of anesthetics in the blood plasma of patients are presented.

  7. Separation of actinides using capillary extraction chromatography-inductively coupled plasma mass spectrometry.

    PubMed

    Peterson, Dominic S; Montoya, Velma M

    2009-08-01

    Trace levels of actinides have been separated on capillary extraction chromatography columns. Detection of the actinides was achieved using an inductively coupled plasma mass spectrometer, which was coupled with the extraction chromatography system. In this study, we compare 30-cm long, 4.6 mm i.d. columns to capillary columns (750 microm i.d.) with lengths from 30 cm up to 150 cm. The columns that were tested were packed with TRU resin. We were able to separate a mixture of five actinides ((232)Th, (238)U, (237)Np, (239)Pu, and (241)Am). This work has application to rapid bioassay as well as automated separations of actinide materials.

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

    PubMed

    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.

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

    PubMed

    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.

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

    USGS Publications Warehouse

    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.

  11. Application of a Plasma Mass Separator to Advanced LWR Spent Fuel Reprocessing

    SciTech Connect

    Freeman, Richard; Miller, Robert; Papay, Larry; Wagoner, John; Ahlfeld, Charles; Czerwinski, Ken

    2006-07-01

    The US Department of Energy (DOE) is investigating spent fuel reprocessing for the purposes of increasing the effective capacity of a deep geological repository, reducing the radiotoxicity of waste placed in the repository and conserving nuclear fuel resources. DOE is considering hydro-chemical processing of the spent fuel after cutting the fuel cladding and fuel dissolution in nitric acid. The front end process, known as UREX, is largely based on the PUREX process and extracts U, Tc as well as fission product gases. A number of additional processing steps have become known as UREX+. One of the steps includes a further chemical treatment of remove Cs and Sr to reduce repository heat load. Other steps include successive extraction of the actinides from residual fission products, including the lanthanides. The additional UREX+ processing renders the actinides suitable for burning as reactor fuel in an advanced reactor to convert actinides to shorter-lived fission products and to produce power. New methods for separating groups of elements by their atomic mass have been developed and can be exploited to enhance spent fuel reprocessing. These physical processes dry the waste streams so that they can be vaporized and singly ionized in plasma that is contained in longitudinal magnetic and perpendicular electric fields. Proper configuration of the fields causes the plasma to rapidly rotate and expel heavier mass ions at the center of the machine. Lower mass ions form closed orbits within the cylindrical plasma column and are transported to either end of the machine. This plasma mass separator was originally developed to reduce the mass of material that must be immobilized in borosilicate glass from DOE defense waste at former weapons production facilities. The plasma mass separator appears to be well-suited for processing the UREX raffinate and solids streams by exploiting the large atomic mass gap that exists between lanthanides (< {approx}180 amu) and actinides

  12. Comprehensive three-dimensional gas chromatography mass spectrometry separation of diesel.

    PubMed

    Wang, Frank Cheng-Yu

    2017-03-17

    Diesel, a complex hydrocarbon mixture, was examined using comprehensive two-dimensional gas chromatography (GC×GC) and a field ionization mass spectrometer (FIMS), which preferentially yields molecular ions, providing an extra dimension for component separation. Molecular ions collected at low mass resolution can be assigned an NM-class (Nominal Mass-class) value that does not completely express hydrogen deficiency. In contrast to formulae and Z-class assignments that are possible from ultrahigh mass resolution, NM-class assignments are not unambiguous; however, the separation provided by GC×GC can result in coelution of components that differ in NM-class. Hence, compounds that are unresolved by GC×GC separation can be resolved by FIMS provided they differ in mass. This technique allows for easy, automated data processing, evaluation of coelution on quantitative analysis (e.g., using FID) and the identification of additional chemical species and structures. The development of GC×GC×MS creates new opportunities to improve the ability to determine hydrocarbon composition and structure in complex petroleum and refined petroleum products.

  13. The outcome of supernovae in massive binaries; removed mass, and its separation dependence

    SciTech Connect

    Hirai, Ryosuke; Sawai, Hidetomo; Yamada, Shoichi

    2014-09-01

    The majority of massive stars are formed in binary systems. It is hence reasonable to expect that most core-collapse supernovae (CCSNe) take place in binaries and the existence of a companion star may leave some imprints in observed features. Having this in mind, we have conducted two-dimensional hydrodynamical simulations of the collisions of CCSNe ejecta with the companion star in an almost-equal-mass (∼10 M {sub ☉}) binary to find out possible consequences of such events. In particular we pay attention to the amount of mass removed and its dependence on the binary separation. In contrast to the previous surmise, we find that the companion mass is stripped not by momentum transfer but by shock heating. Up to 25% of the original mass can be removed for the closest separations and the removed mass decreases as M {sub ub}∝a {sup –4.3} with the binary separation a. By performing some experimental computations with artificially modified densities of incident ejecta, we show that if the velocity of ejecta is fixed, the density of incident ejecta is the single important parameter that actually determines the removed mass as M{sub ub}∝ρ{sub ej}{sup 1.4}. On the other hand, another set of simulations with modified velocities of incident ejecta demonstrate that the strength of the forward shock, which heats up the stellar material and causes the mass loss of the companion star, is actually the key parameter for the removed mass.

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

    SciTech Connect

    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.

  15. Ion Mobility-Mass Correlation Trend Line Separation of Glycoprotein Digests without Deglycosylation

    PubMed Central

    Li, Hongli; Bendiak, Brad; Siems, William F.; Gang, David R.; Hill, Herbert H.

    2013-01-01

    A high-throughput ion mobility mass spectrometer (IMMS) was used to rapidly separate and analyze peptides and glycopeptides derived from glycoproteins. Two glycoproteins, human α-1-acid glycoprotein and antithrombin III were digested with trypsin and subjected to electrospray traveling wave IMMS analysis. No deglycosylation steps were performed; samples were complex mixtures of peptides and glycopeptides. Peptides and glycosylated peptides with different charge states (up to 4 charges) were observed and fell on distinguishable trend lines in 2-D IMMS spectra in both positive and negative modes. The trend line separation patterns matched between both modes. Peptide sequence was identified based on the corresponding extracted mass spectra and collision induced dissociated (CID) experiments were performed for selected compounds to prove class identification. The signal-to-noise ratio of the glycopeptides was increased dramatically with ion mobility trend line separation compared to non-trend line separation, primarily due to selection of precursor ion subsets within specific mobility windows. In addition, isomeric mobility peaks were detected for specific glycopeptides. IMMS demonstrated unique capabilities and advantages for investigating and separating glycoprotein digests in this study and suggests a novel strategy for rapid glycoproteomics studies in the future. PMID:23914139

  16. Binary Cepheids: Separations and Mass Ratios in 5 M ⊙ Binaries

    NASA Astrophysics Data System (ADS)

    Evans, Nancy Evans; Bond, Howard E.; Schaefer, Gail H.; Mason, Brian D.; Karovska, Margarita; Tingle, Evan

    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 ⊙—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 ⊙. 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 ⊙ binaries have systematically shorter periods than do 1 M ⊙ 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. Based in part on observations made with the NASA/ESA Hubble Space Telescope, obtained by the Space Telescope Science Institute. STScI is operated by the Association of Universities for Research in Astronomy, Inc., under NASA contract NAS5-26555.

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

    SciTech Connect

    Evans, Nancy Remage; Karovska, Margarita; Tingle, Evan; Bond, Howard E.; Schaefer, Gail H.; Mason, Brian D. E-mail: heb11@psu.edu

    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.

  18. Structural characterization of bacterial lipopolysaccharides with mass spectrometry and on- and off-line separation techniques.

    PubMed

    Kilár, Anikó; Dörnyei, Ágnes; Kocsis, Béla

    2013-01-01

    The focus of this review is the application of mass spectrometry to the structural characterization of bacterial lipopolysaccharides (LPSs), also referred to as "endotoxins," because they elicit the strong immune response in infected organisms. Recently, a wide variety of MS-based applications have been implemented to the structure elucidation of LPS. Methodological improvements, as well as on- and off-line separation procedures, proved the versatility of mass spectrometry to study complex LPS mixtures. Special attention is given in the review to the tandem mass spectrometric methods and protocols for the analyses of lipid A, the endotoxic principle of LPS. We compare and evaluate the different ionization techniques (MALDI, ESI) in view of their use in intact R- and S-type LPS and lipid A studies. Methods for sample preparation of LPS prior to mass spectrometric analysis are also described. The direct identification of intrinsic heterogeneities of most intact LPS and lipid A preparations is a particular challenge, for which separation techniques (e.g., TLC, slab-PAGE, CE, GC, HPLC) combined with mass spectrometry are often necessary. A brief summary of these combined methodologies to profile LPS molecular species is provided.

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

    NASA Astrophysics Data System (ADS)

    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 < 15.2 mag have a 2MASS match, and that a class of supervised machine learning algorithms, support vector machines (SVM), are efficient classifiers of objects in our multicolour data set. We constructed a 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 < 16.5 mag flux limit. The all-sky 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

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

    NASA Astrophysics Data System (ADS)

    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.

  1. Design and performance of mass-produced sideband separating SIS mixers for ALMA band 4 receivers

    NASA Astrophysics Data System (ADS)

    Kojima, Takafumi; Kuroiwa, Koichi; Takahashi, Toshikazu; Fujii, Yumi; Uzawa, Yoshinori; Asayama, Shin'ichiro; Noguchi, Takashi

    2015-09-01

    We have designed and mass-produced low-noise sideband separating superconductor-insulator-superconductor (SIS) mixers for the Atacama Large Millimeter/submillimeter Array (ALMA) band 4 over the frequency range of 125-163 GHz. An integrated design was adopted for the band 4 sideband separating (2SB) mixer block because of the advantages it offers in terms of compactness, reduced testing time and lower cost. The mixer chip was designed to be robust for handling errors to avoid performance degradation caused by generation of the higher order mode in the mixer chip slot. Detailed analyses revealed its robustness and ability to ensure mass production of the 2SB mixers. Using the robust mixer design in addition to well-established waveguide technologies, all of the 2SB mixers met ALMA specifications for noise temperature and image rejection ratio.

  2. Advances in the helium-jet coupled on-line mass separator RAMA. [Recoil Atom Mass Analyzer

    SciTech Connect

    Moltz, D M; Aysto, J; Cable, M D; Parry, R F; Haustein, P E; Wouters, J M; Cerny, J

    1980-01-01

    General improvements to the on-line mass separator RAMA (Recoil Atom Mass Analyzer) have yielded a greater reliability and efficiency for some elements. A new utilitarian helium-jet chamber has been installed to facilitate quick target and degrader foil changes in addition to a new ion source holder. A higher efficiency hollow-cathode, cathode-extraction ion source, for lower melting point elements (< 1200/sup 0/C) has also been designed. Tests with the beta-delayed proton emitter /sup 37/Ca showed a factor of five increase in yield over the old hollow-cathode, anode-extraction source. A differentially-pumped-tape drive system compatible with both ..gamma..-..gamma.. and ..beta..-..gamma.. experiments has been incorporated into the general detection system. All major operating parameters will soon be monitored by a complete stand-alone microprocessor system which will eventually be upgraded to a closed-loop control system.

  3. Separation of actinides using capillary extraction chromatography-inductively coupled plasma mass spectrometry

    SciTech Connect

    Peterson, Dominic S

    2008-01-01

    Trace levels of actinides have been separated on extraction chromatography columns. Detection of the actinides was achieved using an inductively coupled plasma mass spectrometer (ICP-MS), which was coupled with the extraction chromatography system. In this study we compare 30 cm long, 4.6 mm ID columns to capillary columns (750 {micro}m ID) with lengths from 30 cm up to 150 cm. The columns that were tested were packed with TRU resin. We were able to separate a mixture of five actinides ({sup 232}Th, {sup 238}U, {sup 237}Np, {sup 239}pU, {sup 241}Am). This work has application to rapid bioassay as well as for automated separations of actinide materials.

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

    PubMed

    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.

  5. Electrochemically-Modulated Separation and Mass Spectrometric Analysis of Actinides in Difficult Matrices

    SciTech Connect

    Duckworth, Douglas C.; Liezers, Martin; Lehn, Scott A.; Douglas, Matthew

    2009-01-01

    Electrochemically-modulated separations (EMS) are a straightforward means of isolating and pre-concentrating elements for on-line mass spectrometric analysis. Elements are accumulated at electrochemical working electrodes and subsequently released into a clean carrier solution for spectroscopic analysis. EMS can employ solely aqueous chemistry and uses electrochemical redox adjustment of oxidation state to “trigger” reversible chelation / complexation. Less tractable elements (e.g., uranium and plutonium), based on redox potentials, can therefore be extracted from difficult matrices following redox adjustment and chelation with electrode chelation sites. Simply put, separation is achieved by a small voltage step that is applied to the target electrode to turn “on” or “off” the specific actinide affinity of an electrode. This separation technology employs both redox and chelation chemistry to effect highly selective accumulation of target actinides, and results in element separation, matrix elimination and analyte preconcentration. Prior studies have developed protocols and preliminary insight into EMS processes for U and Pu. U and Pu are released upon oxidation and reduction, respectively, allowing complete separation due to widely divergent redox potentials. T The coupling of EMS on-line with ICP-MS for elemental and isotopic analysis of uranium and plutonium is presented, with a focus on analytical performance metrics and applicability to safeguards and process monitoring via nondestructive analyses.

  6. Electrophoretic Separation-Mass Spectrometric Detection on Polymer Microchip Directly Integrated with a Nanospray Tip

    NASA Astrophysics Data System (ADS)

    Kitagawa, Fumihiko; Shinohara, Hidetoshi; Mizuno, Jun; Otsuka, Koji; Shoji, Shuichi

    We fabricated a polymer chip for microchip electrophoresis-mass spectrometry (MCE—MS). As a substrate material, cycloolefin polymer (COP) was selected due to its high chemical durability and easy metallization for the electrode. A COP microchip with a conventional cross-type channel configuration for the MCE separation was fabricated by hot embossing. After bonding with a rid substrate, a nano electrospray ionization (nano-ESI) tip structure for MS detection was machined directly at the opening of the separation channel end. A gold electrode to keep the electric contact for ESI was deposited around the nanospray tip by electron beam evaporation. When the voltage of 3.0 and 2.0 kV was applied to the inlet and the ESI electrode, respectively, the formation of Taylor cone and stable electrospray were observed at the channel opening. In infusion analysis of caffeine, the MS spectrum with parent mass number of 195, which accords with that of the protonated caffeine, was successfully obtained in the positive mode. Furthermore, the MCE separation and ESI-MS detection of caffeine and arginine was also successfully achieved with resolution of 1.0. Therefore, these results demonstrated that the fabricated microchip integrated with the nano-ESI tip can be employed as the MCE—ESI-MS device.

  7. Integrated Microfluidic Device for Automated Single Cell Analysis using Electrophoretic Separation and Electrospray Ionization Mass Spectrometry

    PubMed Central

    Mellors, J. Scott; Jorabchi, Kaveh; Smith, Lloyd M.; Ramsey, J. Michael

    2010-01-01

    A microfabricated fluidic device was developed for the automated real-time analysis of individual cells using capillary electrophoresis (CE) and electrospray ionization-mass spectrometry (ESI-MS). The microfluidic structure incorporates a means for rapid lysis of single cells within a free solution electrophoresis channel where cellular constituents were separated and an integrated electrospray emitter for ionization of separated components. The eluent was characterized using mass spectrometry. Human erythrocytes were used as a model system for this study. In this monolithically integrated device, cell lysis occurs at a channel intersection using a combination of rapid buffer exchange and an increase in electric field strength. An electroosmotic pump is incorporated at the end of the electrophoretic separation channel to direct eluent to the integrated electrospray emitter. The dissociated heme group and the α and β subunits of hemoglobin from individual erythrocytes were detected as cells continuously flowed through the device. The average analysis throughput was approximately 12 cells per minute demonstrating the potential of this method for high-throughput single cell analysis. PMID:20058879

  8. Charge state separation for protein applications using a quadrupole time-of-flight mass spectrometer.

    PubMed

    Chernushevich, I V; Fell, L M; Bloomfield, N; Metalnikov, P S; Loboda, A V

    2003-01-01

    A novel method for separating ions according to their charge state using a quadrupole time-of-flight mass spectrometer is presented. The benefits of charge state separation are particularly apparent in protein identification applications at low femtomole concentration levels, where in conventional TOF MS spectra peptide ions are often lost in a sea of chemical noise. When doubly and triply charged tryptic peptide ions need to be filtered from singly charged background ions, the latter are suppressed by two to three orders of magnitude, while from 10-50% of multiply charged ions remain. The suppression of chemical noise reduces the need for chromatography and can make this experimental approach the electrospray equivalent of conventional MALDI peptide maps. If unambiguous identification cannot be achieved, MS/MS experiments are performed on the precursor ions identified through charge separation, while the previously described Q2-trapping duty cycle enhancement is tuned for approximately 1.4 of the precursor m/z to enhance intensities of ions with m/z values above that of the precursor. The resulting product ion spectra contain few fragments of impurities and provide quick and unambiguous identification through database search. The multiple charge separation technique requires minimal tuning and may become a useful tool for analysis of complex mixtures.

  9. Evaluation of injection methods for fast, high peak capacity separations with low thermal mass gas chromatography.

    PubMed

    Fitz, Brian D; Mannion, Brandyn C; To, Khang; Hoac, Trinh; Synovec, Robert E

    2015-05-01

    Low thermal mass gas chromatography (LTM-GC) was evaluated for rapid, high peak capacity separations with three injection methods: liquid, headspace solid phase micro-extraction (HS-SPME), and direct vapor. An Agilent LTM equipped with a short microbore capillary column was operated at a column heating rate of 250 °C/min to produce a 60s separation. Two sets of experiments were conducted in parallel to characterize the instrumental platform. First, the three injection methods were performed in conjunction with in-house built high-speed cryo-focusing injection (HSCFI) to cryogenically trap and re-inject the analytes onto the LTM-GC column in a narrower band. Next, the three injection methods were performed natively with LTM-GC. Using HSCFI, the peak capacity of a separation of 50 nl of a 73 component liquid test mixture was 270, which was 23% higher than without HSCFI. Similar peak capacity gains were obtained when using the HSCFI with HS-SPME (25%), and even greater with vapor injection (56%). For the 100 μl vapor sample injected without HSCFI, the preconcentration factor, defined as the ratio of the maximum concentration of the detected analyte peak relative to the analyte concentration injected with the syringe, was determined to be 11 for the earliest eluting peak (most volatile analyte). In contrast, the preconcentration factor for the earliest eluting peak using HSCFI was 103. Therefore, LTM-GC is demonstrated to natively provide in situ analyte trapping, although not to as great an extent as with HSCFI. We also report the use of LTM-GC applied with time-of-flight mass spectrometry (TOFMS) detection for rapid, high peak capacity separations from SPME sampled banana peel headspace.

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

    PubMed Central

    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

  11. Separation and determination of homogenous fatty alcohol ethoxylates by liquid chromatography with mulitstage mass spectrometry.

    PubMed

    Zembrzuska, Joanna; Budnik, Irena; Lukaszewski, Zenon

    2014-07-01

    Alcohol ethoxylates (AEs) are a significant component of a stream of surfactants directed to the aquatic environment. The aim of this work was the investigation of the dependence of the analytical signals of homogeneous AE homologues on liquid chromatography with tandem mass spectrometry conditions, as well as the separation of AEs from the water matrix and, on this basis, the development of an analytical procedure suitable for the determination of AEs in environmental samples. Homogeneous homologues containing dodecyl moiety and 2-9 oxyethylene subunits were investigated. The analytical signals of the investigated homologues were optimized in terms of concentration of ammonium acetate in the mobile phase (optimum 5 mM) and a column temperature (optimum 35°C) of the liquid chromatography with tandem mass spectrometry system. A separation of AEs from the water matrix by liquid-liquid extraction (ethyl acetate, chloroform) or solid-phase extraction (C18 , styrene divinylbenzene, H-RX) was investigated. In a model investigation, the best recoveries (>90%) were obtained with a styrene divinylbenzene cartridge eluted with a 1:1 mixture of chloroform and methanol. However, much worse recoveries were obtained from the river water sample. Better results were obtained for liquid-liquid extraction with ethyl acetate. Recoveries of 62-80% were obtained for homologues having 4-9 oxyethylene subunits, at the lowest spike.

  12. Fast separation of triterpenoid saponins using supercritical fluid chromatography coupled with single quadrupole mass spectrometry.

    PubMed

    Huang, Yang; Zhang, Tingting; Zhou, Haibo; Feng, Ying; Fan, Chunlin; Chen, Weijia; Crommen, Jacques; Jiang, Zhengjin

    2016-03-20

    Triterpenoid saponins (TSs) are the most important components of some traditional Chinese medicines (TCMs) and have exhibited valuable pharmacological properties. In this study, a rapid and efficient method was developed for the separation of kudinosides, stauntosides and ginsenosides using supercritical fluid chromatography coupled with single quadrupole mass spectrometry (SFC-MS). The separation conditions for the selected TSs were carefully optimized after the initial screening of eight stationary phases. The best compromise for all compounds in terms of chromatographic performance and MS sensitivity was obtained when water (5-10%) and formic acid (0.05%) were added to the supercritical carbon dioxide/MeOH mobile phase. Beside the composition of the mobile phase, the nature of the make-up solvent for interfacing SFC with MS was also evaluated. Compared to reversed phase liquid chromatography, the SFC approach showed higher resolution and shorter running time. The developed SFC-MS methods were successfully applied to the separation and identification of TSs present in Ilex latifolia Thunb., Panax quinquefolius L. and Panax ginseng C.A. Meyer. These results suggest that this SFC-MS approach could be employed as a useful tool for the quality assessment of natural products containing TSs as active components.

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

    PubMed

    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.

  14. COMMERCIAL APPLICATION OF PLASMA MASS SEPARATION IN THE ARCHIMEDES FILTER PLANT

    SciTech Connect

    Ahlfeld, C.E.; Gilleland, J.G.; Wagoner, J.D.

    2003-02-27

    This paper describes the commercial application of an innovative plasma mass separator called the Archimedes Filter to a pre-treatment plant that can be integrated into the U.S. Department of Energy (DOE) Hanford and Savannah River Sites to significantly enhance the treatment of radioactive high-level waste. The output of the Archimedes Filter is completely compatible with existing waste immobilization processes such as vitrification and requires no new waste form to be developed. A full-geometric-scale Demonstration Filter Unit (DEMO) has been constructed and is undergoing initial testing at the Archimedes Technology Group Development Facilities in San Diego. Some of the technology and engineering development is being performed by other organizations in collaboration with Archimedes. The Commissariat a l'Energie Atomique (CEA) is developing the plasma calcination technology and all of the associated systems for AFP feed preparation. Two Russian institutes are involved in the development of the ICP torch and injector system. The Remote System Group (UT-Battelle) at ORNL is developing the remote maintenance system for the filter units. Conceptual design of the Archimedes Filter Plant (AFP) is being developed concurrently with the DEMO testing program. The AFP mission is to significantly reduce the cost and accelerate the rate of vitrification of high-level waste by separating low activity waste from the sludge removed from underground storage tanks. Mass separation is accomplished by vaporizing the sludge feed and injecting it into a partially ionized, neutral plasma. In a single pass, heavy ions are deposited near the center of the filter and light mass ions are transported by the plasma to the ends of the cylindrically-shaped vacuum vessel. Responding to the DOE programs for cost reduction and cleanup acceleration, the AFP Project is planned on an expeditious schedule that executes all phases of the project with private sector funding. The initial AFP

  15. Contribution of mass density heterogeneities to the quasigeoid-to-geoid separation

    NASA Astrophysics Data System (ADS)

    Tenzer, Robert; Hirt, Christian; Novák, Pavel; Pitoňák, Martin; Šprlák, Michal

    2016-01-01

    The geoid-to-quasigeoid separation is often computed only approximately as a function of the simple planar Bouguer gravity anomaly and the height of the computation point while disregarding the contributions of terrain geometry and anomalous topographic density as well as the sub-geoid masses. In this study we demonstrate that these contributions are significant and, therefore, should be taken into consideration when investigating the relation between the normal and orthometric heights particularly in the mountainous, polar and geologically complex regions. These contributions are evaluated by applying the spectral expressions for gravimetric forward modelling and using the EIGEN-6C4 gravity model, the Earth2014 datasets of terrain, ice thickness and inland bathymetry and the CRUST1.0 sediment and (consolidated) crustal density data. Since the global crustal density models currently available (e.g. CRUST1.0) have a limited accuracy and resolution, the comparison of individual density contributions is—for consistency—realized with a limited spectral resolution up to a spherical harmonic degree 360 (or 180). The results reveal that the topographic contribution globally varies between -0.33 and 0.57 m, with maxima in Himalaya and Tibet. The contribution of ice considerably modifies the geoid-to-quasigeoid separation over large parts of Antarctica and Greenland, where it reaches ˜ 0.2 m. The contributions of sediments and bedrock are less pronounced, with the values typically varying only within a few centimetres. These results, however, have still possibly large uncertainties due to the lack of information on the actual sediment and bedrock density. The contribution of lakes is mostly negligible; its maxima over the Laurentian Great Lakes and the Baikal Lake reach only several millimetres. The contribution of the sub-geoid masses is significant. It is everywhere negative and reaches extreme values of -4.43 m. According to our estimates, the geoid

  16. Mass Intrusion at Mount St. Helens (WA) Between 2010 and 2014 from Temporal Gravity Variations Mass Intrusion at Mount St. Helens (WA) Between 2010 and 2014 from Temporal Gravity Variations

    NASA Astrophysics Data System (ADS)

    Battaglia, M.; Lisowski, M.; Dzurisin, D.; Poland, M. P.

    2014-12-01

    Repeated high-precision gravity measurements made at Mount St. Helens (WA) have revealed systematic temporal variations in the gravity field several years after the 2004-2008 dome-building eruption. Changes in gravity with respect to a stable reference station 36 km NW of the volcano were measured at 10 sites in the summit region and at 4 sites far afield (10 to 36 km) from the summit in August 2010 and August 2012. After removing the gravity signal associated with changes in mass of the crater glacier and the local (perched) hydrothermal aquifer, the gravity field observed at sites near the volcano's summit significantly increased with respect to sites far from the summit (maximum change 146 ±7 μgal). The pattern of gravity increase is radially symmetrical, with a half-width around 3 km and a point of maximum change centered 1.5 km NW of the 2004-2008 lava dome. Inversion of residual gravity data using the same source geometry, depth and location inferred from geodetic data (a spheroidal source centered 7.5 km beneath the 2004-2008 dome) indicates a mass increase of about 1012 kg. For a reasonable magma density (~2250 kg/m3), the volume of magma intrusion beneath the summit region inferred from gravity exceeds the volume inferred from inversion of geodetic data, suggesting that magma compressibility and other processes are important aspects of magma storage at Mount St. Helens. A third survey will be completed in August 2014, and we will present results of those measurements in the context of the 2010-2012 gravity changes.

  17. A Mass Spectrometry Study of Isotope Separation in the Laser Plume

    NASA Astrophysics Data System (ADS)

    Suen, Timothy Wu

    Accurate quantification of isotope ratios is critical for both preventing the development of illicit weapons programs in nuclear safeguards and identifying the source of smuggled material in nuclear forensics. While isotope analysis has traditionally been performed by mass spectrometry, the need for in situ measurements has prompted the development of optical techniques, such as laser-induced breakdown spectroscopy (LIBS) and laser ablation molecular isotopic spectrometry (LAMIS). These optical measurements rely on laser ablation for direct solid sampling, but several past studies have suggested that the distribution of isotopes in the ablation plume is not uniform. This study seeks to characterize isotope separation in the laser plume through the use of orthogonal-acceleration time-of-flight mass spectrometry. A silver foil was ablated with a Nd:YAG at 355 nm at an energy of 50 muJ with a spot size of 71 mum, for a fluence of 1.3 J/cm2 and an irradiance of 250 MW/cm2. Flat-plate repellers were used to sample the plume, and a temporal profile of the ions was obtained by varying the time delay on the high-voltage pulse. A spatial profile along the axis of the plume was generated by changing the position of the sample, which yielded snapshots of the isotopic composition with time. In addition, the reflectron time-of-flight system was used as an energy filter in conjunction with the repellers to sample slices of the laser plasma orthogonal to the plume axis. Mass spectrometry of the plume revealed a fast ion distribution and a slow ion distribution. Measurements taken across the entire plume showed the fast 109Ag ions slightly ahead in both space and time, causing the 107Ag fraction to drop to 0.34 at 3 mus, 4 mm from the sample surface. Although measurements centered on the near side of the plume did not show isotope separation, the slow ions on the far side of the plume included much more 109Ag than 107Ag. In addition to examining the isotope content of the ablation

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

    NASA Astrophysics Data System (ADS)

    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.

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

    NASA Astrophysics Data System (ADS)

    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.

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

    DOEpatents

    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.

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

    ERIC Educational Resources Information Center

    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…

  2. Single droplet separations and surface partition coefficient measurements using laser ablation mass spectrometry

    PubMed Central

    Jorabchi, Kaveh; Smith, Lloyd M.

    2010-01-01

    Surface activity of analytes plays a significant role in many chemical and physical phenomena. We present here a mass spectrometric method to characterize surface activity and solute partitioning between bulk liquid and the gas-liquid interface in droplets. The approach employs ablation by an IR laser from the surface of a microliter droplet deposited on a stainless steel post. The ablated material is ionized for mass spectrometric analysis by either droplet charging or by post-ionization in an electrospray plume. Three areas of application have been explored using this method; 1) separations in a single droplet: continuous ablation by a series of many successive laser pulses results in faster depletion of more surface active analytes, effectively comprising a surface activity-based separation. 2) Partition coefficient measurements: droplet volume is held constant during ablation by continually replenishing lost solvent. This leads to analyte-specific ion signal decay curves that may be fitted to a model based on Langmuir adsorption isotherms and simple analytical expressions, yielding quantitative values for the analyte surface partition coefficients. 3) Studies of the relationship between surface partitioning and HPLC phase partitioning: comparisons of surface activities measured by laser desorption with retention times in reversed phase HPLC reveal that the relationship between the two partitioning processes is very sensitive to chemical structure. Poor correlation between the retention time and surface activity is also observed within a subcategory of analytes (peptides). This effect is attributed to multi-modal solute-stationary phase interactions. The laser desorption approach presented here provides direct information on analyte surface activities free from the complications encountered in chromatographic methods due to chemical structure variations. PMID:19886638

  3. Separating long-term deformation cycles and atmospheric signals at Mount St. Helens using PS-InSAR

    NASA Astrophysics Data System (ADS)

    Welch, M.

    2015-12-01

    Since its eruption in 1980, Mount St. Helens has experienced multiple inflation-deflation cycles associated with dome building eruptions. During the most recent dome-building episode, which spanned 2004 to 2008, GPS recorded the transition from pre-eruptive inflation to co-eruptive deflation and a final transition back to inflation. Such observations provide important constraints on the timing and mechanics of cyclic magma recharge and extrusion. Currently, the subtle surface deformation signal at St Helens is monitored primarily by ground based geodetic techniques like GPS. Satellite-based InSAR has the potential to substantially augment these techniques by providing spatially continuous, precise measurements of surface displacements, and may also reveal other volcanic or surficial processes too localized to be detected by ground based methods. Traditional interferometry is challenging to apply to volcanoes in the Cascades. Widespread phase decorrelation caused by persistent snow cover and dense vegetation, combined with large, elevation dependent atmospheric phase delays, mask or make deformation signals difficult to detect. By applying StaMPS, a Persistent Scatterers (PS) technique, phase decorrelation is mitigated by utilizing only the pixels with the highest, statistically derived, signal to noise ratio. However, atmospheric water vapor, which delays the radar signal, remains problematic, particularly on the volcano edifice. To assess the bias imposed by the atmosphere, we perform a series of sensitivity tests using a suite of methods including several that rely on the linear or power-law correlation of phase delay to topography and knowledge of the spatial scale of the signal. We also apply methods that calculate wet and dry phase delay from atmospheric reanalysis datasets such as ERA-Interim provided by the ECMWF. SAR data from the ERS, Envisat, and ALOS satellites, along with newer datasets, are processed with these tools to create a time series spanning

  4. Early 21st Century Area and Mass Change of Alpine Glaciers in Western Northern America

    NASA Astrophysics Data System (ADS)

    Menounos, B.; Pelto, B. M.; Fountain, A. G.; Gardner, A. S.; Beedle, M. J.; Riedel, J. L.; Marshall, S. J.; Demuth, M. N.; Vogt, R.; Pelto, M. S.; McNeil, C.; Anslow, F. S.

    2015-12-01

    Exceptionally warm, dry conditions in the Pacific Northwest and southern latitudes of western Canada commenced in 2013 and continue today. The winter of 2014/2015, for example, saw freezing levels in the Cascade Mountains rise to elevations not seen in the instrumental record. Record thin snow packs have similarly occurred for many regions with some mountains lacking any measurable snow cover at the end of the accumulation season. Our study objectives are twofold: First, we quantify recent changes in glacier area and mass and evaluate these changes against longer term records from the region. Second, we address the importance of extreme mass change events for long-term glacier fluctuations and mass change. Our data are derived from air- (LiDAR and 1-m resolution aerial photographs) and space-borne platforms (Landsat 8, WorldView) in addition to direct mass balance measurements of key glaciers throughout the region. WorldView stereo imagery is currently being acquired for select glaciers where we routinely fly LiDAR surveys. Use of varied methods for mass and area change assessment allows us to quantify methodological biases and uncertainties. Long term trends in glacier shrinkage are controlled by warming air temperatures whereas precipitation is an important factor in decadal variability. Glacier retreat, particularly in maritime environments, slowed during the period 2005-2013 relative to retreat rates observed during 1985-2005. Retreat rates for the past two years, however, have strongly accelerated. Our results from Washington, British Columbia and Southeast Alaska indicate that 2014/2015 will be a record year of glacier mass and area loss for the region.

  5. PSEUDOSTREAMERS AS THE SOURCE OF A SEPARATE CLASS OF SOLAR CORONAL MASS EJECTIONS

    SciTech Connect

    Wang, Y.-M.

    2015-04-10

    Using white-light and extreme-ultraviolet imaging observations, we confirm that pseudostreamers (streamers that separate coronal holes of the same polarity) give rise to a different type of coronal mass ejection (CME) from that associated with helmet streamers (defined as separating coronal holes of opposite polarity). Whereas helmet streamers are the source of the familiar bubble-shaped CMEs characterized by gradual acceleration and a three-part structure, pseudostreamers produce narrower, fanlike ejections with roughly constant speeds. These ejections, which are typically triggered by underlying filament eruptions or small, flaring active regions, are confined laterally and channeled outward by the like-polarity open flux that converges onto the pseudostreamer plasma sheet from both sides. In contrast, helmet streamer CMEs are centered on the relatively weak field around the heliospheric current sheet and thus undergo greater lateral expansion. Pseudostreamer ejections have a morphological resemblance to white-light jets from coronal holes; however, unlike the latter, they are not primarily driven by interchange reconnection, and tend to have larger widths (∼20°–30°), lower speeds (∼250–700 km s{sup −1}), and more complex internal structure.

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

    PubMed Central

    Xu, Qingcai; Dong, Yuliang; Zhu, Huayu; Sun, Aide

    2015-01-01

    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. PMID:26819618

  7. Analysis of mouse liver membrane proteins using multidimensional separations and tandem mass spectrometry.

    PubMed

    Wang, Zhuowei; Wang, Min; Tong, Wei

    2010-12-01

    In the field of proteomic investigation, the analysis of membrane proteins still faces many technical challenges. A fundamental question in this puzzle is how to maintain a proper solvent environment to allow the hydrophobic proteins to remain solubilized. We propose that the denaturation of membrane proteins in a highly concentrated urea solution enables them to be ionized such that ionic exchange chromatography can be employed to separate them. The membrane proteins prepared from the mouse liver were dissolved in 6M guanidine hydrochloride, 20mM Tris-HCl, pH 9.0, and loaded onto a tandem chromatography apparatus coupled with Q-Sepharose FF and Sephacryl S-200HR. These columns were able to adsorb 97.87% of the membrane protein preparations. Using a linear NaCl (0-1.0M) gradient, the bound proteins were eluted out at 0.1-1.0M NaCl, and examined by SDS-PAGE. Furthermore the protein bands underwent excision and digestion with trypsin, followed by reverse-phase chromatography for the separation of the digested peptides and ionic-trap mass spectrometry for the identification of the proteins. From the SDS-PAGE gels, the overlap between proteins from neighboring bands was only 21.34%, indicating that the anionic-size exclusion coupling chromatography efficiently separated these membrane proteins. Of a total of 392 proteins identified, 306 were membrane proteins or membrane-associated proteins. Based on the calculation of hydrophobicity, the GRAVY scores of 83 proteins are greater than, or equal to, 0.00. Taking all of this evidence together, our results revealed that this approach is satisfactory for studies on the membrane proteome from the mouse liver.

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

    SciTech Connect

    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.

  9. Integrating Mass Media Instruction: "Connecting" NIE and TV Programs for the 21st Century.

    ERIC Educational Resources Information Center

    Shapley, Barbara

    More high school students watch television regularly than read newspapers. Newspapers in Education coordinators should be involved in teaching their students critical viewing skills. The essential concepts that students need to learn are to: (1) understand what mass media and popular culture mean; (2) understand how the media shape attitudes and…

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

    NASA Astrophysics Data System (ADS)

    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.

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

    NASA Astrophysics Data System (ADS)

    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).

  12. Temporal variation of mass-wasting activity in Mount St. Helens crater, Washington, U. S. A. indicated by seismic activity

    SciTech Connect

    Mills, H.H. )

    1991-11-01

    In the crater of Mount St. Helens, formed during the eruption of 18 May 1980, thousands of rockfalls may occur in a single day, and some rock and dirty-snow avalanches have traveled more than 1 km from their source. Because most seismic activity in the crater is produced by mass wasting, the former can be used to monitor the latter. The number and amplitude of seismic events per unit time provide a generalized measure of mass-wasting activity. In this study 1-min averages of seismic amplitudes were used as an index of rockfall activity during summer and early fall. Plots of this index show the diurnal cycle of rockfall activity and establish that the peak in activity occurs in mid to late afternoon. A correlation coefficient of 0.61 was found between daily maximum temperature and average seismic amplitude, although this value increases to 0.72 if a composite temperature variable that includes the maximum temperature of 1 to 3 preceding days as well as the present day is used. Correlation with precipitation is much weaker.

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

    PubMed

    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.

  14. Multidimensional Mass Spectrometry Coupled with Separation by Polarity or Shape for the Characterization of Sugar-Based Nonionic Surfactants.

    PubMed

    Katzenmeyer, Bryan C; Hague, Shayna F; Wesdemiotis, Chrys

    2016-01-05

    Mass spectrometry (MS) and tandem mass spectrometry (MS/MS) were interfaced with ultra-performance liquid chromatography (UPLC) and ion mobility (IM) separation to characterize a complex nonionic surfactant, consisting of a methylated glucose core (glucam) conjugated with poly(ethylene oxide) (PEO(n)) branches that were partially esterified with stearic acid to form ethoxylated glucam (PEO(n)-glucam) stearates. Reverse-phase LC-MS afforded fast separation according to polarity into five major fractions. Accurate mass measurements of the ions in the mass spectra extracted from these fractions enabled conclusive identification of six components in the surfactant, including PEO(n)-glucam mono-, di-, and tristearates as well as free and esterified PEO(n) as byproducts. MS/MS experiments provided corroborating evidence for the fatty acid content in each fraction based on the number of stearic acid losses observed. With IM-MS, the total surfactant ions were separated according to charge and shape into four distinct bands. Extracted mass spectra confirmed the presence of two disaccharide stearates in the surfactant, which were undetectable by LC-MS. PEO(n)-glucam tristearates were, however, not observed upon IM-MS. Hence, LC-MS and IM-MS unveiled complementary compositional insight. With each method, certain components were particularly well separated from other ingredients (by either polarity or shape), to be detected with confidence. Consequently, combined LC-MS and IM-MS offer a superior approach for the characterization of surfactants and other amphiphilic polymers and for the differentiation of similarly composed amphiphilic blends. It is finally noteworthy that NH4(+) charges minimized chemical noise in MS mode and Li(+) charges maximized the fragmentation efficiency in MS/MS mode.

  15. The direct determination of the masses of unstable atoms with the chalk river on-line isotope separator

    NASA Astrophysics Data System (ADS)

    Sharma, K. S.; Schmeing, H.; Evans, H. C.; Hagberg, E.; Hardy, J. C.; Koslowsky, V. T.

    1989-02-01

    A new technique has been developed to measure the spacing of atomic mass doublets of radioactive isotopes directly with an on-line isotope separator. It relies not on ion detection but on observation of the specific radioactive signature of the isotopes under study. Consequently, line shapes and centroids can be determined, free of interference and with great accuracy, even if the corresponding beams strongly overlap or if they are contaminated by unwanted isobars or isomers. In particular, it is of no consequence if one or both members of the doublet are masked by stable background peaks. Doublets are peak matched as in a conventional mass spectrometer. The technique has been evaluated with beams of radioactive nuclides whose masses are known independently. Based on careful calibrations, two new mass values have been obtained: 72Br, 71 936 340 ± 430 μu and 63Ga, 62 939 570 ± 150 μu.

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

    DTIC Science & Technology

    2016-02-01

    Army Edgewood Chemical Biological Center (Aberdeen Proving Ground , MD). Samples were made at a 100 µg/mL level for analytical separation and a 22 mg/mL...AVAILABILITY STATEMENT Approved for public release; distribution is unlimited. 13. SUPPLEMENTARY NOTES 14. ABSTRACT: Chemical nerve agents such...Phenomenex; Torrance, CA) was used to separate the enantiomers for all V and G agents within 15 min. Atmospheric pressure chemical ionization mode was

  17. Inductively coupled plasma-mass spectrometry as an element-specific detector for field-flow fractionation particle separation

    USGS Publications Warehouse

    Taylor, Howard E.; Garbarino, John R.; Murphy, Deirdre M.; Beckett, Ronald

    1992-01-01

    An inductively coupled plasma-mass spectrometer was used for the quantitative measurement of trace elements In specific,submicrometer size-fraction particulates, separated by sedimentation field-flow fractionation. Fractions were collected from the eluent of the field-flow fractionation centrifuge and nebulized, with a Babington-type pneumatic nebulizer, into an argon inductively coupled plasma-mass spectrometer. Measured Ion currents were used to quantify the major, minor, and trace element composition of the size-separated colloidal (< 1-microm diameter) particulates. The composition of surface-water suspended matter collected from the Yarra and Darling rivers in Australia is presented to illustrate the usefulness of this tool for characterizing environmental materials. An adsorption experiment was performed using cadmium lon to demonstrate the utility for studying the processes of trace metal-suspended sediment interactions and contaminant transport in natural aquatic systems.

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

    PubMed

    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.

  19. Automated Sampling and Imaging of Analytes Separated on Thin-Layer Chromatography Plates Using Desorption Electrospray Ionization Mass Spectrometry

    SciTech Connect

    Van Berkel, Gary J; Kertesz, Vilmos

    2006-01-01

    Modest modifications to the atmospheric sampling capillary of a commercial electrospray mass spectrometer and upgrades to an in-house developed surface positioning control software package (HandsFree TLC/MS ) were used to enable the automated sampling and imaging of analytes on and/or within large area surface substrates using desorption electrospray ionization mass spectrometry. Sampling and imaging of rhodamine dyes separated on TLC plates were used to illustrate some of the practical applications of this system. Examples are shown for user-defined spot sampling from separated bands on a TLC plate (one or multiple spots), scanning of a complete development lane (one or multiple lanes), or imaging of analyte bands in a development lane (i.e. multiple lane scans with close spacing). The post data processing and data display aspects of the software system are also discussed.

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

    NASA Technical Reports Server (NTRS)

    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.

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

    SciTech Connect

    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, 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.

  2. Pyrolysis-gas chromatography/mass spectrometry of a coal extract and its fractions separated by planar chromatography: correlation of structural features with molecular mass

    PubMed

    Islas; Suelves; Carter; Herod; Kandiyoti

    2000-01-01

    The structural characterisation of a coal liquefaction extract and its three fractions separated by planar chromatography has been described. Size exclusion chromatography showed the molecular mass distributions to become progressively larger with decreasing mobility on the plate. UV-fluorescence spectroscopy of the fractions indicated parallel increases in the sizes of polynuclear aromatic ring systems. Analysis by probe-mass spectrometry of the 'whole' coal extract showed the expected array of small polynuclear aromatic groups extending to m/z 450. The probe mass spectra of the lightest fraction ('mobile in pyridine and acetonitrile') showed similar features, except for effects due to vacuum drying to remove solvent. In sharp contrast, the two heaviest fractions ('mobile in pyridine and immobile in acetonitrile' and 'immobile in pyridine') showed no significant ions other than those from residual NMP solvent (m/z 98 and 99). Pyrolysis-gas chromatography/mass spectrometry of these two heaviest fractions showed only traces of aromatic compounds or fragments. The aromatic pyrolysis products of these fractions were too large and involatile to pass through the GC column. The major components observed in the pyrolysis-gas chromatography/mass spectrometry of the two heavy fractions were alkanes and alkenes, ranging between C10-C25. Since none of the samples contained free alkanes, alkenes or cycloalkanes before pyrolysis, they were generated during the pyrolysis step. The shifts of UV-fluorescence spectral intensity to shorter wavelengths with decreasing size indicated by size exclusion chromatography (SEC) provide direct evidence of differences in structure with changing molecular mass. This evidence strongly suggests that species identified as being of large molecular mass in this extract sample are not composed of molecular aggregates. It remains difficult to establish whether and when it would be legitimate to invoke molecular aggregates to explain the large

  3. Dual reductive/oxidative electrochemistry/liquid chromatography/mass spectrometry: Towards peptide and protein modification, separation and identification.

    PubMed

    Büter, Lars; Frensemeier, Lisa M; Vogel, Martin; Karst, Uwe

    2017-01-06

    A new hyphenated technique based on on-line dual (oxidative and reductive) electrochemistry coupled to liquid chromatography and high resolution electrospray mass spectrometry is presented. Two liquid streams are combined, with one containing a disulfide, which is reduced to the respective thiol in an electrochemical cell based on a titanium working electrode. The other stream contains phenol, which is electrochemically activated to benzoquinone on a boron-doped diamond working electrode. Upon combination of the two streams, a Michael addition takes places, leading to the covalent coupling of thiol to quinone. In continuous flow, the reaction mixture is transferred into an injection valve and the products are separated by reversed phase liquid chromatography and detected by electrospray-high resolution mass spectrometry. Proof of concept is demonstrated for low molecular mass disulfides and peptides, but further optimization will be required in future work to achieve efficient protein labelling.

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

    USGS Publications Warehouse

    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.

  5. Non-destructive mapping of dampness and salts in degraded wall paintings in hypogeous buildings: the case of St. Clement at mass fresco in St. Clement Basilica, Rome.

    PubMed

    Di Tullio, Valeria; Proietti, Noemi; Gobbino, Marco; Capitani, Donatella; Olmi, Roberto; Priori, Saverio; Riminesi, Cristiano; Giani, Elisabetta

    2010-03-01

    As is well known, the deterioration of wall paintings due to the capillary rise of water through the walls is a very widespread problem. In this paper, a study of microclimate monitoring, unilateral nuclear magnetic resonance (NMR), and evanescent-field dielectrometry (EFD) was applied to map non-destructively, in situ, and in a quantitative way the distribution of the moisture in an ancient deteriorated wall painting of the eleventh century. Both unilateral NMR and EFD are quite new, fully portable, and non-destructive techniques, and their combination is absolutely new. The approach reported here is proposed as a new analytical protocol to afford the problem of mapping, non-destructively, the moisture in a deteriorated wall painting in a hypogeous building such as that of the second level of St. Clement Basilica, Rome (Italy), where the use of IR thermography is impaired due to the environmental conditions, and the gravimetric tests are forbidden due to the preciousness of the artifact. The moisture distribution was mapped at different depths, from the very first layers of the painted film to a depth of 2 cm. It has also been shown how the map obtained in the first layers of the artwork is affected by the environmental conditions typical of a hypogeous building, whereas the maps obtained at higher depths are representative of the moisture due to the capillary rise of water from the ground. The quantitative analysis of the moisture was performed by calibrating NMR and EFD signals with purposely prepared specimens. This study may be applied before and after performing any intervention aimed at restoring and improving the state of conservation of this type of artwork and reducing the dampness or extracting salts (driven by the variation of moisture content) and monitoring the effectiveness of the performed interventions during the time. This protocol is applicable to any type of porous material.

  6. Chemical Effects in the Separation Process of a Differential Mobility / Mass Spectrometer System

    PubMed Central

    Schneider, Bradley B.; Covey, Thomas R.; Coy, Stephen L.; Krylov, Evgeny V.; Nazarov, Erkinjon G.

