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Sample records for periodic gas sampling

  1. Wet gas sampling

    Energy Technology Data Exchange (ETDEWEB)

    Welker, T.F.

    1997-07-01

    The quality of gas has changed drastically in the past few years. Most gas is wet with hydrocarbons, water, and heavier contaminants that tend to condense if not handled properly. If a gas stream is contaminated with condensables, the sampling of that stream must be done in a manner that will ensure all of the components in the stream are introduced into the sample container as the composite. The sampling and handling of wet gas is extremely difficult under ideal conditions. There are no ideal conditions in the real world. The problems related to offshore operations and other wet gas systems, as well as the transportation of the sample, are additional problems that must be overcome if the analysis is to mean anything to the producer and gatherer. The sampling of wet gas systems is decidedly more difficult than sampling conventional dry gas systems. Wet gas systems were generally going to result in the measurement of one heating value at the inlet of the pipe and a drastic reduction in the heating value of the gas at the outlet end of the system. This is caused by the fallout or accumulation of the heavier products that, at the inlet, may be in the vapor state in the pipeline; hence, the high gravity and high BTU. But, in fact, because of pressure and temperature variances, these liquids condense and form a liquid that is actually running down the pipe as a stream or is accumulated in drips to be blown from the system. (author)

  2. Soil Gas Sampling

    Science.gov (United States)

    Field Branches Quality System and Technical Procedures: This document describes general and specific procedures, methods and considerations to be used and observed when collecting soil gas samples for field screening or laboratory analysis.

  3. IXM gas sampling procedure

    International Nuclear Information System (INIS)

    Pingel, L.A.

    1995-01-01

    Ion Exchange Modules (IXMs) are used at the 105-KE and -KW Fuel Storage Basins to control radionuclide concentrations in the water. A potential safety concern relates to production of hydrogen gas by radiolysis of the water trapped in the ion exchange media of spent IXMs. This document provides a procedure for sampling the gases in the head space of the IXM

  4. Soil Gas Sampling Operating Procedure

    Science.gov (United States)

    EPA Region 4 Science and Ecosystem Support Division (SESD) document that describes general and specific procedures, methods, and considerations when collecting soil gas samples for field screening or laboratory analysis.

  5. Subsurface Noble Gas Sampling Manual

    Energy Technology Data Exchange (ETDEWEB)

    Carrigan, C. R. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Sun, Y. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

    2017-09-18

    The intent of this document is to provide information about best available approaches for performing subsurface soil gas sampling during an On Site Inspection or OSI. This information is based on field sampling experiments, computer simulations and data from the NA-22 Noble Gas Signature Experiment Test Bed at the Nevada Nuclear Security Site (NNSS). The approaches should optimize the gas concentration from the subsurface cavity or chimney regime while simultaneously minimizing the potential for atmospheric radioxenon and near-surface Argon-37 contamination. Where possible, we quantitatively assess differences in sampling practices for the same sets of environmental conditions. We recognize that all sampling scenarios cannot be addressed. However, if this document helps to inform the intuition of the reader about addressing the challenges resulting from the inevitable deviations from the scenario assumed here, it will have achieved its goal.

  6. Retained Gas Sampling Results for the Flammable Gas Program

    International Nuclear Information System (INIS)

    Bates, J.M.; Mahoney, L.A.; Dahl, M.E.; Antoniak, Z.I.

    1999-01-01

    The key phenomena of the Flammable Gas Safety Issue are generation of the gas mixture, the modes of gas retention, and the mechanisms causing release of the gas. An understanding of the mechanisms of these processes is required for final resolution of the safety issue. Central to understanding is gathering information from such sources as historical records, tank sampling data, tank process data (temperatures, ventilation rates, etc.), and laboratory evaluations conducted on tank waste samples

  7. Retained Gas Sampling Results for the Flammable Gas Program

    Energy Technology Data Exchange (ETDEWEB)

    J.M. Bates; L.A. Mahoney; M.E. Dahl; Z.I. Antoniak

    1999-11-18

    The key phenomena of the Flammable Gas Safety Issue are generation of the gas mixture, the modes of gas retention, and the mechanisms causing release of the gas. An understanding of the mechanisms of these processes is required for final resolution of the safety issue. Central to understanding is gathering information from such sources as historical records, tank sampling data, tank process data (temperatures, ventilation rates, etc.), and laboratory evaluations conducted on tank waste samples.

  8. Gabor frames by sampling and periodization

    DEFF Research Database (Denmark)

    Søndergaard, Peter Lempel

    2007-01-01

    By sampling the window of Gabor frame for L-2 (R) belonging to Feichtingers algebra S-0 (R), one obtains a Gabor frame for l(2) (Z). In this article we present a survey of results by R. Orr and A.J.E.M. Janssen and extend their ideas to cover interrelations among Gabor frames for the four spaces L......-2 (R), l(2) (Z), L-2 ([O,L]) and C-L. Some new results about the general dual windows with respect to sampling and periodization are presented as well. This theory is used to show a new result of the Kaiblinger type to construct an approximation to the canonical dual window of a Gabor frame for L-2...

  9. Canonical sampling of a lattice gas

    International Nuclear Information System (INIS)

    Mueller, W.F.

    1997-01-01

    It is shown that a sampling algorithm, recently proposed in conjunction with a lattice-gas model of nuclear fragmentation, samples the canonical ensemble only in an approximate fashion. A residual weight factor has to be taken into account to calculate correct thermodynamic averages. Then, however, the algorithm is numerically inefficient. copyright 1997 The American Physical Society

  10. Tracer gas diffusion sampling test plan

    International Nuclear Information System (INIS)

    Rohay, V.J.

    1993-01-01

    Efforts are under way to employ active and passive vapor extraction to remove carbon tetrachloride from the soil in the 200 West Area an the Hanford Site as part of the 200 West Area Carbon Tetrachloride Expedited Response Action. In the active approach, a vacuum is applied to a well, which causes soil gas surrounding the well to be drawn up to the surface. The contaminated air is cleaned by passage through a granular activated carbon bed. There are questions concerning the radius of influence associated with application of the vacuum system and related uncertainties about the soil-gas diffusion rates with and without the vacuum system present. To address these questions, a series of tracer gas diffusion sampling tests is proposed in which an inert, nontoxic tracer gas, sulfur hexafluoride (SF 6 ), will be injected into a well, and the rates of SF 6 diffusion through the surrounding soil horizon will be measured by sampling in nearby wells. Tracer gas tests will be conducted at sites very near the active vacuum extraction system and also at sites beyond the radius of influence of the active vacuum system. In the passive vapor extraction approach, barometric pressure fluctuations cause soil gas to be drawn to the surface through the well. At the passive sites, the effects of barometric ''pumping'' due to changes in atmospheric pressure will be investigated. Application of tracer gas testing to both the active and passive vapor extraction methods is described in the wellfield enhancement work plan (Rohay and Cameron 1993)

  11. Hydrogen gas sample environment for TOSCA

    International Nuclear Information System (INIS)

    Kibble, Mark G; Ramirez-Cuesta, Anibal J; Goodway, Chris M; Evans, Beth E; Kirichek, Oleg

    2014-01-01

    The idea of using hydrogen as a fuel has gained immense popularity over many years. Hydrogen is abundant, can be produced from renewable resources and is not a greenhouse gas. However development of hydrogen based technology is impossible without understanding of physical and chemical processes that involve hydrogen sometime in extreme conditions such as high pressure or low and high temperatures. Neutron spectroscopy allows measurement of a hydrogen atom motion in variety of samples. Here we describe and discuss a sample environment kit developed for hydrogen gas experiment in a broad range of pressure up to 7 kbar and temperatures from 4 K to 473 K. We also describe para-hydrogen rig which produces para-hydrogen gas required for studying the rotational line of molecular hydrogen

  12. Gas phase acid, ammonia and aerosol ionic and trace element concentrations at Cape Verde during the Reactive Halogens in the Marine Boundary Layer (RHaMBLe) 2007 intensive sampling period

    Science.gov (United States)

    Sander, R.; Pszenny, A. A. P.; Keene, W. C.; Crete, E.; Deegan, B.; Long, M. S.; Maben, J. R.; Young, A. H.

    2013-12-01

    We report mixing ratios of soluble reactive trace gases sampled with mist chambers and the chemical composition of bulk aerosol and volatile inorganic bromine (Brg) sampled with filter packs during the Reactive Halogens in the Marine Boundary Layer (RHaMBLe) field campaign at the Cape Verde Atmospheric Observatory (CVAO) on São Vicente island in the tropical North Atlantic in May and June 2007. The gas-phase data include HCl, HNO3, HONO, HCOOH, CH3COOH, NH3, and volatile reactive chlorine other than HCl (Cl*). Aerosol samples were analyzed by neutron activation (Na, Al, Cl, V, Mn, and Br) and ion chromatography (SO42-, Cl-, Br-, NH4+, Na+, K+, Mg2+, and Ca2+). Content and quality of the data, which are available under doi:10.5281/zenodo.6956, are presented and discussed.

  13. Gas phase acid, ammonia and aerosol ionic and trace element concentrations at Cape Verde during the Reactive Halogens in the Marine Boundary Layer (RHaMBLe 2007 intensive sampling period

    Directory of Open Access Journals (Sweden)

    R. Sander

    2013-12-01

    Full Text Available We report mixing ratios of soluble reactive trace gases sampled with mist chambers and the chemical composition of bulk aerosol and volatile inorganic bromine (Brg sampled with filter packs during the Reactive Halogens in the Marine Boundary Layer (RHaMBLe field campaign at the Cape Verde Atmospheric Observatory (CVAO on São Vicente island in the tropical North Atlantic in May and June 2007. The gas-phase data include HCl, HNO3, HONO, HCOOH, CH3COOH, NH3, and volatile reactive chlorine other than HCl (Cl*. Aerosol samples were analyzed by neutron activation (Na, Al, Cl, V, Mn, and Br and ion chromatography (SO42−, Cl−, Br−, NH4+, Na+, K+, Mg2+, and Ca2+. Content and quality of the data, which are available under doi:10.5281/zenodo.6956, are presented and discussed.

  14. Gas generation from Hanford grout samples

    International Nuclear Information System (INIS)

    Jonah, C.D.; Kapoor, S.; Matheson, M.S.; Mulac, W.A.; Meisel, D.

    1996-01-01

    In an extension of our work on the radiolytic processes that occur in the waste tanks at the Hanford site, we studied the gas generation from grout samples that contained nuclear waste simulants. Grout is one option for the long-term storage of low-level nuclear waste solutions but the radiolytic effects on grout have not been thoroughly defined. In particular, the generation of potentially flammable and hazardous gases required quantification. A research team at Argonne examined this issue and found that the total amount of gases generated radiolytically from the WHC samples was an order of magnitude higher than predicted. This implies that novel pathways fro charge migration from the solid grout to the associated water are responsible for gas evolution. The grout samples produced hydrogen, nitrous oxide, and carbon monoxide as well as nitrogen and oxygen. Yields of each of these substances were determined for doses that are equivalent to about 80 years storage of the grout. Carbon monoxide, which was produced in 2% yield, is of particular importance because even small amounts may adversely affect catalytic conversion instrumentation that has been planned for installation in the storage vaults

  15. Gas-driven pump for ground-water samples

    Science.gov (United States)

    Signor, Donald C.

    1978-01-01

    Observation wells installed for artificial-recharge research and other wells used in different ground-water programs are frequently cased with small-diameter steel pipe. To obtain samples from these small-diameter wells in order to monitor water quality, and to calibrate solute-transport models, a small-diameter pump with unique operating characteristics is required that causes a minimum alternation of samples during field sampling. A small-diameter gas-driven pump was designed and built to obtain water samples from wells of two-inch diameter or larger. The pump is a double-piston type with the following characteristics: (1) The water sample is isolated from the operating gas, (2) no source of electricity is ncessary, (3) operation is continuous, (4) use of compressed gas is efficient, and (5) operation is reliable over extended periods of time. Principles of operation, actual operation techniques, gas-use analyses and operating experience are described. Complete working drawings and a component list are included. Recent modifications and pump construction for high-pressure applications also are described. (Woodard-USGS)

  16. Explosive dome eruptions modulated by periodic gas-driven inflation

    Science.gov (United States)

    Johnson, Jeffrey B.; Lyons, John; Andrews, B. J.; Lees, J.M.