    2013-01-01

    In differential mobility spectrometry (DMS, also referred to as high field asymmetric waveform ion mobility spectrometry, FAIMS), ions are separated on the basis of the difference in their mobility under high and low electric fields. The addition of polar modifiers to the gas transporting the ions through a DMS enhances the formation of clusters in a field-dependent way and thus amplifies the high and low field mobility difference resulting in increased peak capacity and separation power. Observations of the increase in mobility field dependence are consistent with a cluster formation model, also referred to as the dynamic cluster-decluster model. The uniqueness of chemical interactions that occur between an ion and cluster-forming neutrals increases the selectivity of the separation and the depression of low-field mobility relative to high-field mobility increases the compensation voltage and peak capacity. The effect of polar modifiers on the peak capacity across a broad range of chemicals has been investigated. We discuss the theoretical underpinnings which explain the observed effects. In contrast to the result from polar modifiers, we find that using mixtures of inert gases as the transport gas improve resolution by reducing peak width but has very little effect on peak capacity or selectivity. Inert gases do not cluster and thus do not reduce low field mobility relative to high-field mobility. The observed changes in the differential mobility α parameter exhibited by different classes of compounds when the transport gas contains polar modifiers or has a significant fraction of inert gas can be explained on the basis of the physical mechanisms involved in the separation processes. PMID:20121077

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

    NASA Astrophysics Data System (ADS)

    Dickel, T.; Plaß, W. R.; Ayet San Andres, S.; Ebert, J.; Geissel, H.; Haettner, E.; Hornung, C.; Miskun, I.; Pietri, S.; Purushothaman, S.; Reiter, M. P.; Rink, A.-K.; Scheidenberger, C.; Weick, H.; Dendooven, P.; Diwisch, M.; Greiner, F.; Heiße, F.; Knöbel, R.; Lippert, W.; Moore, I. D.; Pohjalainen, I.; Prochazka, A.; Ranjan, M.; Takechi, M.; Winfield, J. S.; Xu, X.

    2015-05-01

    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.

  8. Applications of ICP magnetic sector multicollector mass spectrometry to basic energy research. Final report for period December 1st, 1993 - May 31st, 2000

    SciTech Connect

    Halliday, A.N.

    2002-05-01

    The primary aims of this research were threefold: to develop and utilize the new technique of multiple collector inductively coupled plasma mass spectrometry and apply it to problems in the earth, ocean, and environmental sciences; to develop new chronometers and improve existing chronometers to allow the accurate determination of the ages of geological features and processes; and to study natural fluid-mediated mass transfer processes and source of components in the crust and the oceans. This technique has now become the preferred method for the determination of the isotopic compositions of a variety of elements in the periodic table. The prototype instrument was used to explore a vast array of isotopic systems and demonstrate applicability to problems as different as the origin of the solar system and smelting methods in the Bronze Age. Highlights of the program are briefly summarized under the following topics: tungsten isotopes and the early solar system; trace siderophile and chalcophile element geochemistry; hafnium isotopes and the early development of the continents; evolution of lead isotopic compositions of the oceans; the isotopic composition and residence time of Hf in seawater; the isotopic compositions of Sr, Hf, Pb, and Nd in dust; U-Th disequilibrium dating of carbonates and soils; in situ U-Th disequilibrium dating of opal.

  9. Thermal-Neutron-Induced Fission of 243Cm: Light-Peak Data from the Lohengrin Mass Separator

    SciTech Connect

    Tsekhanovich, I.; Simpson, G.S.; Varapai, N.; Rochman, D.; Sokolov, V.; Fioni, G.; Al Mahamid, Ilham

    2005-05-24

    Thermal-neutron-induced fission of 243Cm was studied at the Lohengrin mass separator. The light-mass peak of the fission-yield curve was investigated, and mass (from A=72 to A=120) and independent-product (for Z=28-37) yields were obtained. A comparison was made of the results obtained on the mass yields with those from the fission of 245Cm as well as with the data given by the JEF-2.2 and ENDF/B-VI libraries. The yield of masses in the superasymmetric region was found to be identical to other fission reactions studied at Lohengrin. Experimental fission-product yields from the fission of 243Cm and 245Cm were able to be well described within a theoretical model, which incorporates standard and superasymmetric fission modes as well as a calculation of the charge-distribution parameters in isobaric chains and neutron multiplicities from primary fragments. A prediction of the yield of Ni isotopes in the fission of 243,245,247Cm was made.

  10. Targeted high-resolution ion mobility separation coupled to ultrahigh-resolution mass spectrometry of endocrine disruptors in complex mixtures.

    PubMed

    Benigni, Paolo; Thompson, Christopher J; Ridgeway, Mark E; Park, Melvin A; Fernandez-Lima, Francisco

    2015-04-21

    Traditional separation and detection of targeted compounds from complex mixtures from environmental matrices requires the use of lengthy prefractionation steps and high-resolution mass analyzers due to the large number of chemical components and their large structural diversity (highly isomeric). In the present work, selected accumulation trapped ion mobility spectrometry (SA-TIMS) is coupled to Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS) for direct separation and characterization of targeted endocrine-disrupting compounds (EDC) from a complex environmental matrix in a single analysis. In particular, targeted identification based on high-resolution mobility (R ∼ 70-120) and ultrahigh-resolution mass measurements (R > 400 000) of seven commonly targeted EDC and their isobars (e.g., bisphenol A, (Z)- and (E)-diethylstilbestrol, hexestrol, estrone, α-estradiol, and 17-ethynylestradiol) is shown from a complex mixture of water-soluble organic matter (e.g., Suwannee River Fulvic Acid Standard II) complemented with reference standard measurements and theoretical calculations (<3% error).

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

    NASA Astrophysics Data System (ADS)

    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.

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

    PubMed

    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.

  13. Fast separation and analysis of reduced monoclonal antibodies with capillary zone electrophoresis coupled to mass spectrometry.

    PubMed

    Zhao, Yimeng; Sun, Liangliang; Knierman, Michael D; Dovichi, Norman J

    2016-02-01

    Capillary zone electrophoresis-electrospray ionization-mass spectrometry (CZE-ESI-MS) was used for analysis of reduced antibodies. We first developed a simple protocol to condition commercial linear-polyacrylamide coated capillaries for use in top-down proteomics. We then suspended reduced antibodies in a solution of 35% acetic acid, 50% acetonitrile in water. Heavy and light chains were baseline resolved within 10 min and with 3-30 µg/mL detection limits using a 0.1% aqueous formic acid background electrolyte. Quintuplicate runs of a two-antibody mixture produced relative standard deviations of ∼1% in migration time and 10% in peak amplitudes. Resolution was further improved for the two-antibody mixture by using 5% acetic acid as the background electrolyte, highlighting the potential of capillary electrophoresis-mass spectrometry for analysis of antibody mixtures.

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

    NASA Astrophysics Data System (ADS)

    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.

  15. Recent advances in enrichment and separation strategies for mass spectrometry-based phosphoproteomics

    PubMed Central

    Yang, Chenxi; Zhong, Xuefei; Li, Lingjun

    2016-01-01

    Due to the significance of protein phosphorylation in various biological processes and signaling events, new analytical techniques for enhanced phosphoproteomics have been rapidly introduced in recent years. The combinatorial use of the phospho-specific enrichment techniques and prefractionation methods prior to MS analysis enables comprehensive profiling of the phosphoproteome and facilitates deciphering the critical roles that phosphorylation plays in signaling pathways in various biological systems. This review places special emphasis on the recent five-year (2009–2013) advances for enrichment and separation techniques that have been utilized for phosphopeptides prior to MS analysis. PMID:24687451

  16. Separation of cis and trans Isomers of Polyproline by FAIMS Mass Spectrometry

    NASA Astrophysics Data System (ADS)

    Creese, Andrew J.; Cooper, Helen J.

    2016-12-01

    High field asymmetric waveform ion mobility spectrometry (FAIMS) is well-established as a tool for separating peptide isomers (sequence inversions and post-translationally modified localization variants). Here, we demonstrate the FAIMS is able to differentiate cis and trans isomers of polyproline. Polyproline assumes an all- cis conformation—the PPI helix—in 1-propanol, and an all- trans conformation—the PPII helix—in aqueous solutions. Differentiation of these conformers may be achieved both through use of a cylindrical FAIMS device and a miniaturized ultrahigh field planar FAIMS device.

  17. Metabonomics study of liver cancer based on ultra performance liquid chromatography coupled to mass spectrometry with HILIC and RPLC separations.

    PubMed

    Chen, Jing; Wang, Wenzhao; Lv, Shen; Yin, Peiyuan; Zhao, Xinjie; Lu, Xin; Zhang, Fengxia; Xu, Guowang

    2009-09-14

    In this study, urinary metabolites from liver cancer patients and healthy volunteers were studied by a metabonomic method based on ultra performance liquid chromatography coupled to mass spectrometry. Both hydrophilic interaction chromatography (HILIC) and reversed-phase liquid chromatography (RPLC) were used to separate the urinary metabolites. Principle component analysis (PCA) and partial least squares to latent structure-discriminant analysis (PLS-DA) models were built to separate the healthy volunteers from the liver cancer patients and to find compounds that are expressed in significantly different amounts between the two populations. 21 metabolite ions were considered as potential biomarkers according to the Variable importance in the Project (VIP) value and S-plot. Compared with RPLC, a more sensitive and stable response can be recorded in HILIC mode due to the high content of organic solvent used. Moreover, the liver cancer group and the healthy volunteers can be better separated based on the data from the HILIC separation, which indicates that HILIC is suitable for urinary metabonomic analysis. In HILIC mode, several polar compounds related to arginine and proline metabolism, alanine and aspartate metabolism, lysine degradation, nicotinate and nicotinamide metabolism were found to be significantly changed in the concentrations of the two different populations: healthy and cancer. In contrast, in RPLC mode, these changed compounds are related to fatty acids oxidation.

  18. Size, separation, structural order, and mass density of molecules packing in water and ice.

    PubMed

    Huang, Yongli; Zhang, Xi; Ma, Zengsheng; Li, Wen; Zhou, Yichun; Zhou, Ji; Zheng, Weitao; Sun, Chang Q

    2013-10-21

    The structural symmetry and molecular separation in water and ice remain uncertain. We present herewith a solution to unifying the density, the structure order and symmetry, the size (H-O length dH), and the separation (d(OO) = d(L) + d(H) or the O:H length d(L)) of molecules packing in water and ice in terms of statistic mean. This solution reconciles: i) the d(L) and the d(H) symmetrization of the O:H-O bond in compressed ice, ii) the d(OO) relaxation of cooling water and ice and, iii) the d(OO) expansion of a dimer and between molecules at water surface. With any one of the d(OO), the density ρ(g·cm⁻³), the d(L), and the d(H), as a known input, one can resolve the rest quantities using this solution that is probing conditions or methods independent. We clarified that: i) liquid water prefers statistically the mono-phase of tetrahedrally-coordinated structure with fluctuation, ii) the low-density phase (supersolid phase as it is strongly polarized with even lower density) exists only in regions consisting molecules with fewer than four neighbors and, iii) repulsion between electron pairs on adjacent oxygen atoms dictates the cooperative relaxation of the segmented O:H-O bond, which is responsible for the performance of water and ice.

  19. Control of Chemical Effects in the Separation Process of a Differential Mobility / Mass Spectrometer System

    PubMed Central

    Schneider, Bradley B.; Coy, Stephen L.; Krylov, Evgeny V.; Nazarov, Erkinjon G.

    2013-01-01

    Differential mobility spectrometry (DMS) separates ions on the basis of the difference in their migration rates under high versus low electric fields. Several models describing the physical nature of this field mobility dependence have been proposed but emerging as a dominant effect is the clusterization model sometimes referred to as the dynamic cluster-decluster model. DMS resolution and peak capacity is strongly influenced by the addition of modifiers which results in the formation and dissociation of clusters. This process increases selectivity due to the unique chemical interactions that occur between an ion and neutral gas phase molecules. It is thus imperative to bring the parameters influencing the chemical interactions under control and find ways to exploit them in order to improve the analytical utility of the device. In this paper we describe three important areas that need consideration in order to stabilize and capitalize on the chemical processes that dominate a DMS separation. The first involves means of controlling the dynamic equilibrium of the clustering reactions with high concentrations of specific reagents. The second area involves a means to deal with the unwanted heterogeneous cluster ion populations emitted from the electrospray ionization process that degrade resolution and sensitivity. The third involves fine control of parameters that affect the fundamental collision processes, temperature and pressure. PMID:20065515

  20. Rapid chiral separation of racemic cetirizine in human plasma using subcritical fluid chromatography-tandem mass spectrometry.

    PubMed

    Eom, Han Young; Kang, Myunghee; Kang, Seung Woo; Kim, Unyong; Suh, Joon Hyuk; Kim, Junghyun; Cho, Hyun-Deok; Jung, Yura; Yang, Dong-Hyug; Han, Sang Beom

    2016-01-05

    A method for fast chiral separation of cetirizine and quantitation of levocetirizine in human plasma using subcritical fluid chromatography with tandem mass spectrometry was developed and validated. The chromatographic separation was performed using a Chiralpak IE column (2.1 mm×150 mm, 5 μm) with an isocratic elution of CO2/organic modifier (55/45, v/v) at a flow rate of 0.85 mL/min. The organic modifier was composed of water/methanol (5/95, v/v). The makeup flow was optimized at water/methanol (10/90, v/v) and 0.2 mL/min. The most influential parameters on the separation of cetirizine affecting resolution, retention time and sensitivity were selected by fractional factorial design. The 3 selected factors were optimized by response surface methodology. Tandem mass spectrometry was used at electrospray ionization, positive ion mode, and multiple-reaction monitoring mode. Isotope-labeled cetirizine-d4 was used as the internal standard. The sample preparation of human plasma was conducted by solid phase extraction of hydrophilic-lipophilic balance (HLB) type. The developed method was validated for selectivity, linearity, precision, accuracy, recovery, limit of quantitation (LOQ), and limit of detection (LOD). The real human plasma samples were analyzed and the pharmacokinetic results were compared with results of previous research. The developed method was found to be reliable based on the similarity between the results of the current and previous methods. The chiral separation for cetirizine and economic feasibility were compared with those of previous studies using normal phase-HPLC or reversed phase-HPLC. The established analytical method could be successfully applied to pharmacokinetic study with reduction in the analysis time and costs.

  1. Bifunctional glass membrane designed to interface SDS-PAGE separations of proteins with the detection of peptides by mass spectrometry.

    PubMed

    Hattan, Stephen J; Du, Jie; Parker, Kenneth C

    2015-04-07

    We describe the construction and characterization of a novel membrane designed to allow proteins separated by gel electrophoresis (SDS-PAGE) to be detected as peptides by mass spectrometry in an efficient and comprehensive manner. The key attribute of the membrane is a bifunctional design that allows for the digestion of protein(s) and retention of the resulting peptides with minimal lateral diffusion. Silane chemistries are used to differentially treat the opposing surfaces of a glass filter paper to enable this unique capability.

  2. Mass losses from Svalbard land-terminating glaciers by the end of the 21st century under an RCP 8.5 scenario

    NASA Astrophysics Data System (ADS)

    Möller, Marco; Navarro, Francisco; Martín-Español, Alba

    2016-04-01

    The high Arctic archipelagos are among the most strongly glacierized landscapes on earth apart from the Greenland and Antarctic ice sheets. Svalbard, one of these archipelagos, holds about 36,000 km2 of glaciers and ice caps and is the region that has shown the least negative mass balance of all the high Arctic regions. However, future projections suggest that the archipelago will experience an unprecedented -for the Arctic- glacier recession over the 21st century. We here present a high-resolution modelling study of the future ice-mass evolution of 29 individual land-terminating glaciers on the Svalbard archipelago under an RCP 8.5 climate forcing, a rather pessimistic scenario that unfortunately seems to be becoming realistic. Our model calculates glacier mass balance and area/volume changes using a temperature-index approach in combination with a surface elevation change parameterization. The initial glacier topographies and volumes have been assessed from extensive ground-penetrating radar measurements carried out in recent years. The calculations are performed for the 21st century and are forced by statistically downscaled output of ten different global circulation models representing the RCP scenario 8.5. By a topography-based extrapolation of the simulation results to the entire archipelago we show that a complete loss of most of Svalbard's land-terminating glaciers and even a deglaciation of certain subregions of the archipelago might occur by the end of the 21st century. 98% of the land-terminating glaciers will have retreated to less than one tenth of their initial extent by 2100, resulting in a loss of 7392±2481 km2 of ice coverage.

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

    PubMed

    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.

  4. Mass transfer limitations in protein separations using ion-exchange membranes.

    PubMed

    Sarfert, F T; Etzel, M R

    1997-03-07

    Sorption of bovine serum albumin to commercial 150-micron pore size membranes was measured in batch and flow experiments. For residence times of 2-40 min, early and broad breakthrough curves and broad asymmetric elution peaks were observed that depended strongly on flow-rate. System dispersion could not explain the flow-rate dependence. Breakthrough and elution curves were analyzed using new models that included Langmuir sorption, convection and diffusion. From the analysis, film mass transfer resistance was found to be the rate-limiting factor. The maximum allowable pore size that eliminates this limitation was calculated for different molecular weight solutes.

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

    PubMed

    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.

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

    NASA Astrophysics Data System (ADS)

    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

  7. Enantiomeric separation in comprehensive two-dimensional gas chromatography with accurate mass analysis.

    PubMed

    Chin, Sung-Tong; Nolvachai, Yada; Marriott, Philip J

    2014-11-01

    Chiral comprehensive two-dimensional gas chromatography (eGC×GC) coupled to quadrupole-accurate mass time-of-flight mass spectrometry (QTOFMS) was evaluated for its capability to report the chiral composition of several monoterpenes, namely, α-pinene, β-pinene, and limonene in cardamom oil. Enantiomers in a standard mixture were fully resolved by direct enantiomeric-GC analysis with a 2,3-di-O-methyl-6-t-butylsilyl derivatized β-cyclodextrin phase; however, the (+)-(R)-limonene enantiomer in cardamom oil was overlapped with other background components including cymene and cineole. Verification of (+)-(R)-limonene components based on characteristic ions at m/z 136, 121, and 107 acquired by chiral single-dimension GC-QTOFMS in the alternate MS/MSMS mode of operation was unsuccessful due to similar parent/daughter ions generated by interfering or co-eluting cymene and cineole. Column phases SUPELCOWAX, SLB-IL111, HP-88, and SLB-IL59, were incorporated as the second dimension column ((2)D) in chiral GC×GC analysis; the SLB-IL59 offered the best resolution for the tested monoterpene enantiomers from the matrix background. Enantiomeric ratios for α-pinene, β-pinene, and limonene were determined to be 1.325, 2.703, and 1.040, respectively, in the cardamom oil sample based on relative peak area data.

  8. Simultaneous chiral separation of methylamphetamine and common precursors using gas chromatography/mass spectrometry.

    PubMed

    Drake, Samantha J; Morrison, Calum; Smith, Frank

    2011-09-01

    Methylamphetamine, ephedrine, and pseudoephedrine were derivatized using trifluoroacetic anhydride and enantiomers of each were analyzed using gas chromatography coupled to mass spectrometry (GC/MS) fitted with a γ-cyclodextrin (Chiraldex™ G-PN) chiral column. A temperature-programmed method was developed and optimized and the results compared with those obtained using a previously published isothermal GC method applied to GC/MS analysis. Trifluoroacetylated 3-(trifluoromethyl)phenethylamine hydrochloride was used as an internal standard, and mass fragmentation patterns are proposed for all derivatives analyzed. Qualitative validation of the optimized chromatographic conditions was completed in accordance with the guidelines published by the United Nations Office on Drugs and Crime (UNODC). Under conditions of repeatability and reproducibility, the method gave relative retention times with a relative standard deviation of less than 0.02% for all six analytes of interest. This surpasses the UNODC's acceptance criteria of 2% for validation of qualitative precision. Ephedrine and pseudoephedrine are common precursors in the clandestine manufacture of methylamphetamine. Seizures of illicit methylamphetamine therefore often contain mixtures of these optically active compounds. The simultaneous enantioseparation of these compounds to produce a profile would provide valuable information to law enforcement agencies regarding the provenance of a methylamphetamine seizure.

  9. Enhancing Biological Analyses with Three Dimensional Field Asymmetric Ion Mobility, Low Field Drift Tube Ion Mobility and Mass Spectrometry (μFAIMS/IMS-MS) Separations

    PubMed Central

    Zhang, Xing; Ibrahim, Yehia M.; Chen, Tsung-Chi; Kyle, Jennifer E.; Norheim, Randolph V.; Monroe, Matthew E.; Smith, Richard D.; Baker, Erin S.

    2015-01-01

    Multidimensional high throughput separations are ideal for analyzing distinct ion characteristics simultaneously in one analysis. We report on the first evaluation of a platform coupling a high speed field asymmetric ion mobility spectrometry microchip (μFAIMS) with drift tube ion mobility and mass spectrometry (IMS-MS). The μFAIMS/IMS-MS platform was used to analyze biological samples and simultaneously acquire multidimensional FAIMS compensation fields, IMS drift times, and accurate ion masses for the detected features. These separations thereby increased the overall measurement separation power, resulting in greater information content and more complete characterization of the complex samples. The separation conditions were optimized for sensitivity and resolving power by the selection of gas compositions and pressures in the FAIMS and IMS separation stages. The resulting performance provided three dimensional separations, benefitting both broad complex mixture studies and targeted analyses by improving isomeric separations and allowing detection of species obscured by interfering peaks. PMID:26140287

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

    PubMed

    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

  11. Advances in sample preparation in electromigration, chromatographic and mass spectrometric separation methods.

    PubMed

    Gilar, M; Bouvier, E S; Compton, B J

    2001-02-16

    The quality of sample preparation is a key factor in determining the success of analysis. While analysis of pharmaceutically important compounds in biological matrixes has driven forward the development of sample clean-up procedures in last 20 years, today's chemists face an additional challenge: sample preparation and analysis of complex biochemical samples for characterization of genotypic or phenotypic information contained in DNA and proteins. This review focuses on various sample pretreatment methods designed to meet the requirements for the analysis of biopolymers and small drugs in complex matrices. We discuss the advances in development of solid-phase extraction (SPE) sorbents, on-line SPE, membrane-based sample preparation, and sample clean-up of biopolymers prior to their analysis by mass spectrometry.

  12. Application of mass-separated focused ion beams in nano-technology

    NASA Astrophysics Data System (ADS)

    Bischoff, L.

    2008-04-01

    FIB applications like writing ion implantation, ion beam mixing or ion beam synthesis in the μm- or nm range often require ion species other than gallium. Therefore alloy liquid metal ion sources (LMIS) have to be developed and applied in FIB tools. The energy distribution of ions emitted from an alloy LMIS is one of the crucial parameters for the performance of a FIB column. Different source materials like AuGe, AuSi, AuGeSi, CoNd, ErNi, ErFeNiCr, MnGe, GaBi, GaBiLi, SnPb, … were investigated with respect to the energy spread of the different ion species as a function of emission current, ion mass and emitter temperature. Different alloy LMIS's have been developed and used in the FZD - FIB system especially for writing implantation to fabricate sub-μm pattern without any lithographic steps. Co and various other ion species were applied to generate CoSi2 nano-structures, like dots and wires by ion beam synthesis or to manipulate the properties of magnetic films. Additionally, the possibility of varying the flux in the FIB by changing the pixel dwell-time can be used for the investigation of the radiation damage and dynamic annealing in Si, Ge and SiC at elevated implantation temperatures. Furthermore, a broad spectrum of ions was employed to study in a fast manner the sputtering process depending on temperature, angle of incidence and ion mass on a couple of target materials. These studies are important for the 3D-fabrication of various kinds of micro-tools by FIB milling.

  13. Identification of human myocardial proteins separated by two-dimensional electrophoresis using an effective sample preparation for mass spectrometry.

    PubMed

    Otto, A; Thiede, B; Müller, E C; Scheler, C; Wittmann-Liebold, B; Jungblut, P

    1996-10-01

    Peptide mass fingerprinting is a powerful tool for the identification of proteins separated by two-dimensional gel electrophoresis (2-DE). The identification of in-gel digested proteins by peptide mass fingerprinting was significantly improve in comparison to blot-digests by using a peptide-collecting device. This device allows the effective purification and concentration of enzymatic digests of low-intensity spots without expensive equipment and is described in detail. Sensitivity in the fmol range was demonstrated by unequivocal identification of bovine serum albumin after sodium dodecyl sulfate--polyacrylamide gel electrophoresis. Furthermore the high performance liquid chromatography pattern of in-gel digests indicated a 2- to 3-fold higher yield of the separated peptides. Therefore, a higher amount of the peptides was available to perform N-terminal sequencing. The identification of 16 proteins from a high-resolution 2-DE gel map of human myocardium tissue has been achieved by means of this technique. Three of these proteins were associated with changes in spot intensity with dilated cardiomyopathy.

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

    NASA Astrophysics Data System (ADS)

    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.

  15. Capillary electrochromatography and capillary electrochromatography-electrospray mass spectrometry for the separation of non-steroidal anti-inflammatory drugs.

    PubMed

    Desiderio, C; Fanali, S

    2000-10-20

    In this study capillary electrochromatography (CEC) was utilized for the separation of ten non-steroidal anti-inflammatory drugs (NSAIDs). Experiments were carried out in a commercially available CE instrument using a packed capillary with RP-18 silica particles where the stationary phase completely filled the capillary. The mobile phase consisted of a mixture of ammonium formate buffer pH 2.5 and acetonitrile. Selectivity and resolution were studied changing the pH and the concentration of the buffer, the acetonitrile content mobile phase and the capillary temperature. The optimum experimental conditions for CEC separation of the studied drug mixture were found using 50 mM ammonium formate pH 2.5-acetonitrile (40:60) at 25 degrees C. The CEC capillary was coupled to an electrospray mass spectrometer for the characterization of the NSAIDs. A mobile phase composed by the same buffer but with a higher concentration of acetonitrile (90%) was used in order to speed up the separation of analytes.

  16. Determination of heavy metals by inductively coupled plasma mass spectrometry after on-line separation and preconcentration

    NASA Astrophysics Data System (ADS)

    Dressler, Valderi L.; Pozebon, Dirce; Curtius, Adilson J.

    1998-10-01

    A method for the determination of Cu, As, Se, Cd, In, Hg, Tl, Pb and Bi in waters and in biological materials by inductively coupled plasma mass spectrometry, after an on-line separation, is described. The matrix separation and analyte preconcentration is accomplished by retention of the analytes complexed with the ammonium salt of O,O-diethyl dithiophosphoric acid in a HNO 3 solution on C 18 immobilized on silica in a minicolumn. Methanol, as eluent, is introduced in the conventional pneumatic nebulizer of the instrument. In order to use the best compromise conditions, concerning the ligand and acid concentrations, the analytes were determined in two separate groups. The enrichment factors were in the range from 5 to 61, depending on the analyte. The limits of detection varied from 0.43 ng L -1 for Bi to 33 ng L -1 for Cu. The sample consumption is only 2.3 mL for each group and the sampling frequency is 21 h -1. The accuracy was tested by analysing five certified reference materials: water, riverine water, urine, bovine muscle and bovine liver. The agreement between obtained and certified concentrations was very good, except for As. The relatively small volume of methanol, used as eluent, minimizes the problems produced by the introduction of organic solvent into the plasma.

  17. Surface-induced dissociation of ion mobility-separated noncovalent complexes in a quadrupole/time-of-flight mass spectrometer.

    PubMed

    Zhou, Mowei; Huang, Chengsi; Wysocki, Vicki H

    2012-07-17

    A custom in-line surface-induced dissociation (SID) device has been incorporated into a commercial ion mobility quadrupole/time-of-flight mass spectrometer in order to provide an alternative and potentially more informative activation method than the commonly used collision-induced dissociation (CID). Complicated sample mixtures can be fractionated by ion mobility (IM) and then dissociated by CID or SID for further structural analysis. Interpretation of SID spectra for cesium iodide clusters was greatly simplified with IM prior to dissociation because products originating from different precursors and overlapping in m/z but separated in drift time can be examined individually. Multiple conformations of two protein complexes, source-activated transthyretin tetramer and nativelike serum amyloid P decamer, were separated in ion mobility and subjected to CID and SID. CID spectra of the mobility separated conformations are similar. However, drastic differences can be observed for SID spectra of different conformations, implying different structures in the gas phase. This work highlights the potential of utilizing IM-SID to study quaternary structures of protein complexes and provides information that is complementary to our recently reported SID-IM approach.

  18. Simultaneous speciation of selenium and arsenic using elevated temperature liquid chromatography separation with inductively coupled plasma mass spectrometry detection

    NASA Astrophysics Data System (ADS)

    Le, X. C.; Li, X.-F.; Lai, V.; Ma, M.; Yalcin, S.; Feldmann, J.

    1998-08-01

    A method was developed for the simultaneous speciation of both arsenic and selenium based on the separation of arsenic and selenium species using high performance liquid chromatography (HPLC) under elevated column temperatures followed by dual-element detection using inductively coupled plasma mass spectrometry (ICPMS). Thirteen arsenic and selenium species, including arsenate, arsenite, monomethylarsonic acid, dimethylarsinic acid, arsenobetaine, arsenocholine, tetramethylarsonium, two arsenosugars, selenate, selenite, selenocystine and selenomethionine, were studied using this approach. The HPLC separation using 70°C constant column temperature resulted in an improved resolution and faster separation of arsenic and selenium species. Nearly baseline resolution of these species was achieved on a reversed phase C18 column using hexanesulfonate as an ion pair reagent. The ICPMS detection of m/ z 75, 77 and 78 enabled simultaneous monitoring of arsenic, selenium, and potential interfering species, such as ArCl. An application of the HPLC/ICPMS technique was demonstrated by the speciation of arsenic and selenium in canned tuna fish. Arsenobetaine and selenocystine were detected as the major arsenic and selenium species, respectively. The technique was also applied to a study on the metabolism of arsenosugars. Speciation of six arsenosugar metabolites in human urine was complete in 19 min at 70°C column temperature, compared to 37 min at room temperature.

  19. Rapid sequential separation of essential oil compounds using continuous heart-cut multi-dimensional gas chromatography-mass spectrometry.

    PubMed

    Yang, Seung-Ok; Kim, Yujin; Kim, Hee-su; Hyun, Sun-Hee; Kim, So-Hyun; Choi, Hyung-Kyoon; Marriott, Philip J

    2011-05-06

    A method for separation and identification of peaks in essential oil samples based on rapid repetitive heart-cutting using multidimensional gas chromatography (MDGC)-mass spectrometry (MS) coupled with a cryotrapping interface is described. Lavender essential oil is analyzed by employing repetitive heart-cut intervals of 1.00 and 1.50 min, achieved in a parallel MDGC-MS/GC-FID experiment. The number of peaks that were detected in 1D GC operation above a given response threshold more than tripled when MDGC-MS employing the cryotrapping module method was used. In addition, MDGC-MS enabled detection of peaks that were not individually evident in 1D GC-MS, owing to effective deconvolution in time of previously overlapped peaks in 1D GC. Thus separation using the cryomodulation approach, without recourse to using deconvolution software, was possible. Peaks widths decreased by about 5-7-fold with the described method, peak capacity increased from about 9 per min to 60 per min, and greater sensitivity results. Repeatability of retention times for replicate analyses in the multidimensional mode was better than 0.02% RSD. The present study suggests that the described heart-cutting technique using MDGC-MS can be used for general improvement in separation and identification of volatile compounds.

  20. INVESTIGATION OF THE FORMATION AND SEPARATION OF AN EXTREME-ULTRAVIOLET WAVE FROM THE EXPANSION OF A CORONAL MASS EJECTION

    SciTech Connect

    Cheng, X.; Ding, M. D.; Zhang, J.; Olmedo, O.; Vourlidas, A.; Liu, Y. E-mail: jzhang7@gmu.edu

    2012-01-20

    We address the nature of EUV waves through direct observations of the formation of a diffuse wave driven by the expansion of a coronal mass ejection (CME) and its subsequent separation from the CME front. The wave and the CME on 2011 June 7 were well observed by the Atmospheric Imaging Assembly on board the Solar Dynamics Observatory. Following the solar eruption onset, marked by the beginning of the rapid increasing of the CME velocity and the X-ray flux of accompanying flare, the CME exhibits a strong lateral expansion. During this impulsive expansion phase, the expansion speed of the CME bubble increases from 100 km s{sup -1} to 450 km s{sup -1} in only six minutes. An important finding is that a diffuse wave front starts to separate from the front of the expanding bubble shortly after the lateral expansion slows down. Also a type II burst is formed near the time of the separation. After the separation, two distinct fronts propagate with different kinematic properties. The diffuse front travels across the entire solar disk, while the sharp front rises up, forming the CME ejecta with the diffuse front ahead of it. These observations suggest that the previously termed EUV wave is a composite phenomenon and driven by the CME expansion. While the CME expansion is accelerating, the wave front is cospatial with the CME front, thus the two fronts are indiscernible. Following the end of the acceleration phase, the wave moves away from the CME front with a gradually increasing distance between them.

  1. Stereoselective separation and pharmacokinetic dissipation of the chiral neonicotinoid sulfoxaflor in soil by ultraperformance convergence chromatography/tandem mass spectrometry.

    PubMed

    Chen, Zenglong; Dong, Fengshou; Xu, Jun; Liu, Xingang; Cheng, Youpu; Liu, Na; Tao, Yan; Pan, Xinglu; Zheng, Yongquan

    2014-10-01

    Ultraperformance convergence chromatography/tandem triple quadrupole mass spectrometry (UPC(2)-MS/MS) is a novel tool in separation science that combines the advantages of supercritical fluid chromatography with ultraperformance liquid chromatography/MS/MS technology. The use of nontoxic CO2 fluid and a postcolumn additive to complement MS/MS allows better control of analyte retention for chiral separation and high-sensitivity determination with different chiral stationary phases. This paper reports the stereoselective separation and determination of the chiral neonicotinoid sulfoxaflor in vegetables and soil by UPC(2)-MS/MS. Baseline resolution (Rs ≥ 1.56) of and high selectivity (LOQ ≤ 1.83 μg/kg) for the four stereoisomers were achieved by postcolumn addition of 1 % formic acid-methanol to a Chiralpak IA-3 using CO₂/isopropanol/acetonitrile as the mobile phase at 40 °C, 2,500 psi, and for 6.5 min in electrospray ionization positive mode. Rearranged Van't Hoff equations afforded the thermodynamic parameters ΔH (ο) and ΔS (ο), which were analyzed to promote understanding of the enthalpy-driven separation of sulfoxaflor stereoisomers. The interday mean recovery, intraday repeatability, and interday reproducibility varied from 72.9 to 103.7%, from 1.8 to 9.2%, and from 3.1 to 9.4%, respectively. The proposed method was used to study the pharmacokinetic dissipation of sulfoxaflor stereoisomers in soil under greenhouse conditions. The estimated half-life ranged from 5.59 to 6.03 d, and statistically nonsignificant enantioselective degradation was observed. This study not only demonstrates that the UPC(2)-MS/MS system is an efficient and sensitive method for sulfoxaflor stereoseparation, but also provides the first experimental evidence of the pharmacokinetic dissipation of sulfoxaflor stereoisomers in the environment.

  2. Determination of sirolimus in rabbit arteries using liquid chromatography separation and tandem mass spectrometric detection.

    PubMed

    Zhang, Jun; Rodila, Ramona; Watson, Pamela; Ji, Qin; El-Shourbagy, Tawakol A

    2007-10-01

    Sirolimus, an effective immunosuppressive agent, is used for drug eluting stents. During stent development, an analytical method for the determination of sirolimus in tissue needs to be established. Normally, tissue samples are homogenized and then analyzed against the calibration standards prepared in a tissue homogenate. This approach provides insufficient control of the homogenization process. In this paper, tissue quality control samples were introduced for the optimization of the homogenization process during method development, but also allowance for the performance evaluation of the entire analytical process. In addition, a new approach using rabbit blood as a homogenization medium was developed to stabilize sirolimus in rabbit tissue homogenates. Calibration standards and quality controls were prepared by spiking different sirolimus working solutions into rabbit blood. Homogenization quality control samples were prepared by injecting other sirolimus working solutions into empty test tubes and pre-cut arteries within pre-defined masses. A high-throughput homogenization procedure was optimized based on the specific chemical properties of sirolimus. The linear dynamic range was between 49.9 pg/mL and 31.9 ng/mL to accommodate the expected artery homogenate concentrations. Additionally, quality controls in rabbit blood were also used in the extraction to support the calibration standards. The accuracy and precision of the quality controls in rabbit blood reflect the extraction performance and the accuracy and precision of the homogenization tissue quality controls reflect the overall performance of the method. The mean bias was between -4.5 and 0.2% for all levels of quality controls in the blood and between 4.8 and 14.9% for all levels of the homogenization tissue quality controls. The CVs of all concentration levels were < or =5.3% for the quality controls in blood and < or =9.2% for the homogenization tissue quality controls. The method was successfully

  3. Serum peptidome patterns of breast cancer based on magnetic bead separation and mass spectrometry analysis

    PubMed Central

    2012-01-01

    Background Breast cancer is one of the most common cancers in the world, and the identification of biomarkers for the early detection of breast cancer is a relevant target. The present study aims to determine serum peptidome patterns for screening of breast cancer. Methods The present work focused on the serum proteomic analysis of 36 healthy volunteers and 37 breast cancer patients using a ClinProt Kit combined with mass spectrometry (MS). This approach allows the determination of peptidome patterns that are able to differentiate the studied populations. An independent group of sera (36 healthy volunteers and 37 breast cancer patients) was used to verify the diagnostic capabilities of the peptidome patterns blindly. An immunoassay method was used to determine the serum mucin 1 (CA15-3) of validation group samples. Results Support Vector Machine (SVM) Algorithm was used to construct the peptidome patterns for the identification of breast cancer from the healthy volunteers. Three of the identified peaks at m/z 698, 720 and 1866 were used to construct the peptidome patterns with 91.78% accuracy. Furthermore, the peptidome patterns could differentiate the validation group achieving a sensitivity of 91.89% (34/37) and a specitivity of 91.67% (33/36) (> CA 15–3, P < 0.05). Conclusions These results suggest that the ClinProt Kit combined with MS shows great potentiality for the diagnosis of breast cancer. Virtual slides The virtual slide(s) for this article can be found here: http://www.diagnosticpathology.diagnomx.eu/vs/1501556838687844 PMID:22521044

  4. Enhancing Biological Analyses with Three Dimensional Field Asymmetric Ion Mobility, Low Field Drift Time Ion Mobility and Mass Spectrometry (µFAIMS/IMS-MS) Separations

    SciTech Connect

    Zhang, Xing; Ibrahim, Yehia M.; Chen, Tsung-Chi; Kyle, Jennifer E.; Norheim, Randolph V.; Monroe, Matthew E.; Smith, Richard D.; Baker, Erin Shammel

    2015-06-30

    We report the first evaluation of a platform coupling a high speed field asymmetric ion mobility spectrometry microchip (µFAIMS) with drift tube ion mobility and mass spectrometry (IMS-MS). The µFAIMS/IMS-MS platform was used to analyze biological samples and simultaneously acquire multidimensional information of detected features from the measured FAIMS compensation fields and IMS drift times, while also obtaining accurate ion masses. These separations thereby increase the overall separation power, resulting increased information content, and provide more complete characterization of more complex samples. The separation conditions were optimized for sensitivity and resolving power by the selection of gas compositions and pressures in the FAIMS and IMS separation stages. The resulting performance provided three dimensional separations, benefitting both broad complex mixture studies and targeted analyses by e.g. improving isomeric separations and allowing detection of species obscured by “chemical noise” and other interfering peaks.

  5. Eastern Caribbean Circulation and Island Mass Effect on St. Croix, US Virgin Islands: A Mechanism for Relatively Consistent Recruitment Patterns

    PubMed Central

    Chérubin, Laurent Marcel; Garavelli, Lysel

    2016-01-01

    The northeastern Caribbean Sea is under the seasonal influence of the Trade Winds but also of the Orinoco/Amazon freshwater plume. The latter is responsible for intensification of the Caribbean Current in general and of its eddy activity in the northern part of the Caribbean Sea. More importantly, we show in this study that the front of the freshwater plume drives a northward flow that impinges directly on the island of St. Croix in the United States Virgin Islands. The angle of incidence of the incoming flow controls the nature of the wake on both sides and ends of the island, which changes from cyclonic to anticylonic wake flow, with either attached or shed eddies. Using an off-line bio-physical model, we simulated the dispersal and recruitment of an abundant Caribbean coral reef fish, the bluehead wrasse (Thalassoma bifasciatum) in the context of the wake flow variability around St. Croix. Our results revealed the role played by the consistent seasonal forcing of the wake flow on the recruitment patterns around the island at the interannual scale. The interannual variability of the timing of arrival and northward penetration of the plume instead controls the nature of the wake, hence the regional spatial recruitment patterns. PMID:26942575

  6. Eastern Caribbean Circulation and Island Mass Effect on St. Croix, US Virgin Islands: A Mechanism for Relatively Consistent Recruitment Patterns.

    PubMed

    Chérubin, Laurent Marcel; Garavelli, Lysel

    2016-01-01

    The northeastern Caribbean Sea is under the seasonal influence of the Trade Winds but also of the Orinoco/Amazon freshwater plume. The latter is responsible for intensification of the Caribbean Current in general and of its eddy activity in the northern part of the Caribbean Sea. More importantly, we show in this study that the front of the freshwater plume drives a northward flow that impinges directly on the island of St. Croix in the United States Virgin Islands. The angle of incidence of the incoming flow controls the nature of the wake on both sides and ends of the island, which changes from cyclonic to anticylonic wake flow, with either attached or shed eddies. Using an off-line bio-physical model, we simulated the dispersal and recruitment of an abundant Caribbean coral reef fish, the bluehead wrasse (Thalassoma bifasciatum) in the context of the wake flow variability around St. Croix. Our results revealed the role played by the consistent seasonal forcing of the wake flow on the recruitment patterns around the island at the interannual scale. The interannual variability of the timing of arrival and northward penetration of the plume instead controls the nature of the wake, hence the regional spatial recruitment patterns.

  7. Chemical separation and mass spectrometry of Cr, Fe, Ni, Zn, and Cu in terrestrial and extraterrestrial materials using thermal ionization mass spectrometry.

    PubMed

    Yamakawa, Akane; Yamashita, Katsuyuki; Makishima, Akio; Nakamura, Eizo

    2009-12-01

    A sequential chemical separation technique for Cr, Fe, Ni, Zn, and Cu in terrestrial and extraterrestrial silicate rocks was developed for precise and accurate determination of elemental concentration by the isotope dilution method (ID). The technique uses a combination of cation-anion exchange chromatography and Eichrom nickel specific resin. The method was tested using a variety of matrixes including bulk meteorite (Allende), terrestrial peridotite (JP-1), and basalt (JB-1b). Concentrations of each element was determined by thermal ionization mass spectrometry (TIMS) using W filaments and a Si-B-Al type activator for Cr, Fe, Ni, and Zn and a Re filament and silicic acid-H3PO4 activator for Cu. The method can be used to precisely determine the concentrations of these elements in very small silicate samples, including meteorites, geochemical reference samples, and mineral standards for microprobe analysis. Furthermore, the Cr mass spectrometry procedure developed in this study can be extended to determine the isotopic ratios of 53Cr/52Cr and 54Cr/52Cr with precision of approximately 0.05epsilon and approximately 0.10epsilon (1epsilon = 0.01%), respectively, enabling cosmochemical applications such as high precision Mn-Cr chronology and investigation of nucleosynthetic isotopic anomalies in meteorites.

  8. Introducing the concept of centergram. A new tool to squeeze data from separation techniques-mass spectrometry couplings.

    PubMed

    Erny, Guillaume L; Simó, Carolina; Cifuentes, Alejandro; Esteves, Valdemar I

    2014-02-21

    In separation techniques hyphenated to mass spectrometry (MS) the bulk from the separation step is continuously flowing into the mass spectrometer where the compounds, arriving at each separation time, are ionized and further separated based on their m/z ratio. An MS detector is recognized as being a universal detector, although it can also be a very selective instrument. In spite of these advantages, classical two dimensional representations from these hyphenated systems, such as those based on the base peak of electropherogram/chromatogram or on the total ion of electropherogram/chromatogram, usually hide a large number of features that if correctly assessed will show the presence of co-migrating species and/or the low abundant ones. The uses of peak picking algorithms to detect and measure as many peaks as possible from a dataset allow extracting much more information. However, a single migrating compound usually produces a multiplicity of ions, making difficult to differentiate peaks generated by the same compound from other peaks due e.g., to closely co-migrating/eluting species. In this work, a new representation is proposed and its usefulness demonstrated with experimental data from capillary electrophoresis-hyphenated to a time of flight mass spectrometer via an electrospray interface. This representation, called centergram, is obtained after using a peak picking methodology that detects electrophoretic peaks of single ions and measure their positions. The centergram is the histogram (i.e. the count of the number of observations that fall into each one of the intervals, known as bins, as determined by the user) of the measured positions. The intensity of the bars in this histogram will indicate the amount of peaks in the whole dataset whose centers are within each interval. As a compound that has been separated and has entered the MS instrument will produce multiple images at the same position along the m/z dimension, the centergram will exhibit a series of

  9. Non-separative headspace solid phase microextraction-mass spectrometry profile as a marker to monitor coffee roasting degree.

    PubMed

    Liberto, Erica; Ruosi, Manuela R; Cordero, Chiara; Rubiolo, Patrizia; Bicchi, Carlo; Sgorbini, Barbara

    2013-02-27

    This study describes a non-separative headspace solid phase microextraction-mass spectrometry (HS-SPME-MS) approach, in view of its application to online monitoring of a roasting process. The system can quickly provide representative and diagnostic fingerprints of the volatile fraction of samples and, in combination with appropriate chemometric pattern recognition and regression techniques, can successfully be applied to characterize, discriminate, and/or correlate patterns with the roasting process. Eighty coffee samples of different varieties, geographical origins, and blends were analyzed. The experimental HS-SPME-MS results show that the TIC fingerprint can be used to discriminate the degree of roasting; diagnostic ion abundance(s) or ratios were closely correlated with the roasting process; both could successfully be used as markers or analytical decision makers, to monitor roasting processes online, and to define quality and safety of roasted coffee.

  10. Separation, Sizing, and Quantitation of Engineered Nanoparticles in an Organism Model Using Inductively Coupled Plasma Mass Spectrometry and Image Analysis.

    PubMed

    Johnson, Monique E; Hanna, Shannon K; Montoro Bustos, Antonio R; Sims, Christopher M; Elliott, Lindsay C C; Lingayat, Akshay; Johnston, Adrian C; Nikoobakht, Babak; Elliott, John T; Holbrook, R David; Scott, Keana C K; Murphy, Karen E; Petersen, Elijah J; Yu, Lee L; Nelson, Bryant C

    2017-01-24

    For environmental studies assessing uptake of orally ingested engineered nanoparticles (ENPs), a key step in ensuring accurate quantification of ingested ENPs is efficient separation of the organism from ENPs that are either nonspecifically adsorbed to the organism and/or suspended in the dispersion following exposure. Here, we measure the uptake of 30 and 60 nm gold nanoparticles (AuNPs) by the nematode, Caenorhabditis elegans, using a sucrose density gradient centrifugation protocol to remove noningested AuNPs. Both conventional inductively coupled plasma mass spectrometry (ICP-MS) and single particle (sp)ICP-MS are utilized to measure the total mass and size distribution, respectively, of ingested AuNPs. Scanning electron microscopy/energy-dispersive X-ray spectroscopy (SEM/EDS) imaging confirmed that traditional nematode washing procedures were ineffective at removing excess suspended and/or adsorbed AuNPs after exposure. Water rinsing procedures had AuNP removal efficiencies ranging from 57 to 97% and 22 to 83%, while the sucrose density gradient procedure had removal efficiencies of 100 and 93 to 98%, respectively, for the 30 and 60 nm AuNP exposure conditions. Quantification of total Au uptake was performed following acidic digestion of nonexposed and Au-exposed nematodes, whereas an alkaline digestion procedure was optimized for the liberation of ingested AuNPs for spICP-MS characterization. Size distributions and particle number concentrations were determined for AuNPs ingested by nematodes with corresponding confirmation of nematode uptake via high-pressure freezing/freeze substitution resin preparation and large-area SEM imaging. Methods for the separation and in vivo quantification of ENPs in multicellular organisms will facilitate robust studies of ENP uptake, biotransformation, and hazard assessment in the environment.

  11. Determination of mercurial species in fish by inductively coupled plasma mass spectrometry with anion exchange chromatographic separation.

    PubMed

    Chen, Xiaopan; Han, Chao; Cheng, Heyong; Liu, Jinhua; Xu, Zigang; Yin, Xuefeng

    2013-09-24

    This work demonstrated the feasibility of mercury speciation analysis by anion exchange chromatographic separation with inductively coupled plasma mass spectrometry detection. For the first time, by complexing with the mobile phase containing 3-mercapto-1-propanesulfonate into negatively charged complexes, fast separation of inorganic mercury (Hg(2+)), monomethylmercury (MeHg), ethylmercury (EtHg) and phenylmercury (PhHg) was achieved within 5 min on a 12.5-mm strong anion exchange column. The detection limits for Hg(2+), MeHg, EtHg and PhHg were 0.008, 0.024, 0.029 and 0.034 μg L(-1), respectively. The relative standard deviations of peak height and peak area (5.0 μg L(-1) for each Hg species) were all below 3%. The determined contents of Hg(2+), MeHg and total Hg in a certified reference material of fish tissue by the proposed method were in good accordance with the certified values with satisfactory recoveries. The relative errors for determining MeHg and total mercury were -2.4% and -1.2%, respectively, with an acceptable range for spike recoveries of 94-101%. Mercury speciation in 11 fish samples were then analyzed after the pretreated procedure. The mercury contents in all fish samples analyzed were found compliant with the criteria of the National Standards of China.

  12. Separation and characterization of phenolic compounds from dry-blanched peanut skins by liquid chromatography-electrospray ionization mass spectrometry.