    2014-01-01

    Volcan Santiaguito (Guatemala) “breathes” with extraordinary regularity as the edifice's conduit system accumulates free gas, which periodically vents to the atmosphere. Periodic pressurization controls explosion timing, which nearly always occurs at peak inflation, as detected with tiltmeters. Tilt cycles in January 2012 reveal regular 26 ± 6 min inflation/deflation cycles corresponding to at least ~101 kg/s of gas fluxing the system. Very long period (VLP) earthquakes presage explosions and occur during cycles when inflation rates are most rapid. VLPs locate ~300 m below the vent and indicate mobilization of volatiles, which ascend at ~50 m/s. Rapid gas ascent feeds pyroclast-laden eruptions lasting several minutes and rising to ~1 km. VLPs are not observed during less rapid inflation episodes; instead, gas vents passively through the conduit producing no infrasound and no explosion. These observations intimate that steady gas exsolution and accumulation in shallow reservoirs may drive inflation cycles at open-vent silicic volcanoes.

  17. Periodic reviews of structural integrity of gas-cooled reactors

    International Nuclear Information System (INIS)

    Banks, P.J.; Stokoe, T.Y.; Thomas, D.L.

    1995-01-01

    Nuclear Electric operates 12 gas-cooled reactor power stations which have been in service for between 5 and 30 years. Periodically, comprehensive reviews of the safety cases are carried out for each station. The approach followed in these reviews in respect of structural integrity is outlined with the use of illustrative examples. (author)

  18. Tests of gas sampling electromagnetic shower calorimeter

    International Nuclear Information System (INIS)

    Barbaro-Galtieri, A.; Carithers, W.; Day, C.; Johnson, K.J.; Wenzel, W.A.; Videau, H.

    1983-01-01

    An electromagnetic shower gas-sampling calorimeter has been tested in both Geiger and proportional discharge modes for incident electron energies in the range 0.125-16 GeV. The 0.2 radiation length-thick layers were lead-fiberglass laminates with cathode strips normal to the sense wires. The 5x10 mm 2 Geiger cells were formed with uniformly spaced nylon fibers perpendicular to the wires. Proportional mode measurements were carried out in the pressure range 1-10 atm. A Monte Carlo simulation is in good agreement with measured shower characteristics and has been used to predict the behavior for oblique of incidence and for various Geiger cell dimensions. (orig.)

  19. Suitability of selected free-gas and dissolved-gas sampling containers for carbon isotopic analysis.

    Science.gov (United States)

    Eby, P; Gibson, J J; Yi, Y

    2015-07-15

    Storage trials were conducted for 2 to 3 months using a hydrocarbon and carbon dioxide gas mixture with known carbon isotopic composition to simulate typical hold times for gas samples prior to isotopic analysis. A range of containers (both pierced and unpierced) was periodically sampled to test for δ(13)C isotopic fractionation. Seventeen containers were tested for free-gas storage (20°C, 1 atm pressure) and 7 containers were tested for dissolved-gas storage, the latter prepared by bubbling free gas through tap water until saturated (20°C, 1 atm) and then preserved to avoid biological activity by acidifying to pH 2 with phosphoric acid and stored in the dark at 5°C. Samples were extracted using valves or by piercing septa, and then introduced into an isotope ratio mass spectrometer for compound-specific δ(13)C measurements. For free gas, stainless steel canisters and crimp-top glass serum bottles with butyl septa were most effective at preventing isotopic fractionation (pierced and unpierced), whereas silicone and PTFE-butyl septa allowed significant isotopic fractionation. FlexFoil and Tedlar bags were found to be effective only for storage of up to 1 month. For dissolved gas, crimp-top glass serum bottles with butyl septa were again effective, whereas silicone and PTFE-butyl were not. FlexFoil bags were reliable for up to 2 months. Our results suggest a range of preferred containers as well as several that did not perform very well for isotopic analysis. Overall, the results help establish better QA/QC procedures to avoid isotopic fractionation when storing environmental gas samples. Recommended containers for air transportation include steel canisters and glass serum bottles with butyl septa (pierced and unpierced). Copyright © 2015 John Wiley & Sons, Ltd.

  20. Periodical gas flow around a well in porous media

    International Nuclear Information System (INIS)

    Shnaid, I.; Olek, S.

    1996-01-01

    Analytical solutions of the linearized governing equation are presented for periodic gas flow around a well in porous media. Two cases are considered: a fully penetrating well and a partially penetrating well. For the first case, a closed form solution is obtained, whereas for the second case the solution is in the form of eigenfunctions expansions. The results have practical application in compressed air energy storage. (authors)

  1. PERIOD ESTIMATION FOR SPARSELY SAMPLED QUASI-PERIODIC LIGHT CURVES APPLIED TO MIRAS

    Energy Technology Data Exchange (ETDEWEB)

    He, Shiyuan; Huang, Jianhua Z.; Long, James [Department of Statistics, Texas A and M University, College Station, TX (United States); Yuan, Wenlong; Macri, Lucas M., E-mail: lmacri@tamu.edu [George P. and Cynthia W. Mitchell Institute for Fundamental Physics and Astronomy, Department of Physics and Astronomy, Texas A and M University, College Station, TX (United States)

    2016-12-01

    We develop a nonlinear semi-parametric Gaussian process model to estimate periods of Miras with sparsely sampled light curves. The model uses a sinusoidal basis for the periodic variation and a Gaussian process for the stochastic changes. We use maximum likelihood to estimate the period and the parameters of the Gaussian process, while integrating out the effects of other nuisance parameters in the model with respect to a suitable prior distribution obtained from earlier studies. Since the likelihood is highly multimodal for period, we implement a hybrid method that applies the quasi-Newton algorithm for Gaussian process parameters and search the period/frequency parameter space over a dense grid. A large-scale, high-fidelity simulation is conducted to mimic the sampling quality of Mira light curves obtained by the M33 Synoptic Stellar Survey. The simulated data set is publicly available and can serve as a testbed for future evaluation of different period estimation methods. The semi-parametric model outperforms an existing algorithm on this simulated test data set as measured by period recovery rate and quality of the resulting period–luminosity relations.