    PubMed

    Ma, Yuanyuan; Kosińska-Cagnazzo, Agnieszka; Kerr, William L; Amarowicz, Ryszard; Swanson, Ruthann B; Pegg, Ronald B

    2014-08-22

    A large variety of phenolic compounds, including phenolic acids (hydroxybenzoic acids, hydroxycinnamic acids, and their esters), stilbenes (trans-resveratrol and trans-piceatannol), flavan-3-ols (e.g., (-)-epicatechin, (+)-catechin, and their polymers {the proanthocyanidins, PACs}), other flavonoids (e.g., isoflavones, flavanols, and flavones, etc.) and biflavonoids (e.g., morelloflavone), were identified in dry-blanched peanut skins (PS) by this study. High-performance liquid chromatography (HPLC) coupled with electrospray ionization mass spectrometry (ESI-MS(n)) was applied to separate and identify the phenolic constituents. Reversed-phase HPLC was employed to separate free phenolic compounds as well as PAC monomers, dimers, and trimers. PACs with a degree of polymerization (DP) of >4 were chromatographed via hydrophilic interaction liquid chromatography (HILIC). Tentative identification of the separated phenolics was based solely on molecular ions and MS(n) fragmentation patterns acquired by ESI-MS in the negative-ion mode. The connection sequence of PAC oligomers (DP <5) could be deduced mainly through characteristic quinone methide (QM) cleavage ions. When the DP reached 6, only a proportion of the flavan-3-ols could be ascertained in the PACs because of the extremely complicated fragmentation patterns involved. The identification of free phenolic acids, stilbenes, and flavonoids was achieved by authentic commercial standards and also by published literature data. Quantification was performed based on peak areas of the UV (free phenolic compounds) or fluorescence (PACs) signals from the HPLC chromatograms and calibration curves of commercial standards. Overall, PS contain significantly more PACs compared to free phenolic compounds.

  13. Relation of Left Ventricular Mass and Infarct Size in Anterior Wall ST-Segment Elevation Acute Myocardial Infarction (from the EMBRACE STEMI Clinical Trial).

    PubMed

    Daaboul, Yazan; Korjian, Serge; Weaver, W Douglas; Kloner, Robert A; Giugliano, Robert P; Carr, Jim; Neal, Brandon J; Chi, Gerald; Cochet, Madeleine; Goodell, Laura; Michalak, Nathan; Rusowicz-Orazem, Luke; Alkathery, Turky; Allaham, Haytham; Routray, Sujit; Szlosek, Donald; Jain, Purva; Gibson, C Michael

    2016-09-01

    Biomarker measures of infarct size and myocardial salvage index (MSI) are important surrogate measures of clinical outcomes after a myocardial infarction. However, there is variability in infarct size unaccounted for by conventional adjustment factors. This post hoc analysis of Evaluation of Myocardial Effects of Bendavia for Reducing Reperfusion Injury in Patients With Acute Coronary Events (EMBRACE) ST-Segment Elevation Myocardial Infarction (STEMI) trial evaluates the association between left ventricular (LV) mass and infarct size as assessed by areas under the curve for creatine kinase-MB (CK-MB) and troponin I release over the first 72 hours (CK-MB area under the curve [AUC] and troponin I [TnI] AUC) and the MSI. Patients with first anterior STEMI, occluded left anterior descending artery, and available LV mass measurement in EMBRACE STEMI trial were included (n = 100) (ClinicalTrials.govNCT01572909). MSI, end-diastolic LV mass on day 4 cardiac magnetic resonance, and CK-MB and troponin I concentrations were evaluated by a core laboratory. After saturated multivariate analysis, dominance analysis was performed to estimate the contribution of each independent variable to the predicted variance of each outcome. In multivariate models that included age, gender, body surface area, lesion location, smoking, and ischemia time, LV mass remained independently associated with biomarker measures of infarct size (CK-MB AUC p = 0.02, TnI AUC p = 0.03) and MSI (p = 0.003). Dominance analysis demonstrated that LV mass accounted for 58%, 47%, and 60% of the predicted variances for CK-MB AUC, TnI AUC, and MSI, respectively. In conclusion, LV mass accounts for approximately half of the predicted variance in biomarker measures of infarct size. It should be considered as an adjustment variable in studies evaluating infarct size.

  14. Multiwavelength observations of NaSt1 (WR 122): equatorial mass loss and X-rays from an interacting Wolf-Rayet binary

    NASA Astrophysics Data System (ADS)

    Mauerhan, Jon; Smith, Nathan; Van Dyk, Schuyler D.; Morzinski, Katie M.; Close, Laird M.; Hinz, Philip M.; Males, Jared R.; Rodigas, Timothy J.

    2015-07-01

    NaSt1 (aka Wolf-Rayet 122) is a peculiar emission-line star embedded in an extended nebula of [N II] emission with a compact dusty core. The object was previously characterized as a Wolf-Rayet (WR) star cloaked in an opaque nebula of CNO-processed material, perhaps analogous to η Car and its Homunculus nebula, albeit with a hotter central source. To discern the morphology of the [N II] nebula we performed narrow-band imaging using the Hubble Space Telescope and Wide-field Camera 3. The images reveal that the nebula has a disc-like geometry tilted ≈12° from edge-on, composed of a bright central ellipsoid surrounded by a larger clumpy ring. Ground-based spectroscopy reveals radial velocity structure (±10 km s-1) near the outer portions of the nebula's major axis, which is likely to be the imprint of outflowing gas. Near-infrared adaptive-optics imaging with Magellan AO has resolved a compact ellipsoid of Ks-band emission aligned with the larger [N II] nebula, which we suspect is the result of scattered He I line emission (λ2.06 μm). Observations with the Chandra X-ray Observatory have revealed an X-ray point source at the core of the nebula that is heavily absorbed at energies <1 keV and has properties consistent with WR stars and colliding-wind binaries. We suggest that NaSt1 is a WR binary embedded in an equatorial outflow that formed as the result of non-conservative mass transfer. NaSt1 thus appears to be a rare and important example of a stripped-envelope WR forming through binary interaction, caught in the brief Roche lobe overflow phase.

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

    PubMed Central

    Salama, Nahla N.; Wang, Shudong

    2009-01-01

    The present study employs time of flight mass 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. PMID:19652756

  16. Quantitative mass spectrometric analysis of ropivacaine and bupivacaine in authentic, pharmaceutical and spiked human plasma without chromatographic separation.

    PubMed

    Salama, Nahla N; Wang, Shudong

    2008-05-28

    The present study employs time of flight mass 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 >or=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.

  17. Analysis of multiple quaternary ammonium compounds in the brain using tandem capillary column separation and high resolution mass spectrometric detection.

    PubMed

    Falasca, Sara; Petruzziello, Filomena; Kretz, Robert; Rainer, Gregor; Zhang, Xiaozhe

    2012-06-08

    Endogenous quaternary ammonium compounds are involved in various physiological processes in the central nervous system. In the present study, eleven quaternary ammonium compounds, including acetylcholine, choline, carnitine, acetylcarnitine and seven other acylcarnitines of low polarity, were analyzed from brain extracts using a two dimension capillary liquid chromatography-Fourier transform mass spectrometry method. To deal with their large difference in hydrophobicities, tandem coupling between reversed phase and hydrophilic interaction chromatography columns was used to separate all the targeted quaternary ammonium compounds. Using high accuracy mass spectrometry in selected ion monitoring mode, all the compounds could be detected from each brain sample with high selectivity. The developed method was applied for the relative quantification of these quaternary ammonium compounds in three different brain regions of tree shrews: prefrontal cortex, striatum, and hippocampus. The comparative analysis showed that quaternary ammonium compounds were differentially distributed across the three brain areas. The analytical method proved to be highly sensitive and reliable for simultaneous determination of all the targeted analytes from brain samples.

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

    PubMed Central

    Rudd, David; Benkendorff, Kirsten; Voelcker, Nicolas H.

    2015-01-01

    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. PMID:25786067

  19. Simultaneous separation and confirmation of amphetamine and related drugs in equine plasma by non-aqueous capillary-electrophoresis-tandem mass spectrometry.

    PubMed

    Li, X Q; Uboh, C E; Soma, L R; Guan, F Y; You, Y W; Kahler, M C; Judy, J A; Liu, Y; Chen, J W

    2010-02-01

    A non-aqueous capillary electrophoresis-mass spectrometry (NACE-MS) method was developed for simultaneous separation and identification of 12 amphetamine and related compounds in equine plasma. Analytes were recovered from plasma by liquid-liquid extraction using methyl tertiary butyl ether (MTBE). A bare fused-silica capillary was used for separation of the analytes. Addition of sheath liquid to the capillary effluent allowed the detection of the analytes by positive electrospray ionization mass spectrometry using full scan data acquisition. The limit of detection (LOD) for the target analytes was 10-200 ng/mL and that of confirmation (LOC) was 50-1000 ng/mL in equine plasma. Capillary electrophoresis (CE) and mass spectrometry (MS) parameters were optimized for full CE separation and MS detection of the analytes. Separation buffer comprised 25 mM ammonium formate in acetonitrile/methanol (20: 80, v/v) plus 1 M formic acid. Sheath liquid was isopropanol-water-formic acid (50:50:0.5, v/v/v). Samples were hydrodynamically injected and separated at 25 kV. Analytes were electrokinetically separated and mass spectrometrically identified and confirmed. This simple, fast, inexpensive and reproducible method was successfully applied to post race equine plasma and research samples in screening for amphetamine and related drugs.

  20. Proceedings of the Annual Meeting of the Association for Education in Journalism and Mass Communication (81st, Baltimore, Maryland, August 5-8, 1998). Mass Communication and Society.

    ERIC Educational Resources Information Center

    Association for Education in Journalism and Mass Communication.

    The Mass Communication and Society section of the Proceedings contains the following 19 papers: "Talk Radio as Forum and Companion: Listener Attitudes and Uses and Gratifications in Austin, Texas" (John Beatty); "'Willingness to Censor': Developing a Quantitative Measurement across Speech Categories and Types of Media"…

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

    NASA Astrophysics Data System (ADS)

    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.

  2. [Bacterial identification based on protein mass spectrometry: A new insight at the microbiology of the 21st century].

    PubMed

    García, Patricia; Allende, Fidel; Legarraga, Paulette; Huilcaman, Marcos; Solari, Sandra

    2012-06-01

    Bacterial identification is important for the proper treatment of infected patients hospitalized with serious infections especially in critical care units. Identification by conventional methods used in microbiology laboratories takes at least 16 hours since a culture is positive. The introduction of mass spectrometry, specifically MALDI-TOF MS (matrix-assisted laser desorption/ ionization time-of-flight mass spectrometer) in the microbiology laboratory could mean a radical change in the identification accuracy, turn around time (6 minutes per bacteria) and cost (about 5 times cheaper than conventional identification). Since its introduction in clinical microbiology laboratories in 2008, many reports about its usefulness in identifying microorganisms from colonies, as well as directly from positive blood cultures and urine samples have been published. This review describes MALDI-TOF MS methodology, its identification performance for bacteria (aerobic and anaerobic), mycobacterium and yeasts, its future applications in microbiology and its main disadvantages.

  3. Characterisation of water masses and phytoplankton nutrient limitation in the East Australian Current separation zone during spring 2008

    NASA Astrophysics Data System (ADS)

    Hassler, C. S.; Djajadikarta, J. R.; Doblin, M. A.; Everett, J. D.; Thompson, P. A.

    2011-03-01

    This study focuses on the comparison of oceanic and coastal cold-core eddies with inner-shelf and East Australian Current (EAC) waters at the time of the spring bloom (October 2008). The surface water was biologically characterised by the phytoplankton biomass, composition, photo-physiology, carbon fixation and by nutrient-enrichment experiments. Marked differences in phytoplankton biomass and composition were observed. Contrasted biomarker composition suggests that biomarkers could be used to track water masses in this area. Divinyl chlorophyll a, a biomarker for tropical Prochlorophytes, was found only in the EAC. Zeaxanthin a biomarker for Cyanophytes, was found only within the oceanic eddy and in the EAC, whereas chlorophyll b (Chlorophytes) was only present in the coastal eddy and at the front between the inner-shelf and EAC waters. This study showed that cold-core eddies can affect phytoplankton, biomass, biodiversity and productivity. Inside the oceanic eddy, greater phytoplankton biomass and a more complex phytoplankton community were observed relative to adjacent water masses (including the EAC). In fact, phytoplankton communities inside the oceanic eddy more closely resembled the community observed in the inner-shelf waters. At a light level close to half-saturation, phytoplankton carbon fixation (gC d -1) in the oceanic eddy was 13-times greater than at the frontal zone between the eddy and the EAC and 3-times greater than in the inner-shelf water. Nutrient-enrichment experiments demonstrated that nitrogen was the major macronutrient limiting phytoplankton growth in water masses associated with the oceanic eddy. Although the effective quantum yield values demonstrate healthy phytoplankton communities, the phytoplankton community bloomed and shifted in response to nitrogen enrichments inside the oceanic eddy and in the frontal zone between this eddy and the EAC. An effect of Si enrichment was only observed at the frontal zone between the eddy and the EAC

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

    NASA Astrophysics Data System (ADS)

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

    2014-04-01

    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 ( 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 c.m. = 1113 keV resonance in the 20 Ne( p, γ)21 Na radiative proton capture reaction.

  5. Modified ion exchange separation for tungsten isotopic measurements from kimberlite samples using multi-collector inductively coupled plasma mass spectrometry.

    PubMed

    Sahoo, Yu Vin; Nakai, Shun'ichi; Ali, Arshad

    2006-03-01

    Tungsten isotope composition of a sample of deep-seated rock can record the influence of core-mantle interaction of the parent magma. Samples of kimberlite, which is known as a carrier of diamond, from the deep mantle might exhibit effects of core-mantle interaction. Although tungsten isotope anomaly was reported for kimberlites from South Africa, a subsequent investigation did not verify the anomaly. The magnesium-rich and calcium-rich chemical composition of kimberlite might engender difficulty during chemical separation of tungsten for isotope analyses. This paper presents a simple, one-step anion exchange technique for precise and accurate determination of tungsten isotopes in kimberlites using multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS). Large quantities of Ca and Mg in kimberlite samples were precipitated and removed with aqueous H(2)SO(4). Highly pure fractions of tungsten for isotopic measurements were obtained following an anion exchange chromatographic procedure involving mixed acids. That procedure enabled efficient removal of high field strength elements (HFSE), such as Hf, Zr and Ti, which are small ions that carry strong charges and develop intense electrostatic fields. The tungsten yields were 85%-95%. Advantages of this system include less time and less use of reagents. Precise and accurate isotopic measurements are possible using fractions of tungsten that are obtained using this method. The accuracy and precision of these measurements were confirmed using various silicate standard rock samples, JB-2, JB-3 and AGV-1.

  6. Analysis of arginine and lysine methylation utilizing peptide separations at neutral pH and electron transfer dissociation mass spectrometry.

    PubMed

    Snijders, Ambrosius P L; Hung, Ming-Lung; Wilson, Stuart A; Dickman, Mark J

    2010-01-01

    Arginine and lysine methylation are widespread protein post-translational modifications. Peptides containing these modifications are difficult to retain using traditional reversed-phase liquid chromatography because they are intrinsically basic/hydrophilic and often fragment poorly during collision induced fragmentation (CID). Therefore, they are difficult to analyze using standard proteomic workflows. To overcome these caveats, we performed peptide separations at neutral pH, resulting in increased retention of the hydrophilic/basic methylated peptides before identification using MS/MS. Alternatively trifluoroacetic acid (TFA) was used for increased trapping of methylated peptides. Electron-transfer dissociation (ETD) mass spectrometry was then used to identify and characterize methylated residues. In contrast to previous reports utilizing ETD for arginine methylation, we observed significant amount of side-chain fragmentation. Using heavy methyl stable isotope labeling with amino acids in cell culture it was shown that, similar to CID, a loss of monomethylamine or dimethylamine from the arginine methylated side-chain during ETD can be used as a diagnostic to determine the type of arginine methylation. CID of lysine methylated peptides does not lead to significant neutral losses, but ETD is still beneficial because of the high charge states of such peptides. The developed LC MS/MS methods were successfully applied to tryptic digests of a number of methylated proteins, including splicing factor proline-glutamine-rich protein (SFPQ), RNA and export factor-binding protein 2 (REF2-I) and Sul7D, demonstrating significant advantages over traditional LC MS/MS approaches.

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

    PubMed

    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.

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

    SciTech Connect

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

    PubMed

    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 CV<30 for all compounds. Also, the method showed a linear response over a range spanning several orders of magnitude. In a QC human plasma sample, we identified and rigorously quantified over 120 eicosanoids.

  10. Hydrologic and mass-movement hazards near McCarthy Wrangell-St Elias National Park and Preserve, Alaska

    USGS Publications Warehouse

    Jones, S.H.; Glass, R.L.

    1993-01-01

    At the confluence of McCarthy Creek and the Kennicott River, about 1 mile from the terminus of Kennicott Glacier, Alaska, McCarthy Creek and Kennicott River basins are prone to several natural hazards including floods; formation and failure of natural dams; stream erosion and sediment deposi- tion; snow avalanches; aufeis; and the mass wasting of rock, soil, and debris. Low-lying areas along the Kennicott River flood annually, commonly during late July or early August, as a result of outbursts from glacier-dammed lakes, but these floods can occur during any month of the year. Flood plains along McCarthy Creek and its tributaries are frequently flooded and prone to rapid erosion and deposition during intense rainfall and periods of rapid snow- melt. Sediments from continual mass wasting accumu- late in stream channels and are mobilized during floods. Several lateral erosion, scour, and deposition resulting from floods in September 1980 and August 1985 destroyed bridges and several historic structures at McCarthy were jeopardized by the rapidly eroding northern streambank of McCarthy Creek. Flood discharges were determined indirectly using the slope-area method at two high-gradient reaches on the Kennicott River, four on McCarthy Creek, and one on Nikolai Creek. During the flood of September 13, 1980, peak discharge for McCarthy Creek at McCarthy was 4,500 cubic feet per second.

  11. Alignment Sensitivity Study of the St. ANA Beam Line

    NASA Astrophysics Data System (ADS)

    Gervais, Michelle; Couder, Manoel; Jung, Hyo Soon; Setoodehnia, Kiana

    2014-09-01

    The St. ANA (STable Accelerator for Nuclear Astrophysics) accelerator is being prepared for use with the St. George recoil mass separator. The accelerator is in working condition for use in direct kinematic experiments but the St. George separator works with inverse kinematics and requires a highly controlled beam restricted by severe position and divergence parameters that are not achieved at the present time. A systematic sensitivity study was conducted using a simulation of the beam line in order to assess the impact of a misalignment in each optical element or in the beam itself. Tests were done with the beam to analyze how the beam behaves at various points in the line and to compare this data with simulation results to determine possible causes of misalignment. The results of these tests and simulations are that the beam characteristics are now better understood and the possible causes of the limitations have been narrowed down. The St. ANA (STable Accelerator for Nuclear Astrophysics) accelerator is being prepared for use with the St. George recoil mass separator. The accelerator is in working condition for use in direct kinematic experiments but the St. George separator works with inverse kinematics and requires a highly controlled beam restricted by severe position and divergence parameters that are not achieved at the present time. A systematic sensitivity study was conducted using a simulation of the beam line in order to assess the impact of a misalignment in each optical element or in the beam itself. Tests were done with the beam to analyze how the beam behaves at various points in the line and to compare this data with simulation results to determine possible causes of misalignment. The results of these tests and simulations are that the beam characteristics are now better understood and the possible causes of the limitations have been narrowed down. Project advisor

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

    PubMed Central

    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

  13. Collision-induced release, ion mobility separation, and amino acid sequence analysis of subunits from mass-selected noncovalent protein complexes.

    PubMed

    Rathore, Deepali; Dodds, Eric D

    2014-09-01

    In recent years, mass spectrometry has become a valuable tool for detecting and characterizing protein-protein interactions and for measuring the masses and subunit stoichiometries of noncovalent protein complexes. The gas-phase dissociation of noncovalent protein assemblies via tandem mass spectrometry can be useful in confirming subunit masses and stoichiometries; however, dissociation experiments that are able to yield subunit sequence information must usually be conducted separately. Here, we furnish proof of concept for a method that allows subunit sequence information to be directly obtained from a protein aggregate in a single gas-phase analysis. The experiments were carried out using a quadrupole time-of-flight mass spectrometer equipped with a traveling-wave ion mobility separator. This instrument configuration allows for a noncovalent protein assembly to be quadrupole selected, then subjected to two successive rounds of collision-induced dissociation with an intervening stage of ion mobility separation. This approach was applied to four model proteins as their corresponding homodimers: glucagon, ubiquitin, cytochrome c, and β-lactoglobulin. In each case, b- and y-type fragment ions were obtained upon further collisional activation of the collisionally-released subunits, resulting in up to 50% sequence coverage. Owing to the incorporation of an ion mobility separation, these results also suggest the intriguing possibility of measuring complex mass, complex collisional cross section, subunit masses, subunit collisional cross sections, and sequence information for the subunits in a single gas-phase experiment. Overall, these findings represent a significant contribution towards the realization of protein interactomic analyses, which begin with native complexes and directly yield subunit identities.

  14. Collision-Induced Release, Ion Mobility Separation, and Amino Acid Sequence Analysis of Subunits from Mass-Selected Noncovalent Protein Complexes

    NASA Astrophysics Data System (ADS)

    Rathore, Deepali; Dodds, Eric D.

    2014-09-01

    In recent years, mass spectrometry has become a valuable tool for detecting and characterizing protein-protein interactions and for measuring the masses and subunit stoichiometries of noncovalent protein complexes. The gas-phase dissociation of noncovalent protein assemblies via tandem mass spectrometry can be useful in confirming subunit masses and stoichiometries; however, dissociation experiments that are able to yield subunit sequence information must usually be conducted separately. Here, we furnish proof of concept for a method that allows subunit sequence information to be directly obtained from a protein aggregate in a single gas-phase analysis. The experiments were carried out using a quadrupole time-of-flight mass spectrometer equipped with a traveling-wave ion mobility separator. This instrument configuration allows for a noncovalent protein assembly to be quadrupole selected, then subjected to two successive rounds of collision-induced dissociation with an intervening stage of ion mobility separation. This approach was applied to four model proteins as their corresponding homodimers: glucagon, ubiquitin, cytochrome c, and β-lactoglobulin. In each case, b- and y-type fragment ions were obtained upon further collisional activation of the collisionally-released subunits, resulting in up to 50% sequence coverage. Owing to the incorporation of an ion mobility separation, these results also suggest the intriguing possibility of measuring complex mass, complex collisional cross section, subunit masses, subunit collisional cross sections, and sequence information for the subunits in a single gas-phase experiment. Overall, these findings represent a significant contribution towards the realization of protein interactomic analyses, which begin with native complexes and directly yield subunit identities.

  15. A complete mass balance of a complex combined anaerobic/aerobic municipal source-separated waste treatment plant.

    PubMed

    Pognani, Michele; Barrena, Raquel; Font, Xavier; Sánchez, Antoni

    2012-05-01

    In this study a combined anaerobic/aerobic full-scale treatment plant designed for the treatment of the source-separated organic fraction of municipal solid waste (OFMSW) was monitored over a period of one year. During this period, full information was collected about the waste input material, the biogas production, the main rejects and the compost characteristics. The plant includes mechanical pre-treatment, dry thermophilic anaerobic digestion, tunnel composting system and a curing phase to produce compost. To perform the monitoring of the entire plant and the individual steps, traditional chemical methods were used but they present important limitations in determining the critical points and the efficiency of the stabilization of the organic matter. Respiration indices (dynamic and cumulative) allowed for the quantitative calculation of the efficiency of each treatment unit. The mass balance was calculated and expressed in terms of Mgy(-1) of wet (total) matter, carbon, nitrogen and phosphorus. Results show that during the pre-treatment step about 32% of the initial wet matter is rejected without any treatment. This also reduces the biodegradability of the organic matter that continues to the treatment process. About 50% of the initial nitrogen and 86.4% of the initial phosphorus are found in the final compost. The final compost also achieves a high level of stabilization with a dynamic respiration index of 0.3±0.1g O(2) per kg of total solids per hour, which implies a reduction of 93% from that of the raw OFMSW, without considering the losses of biodegradable organic matter in the refuse (32% of the total input). The anaerobic digestion process is the main contributor to this stabilization.

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

    PubMed

    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).

  17. Mass

    SciTech Connect

    Quigg, Chris

    2007-12-05

    In the classical physics we inherited from Isaac Newton, mass does not arise, it simply is. The mass of a classical object is the sum of the masses of its parts. Albert Einstein showed that the mass of a body is a measure of its energy content, inviting us to consider the origins of mass. The protons we accelerate at Fermilab are prime examples of Einsteinian matter: nearly all of their mass arises from stored energy. Missing mass led to the discovery of the noble gases, and a new form of missing mass leads us to the notion of dark matter. Starting with a brief guided tour of the meanings of mass, the colloquium will explore the multiple origins of mass. We will see how far we have come toward understanding mass, and survey the issues that guide our research today.

  18. Separate and combined effects of temperature and precipitation change on maize yields in sub-Saharan Africa for mid- to late-21st century

    NASA Astrophysics Data System (ADS)

    Waha, K.; Müller, C.; Rolinski, S.

    2013-07-01

    Maize (Zea mays L.) is one of the most important food crops and very common in all parts of sub-Saharan Africa. In 2010 53 million tons of maize were produced in sub-Saharan Africa on about one third of the total harvested cropland area (~ 33 million ha). Our aim is to identify the limiting agroclimatic variable for maize growth and development in sub-Saharan Africa by analyzing the separated and combined effects of temperature and precipitation. Under changing climate, both climate variables are projected to change severely, and their impacts on crop yields are frequently assessed using process-based crop models. However it is often unclear which agroclimatic variable will have the strongest influence on crop growth and development under climate change and previous studies disagree over this question.

  19. Method for quantitative determination and separation of trace amounts of chemical elements in the presence of large quantities of other elements having the same atomic mass

    DOEpatents

    Miller, C.M.; Nogar, N.S.

    1982-09-02

    Photoionization via autoionizing atomic levels combined with conventional mass spectroscopy provides a technique for quantitative analysis of trace quantities of chemical elements in the presence of much larger amounts of other elements with substantially the same atomic mass. Ytterbium samples smaller than 10 ng have been detected using an ArF* excimer laser which provides the atomic ions for a time-of-flight mass spectrometer. Elemental selectivity of greater than 5:1 with respect to lutetium impurity has been obtained. Autoionization via a single photon process permits greater photon utilization efficiency because of its greater absorption cross section than bound-free transitions, while maintaining sufficient spectroscopic structure to allow significant photoionization selectivity between different atomic species. Separation of atomic species from others of substantially the same atomic mass is also described.

  20. UV photodissociation of trapped ions following ion mobility separation in a Q-ToF mass spectrometer.

    PubMed

    Bellina, Bruno; Brown, Jeffery M; Ujma, Jakub; Murray, Paul; Giles, Kevin; Morris, Michael; Compagnon, Isabelle; Barran, Perdita E

    2014-12-21

    An ion mobility mass spectrometer has been modified to allow optical interrogation of ions with different mass-to-charge (m/z) ratios and/or mobilities (K). An ion gating and trapping procedure has been developed which allows us to store ions for several seconds enabling UV photodissociation (UVPD).

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

    ERIC Educational Resources Information Center

    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…

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

    SciTech Connect

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

    2010-07-15

    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.

  3. Selective extraction, separation, and identification of anthocyanins from Hibiscus sabdariffa L. using solid phase extraction-capillary electrophoresis-mass spectrometry (time-of-flight /ion trap).

    PubMed

    Segura-Carretero, Antonio; Puertas-Mejía, Miguel A; Cortacero-Ramírez, Sonia; Beltrán, Raúl; Alonso-Villaverde, Carlos; Joven, Jorge; Dinelli, Giovanni; Fernández-Gutiérrez, Alberto

    2008-07-01

    A method for selective extraction using SPE, electrophoretic separation at basic condition and the identification by using exact masses and fragmentation patterns has been developed in order to know the anthocyanins in dried calyces of Hibiscus sabdariffa L. A detailed and comparative study of several extraction procedures has been carried out to obtain the maximum number of anthocyanidins from the calyces and then a CE-TOF-MS method in positive mode using ESI has been developed for the separation and rapid identification of anthocyanins in H. sabdariffa L. Delphinidin-3-sambubioside, cyanidin-3-sambubioside have been detected as main components and cyanidin-3-O-rutinoside, delphinidin-3-O-glucoside and cyanidin-3,5-diglucoside, and chlorogenic acid as minor constituents. The confirmation of the anthocyanidins and chlorogenic acid was carried out using fragmentation ions with the IT-mass spectrometer (IT-MS).

  4. 'Proteomic basics--sample preparation and separation': the 1st European Summer School in Kloster Neustift, 12-18 August, 2007 Brixen/Bressanone, South Tyrol, Italy.

    PubMed

    Marcus, Katrin; Kühn-Hölsken, Eva; Schmidt, Carla; Schulenborg, Thomas; Urlaub, Henning

    2008-01-01

    Proteomics is rapidly developing into a routine approach for protein analysis in many laboratories. The series of European-wide Summer Schools 'Proteomics Basics' (http://www.proteomic-basics.eu/) aims at teaching of comprehensive knowledge in proteomics research and applied technologies for master and graduate students and postdocs currently moving into the field of proteomic research. In the next 3 years the series will cover the theoretical basis of the fundamental topics in the various areas of proteomic analysis, i.e. sample preparation and handling, mass spectrometry, post-translational modifications and quantitation given by leading experts in the field. This summer school series embodies a unique advantage in comparison with conventional scientific meetings and university curricula: internationally renowned experts will give a detailed perspective view of the fundamentals of their particular proteome research area, something which is usually not encountered at conferences and congresses. Here, we give a report on the first European Summer School 'Sample Preparation and Handling' within the series 'Proteomic Basics' that was held at the monastery in Neustift close to Bressanone/Brixen, Italy from August 12 to 18, 2007.

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

    PubMed

    Brudin, Stella S; Shellie, Robert A; Haddad, Paul R; Schoenmakers, Peter J

    2010-10-22

    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 made possible by neutralising the first-dimension effluent, containing KOH, prior to transfer to the second-dimension reversed-phase column. A test mixture of 24 low-molar-mass organic acids is used for optimisation of the system. Three food and beverage samples were analysed in order to evaluate the developed methodology, the resulting two-dimensional separation is near-orthogonal, the set-up is simple and all instrumental components are available commercially. The method proved to be robust and suitable for the analysis of wine, orange juice and yogurt.

  6. 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.

    PubMed

    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.

  7. An application of high-speed counter-current chromatography coupled with electrospray ionization mass spectrometry for separation and online identification of coumarins from Peucedanum praeruptorum Dunn.

    PubMed

    Hou, Zhiguo; Xu, Deran; Yao, Shun; Luo, Jianguang; Kong, Lingyi

    2009-08-15

    A new and systematic application for separation and online identification of coumarins from Peucedanum praeruptorum Dunn by preparative high-speed counter-current chromatography coupled with electrospray ionization multi-stage mass spectrometry (prep-HSCCC/ESI-MS(n)) was established. The procedure of separation was guided by the chromatogram of ion current. The structures of acquisitions were deduced by MS information. The hyphenation between prep-HSCCC/ESI-MS(n) was designed to keep the split ratio from 1:20 to 1:200 exactly. Seven compounds were obtained and two new compounds were detected. It was proved that prep-HSCCC/ESI-MS(n) was an effective method for sensitive detection, rapid identification and separation of natural products.

  8. Three-dimensional enhanced lipidomics analysis combining UPLC, differential ion mobility spectrometry, and mass spectrometric separation strategies1[S

    PubMed Central

    Baker, Paul R. S.; Armando, Aaron M.; Campbell, J. Larry; Quehenberger, Oswald; Dennis, Edward A.

    2014-01-01

    Phospholipids serve as central structural components in cellular membranes and as potent mediators in numerous signaling pathways. There are six main classes of naturally occurring phospholipids distinguished by their distinct polar head groups that contain many unique molecular species with distinct fatty acid composition. Phospholipid molecular species are often expressed as isobaric species that are denoted by the phospholipid class and the total number of carbon atoms and double bonds contained in the esterified fatty acyl groups (e.g., phosphatidylcholine 34:2). Techniques to separate these molecules exist, and each has positive and negative attributes. Hydrophilic interaction liquid chromatography uses polar bonded silica to separate lipids by polar head group but not by specific molecular species. Reversed phase (RP) chromatography can separate by fatty acyl chain composition but not by polar head group. Herein we describe a new strategy called differential ion mobility spectrometry (DMS), which separates phospholipid classes by their polar head group. Combining DMS with current LC methods enhances phospholipid separation by increasing resolution, specificity, and signal-to-noise ratio. Additional application of specialized information-dependent acquisition methodologies along with RP chromatography allows full isobaric resolution, identification, and compositional characterization of specific phospholipids at the molecular level. PMID:25225680

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

    NASA Astrophysics Data System (ADS)

    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.

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

    NASA Astrophysics Data System (ADS)

    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.

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

    PubMed

    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.

  12. Rapid separation and identification of furocoumarins in Angelica dahurica by high-performance liquid chromatography with diode-array detection, time-of-flight mass spectrometry and quadrupole ion trap mass spectrometry.

    PubMed

    Zhang, Hai; Gong, Chungui; Lv, Lei; Xu, Yuanjie; Zhao, Liang; Zhu, Zhenyu; Chai, Yifeng; Zhang, Guoqing

    2009-07-01

    High-performance liquid chromatography with diode-array detection (HPLC/DAD), time-of-flight mass spectrometry (HPLC/TOFMS) and quadrupole ion trap mass spectrometry (HPLC/QITMS) were used for separation, identification and structural analysis of furocoumarins in Angelica dahurica. Two furocoumarins (imperatorin and isoimperatorin) in Angelica dahurica extract were identified unambiguously by comparing their relative retention times, characteristic ultraviolet information and accurate mass measurement. A formula database of known furocoumarins in Angelica dahurica was established, against which the other 21 furocoumarins were identified effectively based on the accurate extract masses and formulae acquired by HPLC/TOFMS. In order to distinguish the isomers, multi-stage mass spectrometry (MSn, ion trap mass spectrometry) was used. General fragmentation behavior of the furocoumarins in the ion trap mass spectrometer was studied by the two furocoumarin standards, and their fragmentation rules in MS(n) spectra were summarized. These deduced fragmentation rules of furocoumarins were successfully implemented in distinguishing the three groups of isomers in Angelica dahurica by HPLC/QITMS. By using the three different analytical techniques, 23 furocoumarins in Angelica dahurica were tentatively identified within 30 min. Finally, HPLC/TOFMS fingerprints of Angelica dahurica were established by which it can be concluded that a rapid and effective method based on the three analytical techniques for identification of chemical components was established. This can provide help for further quality control of Angelica dahurica and pharmacology mechanism study of furocoumarins in Angelica dahurica.

  13. Use of microextraction by packed sorbent directly coupled to an electron ionization single quadrupole mass spectrometer as an alternative for non-separative determinations.

    PubMed

    Casas Ferreira, Ana María; Moreno Cordero, Bernardo; Pérez Pavón, José Luis

    2017-02-01

    Sometimes it is not necessary to separate the individual compounds of a sample to resolve an analytical problem, it is enough to obtain a signal profile of the sample formed by all the components integrating it. Within this strategy, electronic noses based on the direct coupling of a headspace sampler with a mass spectrometer (HS-MS) have been proposed. Nevertheless, this coupling is not suitable for the analysis of non-volatile compounds. In order to propose an alternative to HS-MS determinations for non-volatile compounds, here we present the first 'proof of concept' use of the direct coupling of microextraction by packed sorbents (MEPS) to a mass spectrometer device using an electron ionization (EI) and a single quadrupole as ionization source and analyzer, respectively. As target compounds, a set of analytes with different physic-chemical properties were evaluated (2-ethyl-1-hexanol, styrene, 2-heptanone, among others). The use of MEPS extraction present many advantages, such as it is fast, simple, easy to automate and requires small volumes of sample and organic solvents. Moreover, MEPS cartridges are re-usable as samples can be extracted more than 100 times using the same syringe. In order to introduce into the system all the elution volume from the MEPS extraction, a programmable temperature vaporizer (PTV) is proposed as the injector device. Results obtained with the proposed methodology (MEPS-PTV/MS) were compared with the ones obtained based on the separative scheme, i.e. using gas chromatography separation (MEPS-PTV-GC/MS), and both methods provided similar results. Limits of detection were found to be between 3.26 and 146.6μgL(-1) in the non-separative scheme and between 0.02 and 1.72μgL(-1) when the separative methodology was used. Repeatability and reproducibility were evaluated with values below 17% in all cases.

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

    PubMed

    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.

  15. A design study for a compact two stage in-flight separator with a high mass resolution and large acceptance

    SciTech Connect

    Hwang, Ji-Gwang; Kim, Eun-San; Hatanaka, Kichiji

    2015-03-15

    The rare isotope beam separator with a large angular acceptance and energy acceptance is essential for examining the characteristics of unstable nuclei and exotic nuclear reactions. Careful design, however, is required to compensate for the effects of high order aberrations induced by large aperture magnets, which are used to collect rare isotopes obtained from a high energy primary heavy-ion beam hitting a target. In order to minimize the effect of the high order aberration, the optics was based on the mirror symmetry optics, which provides smaller high order aberrations, for the separation of {sup 132}Sn produced by a fission reaction between the primary beam of {sup 238}U and a relatively thick Pb target. The designed optics provides energy acceptance (full), horizontal angular acceptance, and vertical acceptance of approximately 8%, 60 mrad, and 130 mrad, respectively.

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

    Technology Transfer Automated Retrieval System (TEKTRAN)

    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...

  17. UTILITY OF THREE TYPES OF MASS SPECTROMETERS FOR DETERMINING ELEMENTAL COMPOSITIONS OF IONS FORMED FROM CHROMATOGRAPHICALLY SEPARATED COMPOUNDS

    EPA Science Inventory

    Sponsor Referee: Douglas F. Barofsky, Oregon State University Concentration factors of 1000 and more reveal dozens of compounds in extracts of water supplies. Library mass spectra for most of these compounds are not available, and alternative means of identification are needed. D...

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

    PubMed

    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.

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

    PubMed

    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.

  20. Geoeffectiveness (D (sub st) and K (sub p)) of Interplanetary Coronal Mass Ejections During 1995-2009 and Implications for Storm Forecasting

    NASA Technical Reports Server (NTRS)

    Richardson, I. G.; Cane, H. V.

    2011-01-01

    We summarize the geoeffectiveness (based on the Dst and Kp indices) of the more than 300 interplanetary coronal mass ejections (ICMEs) that passed the Earth during 1996-2009, encompassing solar cycle 23. We subsequently estimate the probability that an ICME will generate geomagnetic activity that exceeds certain thresholds of Dst or Kp, including the NOAA "G" storm scale, based on maximum values of the southward magnetic field component (Bs), the solar wind speed (V), and the y component (Ey) of the solar wind convective electric field E = -V x B, in the ICME or sheath ahead of the ICME. Consistent with previous studies, the geoeffectiveness of an ICME is correlated with Bs or Ey approx.= VBs in the ICME or sheath, indicating that observations from a solar wind monitor upstream of the Earth are likely to provide the most reliable forecasts of the activity associated with an approaching ICME. There is also a general increase in geoeffectiveness with ICME speed, though the overall event-to-event correlation is weaker than for Bs and Ey. Nevertheless, using these results, we suggest that the speed of an ICME approaching the Earth inferred, for example, from routine remote sensing by coronagraphs on spacecraft well separated from the Earth or by all-sky imagers, could be used to estimate the likely geoeffectiveness of the ICME (our "comprehensive" ICME database provides a proxy for ICMEs identified in this way) with a longer lead time than may be possible using an upstream monitor

  1. Online matrix removal platform for coupling gel-based separations to whole protein electrospray ionization mass spectrometry.

    PubMed

    Kim, Ki Hun; Compton, Philip D; Tran, John C; Kelleher, Neil L

    2015-05-01

    A fractionation method called gel-eluted liquid fraction entrapment electrophoresis (GELFrEE) has been used to dramatically increase the number of proteins identified in top-down proteomic workflows; however, the technique involves the use of sodium dodecyl sulfate (SDS), a surfactant that interferes with electrospray ionization. Therefore, an efficient removal of SDS is absolutely required prior to mass analysis. Traditionally, methanol/chloroform precipitation and spin columns have been used, but they lack reproducibility and are difficult to automate. Therefore, we developed an in-line matrix removal platform to enable the direct analysis of samples containing SDS and salts. Only small molecules like SDS permeate a porous membrane and are removed in a manner similar to cross-flow filtration. With this device, near-complete removal of SDS is accomplished within 5 min and proteins are subsequently mobilized into a mass spectrometer. The new platform was optimized for the analysis of GELFrEE fractions enriched for histones extracted from human HeLa cells. All four core histones and their proteoforms were detected in a single spectrum by high-resolution mass spectrometry. The new method versus protein precipitation/resuspension showed 2- to 10-fold improved signal intensities, offering a clear path forward to improve proteome coverage and the efficiency of top-down proteomics.

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

    SciTech Connect

    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.

  3. Separation and characterization of phenolic compounds from U.S. pecans by liquid chromatography-tandem mass spectrometry.

    PubMed

    Robbins, Katherine S; Ma, Yuanyuan; Wells, M Lenny; Greenspan, Phillip; Pegg, Ronald B

    2014-05-14

    The phenolic acids and proanthocyanidins (PACs) of pecans possess bioactive properties, which might be useful in retarding the onset of and ameliorating the status of certain chronic disease states. There is a general lack of information in the literature regarding such compounds, especially the PACs. Crude phenolic extracts pooled from eight commercially significant cultivars were selected based on their relatively high antioxidant capacities. The pooled extracts were separated via Sephadex LH-20 column chromatography into five ethanolic low-molecular-weight (LMW) fractions and one acetonic high-molecular-weight (HMW) fraction. The preparations were then characterized using RP-HPLC-ESI-MS/MS and diol-phase HPLC-ESI-MS/MS in order to determine the key constituents present in the LMW and HMW fractions, respectively. As previously observed in pecan nutmeat, ellagic acid and (+)-catechin were found to be the major phenolics in the LMW fractions. The last eluting LMW fraction did not contain phenolic acids; rather it possessed PAC monomers and dimers. The HMW fraction comprised a majority of its PACs as dimers; yet, monomers, trimers, tetramers, pentamers, and hexamers were also separated and characterized.

  4. (211)Rn/(211)At and (209)At production with intense mass separated Fr ion beams for preclinical (211)At-based α-therapy research.

    PubMed

    Crawford, Jason R; Kunz, Peter; Yang, Hua; Schaffer, Paul; Ruth, Thomas J

    2017-04-01

    Mass-separated francium beams ((211)Fr or (213)Fr) were implanted into solid targets for producing (211)Rn (14.6h half-life) or (209)At (5.41h), in situ. (211)Rn was transferred to dodecane and isolated from contaminants, providing sources for (211)At (7.21h) production by (211)Rn decay (73%). (209)At was recovered with high radionuclidic purity in aqueous solutions, directly. These experiments demonstrated Fr beam implantations as a novel method for producing preclinical quantities of (211)Rn/(211)At (for therapy) and (209)At (for imaging).

  5. Application of different modes of thin-layer chromatography and mass spectrometry for the separation and detection of large and small biomolecules.

    PubMed

    Tuzimski, Tomasz

    2011-12-09

    Biomolecules are widespread throughout the world. A biomolecule is any organic molecule produced by a living organism, including large polymeric molecules such as proteins, polysaccharides and nucleic acids. Many sample preparation techniques are used in biomolecule analysis; the method selected depends on the complexity of the sample, the nature of the matrix and the analytes, and the analytical technique available. This review covers the current state of knowledge on thin-layer chromatography and mass spectrometry for qualitative analysis of biomolecules. In the first part of the paper the reader will gain useful information to avoid some problems about performing various modes of thin-layer chromatography combined with mass spectrometry experiments and in the second part he will find useful information for application of these techniques for separation, detection, and qualitative investigation of structures and quantitative determination of biomolecules such as proteins, peptides, oligonucleotides, amino acids, DNA, RNA, and lipids.

  6. Separation and identification of peptides from gel-isolated membrane proteins using a microfabricated device for combined capillary electrophoresis/nanoelectrospray mass spectrometry.

    PubMed

    Li, J; Kelly, J F; Chernushevich, I; Harrison, D J; Thibault, P

    2000-02-01

    The coupling of microfabricated devices to nanoelectrospray mass spectrometers using both a triple quadrupole and a quadrupole time-of-flight mass spectrometer (QqTOF MS) is presented for the analysis of trace-level membrane proteins. Short disposable nanoelectrospray emitters were directly coupled to the chip device via a low dead volume connection. The analytical performance of this integrated device in terms of sensitivity and reproducibility was evaluated for standard peptide mixtures. A concentration detection limit ranging from 3.2 to 43.5 nM for different peptides was achieved in selected ion monitoring, thus representing a 10-fold improvement in sensitivity compared to that of microelectrospray using the same chip/mass spectrometer. Replicate injections indicated that reproducibility of migration time was typically less than 3.1% RSD whereas RSD values of 6-13% were observed on peak areas. Although complete resolution of individual components is not typically achieved for complex digests, the present chip capillary electrophoresis (chip-CE) device enabled proper sample cleanup and partial separation of multicomponent samples prior to mass spectral identification. Analyses of protein digests were typically achieved in less than 1.5 min with peak widths of 1.8-2.5 s (half-height definition) as indicated from individual reconstructed ion electropherograms. The application of this chip-CE/QqTOF MS system is further demonstrated for the identification of membrane proteins which form a subset of the Haemophilus influenzae proteome. Bands first separated by 1D-gel electrophoresis were excised and digested, and extracted tryptic peptides were loaded on the chip without any further sample cleanup or on-line adsorption preconcentration. Accurate molecular mass determination (< 5 ppm) in peptide-mapping experiments was obtained by introducing an internal standard via a postseparation channel. The analytical potential of this integrated device for the identification of

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

    PubMed

    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.

  8. Study of chloropropanols in soy sauce by gas chromatography-triple quadrupole mass spectrometry with coupled column separation without derivatisation.

    PubMed

    Xu, X-M; Wu, H-W; He, H-L; Huang, B-F; Han, J-L; Ren, Y-P

    2013-01-01

    A qualitative and quantitative determination method for chloropropanols in soy sauce was developed by GC-MS/MS with coupled column separation without derivatisation. The target compounds were 1,3-dichloropropan-2-ol (1,3-DCP), 2,3-dichloropropan-1-ol (2,3-DCP), 3-monochloropropane-1,2-diol (3-MCPD) and 2-monochloropropane-1,3-diol (2-MCPD). 3-MCPD-d(5) was used as an isotope internal standard for MCPDs and 1,3-DCP-d(5) for DCPs. After spiking with internal standards and mixed with 1 g of Extrelut™ NT, about 1 g of the sample was washed by 4 ml of hexane and the analytes were eluted with 15 ml of 95% (v/v) ethyl ether/hexane mixture. The concentrated extract was directly injected without derivatisation, separated by a coupled column - a 3 m Innowax (polyethylene glycol) combined with a 30 m DB-5 ms ((5%-phenyl)-methylpolysiloxane) by a quartz capillary column connector - and detected by GC-MS/MS. The limits of detection (LODs) in the sample matrix were 1.0, 2.5, 5.0 and 5.0 µg kg(-1) for the above chloropropanols, respectively. The relative proportions of 2-MCPD/3-MCPD ranged from 0.19 to 3.74 in soy sauce samples. 2,3-DCP and 2-MCPD were more stable than 1,3-DCP and 3-MCPD under alkaline condition. The levels of chloropropanols can be decreased by an alkaline treatment process.

  9. Separation and identification of an oligomeric light stabilizer Chimassorb 944 by gradient elution chromatography coupled with matrix-assisted laser desorption/ionization mass spectrometry.

    PubMed

    Kong, Xiu; Diao, Xingli; Wan, Qian-Hong

    2014-10-17

    A non-aqueous reversed-phase high-performance liquid chromatographic (HPLC) method has been developed to separate a light stabilizer Chimassorb 944 into individual oligomers, which are further identified using pre-column fluorescent derivatization and matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS). Consistent with previous studies, we find that the Chimassorb 944 product is a complex mixture consisting of a homologous series with the amine end groups and the number of repeat units (n) span from 1 to 26. In addition to the dominant linear species, cyclic oligomers are present at relatively high levels in the low-mass range. Their concentration decreases rapidly with the length of the oligomer backbone and becomes undetectable when n>7. Moreover, comparison of the HPLC and MALDI-MS molar mass distributions of Chimassorb 944 shows that the HPLC analysis produces greater molar mass averages and thus offers an effective means for accurate measure of the relative abundances of the oligomers.

  10. Biological control of sentinel egg masses of the exotic invasive stink bug halyomorpha halys (Stål) in Mid-Atlantic USA ornamental landscapes

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Biological invasions have far reaching effects on native plant and arthropod communities. This study evaluated the effect of natural enemies on eggs of the exotic invasive stink bug Halyomorpha halys (Stål) in experimental plots comprising species pairs of 16 ornamental trees and shrub genera from e...

  11. Use of liquid chromatography- quadrupole time-of-flight mass spectrometry for enantioselective separation and determination of pyrisoxazole in vegetables, strawberry and soil.