  2. The duration of the transitory period of public gas distribution

    International Nuclear Information System (INIS)

    Gazzola, D.

    2006-01-01

    The article describes the interpretative problems concerning the duration of the transitory period of public gas distribution after law decree 273/05 came into effect. This decree is the third legislative measure which, in a period of five years, reforms the transitory provisions. The article outlines the normative background of legislative decree n. 164/00 (so called Letta decree) and law n. 239/04 (so called Marzano law) and it analyses their judicial interpretations. It then explains the changes introduced by law decree n. 273/05 and the new interpretative problems there might be with reference to this decree. The decree clarifies the due date of the transitory period and specifies that the date of 31st December 2005 is postponed to 31st December 2007. The Administrative Tribunal of Lombardia Region Brescia tried to limit the effects of law decree n. 273/05, stating that the new expiration date could not regard the contracts for which the local authorities had already acknowledged the previous due date. The State Council argued instead that the new law decree regards all the contracts. This decree also clarifies that the chances of increasing duration ex art. 15, comma 7, legislative decree n. 164/00, applies automatically, but it doesn't solve the interpretative problem concerning the possibility of adding up more than one of these chances. The article focuses on the problems of the public gas distribution after the reform of this sector with the implementation of directive n. 98/30/CE and it underlines that the various legislative measures of these years are indicative of the difficulty to allow a gradual transition towards a liberalized market. In this context, law decree n. 273/05 is the last legislative measure which tries to guarantee a balance between the rapid liberalization of the market, on one hand, and the interests of the firms which had contracts when the reform came into effect, on the other hand [it

  3. Relationship between gas production and starch degradation in feed samples

    NARCIS (Netherlands)

    Chai, W.Z.; Gelder, van A.H.; Cone, J.W.

    2004-01-01

    An investigation was completed of the possibilities to estimate starch fermentation in rumen fluid using the gas production technique by incubating the total sample. Gas production from six starchy feed ingredients and eight maize silage samples were recorded and related to starch degradation

  4. Neonatal blood gas sampling methods | Goenka | South African ...

    African Journals Online (AJOL)

    There is little published guidance that systematically evaluates the different methods of neonatal blood gas sampling, where each method has its individual benefits and risks. This review critically surveys the available evidence to generate a comparison between arterial and capillary blood gas sampling, focusing on their ...

  5. Unsupervised Ensemble Anomaly Detection Using Time-Periodic Packet Sampling

    Science.gov (United States)

    Uchida, Masato; Nawata, Shuichi; Gu, Yu; Tsuru, Masato; Oie, Yuji

    We propose an anomaly detection method for finding patterns in network traffic that do not conform to legitimate (i.e., normal) behavior. The proposed method trains a baseline model describing the normal behavior of network traffic without using manually labeled traffic data. The trained baseline model is used as the basis for comparison with the audit network traffic. This anomaly detection works in an unsupervised manner through the use of time-periodic packet sampling, which is used in a manner that differs from its intended purpose — the lossy nature of packet sampling is used to extract normal packets from the unlabeled original traffic data. Evaluation using actual traffic traces showed that the proposed method has false positive and false negative rates in the detection of anomalies regarding TCP SYN packets comparable to those of a conventional method that uses manually labeled traffic data to train the baseline model. Performance variation due to the probabilistic nature of sampled traffic data is mitigated by using ensemble anomaly detection that collectively exploits multiple baseline models in parallel. Alarm sensitivity is adjusted for the intended use by using maximum- and minimum-based anomaly detection that effectively take advantage of the performance variations among the multiple baseline models. Testing using actual traffic traces showed that the proposed anomaly detection method performs as well as one using manually labeled traffic data and better than one using randomly sampled (unlabeled) traffic data.

  6. Portable tester for determining gas content within a core sample

    Science.gov (United States)

    Garcia, F. Jr.; Schatzel, S.J.

    1998-04-21

    A portable tester is provided for reading and displaying the pressure of a gas released from a rock core sample stored within a sealed container and for taking a sample of the released pressurized gas for chemical analysis thereof for subsequent use in a modified direct method test which determines the volume of gas and specific type of gas contained within the core sample. The portable tester includes a pair of low and high range electrical pressure transducers for detecting a gas pressure; a pair of low and high range display units for displaying the pressure of the detected gas; a selector valve connected to the low and high range pressure transducers and a selector knob for selecting gas flow to one of the flow paths; control valve having an inlet connection to the sealed container; and outlets connected to: a sample gas canister, a second outlet port connected to the selector valve means for reading the pressure of the gas from the sealed container to either the low range or high range pressure transducers, and a connection for venting gas contained within the sealed container to the atmosphere. A battery is electrically connected to and supplies the power for operating the unit. The pressure transducers, display units, selector and control valve means and the battery is mounted to and housed within a protective casing for portable transport and use. 5 figs.

  7. Apparatus and method for maintaining multi-component sample gas constituents in vapor phase during sample extraction and cooling

    Science.gov (United States)

    Felix, Larry Gordon; Farthing, William Earl; Irvin, James Hodges; Snyder, Todd Robert

    2010-05-11

    A dilution apparatus for diluting a gas sample. The apparatus includes a sample gas conduit having a sample gas inlet end and a diluted sample gas outlet end, and a sample gas flow restricting orifice disposed proximate the sample gas inlet end connected with the sample gas conduit and providing fluid communication between the exterior and the interior of the sample gas conduit. A diluted sample gas conduit is provided within the sample gas conduit having a mixing end with a mixing space inlet opening disposed proximate the sample gas inlet end, thereby forming an annular space between the sample gas conduit and the diluted sample gas conduit. The mixing end of the diluted sample gas conduit is disposed at a distance from the sample gas flow restricting orifice. A dilution gas source connected with the sample gas inlet end of the sample gas conduit is provided for introducing a dilution gas into the annular space, and a filter is provided for filtering the sample gas. The apparatus is particularly suited for diluting heated sample gases containing one or more condensable components.