    PubMed

    Qi, Peipei; Yuan, Yuwei; Wang, Zhiwei; Wang, Xiangyun; Xu, Hao; Zhang, Hu; Wang, Qiang; Wang, Xinquan

    2016-06-03

    The present work firstly described the enantio-separation and determination of pyrisoxazole enantiomers in vegetables, strawberry and soil samples by chiral liquid chromatography coupled to quadrupole time-of-flight mass spectrometry (LC-Q-TOF/MS). Pyrisoxazole has two chiral carbon atoms and consists of four stereoisomers. Taking the specific optical rotation measurement and MS analysis data into consideration, the four enantiomers were discriminated as (-)-A, (+)-A, (+)-B and (-)-B corresponding to their elution order under the optimum chromatographic condition. Influences of the mobile phase and column temperature on the enantio-separation selectivity of pyrisoxazole were explored. The perfect baseline separation of pyrisoxazole enantiomers can be achieved within 10min using methanol- water (70:30, v/v) as mobile phase on chiral Lux Cellulose-3 column. The thermodynamic analysis demonstrated that the enantioseparation of (-)-A and (+)-A, (+)-A and (+)-B were enthalpy driven separation, while the enantioseparation of (+)-B and (-)-B was entropy driven separation. Under the optimum method, method validation including matrix effect, linearity, sensitivity and precision were performed. At the spiked concentration of 10, 50 and 100μgkg(-1), the recoveries of the pyrisoxazole enantiomers in cucumber, tomato, pakchoi, pepper and strawberry samples were 64.2-100% (RSD≤14%); While they were relatively higher in soil samples and all around 120% (RSD ≤10%). The limits of detection are in the range from 0.2 to 1.0μgkg(-1) for cucumber, tomato, pakchoi, pepper, strawberry and soil samples. The developed method was then utilized for monitoring the degradation kinetics of pyrisoxazole enantiomers in strawberry under field trials, which provided the environmental behavior data of chiral pyrisoxazole enantiomers and consequently for further health risk assessment of the chiral pesticides.

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

    PubMed

    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 < 3 % and RSD < 6 %, respectively. The method was applied in order to determine carotenoids in 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.

  13. Background correction in separation techniques hyphenated to high-resolution mass spectrometry - Thorough correction with MS scans recorded as profile spectra.

    PubMed

    Erny, Guillaume L; Acunha, Tanize; Simó, Carolina; Cifuentes, Alejandro; Alves, Arminda

    2017-03-01

    Separation techniques hyphenated with high-resolution mass spectrometry have been a true revolution in analytical separation techniques. Such instruments not only provide unmatched resolution, but they also allow measuring the peaks accurate masses that permit identifying monoisotopic formulae. However, data files can be large, with a major contribution from background noise and background ions. Such unnecessary contribution to the overall signal can hide important features as well as decrease the accuracy of the centroid determination, especially with minor features. Thus, noise and baseline correction can be a valuable pre-processing step. The methodology that is described here, unlike any other approach, is used to correct the original dataset with the MS scans recorded as profiles spectrum. Using urine metabolic studies as examples, we demonstrate that this thorough correction reduces the data complexity by more than 90%. Such correction not only permits an improved visualisation of secondary peaks in the chromatographic domain, but it also facilitates the complete assignment of each MS scan which is invaluable to detect possible comigration/coeluting species.

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

    PubMed

    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.

  15. Separation of stereoisomers of several furan derivatives by capillary gas chromatography-mass spectrometry, supercritical fluid chromatography, and liquid chromatography using chiral stationary phases.

    PubMed

    Kasai, Hiroko F; Tsubuki, Masayoshi; Takahashi, Kazunori; Shirao, Mika; Matsumoto, Yohichiro; Honda, Toshio; Seyama, Yoshiyuki

    2002-11-15

    The direct separation of several stereoisomers (enantiomers and geometrical isomers) of furan derivatives, important intermediates for the synthesis of physiologically active natural products, was achieved using capillary gas chromatography/mass spectrometry with a per-O-methyl-beta-cyclodextrin, supercritical fluid chromatography and high-performance liquid chromatography with a tris(3,5-dimethylphenylcarbamate) of cellulose or amylose for the chiral stational phases, respectively. The temperature dependence of the peak resolution (Rs) and the retention factor (k) over the range of 110-130 degrees was studied using crotyl furfuryl ether in gas chromatography. Successive increases in the Rs value and of the difference between the k value of the E-isomer and the k value of the Z-isomer were observed when the gradient temperature was decreased. The per-O-methyl-beta-cyclodextrin column was suitable for use with volatile furan ethers whose molecular masses are between 150 and 180. In conclusion, the separation of thermally unstable furan derivatives was accomplished using supercritical fluid chromatography and high-performance liquid chromatography.

  16. A protein molecular weight map of ES2 clear cell ovarian carcinoma cells using a two-dimensional liquid separations/mass mapping technique.

    PubMed

    Wang, Haixing; Kachman, Maureen T; Schwartz, Donald R; Cho, Kathleen R; Lubman, David M

    2002-09-01

    A molecular weight map of the protein content of ES2 human clear cell ovarian carcinoma cells has been produced using a two-dimensional (2-D) liquid separations/mass mapping technique. This method uses a 2-D liquid separation of proteins from whole cell lysates coupled on-line to an electrospray ionization-time of flight (ESI-TOF) mass spectrometer to map the accurate intact molecular weight (M(r)) of the protein content of the cells. The two separation dimensions involve the use of liquid isoelectric focusing as the first phase and nonporous silica reversed-phase high-performance liquid chromatography (HPLC) as the second phase of separation. The detection by ESI-TOF-MS provides an image of pI versus M(r) analogous to 2-D gel electrophoresis. Each protein is then identified based upon matrix-assisted laser desorption/ionization (MALDI)-TOF-MS peptide mapping and intact M(r) so that a standard map is produced against which other ovarian carcinoma cell lines can be compared. The accurate intact M(r) together with the pI fraction, and peptide map serve to tag the protein for future interlysate comparisons. An internal standard is also used to provide a means for quantitation for future interlysate studies. In the ES2 cell line under study it is shown that nearly 900 M(r) bands are detected over 17 pI fractions from pH 4 to 12 and a M(r) range up to 85 kDa and that around 290 of these bands can be identified using mass spectrometric based techniques. The protein M(r) is detected within an accuracy of 150 ppm and it is shown that many of the proteins in this human cancer sample are modified compared to the database. The protein M(r) map may serve as a highly reproducible standard Web-based method for comparing proteins from related human cell lines.

  17. Characterization of Diesel Fuel by Chemical Separation Combined with Capillary Gas Chromatography (GC) Isotope Ratio Mass Spectrometry (IRMS)

    SciTech Connect

    Harvey, Scott D.; Jarman, Kristin H.; Moran, James J.; Sorensen, Christina M.; Wright, Bob W.

    2011-09-15

    The purpose of this study was to perform a preliminary investigation of compound-specific isotope analysis (CSIA) of diesel fuels to evaluate whether the technique could distinguish between the diesel samples from different sources/locations. The ability to differentiate or correlate diesel samples could be valuable for detecting fuel tax evasion schemes. Two fractionation techniques were used to isolate the n-alkanes from the fuel. Both δ13C and δD values for the n-alkanes were then determined by CSIA in each sample. Plots of δD versus δ13C with sample n-alkane points connected in order of increasing carbon number gave well separated clusters with characteristic shapes for each sample. Principal components analysis (PCA) with δ13C, δD, or combined δ13C and δD data on the yielded scores plots that could clearly differentiate the samples, thereby demonstrating the potential of this approach for fingerprinting fuel samples using the δ13C and δD values.

  18. Structural characterization of synthetic polymers and copolymers using multidimensional mass spectrometry interfaced with thermal degradation, liquid chromatography and/or ion mobility separation

    NASA Astrophysics Data System (ADS)

    Alawani, Nadrah

    This dissertation focuses on coupling mass spectrometry (MS) and tandem mass spectrometry (MS/MS) to thermal degradation, liquid chromatography (LC) and/or ion mobility (IM) spectrometry for the characterization of complex mixtures. In chapter II, an introduction of the history and the principles of MS and LC are discussed. Chapter III illustrates the materials and instrumentation used to complete this dissertation. Polyethers have been characterized utilizing MS/MS, as presented in Chapter IV and Chapter VI. Diblock copolymers of polyethylene oxide and polycaprolactone, PEO-b-PCL, have been characterized by matrix-assisted laser desorption/ionization quadrupole/time-of-flight mass spectrometry (MALDI-Q/ToF) and LC-MS/MS (Chapter V). Thermoplastic elastomers have been characterized by thermal degradation using an atmospheric solids analysis probe (ASAP) and ion mobility mass spectrometry (IM-MS), as discussed in Chapter VII. Interfacing separation techniques with mass spectrometry permitted the detection of species present with low concentration in complex materials and improved the sensitivity of MS. In chapter IV, the fragmentation mechanisms in MS/MS experiments of cyclic and linear poly(ethylene oxide) macroinitiators are discussed. This study aimed at determining the influence of end groups on the fragmentation pathways. In the study reported in Chapter V, ultra high performance liquid chromatography (UHPLC) was interfaced with MS and MS/MS to achieve the separation and in-depth characterization and separation of amphiphilic diblock copolymers (PEO- b-PCL) in which the architecture of the PEO block is linear or cyclic. Applying UPLC-MS and UPLC-MS/MS provides fast accurate information about the number and type of the blocks in the copolymers. Chapter VI reports MS/MS and IM-MS analyses which were performed to elucidate the influence of molecular size and collision energy on the fragmentation pathways of polyethers subjected to collisionally activated

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

    PubMed

    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.

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

    PubMed

    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

  1. St. Lucia.

    PubMed

    1987-06-01

    The population of St Lucia was 123,000 in 1986, with an annual growth rate of 2%. The infant mortality rate stands at 22.2/1000 live births, and life expectancy is 70.3 years for males and 74.9 years for females. The literacy rate is 78%. St Lucia's labor force is allocated as follows: agriculture, 36.6%; industry and commerce, 20.1%; and services, 18.1%. The gross national product (GNP) was US$146 million in 1985, with an annual growth rate of 3% and a per capita GNP of $1071. St Lucia is a parliamentary democracy modeled on the British Westminster system. The island is divided into 16 parishes and 1 urban area (the capital, Castries). St Lucia is currently a politically stable country, although the high level of youth unemployment is a cause for concern. Ongoing stability may depend on the government's ability to provide services such as jobs and housing. The economy has evolved from a monocrop sugar plantation type to a diversified economy based on agriculture, industry, and tourism. Agriculture, dominated by the banana industry, is characterized by the participation of a large number of small and medium-sized enterprises. Industry is being encouraged through the provision of incentives such as tax rebates. The government is attempting to maintain a sound investment climate through a tripartite dialogue with the private sector and trade unions. Overall economic policy is predicated on the attraction of sound investments, by both local and foreign entities, to accelerate the rate of economic growth, solve the unemployment problem, and generate a solid balance-of-payments position.

  2. Comparative Proteome Analyses of Human Plasma Following in vivo Lipopolysaccharide Administration Using Multidimensional Separations Coupled with Tandem Mass Spectrometry

    PubMed Central

    Qian, Wei-Jun; Jacobs, Jon M.; Camp, David G.; Monroe, Matthew E.; Moore, Ronald J.; Gritsenko, Marina A.; Calvano, Steve E.; Lowry, Stephen F.; Xiao, Wenzhong; Moldawer, Lyle L.; Davis, Ronald W.; Tompkins, Ronald G.; Smith, Richard D.

    2007-01-01

    There is significant interest in characterization of the human plasma proteome due to its potential for providing biomarkers applicable to clinical diagnosis and treatment and for gaining a better understanding of human diseases. We describe here a strategy for the comparative proteome analyses of human plasma, which is applicable to biomarker identifications for various disease states. Multidimensional liquid chromatography-mass spectrometry has been applied to make comparative proteome analyses of plasma samples from an individual prior to and 9 h after lipopolysaccharide (LPS) administration. Peptide peak areas and the number of peptide identifications for each protein were used to evaluate the reproducibility of LC-MS/MS and to compare relative changes in protein concentration between the samples following LPS treatment. A total of 804 distinct plasma proteins (not including immunoglobulins) were confidently identified with 32 proteins observed to be significantly increased in concentration following LPS administration, including several known inflammatory response or acute-phase mediators such as C-reactive protein, serum amyloid A and A2, LPS-binding protein, LPS-responsive and beige-like anchor protein, hepatocyte growth factor activator, and von Willebrand factor, and thus constituting potential biomarkers for inflammatory response. PMID:15627965

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

    PubMed

    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.

  4. Optimization of separation and detection conditions for the multiresidue analysis of pesticides in grapes by comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry.

    PubMed

    Banerjee, Kaushik; Patil, Sangram H; Dasgupta, Soma; Oulkar, Dasharath P; Patil, Shubhangi B; Savant, Rahul; Adsule, Pandurang G

    2008-05-09

    A comprehensive GCxGC-TOFMS method was optimized for multiresidue analysis of pesticides using a combination of a non-polar (RTX-5MS, 10 m x 0.18 mm x 0.2 microm) and a polar capillary column (TR-50MS, 1 m x 0.1 mm x 0.1 microm), connected in series through a dual stage thermal modulator. The method resolved the co-elution problems as observed in full scan one-dimensional GC-MS analysis and allowed chromatographic separation of 51 pesticides within 24 min run time with library-searchable mass spectrometric confirmation. Four pesticides, viz. chlorpyrifos-methyl, vinclozoline, parathion-methyl and heptachlor could be baseline separated on GCxGC, which were otherwise closely eluting and interfering each other's detection in 1D GC-MS run. Similarly, it could be possible to separate myclobutanil, buprofezin, flusilazole and oxyfluorfen on GCxGC. Although in 1D GC-MS, these closely eluting compounds could be identified through deconvolution algorithm and 'peak-find' option of the Chromatof software but the spectral purity significantly improved on GCxGC analysis. Thorough optimization was accomplished for the oven temperature programming, ion source temperature and GCxGC parameters like modulation period, duration of hot pulses, modulation-offset temperature, acquisition rate, etc. to achieve best possible separation of the test compounds. The limit of detection significantly improved by 2-12 times on GCxGC-TOFMS against GC-TOFMS because of sharper and narrower peak shapes. The method was tested for grape matrix after preparing the samples using previously described method and recoveries of the entire test pesticides were within 70-110% at 10 ng/g level of fortification. GCxGC-TOFMS was found to be an excellent technique for library-based screening of pesticides with high accuracy and sensitivity.

  5. Separation and fragmentation study of isocoproporphyrin derivatives by UHPLC-ESI-exact mass MS/MS and identification of a new isocoproporphyrin sulfonic acid metabolite.

    PubMed

    Benton, Christopher M; Lim, Chang Kee; Moniz, Caje; Baxter, Sinéad L; Jones, Donald J L

    2014-01-01

    Isocoproporphyrin and its derivatives are commonly used as biomarkers of porphyria cutanea tarda, heavy metal toxicity and hexachlorobenzene (HCB) intoxication in humans and animals. However, most are isobaric with other porphyrins and reference materials are unavailable commercially. The structural characterisation of these porphyrins is important but very little data is available. We report here the separation and characterisation of isocoproporphyrin, deethylisocoproporphyrin, hydroxyisocoproporphyrin and ketoisocoproporphyrin, isolated in the faeces of rats fed with a diet containing HCB, by ultra high performance liquid chromatography-exact mass tandem mass spectrometry (UHPLC-MS/MS). Furthermore, we report the identification and characterisation of a previously unreported porphyrin metabolite, isocoproporphyrin sulfonic acid isolated in the rat faeces. The measured mass-to-charge ratio (m/z) of the precursor ion was m/z 735.2338, corresponding to a molecular formula of C36H39N4O11S with an error of 0.3 ppm from the calculated m/z 735.2336. The MS/MS data was consistent with an isocoproporphyrin sulfonic acid structure, derived from dehydroisocoproporphyrinogen by sulfonation of the vinyl group. The metabolite was present in a greater abundance than other isocoproporphyrin derivatives and may be a more useful biomarker for HCB intoxication.

  6. 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.

    PubMed

    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.

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

    NASA Astrophysics Data System (ADS)

    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.

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

    PubMed

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

    2008-09-15

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

  9. A rapid method for the separation of vitamin D and its metabolites by ultra-high performance supercritical fluid chromatography-mass spectrometry.

    PubMed

    Jumaah, Firas; Larsson, Sara; Essén, Sofia; Cunico, Larissa P; Holm, Cecilia; Turner, Charlotta; Sandahl, Margareta

    2016-04-01

    In this study, a new supercritical fluid chromatography-mass spectrometry (SFC-MS) method has been developed for the separation of nine vitamin D metabolites within less than eight minutes. This is the first study of analysis of vitamin D and its metabolites carried out by SFC-MS. Six columns of orthogonal selectivity were examined, and the best separation was obtained by using a 1-aminoanthracene (1-AA) column. The number and the position of hydroxyl groups in the structure of the studied compounds as well as the number of unsaturated bonds determine the physiochemical properties and, thus the separation of vitamin D metabolites that is achieved on this column. All D2 and the D3 forms were baseline separated with resolution values>1.5. The effects of pressure, temperature, flow rate and different gradient modes were studied. Electrospray ionization (ESI) and atmospheric pressure chemical ionization (APCI) were compared in positive mode, both by direct infusion and after SFC separation. The results showed that the sensitivity in APCI(+) was higher than in ESI(+) using direct infusion. In contrast, the sensitivity in APCI(+) was 6-fold lower than in ESI(+) after SFC separation. The SFC-MS method was validated between 10 and 500ng/mL for all analytes with coefficient of determination (R(2))≥0.999 for all calibration curves. The limits of detection (LOD) were found to range between 0.39 and 5.98ng/mL for 24,25-dihydroxyvitamin D3 (24,25(OH)2D3) and 1-hydroxyvitamin D2 (1OHD2), respectively. To show its potential, the method was applied to human plasma samples from healthy individuals. Vitamin D3 (D3), 25-hydroxyvitamin D3 (25OHD3) and 24,25(OH)2D3 were determined in plasma samples and the concentrations were 6.6±3.0ng/mL, 23.8±9.2ng/mL and 5.4±2.7ng/mL, respectively.

  10. A WIDELY SEPARATED, HIGHLY OCCLUDED COMPANION TO THE NEARBY LOW-MASS T TAURI STAR TWA 30

    SciTech Connect

    Looper, Dagny L.; Pitts, Mark A.; Bochanski, John J.; Burgasser, Adam J.; Mohanty, Subhanjoy; Mamajek, Eric E.; Faherty, Jacqueline K.; West, Andrew A.

    2010-11-15

    We report the discovery of TWA 30B, a wide ({approx}3400 AU), co-moving M dwarf companion to the nearby ({approx}42 pc) young star TWA 30. Companionship is confirmed from their statistically consistent proper motions and radial velocities (RVs), as well as a chance alignment probability of only 0.08%. Like TWA 30A, the spectrum of TWA 30B shows signatures of an actively accreting disk (H I and alkali line emission) and forbidden emission lines tracing outflowing material ([O I], [O II], [O III], [S II], and [N II]). We have also detected [C I] emission in the optical data, marking the first such detection of this line in a pre-main-sequence star. Negligible RV shifts in the emission lines relative to the stellar frame of rest ({Delta}V {approx}< 30 km s{sup -1}) indicate that the outflows are viewed in the plane of the sky and that the corresponding circumstellar disk is viewed edge-on. Indeed, TWA 30B appears to be heavily obscured by its disk, given that it is 5 mag fainter than TWA 30A at K band despite having a slightly earlier spectral type (M4 versus M5). The near-infrared spectrum of TWA 30B also evinces an excess that varies on day timescales, with colors that follow classical T Tauri tracks as opposed to variable reddening (as is the case for TWA 30A). Multi-epoch data show this excess to be well modeled by a black body component with temperatures ranging from 630 to 880 K and emitting areas that scale inversely with the temperature. The variable excess may arise from disk structure such as a rim or a warp at the inner disk edge located at a radial distance of {approx}3-5 R{sub sun}. As the second and third closest actively accreting and outflowing stars to the Sun (after TWA 3), TWA 30AB presents an ideal system for a detailed study of star and planetary formation processes at the low-mass end of the hydrogen-burning spectrum.

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

    SciTech Connect

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

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

    SciTech Connect

    Ognibene, Theodore Joseph

    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.

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

    NASA Astrophysics Data System (ADS)

    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

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

    NASA Astrophysics Data System (ADS)

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

    2014-10-01

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

  15. Cod (Gadus morhua) muscle proteome cataloging using 1D-PAGE protein separation, nano-liquid chromatography peptide fractionation, and linear trap quadrupole (LTQ) mass spectrometry.

    PubMed

    Gebriel, Mohammed; Uleberg, Kai-Erik; Larssen, Eivind; Bjørnstad, Anne Hjelle; Sivertsvik, Morten; Møller, Simon Geir

    2010-12-08

    Because Atlantic cod (Gadus morhua) has high economic value and its protein-rich muscle tissue is a food source, an increased understanding of the effects and consequences of environmental, nutritional, biological, and industrial factors on meat quality is necessary. To gain insight into cod muscle tissue protein composition, a large-scale proteomics approach has been used. One-dimensional polyacrylamide gel electrophoresis, nanoflow liquid chromatography peptide separation, and linear trap quadrupole mass spectrometry were used to identify 4804 peptides, which retrieved 9113 cod expressed sequence tags (ESTs), which in turn were mapped to 446 unique proteins. The same data set identified 3924 proteins from the zebrafish protein database, which highlights the complementary value of the two approaches. The generated data sets will act as a foundation for studies related to physiological status assessment of cod under different environmental conditions, screening for diseases, and biomarker identification for assessment of fish quality during industrial processing and preservation.

  16. Femtomolar concentration detection limit and zeptomole mass detection limit for protein separation by capillary isoelectric focusing and laser-induced fluorescence detection.

    PubMed

    Ramsay, Lauren M; Dickerson, Jane A; Dada, Oluwatosin; Dovichi, Norman J

    2009-03-01

    Fluorescence tends to produce the lowest detection limits for most forms of capillary electrophoresis. Two issues have discouraged its use in capillary isoelectric focusing. The first issue is fluorescent labeling of proteins. Most labeling reagents react with lysine residues and convert the cationic residue to a neutral or anionic product. At best, these reagents perturb the isoelectric point of the protein. At worse, they convert each protein into hundreds of different fluorescent products that confound analysis. The second issue is the large background signal generated by impurities within commercial ampholytes. This background signal is particularly strong when excited in the blue portion of the spectrum, which is required by many common fluorescent labeling reagents. This paper addresses these issues. For labeling, we employ Chromeo P540, which is a fluorogenic reagent that converts cationic lysine residues to cationic fluorescent products. The reaction products are excited in the green, which reduces the background signal generated by impurities present within the ampholytes. To further reduce the background signal, we photobleach ampholytes with high-power photodiodes. Photobleaching reduced the noise in the ampholyte blank by an order of magnitude. Isoelectric focusing performed with photobleached pH 3-10 ampholytes produced concentration detection limits of 270 +/- 25 fM and mass detection limits of 150 +/- 15 zmol for Chromeo P540 labeled beta-lactoglobulin. Concentration detection limits were 520 +/- 40 fM and mass detection limits were 310 +/- 30 zmol with pH 4-8 ampholytes. A homogenate was prepared from a Barrett's esophagus cell line and separated by capillary isoelectric focusing, reproducibly generating dozens of peaks. The sample taken for the separation was equal to the labeled protein homogenate from three cells.

  17. ST - SCHEDULE TRACKER COMPUTER PROGRAM

    NASA Technical Reports Server (NTRS)

    Collazo, F. F.

    1994-01-01

    The Schedule Organizer, SO (COSMIC Program MSC-21525), Schedule Tracker, ST, and Schedule Report Generator, SRG (COSMIC Program MSC-21527), are programs that manipulate data base files in ways that are advantageous to scheduling applications. Originally designed for the Space Shuttle flight schedule, the program can be easily modified for other scheduling situations. Schedule Organizer provides a simple method for generating distribution lists. These distribution lists contain readers' names for each task schedule defined by the input files. Schedule Tracker provides an effective method for tracking tasks that are 'past due' and/or 'near term'. ST generates reports for each responsible staff member with one or more assigned tasks that fall within the two listed categories. This enables an engineering manager to monitor tasks assigned to staff by running ST on a weekly basis. ST only lists tasks on reports that have become past due or are scheduled for recent completion (near term). Schedule Report Generator provides a simple method for generating periodic schedule reports. ST and SRG use the same data base file as input. The common data base file has a maximum number of 400 entries. The time span of all three programs is nineteen months. Both of these maximum numbers can be modified by the user. ST requires the VMS Operating System on DEC VAX and was written in PL/1 and DEC Command Language (DCL). The program requires a memory of 233KB. ST can be purchased separately or in a package (COSMIC Program COS-10021) containing SO, ST, and SRG. ST was developed in 1985.

  18. Separation and measurement of Pa, Th, and U isotopes in marine sediments by microwave-assisted digestion and multiple collector inductively coupled plasma mass spectrometry.

    PubMed

    Negre, César; Thomas, Alexander L; Mas, José Luis; Garcia-Orellana, Jordi; Henderson, Gideon M; Masqué, Pere; Zahn, Rainer

    2009-03-01

    This manuscript describes a new protocol for determination of Pa/Th/U in marine sediments. It is based on microwave-assisted digestion and represents an important reduction of working time over conventional hot-plate digestion methods, and the use of HClO(4) is avoided. Although Th and U are completely dissolved with a first microwave step, around 40% of (231)Pa remains undissolved, and a short hot-plate step with reverse aqua regia is required to achieve total digestion and spike equilibration. Next, the method involves a separation of these elements and a further purification of the Pa fraction using Dowex AG1-X8 resin. Separation with Bio-Rad and Sigma-Aldrich resins was compared; although both perform similarly for Th and U, Pa yields are higher with Bio-Rad. Finally, samples are measured using a Nu instruments multiple collector inductively coupled plasma mass spectrometer (MC-ICPMS). Overall chemical yields range around 50% for Pa, 60% for Th, and 70% for U.

  19. Polar Aprotic Modifiers for Chromatographic Separation and Back-Exchange Reduction for Protein Hydrogen/Deuterium Exchange Monitored by Fourier Transform Ion Cyclotron Resonance Mass Spectrometry

    NASA Astrophysics Data System (ADS)

    Valeja, Santosh G.; Emmett, Mark R.; Marshall, Alan G.

    2012-04-01

    Hydrogen/deuterium exchange monitored by mass spectrometry is an important non-perturbing tool to study protein structure and protein-protein interactions. However, water in the reversed-phase liquid chromatography mobile phase leads to back-exchange of D for H during chromatographic separation of proteolytic peptides following H/D exchange, resulting in incorrect identification of fast-exchanging hydrogens as unexchanged hydrogens. Previously, fast high-performance liquid chromatography (HPLC) and supercritical fluid chromatography have been shown to decrease back-exchange. Here, we show that replacement of up to 40% of the water in the LC mobile phase by the modifiers, dimethylformamide (DMF) and N-methylpyrrolidone (NMP) (i.e., polar organic modifiers that lack rapid exchanging hydrogens), significantly reduces back-exchange. On-line LC micro-ESI FT-ICR MS resolves overlapped proteolytic peptide isotopic distributions, allowing for quantitative determination of the extent of back-exchange. The DMF modified solvent composition also improves chromatographic separation while reducing back-exchange relative to conventional solvent.

  20. Polar Aprotic Modifiers for Chromatographic Separation and Back-Exchange Reduction for Protein Hydrogen/Deuterium Exchange Monitored by Fourier Transform Ion Cyclotron Resonance Mass Spectrometry

    PubMed Central

    Valeja, Santosh G.; Emmett, Mark R.; Marshall, Alan G.

    2013-01-01

    Hydrogen/deuterium exchange monitored by mass spectrometry is an important non-perturbing tool to study protein structure and protein–protein interactions. However, water in the reversed-phase liquid chromatography mobile phase leads to back-exchange of D for H during chromatographic separation of proteolytic peptides following H/D exchange, resulting in incorrect identification of fast-exchanging hydrogens as unexchanged hydrogens. Previously, fast high-performance liquid chromatography (HPLC) and supercritical fluid chromatography have been shown to decrease back-exchange. Here, we show that replacement of up to 40% of the water in the LC mobile phase by the modifiers, dimethylformamide (DMF) and N-methylpyrrolidone (NMP) (i.e., polar organic modifiers that lack rapid exchanging hydrogens), significantly reduces back-exchange. On-line LC micro-ESI FT-ICR MS resolves overlapped proteolytic peptide isotopic distributions, allowing for quantitative determination of the extent of back-exchange. The DMF modified solvent composition also improves chromatographic separation while reducing back-exchange relative to conventional solvent. PMID:22298288

  1. [Study on the method of nanometer-size zirconium dioxide enrichment separation and inductively coupled plasma mass spectrometry determination of trace barium(II) in water].

    PubMed

    Du, Ying-Qiu; Yin, Yi-Dong; Fan, Nai-Ying; Chen, Peng-Gang; Zhang, Xiao-Bo; Ren, Hong-Bo; Chen, Guo-You; Qu, Qiu-Yao; Sun, Zhi-Bo; Chen, Yue-Xin

    2012-11-01

    Monoclinic fusiform zirconium dioxide (ZrO2) nanoparticles were synthesized by hydrothermal method, a method was established based on monoclinic fusiform nanometer-sized ZrO2 enrichment separation, and trace barium in water was determined by inductively coupled plasma mass spectrometry (ICP-MS). The detection limit for Ba(II) was 0.007 ng x mL(-1), and the relative standard deviation was 0.13% (n = 11). The optimal enrichment separation conditions of nanometer-sized ZrO2 for Ba(II) were studied in detail, it was found that the percentage of adsorbed Ba(II) was more than 99% under pH 10.0 and 2 mL 0.5 mol x L(-1) HCl was sufficient for elution of Ba(II) by more than 98%. The static adsorption capacity of ZrO2 to Ba(II) was 196.6 microg x g(-1) and enrichment factor was 250. Properties of nanometer-sized ZrO2 were discussed through regeneration experiment and effects of co-existing ions and contrast experiment to ordinary ZrO2, adsorption properties of nanometer-sized ZrO2 were applied to real samples in the analysis of Ba(II) and the determination was carried out by ICP-MS with satisfactory results.

  2. Separation and identification of underivatized plasma acylcarnitine isomers using liquid chromatography-tandem mass spectrometry for the differential diagnosis of organic acidemias and fatty acid oxidation defects.

    PubMed

    Peng, Minzhi; Fang, Xiefan; Huang, Yonglan; Cai, Yanna; Liang, Cuili; Lin, Ruizhu; Liu, Li

    2013-12-06

    A simple HPLC-MS/MS method has been established to separate and identify underivatized acylcarnitine isomers. Human plasma samples were deproteinized and concentrated. Acylcarnitines were separated on a reverse phase column and detected with triple quadrupole linear ion trap mass spectrometry. Deuterium-labeled internal standards were used for quantitation. To identify acylcarnitines without pure standards, information-dependent acquisition linking to enhanced product ion scan mode was used. 112 acylcarnitines, including stereoisomers, were found in samples of patients. Dicarboxylic acylcarnitines, such as methylmalonylcarnitine and glutarylcarnitine, were detected with high sensitivity. Three stereoisomers of (R,S)2-methyl-3-hydroxy butyrylcarnitine were detected in samples of patients with β-ketothiolase deficiency. Validation results revealed excellent precision and accuracy of the method. In general the within- and between-run coefficients of variation (CV%) were less than 15%, and recoveries were in the range of 92.7-117.5%. In addition, the reference intervals of acylcarnitines for children aged 3-day to13-year old were established. Using the new method and reference intervals, we have correctly diagnosed 49 patients with fatty acid oxidation defects or organic acidemias in 176 high-risk patients.

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

    PubMed

    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.

  4. Thin layer chromatography/plasma assisted multiwavelength laser desorption ionization mass spectrometry for facile separation and selective identification of low molecular weight compounds.

    PubMed

    Zhang, Jialing; Zhou, Zhigui; Yang, Jianwang; Zhang, Wei; Bai, Yu; Liu, Huwei

    2012-02-07

    A novel plasma assisted multiwavelength (1064, 532, and 355 nm) laser desorption ionization mass spectrometry (PAMLDI-MS) system was fabricated and applied in the analysis of low molecular weight compounds through combination with thin layer chromatography (TLC). The TLC/PAMLDI-MS system successfully integrated TLC, the multiwavelength laser ablation, and the excitated state plasma from direct analysis in real time (DART) and was proved to be effective in the facile separation and selective identification of low molecular weight compounds. An automated three-dimensional platform was utilized to facilitate the analysis procedures with all the parameters of the TLC/PAMLDI-MS systematically optimized, and the desorption/ionization mechanisms were discussed. The successful combination of three-wavelength laser with DART based system extended the range of the analytes and provided broad possibilities for the compound desorption from the TLC. The experimental results clearly showed that the laser desorption was wavelength dependent. The PAMLDI-MS system was successfully applied in the detection of low molecular weight compounds from different kinds of samples separated on a normal-phase silica gel, such as dye mixtures, drug standards, and tea extract, with the detection level of 5 ng/mm(2).

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

    PubMed

    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.

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

    PubMed

    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.

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

    USGS Publications Warehouse

    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.

  8. Benefits of prolonged gradient separation for high-performance liquid chromatography-tandem mass spectrometry quantitation of plasma total 15-series F-isoprostanes.

    PubMed

    Taylor, Alan W; Bruno, Richard S; Frei, Balz; Traber, Maret G

    2006-03-01

    The F(2)-isoprostanes are products of free-radical-induced oxidation of arachidonic acid (AA) that are stereoisomers of prostaglandin F(2alpha) (PGF(2alpha)). We describe a method for quantitation of several 15-series PGF isomers (15-PGFs) and AA by high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS-MS). Plasma samples were subjected to alkaline hydrolysis and acidified, and total (free + esterified) 15-PGFs and AA were extracted with organic solvents. The analytes were separated by gradient reverse-phase HPLC and detected by multiple reaction monitoring on a triple-quadrupole mass spectrometer, using deuterated internal standards for quantitation. The assay had a linear range of 1-40 pg of 8-iso-PGF(2alpha) on column and can quantify as little as 40 pg/mL (0.11 nM) in plasma. Outcomes significantly correlated (p < 0.0001) with data obtained by gas chromatography-mass spectrometry GC-MS or enzyme-linked immunosorbent assay. All plasma 15-PGF isomers increased over time with in vitro cigarette smoke exposure and correlated (p < 0.0001) with each other. The same strong inter-15-PGF correlations were observed in plasma from healthy young adult subjects. The coefficients of variation of HPLC-MS-MS measurements (24-32%) were smaller than those obtained by GC-MS (53%). Thus, HPLC-MS-MS potentially offers greater precision and allows quantitation of more compounds with simpler sample preparation than existing methods. Ours is the first validated quantitative assay using HPLC-tandem MS applied to plasma total 15-PGFs.

  9. Dietary Protein Intake and Lean Muscle Mass in Survivors of Childhood Acute Lymphoblastic Leukemia: Report From the St. Jude Lifetime Cohort Study

    PubMed Central

    Boland, Alexandra M.; Gibson, Todd M.; Lu, Lu; Kaste, Sue C.; DeLany, James P.; Partin, Robyn E.; Lanctot, Jennifer Q.; Howell, Carrie R.; Nelson, Heather H.; Chemaitilly, Wassim; Pui, Ching-Hon; Robison, Leslie L.; Mulrooney, Daniel A.; Hudson, Melissa M.

    2016-01-01

    Background Survivors of childhood acute lymphoblastic leukemia (ALL) are at risk for low lean muscle mass and muscle weakness, which may contribute to inactivity and early development of chronic diseases typically seen in older adults. Although increasing protein intake, in combination with resistance training, improves lean muscle mass in other populations, it is not known whether muscular tissue among survivors of ALL, whose impairments are treatment-related, will respond similarly. Objective The aim of this study was to evaluate associations among dietary protein intake, resistance training, and lean muscle mass in survivors of ALL and age-, sex-, and race-matched controls. Design This was a cross-sectional study. Methods Lean muscle mass was determined with dual-energy x-ray absorptiometry, dietary information with 24-hour recalls, and participation in resistance training with a questionnaire. Participants were 365 survivors of ALL (52% male; 87% white; median age=28.5 years, range=23.6–31.7) and 365 controls with no previous cancer. Results Compared with controls, survivors of ALL had lower lean muscle mass (55.0 versus 57.2 kg, respectively) and lower percentage of lean muscle mass (68.6% versus 71.4%, respectively) than controls. Similar proportions of survivors (71.1%) and controls (69.7%) met recommended dietary protein intake (0.8 g/kg/d). Survivors (45.4%) were less likely to report resistance training than controls (53.8%). In adjusted models, 1-g higher protein intake per kilogram of body mass per day was associated with a 7.9% increase and resistance training ≥1×wk, with a 2.8% increase in lean muscle mass. Limitations The cross-sectional study design limits temporal evaluation of the association between protein intake and lean muscle mass. Conclusions The findings suggest that survivors of childhood ALL with low lean muscle mass may benefit from optimizing dietary protein intake in combination with resistance training. Research is needed to

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

    NASA Astrophysics Data System (ADS)

    Bailey, Vanessa; Hinz, Philip M.; 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.

    2013-04-01

    We present a 3-5 μm LBT/MMT adaptive optics imaging study of three Upper Scorpius stars with brown dwarf (BD) companions with very low masses/mass ratios (M BD <25 M Jup; M BD/M sstarf ≈ 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 μm and 24 μm 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 μm excess in the system may be explained by the contribution from this disk. 1RXS 1609B exhibits no 3-4 μm excess, nor does its primary; however, the system as a whole has a modest 24 μm 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 μm 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 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. Observations reported here were obtained at the LBT and MMT Observatories. The MMT Observatory is a joint facility of the University of Arizona and the Smithsonian Institution. The LBT is an international collaboration among institutions in the United States, Italy, and Germany. LBT Corporation partners are: The University of Arizona on behalf of the Arizona university system; Istituto Nazionale di Astrofisica, Italy; LBT

  11. Separation and characterization of soluble esterified and glycoside-bound phenolic compounds in dry-blanched peanut skins by liquid chromatography-electrospray ionization mass spectrometry.

    PubMed

    Ma, Yuanyuan; Kosińska-Cagnazzo, Agnieszka; Kerr, William L; Amarowicz, Ryszard; Swanson, Ruthann B; Pegg, Ronald B

    2014-11-26

    A large variety of soluble phenolic compounds, including phenolic acids (hydroxybenzoic acids, ethyl protocatechuate, and hydroxycinnamic acids, as well as phenylacetic acid and phenyllactic acid), stilbenes (trans-piceatannol and trans-3,3',5,5'-tetrahydroxy-4'-methoxystilbene), flavan-3-ols (e.g., (-)-epicatechin, (+)-catechin, (-)-epiafzelechin, and their polymers (the proanthocyanidins, PACs)), other flavonoids (e.g., isoflavones, flavanols, and flavones), and biflavonoids, were released from esters and glycosides by base/acid hydrolysis and identified in acetonic extracts of dry-blanched peanut skins (PS). Reversed-phase high-performance liquid chromatography (RP-HPLC) coupled with electrospray ionization mass spectrometry (ESI-MS(n)) was applied to separate and identify the phenolic constituents. Tentative identification of the separated phenolics was based on molecular ions and MS(n) fragmentation patterns acquired by ESI-MS in the negative-ion mode. Identification of free phenolic acids, stilbenes, and flavonoids was also achieved by commercial standards and by published literature data. Quantification was performed on the basis of peak areas of the UV signals from the HPLC chromatograms and calibration curves of the commercial standards. The flavonoids of PS exist mostly in glycoside-bound forms, but the aglycones can be liberated upon acid hydrolysis. PS contain significantly more PACs compared to free phenolic compounds: PAC monomers to tetramers constituted 92.0% of esterified phenolic compounds. The PAC monomer ((+)-catechin) and dimers are the main phenolics released from glycosides and account for 31.7 and 59.1%, respectively, of the total glycoside-bound phenolic compounds.

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

    NASA Technical Reports Server (NTRS)

    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.

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

    PubMed

    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.

  14. Separation of a BMS drug candidate and acyl glucuronide from seven glucuronide positional isomers in rat plasma via high-performance liquid chromatography with tandem mass spectrometric detection.

    PubMed

    Xue, Y-J; Simmons, Neal J; Liu, Jane; Unger, Steve E; Anderson, Danielle F; Jenkins, Rand G

    2006-01-01

    A high-performance liquid chromatography/tandem mass spectrometry (LC/MS/MS) method has been developed and validated for the determination of a BMS drug candidate and its acyl glucuronide (1-O-beta glucuronide) in rat plasma. A 50-microL aliquot of each plasma sample was fortified with acetonitrile containing the internal standard to precipitate proteins and extract the analytes of interest. After mixing and centrifugation, the supernatant from each sample was transferred to a 96-well plate and injected into an LC/MS/MS system. Chromatographic separation was achieved isocratically on a Phenomenex Luna C(18), 3 mm x 150 mm, 3 microm column. The mobile phase contained 0.075% formic acid in 70:30 (v/v) acetonitrile/water. Under the optimized chromatographic conditions, the BMS drug candidate and its acyl glucuronide were separated from its seven glucuronide positional isomers within 10 min. Resolution of the parent from all glucuronides and acyl glucuronide from its positional isomers was critical to avoid their interference with quantitation of parent or acyl glucuronide. Detection was by positive ion electrospray MS/MS on a Sciex API 4000. The standard curve, which ranged from 5 to 5000 ng/mL, was fitted to a 1/x(2) weighted quadratic regression model for both the BMS drug candidate and its acyl glucuronide. Whole blood and plasma stability experiments were conducted to establish the sample collection, storage, and processing conditions. The validation results demonstrated that this method was rugged and repeatable. The same methodology has also been used in mouse and human plasma for the determination of the BMS drug candidate and its acyl glucuronide.

  15. Comprehensive analysis of dipeptides in alcoholic beverages by tag-based separation and determination using liquid chromatography/electrospray ionization tandem mass spectrometry and quadrupole-time-of-flight mass spectrometry.

    PubMed

    Takahashi, Kei; Tokuoka, Masafumi; Kohno, Hiromi; Sawamura, Nobuko; Myoken, Yuka; Mizuno, Akihiro

    2012-06-15

    Fermented foods and beverages contain several different types of dipeptides, which are believed to be important components for taste. To date, however, a method for the comprehensive analysis of dipeptides in these products has not yet been established. In this study, comprehensive analysis of dipeptides in alcoholic beverages was performed by a high-resolution separation method based on the structural characteristics of 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate (AQC)-derivatized dipeptides as well as dipeptide quantification and structural estimation using ultra-high-pressure liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) and UHPLC-quadrupole time-of-flight mass spectrometry (UHPLC-Q-TOFMS), respectively. Dipeptide content was found to differ considerably among Japanese sake, beer, and wine; UHPLC-MS/MS analysis revealed that many types of dipeptides are present in sake. Dipeptide quantification analysis identified 32 types of dipeptides within the concentration range of 1.1-97.2 μM in sake. The analysis was validated by dipeptide recovery of 64.0-107.2% (2.5 μM of standard) with a relative standard deviation of ≤33.2% from an actual alcoholic sample. Furthermore, UHPLC-Q-TOFMS analysis suggested the existence of more than 35 types of dipeptides in sake. Thus, by the combined analysis methods, we discovered that more than 60 dipeptides are present in sake. This research is the first report of dipeptide profiling of fermented alcoholic beverages by comprehensive analysis.

  16. Orbital Stability of High Mass Planetary Systems

    NASA Astrophysics Data System (ADS)

    Morrison, Sarah J.; Kratter, Kaitlin M.

    2016-05-01

    In light of the observation of systems like HR 8799 that contain several planets with planet-star mass ratios larger than Jupiter's, we explore the relationships between planet separation, mass, and stability timescale for high mass multi-planet systems detectable via direct imaging. We discuss the role of overlap between 1st and sometimes 2nd order mean motion resonances, and show how trends in stability time vary from previous studies of lower mass multi-planet systems. We show that extrapolating empirically derived relationships between planet mass, separation, and stability timescale derived from lower mass planetary systems misestimate the stability timescales for higher mass planetary systems by more than an order of magnitude at separations near the Hill stability limit. We also address what metrics of planet separation are most useful for estimating a system's dynamical stability. We apply these results to young, gapped, debris disk systems of the ScoCen association in order to place limits on the maximum mass and number of planets that could persist for the lifetimes of the disks. These efforts will provide useful constraints for on-going direct imaging surveys. By setting upper limits on the most easily detectable systems, we can better interpret both new discoveries and non-dectections.

  17. Separation and characterization of metallothionein in the liver of sea turtles by high performance liquid chromatographylinductively coupled plasma-mass spectrometry

    NASA Astrophysics Data System (ADS)

    Shinsuke, T.; Yasumi, A.; Takashi, K.

    2003-05-01

    To investigate whether trace metals bind to metallothioneins (MTs) in the hepatocytosol of green turtles (Chelonia mydas) and hawksbill turtles (Eretmochelys imbricata), MT fraction was obtained by ultracentrifugation and gel filtration methods. MTs separated from hepatocytosol were further purified and characterized by high performance liquid chromatography/inductively coupled plasma-mass spectrometry. In addition, the involvement of MTs in the accumulation of trace metals in the liver of sea turtle was examine. Gel filtration analysis showed that significant amounts of Cu, Zn, Ag and Cd were bound to MT in the cytosol of sea turtles, suggesting that such trace metals were primarily detoxified by interaction with MTs in the liver. Elution profiles of these trace metals by anion-exchange chromatography were different between green turtles and hawksbill turtles. These results suggest the presence of multiple isoforms of MT in the liver of both sea turtles; however, constituents of isoforms were different between green and hawksbill turtles. In both species, we observed the elevation of the height of a specific peak in elution profile with an increase in Cu concentration in hepatocytosol. This result suggests the presence of a novel MT isoform related to copper accumulation in the liver of sea turtles.

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

    PubMed

    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.

  19. Development of a fast capillary electrophoresis-time-of-flight mass spectrometry method for the speciation of organotin compounds under separation conditions of high electrical field strengths.

    PubMed

    Malik, Ashok Kumar; Grundmann, Marco; Matysik, Frank-Michael

    2013-11-15

    A novel approach has been developed for the separation of organotin species with capillary electrophoresis hyphenated to time-of-flight mass spectrometry. It has been applied to the development of a method for the determination and speciation of organotin compounds namely, dibutyltin (DBT), tributyltin (TBT), diphenyltin (DPT) and triphenyltin (TPT) in water samples. Experiments were made with a special laboratory constructed CE instrument. A non-aqueous buffer system compatible with TOF-MS has been developed using ammonium acetate-acetic acid (50 mM and 1 M) in acetonitrile: methanol (80:20). The total analysis time is less than 3 min for these compounds under the conditions developed. The method has been applied successfully to the determination of these compounds in river water samples. Detection limits of the CE-TOF-MS method were between 1 and 8×10(-7) M, and between 2 and 11×10(-9) M (0.46 to 3.2 µg L(-1)) when used in conjunction with solid phase extraction. The short analysis time as well as good sensitivity and selectivity make it a useful approach for the fast screening of organotin compounds.

  20. Investigation of natural phosphatidylcholine sources: separation and identification by liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS2) of molecular species.

    PubMed

    Le Grandois, Julie; Marchioni, Eric; Zhao, Minjie; Giuffrida, Francesca; Ennahar, Saïd; Bindler, Françoise

    2009-07-22

    This study is a contribution to the exploration of natural phospholipid (PL) sources rich in long-chain polyunsaturated fatty acids (LC-PUFAs) with nutritional interest. Phosphatidylcholines (PCs) were purified from total lipid extracts of different food matrices, and their molecular species were separated and identified by liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS(2)). Fragmentation of lithiated adducts allowed for the identification of fatty acids linked to the glycerol backbone. Soy PC was particularly rich in species containing essential fatty acids, such as (18:2-18:2)PC (34.0%), (16:0-18:2)PC (20.8%), and (18:1-18:2)PC (16.3%). PC from animal sources (ox liver and egg yolk) contained major molecular species, such as (16:0-18:2)PC, (16:0-18:1)PC, (18:0-18:2)PC, or (18:0-18:1)PC. Finally, marine source (krill oil), which was particularly rich in (16:0-20:5)PC and (16:0-22:6)PC, appeared to be an interesting potential source for food supplementation with LC-PUFA-PLs, particularly eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA).

  1. Determination of Os by isotope dilution-inductively coupled plasma-mass spectrometry with the combination of laser ablation to introduce chemically separated geological samples

    NASA Astrophysics Data System (ADS)

    Sun, Yali; Ren, Minghao; Xia, Xiaoping; Li, Congying; Sun, Weidong

    2015-11-01

    A method was developed for the determination of trace Os in geological samples by laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) with the combination of chemical separation and preconcentration. Samples are digested using aqua regia in Carius tubes, and the Os analyte is converted into volatile OsO4, which is distilled and absorbed with HBr. The HBr solution is concentrated for further Os purification using the microdistillation technique. The purified Os is dissolved in 10 μl of 0.02% sucrose-0.005% H3PO4 solution and then evaporated on pieces of perfluoroalkoxy (PFA) film, resulting in the formation of a tiny object (< 3 × 104 μm2 superficial area). Using LA-ICP-MS measurements, the object can give Os signals at least 100 times higher than those provided by routine solution-ICP-MS while successfully avoiding the memory effect. The procedural blank and detection limit in the developed technique are 3.0 pg and 1.8 pg for Os, respectively when 1 g of samples is taken. Reference materials (RM) are analyzed, and their Os concentrations obtained by isotope dilution are comparable to reference or literature values. Based on the individual RM results, the precision is estimated within the range of 0.6 to 9.4% relative standard deviation (RSD), revealing that this method is applicable to the determination of trace Os in geological samples.