  8. Soil Gas Sample Handling: Evaluation of Water Removal and Sample Ganging

    Energy Technology Data Exchange (ETDEWEB)

    Fritz, Brad G. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Abrecht, David G. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Hayes, James C. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Mendoza, Donaldo P. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States)

    2016-10-31

    Soil gas sampling is currently conducted in support of Nuclear Test Ban treaty verification. Soil gas samples are collected and analyzed for isotopes of interest. Some issues that can impact sampling and analysis of these samples are excess moisture and sample processing time. Here we discuss three potential improvements to the current sampling protocol; a desiccant for water removal, use of molecular sieve to remove CO2 from the sample during collection, and a ganging manifold to allow composite analysis of multiple samples.

  9. PROTOCOL FOR GAS SAMPLING AND ANALYSIS IN STRANDED MARINE MAMMALS

    OpenAIRE

    sprotocols

    2015-01-01

    Authors: Yara Bernaldo de Quirós, Óscar González-Díaz, Manuel Arbelo, Marisa Andrada & Antonio Fernández ### Abstract Gas sampling in stranded marine mammals can now be performed in situ using the appropriate vacuum tubes, insulin syringes and an aspirometer. Glass vacuum tubes are used for extraction of gas from cavities such as the intestine, pterigoyd air sacs, pneumothorax or subcapsular emphysema as well as for storage of the gas sample at room temperature and pressure. Insulin s...

  10. Radioactively induced noise in gas-sampling uranium calorimeters

    International Nuclear Information System (INIS)

    Gordon, H.A.; Rehak, P.

    1982-01-01

    The signal induced by radioactivity of a U 238 absorber in a cell of a gas-sampling uranium calorimeter was studied. By means of Campbell's theorem, the levels of the radioactively induced noise in uranium gas-sampling calorimeters was calculated. It was shown that in order to obtain similar radioactive noise performance as U-liquid argon or U-scintillator combinations, the α-particles from the uranium must be stopped before entering the sensing volume of gas-uranium calorimeters

  11. GNS Castor V/21 Headspace Gas Sampling 2014

    Energy Technology Data Exchange (ETDEWEB)

    Winston, Philip Lon [Idaho National Lab. (INL), Idaho Falls, ID (United States)

    2016-01-01

    Prior to performing an internal visual inspection, samples of the headspace gas of the GNS Castor V/21 cask were taken on June 12, 2014. These samples were taken in support of the CREIPI/Japanese nuclear industry effort to validate fuel integrity without visual inspection by measuring the 85Kr content of the cask headspace

  12. Diffusion probe for gas sampling in undisturbed soil

    DEFF Research Database (Denmark)

    Petersen, Søren O

    2014-01-01

    Soil-atmosphere fluxes of trace gases such as methane (CH4) and nitrous oxide (N2O) are determined by complex interactions between biological activity and soil conditions. Soil gas concentration profiles may, in combination with other information about soil conditions, help to understand emission...... controls. This note describes a simple and robust diffusion probe for soil gas sampling as part of flux monitoring programs. It can be deployed with minimum disturbance of in-situ conditions, also at sites with a high or fluctuating water table. Separate probes are used for each sampling depth...... on peat soils used for grazing showed soil gas concentrations of CH4 and N2O as influenced by topography, site conditions, and season. The applicability of the diffusion probe for trace gas monitoring is discussed....

  13. Ballistic magnetotransport in a suspended two-dimensional electron gas with periodic antidot lattices

    Energy Technology Data Exchange (ETDEWEB)

    Zhdanov, E. Yu., E-mail: zhdanov@isp.nsc.ru; Pogosov, A. G.; Budantsev, M. V.; Pokhabov, D. A.; Bakarov, A. K. [Siberian Branch of the Russian Academy of Sciences, Rzhanov Institute of Semiconductor Physics (Russian Federation)

    2017-01-15

    The magnetoresistance of suspended semiconductor nanostructures with a two-dimensional electron gas structured by periodic square antidot lattices is studied. It is shown that the ballistic regime of electron transport is retained after detaching the sample from the substrate. Direct comparative analysis of commensurability oscillations of magnetoresistance and their temperature dependences in samples before and after suspension is performed. It is found that the temperature dependences are almost identical for non-suspended and suspended samples, whereas significant differences are observed in the nonlinear regime, caused by direct current passage. Commensurability oscillations in the suspended samples are more stable with respect to exposure to direct current, which can be presumably explained by electron–electron interaction enhancement after detaching nanostructures from the high-permittivity substrate.

  14. Portable automation of static chamber sample collection for quantifying soil gas flux

    Science.gov (United States)

    The collection of soil gas flux using the static chamber method is labor intensive. The number of chambers that can be sampled in a given time period is limited by the spacing between chambers and the availability of trained research technicians. However, the static chamber method can limit spatial ...

  15. Determination of thiobencarb in water samples by gas ...

    African Journals Online (AJOL)

    Homogeneous liquid-liquid microextraction via flotation assistance (HLLME-FA) coupled with gas chromatography-flame ionization detection (GC-FID) was applied for the extraction and determination of thiobencarb in water samples. In this study, a special extraction cell was designed to facilitate collection of the ...

  16. On-line Automated Sample Preparation-Capillary Gas Chromatography for the Analysis of Plasma Samples.

    NARCIS (Netherlands)

    Louter, A.J.H.; van der Wagt, R.A.C.A.; Brinkman, U.A.T.

    1995-01-01

    An automated sample preparation module, (the automated sample preparation with extraction columns, ASPEC), was interfaced with a capillary gas chromatograph (GC) by means of an on-column interface. The system was optimised for the determination of the antidepressant trazodone in plasma. The clean-up

  17. PlanetVac: Sample Return with a Puff of Gas

    Science.gov (United States)

    Zacny, K.; Mueller, R.; Betts, B. H.