  2. A novelty strategy for the fast analysis of sulfonamide antibiotics in fish tissue using magnetic separation with high-performance liquid chromatography-tandem mass spectrometry.

    PubMed

    Li, Jincheng; Liu, Huan; Zhang, Jing; Liu, Yang; Wu, Lidong

    2016-08-01

    A simple, fast and low-cost extraction method with high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) determination was developed on sulfonamide antibiotics (SAs) in fish tissue. Magnetic separation was first introduced into the rapid sample preparation procedure combined with acetonitrile extraction for the analysis of SAs. Partitioning was rapidly achieved between acetonitrile solution and solid matrix by applying an external magnetic field. Acetonitrile solution was collected and concentrated under a nitrogen stream. The residue was redissolved with 1‰ formic acid aqueous solution and defatted with n-hexane before analysis. The recoveries of SAs were in the range of 74.87-104.74%, with relative standard deviations <13%. The limits of quantification and the limits of detection for SAs ranged from 5.0 to 25.0 μg (kg-1) and from 2.5 to 10.0 μg (kg-1) , respectively. The presented extraction method proved to be a rapid method which only took 20 min for one sample preparation procedure. Copyright © 2016 John Wiley & Sons, Ltd.

  3. Early 21st-Century Mass loss of the North-Atlantic Glaciers and Ice Caps (Arne Richter Award for Outstanding Young Scientists Lecture)

    NASA Astrophysics Data System (ADS)

    Wouters, Bert; Ligtenberg, Stefan; Moholdt, Geir; Gardner, Alex S.; Noel, Brice; Kuipers Munneke, Peter; van den Broeke, Michiel; Bamber, Jonathan L.

    2016-04-01

    Historically, ice loss from mountain glaciers and ice caps has been one of the largest contributors to sea level rise over the last century. Of particular interest are the glaciers and ice caps in the North-Atlantic region of the Arctic. Despite the cold climate in this area, considerable melting and runoff occurs in summer. A small increase in temperature will have an immediate effect on these processes, so that a large change in the Arctic ice volume can be expected in response to the anticipated climate change in the coming century. Unfortunately, direct observations of glaciers are sparse and are biased toward glaciers systems in accessible, mostly maritime, climate conditions. Remote sensing is therefore essential to monitor the state of the the North-Atlantic glaciers and ice caps. In this presentation, we will discuss the progress that has been made in estimating the ice mass balance of these regions, with a particular focus on measurements made by ESA's Cryosat-2 radar altimeter mission (2010-present). Compared to earlier altimeter mission, Cryosat-2 provides unprecedented coverage of the cryosphere, with a resolution down to 1 km or better and sampling at monthly intervals. Combining the Cryosat-2 measurements with the laser altimetry data from ICESat (2003-2009) gives us a 12 yr time series of glacial mass loss in the North Atlantic. We find excellent agreement between the altimetry measurements and independent observations by the GRACE mission, which directly 'weighs' the ice caps, albeit at a much lower resolution. Mass loss in the region has increased from 120 Gigatonnes per year in 2003-2009 to roughly 140 Gt/yr in 2010-2014, with an important contribution from Greenland's peripheral glaciers and ice caps. Importantly, the mass loss is not stationary, but shows large regional interannual variability, with mass loss shifting between eastern and western regions from year to year. Comparison with regional climate models shows that these shifts can be

  4. Astronomical constraints on the duration of the early Jurassic Hettangian stage and recovery rates following the end-Triassic mass extinction (St Audrie's Bay/East Quantoxhead, UK)

    NASA Astrophysics Data System (ADS)

    Ruhl, M.; Deenen, M. H. L.; Abels, H. A.; Bonis, N. R.; Krijgsman, W.; Kürschner, W. M.

    2010-06-01

    The end-Triassic environmental crisis with major extinctions in the marine realm is followed by successive recovery in the lower Jurassic Hettangian Stage. Accurate timing of events is however still poorly constrained. In this study, combined field observations and physical and chemical proxy records, covering the uppermost Triassic and lower Jurassic marine successions of St Audrie's Bay and East Quantoxhead (UK), have been used to construct a floating astronomical time-scale of ∼ 2.5 Myr in length. This time-scale is based on the recognition of meters thick cycles in limestone and (black) shale predominance and concurrent variability in physical and chemical proxy records. Three to five individual black-shale beds occur within these meter-scale sedimentary bundles and are interpreted to reflect precession-controlled changes in monsoon intensity, while the bundles are interpreted as forced by the ∼ 100-kyr eccentricity cycle. On the basis of these findings, we propose an astronomically constrained duration of the Hettangian stage of 1.8 Myr in the UK and unequal duration of Hettangian ammonite zones (Psilocerasplanorbis zone: ∼ 250 kyr; Alsatitesliasicus zone: ∼ 750 kyr; Schlotheimiaangulata zone: ∼ 800 kyr). Within this astronomical framework, the extinction interval and coinciding negative CIE represent 1 to 2 precession cycles (∼ 20-40 kyr). The amount of time succeeding the end-Triassic negative carbon isotope excursion (CIE) and preceding the first Jurassic ammonite occurrence (in the UK) is constrained to 6 climatic precession cycles (∼ 120 kyr). Cyclostratigraphic correlation to the astronomically-tuned sedimentary record of the continental Newark basin (USA) allows to locate the stratigraphic position of the marine defined Triassic-Jurassic and Hettangian-Sinemurian boundary in the continental realm. Continuous low δ13CTOC values throughout the Hettangian and early Sinemurian, succeeding volcanic activity in the Central Atlantic Magmatic

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

    USGS Publications Warehouse

    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

  6. Rebuilding Mount St. Helens

    USGS Publications Warehouse

    Schilling, Steve P.; Ramsey, David W.; Messerich, James A.; Thompson, Ren A.

    2006-01-01

    On May 18, 1980, Mount St. Helens, Washington exploded in a spectacular and devastating eruption that shocked the world. The eruption, one of the most powerful in the history of the United States, removed 2.7 cubic kilometers of rock from the volcano's edifice, the bulk of which had been constructed by nearly 4,000 years of lava-dome-building eruptions. In seconds, the mountain's summit elevation was lowered from 2,950 meters to 2,549 meters, leaving a north-facing, horseshoe-shaped crater over 2 kilometers wide. Following the 1980 eruption, Mount St. Helens remained active. A large lava dome began episodically extruding in the center of the volcano's empty crater. This dome-building eruption lasted until 1986 and added about 80 million cubic meters of rock to the volcano. During the two decades following the May 18, 1980 eruption, Crater Glacier formed tongues of ice around the east and west sides of the lava dome in the deeply shaded niche between the lava dome and the south crater wall. Long the most active volcano in the Cascade Range with a complex 300,000-year history, Mount St. Helens erupted again in the fall of 2004 as a new period of dome building began within the 1980 crater. Between October 2004 and February 2006, about 80 million cubic meters of dacite lava erupted immediately south of the 1980-86 lava dome. The erupting lava separated the glacier into two parts, first squeezing the east arm of the glacier against the east crater wall and then causing equally spectacular crevassing and broad uplift of the glacier's west arm. Vertical aerial photographs document dome growth and glacier deformation. These photographs enabled photogrammetric construction of a series of high-resolution digital elevation models (DEMs) showing changes from October 4, 2004 to February 9, 2006. From the DEMs, Geographic Information Systems (GIS) applications were used to estimate extruded volumes and growth rates of the new lava dome. The DEMs were also used to quantify dome

  7. Polysialylated N-Glycans Identified in Human Serum Through Combined Developments in Sample Preparation, Separations and Electrospray ionization-mass spectrometry

    SciTech Connect

    Kronewitter, Scott R.; Marginean, Ioan; Cox, Jonathan T.; Zhao, Rui; Hagler, Clay D.; Shukla, Anil K.; Carlson, Timothy S.; Adkins, Joshua N.; Camp, David G.; Moore, Ronald J.; Rodland, Karin D.; Smith, Richard D.

    2014-09-02

    The N-glycan diversity of human serum glycoproteins, i.e. the human blood serum N-glycome, is complex due to the range of glycan structures potentially synthesizable by human glycosylation enzymes. The reported glycome, however, is limited by methods of sample preparation, available analytical platforms, e.g., based upon electrospray ionization-mass spectrometry (ESI-MS), and software tools for data analysis. In this report, several improvements have been implemented in sample preparation and analysis to extend ESI-MS glycan characterization and to provide an improved view of glycan diversity. Sample preparation improvements include acidified, microwave-accelerated, PNGase F N-glycan release, and sodium borohydride reduction were optimized to improve quantitative yields and conserve the number of glycoforms detected. Two-stage desalting (during solid phase extraction and on the analytical column) increased the sensitivity by reducing analyte signal division between multiple reducing-end-forms or cation adducts. On-line separations were improved by using extended length graphitized carbon columns and adding TFA as an acid modifier to a formic acid/reversed phase gradient which provides additional resolving power and significantly improved desorption of both large and heavily sialylated glycans. To improve MS sensitivity and provide gentler ionization conditions at the source-MS interface, subambient pressure ionization with nanoelectrospray (SPIN) has been utilized. When method improvements are combined together with the Glycomics Quintavariate Informed Quantification (GlyQ-IQ) recently described1 these technologies demonstrate the ability to significantly extend glycan detection sensitivity and provide expanded glycan coverage. We demonstrate application of these advances in the context of the human serum glycome, and for which our initial observations include detection of a new class of heavily sialylated N-glycans, including polysialylated N-glycans.

  8. Strong anion exchange liquid chromatographic separation of protein amino acids for natural 13C-abundance determination by isotope ratio mass spectrometry.

    PubMed

    Abaye, Daniel A; Morrison, Douglas J; Preston, Tom

    2011-02-15

    Amino acids are the building blocks of proteins and the analysis of their (13)C abundances is greatly simplified by the use of liquid chromatography (LC) systems coupled with isotope ratio mass spectrometry (IRMS) compared with gas chromatography (GC)-based methods. To date, various cation exchange chromatography columns have been employed for amino acid separation. Here, we report strong anion exchange chromatography (SAX) coupled to IRMS with a Liquiface interface for amino acid δ(13)C determination. Mixtures of underivatised amino acids (0.1-0.5 mM) and hydrolysates of representative proteins (prawns and bovine serum albumin) were resolved by LC/IRMS using a SAX column and inorganic eluents. Background inorganic carbon content was minimised through careful preparation of alkaline reagents and use of a pre-injector on-line carbonate removal device. SAX chromatography completely resolved 11 of the 16 expected protein amino acids following acid hydrolysis in underivatised form. Basic and neutral amino acids were resolved with 35 mM NaOH in isocratic mode. Elution of the aromatic and acidic amino acids required a higher hydroxide concentration (180 mM) and a counterion (NO 3-, 5-25 mM). The total run time was 70 min. The average δ(13)C precision of baseline-resolved peaks was 0.75‰ (range 0.04 to 1.06‰). SAX is a viable alternative to cation chromatography, especially where analysis of basic amino acids is important. The technology shows promise for (13)C amino acid analysis in ecology, archaeology, forensic science, nutrition and protein metabolism.

  9. Separated Shoulder

    MedlinePlus

    Separated shoulder Overview By Mayo Clinic Staff A separated shoulder is an injury to the ligaments that hold your collarbone (clavicle) to your shoulder blade. In a mild separated shoulder, the ligaments ...

  10. Parents' and adolescents' willingness to be vaccinated against serogroup B meningococcal disease during a mass vaccination in Saguenay-Lac-St-Jean (Quebec).

    PubMed

    Dubé, Eve; Gagnon, Dominique; Hamel, Denis; Belley, Sylvie; Gagné, Hélène; Boulianne, Nicole; Landry, Monique; Bettinger, Julie A

    2015-01-01

    A mass vaccination campaign with the 4CMenB vaccine (Bexsero®; Novartis Pharmaceutical Canada Inc) was launched in a serogroup B endemic area in Quebec. A telephone survey was conducted to assess parental and adolescent opinions about the acceptability of the vaccine. Intent to receive the vaccine or vaccine receipt was reported by the majority of parents (93%) and adolescents (75%). Meningitis was perceived as being a dangerous disease by the majority of parents and adolescents. The majority of respondents also considered the 4CMenB vaccine to be safe and effective. The main reason for positive vaccination intention or behaviour was self-protection, while a negative attitude toward vaccination in general was the main reason mentioned by parents who did not intend to have their child vaccinated. Adolescents mainly reported lack of interest, time or information, and low perceived susceptibility and disease severity as the main reasons for not intending to be vaccinated or not being vaccinated.

  11. Role of Strouhal number (St) in free swimming

    NASA Astrophysics Data System (ADS)

    Saadat, Mehdi; Haj-Hariri, Hossein

    2012-11-01

    St of 0.2-0.4 has become synonymous with efficient self propulsion. Is it the cause, or an effect? As has been argued by a number of authors, St alone is insufficient to decide optimal motion because many inefficient combinations of amplitude and frequency lead to the same St. In this talk we show a simple ramification of free swimming where the swim speed and St are outputs. The iso-lines for speed, St, and thrust coincide so long as there is no massive leading-edge separation. It appears that St is simply related to how the drag coefficient and geometry of the body relates to the thrust coefficient and geometry of the propulsor. For a given combination of propulsor and body, St of motion is essentially independent of amplitude, frequency, and speed, and is only a function of shape. Some motions are efficient, and some are not. But they all have the same St. Supported by ONR MURI.

  12. Parents’ and adolescents’ willingness to be vaccinated against serogroup B meningococcal disease during a mass vaccination in Saguenay–Lac-St-Jean (Quebec)

    PubMed Central

    Dubé, Eve; Gagnon, Dominique; Hamel, Denis; Belley, Sylvie; Gagné, Hélène; Boulianne, Nicole; Landry, Monique; Bettinger, Julie A

    2015-01-01

    A mass vaccination campaign with the 4CMenB vaccine (Bexsero®; Novartis Pharmaceutical Canada Inc) was launched in a serogroup B endemic area in Quebec. A telephone survey was conducted to assess parental and adolescent opinions about the acceptability of the vaccine. Intent to receive the vaccine or vaccine receipt was reported by the majority of parents (93%) and adolescents (75%). Meningitis was perceived as being a dangerous disease by the majority of parents and adolescents. The majority of respondents also considered the 4CMenB vaccine to be safe and effective. The main reason for positive vaccination intention or behaviour was self-protection, while a negative attitude toward vaccination in general was the main reason mentioned by parents who did not intend to have their child vaccinated. Adolescents mainly reported lack of interest, time or information, and low perceived susceptibility and disease severity as the main reasons for not intending to be vaccinated or not being vaccinated. PMID:26236359

  13. Rapid assessment of human amylin aggregation and its inhibition by copper(II) ions by laser ablation electrospray ionization mass spectrometry with ion mobility separation

    SciTech Connect

    Li, Hang; Ha, Emmeline; Donaldson, Robert P.; Jeremic, Aleksandar M.; Vertes, Akos

    2015-09-09

    Native electrospray ionization (ESI) mass spectrometry (MS) is often used to monitor noncovalent complex formation between peptides and ligands. The relatively low throughput of this technique, however, is not compatible with extensive screening. Laser ablation electrospray ionization (LAESI) MS combined with ion mobility separation (IMS) can analyze complex formation and provide conformation information within a matter of seconds. Islet amyloid polypeptide (IAPP) or amylin, a 37-amino acid residue peptide, is produced in pancreatic beta-cells through proteolytic cleavage of its prohormone. Both amylin and its precursor can aggregate and produce toxic oligomers and fibrils leading to cell death in the pancreas that can eventually contribute to the development of type 2 diabetes mellitus. The inhibitory effect of the copper(II) ion on amylin aggregation has been recently discovered, but details of the interaction remain unknown. Finding other more physiologically tolerated approaches requires large scale screening of potential inhibitors. In this paper, we demonstrate that LAESI-IMS-MS can reveal the binding stoichiometry, copper oxidation state, and the dissociation constant of human amylin–copper(II) complex. The conformations of hIAPP in the presence of copper(II) ions were also analyzed by IMS, and preferential association between the β-hairpin amylin monomer and the metal ion was found. The copper(II) ion exhibited strong association with the —HSSNN– residues of the amylin. In the absence of copper(II), amylin dimers were detected with collision cross sections consistent with monomers of β-hairpin conformation. When copper(II) was present in the solution, no dimers were detected. Thus, the copper(II) ions disrupt the association pathway to the formation of β-sheet rich amylin fibrils. Using LAESI-IMS-MS for the assessment of amylin–copper(II) interactions demonstrates the utility of this technique for the high-throughput screening of potential

  14. Rapid assessment of human amylin aggregation and its inhibition by copper(II) ions by laser ablation electrospray ionization mass spectrometry with ion mobility separation

    DOE PAGES

    Li, Hang; Ha, Emmeline; Donaldson, Robert P.; ...

    2015-09-09

    Native electrospray ionization (ESI) mass spectrometry (MS) is often used to monitor noncovalent complex formation between peptides and ligands. The relatively low throughput of this technique, however, is not compatible with extensive screening. Laser ablation electrospray ionization (LAESI) MS combined with ion mobility separation (IMS) can analyze complex formation and provide conformation information within a matter of seconds. Islet amyloid polypeptide (IAPP) or amylin, a 37-amino acid residue peptide, is produced in pancreatic beta-cells through proteolytic cleavage of its prohormone. Both amylin and its precursor can aggregate and produce toxic oligomers and fibrils leading to cell death in the pancreasmore » that can eventually contribute to the development of type 2 diabetes mellitus. The inhibitory effect of the copper(II) ion on amylin aggregation has been recently discovered, but details of the interaction remain unknown. Finding other more physiologically tolerated approaches requires large scale screening of potential inhibitors. In this paper, we demonstrate that LAESI-IMS-MS can reveal the binding stoichiometry, copper oxidation state, and the dissociation constant of human amylin–copper(II) complex. The conformations of hIAPP in the presence of copper(II) ions were also analyzed by IMS, and preferential association between the β-hairpin amylin monomer and the metal ion was found. The copper(II) ion exhibited strong association with the —HSSNN– residues of the amylin. In the absence of copper(II), amylin dimers were detected with collision cross sections consistent with monomers of β-hairpin conformation. When copper(II) was present in the solution, no dimers were detected. Thus, the copper(II) ions disrupt the association pathway to the formation of β-sheet rich amylin fibrils. Using LAESI-IMS-MS for the assessment of amylin–copper(II) interactions demonstrates the utility of this technique for the high-throughput screening of

  15. Speciation of metallothionein-like proteins of the mussel Mytilus edulis by orthogonal separation mechanisms with inductively coupled plasma-mass spectrometry detection: effect of selenium administration

    NASA Astrophysics Data System (ADS)

    Ferrarello, Claudio N.; del Rosario Fernández de la Campa, María.; Francisco Carrasco, José; Sanz-Medel, Alfredo

    2002-03-01

    Several complementary separation mechanisms (size-exclusion chromatography, SEC; fast protein liquid chromatography, FPLC; reverse-phase chromatography, RPC) have been coupled to inductively coupled plasma mass spectrometry (ICP-MS) detection to investigate the speciation of Cd, Se, Cu and Zn in mussel hepatopancreas. SEC with double-focusing (DF) ICP-MS detection was used first for speciation analysis of those four trace elements, both in uncontaminated mussels and in mussels exposed to Cd (500 μg l -1) or to Cd+Se (500 μg l -1 of each element). Observed SEC results indicated that Se does not seem to significantly bind to metallothionein-like proteins (MLPs) 'in vivo'. Total cytosolic Cd and MLPs content were lower in Cd+Se exposed mussels than those exposed to Cd only. For each treatment, 50 μl of the SEC peak fraction containing the MLPs was used to perform fast protein liquid chromatography coupled 'on-line' with a quadrupole (Q) ICP-MS. 82Se and 114Cd isotopes were simultaneously monitored. Four and five Cd/MLPs isoforms were then detected in mussels exposed to only Cd and Cd+Se, respectively. In contrast, no signs of Se/MLP isoforms were found for both treatments. Subsequently, the bulk of MLPs eluting from the FPLC system were isolated and lyophilizated. A 50-μl aliquot of such reconstituted lyophilisate was then injected into a Vydac C 8 Reverse-Phase column directly connected to the Q-ICP-MS. Results confirmed the presence of one more Cd/MLP peak in those mussels exposed to Cd+Se. However, the number of Cd/MLP peaks detected decreased to three and four in only Cd and Cd+Se exposed animals, respectively. These results tend to indicate that Se, which does not trigger the biosynthesis of MLPs, could probably orient such synthesis towards the generation of a new Cd/MLP isoform in mussels submitted to both elements. The possible interrelation/complementation between Se and MLP against Cd toxicity is discussed.

  16. Ultracapacitor separator

    DOEpatents

    Wei, Chang; Jerabek, Elihu Calvin; LeBlanc, Jr., Oliver Harris

    2001-03-06

    An ultracapacitor includes two solid, nonporous current collectors, two porous electrodes separating the collectors, a porous separator between the electrodes and an electrolyte occupying the pores in the electrodes and separator. The electrolyte is a polar aprotic organic solvent and a salt. The porous separator comprises a wet laid cellulosic material.

  17. St. John's Wort (image)

    MedlinePlus

    The herb St. John's Wort is believed to be helpful in relieving mild to moderate depression, but should only be taken under a physician's supervision. St. John's Wort may clash with other medications or foods a ...

  18. Roegneria alashanica Keng: a species with the StStSt(Y)St(Y) genome constitution.

    PubMed

    Wang, Richard R-C; Jensen, Kevin B

    2017-03-17

    The genome constitution of tetraploid Roegneria alashanica Keng has been in question for a long time. Most scientific studies have suggested that R. alashanica had two versions of the St genome, St1St2, similar to that of Pseudoroegneria elytrigioides (C. Yen & J.L. Yang) B.R. Lu. A study, however, concluded that R. alashanica had the StY genome formula typical for tetraploid species of Roegneria. For the present study, R. alashanica, Elymus longearistatus (Bioss.) Tzvelev (StY genomes), Pseudoroegneria strigosa (M. Bieb.) Á. Löve (St), Pseudoroegneria libanoctica (Hackel) D.R. Dewey (St), and Pseudoroegneria spicata (Pursh) Á. Löve (St) were screened for the Y-genome specific marker B14(F+R)269. All E. longearistatus plants expressed intense bands specific to the Y genome. Only 6 of 10 R. alashanica plants exhibited relatively faint bands for the STS marker. Previously, the genome in species of Pseudoroegneria exhibiting such faint Y-genome specific marker was designated as St(Y). Based on these results, R. alashanica lacks the Y genome in E. longearistatus but likely possess two remotely related St genomes, St and St(Y). According to its genome constitution, R. alashanica should be classified in the genus Pseudoroenera and given the new name Pseudoroegneria alashanica (Keng) R.R.-C. Wang and K.B. Jensen.

  19. Evaluation of Enhanced Comprehensive 2-D Gas Chromatography-Time-Of-Flight Mass Spectrometry for the Separation of Recalcitrant Polychlorinated Biphenyl Isomers

    EPA Science Inventory

    The separation of some recalcitrant polychlorinated biphenyl (PCB) isomers in extracts from environmental compartments has been a daunting task for environmental chemists. Summed quantitation values for coeluting PCB isomers are often reported. This composite data obscures the ac...

  20. Separation of plutonium and neptunium species by capillary electrophoresis-inductively coupled plasma-mass spectrometry and application to natural groundwater samples.

    PubMed

    Kuczewski, Bernhard; Marquardt, Christian M; Seibert, Alice; Geckeis, Horst; Kratz, Jens Volker; Trautmann, Norbert

    2003-12-15

    Capillary electrophoresis (CE) was coupled to ICPMS in order to combine the good performance of this separation technique with the high sensitivity of the ICPMS for the analysis of plutonium and neptunium oxidation states. The combination of a fused-silica capillary with a MicroMist AR 30-I-FM02 nebulizer and a Cinnabar small-volume cyclonic spray chamber yielded the best separation results. With this setup, it was possible to separate a model element mixture containing neptunium (NpO2(+)), uranium (UO2(2+)), lanthanum (La3+), and thorium (Th4+) in 1 M acetic acid. The same conditions were also suitable for the separation of various oxidation states of plutonium and neptunium in different aqueous samples. All separations were obtained within less than 15 min. A detection limit of 50 ppb identical with 2 x 10(-7) M (3-fold standard deviation of a blank) was achieved. To prove the negligible disturbance of the plutonium and neptunium redox equilibria during the CE separations, plutonium and neptunium speciation by CE-ICPMS in acidic solutions was compared with the results of UV/visible absorption spectroscopy and was found to be in good agreement. The CE-ICPMS system was also applied to study the reduction of Pu(VI) in a humic acid-containing groundwater at different pH values.

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

    SciTech Connect

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

    2016-02-18

    This article describes how 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.

  2. Microfabrication, separations, and detection by mass spectrometry on ultrathin-layer chromatography plates prepared via the low-pressure chemical vapor deposition of silicon nitride onto carbon nanotube templates.

    PubMed

    Kanyal, Supriya S; Häbe, Tim T; Cushman, Cody V; Dhunna, Manan; Roychowdhury, Tuhin; Farnsworth, Paul B; Morlock, Gertrud E; Linford, Matthew R

    2015-07-24

    Microfabrication of ultrathin-layer chromatography (UTLC) plates via conformal deposition of silicon nitride by low-pressure chemical vapor deposition onto patterned carbon nanotube (CNT) scaffolds was demonstrated. After removal of the CNTs and hydroxylation, the resulting UTLC phase showed no expansion or distortion of their microfeatures and the absence/reduction of remaining nitrogenic species. Developing time of a mixture of lipophilic dyes on this UTLC plates was 86% shorter than on high-performance thin-layer chromatography (HPTLC) plates. A water-soluble food dye mixture was also separated resulting in low band broadening and reduced developing time compared to HPTLC. For the latter example, mobile phase optimization on a single UTLC plate consisted of 14 developments with different mobile phases, each preceded by a plate prewashing step. The same plate was again reused for additional 11 separations under varying conditions resulting in a development procedure with a mean separation efficiency of 233,000theoretical plates/m and a reduced mobile phase consumption of only 400μL. This repeated use proved the physical robustness of the ultrathin layer and its resistance to damage. The layer was highly suited for hyphenation to ambient mass spectrometry, including desorption electrospray ionization (DESI) mass spectrometry imaging and direct analysis in real time (DART) mass spectrometry.

  3. This-layer chromatography/electrospray ionization triple-quadrupole linear ion trap mass spectrometry system: analysis of rhodamine dyes separated on reversed-phase C8 plates

    SciTech Connect

    Ford, Michael J; Kertesz, Vilmos; Van Berkel, Gary J

    2005-01-01

    The direct analysis of separated rhodamine dyes on reversed-phase C{sub 8} thin-layer chromatography plates using a surface sampling/electrospray emitter probe coupled with a triple-quadrupole linear ion trap mass spectrometer is presented. This report represents continuing work to advance the performance metrics and utility of this basic surface sampling electrospray mass spectrometry system for the analysis of thin-layer chromatography plates. Experimental results examining the role of sampling probe spray end configuration on liquid aspiration rate and gas-phase ion signal generated are discussed. The detection figures-of-merit afforded by full-scan, automated product ion and selected reaction monitoring modes of operation were examined. The effect of different eluting solvents on mass spectrum signal levels with the reversed-phase C{sub 8} plate was investigated. The combined effect of eluting solvent flow-rate and development lane surface scan rate on preservation of chromatographic resolution was also studied. Analysis of chromatographically separated red pen ink extracts from eight different pens using selected reaction monitoring demonstrated the potential of this surface sampling electrospray mass spectrometry system for targeted compound analysis with real samples.

  4. Chiral Separations

    NASA Astrophysics Data System (ADS)

    Stalcup, A. M.

    2010-07-01

    The main goal of this review is to provide a brief overview of chiral separations to researchers who are versed in the area of analytical separations but unfamiliar with chiral separations. To researchers who are not familiar with this area, there is currently a bewildering array of commercially available chiral columns, chiral derivatizing reagents, and chiral selectors for approaches that span the range of analytical separation platforms (e.g., high-performance liquid chromatography, gas chromatography, supercritical-fluid chromatography, and capillary electrophoresis). This review begins with a brief discussion of chirality before examining the general strategies and commonalities among all of the chiral separation techniques. Rather than exhaustively listing all the chiral selectors and applications, this review highlights significant issues and differences between chiral and achiral separations, providing salient examples from specific classes of chiral selectors where appropriate.

  5. Water separator

    NASA Technical Reports Server (NTRS)

    Dunn, W. F.; Austin, I. G. (Inventor)

    1964-01-01

    An apparatus for separating liquids from gases or gaseous fluids is described. Features of the apparatus include: (1) the collection and removal of the moisture in the fluid is not dependent upon, or affected by gravity; (2) all the collected water is cyclically drained from the apparatus irrespective of the attitude of the separator; and (3) a fluid actuator is utilized to remove the collected water from the separator.

  6. Battery separators.

    PubMed

    Arora, Pankaj; Zhang, Zhengming John

    2004-10-01

    The ideal battery separator would be infinitesimally thin, offer no resistance to ionic transport in electrolytes, provide infinite resistance to electronic conductivity for isolation of electrodes, be highly tortuous to prevent dendritic growths, and be inert to chemical reactions. Unfortunately, in the real world the ideal case does not exist. Real world separators are electronically insulating membranes whose ionic resistivity is brought to the desired range by manipulating the membranes thickness and porosity. It is clear that no single separator satisfies all the needs of battery designers, and compromises have to be made. It is ultimately the application that decides which separator is most suitable. We hope that this paper will be a useful tool and will help the battery manufacturers in selecting the most appropriate separators for their batteries and respective applications. The information provided is purely technical and does not include other very important parameters, such as cost of production, availability, and long-term stability. There has been a continued demand for thinner battery separators to increase battery power and capacity. This has been especially true for lithiumion batteries used in portable electronics. However, it is very important to ensure the continued safety of batteries, and this is where the role of the separator is greatest. Thus, it is essential to optimize all the components of battery to improve the performance while maintaining the safety of these cells. Separator manufacturers should work along with the battery manufacturers to create the next generation of batteries with increased reliability and performance, but always keeping safety in mind. This paper has attempted to present a comprehensive review of literature on separators used in various batteries. It is evident that a wide variety of separators are available and that they are critical components in batteries. In many cases, the separator is one of the major factors

  7. Separation and characterization of bufadienolides in toad skin using two-dimensional normal-phase liquid chromatography×reversed-phase liquid chromatography coupled with mass spectrometry.

    PubMed

    Zhang, Yun; Jin, Hongli; Li, Xiaolong; Zhao, Jianqiang; Guo, Xiujie; Wang, Jixia; Guo, Zhimou; Zhang, Xiuli; Tao, Yanduo; Liu, Yanfang; Chen, Deliang; Liang, Xinmiao

    2016-07-15

    Bufadienolides possess various bioactivities especially antitumor. Due to the high structural diversity, the separation of bufadienolides often suffers from coelution problem on conventional RP columns. In this work, an off-line two-dimensional normal-phase liquid chromatography×reversed-phase liquid chromatography (2D-NPLC×RPLC) method was developed to separate and characterize bufadienolides in toad skin. Several RP and NP columns were evaluated with five reference bufadienlides. The XUnion C18 and XAmide columns exhibited superior chromatographic performances for bufadienlide separation, and were selected in RPLC and NPLC, respectively. RPLC was used in the second-dimension for the good compatibility with MS, while NPLC was adopted in the first-dimension. The orthogonality of the 2D-NPLC×RPLC system was investigated by the geometric approach using fifteen bufadienolide mixtures. The result was 49.6%, demonstrating reasonable orthogonality of this 2D-LC system. By combining the 2D-LC system with MS, 64 bufadienlides including 33 minor ones and 11 pairs of isomers in toad skin were identified. This off-line 2D-NPLC×RPLC allowed to solve the coelution problem of bufadienlides in one-dimension RPLC, and thus facilitated the identification significantly.

  8. Separation of the fatty acids in menhaden oil as methyl esters with a highly polar ionic liquid gas chromatographic column and identification by time of flight mass spectrometry.

    PubMed

    Fardin-Kia, Ali Reza; Delmonte, Pierluigi; Kramer, John K G; Jahreis, Gerhard; Kuhnt, Katrin; Santercole, Viviana; Rader, Jeanne I

    2013-12-01

    The fatty acids contained in marine oils or products are traditionally analyzed by gas chromatography using capillary columns coated with polyethylene glycol phases. Recent reports indicate that 100 % cyanopropyl siloxane phases should also be used when the analyzed samples contain trans fatty acids. We investigated the separation of the fatty acid methyl esters prepared from menhaden oil using the more polar SLB-IL111 (200 m × 0.25 mm) ionic liquid capillary column and the chromatographic conditions previously optimized for the separation of the complex mixture of fatty acid methyl esters prepared from milk fat. Identifications of fatty acids were achieved by applying Ag(+)-HPLC fractionation and GC-TOF/MS analysis in CI(+) mode with isobutane as the ionization reagent. Calculation of equivalent chain lengths confirmed the assignment of double bond positions. This methodology allowed the identification of 125 fatty acids in menhaden oil, including isoprenoid and furanoid fatty acids, and the novel 7-methyl-6-hexadecenoic and 7-methyl-6-octadecenoic fatty acids. The chromatographic conditions applied in this study showed the potential of separating in a single 90-min analysis, among others, the short chain and trans fatty acids contained in dairy products, and the polyunsaturated fatty acids contained in marine products.

  9. Separation and identification of purine nucleosides in the urine of patients with malignant cancer by reverse phase liquid chromatography/electrospray tandem mass spectrometry.

    PubMed

    Li, Hua-Yu; Wang, Shao-Min; Liu, Hong-Min; Bu, Shan-Shan; Li, Juan; Han, Dong; Zhang, Ming-zhi; Wu, Guang-Yin

    2009-05-01

    Urinary-modified nucleosides have a potential role as cancer biomarkers for a number of malignant diseases. High performance liquid chromatography (HPLC) was combined with full-scan mass spectrometry, MS/MS analysis and accurate mass measurements in order to identify purine nucleosides purified from urine. Potential purine nucleosides were assessed by their evident UV absorbance in the HPLC chromatogram and then further examined by the mass spectrometric techniques. In this manner, numerous modified purine nucleosides were identified in the urine samples from cancer patients including xanthine, adenosine, N1-methyladenosine, 5'-deoxy-5'-methylthioadenosine, 2-methyladenosine, N6-threonylcarbamoyladenosine, inosine, N1-methylinosine, guanosine, N1-methylguanosine, N7-methylguanine, N2-methylguanosine, N2,N2-dimethyguanosine, N2,N2,N7-trimethylguanosine. Furthermore, a number of novel purine nucleosides were tentatively identified via critical interpretation of the combined mass spectrometric data including N3-methyladenosine, N7-methyladenine, 5'-dehydro-2'-deoxyinosine, N3-methylguanine, O6-methylguanosine, N1,N2,N7-trimethylguanosine, N1-methyl-N2-ethylguanosine and N7-methyl-N1-ethylguanosine.

  10. Rapid separation and characterization of diterpenoid alkaloids in processed roots of Aconitum carmichaeli using ultra high performance liquid chromatography coupled with hybrid linear ion trap-Orbitrap tandem mass spectrometry.

    PubMed

    Xu, Wen; Zhang, Jing; Zhu, Dayuan; Huang, Juan; Huang, Zhihai; Bai, Junqi; Qiu, Xiaohui

    2014-10-01

    The lateral root of Aconitum carmichaeli, a popular traditional Chinese medicine, has been widely used to treat rheumatic diseases. For decades, diterpenoid alkaloids have dominated the phytochemical and biomedical research on this plant. In this study, a rapid and sensitive method based on ultra high performance liquid chromatography coupled with linear ion trap-Orbitrap tandem mass spectrometry was developed to characterize the diterpenoid alkaloids in Aconitum carmichaeli. Based on an optimized chromatographic condition, more than 120 diterpenoid alkaloids were separated with good resolution. Using a systematic strategy that combines high resolution separation, highly accurate mass measurements and a good understanding of the diagnostic fragment-based fragmentation patterns, these diterpenoid alkaloids were identified or tentatively identified. The identification of these chemicals provided essential data for further phytochemical studies and toxicity research of Aconitum carmichaeli. Moreover, the ultra high performance liquid chromatography with linear ion trap-Orbitrap mass spectrometry platform was an effective and accurate tool for rapid qualitative analysis of secondary metabolite productions from natural resources.

  11. 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)

    NASA Astrophysics Data System (ADS)

    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.

  12. Development of a comprehensive two-dimensional hydrophilic interaction chromatography/quadrupole time-of-flight mass spectrometry system and its application in separation and identification of saponins from Quillaja saponaria.

    PubMed

    Wang, Yuan; Lu, Xin; Xu, Guowang

    2008-02-15

    Hydrophilic interaction chromatography (HILIC) was used in two dimensions in a comprehensive two-dimensional HILIC hyphenated with a quadrupole time-of-flight mass spectrometry (HILICxHILIC-Q-TOF-MS) system for the analysis of complex samples of hydrophilic compounds. A TSKgel Amide-80 column was employed as the first dimension, and a short PolyHydroxyethyl A column was as the second dimension. The column system showed moderate orthogonality at defined operational conditions. A high speed Q-TOF-MS detector as a third complementary dimension significantly improved the peak capacity. The separation capability of the developed HILICxHILIC-Q-TOF-MS system was tested by separating an extract from Quillaja saponaria. The major components, quillaja saponins, in the extract were well identified by means of [M-H](-) ions, characteristic product ions, and their two-dimensional retention behaviors. Several pairs of isomers, which were often co-eluted on conventional LC-MS methods and had similar fragmentation characteristics in MS/MS spectra, were well separated on the two-dimensional system based on their different hydrophilicity. The developed comprehensive two-dimensional HILIC system demonstrates unique selectivity for hydrophilic compounds and satisfactory peak capacity and resolution for analogues by making sufficient use of two-dimensional separation plane.

  13. Enrichment, resolution, and identification of nickel porphyrins in petroleum asphaltene by cyclograph separation and atmospheric pressure photoionization Fourier transform ion cyclotron resonance mass spectrometry.

    PubMed

    Qian, Kuangnan; Edwards, Kathleen E; Mennito, Anthony S; Walters, Clifford C; Kushnerick, J Douglas

    2010-01-01

    We report here the first high resolution mass spectrometric evidence of nickel porphyrins in petroleum. A petroleum asphaltene sample is fractionated by a silica-gel cyclograph. Nickel content is enriched by approximately 3 fold in one of the cyclograph fractions. The fraction is subsequently analyzed by atmospheric pressure photoionization (APPI) Fourier transform ion cyclotron resonance mass spectrometry (FTICR MS) with an average mass resolving power of over 500 K (M/DeltaM(fwhm)). Similar to vanadyl porphyrins, monocylcoalkano-type (presumed to be deocophylerythro-etioporphyrin DPEP) Ni porphyrins are found to be the most abundant family followed by etio, bicycloalkano-type, and rhodo-monocylcoalkano-type Ni porphyrins. A Z number ranging from -28 to -44 and a carbon number ranging from 26 to 41 were observed. A significant amount of nickel and vanadyl geoporphyrins are in more condensed tetrapyrrolic cores than just chlorophyll-derived DPEP- and etioporphyrins. Ni has a higher etio/DPEP ratio and rhodo-etio/rhodo-DPEP ratio than does VO.

  14. 21st Century Scholars

    ERIC Educational Resources Information Center

    Clark, Terrence

    2009-01-01

    Bethpage Union Free School District in New York is a high-performing district by almost any current accountability measure. Yet administrators and teachers worried that they were not doing enough to prepare their students as critical thinkers for the 21st century. Inspired by the curriculum framework of the Partnership for 21st Century Skills, the…

  15. Simultaneous enantioselective separation of azelastine and three of its metabolites for the investigation of the enantiomeric metabolism in rats. I. Liquid chromatography-ionspray tandem mass spectrometry and electrokinetic capillary chromatography.

    PubMed

    Heinemann, Ute; Blaschke, Gottfried; Knebel, Norbert

    2003-08-15

    Enantioselective separation methods and the enantioselective determination of the anti-allergic drug azelastine and of three of its main phase I metabolites in a biological matrix underwent chromatographic and electrophoretic investigations. An enantioselective assay of a coupling of HPLC using a beta-cyclodextrin chiral stationary phase to ionspray tandem mass spectrometry is presented. Additionally, this assay is compared to another enantioselective assay using electrokinetic capillary chromatography with beta-cyclodextrin and carboxymethyl-beta-cyclodextrin in polyacrylamide-coated capillaries. For capillary electrophoresis (CE) the importance of polyacrylamide coating for the validation of this separation method is highlighted. Extracted rat plasma samples of enantioselective metabolism studies were measured by both validated assays. Differences in the pharmacokinetics and pharmacodynamics were evaluated for the main substance azelastine and its main metabolite demethylazelastine. So, a first hint about the enantioselectivity of biotransformation of azelastine in rats was seen after oral application of either enantiomer or the racemate to rats.

  16. The offline combination of thin-layer chromatography and high-performance liquid chromatography with diode array detection and micrOTOF-Q mass spectrometry for the separation and identification of spinochromes from sea urchin (Strongylocentrotus droebachiensis) shells.

    PubMed

    Shikov, Alexander N; Ossipov, Vladimir I; Martiskainen, Olli; Pozharitskaya, Olga N; Ivanova, Svetlana A; Makarov, Valery G

    2011-12-16

    Thin-layer chromatography (TLC) with off-line high-performance liquid chromatography coupled to diode array detection and micrOTOF-Q mass spectrometry (HPLC-DAD-MS) resulted in the successful fractionation, separation and identification of spinochrome pigments from sea urchin (Strongylocentrotus droebachiensis) shells. Two fractions of pigments were separated by TLC and eluted with methanol using a TLC-MS interface. HPLC-DAD-MS analysis of the fractions indicated the presence of six sea urchin pigments: spinochrome monomers B and D, three spinochrome dimers (anhydroethylidene-6,6'-bis(2,3,7-trihydroxynaphthazarin) and its isomer and ethylidene-6,6'-bis(2,3,7-trihydroxynaphthazarin)), and one pigment that was preliminary identified as a spinochrome dimer with the structural formula C(22)H(16)O(16).

  17. Proteome analysis of Myxococcus xanthus by off-line two-dimensional chromatographic separation using monolithic poly-(styrene-divinylbenzene) columns combined with ion-trap tandem mass spectrometry.

    PubMed

    Schley, Christian; Altmeyer, Matthias O; Swart, Remco; Müller, Rolf; Huber, Christian G

    2006-10-01

    Myxobacteria are potent producers of secondary metabolites exhibiting diverse biological activities and pharmacological potential. The proteome of Myxococcus xanthus DK1622 was characterized by two-dimensional chromatographic separation of tryptic peptides from a lysate followed by tandem mass spectrometric identification. The high degree of orthogonality of the separation system employing polymer-based strong cation-exchange and monolithic reversed-phase stationary phases was clearly demonstrated. Upon automated database searching, 1312 unique peptides were identified, which were associated with 631 unique proteins. High-molecular polyketide synthetases and nonribosomal peptide synthetases, known to be involved in the biosynthesis of various secondary metabolites, were readily detected. Besides the identification of gene products associated with the production of known secondary metabolites, proteins could also be identified for six gene clusters, for which no biosynthetic product has been known so far.

  18. Serial mixed-mode cation- and anion-exchange solid-phase extraction for separation of basic, neutral and acidic pharmaceuticals in wastewater and analysis by high-performance liquid chromatography-quadrupole time-of-flight mass spectrometry.

    PubMed

    Lavén, Martin; Alsberg, Tomas; Yu, Yong; Adolfsson-Erici, Margaretha; Sun, Hongwen

    2009-01-02

    A novel solid-phase extraction (SPE) method is presented whereby 15 basic, neutral and acidic pharmaceuticals in wastewater were simultaneously extracted and subsequently separated into different fractions. This was achieved using mixed-mode cation- and anion-exchange SPE (Oasis MCX and MAX) in series. Analysis was performed by high-performance liquid chromatography-quadrupole time-of-flight mass spectrometry (HPLC/QTOF-MS). A fast separation was achieved, with all compounds eluting within 6min, narrow chromatographic peaks, with a peak base width of 6s on average, and a high mass accuracy of quantified wastewater sample ions, with average mass errors in absolute value of 0.7mDa or 2.7ppm. The recovery of the SPE method in the analysis of sewage treatment plant (STP) influent and effluent wastewater was on average 80% and the ion suppression 30%. For less demanding samples Oasis MCX used alone may be an alternative method, although for STP influent waters containing high loads of organic compounds the clean-up achieved using only Oasis MCX was insufficient, leading to unreliable quantitation. Furthermore, serial SPE separation according to molecular charge added an additional degree of analyte confirmation. For quantitation, an approach combining external standard calibration curves, isotopically labelled surrogate standards and single-point standard addition was used. The applicability of the method was demonstrated in the analysis of influent and effluent wastewater from an STP, using small sample volumes (25-50mL). The effluent wastewater had been subjected to three different treatments; activated sludge, activated sludge followed by ozonation, and a membrane bioreactor (MBR). Ozone treatment proved superior in removal of the analysed pharmaceuticals, while the MBR provided higher removal efficiencies than the activated sludge process.

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

    PubMed

    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. 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.

    PubMed

    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.

  1. 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.

    PubMed

    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.

  2. Stereoisomers Separation

    NASA Astrophysics Data System (ADS)

    Wieczorek, Piotr

    The use of capillary electrophoresis for enantiomer separation and optical purity determination is presented. The contents start with basic information about the nature of stereoizomers and the mechanism of enantioseparation using capillary electrophoresis techniques. The molecules to be separated show identical chemical structure and electrochemical behavior. Therefore, the chiral recognition of enantiomers is possible only by bonding to chiral selector and the separation based on very small differences in complexation energies of diastereomer complexes formed. This method is useful for this purpose due to the fact that different compounds can be used as chiral selectors. The mostly used chiral selectors like cyclodextrins, crown ethers, chiral surfactants, macrocyclic antibiotics, transition metal complexes, natural, and synthetic polymers and their application for this purpose is also discussed. Finally, examples of practical applications of electromigration techniques for enantiomers separation and determination are presented.

  3. Mist separator

    SciTech Connect

    Moran, T.M.

    1984-04-17

    An apparatus for the removal of particulates from a flowing gas stream and a process for its use are provided. A perforated screen separator formed as a plate having parallel rows of perforations formed by pushing alternating strips of the plate material forward and backward from the plane of the plate is used. The perforated screen separator may be used alone or with a fiber bed mist eliminator for increased particulate removal.

  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).

    PubMed

    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. Separation of geometric isomers of native lutein diesters in marigold (Tagetes erecta L.) by high-performance liquid chromatography-mass spectrometry.

    PubMed

    Tsao, Rong; Yang, Raymond; Young, J Christopher; Zhu, Honghui; Manolis, Tony

    2004-08-06

    Lutein is found in many foods; the richest and purest plant source is marigold flower (Tagetes erecta L.). In this plant, lutein is in the form of saturated fatty acid diesters. By using a binary mobile phase consisting of ethyl acetate and acetonitrile-methanol (9:1), improved separation was achieved on a C18-bonded phase. The unique absorption of lutein cis isomers at 330nm was used in combination with MS to identify the novel cis-lutein isomeric dimyristate, myristate-palmitate, dipalmitate, and palmitate-stearate diesters, as well as the rare combinations of both trans- and cis-lutein laurate-palmitate and trans- and cis-lutein myristate-stearate. The presence of the all-trans-lutein laurate-myristate, dimyristate, myristate-palmitate, palmitate-stearate, and distearate diesters, reported by others, was also confirmed.

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

    PubMed

    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.

  7. Separation and quantitation of milk whey proteins of close isoelectric points by on-line capillary isoelectric focusing--electrospray ionization mass spectrometry in glycerol-water media.

    PubMed

    Lecoeur, Marie; Gareil, Pierre; Varenne, Anne

    2010-11-12

    On-line coupling between CIEF and ESI/MS based on the use of bare fused-silica capillaries and glycerol-water media, recently developed in our laboratory, has been investigated for the separation of milk whey proteins that present close pI values. First, a new rinsing procedure, compatible with MS detection, has been developed to desorb these rather hydrophobic proteins (α-casein (α-CN), bovine serum albumin (BSA), lactoferrin (LF)) from the inner capillary wall and to avoid capillary blockages. Common hydrochloric acid washing solution was replaced by a multi-step sequence based on the use of TFA, ammonia and ethanol. To achieve the separation of major whey proteins (β-lactoglobulin A (β-LG A), β-lactoglobulin B (β-LG B), α-lactalbumin (α-LA) and BSA, which possess close pI values (4.5-5.35), CIEF parameters i.e. carrier ampholyte nature, capillary partial filling length with ampholyte/protein mixture and focusing time, have been optimized with respect to total analysis time, sensitivity and precision on pI determination. After optimization of sheath liquid composition (80:20 (v/v) methanol-water+1% HCOOH), quantitation of β-LG A, β-LG B, α-LA and BSA was performed. The limits of detection obtained from extracted ion current (EIC) and single ion monitoring (SIM) modes were in the 57-136 nM and 11-68 nM range, respectively. Finally, first results obtained from biological samples demonstrated the suitability of CIEF-MS as a potential alternative methodology to 2D-PAGE to diagnose milk protein allergies.