    2014-12-01

    PlanetVac is a regolith sample acquisition mission concept that uses compressed gas to blow material from the surface up a pneumatic tube and directly into a sample return container. The PlanetVac sampling device is built into the lander legs to eliminate cost and complexity associated with robotic arms and scoops. The pneumatic system can effectively capture fine and coarse regolith, including small pebbles. It is well suited for landed missions to Mars, asteroids, or the Moon. Because of the low pressures on all those bodies, the technique is extremely efficient. If losses are kept to minimum, 1 gram of compressed gas could efficiently lift 6000 grams of soil. To demonstrate this approach, the PlanetVac lander with four legs and two sampling tubes has been designed, integrated, and tested. Vacuum chamber testing was performed using two well-known planetary regolith simulants: Mars Mojave Simulant (MMS) and lunar regolith simulant JSC-1A. One of the two sampling systems was connected to a mockup of an earth return rocket while the second sampling system was connected to a lander deck mounted instrument (clear box for easy viewing). The tests included a drop from a height of approximately 50 cm onto the bed of regolith, deployment of sampling tubes into the regolith, pneumatic acquisition of sample into an instrument (sample container) and the rocket, and the launch of the rocket. The demonstration has been successful and can be viewed here: https://www.youtube.com/watch?v=DjJXvtQk6no. In most of the tests, 20 grams or more of sample was delivered to the 'instrument' and approximately 5 grams of regolith was delivered into a sampling chamber within the rocket. The gas lifting efficiency was calculated to be approximately 1000:1; that is 1 gram of gas lofted 1000 grams of regolith. Efficiencies in lower gravity environments are expected to be much higher. This successful, simple and lightweight sample capture demonstration paves the way to using such sampling system

  18. Portable Automation of Static Chamber Sample Collection for Quantifying Soil Gas Flux

    Energy Technology Data Exchange (ETDEWEB)

    Davis, Morgan P.; Groh, Tyler A.; Parkin, Timothy B.; Williams, Ryan J.; Isenhart, Thomas M.; Hofmockel, Kirsten S.

    2018-01-01

    Quantification of soil gas flux using the static chamber method is labor intensive. The number of chambers that can be sampled is limited by the spacing between chambers and the availability of trained research technicians. An automated system for collecting gas samples from chambers in the field would eliminate the need for personnel to return to the chamber during a flux measurement period and would allow a single technician to sample multiple chambers simultaneously. This study describes Chamber Automated Sampling Equipment (FluxCASE) to collect and store chamber headspace gas samples at assigned time points for the measurement of soil gas flux. The FluxCASE design and operation is described, and the accuracy and precision of the FluxCASE system is evaluated. In laboratory measurements of nitrous oxide (N2O), carbon dioxide (CO2), and methane (CH4) concentrations of a standardized gas mixture, coefficients of variation associated with automated and manual sample collection were comparable, indicating no loss of precision. In the field, soil gas fluxes measured from FluxCASEs were in agreement with manual sampling for both N2O and CO2. Slopes of regression equations were 1.01 for CO2 and 0.97 for N2O. The 95% confidence limits of the slopes of the regression lines included the value of one, indicating no bias. Additionally, an expense analysis found a cost recovery ranging from 0.6 to 2.2 yr. Implementing the FluxCASE system is an alternative to improve the efficiency of the static chamber method for measuring soil gas flux while maintaining the accuracy and precision of manual sampling.

  19. LEAK AND GAS PERMEABILITY TESTING DURING SOIL-GAS SAMPLING AT HAL'S CHEVRON LUST SITE IN GREEN RIVER, UTAH

    Science.gov (United States)

    The results of gas permeability and leak testing during active soil-gas sampling at Hal’s Chevron LUST Site in Green River, Utah are presented. This study was conducted to support development of a passive soil-gas sampling method. Gas mixtures containing helium and methane were...

  20. Application of Notched Long-Period Fiber Grating Based Sensor for CO2 Gas Sensing

    Science.gov (United States)

    Wu, Chao-Wei; Chiang, Chia-Chin

    2016-01-01

    An inductively coupled plasma etching process to fabricate notched long-period fiber gratings for CO2 gas sensing is proposed in this article. In the gas sensing test, the 15% mixed CO2 gas was used for characterization of CO2 adsorption by the amine-modified nanoporous silica foams of the notched long-period fiber grating sensor. The results shows the spectra were changed with the CO2 gas flow within 13 min. During the absorption process, the transmission of the resonant dip was decreased by 2.884 dB. Therefore, the proposed notched long-period fiber grating gas sensor shows good performance and is suitable as a gas sensor for monitoring the CO2 adsorption process.

  1. Atmospheric Gas Tracers in Groundwater: Theory, Sampling. Measurement and Interpretation

    International Nuclear Information System (INIS)

    Bayari, C.S.

    2002-01-01

    Some of the atmospheric gasses posses features that are sought in an environmental tracer of hydrogeologic interest. Among these, chlorofluorocarbons, sulfur hegzafluoride, carbon tetrachloride, methyl chloroform, krypton-85 etc. have found increasing use in groundwater age dating studies during the last ten years. This paper explains the theory of their use as tracer and discusses the major concerns as related to their sampling and analyses. Factors affecting their applicability and the approach to interpret tracer gas data is briefly outlined

  2. STAR FORMATION LAWS: THE EFFECTS OF GAS CLOUD SAMPLING

    International Nuclear Information System (INIS)

    Calzetti, D.; Liu, G.; Koda, J.

    2012-01-01

    Recent observational results indicate that the functional shape of the spatially resolved star formation-molecular gas density relation depends on the spatial scale considered. These results may indicate a fundamental role of sampling effects on scales that are typically only a few times larger than those of the largest molecular clouds. To investigate the impact of this effect, we construct simple models for the distribution of molecular clouds in a typical star-forming spiral galaxy and, assuming a power-law relation between star formation rate (SFR) and cloud mass, explore a range of input parameters. We confirm that the slope and the scatter of the simulated SFR-molecular gas surface density relation depend on the size of the sub-galactic region considered, due to stochastic sampling of the molecular cloud mass function, and the effect is larger for steeper relations between SFR and molecular gas. There is a general trend for all slope values to tend to ∼unity for region sizes larger than 1-2 kpc, irrespective of the input SFR-cloud relation. The region size of 1-2 kpc corresponds to the area where the cloud mass function becomes fully sampled. We quantify the effects of selection biases in data tracing the SFR, either as thresholds (i.e., clouds smaller than a given mass value do not form stars) or as backgrounds (e.g., diffuse emission unrelated to current star formation is counted toward the SFR). Apparently discordant observational results are brought into agreement via this simple model, and the comparison of our simulations with data for a few galaxies supports a steep (>1) power-law index between SFR and molecular gas.

  3. Calculation of nonstationary gas-dynamic flows with periodic local supply of energy

    International Nuclear Information System (INIS)

    Mikhailova, N.V.; Myshetskaya, E.E.; Rakhimov, A.T.; Favorskii, A.P.