  8. Combined cation-exchange and extraction chromatographic method of preconcentration and concomitant separation of bismuth(III) with high molecular mass liquid cation exchanger.

    PubMed

    Mandal, Bhabatosh; Ghosh, Niladri

    2010-10-15

    A selective method has been developed for the extraction chromatographic separation of Bi(III) with Versatic 10 coated on silanized silica gel (SSG). Bi(III) has been quantitatively extracted from 0.1 M acetate buffer at the range of pH 5.0-5.5. The result showed that the solution pH, influent volume, flow-rate and solution temperature would affect the sorption of Bi(III). The sorbed Bi(III) was eluted with 0.1 M H(2)SO(4). The extractor system has got good values of exchange capacity (1.42 meq. of H(+) g(-1) of dry exchanger at 25 degrees C), break-through capacity (19.75 mg g(-1) at pH 5.5) and column efficiencies (300) with respect to Bi(III). The positive value of DeltaH (12.63 kJ mol(-1)) and DeltaS (0.271 kJ mol(-1) K(-1)) and negative value of DeltaG (-68.241 kJ mol(-1)) indicated that the sorption process was endothermic, entropy gaining and spontaneous in nature. P.F. has been optimized at 76.4+/-0.3 and the desorption constants K(desorption) (8x10(-3)) and K'(desorption) (1.4x10(-1)) have been determined. R(f) values and selectivity factors for diverse metal ions with respect to that of Bi(III) have been determined by ion-exchange paper chromatography. Bi(III) has been separated from synthetic mixtures containing its congeners and other metal ions associated with it in ores and alloy samples. The method was found effective for removal of Bi(III) from different water samples. A plausible mechanism for the extraction of Bi(III) has been suggested.

  9. Liquid chromatography/atmospheric pressure chemical ionization tandem mass spectrometry enantiomeric separation of dl-threo-methylphenidate, (Ritalin) using a macrocyclic antibiotic as the chiral selector.

    PubMed

    Ramos, L; Bakhtiar, R; Majumdar, T; Hayes, M; Tse, F

    1999-01-01

    Vancomycin, a macrocyclic antibiotic, is an amphoteric glycopeptide produced by Streptomyces orientalis which has proven to be a viable chiral selector for high performance liquid chromatograph (HPLC) (D. W. Armstrong, Y. Tang, S. Chen, Y. Zhou, C. Bagwill and J-R. Chen, Anal. Chem. (1994; 66: 1473). While it is related to other glycopeptide antibiotics, vancomycin has a number of unique structural features, including 18 stereogenic centers, five aromatic rings, and two side chains one of which is a carbohydrate dimer. Therefore, a vancomycin-based stationary phase appears to be multimodal in that it can be utilized in both normal-phase and reversed-phase liquid chromatography. Consequently, the enantiomeric separation may be operative via several mechanisms, including pi-pi complexation, dipole stacking, inclusion, hydrogen bonding, or combinations of these interactions. LC/MS/MS is a powerful tool for quantitative analysis when evaluated on the basis of speed, specificity, reliability and sensitivity. For these reasons, the present paper explored the feasibility of bonded macrocyclic glycopeptide phases for chiral LC/MS/MS quantitative analysis. Methylphenidate was used as a model compound. A rapid chiral bioanalytical method (<7.5 min) for the determination of the enantiomers of methylphenidate was developed. A lower limit of quantification (LLOQ) of 87 pg/mL was attained for the human plasma assay. This is to our knowledge the first example of enantioselective reversed-phase LC/MS/MS for methylphenidate. The chiral column was relatively cost effective and exhibited excellent performance with no separation deterioration observed after approximately 2500 injections.

  10. Product separator

    DOEpatents

    Welsh, Robert A.; Deurbrouck, Albert W.

    1976-01-20

    A secondary light sensitive photoelectric product separator for use with a primary product separator that concentrates a material so that it is visually distinguishable from adjacent materials. The concentrate separation is accomplished first by feeding the material onto a vibratory inclined surface with a liquid flow, such as a wet concentrating table. Vibrations generally perpendicular to the stream direction of flow cause the concentrate to separate from its mixture according to its color. When the concentrate and its surrounding stream reach the recovery end of the table, a detecting device notes the line of color demarcation and triggers a signal if it differs from a normal condition. If no difference is noted nothing moves on the second separator. However, if a difference is detected in the constant monitoring of the color line's location, a product splitter and recovery unit normally positioned near the color line at the recovery end, moves to a new position. In this manner the selected separated concentrate is recovered at a maximum rate regardless of variations in the flow stream or other conditions present.

  11. On-line stop-flow two-dimensional liquid chromatography-mass spectrometry method for the separation and identification of triterpenoid saponins from ginseng extract.

    PubMed

    Wang, Shuangyuan; Qiao, Lizhen; Shi, Xianzhe; Hu, Chunxiu; Kong, Hongwei; Xu, Guowang

    2015-01-01

    A method based on stop-flow two-dimensional liquid chromatography coupled with electrospray ionization mass spectrometry (2D LC-ESI MS) was established and applied to analyze triterpenoid saponins from the main root of ginseng. Due to the special structure of triterpenoid saponins (they contain polar sugar side chains and nonpolar aglycones), hydrophilic interaction chromatography (HILIC) and reversed-phase liquid chromatography (RPLC) were used for the two dimensions, respectively. A trap column was used to connect the two dimensions. The dilution effect, which is one of the main shortcomings of traditional comprehensive 2D LC methods, was largely avoided. The peak capacity of this system was 747 and the orthogonality was 56.6 %. Compared with one-dimensional HILIC or RP LC MS analysis, 257 and 185 % more mass spectral peaks (ions with intensities that were higher than 1,000) were obtained from the ginseng main root extracts, and 94 triterpenoid saponins were identified based on MS(n) information and summarized aglycone structures. Given its good linearity and repeatability, the established method was successfully applied to classify ginsengs of different ages (i.e., years of growth), and 19 triterpenoid saponins were found through statistical analysis to vary in concentration depending on the age of the ginseng.

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

    PubMed

    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.

  13. Large volume injection in ion chromatography Separation of rubidium and strontium for on-line inductively coupled plasma mass spectrometry determination of strontium isotope ratios.

    PubMed

    García-Ruiz, Silvia; Moldovan, Mariella; García Alonso, J Ignacio

    2007-05-18

    Large volume injection, up to 5 mL, was evaluated and optimised for the on-line ion chromatographic separation of Rb and Sr before ICP-MS measurement of Sr isotope ratios. Flat-topped chromatographic peaks, ideally suited for multicollector ICP-MS isotope ratio measurements, could be obtained when the composition of the mobile phase (nitric acid and 18-crown-6 ether) was identical to the matrix of the sample. Under those conditions rubidium eluted at the dead volume of the column while strontium produced a flat-topped transient signal with several minutes of stable plateau. On-line data acquisition during several minutes at the plateau of Sr signal allowed high precision Sr isotope ratio measurement. The developed procedure was evaluated for Sr isotope ratio measurements on different types of samples, including cider, apples, apple leaves, and soil extracts, in the frame of a long-term project aiming at origin authentication using strontium isotope ratio measurements. It was observed that sample matrix caused broadening of the strontium chromatographic peak and loss of flat-topped peak profile. Under those circumstances the addition of the complexing crown-ether 18-crown-6 both to samples and chromatographic eluent provided two distinct advantages. First, a drastic increase in the retention of strontium was observed which could be modulated by increasing the concentration of nitric acid in the eluent up to 900 mM. This increase in the eluent HNO(3) concentration allowed the application of the method to acid soil digests and other high acidity samples. Second, the matrix of the sample did not affect any more the chromatographic peak profile and similar chromatographic separations could be obtained for samples and standards maintaining the flat-topped Sr peak profile. Sample preparation consisted of a simple 1:10 dilution of the cider or pre-treated solid samples by adding HNO(3) (900 mM) and 18-crown-6 ether (5mM) to obtain similar composition in the sample solution

  14. Online reverse phase-high-performance liquid chromatography-fluorescence detection-electrospray ionization-mass spectrometry separation and characterization of heparan sulfate, heparin, and low-molecular weight-heparin disaccharides derivatized with 2-aminoacridone.

    PubMed

    Galeotti, Fabio; Volpi, Nicola

    2011-09-01

    A high-resolution online reverse-phase-high-performance liquid chromatography (RP-HPLC)-fluorescence detector (Fd)-electrospray ionization-mass spectrometry (ESI-MS) separation and structural characterization of disaccharides prepared from heparin (Hep), heparan sulfate (HS), and various low-molecular-weight (LMW)-Hep using heparin lyases and derivatization with 2-aminoacridone (AMAC) are described. A total of 12 commercially available Hep/HS-derived unsaturated disaccharides were separated and unambiguously identified on the basis of their retention times and mass spectra. The constituent disaccharides of various samples, including unfractionated Hep/HS, fast-moving and slow-moving Hep components, and several marketed products, were characterized. Furthermore, for the first time, the saturated trisulfated disaccharide belonging to the nonreducing end of Heps was detected as being approximately 2% in unfractionated samples and ~15-21% in LMW-Heps prepared by nitrous acid depolymerization. No desalting of the commercial products prior to enzymatic digestion or prepurification steps to eliminate any excess of AMAC reagent or interference from proteins, peptides, and other sample impurities before RP-HPLC-Fd-ESI-MS injection were necessary. This method has applicability for the rapid differentiation of pharmaceutical Heps and LMW-Heps prepared by means of different depolymerization processes and for compositional analysis of small amounts of samples derived from biological sources by using the highly sensitive fluorescence detector.

  15. 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.

    PubMed

    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.

  16. Map Separates

    USGS Publications Warehouse

    ,

    2001-01-01

    U.S. Geological Survey (USGS) topographic maps are printed using up to six colors (black, blue, green, red, brown, and purple). To prepare your own maps or artwork based on maps, you can order separate black-and-white film positives or negatives for any color printed on a USGS topographic map, or for one or more of the groups of related features printed in the same color on the map (such as drainage and drainage names from the blue plate.) In this document, examples are shown with appropriate ink color to illustrate the various separates. When purchased, separates are black-and-white film negatives or positives. After you receive a film separate or composite from the USGS, you can crop, enlarge or reduce, and edit to add or remove details to suit your special needs. For example, you can adapt the separates for making regional and local planning maps or for doing many kinds of studies or promotions by using the features you select and then printing them in colors of your choice.

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

    PubMed

    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.

  18. Application of capillary isotachophoresis-based multidimensional separations coupled with electrospray ionization-tandem mass spectrometry for characterization of mouse brain mitochondrial proteome

    PubMed Central

    Fang, Xueping; Wang, Weijie; Yang, Li; Chandrasekaran, Krish; Kristian, Tibor; Balgley, Brian M.; Lee, Cheng S.

    2017-01-01

    By employing a capillary ITP (CITP)/CZE-based proteomic technology, a total of 1795 distinct mouse Swiss-Prot protein entries (or 1705 nonredundant proteins) are identified from synaptic mitochondria isolated from mouse brain. The ultrahigh resolving power of CITP/CZE is evidenced by the large number of distinct peptide identifications measured from each CITP fraction together with the low peptide fraction overlapping among identified peptides. The degree of peptide overlapping among CITP fractions is even lower than that achieved using combined CIEF/nano-RP LC separations for the analysis of the same mitochondrial sample. When evaluating the protein sequence coverage by the number of distinct peptides mapping to each mitochondrial protein identification, CITP/CZE similarly achieves superior performance with 1041 proteins (58%) having 3 or more distinct peptides, 233 (13%) having 2 distinct peptides, and 521 (29%) having a single distinct peptide. The reproducibility of protein identifications is found to be around 86% by comparing proteins identified from repeated runs of the same mitochondrial sample. The analysis of the mouse mitochondrial proteome by two CITP/CZE runs results in the detection of 2095 distinct mouse Swiss-Prot protein entries (or 1992 nonredundant proteins), corresponding to 59% coverage of the updated Maestro mitochondrial reference set. The collective analysis from combined CITP/CZE and CIEF-based proteomic studies yields the identification of 2191 distinct mitochondrial protein entries (or 2082 nonredundant proteins), corresponding to 76% coverage of the MitoP2-database reference set. PMID:18425750

  19. [Separation and identification of oligosaccharides labeled with 3-amino-9-ethylcarbazole using high performance liquid chromatography and matrix-assisted laser desorption/ionization time-of-flight mass spectrometry].

    PubMed

    Mou, Qing; Zhang, Ying; Huang, Linjuan; Wang, Zhongfu

    2009-01-01

    A pre-column derivatization method for the determination of oligosaccharides based ion a labeling reagent 3-amino-9-ethylcarbazole (AEC) was proposed. The enamines were generated by the reaction of the reducing ends of oligosaccharides and the primary amines of AEC, and then reduced to secondary amines by NaBH3CN, making oligosaccharides labeled by AEC. The derivatives were separated by reversed-phase high performance liquid chromatography (RP-HPLC), and then directly analyzed by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS). The HPLC separation was carried out on a Waters Symmetry C18 column (3.9 mm x 150 mm, 5 microm) with a gradient elution (acetonitrile and ammonium acetate as mobile phases at a flow rate of 1 mL/min) and ultraviolet detection at 254 nm. Under the optimized derivatization and HPLC conditions, the derivatized oligosaccharides were separated, and the derivatization with AEC increased the sensitivity of MS detection. The developed method for the analysis of oligosaccharides is satisfactory.

  20. Separation of closely eluting chloronaphthalene congeners by two-dimensional gas chromatography/quadrupole mass spectrometry: an advanced tool in the study and risk analysis of dioxin-like chloronaphthalenes.

    PubMed

    Hanari, Nobuyasu; Falandysz, Jerzy; Nakano, Takeshi; Petrick, Gert; Yamashita, Nobuyoshi

    2013-08-02

    Two capillary columns of different polarity were applied in a two-dimensional gas chromatography system coupled to a quadrupole mass spectrometric detection (GCxGC/qMS) in order to separate and identify all of the possible 22 isomers of tetra-, 14 of penta- and 10 of hexachloronaphthalene that may occur in selected industrial chemicals. The two-dimensional GCxGC separation was achieved using Rt-β DEXcst and DB-WAX phases, and data imaging was done by 2D and 3D mapping. This combination allows for the analysis of all tetra- to hexachloronaphthalene congeners in a single instrumental run without any pre-separation or fractionation of the analytes. The novel methodology described here can assist in the accurate determination and expression of dioxin-like toxicity of tetrachloronaphthalenes to octachloronaphthalene that are usually present as mixtures at least in abiotic materials such as technical chloronaphthalene formulations (e.g. Halowax mixtures), and wastes containing Halowaxes and other CN formulations.

  1. 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.

    PubMed

    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.

  2. 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.

    PubMed

    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.

  3. 6. VIEW FROM CHESTNUT ST. (upper), WALNUT ST. (lower) THIRD ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    6. VIEW FROM CHESTNUT ST. (upper), WALNUT ST. (lower) THIRD ST. (right) AND FOURTH ST. (left), SHOWING CARPENTERS HALL, FIRST BANK OF U.S. AND SECOND BANK OF U.S. - Independence National Historical Park, Walnut, Sixth, Chestnut & Second Streets, Philadelphia, Philadelphia County, PA

  4. ISOTOPE SEPARATORS

    DOEpatents

    Bacon, C.G.

    1958-08-26

    An improvement is presented in the structure of an isotope separation apparatus and, in particular, is concerned with a magnetically operated shutter associated with a window which is provided for the purpose of enabling the operator to view the processes going on within the interior of the apparatus. The shutier is mounted to close under the force of gravity in the absence of any other force. By closing an electrical circuit to a coil mouated on the shutter the magnetic field of the isotope separating apparatus coacts with the magnetic field of the coil to force the shutter to the open position.

  5. Isotope separation

    DOEpatents

    Bartlett, Rodney J.; Morrey, John R.

    1978-01-01

    A method and apparatus is described for separating gas molecules containing one isotope of an element from gas molecules containing other isotopes of the same element in which all of the molecules of the gas are at the same electronic state in their ground state. Gas molecules in a gas stream containing one of the isotopes are selectively excited to a different electronic state while leaving the other gas molecules in their original ground state. Gas molecules containing one of the isotopes are then deflected from the other gas molecules in the stream and thus physically separated.

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

    USGS Publications Warehouse

    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.

  7. Selective separation and characterization of the stress degradation products of ondansetron hydrochloride by liquid chromatography with quadrupole time-of-flight mass spectrometry.

    PubMed

    Talluri, Murali V N Kumar; Keshari, Kundan Kumar; Kalariya, Pradipbhai D; Srinivas, Ragampeta

    2015-05-01

    Ondansetron hydrochloride was subjected to forced degradation studies under various conditions of hydrolysis (acidic, basic, and neutral), oxidation, photolysis, and thermal as prescribed by International Conference on Harmonisation guideline Q1A (R2). A simple, selective, precise, and accurate high-performance liquid chromatography method was developed on a Waters Xterra C18 (150 × 4.6 mm id, 3.5 μm) column using 10 mM ammonium formate (pH 3.0)/methanol as a mobile phase in gradient elution mode at a flow rate of 0.6 mL/min. The method was extended to liquid chromatography quadrupole time-of-flight tandem mass spectrometry for identification and structural characterization of stress degradation products of ondansetron. The drug showed significant degradation in base hydrolytic and photolytic stress conditions in the liquid state, while it was found to be stable in neutral, acidic, thermal, and oxidative stress conditions. A total of five degradation products were characterized and most probable mechanisms for the formation of degradation products have been proposed on the basis of a comparison of the fragmentation of the [M + H](+) ions of the drug and its degradation products. Finally, the developed method was validated in terms of specificity, linearity, accuracy, precision, and robustness as per International Conference on Harmonisation guideline Q2 (R1).

  8. Multiple heart-cutting two dimensional liquid chromatography mass spectrometry: Towards real time determination of related impurities of bio-pharmaceuticals in salt based separation methods.

    PubMed

    Petersson, Patrik; Haselmann, Kim; Buckenmaier, Stephan

    2016-10-14

    Many of the chromatographic methods used in industry to determine related impurities in bio pharmaceuticals employ salt containing mobile phases. "Salty" mobile phases often provide superior chromatographic performance but are not compatible with mass spectrometry (MS) detection. Peak tracking necessary for method development is therefore often based on peak areas and the chemist's experience/intuition. In addition, MS characterization of impurities usually is done by offline fraction collection, which apart from being time consuming often suffers from poor recovery or the degradation of impurities collected. The recent development of multiple heart-cutting (MHC) two-dimensional liquid chromatography (2D-LC) provides a way to address these problems. This study shows how MHC 2D-LC-MS can be used to obtain almost real time MS data for bovine insulin related impurities present at low level (<0.03%). High quality MS spectra were obtained even for a first dimension using a mobile phase containing high concentrations of sodium, sulphate and phosphate. Thereby MHC 2D-LC-MS offers a possibility to eliminate the guesswork currently associated with peak tracking during method development. Furthermore, in contrast to current characterization methods involving fraction collection, solvent reduction/exchange etc., MS determination is done directly, which markedly shortens the workflow (from days to hours) and reduces the risk for poor recovery and degradation.

  9. 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.

    PubMed

    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.

  10. 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.

    PubMed

    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.

  11. SEPARATION PROCESS

    DOEpatents

    Stoughton, R.W.

    1961-10-24

    A process for separating tetravalent plutonium from aqueous solutions and from niobium and zirconium by precipitation on lanthanum oxalate is described. The oxalate ions of the precipitate may be decomposed by heating in the presence of an oxidizing agent, forming a plutonium compound readily soluble in acid. (AEC)

  12. Plasma separation

    NASA Technical Reports Server (NTRS)

    Steurer, Wolfgang

    1992-01-01

    This process employs a thermal plasma for the separation and production of oxygen and metals. It is a continuous process that requires no consumables and relies entirely on space resources. The almost complete absence of waste renders it relatively clean. It can be turned on or off without any undesirable side effects or residues. The prime disadvantage is its high power consumption.

  13. Electrochromatographic separation of proteins

    NASA Technical Reports Server (NTRS)

    Basak, S. K.; Velayudhan, A.; Kohlmann, K.; Ladisch, M. R.; Mitchell, C. A. (Principal Investigator)

    1995-01-01

    We have developed a modified electrochromatography system which minimizes Joule heating at electric field strengths up to 125 V/cm. A non-linear equilibrium model is described which incorporates electrophoretic mobility, hydrodynamic flow velocity, and an electrically induced concentration polarization at the surface of the stationary phase. This model is able to provide useful estimates of protein retention time and velocity in a column packed with Sephadex gel and subjected to an electric field. A correlation of electrophoretic mobility of peptide and proteins with respect to their charge, molecular mass, and asymmetry enables the selection of solute target molecules for electrochromatographic separations. Good separation of protein mixtures have been obtained.

  14. 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.

    PubMed

    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.

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

    PubMed

    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.

  16. Gas separating

    DOEpatents

    Gollan, Arye Z.

    1990-12-25

    Feed gas is directed tangentially along the non-skin surface of gas separation membrane modules comprising a cylindrical bundle of parallel contiguous hollow fibers supported to allow feed gas to flow from an inlet at one end of a cylindrical housing through the bores of the bundled fibers to an outlet at the other end while a component of the feed gas permeates through the fibers, each having the skin side on the outside, through a permeate outlet in the cylindrical casing.

  17. Gas separating

    DOEpatents

    Gollan, Arye

    1988-01-01

    Feed gas is directed tangentially along the non-skin surface of gas separation membrane modules comprising a cylindrical bundle of parallel contiguous hollow fibers supported to allow feed gas to flow from an inlet at one end of a cylindrical housing through the bores of the bundled fibers to an outlet at the other end while a component of the feed gas permeates through the fibers, each having the skin side on the outside, through a permeate outlet in the cylindrical casing.

  18. Dust separator

    SciTech Connect

    Borow, H.

    1987-01-27

    This patent describes a gas filter apparatus for separating solids from a gas stream comprising a housing having a top, base, and side walls defining a chamber, a partition wall extending across the chamber and separating the chamber into an upper compartment and a lower compartment. A gas inlet conveyor tube in the chamber passes downwardly of the partition and into the lower compartment, the portion of the conveyor tube passing through the upper compartment being impervious and the portion of the conveyor tube extending downwardly into the lower compartment being provided with exit means including exit apertures at least in the area of the conveyor tube adjacent the partition wall. The partition wall is provided with openings surrounding the conveyor tube and communicates the lower compartment with the upper compartment. A filter means in the form of filter tubes covers each opening in the partition wall and extends downwardly in the lower compartment and parallel to the conveyor tube, at least one gas outlet communicating with the upper compartment. A suction means is associated with the gas outlet to provide a reduced pressure within the chamber. A discharge means at the base of the housing is associated with the lower compartment for discharging solid matter separated from the gas stream. The solid laden gas is conveyed into the lower compartment downwardly by the conveying tube and the gas of the stream is drawn from the conveyor tube immediately past the partition, through the surrounding filter tubes in order to prevent the formation of counter gas flows to the gravity discharge of the solids being separated from the gas stream.

  19. Separation system

    DOEpatents

    Rubin, Leslie S.

    1986-01-01

    A separation system for dewatering radioactive waste materials includes a disposal container, drive structure for receiving the container, and means for releasably attaching the container to the drive structure. Separation structure disposed in the container adjacent the inner surface of the side wall structure retains solids while allowing passage of liquids. Inlet port structure in the container top wall is normally closed by first valve structure that is centrifugally actuated to open the inlet port and discharge port structure at the container periphery receives liquid that passes through the separation structure and is normally closed by second valve structure that is centrifugally actuated to open the discharge ports. The container also includes coupling structure for releasable engagement with the centrifugal drive structure. Centrifugal force produced when the container is driven in rotation by the drive structure opens the valve structures, and radioactive waste material introduced into the container through the open inlet port is dewatered, and the waste is compacted. The ports are automatically closed by the valves when the container drum is not subjected to centrifugal force such that containment effectiveness is enhanced and exposure of personnel to radioactive materials is minimized.

  20. [Historical study of separation technology innovation in the field of pharmaceutical science].

    PubMed

    Yamakawa, Koji; Nishitani, Kiyoshi

    2003-01-01

    The separation of organic compounds has been carried out using the method of distillation and recrystallization since the 17th century.1st separation technology innovation (1950s to 1960s). After World War II, the science of separating organic compounds evolved to the use of paper or column chromatography. 2nd separation technology innovation (1960s to 1980s). In the 1960s, thin-layer chromatograpy (TLC) was developed. TLC is a convenient analytical technique for organic compounds. Separation methods for organic compounds using column chromatography and preparative TLC were carried out as practical applications. Gas chromatography (GC) was also introduced in the 1960s. GC is a useful analytical method for a mixture of various volatile organic compounds. Many GC instruments with new kinds of sensors were developed. Gas chromatography of nonbenzenoid organometallic compounds and metal complexes was successfully conducted by the author. 3rd separation technology innovation (1980s to 1990s). In the 1980s, high-performance liquid-chromatography (HPLC) was developed. HPLC analytical methods were useful for various kinds of organic compounds. In the 1990s, LC-MS and LC-NMR instruments were introduced for biomedical products. 4th separation technology innovation (1990s to present). Several new ionization methods for mass-spectrometry (electrospray, matrix-aided lazer desorption ionization, etc) are applied for proteins and biomedical products. Several new separation technologies (supercritical field chromatography, capillary electrophoresis, field-flow fractionization, etc.) are now being developed.

  1. St. Louis, Missouri

    NASA Technical Reports Server (NTRS)

    2007-01-01

    St. Louis is tucked in a bend of the Mississippi River, just south of the point at which the Illinois River joins the larger Mississippi, and where the Missouri River flows in from the west. Drainage patterns to the east, on the Illinois side, are highlighted with green vegetation. Meandering rivers in the verdant Ozark Plateau appear to the south and west.

    This true-color view from NASA's Multi-angle Imaging SpectroRadiometer (MISR) was taken with the instrument's downward looking (nadir) camera on October 15, 2005. The urban areas of greater St. Louis show up as grey-white, including nearby Kirkwood, Webster Groves, Clayton, University City, Ferguson, St. Ann, St. Charles, and East St. Louis. The region is home to nearly three million people.

    MISR was built and is managed by NASA's Jet Propulsion Laboratory, Pasadena, Calif., for NASA's Science Mission Directorate, Washington, DC. The Terra satellite is managed by NASA's Goddard Space Flight Center, Greenbelt, Md. JPL is a division of the California Institute of Technology.

  2. Online Capillary IsoElectric Focusing-ElectroSpray Ionization Mass Spectrometry (CIEF-ESI MS) in Glycerol-Water Media for the Separation and Characterization of Hydrophilic and Hydrophobic Proteins.

    PubMed

    Mokaddem, Meriem; d'Orlyé, Fanny; Varenne, Anne

    2016-01-01

    Capillary isoelectric focusing (CIEF) is a high-resolution technique for the separation of ampholytes, such as proteins, according to their isoelectric point. CIEF coupled online with MS is regarded as a promising alternative to 2-D PAGE for fast proteome analysis with high-resolving capabilities and enhanced structural information without the drawbacks of conventional slab-gel electrophoresis. However, online coupling has been rarely described, as it presents some difficulties. A new methodology for the online coupling of CIEF with electrospray ionization mass spectrometry (ESI-MS) has been developed in glycerol-water media. This new integrated methodology provides a mean for the characterization of a large number of hydrophilic and hydrophobic 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.

    PubMed

    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. 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

    PubMed Central

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

    2016-01-01

    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 150–5,000 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. PMID:26460073

  5. Countercurrent chromatography separation of saponins by skeleton type from Ampelozizyphus amazonicus for off-line ultra-high-performance liquid chromatography/high resolution accurate mass spectrometry analysis and characterisation.

    PubMed

    de Souza Figueiredo, Fabiana; Celano, Rita; de Sousa Silva, Danila; das Neves Costa, Fernanda; Hewitson, Peter; Ignatova, Svetlana; Piccinelli, Anna Lisa; Rastrelli, Luca; Guimarães Leitão, Suzana; Guimarães Leitão, Gilda

    2017-01-20

    Ampelozizyphus amazonicus Ducke (Rhamnaceae), a medicinal plant used to prevent malaria, is a climbing shrub, native to the Amazonian region, with jujubogenin glycoside saponins as main compounds. The crude extract of this plant is too complex for any kind of structural identification, and HPLC separation was not sufficient to resolve this issue. Therefore, the aim of this work was to obtain saponin enriched fractions from the bark ethanol extract by countercurrent chromatography (CCC) for further isolation and identification/characterisation of the major saponins by HPLC and MS. The butanol extract was fractionated by CCC with hexane - ethyl acetate - butanol - ethanol - water (1:6:1:1:6; v/v) solvent system yielding 4 group fractions. The collected fractions were analysed by UHPLC-HRMS (ultra-high-performance liquid chromatography/high resolution accurate mass spectrometry) and MS(n). Group 1 presented mainly oleane type saponins, and group 3 showed mainly jujubogenin glycosides, keto-dammarane type triterpene saponins and saponins with C31 skeleton. Thus, CCC separated saponins from the butanol-rich extract by skeleton type. A further purification of group 3 by CCC (ethyl acetate - ethanol - water (1:0.2:1; v/v)) and HPLC-RI was performed in order to obtain these unusual aglycones in pure form.

  6. Separation and characterization of humic acids from Antarctica by capillary electrophoresis and matrix-assisted laser desorption ionization time-of-flight mass spectrometry. Inclusion complexes of humic acids with cyclodextrins.

    PubMed

    Gajdosová, Dagmar; Novotná, Klára; Prosek, Pavel; Havel, Josef

    2003-10-03

    A new capillary electrophoresis procedure based on micellar electrokinetic capillary chromatography for the separation of humic acids (HAs) isolated from Antarctica soil was developed. The HAs were separated and characterized using a background electrolyte containing 0.09 M borate+0.09 M Tris+0.001 M EDTA (BTE) of pH 8.3, modified with alpha-, beta-, or gamma-cyclodextrins (CDs) and sodium dodecyl sulfate. It was found that from alkaline solution of HAs in the presence of CDs, the HAs are not completely precipitated with a strong acid and a certain part (some fractions) remains soluble. Mass spectrometry shows that HAs contain 15-25 simple low-Mr compounds and several families of compounds with similar structure (m/z approximately 800-1200). Comparison of HA analysis from Antarctica soil with those of soil HAs from the American continent show a high similarity between the samples and confirm several identical compounds and some with very similar structural units.

  7. Rapid extraction and reverse phase-liquid chromatographic separation of mercury(II) and methylmercury in fish samples with inductively coupled plasma mass spectrometric detection applying oxygen addition into plasma.

    PubMed

    Döker, Serhat; Boşgelmez, İffet İpek

    2015-10-01

    A simple and sensitive procedure was developed for extraction and speciation of mercury in fish. Species separation was accomplished with reverse phase-high performance liquid chromatography (HPLC) hyphenated to inductively coupled plasma mass spectrometry (ICP-MS). Oxygen addition into plasma allowed use of organic-rich mobile phase, achieving species separation in 4 min. Mercury species extraction was achieved by microwave exposure for 2 min at mild conditions (60°C, pH 2.0), avoiding necessity of neutralizing sample prior to injection in HPLC, and reducing number of sample preparation steps, analytical source of errors and inter conversion of species. Limit of detection for entire procedure was found to be 0.2 and 0.1 ng g(-1) for mercuric ion and methylmercury, respectively. The method was applied to certified reference materials (TORT-2 and DORM-2) and commercialized fish samples (Mullus barbatus, Sparus aurata, Trachurus mediterraneus, Mugil soiuy, Dicentrarchus labrax, and Pomatomus saltatrix) from Black Sea.

  8. Simultaneous separation of chlorinated/brominated dioxins, polychlorinated biphenyls, polybrominated diphenyl ethers and their methoxylated derivatives from hydroxylated analogues on molecularly imprinted polymers prior to gas/liquid chromatography and mass spectrometry.

    PubMed

    Roszko, Marek; Szymczyk, Krystyna; Jędrzejczak, Renata

    2015-11-01

    Polychlorinated dibenzo-p-dioxins/furans (PCDD/Fs), polychlorinated biphenyls (PCBs) and polybrominated diphenyl ethers (PBDEs) are important contaminants in the environment. In recent years also polybrominated dibenzo-p-dioxins/dibenzofurans (PBDD/Fs) have been reported as emerging environmental stressors. It has been suggested that hydroxylated polybrominated biphenyl ethers (OH-BDEs) are important - may be even the most important - precursors of brominated dioxins/furans. The aim of this study was to develop a robust, time-saving analytical procedure to collectively separate in animal tissues such compounds prior to determination of individual substances with a gas/liquid chromatograph coupled to an ion trap/time-of-flight mass spectrometer (GC/IT-MS or UPLC/TOF-MS). Two OH-CB/BDE separation methods including alkaline extraction and molecularly imprinted polymers (MIP) were compared. Performance of both methods was validated: absolute recovery values were in the 47-90% range depending on the compound, while recovery relative standard deviation was below 20% in most cases. Levels of the studied compounds have been assessed in some real life samples.

  9. Separation and quantification of silver nanoparticles and silver ions using reversed phase high performance liquid chromatography coupled to inductively coupled plasma mass spectrometry in combination with isotope dilution analysis.

    PubMed

    Sötebier, Carina A; Weidner, Steffen M; Jakubowski, Norbert; Panne, Ulrich; Bettmer, Jörg

    2016-10-14

    A reversed phase high performance liquid chromatography coupled to an inductively coupled plasma mass spectrometer (HPLC-ICP-MS) approach in combination with isotope dilution analysis (IDA) for the separation and parallel quantification of nanostructured and ionic silver (Ag) is presented. The main focus of this work was the determination of the ionic Ag concentration. For a sufficient stabilization of the ions without dissolving the nanoparticles (NPs), the eluent had to be initially optimized. The determined Ag ion concentration was in a good agreement with results obtained using ultrafiltration. Further, the mechanism of the NP separation in the HPLC column was investigated. Typical size exclusion effects were found by comparing results from columns with different pore sizes. Since the recovery rates decreased with increasing Ag NP size and large Ag NPs did not elute from the column, additional interactions of the particles with the stationary phase were assumed. Our results reveal that the presented method is not only applicable to Ag NPs, but also to gold and polystyrene NPs. Finally, IDA-HPLC-ICP-MS experiments in single particle mode were performed to determine the particle cut-off size. The comparison with conventional spICP-MS experiments resulted in a similar diameter and particle size distribution.

  10. Gas separating

    DOEpatents

    Gollan, A.

    1988-03-29

    Feed gas is directed tangentially along the non-skin surface of gas separation membrane modules comprising a cylindrical bundle of parallel contiguous hollow fibers supported to allow feed gas to flow from an inlet at one end of a cylindrical housing through the bores of the bundled fibers to an outlet at the other end while a component of the feed gas permeates through the fibers, each having the skin side on the outside, through a permeate outlet in the cylindrical casing. 3 figs.

  11. Gas separating

    DOEpatents

    Gollan, A.Z.

    1990-12-25

    Feed gas is directed tangentially along the non-skin surface of gas separation membrane modules comprising a cylindrical bundle of parallel contiguous hollow fibers supported to allow feed gas to flow from an inlet at one end of a cylindrical housing through the bores of the bundled fibers to an outlet at the other end while a component of the feed gas permeates through the fibers, each having the skin side on the outside, through a permeate outlet in the cylindrical casing. 3 figs.

  12. Analysis of antibody-drug conjugates by comprehensive on-line two-dimensional hydrophobic interaction chromatography x reversed phase liquid chromatography hyphenated to high resolution mass spectrometry. I - Optimization of separation conditions.

    PubMed

    Sarrut, Morgan; Corgier, Amélie; Fekete, Szabolcs; Guillarme, Davy; Lascoux, David; Janin-Bussat, Marie-Claire; Beck, Alain; Heinisch, Sabine

    2016-10-01

    Antibody-drug-conjugates (ADCs) manufacturing leads to a mixture of species which needs to be characterized during development and for further quality control. The coupling of on-line HIC x RPLC to high resolution mass spectrometry can be considered as a very efficient analytical method, providing extensive information on ADC sample, within a reduced time scale. Our intention in this first paper is to present the approach used to rationally optimize the numerous conditions that can affect the quality of the 2D-separation. HIC and RPLC conditions were therefore optimized to prevent salt precipitation due to solvent mixing and to enhance sensitivity, while limiting the total analysis time. We demonstrated that adding salt in the sample solvent before HIC injection allows a significant peak shape improvement. The gradient profile was also carefully optimized in both dimensions, leading to a two-step gradient in HIC and bracketed gradient in RPLC. This study shows that on-line HIC x RPLC hyphenated to high resolution mass spectrometry is a useful method to obtain rapid and extensive structural information on the peaks observed in the first HIC dimension, thereby leading, in a single step requiring 75min, to the precise determination of the average drug-to-antibody ratio (DAR) by HIC as well as the knowledge of the drug load distribution for a particular DAR. The structural characterization of ADC fragments by RPLC-QTOF will be discussed in the second part of this two-part series.

  13. View of looking southeast of 2313 31st St. hipped ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    View of looking southeast of 2313 31st St. - hipped roof house with engaged porch located in Shawmut Mill village section of Valley - 2313 Thirty-first Street (House), 2313 Thirty-first Street, Valley, Chambers County, AL

  14. Mt. St. Helens Memories.

    ERIC Educational Resources Information Center

    Sharp, Len

    1992-01-01

    Provides a personal account of one science teacher's participation in a teacher workshop in which teachers learned about volcanic development, types of eruption, geomorphology, plate tectonics, volcano monitoring, and hazards created by volcanoes by examining Mt. St. Helens. Provides a graphic identifying volcanoes active since 1975. (MDH)

  15. Candide in St. Louis

    ERIC Educational Resources Information Center

    Yee, Roger

    1974-01-01

    A young, St. Louis, Missouri, architectural firm, seeking a personal style of practice, has succeeded in creating structures that reveal client input, and which are sensitive, articulate, and at ease with complexity. Describes an elementary school, a condominium, a shopping mall, a high school, and a "community mall." Illustrated with photographs…

  16. The St. Louis Motor

    ERIC Educational Resources Information Center

    Greenslade, Thomas B., Jr.

    2011-01-01

    The St. Louis Motor, invented in 1909, is unique among physics apparatus for being named for a geographical place rather than a physicist. The sturdy little device (Fig. 1) has never been out of production. Any older school or physics department that has not done a catastrophic housecleaning in the last 20 years will certainly have a small flock…

  17. Particle separator

    DOEpatents

    Hendricks, Charles D.

    1990-01-01

    Method and apparatus (10) are provided for separating and classifying particles (48,50,56) by dispersing the particles within a fluid (52) that is upwardly flowing within a cone-shaped pipe (12) that has its large end (20) above its small end (18). Particles of similar size and shape (48,50) migrate to individual levels (A,B) within the flowing fluid. As the fluid is deflected by a plate (42) at the top end of the pipe (12), the smallest particles are collected on a shelf-like flange (40). Ever larger particles are collected as the flow rate of the fluid is increased. To prevent particle sticking on the walls (14) of the pipe (12), additional fluid is caused to flow into the pipe (12) through holes (68) that are specifically provided for that purpose. Sticking is further prevented by high frequency vibrators (70) that are positioned on the apparatus (10).

  18. Particle separation

    DOEpatents

    Moosmuller, Hans [Reno, NV; Chakrabarty, Rajan K [Reno, NV; Arnott, W Patrick [Reno, NV

    2011-04-26

    Embodiments of a method for selecting particles, such as based on their morphology, is disclosed. In a particular example, the particles are charged and acquire different amounts of charge, or have different charge distributions, based on their morphology. The particles are then sorted based on their flow properties. In a specific example, the particles are sorted using a differential mobility analyzer, which sorts particles, at least in part, based on their electrical mobility. Given a population of particles with similar electrical mobilities, the disclosed process can be used to sort particles based on the net charge carried by the particle, and thus, given the relationship between charge and morphology, separate the particles based on their morphology.

  19. Particle separation

    NASA Technical Reports Server (NTRS)

    Moosmuller, Hans (Inventor); Chakrabarty, Rajan K. (Inventor); Arnott, W. Patrick (Inventor)

    2011-01-01

    Embodiments of a method for selecting particles, such as based on their morphology, is disclosed. In a particular example, the particles are charged and acquire different amounts of charge, or have different charge distributions, based on their morphology. The particles are then sorted based on their flow properties. In a specific example, the particles are sorted using a differential mobility analyzer, which sorts particles, at least in part, based on their electrical mobility. Given a population of particles with similar electrical mobilities, the disclosed process can be used to sort particles based on the net charge carried by the particle, and thus, given the relationship between charge and morphology, separate the particles based on their morphology.

  20. Determination of biocides as well as some biocide metabolites from facade run-off waters by solid phase extraction and high performance liquid chromatographic separation and tandem mass spectrometry detection.

    PubMed

    Bester, K; Lamani, X

    2010-08-06

    Biocides are used to protect buildings, boats, and other materials from microbial infestations. A huge variety of compounds are being used: isothiazolinones, e.g., to prevent bacterial growth in paints, triazines and phenylureas against algal growth on water exposed materials while carbamates are used against fungal investations. However these biocides can be leached from the respective materials. As these are very effective compounds it is important to know the concentrations of these biocides in the leachates as well as their leaching behaviour to assess their risk to the environment. In this study, a method for the determination of biocides from facade material run-off water by means of high performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS) was developed. Due to the amphiphilic character and the expected varying pH-values in the samples, the extractions as well as the HPLC-method development proved to be demanding. The water samples (leachates) were buffered with a phosphate buffer to pH 7. As some of the biocides are very hydrophilic, different SPE cartridges were tested to identify the SPE material with the highest recovery rates for all compounds. For gaining a good separation, analyte trapping was performed on the HPLC column. Quantification was performed using a mass spectrometer in multi-reaction monitoring with two transitions per compound. The final recovery rates were conducted using a cartridge with a divenylbenzyl polymer sorbent. A combination of methanol and acetonitrile as eluents was used to reach recovery rates in the range of 70-100%. The limit of quantification for the compounds of interest ranged from 0.01 to 0.1 microg/L.

  1. The St. Louis Motor

    NASA Astrophysics Data System (ADS)

    Greenslade, Thomas B.

    2011-10-01

    The St. Louis Motor, invented in 1909, is unique among physics apparatus for being named for a geographical place rather than a physicist. The sturdy little device (Fig. 1) has never been out of production. Any older school or physics department that has not done a catastrophic housecleaning in the last 20 years will certainly have a small flock of them in the back room.

  2. St. Kitts and Nevis.

    PubMed

    1989-11-01

    St. Kitts and Nevis have areas of 68 and 36 square miles respectively and the terrain is mountainous. The population is 45,800 total and the annual growth rate is .2%. The ethnic make up is almost all black African with some British, Portuguese, and Lebanese. The religions are primarily Anglican, with evangelical Protestant and Catholic minorities. Infant mortality stands at 41/1000. The government is a constitutional monarchy with a Westminster type parliament. There is a governor, a prime minister, a cabinet, an 11 -member appointed upper house and a 11- member elected house of representatives. The gross national product is $83 million and the annual growth rate is 4.6%. There are no natural resources, and agricultural products include sugarcane, cotton, peanuts, and vegetables. Industry is made up of manufacturing 12.9%, transport and communications 13%, construction 9.1% and hotels and restaurants 4.5%. The Federation of St. Kitts and Nevis became independent in 1983. The government diversified the agriculture by planting other crops than sugar, producing gelled ethanol, and developing a cane spirits liquor. Tourism has grown the most and in 1987 passed sugar as the main source of income. International aid will assist in finishing a road that will open the southeast area of St. Kitts for construction of hotels, where some of the best beaches are located.

  3. Development of a rapid method for the simultaneous separation and determination of 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanol and its N- and O-glucuronides in human urine by liquid chromatography-tandem mass spectrometry.

    PubMed

    Yao, Li; Zheng, Saijing; Guan, Yafeng; Yang, Jun; Liu, Baizhan; Wang, Weimiao; Zhu, Xiaolan

    2013-07-25

    Determination of the tobacco-specific nitrosamine metabolite 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanol (NNAL) and its N- and O-glucuronides (NNAL-N-Gluc and NNAL-O-Gluc) is important for toxicology analysis of tobacco smoke induced carcinogenicity and the understanding of detoxification mechanisms of the carcinogenic nitrosamine in humans. But previously reported indirect measurement methods involving enzymolysis and base treatment steps were tedious and time-consuming. In this work, a direct measurement method for simultaneous determination of urinary NNAL, NNAL-N-Gluc and NNAL-O-Gluc by liquid chromatography-tandem mass spectrometry (LC-MS/MS) in a single run was developed for the first time without the need to perform enzymatic or base hydrolysis. Urine samples were purified using dichloromethane and further extracted by solid-phase extraction. Then they were analyzed by LC-MS/MS operated in electrospray positive ionization mode. Chromatographic separation was achieved on a Phenomenex Kinetex PFP column within 6 min. The proposed method was validated and the results demonstrated that the method can produce satisfactory recoveries and reproducibility for the analytes. The applicability of this newly developed method was investigated for the simultaneous analysis of the three metabolites in smokers' urine and the obtained results were comparable to those detected using the conventional enzymolysis method.

  4. [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].

    PubMed

    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.

  5. Determination and separation of bisphenol A, phthalate metabolites and structural isomers of parabens in human urine with conventional high-pressure liquid chromatography combined with electrospray ionisation tandem mass spectrometry.

    PubMed

    Myridakis, Antonis; Balaska, Eirini; Gkaitatzi, Christina; Kouvarakis, Antonis; Stephanou, Euripides G

    2015-03-01

    Phthalates, bisphenol A (BPA) and parabens (PBs), organic chemicals widely used in everyday products, are considered to be endocrine disruptors. We propose a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the determination of seven phthalate metabolites, six PBs and BPA in human urine. All three categories of the above endocrine disruptors were simultaneously extracted from 1 mL of human urine using solid phase extraction. In addition, with a conventional reversed phase LC column, we achieved for the first time the separation of three pairs of structural isomers, namely iso-/n-butyl paraben, propyl paraben and monobutyl phthalate. LC-MS/MS was operated and tested in both electrospray ionisation (ESI) and atmospheric pressure chemical ionisation (APCI). ESI was selected for the analysis due to its superior stability and repeatability. The method limit of detection (mLOD), achieved for a single set of high-performance LC conditions, ranged from 0.01 to 0.84 ng/mL for phthalate metabolites, from 0.06 to 0.24 ng/mL for PBs and was 2.01 ng/mL for BPA. Derivatisation of BPA with dansyl chloride lowered its mLOD to 0.007 ng/mL. Blank contamination was non-detectable. The present method was successfully applied for the analysis of the above-mentioned compounds in 80 male human urine samples.

  6. Multidimensional peptide separations in proteomics.

    PubMed

    Link, Andrew J

    2002-12-01

    Multidimensional peptide separation will play an increasingly important role in the drive to identify and quantitate the proteome. By increasing the peak and load capacity, multidimensional approaches increase the number and dynamic range of peptides that can be analyzed in a complex biological organism. Separation methods using different physical properties of peptides have been combined with varying degrees of success. The ultimate goal is a rapid separation strategy that can be coupled with analytical methods, such as mass spectrometry, to provide comprehensive monitoring of the changing concentration, interactions, and structures of proteins in the proteome.

  7. Testing Orions Fairing Separation System

    NASA Technical Reports Server (NTRS)

    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.

  8. Mount St. Helens Rebirth

    NASA Technical Reports Server (NTRS)

    2002-01-01

    The catastrophic eruption of Mt. St. Helens 20 years ago today (on May 18, 1980), ranks among the most important natural events of the twentieth century in the United States. Because Mt. St. Helens is in a remote area of the Cascades Mountains, only a few people were killed by the eruption, but property damage and destruction totaled in the billions of dollars. Mount St. Helens is an example of a composite or stratovolcano. These are explosive volcanoes that are generally steep-sided, symmetrical cones built up by the accumulation of debris from previous eruptions and consist of alternating layers of lava flows, volcanic ash and cinder. Some of the most photographed mountains in the world are stratovolcanoes, including Mount Fuji in Japan, Mount Cotopaxi in Ecuador, Mount Hood in Oregon, and Mount Rainier in Washington. The recently erupting Mount Usu on the island of Hokkaido in Japan is also a stratovolcano. Stratovolcanoes are characterized by having plumbing systems that move magma from a chamber deep within the Earth's crust to vents at the surface. The height of Mt. St. Helens was reduced from about 2950 m (9677 ft) to about 2550 m (8364 ft) as a result of the explosive eruption on the morning of May 18. The eruption sent a column of dust and ash upwards more than 25 km into the atmosphere, and shock waves from the blast knocked down almost every tree within 10 km of the central crater. Massive avalanches and mudflows, generated by the near-instantaneous melting of deep snowpacks on the flanks of the mountain, devastated an area more than 20 km to the north and east of the former summit, and rivers choked with all sorts of debris were flooded more than 100 km away. The area of almost total destruction was about 600 sq. km. Ash from the eruption cloud was rapidly blown to the northeast and east producing lightning which started many small forest fires. An erie darkness caused by the cloud enveloped the landscape more than 200 km from the blast area, and ash

  9. Proceedings of the Annual Meeting of the Association for Education in Journalism and Mass Communication (81st, Baltimore, Maryland, August 5-8, 1998). Media Management and Economics; Magazine.

    ERIC Educational Resources Information Center

    Association for Education in Journalism and Mass Communication.

    The Media Management and Economics--Magazine section of the Proceedings contains the following 12 papers: "Not the Same Story: Differences in Sexual Harassment of Women Who Work in Newspaper and Television Newsrooms" (Lori Bergen); "Modeling Strategy for Mass Media: A Resource-Based Approach" (Hugh J. Martin); "The Impact…

  10. Streaming effect of wall oscillation to boundary layer separation

    NASA Technical Reports Server (NTRS)

    Wu, X. H.; Wu, J. Z.; Wu, J. M.

    1991-01-01

    This paper presents a preliminary theoretical result on the time averaged streaming effect of local forcing excitation to the boundary layer separation from smooth surface. The problem is formulated as a periodic disturbance to a basic steady breakaway separating flow, for which the data are taken from a numerical triple-deck solution. The ratio of Strouhal number St and Reynolds number Re plays an important role, both being assumed sufficiently high. The analytical and numerical results show that this streaming effect is quite strong at proper values of St/Re exp 1/4, which may delay or even suppress the separation.

  11. Mount St. Helens Flyover

    NASA Technical Reports Server (NTRS)

    2002-01-01

    This Advanced Spaceborne Thermal Emission and Reflection Radiometer (ASTER) image of Mt. St. Helens volcano in Washington State was acquired on August 8, 2000 and covers an area of 37 by 51 km. Mount Saint Helens, a volcano in the Cascade Range of southwestern Washington that had been dormant since 1857, began to show signs of renewed activity in early 1980. On 18 May 1980, it erupted with such violence that the top of the mountain was blown off, spewing a cloud of ash and gases that rose to an altitude of 19 kilometers. The blast killed about 60 people and destroyed all life in an area of some 180 square kilometers (some 70 square miles), while a much larger area was covered with ash and debris. It continues to spit forth ash and steam intermittently. As a result of the eruption, the mountain's elevation decreased from 2,950 meters to 2,549 meters. The simulated fly-over was produced by draping ASTER visible and near infrared image data over a digital topography model, created from ASTER's 3-D stereo bands. The color was computer enhanced to create a 'natural' color image, where the vegetation appears green. The topography has been exaggerated 2 times to enhance the appearance of the relief. Landsat7 aquired an image of Mt. St. Helens on August 22, 1999. Image and animation courtesy NASA/GSFC/MITI/ERSDAC/JAROS, and U.S./Japan ASTER Science Team.

  12. Solid phase microextraction coupled with comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry for high-resolution metabolite profiling in apples: implementation of structured separations for optimization of sample preparation procedure in complex samples.

    PubMed

    Risticevic, Sanja; DeEll, Jennifer R; Pawliszyn, Janusz

    2012-08-17

    Metabolomics currently represents one of the fastest growing high-throughput molecular analysis platforms that refer to the simultaneous and unbiased analysis of metabolite pools constituting a particular biological system under investigation. In response to the ever increasing interest in development of reliable methods competent with obtaining a complete and accurate metabolomic snapshot for subsequent identification, quantification and profiling studies, the purpose of the current investigation is to test the feasibility of solid phase microextraction for advanced fingerprinting of volatile and semivolatile metabolites in complex samples. In particular, the current study is focussed on the development and optimization of solid phase microextraction (SPME) - comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry (GC × GC-ToFMS) methodology for metabolite profiling of apples (Malus × domestica Borkh.). For the first time, GC × GC attributes in terms of molecular structure-retention relationships and utilization of two-dimensional separation space on orthogonal GC × GC setup were exploited in the field of SPME method optimization for complex sample analysis. Analytical performance data were assessed in terms of method precision when commercial coatings are employed in spiked metabolite aqueous sample analysis. The optimized method consisted of the implementation of direct immersion SPME (DI-SPME) extraction mode and its application to metabolite profiling of apples, and resulted in a tentative identification of 399 metabolites and the composition of a metabolite database far more comprehensive than those obtainable with classical one-dimensional GC approaches. Considering that specific metabolome constituents were for the first time reported in the current study, a valuable approach for future advanced fingerprinting studies in the field of fruit biology is proposed. The current study also intensifies the understanding of SPME

  13. Isobar separator for radioactive nuclear beams project

    SciTech Connect

    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.

  14. The double well mass filter

    DOE PAGES

    Gueroult, Renaud; Rax, Jean -Marcel; Fisch, Nathaniel J.

    2014-02-03

    Various mass filter concepts based on rotating plasmas have been suggested with the specific purpose of nuclear waste remediation. We report on a new rotating mass filter combining radial separation with axial extraction. Lastly, the radial separation of the masses is the result of a “double-well” in effective radial potential in rotating plasma with a sheared rotation profile.

  15. Shoulder separation - aftercare

    MedlinePlus

    Separated shoulder - aftercare; Acromioclavicular joint separation - aftercare; A/C separation - aftercare ... Most shoulder separation injuries are caused by falling onto the shoulder. This causes a tear in the tissue that connects the ...

  16. Characterization of the cod (Gadus morhua) steroidogenic acute regulatory protein (StAR) sheds light on StAR gene structure in fish.

    PubMed

    Goetz, Frederick W; Norberg, Birgitta; McCauley, Linda A R; Iliev, Dimitar B

    2004-03-01

    The full-length cDNA for the cod (Gadus morhua) StAR was cloned by RT-PCR and library screening using ovarian RNA. From the library screening, 2 size classes of cDNA were obtained; a 1577 bp cDNA (cStAR1) and a 2851 bp cDNA (cStAR2). The cStAR1 cDNA presumably encodes a protein of 286 amino acids. The cStAR2 cDNA was composed of 6 separated sequences that contained all of the coding regions of cStAR1 when added together, but also contained 5 noncoding regions not observed in cStAR1. Polymerase chain reactions of cod genomic DNA produced products slightly larger than cStAR2. The sequence of these products were the same as cStAR2 but revealed one additional noncoding region (intron). Thus, the fish StAR gene contains the same number of exons (7) and introns (6) as observed in mammals, but is approximately half the size of the mammalian gene. Using Northern analysis and RT-PCR, cStAR1 expression was observed only in testes, ovaries and head kidneys. Polymerase chain reaction products were also observed using cDNA from steroidogenic tissues and primers designed to regions specific for cStAR2, indicating that cStAR2 is expressed in tissues and may account for the presence of larger transcripts observed on Northern blots.

  17. Mt. St. Helens

    NASA Technical Reports Server (NTRS)

    2001-01-01

    [figure removed for brevity, see original site] [figure removed for brevity, see original site] Figure 1 Movie

    This 3-D anaglyph image of Mt. St. Helens volcano combines the nadir-looking and back-looking band 3 images of ASTER. To view the image in stereo, you will need blue-red glasses. Make sure to look through the red lens with your left eye. Figure 1: This ASTER image of Mt. St. Helens volcano in Washington was acquired on August 8, 2000 and covers an area of 37 by 51 km. Mount Saint Helens, a volcano in the Cascade Range of southwestern Washington that had been dormant since 1857, began to show signs of renewed activity in early 1980. On 18 May 1980, it erupted with such violence that the top of the mountain was blown off, spewing a cloud of ash and gases that rose to an altitude of 19 kilometers. The blast killed about 60 people and destroyed all life in an area of some 180 square kilometers (some 70 square miles), while a much larger area was covered with ash and debris. It continues to spit forth ash and steam intermittently. As a result of the eruption, the mountain's elevation decreased from 2,950 meters to 2,549 meters. The image is centered at 46.2 degrees north latitude, 122.2 degrees west longitude.

    Movie: The simulated fly-over was produced by draping ASTER visible and near infrared image data over a digital topography model, created from ASTER's 3-D stereo bands. The color was computer enhanced to create a natural color image, where the vegetation appears green. The topography has been exaggerated 2 times to enhance the appearance of the relief.

    The U.S. science team is located at NASA's Jet Propulsion Laboratory, Pasadena, Calif. The Terra mission is part of NASA's Science Mission Directorate.

  18. 21st Century Skills Map

    ERIC Educational Resources Information Center

    Partnership for 21st Century Skills, 2011

    2011-01-01

    The Partnership for 21st Century Skills (P21) has forged alliances with key national organizations representing the core academic subjects, including Social Studies, English, Math, Science, Geography, World Languages and the Arts. These collaborations have resulted in the development of 21st Century Skills Maps that illustrate the essential…

  19. Primary mass standard based on atomic masses

    NASA Astrophysics Data System (ADS)

    Becker, Peter; Gläser, Michael

    2006-04-01

    The paper summarises the activities of several national and international Metrology Institutes in replacing the kilogram artefact, the unit of mass, by the mass of a certain number of atoms, in particular the atomic masses of silicon or bismuth. This task is based on two different experiments: a very accurate determination of the Avogadro constant, NA, measuring the density and lattice parameter of an enriched silicon-28 crystal, and the accumulation of decelerated bismuth-209 ions by using a mass separator. The relative measurement uncertainties reached so far are in the first case 2 parts in 107, and in the latter several part in 104. The bismuth experiment is still in an early state of the work. The ratios between the masses of 28Si or 209Bi, respectively, and the present atomic mass standard, the mass of 12C, can be determined with an accuracy now approaching 10-10 using high precision Penning traps mass spectrometers.

  20. Apparatus for diffusion separation

    DOEpatents

    Nierenberg, William A.; Pontius, Rex B.

    1976-08-10

    1. The method of testing the separation efficiency of porous permeable membranes which comprises causing a stream of a gaseous mixture to flow into contact with one face of a finely porous permeable membrane under such conditions that a major fraction of the mixture diffuses through the membrane, maintaining a rectangular cross section of the gaseous stream so flowing past said membrane, continuously recirculating the gas that diffuses through said membrane and continuously withdrawing the gas that does not diffuse through said membrane and maintaining the volume of said recirculating gas constant by continuously introducing into said continuously recirculating gas stream a mass of gas equivalent to that which is continuously withdrawn from said gas stream and comparing the concentrations of the light component in the entering gas, the withdrawn gas and the recirculated gas in order to determine the efficiency of said membrane.

  1. Ferrofluid separator for nonferrous scrap separation

    NASA Technical Reports Server (NTRS)

    Kaiser, R.; Mir, L.

    1974-01-01

    Behavior of nonmagnetic objects within separator is essentially function of density, and independent of size or shape of objects. Results show close agreement between density of object and apparent density of ferrofluid required to float it. Results also demonstrate that very high separation rates are achievable by ferrofluid sink-float separation.

  2. Anomalous magnetoresponse and the Stückelberg axion in holography

    NASA Astrophysics Data System (ADS)

    Jimenez-Alba, Amadeo; Landsteiner, Karl; Melgar, Luis

    2014-12-01

    We study the magnetoresponse with nonconserved currents in holography. Nonconserved currents are dual to massive vector fields in anti-de Sitter (AdS). We introduce the mass in a gauge invariant way via the Stückelberg mechanism. In particular we find generalizations of the chiral magnetic effect, the chiral separation effect and the chiral magnetic wave. Since the associated charge is not conserved we need to source it explicitly by a coupling, the generalization of the chemical potential. In this setup we find that in general the anomalous transport phenomena are still realized. The values we find for nonzero mass connect continuously to the values of the anomalous conductivities of the consistent currents, i.e. the proper chiral magnetic effect vanishes for all masses (as it does for the consistent current in the zero mass case) whereas the chiral separation effect is fully present. The generalization of the chiral magnetic wave shows that for small momenta there is no propagating wave but two purely absorptive modes (one of them diffusive). At higher momenta we recover the chiral magnetic wave as a combination of the two absorptive modes. We also study the negative magneto resistivity and find that it grows quadratically with the magnetic field. The chiral magnetic wave and the negative magneto resistivity are manifestations of the chiral magnetic effect that takes place when the (nonconserved) charge is allowed to fluctuate freely in contrast to the case where the charge is fixed by an explicit source. Since the (classical) U (1 )A symmetry of QCD is not at all a symmetry at the quantum level we also argue that using massive vectors in AdS to model the axial singlet current might result in a more realistic holographic model of QCD and should be a good starting point to investigate the dynamics of anomalous transport in the strongly coupled quark gluon plasma.

  3. ST2249-MRSA-III: a second major recombinant methicillin-resistant Staphylococcus aureus clone causing healthcare infection in the 1970s.

    PubMed

    Nimmo, G R; Steen, J A; Monecke, S; Ehricht, R; Slickers, P; Thomas, J C; Appleton, S; Goering, R V; Robinson, D A; Coombs, G W

    2015-05-01

    Typing of healthcare-associated methicillin-resistant Staphylococcus aureus (MRSA) from Australia in the 1970s revealed a novel clone, ST2249-MRSA-III (CC45), present from 1973 to 1979. This clone was present before the Australian epidemic caused by the recombinant clone, ST239-MRSA-III. This study aimed to characterize the genome of ST2249-MRSA-III to establish its relationship to other MRSA clones. DNA microarray analysis was conducted and a draft genome sequence of ST2249 was obtained. The recombinant structure of the ST2249 genome was revealed by comparisons to publicly available ST239 and ST45 genomes. Microarray analysis of genomic DNA of 13 ST2249 isolates showed gross similarities with the ST239 chromosome in a segment around the origin of replication and with ST45 for the remainder of the chromosome. Recombination breakpoints were precisely determined by the changing pattern of nucleotide polymorphisms in the genome sequence of ST2249 isolate SK1585 compared with ST239 and ST45. One breakpoint was identified to the right of oriC, between sites 1014 and 1065 of the gene D484_00045. Another was identified to the left of oriC, between sites 1185 and 1248 of D484_01632. These results indicate that ST2249 inherited approximately 35.3% of its chromosome from an ST239-like parent and 64.7% from an ST45-like parent. ST2249-MRSA-III resulted from a major recombination between parents that resemble ST239 and ST45. Although only limited Australian archival material is available, the oldest extant isolate of ST2249 predates the oldest Australian isolate of ST239 by 3 years. It is therefore plausible that these two recombinant clones were introduced into Australia separately.

  4. Method and means for separating and classifying superconductive particles

    DOEpatents

    Park, Jin Y.; Kearney, Robert J.

    1991-01-01

    The specification and drawings describe a series of devices and methods for classifying and separating superconductive particles. The superconductive particles may be separated from non-superconductive particles, and the superconductive particles may be separated by degrees of susceptibility to the Meissner effect force. The particles may also be simultaneously separated by size or volume and mass to obtain substantially homogeneous groups of particles. The separation techniques include levitation, preferential sedimentation and preferential concentration. Multiple separation vector forces are disclosed.

  5. Shell Separation for Mirror Replication

    NASA Technical Reports Server (NTRS)

    1999-01-01

    NASA's Space Optics Manufacturing Center has been working to expand our view of the universe via sophisticated new telescopes. The Optics Center's goal is to develop low-cost, advanced space optics technologies for the NASA program in the 21st century - including the long-term goal of imaging Earth-like planets in distant solar systems. To reduce the cost of mirror fabrication, Marshall Space Flight Center (MSFC) has developed replication techniques, the machinery, and materials to replicate electro-formed nickel mirrors. Optics replication uses reusable forms, called mandrels, to make telescope mirrors ready for final finishing. MSFC optical physicist Bill Jones monitors a device used to chill a mandrel, causing it to shrink and separate from the telescope mirror without deforming the mirror's precisely curved surface.

  6. Separation Anxiety (For Parents)

    MedlinePlus

    ... Old Feeding Your 1- to 2-Year-Old Separation Anxiety KidsHealth > For Parents > Separation Anxiety Print A ... help both of you get through it. About Separation Anxiety Babies adapt pretty well to other caregivers. ...

  7. DETERMINATION OF PESTICIDES IN COMPOSITE DIETARY SAMPLES BY GAS CHROMATOGRAPHY/MASS SPECTROMETRY IN THE SELECTED ION MONITORING MODE USING A TEMPERATURE PROGRAMMABLE LARGE VOLUME INJECTOR WITH PRE-SEPARATION COLUMN

    EPA Science Inventory

    Use of a temperature-programmable pre-separation column in the gas chromatographic injection port permits determination of a wide range of semi-volatile pesticides including organochlorines, organophosphates, triazines, and anilines in fatty composite dietary samples while reduci...

  8. Spacecraft -- Capsule Separation (Animation)

    NASA Technical Reports Server (NTRS)

    2005-01-01

    [figure removed for brevity, see original site] Click on the image for Spacecraft -- Capsule Separation animation

    This animation shows the return capsule separating from the Stardust spacecraft.

  9. Mount St. Helens

    NASA Technical Reports Server (NTRS)

    2005-01-01

    This Advanced Spaceborne Thermal Emission and Reflection Radiometer (ASTER) image of Mount St. Helens was captured one week after the March 8, 2005, ash and steam eruption, the latest activity since the volcano's reawakening in September 2004. The new lava dome in the southeast part of the crater is clearly visible, highlighted by red areas where ASTER's infrared channels detected hot spots from incandescent lava. The new lava dome is 155 meters (500 feet) higher than the old lava dome, and still growing.

    With its 14 spectral bands from the visible to the thermal infrared wavelength region, and its high spatial resolution of 15 to 90 meters (about 50 to 300 feet), ASTER images Earth to map and monitor the changing surface of our planet.

    ASTER is one of five Earth-observing instruments launched December 18, 1999, on NASA's Terra satellite. The instrument was built by Japan's Ministry of Economy, Trade and Industry. A joint U.S./Japan science team is responsible for validation and calibration of the instrument and the data products.

    The broad spectral coverage and high spectral resolution of ASTER provides scientists in numerous disciplines with critical information for surface mapping, and monitoring of dynamic conditions and temporal change. Example applications are: monitoring glacial advances and retreats; monitoring potentially active volcanoes; identifying crop stress; determining cloud morphology and physical properties; wetlands evaluation; thermal pollution monitoring; coral reef degradation; surface temperature mapping of soils and geology; and measuring surface heat balance.

    The U.S. science team is located at NASA's Jet Propulsion Laboratory, Pasadena, Calif. The Terra mission is part of NASA's Science Mission Directorate.

    Size: 21.9 by 24.4 kilometers (13.6 by 15.1 miles) Location: 46.2 degrees North latitude, 122.2 degrees West longitude Orientation: North at top Image Data: ASTER bands 8, 3, and 1 Original Data Resolution

  10. Hydrocyclone separation system

    SciTech Connect

    Worrell, J.R.; Wakley, W.D.; Young, G.A.

    1990-05-22

    This patent describes a hydrocyclone separation system for separating a fluid mixture into at least two components having differing densities. It comprises: a first hydrocyclone separator and a second hydrocyclone separator contained within an elongated protective conduit and each being substantially parallel to a longitudinal axis of the conduit, each hydrocyclone separator having a tangential fluid inlet, an overflow fluid outlet and an underflow fluid outlet; and the first hydrocyclone separator and the second hydrocyclone separator being oppositely disposed with respect to each other with the underflow fluid outlet of the first hydrocyclone separator being spaced immediately adjacent to the tangential fluid inlet of the second hydrocyclone separator and the overflow fluid outlet of the first hydrocyclone separator being spaced immediately adjacent the underflow fluid outlet of the second hydrocyclone separator.

  11. Spherical tokamak (ST) transmutation of nuclear wastes

    SciTech Connect

    Peng, Yueng Kay Martin; Cheng, E.T.; Galambos, John D; Cerbone, R. J.

    1995-01-01

    The concept for an ST fusion core that drives a He-cooled, actinide-bearing, molten-salt blanket of moderate power density to generate electricity is examined for the first time. The results show that the fusion core is suited for this purpose and require a level of plasma, power density, engineering, and material performances moderate in comparison with what has been considered desirable for fusion-only power plants. The low aspect ratio of ST introduces a relatively thick, diverted scrape-off layer which leads to reduced heat fluxes at the limiter and divertor tiles. The use of a demountable, water-cooled, single-turn copper center leg for the toroidal field coils enables simplifications of the fusion core configuration and improves overall practicality for future power applications. These result in much reduced size and cost of the fusion core for the transmutation power plant relative to an optimized fusion-only fusion core. Surrounded by a separate tritium-breeding zone, the molten-salt blanket concept is in principle less complex and costly than the thermal breeding blankets for fusion. These combine to effect major reductions in the cost and weight of the power core equipment for the transmutation power plant. The minimum cost of electricity for such a power plant is thus reduced from the best fusion-only counterpart by more than 30%, based on consistent but approximate modeling. The key issues, development steps, and the potential value inherent in the ST fusion core in addressing the world needs for nuclear waste reduction and energy production are discussed.

  12. Separation in 5 Msun Binaries

    NASA Astrophysics Data System (ADS)

    Evans, Nancy R.; Bond, H. E.; Schaefer, G.; Mason, B. D.; Karovska, M.; Tingle, E.

    2013-01-01

    Cepheids (5 Msun stars) provide an excellent sample for determining the binary properties of fairly massive stars. International Ultraviolet Explorer (IUE) observations of Cepheids brighter than 8th magnitude resulted in a list of ALL companions more massive than 2.0 Msun uniformly sensitive to all separations. Hubble Space Telescope Wide Field Camera 3 (WFC3) has resolved three of these binaries (Eta Aql, S Nor, and V659 Cen). Combining these separations with orbital data in the literature, we derive an unbiased distribution of binary separations for a sample of 18 Cepheids, and also a distribution of mass ratios. The distribution of orbital periods shows that the 5 Msun binaries prefer shorter periods than 1 Msun stars, reflecting differences in star formation processes.

  13. 18-Degree-of-Freedom Controller Design for the ST7 Disturbance Reduction System

    NASA Technical Reports Server (NTRS)

    Markley, F. L.; Maghami, P. G.; Houghton, M. B.; Hsu, O. C.

    2003-01-01

    This paper presents the overall design and analysis process of the spacecraft controller being developed at NASA's Goddard Space Flight Center to close the loop between the GRS and the micro-newton colloidal thrusters. The essential dynamics of the ST7-DRS are captured in a simulation including eighteen rigid-body dynamic degrees of freedom: three translations and three rotations for the spacecraft and for each test mass. The ST7 DRS comprises three control systems: the attitude control system (ACS) to maintain a sun-pointing attitude; the drag free control (DFC) to center the spacecraft about the test masses; and the test mass suspension control. This paper summarizes the control design and analysis of the ST7-DRS 18-DOF model, and is an extension of previous analyses employing a 7-DOF planar model of ST-7.

  14. 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.

    PubMed

    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.

  15. Analyse der Störfestigkeit nichtlinearer Schaltungen gegenüber leitungsgebundenen elektromagnetischen Störungen mit multi-input Wiener/Hammerstein-Modellen

    NASA Astrophysics Data System (ADS)

    Stegemann, S.; John, W.; Mathis, W.

    2012-09-01

    In dieser Arbeit wird der Einfluss von leitungsgebundenen Störungen untersucht, welche in einen beliebigen Eingang (Signaleingang, Spannungsversorgung, Masse-Potenzial, etc.) einer Analogschaltung einkoppeln. Die zu untersuchende Schaltung wird dazu durch einen Wiener/Hammerstein-Ansatz als nichtlineares System mit zwei Eingängen modelliert. Mit Hilfe dieses Blockmodells werden analytische Ausdrücke derjenigen Frequenzanteile bestimmt, die durch Intermodulationen zwischen Stör- und Eingangssignal am Ausgang einer Schaltung entstehen.

  16. Pharmacokinetics and bioavailability of ST 1435 administered by different routes.

    PubMed

    Noé, G; Salvatierra, A; Heikinheimo, O; Maturana, X; Croxatto, H B

    1993-12-01

    The ovulation inhibiting potency of the synthetic progestin ST 1435 (Nestorone) is high after parenteral administration and practically nil after oral administration. The purpose of this study was to determine the pharmacokinetic parameters of ST 1435 after single oral or intravenous administration or after long-term treatment with subdermal implants in women. After administration, as a single i.v. bolus, the plasma disappearance rate of immunoreactive ST 1435 had two components with half-lives (mean +/- SE) of 3.5 +/- 0.5 and 83 +/- 14 min, respectively. The volume of distribution was 4.7 +/- 1.3 L/Kg and the metabolic clearance rate was 55 +/- 6 L/Kg/d. After oral administration, the bioavailability was about 10% of the dose. After chronic subdermal administration, the plasmatic clearance was slower than following the acute doses. These results show that ST 1435 has shorter half-lives and a faster clearance rate than progestins which bind SHBG. The large volume of distribution indicates accumulation in the extravascular space and was expected in view of the high affinity of ST 1435 for progesterone receptors. The slower plasma elimination rate after chronic administration was attributed to the re-entry of a larger mass of drug from the extravascular space, and/or accumulation of immunoreactive metabolites with slower clearance than the parent steroid.

  17. [History of St. Johns wort].

    PubMed

    Pöldinger, W

    2000-12-14

    St.-John's wort owes its name to the fact that it flowers at the time of the summer solstice on or around St. John's day on 24 June. Having been administered as a remedy by the Roman military doctor Proscurides as early as the 1st century AD, it was mainly used for magic potions during the Middle Ages. It was not only used to protect humans and animals against witches, demons and evil diseases, but it was also added to the fire when moulding "Freikugel" [1]. Paracelsus was one of the first doctors to concern themselves with St.-John's wort. However, where it had formerly been used for a plethora of indications, in more recent times it has found its place in the treatment of depression and anxiety disorders. In numerous clinical double-blind trials against placebo and other antidepressants the whole extract of St.-John's wort, e.g. as in Jarsin coated tablets, has proved to be just as effective as the other antidepressants for mild and moderate depression, but not for severe depression.

  18. Soluble ST2 Levels and Left Ventricular Structure and Function in Patients With Metabolic Syndrome

    PubMed Central

    Celic, Vera; Majstorovic, Anka; Pencic-Popovic, Biljana; Sljivic, Aleksandra; Lopez-Andres, Natalia; Roy, Ignacio; Escribano, Elena; Beunza, Maite; Melero, Amaia; Floridi, Federico; Magrini, Laura; Marino, Rossella; Salerno, Gerardo; Cardelli, Patrizia

    2016-01-01

    Background A biomarker that is of great interest in relation to adverse cardiovascular events is soluble ST2 (sST2), a member of the interleukin family. Considering that metabolic syndrome (MetS) is accompanied by a proinflammatory state, we aimed to assess the relationship between sST2 and left ventricular (LV) structure and function in patients with MetS. Methods A multicentric, cross-sectional study was conducted on180 MetS subjects with normal LV ejection fraction as determined by echocardiography. LV hypertrophy (LVH) was defined as an LV mass index greater than the gender-specific upper limit of normal as determined by echocardiography. LV diastolic dysfunction (DD) was assessed by pulse-wave and tissue Doppler imaging. sST2 was measured by using a quantitative monoclonal ELISA assay. Results LV mass index (β=0.337, P<0.001, linear regression) was independently associated with sST2 concentrations. Increased sST2 was associated with an increased likelihood of LVH [Exp (B)=2.20, P=0.048, logistic regression] and increased systolic blood pressure [Exp (B)=1.02, P=0.05, logistic regression]. Comparing mean sST2 concentrations (adjusted for age, body mass index, gender) between different LV remodeling patterns, we found the greatest sST2 level in the group with concentric hypertrophy. There were no differences in sST2 concentration between groups with and without LV DD. Conclusions Increased sST2 concentration in patients with MetS was associated with a greater likelihood of exhibiting LVH. Our results suggest that inflammation could be one of the principal triggering mechanisms for LV remodeling in MetS. PMID:27578507

  19. RESONATOR PARTICLE SEPARATOR

    DOEpatents

    Blewett, J.P.; Kiesling, J.D.

    1963-06-11

    A wave-guide resonator structure is designed for use in separating particles of equal momentum but differing in mass, having energies exceeding one billion eiectron volts. The particles referred to are those of sub-atomic size and are generally produced as a result of the bombardment of a target by a beam such as protons produced in a high energy accelerator. In the resonator a travelling electric wave is produced which travels at the same rate of speed as the unwanted particle which is thus deflected continuously over the length of the resonator. The wanted particle is slightly out of phase with the travelling wave so that over the whole length of the resonator it has a net deflection of substantially zero. The travelling wave is established in a wave guide of rectangular cross section in which stubs are provided to store magnetic wave energy leaving the electric wave energy in the main structure to obtain the desired travelling wave and deflection. The stubs are of such shape and spacing to establish a critical mathemitical relationship. (AEC)

  20. RESONATOR PARTICLE SEPARATOR

    DOEpatents

    Blewett, J.P.

    1962-01-01

    A wave guide resonator structure is described for use in separating particles of equal momentum but differing in mass and having energies exceeding one billion electron volts. The particles are those of sub-atomic size and are generally produced as a result of the bombardment of a target by a beam such as protons produced in a high-energy accelerator. In this wave guide construction, the particles undergo preferential deflection as a result of the presence of an electric field. The boundary conditions established in the resonator are such as to eliminate an interfering magnetic component, and to otherwise phase the electric field to obtain a traveling wave such as one which moves at the same speed as the unwanted particle. The latter undergoes continuous deflection over the whole length of the device and is, therefore, eliminated while the wanted particle is deflected in opposite directions over the length of the resonator and is thus able to enter an exit aperture. (AEC)

  1. SO/ST/SRG - SCHEDULING PROGRAMS

    NASA Technical Reports Server (NTRS)

    Collazo, F. F.

    1994-01-01

    ). Schedule Report Generator provides a simple method for generating periodic schedule reports. SRG sorts three types of reports using one or more data fields as sort keys. One type is sorted using the calendar year as the primary key and the end date as the secondary key. Another type is sorted by flight number. A third type of report, Waterfall plots, is also generated by SRG using the end date as the sorting key. SRG requires as input a single file or two concatenated files with up to 400 single line entries. The user constructs the input file by using the LSE editor VAX utility prior to the execution of the program. The user is able to modify the current functional description text lines just displayed. SO, ST and SRG use the same data base file as input. The common data base file has a maximum number of 400 entries. The time span of all three programs is nineteen months. Both of these maximum numbers can be modified by the user. The programs require the VMS Operating System on DEC VAX and were written in PL/1 and DEC Command Language (DCL). SO requires a memory of 61 KB; ST requires 233 KB; and SRG requires 371 KB. The programs can also be purchased separately. They were developed in 1985.

  2. Separation and measurement of flame-formed high molecular weight polycyclic aromatic hydrocarbons by size-exclusion chromatography and laser desorption/ionization time-of-flight mass spectrometry.

    PubMed

    Apicella, B; Millan, M; Herod, A A; Carpentieri, A; Pucci, P; Ciajolo, A

    2006-01-01

    The partial contribution of polycyclic aromatic hydrocarbons (PAH), capable of being detected by gas chromatography (GC-PAH), both to the total mass of the extractable organic fraction of flame-formed carbon particulates and to its UV-visible absorption and fluorescence spectra, has been determined by previous work. This contribution indicates the presence of PAH of molecular weight (MW) greater than 400 Da not accessible to conventional analysis. The detection of species in this higher MW range is important for both their potential toxicology and their possible role in soot formation. In the present work extracts of soots have been analyzed by linear mode laser desorption/ionization time-of-flight mass spectrometry (LDI-TOF-MS) to extend the MW range that can be analyzed beyond the GC-PAH. The results have been compared with both analysis by reflector mode LDI-TOF-MS and the MW evaluation obtained by SEC analysis, as the shortcomings and advantages of both techniques appear to be complementary. Matching the results from the two techniques could give interesting insights in the molecular mass range between GC-PAH and the first soot particles (of mass > 2000 Da). Mass spectra in this molecular mass range have been obtained with a main ion sequence spacing of 24 Th and a minor ion sequence also with a spacing of 24 Th but off-set by 12 Th with respect to the main sequence. The two ion progressions have been interpreted by attributing the predominant peaks mainly to PAH with even-carbon numbers and the smaller ones to cyclopenta-fused ring PAH. These distributions indicate the occurrence of two competitive mechanisms in the growth of PAH and soot nucleation, i.e. the addition of acetylene (HACA mechanism) and the incorporation of pentagons by large polycyclic aromatic molecules into their aromatic bonding network.

  3. Simultaneous separation and determination of phenolic acids, pentapeptides, and triterpenoid saponins in the root of Aster tataricus by high-performance liquid chromatography coupled with electrospray ionization quadrupole time-of-flight mass spectrometry.

    PubMed

    Zhao, Dong-Xia; Hu, Bing-Qiang; Zhang, Mian; Zhang, Chao-Feng; Xu, Xiang-Hong

    2015-02-01

    We established a qualitative method to analyze the main chemical compositions of the root of Aster tataricus. Most of the peaks were separated on a C(18) column packed with 5.0 μm particles, and 28 compounds were identified, including 11 chlorogenic acids, ten astins/asterinins, and seven astersaponins, four of which were reported for the first time from A. tataricus. Furthermore, we developed a reliable method for the simultaneous quantification of 3-caffeoylquinic acid, 3,4-dicaffeoylquinic acid, 3,5-dicaffeoylquinic acid, astin A, astin B, astin C, astersaponin A, and astersaponin C, and the qualified separations were achieved only on a C18 column packed with 2.7 μm particles. The method was used to measure the concentrations of eight components in samples from two major producing areas in China, and the average contents in samples from Bozhou (Anhui) were higher than those in samples from Anguo (Hebei).

  4. St. Louis FUSRAP Lessons Learned

    SciTech Connect

    Eberlin, J.; Williams, D.; Mueller, D.

    2003-02-26

    The purpose of this paper is to present lessons learned from fours years' experience conducting Remedial Investigation and Remedial Action activities at the St. Louis Downtown Site (SLDS) under the Formerly Utilized Sites Remedial Action Program (FUSRAP). Many FUSRAP sites are experiencing challenges conducting Remedial Actions within forecasted volume and budget estimates. The St. Louis FUSRAP lessons learned provide insight to options for cost effective remediation at FUSRAP sites. The lessons learned are focused on project planning (budget and schedule), investigation, design, and construction.

  5. Food safety in the 21st century.

    PubMed

    Käferstein, F; Abdussalam, M

    1999-01-01

    The global importance of food safety is not fully appreciated by many public health authorities despite a constant increase in the prevalence of foodborne illness. Numerous devastating outbreaks of salmonellosis, cholera, enterohaemorrhagic Escherichia coli infections, hepatitis A and other diseases have occurred in both industrialized and developing countries. In addition, many of the re-emerging or newly recognized pathogens are foodborne or have the potential of being transmitted by food and/or drinking water. More foodborne pathogens can be expected because of changing production methods, processes, practices and habits. During the early 21st century, foodborne diseases can be expected to increase, especially in developing countries, in part because of environmental and demographic changes. These vary from climatic changes, changes in microbial and other ecological systems, to decreasing freshwater supplies. However, an even greater challenge to food safety will come from changes resulting directly in degradation of sanitation and the immediate human environment. These include the increased age of human populations, unplanned urbanization and migration and mass production of food due to population growth and changed food habits. Mass tourism and the huge international trade in food and feed is causing food and feedborne pathogens to spread transnationally. As new toxic agents are identified and new toxic effects recognized, the health and trade consequences of toxic chemicals in food will also have global implications. Meeting the huge challenge of food safety in the 21st century will require the application of new methods to identify, monitor and assess foodborne hazards. Both traditional and new technologies for assuring food safety should be improved and fully exploited. This needs to be done through legislative measures where suitable, but with much greater reliance on voluntary compliance and education of consumers and professional food handlers. This will

  6. Food safety in the 21st century.

    PubMed Central

    Käferstein, F.; Abdussalam, M.

    1999-01-01

    The global importance of food safety is not fully appreciated by many public health authorities despite a constant increase in the prevalence of foodborne illness. Numerous devastating outbreaks of salmonellosis, cholera, enterohaemorrhagic Escherichia coli infections, hepatitis A and other diseases have occurred in both industrialized and developing countries. In addition, many of the re-emerging or newly recognized pathogens are foodborne or have the potential of being transmitted by food and/or drinking water. More foodborne pathogens can be expected because of changing production methods, processes, practices and habits. During the early 21st century, foodborne diseases can be expected to increase, especially in developing countries, in part because of environmental and demographic changes. These vary from climatic changes, changes in microbial and other ecological systems, to decreasing freshwater supplies. However, an even greater challenge to food safety will come from changes resulting directly in degradation of sanitation and the immediate human environment. These include the increased age of human populations, unplanned urbanization and migration and mass production of food due to population growth and changed food habits. Mass tourism and the huge international trade in food and feed is causing food and feedborne pathogens to spread transnationally. As new toxic agents are identified and new toxic effects recognized, the health and trade consequences of toxic chemicals in food will also have global implications. Meeting the huge challenge of food safety in the 21st century will require the application of new methods to identify, monitor and assess foodborne hazards. Both traditional and new technologies for assuring food safety should be improved and fully exploited. This needs to be done through legislative measures where suitable, but with much greater reliance on voluntary compliance and education of consumers and professional food handlers. This will

  7. Magnetic separation of algae

    SciTech Connect

    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.

  8. Separation anxiety in children

    MedlinePlus

    ... this 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 ...

  9. Ionene membrane battery separator

    NASA Technical Reports Server (NTRS)

    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.

  10. Control of the ST7 Disturbance Reduction System Flight Experiment

    NASA Technical Reports Server (NTRS)

    Maghami, P. G.; Hsu, O. C,; ODonnell, J. R., Jr.

    2007-01-01

    The Space Technology 7 (ST7) experiment will perform an on-orbit system-level validation of two specific Disturbance Reduction System technologies: colloidal micronewton thrusters and drag-free control. The ST7 Disturbance Reduction System (DRS) is designed to maintain the spacecraft s position with respect to a free-floating test mass while limiting the residual accelerations of that test mass over the frequency range of 1 to 30 mHz. This paper presents the overall design and analysis of the spacecraft drag-free and attitude controllers, with particular attention given to its primary mission mode. These controllers close the loop between the drag-free sensors and the colloidal micronewton thrusters.

  11. Meniscus Membranes For Separation

    DOEpatents

    Dye, Robert C.; Jorgensen, Betty; Pesiri, David R.

    2005-09-20

    Gas separation membranes, especially meniscus-shaped membranes for gas separations are disclosed together with the use of such meniscus-shaped membranes for applications such as thermal gas valves, pre-concentration of a gas stream, and selective pre-screening of a gas stream. In addition, a rapid screening system for simultaneously screening polymer materials for effectiveness in gas separation is provided.

  12. Meniscus membranes for separations

    DOEpatents

    Dye, Robert C.; Jorgensen, Betty; Pesiri, David R.

    2004-01-27

    Gas separation membranes, especially meniscus-shaped membranes for gas separations are disclosed together with the use of such meniscus-shaped membranes for applications such as thermal gas valves, pre-concentration of a gas stream, and selective pre-screening of a gas stream. In addition, a rapid screening system for simultaneously screening polymer materials for effectiveness in gas separation is provided.

  13. Separation in Binary Alloys

    NASA Technical Reports Server (NTRS)

    Frazier, D. O.; Facemire, B. R.; Kaukler, W. F.; Witherow, W. K.; Fanning, U.

    1986-01-01

    Studies of monotectic alloys and alloy analogs reviewed. Report surveys research on liquid/liquid and solid/liquid separation in binary monotectic alloys. Emphasizes separation processes in low gravity, such as in outer space or in free fall in drop towers. Advances in methods of controlling separation in experiments highlighted.

  14. SEARCHING FOR NEW YELLOW SYMBIOTIC STARS: POSITIVE IDENTIFICATION OF StHα63

    SciTech Connect

    Baella, N. O.; Pereira, C. B.; Alvarez-Candal, A.

    2016-04-15

    Yellow symbiotic stars are useful targets for probing whether mass transfer has happened in their binary systems. However, the number of known yellow symbiotic stars is very scarce. We report spectroscopic observations of five candidate yellow symbiotic stars that were selected by their positions in the 2MASS (J − H) versus (H − K{sub s}) diagram and which were included in some emission-line catalogs. Among the five candidates, only StHα63 is identified as a new yellow symbiotic star because of its spectrum and its position in the [TiO]{sub 1}–[TiO]{sub 2} diagram, which indicates a K4–K6 spectral type. In addition, the derived electron density (∼10{sup 8.4} cm{sup −3}) and several emission-line intensity ratios provide further support for that classification. The other four candidates are rejected as symbiotic stars because three of them actually do not show emission lines and the fourth one only Balmer emission lines. We also found that the WISE W3–W4 index clearly separates normal K-giants from yellow symbiotic stars and therefore can be used as an additional tool for selecting candidate yellow symbiotic stars.

  15. Metrics For Comparing Plasma Mass Filters

    SciTech Connect

    Abraham J. Fetterman and Nathaniel J. Fisch

    2012-08-15

    High-throughput mass separation of nuclear waste may be useful for optimal storage, disposal, or environmental remediation. The most dangerous part of nuclear waste is the fission product, which produces most of the heat and medium-term radiation. Plasmas are well-suited to separating nuclear waste because they can separate many different species in a single step. A number of plasma devices have been designed for such mass separation, but there has been no standardized comparison between these devices. We define a standard metric, the separative power per unit volume, and derive it for three different plasma mass filters: the plasma centrifuge, Ohkawa filter, and the magnetic centrifugal mass filter. __________________________________________________

  16. Metrics for comparing plasma mass filters

    SciTech Connect

    Fetterman, Abraham J.; Fisch, Nathaniel J.

    2011-10-15

    High-throughput mass separation of nuclear waste may be useful for optimal storage, disposal, or environmental remediation. The most dangerous part of nuclear waste is the fission product, which produces most of the heat and medium-term radiation. Plasmas are well-suited to separating nuclear waste because they can separate many different species in a single step. A number of plasma devices have been designed for such mass separation, but there has been no standardized comparison between these devices. We define a standard metric, the separative power per unit volume, and derive it for three different plasma mass filters: the plasma centrifuge, Ohkawa filter, and the magnetic centrifugal mass filter.

  17. The Greening of St Patrick's.

    ERIC Educational Resources Information Center

    Barron, Jennie

    1993-01-01

    The grade 6-7 class at St. Patrick's School in Hamilton (Ontario) engages in outdoor environmental projects to enhance classroom learning. Some student activities have been (1) worm composting; (2) tree planting; (3) restoring tern nesting areas; and (4) planning and cultivating a sophisticated garden on school grounds. (KS)

  18. Fort St. Vrain experience report

    SciTech Connect

    Not Available

    1980-06-01

    This report describes the core region constraint devices (RCDs) which will be installed in Fort St. Vrain to remedy core temperature fluctuations at high power-to-flow thresholds, summarizes the engineering analyses supporting the design, and evaluates effects on fuel handling operations. (DLC)

  19. The 21st Century Learner.

    ERIC Educational Resources Information Center

    Sheppard, Beverly

    The profound changes of the 21st century are transforming America into what must become a learning society. Never before have museums, libraries and the whole of the non-formal sector of educational institutions faced such challenges and opportunities. The demand is great for fresh and innovative thinking to construct a bold, new learning network…

  20. The Secrets of St. Agnes

    ERIC Educational Resources Information Center

    Ross, Janell

    2006-01-01

    This article reveals the disturbing truths uncovered by a retired biology professor about the past practices of a North Carolina hospital. In the 1990s, Irene Clark was a biology professor at St. Augustine's College, a historically Black college in Raleigh, North Carolina. One day, a janitor asked the native Virginian what she knew about the…

  1. Mount St. Helens aerosol evolution

    SciTech Connect

    Oberbeck, V.R.; Farlow, N.H.

    1982-08-01

    Stratospheric aerosol samples were collected using a wire impactor during the year following the eruption of Mount St. Helens. Analysis of samples shows that aerosol volume increased for 6 months due to gas-to-particle conversion and then decreased to background levels in the following 6 months.

  2. Mount St. Helens aerosol evolution

    SciTech Connect

    Oberbeck, V.R.; Farlow, N.H.; Fong, W.; Snetsinger, K.G.; Ferry, G.V.; Hayes, D.M.

    1982-09-01

    Stratospheric aerosol samples were collected using a wire impactor during the year following the eruption of Mt. St. Helens. Analysis of samples show that aerosol volume increased for 6 months due to gas-to-particle conversion and then decreased to background levels in the following 6 months.

  3. Toward 21st Century Supports

    ERIC Educational Resources Information Center

    Umphrey, Jan

    2010-01-01

    This article presents an interview with Linda Darling-Hammond, Charles Ducommun Professor of Education at Stanford University, director of the Stanford Center for Opportunity Policy and Education, and codirector of the school redesign network at Stanford. In this interview, Darling-Hammond describes the term "21st century skills" and shares her…

  4. 41st Aerospace Mechanisms Symposium

    NASA Technical Reports Server (NTRS)

    Boesiger, Edward A. (Editor)

    2012-01-01

    The proceedings of the 41st Aerospace Mechanisms Symposium are reported. JPL hosted the conference, which was held in Pasadena Hilton, Pasadena, California on May 16-18, 2012. Lockheed Martin Space Systems cosponsored the symposium. Technology areas covered include gimbals and positioning mechanisms, components such as hinges and motors, CubeSats, tribology, and Mars Science Laboratory mechanisms.

  5. Safety shutdown separators

    DOEpatents

    Carlson, Steven Allen; Anakor, Ifenna Kingsley; Farrell, Greg Robert

    2015-06-30

    The present invention pertains to electrochemical cells which comprise (a) an anode; (b) a cathode; (c) a solid porous separator, such as a polyolefin, xerogel, or inorganic oxide separator; and (d) a nonaqueous electrolyte, wherein the separator comprises a porous membrane having a microporous coating comprising polymer particles which have not coalesced to form a continuous film. This microporous coating on the separator acts as a safety shutdown layer that rapidly increases the internal resistivity and shuts the cell down upon heating to an elevated temperature, such as 110.degree. C. Also provided are methods for increasing the safety of an electrochemical cell by utilizing such separators with a safety shutdown layer.

  6. 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.

    PubMed

    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.

  7. Acoustofluidic bacteria separation

    NASA Astrophysics Data System (ADS)

    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.

  8. Magnetic Separator Enhances Treatment Possibilities

    NASA Technical Reports Server (NTRS)

    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.

  9. 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.

    PubMed

    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.

  10. Momentum errors in an RF separated beam

    SciTech Connect

    T. Kobilarcik

    2002-09-19

    The purity of an RF separated beam is affected by the difference in mass of the particle types and the momentum bite of the beam. The resulting time-of-flight difference between different types allows separation to occur; the finite momentum bite results in chromatic aberration. Both these features also give rise to a particle type dependent velocity bite, which must also be taken into account. This memo demonstrates a generalizable method for calculating the effect.

  11. 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.

    PubMed

    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 <14.87%) and recovery (89.4-105.8%) of the method were achieved. A major advantage of the proposed method is that it can almost detect members of all eight groups of 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.

  12. Combined cation-exchange and extraction chromatographic method of pre-concentration and concomitant separation of Cu(II) with high molecular mass liquid cation exchanger after its online detection.

    PubMed

    Mandal, B; Roy, U S; Datta, D; Ghosh, N

    2011-08-19

    A selective method has been developed for the extraction chromatographic trace level separation of Cu(II) with Versatic 10 (liquid cation exchanger) coated on silanised silica gel (SSG-V10). Cu(II) has been extracted from 0.1M acetate buffer at the range of pH 4.0-5.5. The effects of foreign ions, pH, flow-rate, stripping agents on extraction and elution have been investigated. Exchange capacity of the prepared exchanger at different temperatures with respect to Cu(II) has been determined. The extraction equilibrium constant (K(ex)) and different standard thermodynamic parameters have also been calculated by temperature variation method. Positive value of ΔH (7.98 kJ mol⁻¹) and ΔS (0.1916 kJ mol⁻¹) and negative value of ΔG (-49.16 kJ mol⁻¹) indicated that the process was endothermic, entropy gaining and spontaneous. Preconcentration factor was optimized at 74.7 ± 0.2 and the desorption constants K(desorption)¹(1.4 × 10⁻²) and K(desorption)²(9.8 × 10⁻²) were determined. The effect of pH on R(f) values in ion exchange paper chromatography has been investigated. In order to investigate the sorption isotherm, two equilibrium models, the Freundlich and Langmuir isotherms, were analyzed. Cu(II) has been separated from synthetic binary and multi-component mixtures containing various metal ions associated with it in ores and alloy samples. The method effectively permits sequential separation of Cu(II) from synthetic quaternary mixture containing its congeners Bi(III), Sn(II), Hg(II) and Cu(II), Cd(II), Pb(II) of same analytical group. The method was found effective for the selective detection, removal and recovery of Cu(II) from industrial waste and standard alloy samples following its preconcentration on the column. A plausible mechanism for the extraction of Cu(II) has been suggested.

  13. Combining poly(dimethyldiphenylsiloxane) and nitrile phases for improving the separation and quantitation of benzalkonium chloride homologues: In-tube solid phase microextraction-capillary liquid chromatography-diode array detection-mass spectrometry for analyzing industrial samples.

    PubMed

    Prieto-Blanco, M C; Moliner-Martinez, Y; Campíns-Falcó, P

    2013-07-05

    The retention and separation of four homologues of benzalkonium chloride (alkyl (C12, C14, C16, C18) dimethylbenzylammonium chloride) have been studied in poly(dimethyldiphenylsiloxane) (TRB) and nitrile capillary phases, respectively. Under the optimized conditions (50% acetonitrile in processed samples, 35% of diphenyl content of the TRB, capillary length 43cm and water:methanol 60:40 as replacing solvent), the extraction efficiency was similar for all the homologues with satisfactory reproducibility and independently of the amount and proportion of homologues. Industrial samples with high viscosity or with complex composition and washes waters have been analyzed without previous treatment. The coupling of IT-SPME-CapLC-DAD to MS detection allowed the determination of the minority homologues (C16 and C18) in the industrial samples and washes waters. No matrix effect was found.

  14. Development of a coupled diffusion denuder system combined with gas chromatography/mass spectrometry for the separation and quantification of molecular iodine and the activated iodine compounds iodine monochloride and hypoiodous acid in the marine atmosphere.