    The paper considers the motion of a flow of gas with local supply of energy periodic in time. Solution of the problem in one-dimensional formulation in the approximation of an ideal nonviscous non-heat-conducting gas is carried out by numerical methods. The possibility of emergence of the flow into a periodic regime is established and the rate of this process is calculated. The character of the periodic structure is investigated in dependence on the frequency of the superimposition of perturbations and the Mach number in unperturbed flow of the gas

  4. Tank 241-C-111 headspace gas and vapor sample results - August 1993 samples

    International Nuclear Information System (INIS)

    Huckaby, J.L.

    1994-01-01

    Tank 241-C-111 is on the ferrocyanide Watch List. Gas and vapor samples were collected to assure safe conditions before planned intrusive work was performed. Sample analyses showed that hydrogen is about ten times higher in the tank headspace than in ambient air. Nitrous oxide is about sixty times higher than ambient levels. The hydrogen cyanide concentration was below 0.04 ppbv, and the average NO x concentration was 8.6 ppmv

  5. HTGR gas-turbine program. Semiannual progress report for period ending March 31, 1980

    International Nuclear Information System (INIS)

    1982-01-01

    This report describes the conceptual design and analysis performed by General Atomic Company and its subcontractors for the US Department of Energy on the direct cycle gas turbine high-temperature gas-cooled reactor. The primary accomplishments for this period were cost reduction studies, turbomachinery failure analysis, and alternate plant concept evaluation

  6. Monte Carlo simulation of a gas-sampled hadron calorimeter

    Energy Technology Data Exchange (ETDEWEB)

    Chang, C Y; Kunori, S; Rapp, P; Talaga, R; Steinberg, P; Tylka, A J; Wang, Z M

    1988-02-15

    A prototype of the OPAL barrel hadron calorimeter, which is a gas-sampled calorimeter using plastic streamer tubes, was exposed to pions at energies between 1 and 7 GeV. The response of the detector was simulated using the CERN GEANT3 Monte Carlo program. By using the observed high energy muon signals to deduce details of the streamer formation, the Monte Carlo program was able to reproduce the observed calorimeter response. The behavior of the hadron calorimeter when placed behind a lead glass electromagnetic calorimeter was also investigated.

  7. Experience with environmental sampling at gas centrifuge enrichment plants

    International Nuclear Information System (INIS)

    Ekenstam, G. af; Bush, W.; Janov, J.; Kuhn, E.; Ryjinski, M.

    2001-01-01

    Environmental sampling has been used routinely by the IAEA since 1996 after the IAEA Board of Governors approved it in March 1995 as a new technique to strengthen safeguards and improve efficiency. In enrichment plants it is used to confirm that there has been no production of highly enriched uranium (HEU), or production of uranium at above the declared enrichment. The use of environmental sampling is based on the assumption that every process, no matter how leak tight, will release small amounts of process material to the environment. Even though these releases of nuclear material are extremely small in gas centrifuge enrichment plants, and well below levels of concern from a health physics and safety standpoint, they are detectable and their analysis provides an indication of the enrichment of the material that has been processed in the plant. The environmental samples at enrichment plants are collected by swiping selected areas of the plant with squares of cotton cloth (10x10 cm) from sampling kits prepared in ultra clean condition. The squares of cotton cloth sealed in plastic bags are sent for analysis to the Network Analytical Laboratories. The analysis includes the measurement of the uranium isotopic composition in uranium-containing particles by Thermal lonization Mass Spectroscopy (TIMS) or Secondary ION Mass Spectroscopy (SIMS). Since the implementation of environmental sampling, swipes have been collected from 240 sampling points at three gas centrifuge plants of URENCO, which have a total throughput of more than 8,000 tonnes of uranium per year. The particle analysis results generally reflected the known operational history of the plants and confirmed that they had only been operated to produce uranium with enrichment less than 5% 235 U. The information about the content of the minor isotopes 234 U and 236 U also indicates that depleted and recycled uranium were sometimes used as feed materials in some plants. An example is given of the TIMS particle

  8. POLYP: an automatic device for drawing sequential samples of gas

    Energy Technology Data Exchange (ETDEWEB)

    Gaglione, P; Koechler, C; Stanchi, L

    1974-12-01

    Polyp is an automatic device consisting of electronic equipment which drives sequentially 8 small pumps for drawing samples of gas. The electronic circuit is driven by a quartz oscillator and allows for the preselection of a waiting time in such a manner that a set of similar instruments placed in suitable position in the open country will start simultaneously. At the same time the first pump of each instrument will inflate a plastic bag for a preset time. The other seven pumps will inflate sequentially the other bags. The instrument is powered by rechargeable batteries and realized with C-MUS integrated circuits for a nearly negligible consumption. As it is foreseen for field operation it is waterproof.

  9. POLYP: an automatic device for drawing sequential samples of gas

    International Nuclear Information System (INIS)

    Gaglione, P.; Koechler, C.; Stanchi, L.

    1974-12-01

    POLYP is an automatic device consisting of an electronic equipment which drives sequentially 8 small pumps for drawing samples of gas. The electronic circuit is driven by a quartz oscillator and allows for the preselection of a waiting time in such a manner that a set of similar instruments placed in suitable position in the open country will start simultaneously. At the same time the first pump of each instrument will inflate a plastic bag for a preset time. Thereafter the other seven pumps will inflate sequentially the other bag. The instrument is powered by rechargeable batteries and realized with C-MOS integrated circuits for a nearly negligible consumption. As it is foreseen for field operation it is waterproof

  10. Analysis of the Retained Gas Sample (RGS) Extruder Assembly

    International Nuclear Information System (INIS)

    Coverdell, B.L.

    1995-09-01

    In order for the Retained Gas Sample (RGS) Extruder Assembly to be safely used it was determined by the cognizant engineer that analysis was necessary. The use of the finite-element analysis (FEA) progarm COSMOS/M version 1.71 permitted a quick, easy, and detailed stress analysis of the RGS Extruder Assembly. The FEA model is a three dimensional model using the SHELL4T element type. From the results of the FEA, the cognizant engineer determined that the RGS extruder would be rated at 10,000 lbf and load tested to 12,000 lbf. The respective input and output files for the model are EXTR02.GFM and EXTR02.OUT and can be found on the attached tape

  11. Blood gas sample spiking with total parenteral nutrition, lipid emulsion, and concentrated dextrose solutions as a model for predicting sample contamination based on glucose result.