    PubMed

    Huang, Ru-Jin; Hoffmann, Thorsten

    2009-03-01

    This study concerns the development of a coupled diffusion denuder system capable of separating and quantifying gaseous molecular iodine (I(2)) and two other highly reactive iodine species, ICl and HOI, which are collectively named activated iodine compounds (AIC). Both I(2) and AIC are key species in the atmospheric chemistry of iodine. 1,3,5-Trimethoxybenzene (1,3,5-TMB)- and alpha-cyclodextrin/(129)I(-) (alpha-CD/(129)I(-))-coated denuders proved to be suitable for the collection of gaseous AIC and I(2), respectively. The experimental collection efficiencies for AIC (tested as ICl) and I(2) agreed well with the theoretical values for gas flow rates in the range between 300 and 1800 mL min(-1). The coupled denuder system (1,3,5-TMB-coated denuder as front-denuder coupled upstream of an alpha-CD/(129)I(-)-coated denuder) was applied successfully to separate test gas mixtures of ICl and I(2) at various mixing ratios in the laboratory. The operation of both denuder systems was demonstrated to be independent of relative humidity (0-100%) and storage period (at least 2 weeks prior to and after sampling). Detection limits were achieved at sub-parts-per-trillion-by-volume (sub-pptv) level. The presented method provides a reliable and practical approach for the speciation of gaseous iodine compounds. In addition, we report for the first time ambient air measurements of AIC mixing ratios, carried out at the atmospheric research station in Mace Head, Ireland. A maximum concentration of AIC of 30.2 pptv was observed for nighttime measurements and 6.0 pptv for daytime measurements. A similar diurnal pattern was found for I(2) with an average concentration level of 23.2 pptv during daytime and 85.1 pptv during nighttime, indicating a strong correlation with AIC.

  15. 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.

    PubMed

    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.

  16. [Separation anxiety. Theoretical considerations].

    PubMed

    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

  17. Isotope separation by photochromatography

    DOEpatents

    Suslick, K.S.

    1975-10-03

    A photochromatographic method for isotope separation is described. An isotopically mixed molecular species is adsorbed on an adsorptive surface, and the adsorbed molecules are irradiated with radiation of a predetermined wavelength which will selectively excite desired isotopic species. Sufficient energy is transferred to the excited molecules to desorb them from the surface and thus separate them from the undesired isotopic species. The method is particularly applicable to the separation of hydrogen isotopes. (BLM)

  18. Isotope separation by photochromatography

    DOEpatents

    Suslick, Kenneth S.

    1977-01-01

    An isotope separation method which comprises physically adsorbing an isotopically mixed molecular species on an adsorptive surface and irradiating the adsorbed molecules with radiation of a predetermined wavelength which will selectively excite a desired isotopic species. Sufficient energy is transferred to the excited molecules to desorb them from the surface and thereby separate them from the unexcited undesired isotopic species. The method is particularly applicable to the separation of hydrogen isotopes.

  19. Membrane separation systems

    SciTech Connect

    Baker, R.W.; Cussler, E.L.; Eykamp, W.; Koros, W.J.; Riley, R.L.; Strathman, R.H.

    1991-01-01

    This book discusses developments and future directions in the field of membrane separation systems. It describes research needed to bring energy-saving membrane separation processes to technical and commercial readiness for commercial acceptance within the next 5 to 20 years. The assessment was conducted by a group of six internationally known membrane separations experts who examined the worldwide status of research in seven major membrane areas. These encompassed four mature technology areas: reverse osmosis, microfiltration, ultrafiltration, and electrodialysis; two developing areas: gas separation and pervaporation; and one emerging technology; facilitated transport.

  20. The ADvanced SEParation (ADSEP)

    NASA Technical Reports Server (NTRS)

    1998-01-01

    The ADvanced SEParation (ADSEP) commercial payload is making use of major advances in separation technology: The Phase Partitioning Experiment (PPE); the Micorencapsulation experiment; and the Hemoglobin Separation Experiment (HSE). Using ADSEP, commercial researchers will attempt to determine the partition coefficients for model particles in a two-phase system. With this information, researchers can develop a higher resolution, more effective cell isolation procedure that can be used for many different types of research and for improved health care. The advanced separation technology is already being made available for use in ground-based laboratories.

  1. Pre-Separation Guide

    DTIC Science & Technology

    1992-03-04

    hands; V Prosthetic appliances, sensory , Veteran Counseling and rehabilitative aids; To allow service members to better V Medical care for Dependents...Atlanta 30365 800-827-0634 San Diego 92108 telephone: local 881-1776 or telephone: local 297-8220 or 800-827-2039 Iowa 800-532-3811 210 Walnut St...STATE SERVED Federal Office Building IOWA MISSOURI Room 1 100 KANSAS NEBRASKA 911 Walnut Street Kansas City, MO 64106 Telephone: 816/426-3856 REGION

  2. Peptide mass fingerprinting.

    PubMed

    Thiede, Bernd; Höhenwarter, Wolfgang; Krah, Alexander; Mattow, Jens; Schmid, Monika; Schmidt, Frank; Jungblut, Peter R

    2005-03-01

    Peptide mass fingerprinting by MALDI-MS and sequencing by tandem mass spectrometry have evolved into the major methods for identification of proteins following separation by two-dimensional gel electrophoresis, SDS-PAGE or liquid chromatography. One main technological goal of proteome analyses beside high sensitivity and automation was the comprehensive analysis of proteins. Therefore, the protein species level with the essential information on co- and post-translational modifications must be achieved. The power of peptide mass fingerprinting for protein identification was described here, as exemplified by the identification of protein species with high molecular masses (spectrin alpha and beta), low molecular masses (elongation factor EF-TU fragments), splice variants (alpha A crystallin), aggregates with disulfide bridges (alkylhydroperoxide reductase), and phosphorylated proteins (heat shock protein 27). Helpful tools for these analyses were the use of the minimal protein identifier concept and the software program MS-Screener to remove mass peaks assignable to contaminants and neighbor spots.

  3. The 21st century propulsion

    NASA Technical Reports Server (NTRS)

    Haloulakos, V. E.; Boehmer, C.

    1990-01-01

    The prediction of future space travel in the next millennium starts by examining the past and extrapolating into the far future. Goals for the 21st century include expanded space travel and establishment of permanent manned outposts, and representation of Lunar and Mars outposts as the most immediate future in space. Nuclear stage design/program considerations; launch considerations for manned Mars missions; and far future propulsion schemes are outlined.

  4. The Wake of St. Vincent.

    NASA Astrophysics Data System (ADS)

    Smith, Ronald B.; Gleason, Arthur C.; Gluhosky, Paul A.; Grubii, Vanda

    1997-03-01

    The island of St. Vincent and the other Windward Islands in the southeastern Caribbean were chosen as a field site for the study of weak mountain wakes. By the authors' definition, a `weak wake' forms when the potential vorticity generated by a mountain is not strong enough to advect itself into eddies; rather, it is simply advected downstream by the ambient flow. GOES-8 and Landsat sunglint images unambiguously revealed that the mountainous Windward Islands have remarkably long straight wakes. The length of St. Vincent's wake exceeds 300 km although its width is only 20 km. Near the islands, the wake structures reflect the details of the island topography. These wakes do not exhibit any obvious diurnal effect.Boat surveys in the lee of St. Vincent confirmed the existence of features seen in the images: the sharp wake boundary, the small valley-induced jet embedded in the near wake, and the absence of any reverse flow. Aircraft surveys gave evidence of descent over the island and showed that the wake air is relatively warm and dry. The length of the wake (L) agrees with the formula L = H/2CD (where H is the wake depth and CD is the surface drag coefficient), implying that the reacceleration of the wake air is caused by the ambient streamwise pressure gradient rather than by lateral entrainment of momentum or geostrophic adjustment.Two numerical models were used to simulate St. Vincent's wake, a single-layer hydrostatic model and a 3D nonhydrostatic model. Both models indicated that air descent, acceleration, wave breaking, and weak potential vorticity generation occur over the island, causing a long straight wake.

  5. Continuous separation of proteins by annular chromatography

    SciTech Connect

    Bloomingburg, G.F.; Bauer, J.S.; Carta, G. ); Byers, C.H. )

    1991-05-01

    In this paper, the separation of protein mixtures by continuous annular chromatography (CAC) is studied in a preparative-scale apparatus. S-Sepharose, a strong-acid porous cation-exchange resin is used as the separation medium, and mixtures of albumin, hemoglobin and cytochrome c are used as model separation system. Equilibrium and mass-transfer parameters are developed for this system on the basis of fixed-bed chromatograph experiments. A mathematical model is then successfully used in conjunction with these parameters to simulate the performance of the CAC separations. The continuous separation performance of the annular apparatus is found to be essentially the same as the batchwise performance of an equivalent conventional chromatograph, making the unit attractive for preparative and process-scale applications where continuous throughput is desirable.

  6. Adventures in maceral separation

    SciTech Connect

    Dyrkacz, G.R.

    1994-02-01

    Progress has been made in recent years in the science of maceral separation. However, there are many areas that can be improved and new areas investigated. Power of density gradient centrifugation to physically resolve macerals and submaceral species coupled with other instrumental techniques is attractive for defining the limits of coal heterogeneity as well as investigating the ability of other separation methods.

  7. Method for separating isotopes

    DOEpatents

    Jepson, B.E.

    1975-10-21

    Isotopes are separated by contacting a feed solution containing the isotopes with a cyclic polyether wherein a complex of one isotope is formed with the cyclic polyether, the cyclic polyether complex is extracted from the feed solution, and the isotope is thereafter separated from the cyclic polyether.

  8. URANIUM SEPARATION PROCESS

    DOEpatents

    McVey, W.H.; Reas, W.H.

    1959-03-10

    The separation of uranium from an aqueous solution containing a water soluble uranyl salt is described. The process involves adding an alkali thiocyanate to the aqueous solution, contacting the resulting solution with methyl isobutyl ketons and separating the resulting aqueous and organic phase. The uranium is extracted in the organic phase as UO/sub 2/(SCN)/sub/.

  9. Vanguard Satellite Separation Mechanisms

    NASA Technical Reports Server (NTRS)

    Baumann, Robert C.

    1961-01-01

    Early in the Vanguard program it became apparent that a thoroughly reliable means of separating the satellite packages from the third-stage rocket would be required. A completely self -contained standard mechanism was developed with redundant firing circuits for use on both test vehicles and satellite-launching vehicles. A change in the experimental objectives of the test-vehicle payload units necessitated modification of some of the standard separation mechanisms. A strap, pull-pin, girth-ring separation device was developed which employed the basic actuation of the standard mechanisms. Evidence of residual burning of the third stage made it necessary to delay separation longer than the time designed into the long-delay separation device. The standard separation mechanism was modified and integrated with the satellite command receiver system so that a ground command after third-stage burnout would cause separation. Flight performance of the various separation mechanisms proved their reliability; they performed without failure in all Vanguard launchings.

  10. Working with Separation

    ERIC Educational Resources Information Center

    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)

  11. Overview of membrane separations

    SciTech Connect

    Noble, R.D.

    1987-01-01

    The field of membrane separations is discussed. The major membrane types and applications are outlined. The outlook with respect to research activities and commercial applications is surveyed. The advantages and disadvantages of this separation process are discussed. Certain applications where membranes may save energy and improve productivity are also discussed.

  12. 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.

    PubMed

    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.

  13. Separators for flywheel rotors

    DOEpatents

    Bender, D.A.; Kuklo, T.C.

    1998-07-07

    A separator forms a connection between the rotors of a concentric rotor assembly. This separator allows for the relatively free expansion of outer rotors away from inner rotors while providing a connection between the rotors that is strong enough to prevent disassembly. The rotor assembly includes at least two rotors referred to as inner and outer flywheel rings or rotors. This combination of inner flywheel ring, separator, and outer flywheel ring may be nested to include an arbitrary number of concentric rings. The separator may be a segmented or continuous ring that abuts the ends of the inner rotor and the inner bore of the outer rotor. It is supported against centrifugal loads by the outer rotor and is affixed to the outer rotor. The separator is allowed to slide with respect to the inner rotor. It is made of a material that has a modulus of elasticity that is lower than that of the rotors. 10 figs.

  14. Separators for flywheel rotors

    DOEpatents

    Bender, Donald A.; Kuklo, Thomas C.

    1998-01-01

    A separator forms a connection between the rotors of a concentric rotor assembly. This separator allows for the relatively free expansion of outer rotors away from inner rotors while providing a connection between the rotors that is strong enough to prevent disassembly. The rotor assembly includes at least two rotors referred to as inner and outer flywheel rings or rotors. This combination of inner flywheel ring, separator, and outer flywheel ring may be nested to include an arbitrary number of concentric rings. The separator may be a segmented or continuous ring that abuts the ends of the inner rotor and the inner bore of the outer rotor. It is supported against centrifugal loads by the outer rotor and is affixed to the outer rotor. The separator is allowed to slide with respect to the inner rotor. It is made of a material that has a modulus of elasticity that is lower than that of the rotors.

  15. Substituted polyacetylene separation membrane

    DOEpatents

    Pinnau, I.; Morisato, Atsushi

    1998-01-13

    A separation membrane is described which is useful for gas separation, particularly separation of C{sub 2+} hydrocarbons from natural gas. The invention encompasses the membrane itself, methods of making it and processes for using it. The membrane comprises a polymer having repeating units of a hydrocarbon-based, disubstituted polyacetylene, having the general formula shown in the accompanying diagram, wherein R{sub 1} is chosen from the group consisting of C{sub 1}-C{sub 4} alkyl and phenyl, and wherein R{sub 2} is chosen from the group consisting of hydrogen and phenyl. In the most preferred embodiment, the membrane comprises poly(4-methyl-2-pentyne) [PMP]. The membrane exhibits good chemical resistance and has super-glassy properties with regard to separating certain large, condensable permeant species from smaller, less-condensable permeant species. The membranes may also be useful in other fluid separations. 4 figs.

  16. Substituted polyacetylene separation membrane

    DOEpatents

    Pinnau, Ingo; Morisato, Atsushi

    1998-01-13

    A separation membrane useful for gas separation, particularly separation of C.sub.2+ hydrocarbons from natural gas. The invention encompasses the membrane itself, methods of making it and processes for using it. The membrane comprises a polymer having repeating units of a hydrocarbon-based, disubstituted polyacetylene, having the general formula: ##STR1## wherein R.sub.1 is chosen from the group consisting of C.sub.1 -C.sub.4 alkyl and phenyl, and wherein R.sub.2 is chosen from the group consisting of hydrogen and phenyl. In the most preferred embodiment, the membrane comprises poly(4-methyl-2-pentyne) ›PMP!. The membrane exhibits good chemical resistance and has super-glassy properties with regard to separating certain large, condensable permeant species from smaller, less-condensable permeant species. The membranes may also be useful in other fluid separations.

  17. Isothermal separation processes

    NASA Technical Reports Server (NTRS)

    England, C.

    1982-01-01

    The isothermal processes of membrane separation, supercritical extraction and chromatography were examined using availability analysis. The general approach was to derive equations that identified where energy is consumed in these processes and how they compare with conventional separation methods. These separation methods are characterized by pure work inputs, chiefly in the form of a pressure drop which supplies the required energy. Equations were derived for the energy requirement in terms of regular solution theory. This approach is believed to accurately predict the work of separation in terms of the heat of solution and the entropy of mixing. It can form the basis of a convenient calculation method for optimizing membrane and solvent properties for particular applications. Calculations were made on the energy requirements for a membrane process separating air into its components.

  18. Nanoscale pillar arrays for separations

    DOE PAGES

    Kirchner, Teresa; Strickhouser, Rachel; Hatab, Nahla; ...

    2015-04-01

    The work presented herein evaluates silicon nano-pillar arrays for use in planar chromatography. Electron beam lithography and metal thermal dewetting protocols were used to create nano-thin layer chromatography platforms. With these fabrication methods we are able to reduce the size of the characteristic features in a separation medium below that used in ultra-thin layer chromatography; i.e. pillar heights are 1-2μm and pillar diameters are typically in the 200- 400nm range. In addition to the intrinsic nanoscale aspects of the systems, it is shown they can be further functionalized with nanoporous layers and traditional stationary phases for chromatography; hence exhibit broad-rangingmore » lab-on-a-chip and point-of-care potential. Because of an inherent high permeability and very small effective mass transfer distance between pillars, chromatographic efficiency can be very high but is enhanced herein by stacking during development and focusing while drying, yielding plate heights in the nm range separated band volumes. Practical separations of fluorescent dyes, fluorescently derivatized amines, and anti-tumor drugs are illustrated.« less

  19. Nanoscale pillar arrays for separations

    SciTech Connect

    Kirchner, Teresa; Strickhouser, Rachel; Hatab, Nahla; Charlton, Jennifer; Kravchenko, Ivan I.; Lavrik, Nickolay V.; Sepaniak, Michael J.

    2015-04-01

    The work presented herein evaluates silicon nano-pillar arrays for use in planar chromatography. Electron beam lithography and metal thermal dewetting protocols were used to create nano-thin layer chromatography platforms. With these fabrication methods we are able to reduce the size of the characteristic features in a separation medium below that used in ultra-thin layer chromatography; i.e. pillar heights are 1-2μm and pillar diameters are typically in the 200- 400nm range. In addition to the intrinsic nanoscale aspects of the systems, it is shown they can be further functionalized with nanoporous layers and traditional stationary phases for chromatography; hence exhibit broad-ranging lab-on-a-chip and point-of-care potential. Because of an inherent high permeability and very small effective mass transfer distance between pillars, chromatographic efficiency can be very high but is enhanced herein by stacking during development and focusing while drying, yielding plate heights in the nm range separated band volumes. Practical separations of fluorescent dyes, fluorescently derivatized amines, and anti-tumor drugs are illustrated.

  20. LISA Propulsion Module Separation Study

    NASA Technical Reports Server (NTRS)

    Merkowitz, Stephen

    2004-01-01

    The Laser Interferometer Space Antenna (LISA) mission is a space-borne gravitational wave detector consisting of three spacecraft in heliocentric orbit. Each spacecraft is delivered to it 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 baselined for the sciencecraft are micronewton level thrusters, such as FEEP or colloid thrusters, that are used to balance the 30-40 microN of solar radiation pressure and provide the drag-free and attitude control of the spacecraft. 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 design study of the propulsion module separation system that is shown to safely deliver the LISA sciencecraft to its final operational orbit.

  1. Nanoscale pillar arrays for separations.

    PubMed

    Kirchner, Teresa B; Strickhouser, Rachel B; Hatab, Nahla A; Charlton, Jennifer J; Kravchenko, Ivan I; Lavrik, Nickolay V; Sepaniak, Michael J

    2015-05-21

    The work presented herein evaluates silicon nano-pillar arrays for use in planar chromatography. Electron beam lithography and metal thermal dewetting protocols were used to create nano-thin layer chromatography platforms. With these fabrication methods we are able to reduce the size of the characteristic features in a separation medium below that used in ultra-thin layer chromatography; i.e. pillar heights are 1-2 μm and pillar diameters are typically in the 200-400 nm range. In addition to the intrinsic nanoscale aspects of the systems, it is shown they can be further functionalized with nanoporous layers and traditional stationary phases for chromatography; hence exhibit broad-ranging lab-on-a-chip and point-of-care potential. Because of an inherent high permeability and very small effective mass transfer distance between pillars, chromatographic efficiency can be very high but is enhanced herein by stacking during development and focusing while drying, yielding plate heights in the nm range separated band volumes. Practical separations of fluorescent dyes, fluorescently derivatized amines, and anti-tumor drugs are illustrated.

  2. Echocardiographic and phonocardiographic assessment of the St. Jude cardiac valve prosthesis.

    PubMed

    DePace, N L; Kotler, M N; Mintz, G S; Lichtenberg, R; Goel, I P; Segal, B L

    1981-09-01

    Forty-three consecutive patients with a St. Jude mitral, aortic, or combined prosthesis were studied by simultaneous phonocardiography and echocardiography. Twenty-eight patients had a mitral prosthesis, 20 an aortic prosthesis, and five had both. No opening click was recorded in any patient; however, a loud aortic or mitral closing click was recorded in all 43 patients. In patients with St. Jude mitral valve prosthesis, an echo-free space separated the two leaflets during diastole; seven of these also had a mid-diastolic closing and late diastolic reopening motion; two of the seven had an associated closing mid-diastolic click. A mid-diastolic rumble was recorded in six of 28 patients with St. Jude mitral valve prosthesis. In patients with a St. Jude aortic valve prosthesis, left atrium leaflet motion was recorded in 17 of 20 patients and was indistinguishable in appearance from echocardiograms obtained with various eccentric monocusp valves. In addition, we report one case of malfunction of a St. Jude mitral valve and one case of a paravalvular leak diagnosed by echophonocardiography. We concluded that the St. Jude cardiac prosthesis has variable normal phonocardiographic-echocardiographic patterns. Knowledge of these variable patterns is important in assessing patients with suspected malfunction of a St. Jude cardiac prosthesis.

  3. 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.

    PubMed

    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™.

  4. A systematic review of the separate and combined effects of energy restriction and exercise on fat-free mass in middle-aged and older adults: implications for sarcopenic obesity.

    PubMed

    Weinheimer, Eileen M; Sands, Laura P; Campbell, Wayne W

    2010-07-01

    The systematic review presented here assessed the effects of energy restriction (ER) and exercise (EX) on fat-free mass (FFM) in overweight and obese middle-aged and older adults. PubMed was searched using the key words "weight loss or energy restriction" AND "skeletal muscle or body composition," with limitations set for "human" and "middle-aged and aged." Results from 52 studies are reported as the percentages of EX (mainly aerobic training), ER, or ER+EX groups that had a specified change in body weight and FFM, since insufficient data were available for a meta-analysis. The EX groups had modest body weight and FFM changes. Eighty-one percent and 39% of the ER and ER+EX groups, respectively, lost > or = 15% of body weight as FFM. These findings suggest that exercise is an effective tool to help men and postmenopausal women aged > or = 50 years, with a BMI greater than 25 kg/m(2) preserve FFM after moderate ER-induced weight loss, which is important for combating sarcopenic obesity.

  5. 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.

    PubMed

    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 <1 g, 0.01 g for this study) and solvent (<20 mL) than the conventional system. To sum up, the proposed method could be recommended as a new approach in the extraction and analysis of essential oil.

  6. Investigation of the separation of heterocyclic aromatic amines by reversed phase ion-pair liquid chromatography coupled with tandem mass spectrometry: the role of ion pair reagents on LC-MS/MS sensitivity.

    PubMed

    Bianchi, F; Careri, M; Corradini, C; Elviri, L; Mangia, A; Zagnoni, I

    2005-10-25

    Reversed phase ion-pair chromatography (RP-IPC) of seven heterocyclic aromatic amines encompassing quinoline (IQ, MeIQ), quinoxaline (MeIQx), pyridine (PhIP) and carboline derivatives (AalphaC, Harman, Norharman) was carried out with formate as counter ion in an aqueous eluent with acetonitrile as organic modifier. TSKgel ODS-80TS was used as the stationary phase. With the aim of acquiring a better insight into the mutual influence of ion-pair reagent and the organic modifier upon solute retention, the study was performed by using an experimental design approach able to evidencing the effect of the simultaneous variation of the two factors. A model for the chromatographic behavior of the amines is proposed that includes classical ion-pair mechanism involving formate in the case of MeIQx, PhIP, Harman and Norharman. A competitive ion-exchange mechanism was hypothesized to govern retention of quinoline compounds, whereas electrostatic interactions and hydrogen bond formation with the silanols of the stationary phase were judged to be responsible for the retention of AalphaC. Further, the chromatographic behavior of the analytes using the formic acid-ammonium formate buffer in the mobile phase was compared with that observed using acetic acid-ammonium acetate buffer. The method based on the use of RP IPC with tandem mass spectrometry when the eluent contained formate buffer at pH 2.8 exhibited higher detectability with respect to that achieved using the acetate buffer.

  7. Process for phase separation

    DOEpatents

    Comolli, Alfred G.

    1979-01-01

    This invention provides a continuous process for separating a gaseous phase from a hydrocarbon liquid containing carbonaceous particulates and gases. The liquid is fed to a cylindrical separator, with the gaseous phase being removed therefrom as an overhead product, whereas the hydrocarbon liquid and the particulates are withdrawn as a bottoms product. By feeding the liquid tangentially to the separator and maintaining a particulate-liquid slurry downward velocity of from about 0.01 to about 0.25 fps in the separator, a total solids weight percent in the slurry of from about 0.1 to about 30%, a slurry temperature of from about 550.degree. to about 900.degree. F., a slurry residence time in the separator of from about 30 to about 360 seconds, and a length/diameter ratio for the separator of from about 20/1 to about 50/1, so that the characterization factor, .alpha., defined as ##STR1## DOES NOT EXCEED ABOUT 48 (.degree.R sec.sup.2)/ft, the deposit of carbonaceous materials on the interior surface of the separator may be substantially eliminated.

  8. NASA's New Millennium ST-8 Mission

    NASA Astrophysics Data System (ADS)

    Bothwell, M.; Stevens, C. M.; Chmielewski, A. B.; Fujita, T.; Minning, C.; Nelson, R. M.; Ku, J.; McEachen, M. E.; Sampson, J. R.

    2005-12-01

    NASA's Space Technology 8 project (ST-8) is subsystem demonstration which will validate four technologies that have been identified as necessary to enable future NASA space science missions. NASA's New Millennium Program, with input from the science community, identified the following four technologies: Miniature Loop Heat Pipe with Multiple Evaporators Thermal Management System (MLHP), Scalable Architecture for the Investigation of the Load Managing Attributes of a Slender Truss (SAILMAST), Next Generation UltraFlex (NGU), and Environmentally Adaptive Fault Tolerant Computing (EAFTC). Once validated on a deep space mission, these technologies will be available for use on future science missions. Examples of previous enabling technologies demonstrated by NMP are the ion engines on Deep Space 1 and the Autonomous Sciencecraft Experiment demonstrated by ST6. The MLHP, provided by NASA's Goddard Space Flight Center will demonstrate that a loop heat pipe with multiple evaporators and condensers can transport large heat loads over long distances without external pumping. It is expected that this technology will enable more precise temperature control decreasing the mass, power, and volume of small remote sensing and surface-based spacecraft. The SAILMAST experiment is a deployable gossamer mast technology, which will validate its load-carrying characteristics by correlating in-flight measurements with analytical predictions. It will enable a new class of missions, which employ solar sail propulsion technology. The NGU will demonstrate the next generation in ultra-lightweight fan-folded flexible solar arrays, providing ultra-high specific power (170-220 W/kg BOL), ultra-compact stowage volume (>33 W/m3), and high deployed stiffness. The result is less mass and volume needed for power generation on future spacecraft. The EAFTC will integrate commercial-off-the-shelf (COTS) processing components and fault-tolerant control algorithms to provide an adaptable, high

  9. Approach to forecasting daily maximum ozone levels in St. Louis

    NASA Technical Reports Server (NTRS)

    Prior, E. J.; Schiess, J. R.; Mcdougal, D. S.

    1981-01-01

    Measurements taken in 1976 from the St. Louis Regional Air Pollution Study (RAPS) data base, conducted by EPA, were analyzed to determine an optimum set of air-quality and meteorological variables for predicting maximum ozone levels for each day in 1976. A 'leaps and bounds' regression analysis was used to identify the best subset of variables. Three particular variables, the 9 a.m. ozone level, the forecasted maximum temperature, and the 6-9 a.m. averaged wind speed, have useful forecasting utility. The trajectory history of air masses entering St. Louis was studied, and it was concluded that transport-related variables contribute to the appearance of very high ozone levels. The final empirical forecast model predicts the daily maximum ozone over 341 days with a standard deviation of 11 ppb, which approaches the estimated error.

  10. Effects of volcanism on the glaciers of Mount St. Helens

    USGS Publications Warehouse

    Brugman, Melinda M.; Post, Austin

    1981-01-01

    The cataclysmic eruption of Mount St. Helens May 18, 1980, removed 2.9 km2 (about 0.13 km3) of glacier snow and ice including a large part of Shoestring, Forsyth, Wishbone, Ape, Nelson, and all of Loowit and Leschi Glaciers. Minor eruptions and bulging of the volcano from March 27 to May 17 shattered glaciers which were on the deforming rock and deposited ash on other glaciers. Thick ash layers persisted after the May 18 eruption through the summer on most of the remaining snow and ice, and protected winter snow from melting on Swift and Dryer Glaciers. Melting and recrystalization of snow and ice surviving on Mount St. Helens could cause and lubricate mudflows and generate outburst floods. Study of glaciers that remain on this active volcano may assist in recognizing potential hazards on other volcanoes and lead to new contributions to knowledge of the transient response of glaciers to changes in mass balance or geometry.

  11. Chromatographic hydrogen isotope separation

    DOEpatents

    Aldridge, Frederick T.

    1981-01-01

    Intermetallic compounds with the CaCu.sub.5 type of crystal structure, particularly LaNiCo.sub.4 and CaNi.sub.5, exhibit high separation factors and fast equilibrium times and therefore are useful for packing a chromatographic hydrogen isotope separation colum. The addition of an inert metal to dilute the hydride improves performance of the column. A large scale mutli-stage chromatographic separation process run as a secondary process off a hydrogen feedstream from an industrial plant which uses large volumes of hydrogen can produce large quantities of heavy water at an effective cost for use in heavy water reactors.

  12. Chromatographic hydrogen isotope separation

    DOEpatents

    Aldridge, F.T.

    Intermetallic compounds with the CaCu/sub 5/ type of crystal structure, particularly LaNiCo/sub 4/ and CaNi/sub 5/, exhibit high separation factors and fast equilibrium times and therefore are useful for packing a chromatographic hydrogen isotope separation column. The addition of an inert metal to dilute the hydride improves performance of the column. A large scale multi-stage chromatographic separation process run as a secondary process off a hydrogen feedstream from an industrial plant which uses large volumes of hydrogen cn produce large quantities of heavy water at an effective cost for use in heavy water reactors.

  13. Asymmetric gas separation membranes

    SciTech Connect

    Malon, R. F.; Zampini, A.

    1984-12-04

    Asymmetric gas separation membranes of materials having selective permeation of at least one gas of a gaseous mixture over that of one or more remaining gases of the gaseous mixture, exhibit significantly improved permeation selectivities for the at least one gas when the asymmetric membrane is contacted on one or both surfaces with an effective amount of a Lewis acid. The improved asymmetric gas separation membranes, process for producing the improved membrane, and processes utilizing such membranes for selectively separating at least one gas from a gaseous mixture by permeation are disclosed.

  14. Asymmetric gas separation membranes

    SciTech Connect

    Malon, R. F.; Zampini, A.

    1984-09-18

    Asymmetric gas separation membranes of materials having selective permeation of at least one gas of a gaseous mixture over that of one or more remaining gases of the gaseous mixture, exhibit significantly improved permeation selectivities for the at least one gas when the asymmetric membrane is contacted on one or both surfaces with an effective amount of a Br nsted-Lowry acid. The improved asymmetric gas separation membranes, process for producing the improved membrane, and processes utilizing such membranes for selectively separating at least one gas from a gaseous mixture by permeation are disclosed.

  15. Enhance separations with electricity

    SciTech Connect

    Muralidhara, H.S.

    1994-05-01

    To satisfy growing environmental regulations, control energy costs, or just to stay competitive, one must improve existing separation technologies and make them more efficient. New challenges in food processing and requirements for novel purification technologies in the biotech industry also will require more efficient separation techniques. This paper discusses some enhanced separation processes based on the application of an electric field in the combined-fields approach. In a combined-fields approach, the emphasis is on the generation of additional driving forces to work simultaneously with the conventional driving force of the process. Here the authors concentrate on the application of an electric field to generate the additional driving force.

  16. 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.

    PubMed

    de Jong, Jeroen; Schoemann, Véronique; Lannuzel, Delphine; Tison, Jean-Louis; Mattielli, Nadine

    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(-1) level, by isotope dilution multiple collector inductively coupled plasma mass spectrometry (ID-MC-ICP-MS) using a (54)Fe spike and measuring the (57)Fe/(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(-1), n=21, 3 x S.D. limit of detection per session 0.020-0.069 nmol L(-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(2)O(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(-1)) and Deep-2 (0.91+/-0.17 nmol L(-1)) and obtained results that were in excellent agreement with their DFe consensus values: 0.118+/-0.028 nmol L(-1) (n=7) for Surface-1 and 0.932+/-0.059 nmol L(-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 approximately 0.6 nmol L(-1) and bottom water enrichment up to 23 nmol L(-1) DFe.

  17. PREFACE: 1st European Conference on Gas Micro Flows (GasMems 2012)

    NASA Astrophysics Data System (ADS)

    Frijns, Arjan; Valougeorgis, Dimitris; Colin, Stéphane; Baldas, Lucien

    2012-05-01

    The aim of the 1st European Conference on Gas Micro Flows is to advance research in Europe and worldwide in the field of gas micro flows as well as to improve global fundamental knowledge and to enable technological applications. Gas flows in microsystems are of great importance and touch almost every industrial field (e.g. fluidic microactuators for active control of aerodynamic flows, vacuum generators for extracting biological samples, mass flow and temperature micro-sensors, pressure gauges, micro heat-exchangers for the cooling of electronic components or for chemical applications, and micro gas analyzers or separators). The main characteristic of gas microflows is their rarefaction, which for device design often requires modelling and simulation both by continuous and molecular approaches. In such flows various non-equilibrium transport phenomena appear, while the role played by the interaction between the gas and the solid device surfaces becomes essential. The proposed models of boundary conditions often need an empirical adjustment strongly dependent on the micro manufacturing technique. The 1st European Conference on Gas Micro Flows is organized under the umbrella of the recently established GASMEMS network (www.gasmems.eu/) consisting of 13 participants and six associate members. The main objectives of the network are to structure research and train researchers in the fields of micro gas dynamics, measurement techniques for gaseous flows in micro experimental setups, microstructure design and micro manufacturing with applications in lab and industry. The conference takes place on June 6-8 2012, at the Skiathos Palace Hotel, on the beautiful island of Skiathos, Greece. The conference has received funding from the European Community's Seventh Framework Programme FP7/2007-2013 under grant agreement ITN GASMEMS no. 215504. It owes its success to many people. We would like to acknowledge the support of all members of the Scientific Committee and of all

  18. Molten salt electrolyte separator

    DOEpatents

    Kaun, Thomas D.

    1996-01-01

    A molten salt electrolyte/separator for battery and related electrochemical systems including a molten electrolyte composition and an electrically insulating solid salt dispersed therein, to provide improved performance at higher current densities and alternate designs through ease of fabrication.

  19. Inorganic separator technology program

    NASA Technical Reports Server (NTRS)

    Smatko, J. S.; Weaver, R. D.; Kalhammer, F. R.

    1973-01-01

    Testing and failure analyses of silver zinc cells with largely inorganic separators were performed. The results showed that the wet stand and cycle life objective of the silver-zinc cell development program were essentially accomplished and led to recommendations for cell composition, design, and operation that should yield further improvement in wet and cycle life. A series of advanced inorganic materials was successfully developed and formulated into rigid and semiflexible separator samples. Suitable screening tests for evaluation of largely inorganic separators were selected and modified for application to the separator materials. The results showed that many of these formulations are potentially superior to previously used materials and permitted selection of three promising materials for further evaluation in silver-zinc cells.

  20. Laminar-Separation Sensor

    NASA Technical Reports Server (NTRS)

    Manuel, G. S.; Carraway, D. L.; Lee, C. C.

    1991-01-01

    Reduction of viscous drag on airplanes explores limits of practical applications of natural laminar flow. Wind-tunnel and flight tests conducted to explore abilities of hot-film sensors to identify separation of laminar flow as principal mode of amplification of instability leading to transition from laminar to turbulent flow. Two different laminar-separation-sensor configurations developed and used to detect boundary-layer transitions. Results show hot-film laminar-separation-sensor technique viable means for detecting existence of transition as well as for indicating reversed flow in laminar-separation bubble. Refinement of sensor configurations provides tools necessary to explore, in all speed regimes, practical limits of laminar-flow applications and viscous-drag-reduction technology.

  1. Separable Arrowhead Microneedles

    PubMed Central

    Chu, Leonard Y.; Prausnitz, Mark R.

    2010-01-01

    Hypodermic needles cause pain and bleeding, produce biohazardous sharp waste and require trained personnel. To address these issues, we introduce separable arrowhead microneedles that rapidly and painlessly deliver drugs and vaccines to the skin. These needles are featured by micron-size sharp tips mounted on blunt shafts. Upon insertion in the skin, the sharp-tipped polymer arrowheads encapsulating drug separate from their metal shafts and remain embedded in the skin for subsequent dissolution and drug release. The blunt metal shafts can then be discarded. Due to rapid separation of the arrowhead tips from the shafts within seconds, administration using arrowhead microneedles can be carried out rapidly, while drug release kinetics can be independently controlled based on separable arrowhead formulation. Thus, drug and vaccine delivery using arrowhead microneedles are designed to offer a quick, convenient, safe and potentially self-administered method of drug delivery as an alternative to hypodermic needles. PMID:21047538

  2. Booster separation motor

    NASA Technical Reports Server (NTRS)

    1981-01-01

    The design, development, fabrication, testing, evaluation and flight qualification of the space shuttle booster separation motor is discussed. Delivery of flight hardware to support the research and development flights of the space shuttle is discussed.

  3. Separation by solvent extraction

    DOEpatents

    Holt, Jr., Charles H.

    1976-04-06

    17. A process for separating fission product values from uranium and plutonium values contained in an aqueous solution, comprising adding an oxidizing agent to said solution to secure uranium and plutonium in their hexavalent state; contacting said aqueous solution with a substantially water-immiscible organic solvent while agitating and maintaining the temperature at from -1.degree. to -2.degree. C. until the major part of the water present is frozen; continuously separating a solid ice phase as it is formed; separating a remaining aqueous liquid phase containing fission product values and a solvent phase containing plutonium and uranium values from each other; melting at least the last obtained part of said ice phase and adding it to said separated liquid phase; and treating the resulting liquid with a new supply of solvent whereby it is practically depleted of uranium and plutonium.

  4. Microsystem capillary separations

    DOEpatents

    TeGrotenhuis, Ward E [Kennewick, WA; Wegeng, Robert S [Richland, WA; Whyatt, Greg A [West Richland, WA; Stenkamp, Victoria S [Richland, WA; Gauglitz, Phillip A [Richland, WA

    2003-12-23

    Laminated, multiphase separators and contactors having wicking structures and gas flow channels are described. Some preferred embodiments are combined with microchannel heat exchange. Integrated systems containing these components are also part of the present invention.

  5. Separator for alkaline batteries

    NASA Technical Reports Server (NTRS)

    Hoyt, H. W.; Pfluger, H. L.

    1968-01-01

    Separator compositions have been tested as components of three-plate silver-zinc oxide cells in a standard cycling test. Six materials meet imposed requirements, giving cycling performance superior to cellophane.

  6. Monitored separation device

    NASA Technical Reports Server (NTRS)

    Jackson, George William (Inventor); Willson, Richard Coale (Inventor); Fox, George Edward (Inventor)

    2011-01-01

    A device for separating and purifying useful quantities of particles comprises: a. an anolyte reservoir connected to an anode, the anolyte reservoir containing an electrophoresis buffer; b. a catholyte reservoir connected to a cathode, the catholyte reservoir also containing the electrophoresis buffer; c. a power supply connected to the anode and to the cathode; d. a column having a first end inserted into the anolyte reservoir, a second end inserted into the catholyte reservoir, and containing a separation medium; e. a light source; f. a first optical fiber having a first fiber end inserted into the separation medium, and having a second fiber end connected to the light source; g. a photo detector; h. a second optical fiber having a third fiber end inserted into the separation medium, and having a fourth fiber end connected to the photo detector; and i. an ion-exchange membrane in the anolyte reservoir.

  7. Separation of Craniopagus Twins.

    PubMed

    Johnson, Reuben; Weir, Philip

    2016-01-01

    Separation of craniopagus twins is fraught by ethical issues. The surgery is high risk and may involve the sacrifice of one twin. We review surgical successes in separation of craniopagus twins and consider ethical and legal concepts affecting the decision to undertake such procedures. Our discussion considers how Gillett's potentiality principle and the concept of moral permissibility may be used to arrive at fair and realistic decisions.

  8. Hydrogen separation process

    DOEpatents

    Mundschau, Michael; Xie, Xiaobing; Evenson, IV, Carl; Grimmer, Paul; Wright, Harold

    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.

  9. SEPARATIONS BY ELECTRODIALYSIS

    DOEpatents

    Webb, W.H.; Vie, J.D.

    1962-06-12

    A method is given for separating cesium, cerium, zirconium, and uranyl ions frora a common solution by electrodialysis. An anion exchange membrane and a cation exchange membrane are placed on either side of the feed solution compartment; the former is in electrolytic contact with an anode and the latter with cathode. On acidification of the feed solution to a critical value of 0.5 N and passage of a current from the anode to the cathode, the desired separations tske place. (AEC)

  10. ST Segment Elevation with Normal Coronaries

    PubMed Central

    Sethi, Pooja; Sharma, Ashwini; Paul, Timir

    2016-01-01

    Noncardiac causes should be kept in the differential while evaluating ST elevation on EKG. Rarely abdominal pathologies like acute pancreatitis can present with ST elevation in the inferior leads. Once acute coronary syndrome is ruled out by emergent cardiac catheterization alternative diagnosis should be sorted. Abdominal pathologies, like acute pancreatitis and acute cholecystitis, can present with ST elevation in the inferior leads. Treating the underlying condition would result in resolution of these EKG changes. PMID:27403165

  11. St. Louis Area Earthquake Hazards Mapping Project

    USGS Publications Warehouse

    Williams, Robert A.; Steckel, Phyllis; Schweig, Eugene

    2007-01-01

    St. Louis has experienced minor earthquake damage at least 12 times in the past 200 years. Because of this history and its proximity to known active earthquake zones, the St. Louis Area Earthquake Hazards Mapping Project will produce digital maps that show variability of earthquake hazards in the St. Louis area. The maps will be available free via the internet. They can be customized by the user to show specific areas of interest, such as neighborhoods or transportation routes.

  12. Experimental Evaluation of StRATUS (Preprint)

    DTIC Science & Technology

    2014-04-01

    AFRL-RQ-WP-TP-2014-0142 EXPERIMENTAL EVALUATION OF StRATUS (PREPRINT) Michael A. Falugi Structures Technology Branch Aerospace...Conference Paper Preprint 01 May 2012 – 28 February 2014 4. TITLE AND SUBTITLE EXPERIMENTAL EVALUATION OF StRATUS (PREPRINT) 5a. CONTRACT NUMBER...Steel Reinforced Advanced Thin Unitized Structure ( StRATUS ) is a new hybrid laminate concept composed of carbon fiber composite sandwiched between thin

  13. St. John's wort - an overview.

    PubMed

    Linde, Klaus

    2009-06-01

    This article aims to summarize the current state of knowledge on St. John's wort (Hypericum perforatum L.) which is one of the oldest and best investigated medicinal herbs. Dried alcoholic extracts are the most important preparations on the market although a variety of other preparations are available. Depressive disorders according to modern diagnostic standards are the best known and most widely investigated indication although the more traditional, broader indication of 'psycho-vegetative disorders, depressive disorders, anxiety and/or nervous agitation', including diagnoses such as somatoform disorders, might more adequately describe what Hypericum extracts are actually used for by many practitioners. The exact mechanisms of action are still unclear, but the available research clearly shows that various bioactive constituents contribute to the clinical effects reported, often in a synergistic manner. Hypericum extracts have consistently shown activity in pharmacological models related to antidepressant effects. Randomized clinical trials show that Hypericum extracts are more effective than placebo and similarly effective as standard antidepressants while having better tolerability in the acute treatment of major depressive episodes. The most important risk associated with Hypericum extracts are interactions with other drugs. Therefore, physicians need to be informed whether their patients take St. John's wort products. If the risk of interactions is adequately taken into account, high quality Hypericum extracts are an effective and safe tool in the hand of qualified health profession-als in primary care.

  14. ACTH Action on StAR Biology.

    PubMed

    Clark, Barbara J

    2016-01-01

    Adrenocorticotropin hormone (ACTH) produced by the anterior pituitary stimulates glucocorticoid synthesis by the adrenal cortex. The first step in glucocorticoid synthesis is the delivery of cholesterol to the mitochondrial matrix where the first enzymatic reaction in the steroid hormone biosynthetic pathway occurs. A key response of adrenal cells to ACTH is activation of the cAMP-protein kinase A (PKA) signaling pathway. PKA activation results in an acute increase in expression and function of the Steroidogenic Acute Regulatory protein (StAR). StAR plays an essential role in steroidogenesis- it controls the hormone-dependent movement of cholesterol across the mitochondrial membranes. Currently StAR's mechanism of action remains a major unanswered question in the field. However, some insight may be gained from understanding the mechanism(s) controlling the PKA-dependent phosphorylation of StAR at S194/195 (mouse/human StAR), a modification that is required for function. This mini-review provides a background on StAR's biology with a focus on StAR phosphorylation. The model for StAR translation and phosphorylation at the outer mitochondrial membrane, the location for StAR function, is presented to highlight a unifying theme emerging from diverse studies.

  15. ACTH Action on StAR Biology

    PubMed Central

    Clark, Barbara J.

    2016-01-01

    Adrenocorticotropin hormone (ACTH) produced by the anterior pituitary stimulates glucocorticoid synthesis by the adrenal cortex. The first step in glucocorticoid synthesis is the delivery of cholesterol to the mitochondrial matrix where the first enzymatic reaction in the steroid hormone biosynthetic pathway occurs. A key response of adrenal cells to ACTH is activation of the cAMP-protein kinase A (PKA) signaling pathway. PKA activation results in an acute increase in expression and function of the Steroidogenic Acute Regulatory protein (StAR). StAR plays an essential role in steroidogenesis- it controls the hormone-dependent movement of cholesterol across the mitochondrial membranes. Currently StAR's mechanism of action remains a major unanswered question in the field. However, some insight may be gained from understanding the mechanism(s) controlling the PKA-dependent phosphorylation of StAR at S194/195 (mouse/human StAR), a modification that is required for function. This mini-review provides a background on StAR's biology with a focus on StAR phosphorylation. The model for StAR translation and phosphorylation at the outer mitochondrial membrane, the location for StAR function, is presented to highlight a unifying theme emerging from diverse studies. PMID:27999527

  16. VIEW SOUTH ON CLARK ST.BUILDING 101 CLARK ST. ROPE SHOP ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    VIEW SOUTH ON CLARK ST.-BUILDING 101 CLARK ST. ROPE SHOP (1917) - John A. Roebling's Sons Company & American Steel & Wire Company, South Broad, Clark, Elmer, Mott & Hudson Streets, Trenton, Mercer County, NJ

  17. The Archimedes Plasma Mass Filter

    NASA Astrophysics Data System (ADS)

    Miller, R. L.; Ohkawa, T.; Agnew, S. F.; Cluggish, B. P.; Freeman, R. L.; Gilleland, J.; Putvinski, S.; Sevier, L.; Umstadter, K. R.

    2001-10-01

    Archimedes Technology Group is developing a plasma technology, called the Archimedes Plasma Mass Filter, which can separate a waste mixture ion by ion into mass groups and as such represents a major advance in waste separations technology. The filter is a plasma device employing a magnetic and electric field configuration that acts as a low-mass-pass filter for ions. Ions with mass above a tunable “cutoff mass” are expelled from the plasma. The Archimedes Plasma Mass Filter satisfies all of the requirements of an economic mass separator system: good single-pass separation, acceptable energy cost per ion, and high material throughput. This technology could significantly reduce the volume of radioactive waste at the Hanford Site in Richland, Washington, which is storing sixty percent of the nation’s defense nuclear waste. The potential waste reduction is dramatic because 82 wtpresently scheduled to be vitrified (immobilized and stored in glass) at Hanford are below mass number 60 while 99.9the radioactivity comes from atoms above mass number 89. We will present the plasma physics basis for the filter effect, the fundamental parameter constraints, and modeling results of filter operation.

  18. Gulf stream separation dynamics

    NASA Astrophysics Data System (ADS)

    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.

  19. Carter separable electromagnetic fields

    NASA Astrophysics Data System (ADS)

    Lynden-Bell, D.

    2000-02-01

    The purely electromagnetic analogue in flat space of Kerr's metric in general relativity is only rarely considered. Here we carry out in flat space a programme similar to Carter's investigation of metrics in general relativity in which the motion of a charged particle is separable. We concentrate on the separability of the motion (be it classical, relativistic or quantum) of a charged particle in electromagnetic fields that lie in planes through an axis of symmetry. In cylindrical polar coordinates (t,R,φ,z) the four-vector potential takes the form [formmu2] is the unit toroidal vector. The forms of the functions Φ(R,z) and A(R,z) are sought that allow separable motion. This occurs for relativistic motion only when AR,Φ and A2-Φ2 are all of the separable form ζ(λ)-η(μ)]/(λ-μ), where ζ and η are arbitrary functions, and λ and μ are spheroidal coordinates or degenerations thereof. The special forms of A and Φ that allow this are deduced. They include the Kerr metric analogue, with E+iB=-∇{q[(r-ia).(r-ia)]-1/2}. Rather more general electromagnetic fields allow separation when the motion is non-relativistic. The investigation is extended to fields that lie in parallel planes. Connections to Larmor's theorem are remarked upon.

  20. Organic Separation Test Results

    SciTech Connect

    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.