    Science.gov (United States)

    Jara-Aguirre, Jose C; Smeets, Steven W; Wockenfus, Amy M; Karon, Brad S

    2018-05-01

    Evaluate the effects of blood gas sample contamination with total parenteral nutrition (TPN)/lipid emulsion and dextrose 50% (D50) solutions on blood gas and electrolyte measurement; and determine whether glucose concentration can predict blood gas sample contamination with TPN/lipid emulsion or D50. Residual lithium heparin arterial blood gas samples were spiked with TPN/lipid emulsion (0 to 15%) and D50 solutions (0 to 2.5%). Blood gas (pH, pCO2, pO2), electrolytes (Na+, K+ ionized calcium) and hemoglobin were measured with a Radiometer ABL90. Glucose concentration was measured in separated plasma by Roche Cobas c501. Chart review of neonatal blood gas results with glucose >300 mg/dL (>16.65 mmol/L) over a seven month period was performed to determine whether repeat (within 4 h) blood gas results suggested pre-analytical errors in blood gas results. Results were used to determine whether a glucose threshold could predict contamination resulting in blood gas and electrolyte results with greater than laboratory-defined allowable error. Samples spiked with 5% or more TPN/lipid emulsion solution or 1% D50 showed glucose concentration >500 mg/dL (>27.75 mmol/L) and produced blood gas (pH, pO 2 , pCO 2 ) results with greater than laboratory-defined allowable error. TPN/lipid emulsion, but not D50, produced greater than allowable error in electrolyte (Na + ,K + ,Ca ++ ,Hb) results at these concentrations. Based on chart review of 144 neonatal blood gas results with glucose >250 mg/dL received over seven months, four of ten neonatal intensive care unit (NICU) patients with glucose results >500 mg/dL and repeat blood gas results within 4 h had results highly suggestive of pre-analytical error. Only 3 of 36 NICU patients with glucose results 300-500 mg/dL and repeat blood gas results within 4 h had clear pre-analytical errors in blood gas results. Glucose concentration can be used as an indicator of significant blood sample contamination with either TPN

  12. The World gas model. A multi-period mixed complementarity model for the global natural gas market

    International Nuclear Information System (INIS)

    Egging, Ruud; Holz, Franziska; Gabriel, Steven A.

    2010-01-01

    We provide the description, mathematical formulation and illustrative results of the World Gas Model, a multi-period complementarity model for the global natural gas market with explicit consideration of market power in the upstream market. Market players include producers, traders, pipeline and storage operators, LNG (liquefied natural gas) liquefiers and regasifiers as well as marketers. The model data set contains more than 80 countries and regions and covers 98% of world wide natural gas production and consumption. We also include a detailed representation of cross-border natural gas pipelines and constraints imposed by long-term contracts in the LNG market. The model is calibrated to match production and consumption projections from the PRIMES [EC. European energy and transport: trends to 2030-update 2007. Brussels: European Commission; 2008] and POLES models [EC. World energy technology outlook - 2050 (WETO-H2). Brussels: European Commission; 2006] up to 2030. The results of our numerical simulations illustrate how the supply shares of pipeline and LNG in various regions in the world develop very differently over time. LNG will continue to play a major role in the Asian market, also for new importers like China and India. Europe will expand its pipeline import capacities benefiting from its relative proximity to major gas suppliers. (author)

  13. Two-Phase Gas-Liquid Flow Structure Characteristics under Periodic Cross Forces Action

    Directory of Open Access Journals (Sweden)

    V. V. Perevezentsev

    2015-01-01

    Full Text Available The article presents a study of two-phase gas-liquid flow under the action of periodic cross forces. The work objective is to obtain experimental data for further analysis and have structure characteristics of the two-phase flow movement. For research, to obtain data without disturbing effect on the flow were used optic PIV (Particle Image Visualization methods because of their noninvasiveness. The cross forces influence was provided by an experimental stand design to change the angular amplitudes and the periods of channel movement cycle with two-phase flow. In the range of volume gas rates was shown a water flow rate versus the inclination angle of immovable riser section and the characteristic angular amplitudes and periods of riser section inclination cycle under periodic cross forces. Data on distribution of average water velocity in twophase flow in abovementioned cases were also obtained. These data allowed us to draw a conclusion that a velocity distribution depends on the angular amplitude and on the period of the riser section roll cycle. This article belongs to publications, which study two-phase flows with no disturbing effect on them. Obtained data give an insight into understanding a pattern of twophase gas-liquid flow under the action of periodic cross forces and can be used to verify the mathematical models of the CFD thermo-hydraulic codes. In the future, the work development expects taking measurements with more frequent interval in the ranges of angular amplitudes and periods of the channel movement cycle and create a mathematical model to show the action of periodic cross forces on two-phase gas-liquid flow.

  14. Event Processing and Variable Part of Sample Period Determining in Combined Systems Using GA

    Science.gov (United States)

    Strémy, Maximilián; Závacký, Pavol; Jedlička, Martin

    2011-01-01

    This article deals with combined dynamic systems and usage of modern techniques in dealing with these systems, focusing particularly on sampling period design, cyclic processing tasks and related processing algorithms in the combined event management systems using genetic algorithms.

  15. Constraining the Dynamics of Periodic Behavior at Mt. Semeru, Indonesia, Combining Numerical Modeling and Field Measurements of Gas emission

    Science.gov (United States)

    Smekens, J.; Clarke, A. B.; De'Michieli Vitturi, M.; Moore, G. M.

    2012-12-01

    Mt. Semeru is one of the most active explosive volcanoes on the island of Java in Indonesia. The current eruption style consists of small but frequent explosions and/or gas releases (several times a day) accompanied by continuous lava effusion that sporadically produces block-and-ash flows down the SE flank of the volcano. Semeru presents a unique opportunity to investigate the magma ascent conditions that produce this kind of persistent periodic behavior and the coexistence of explosive and effusive eruptions. In this work we use DOMEFLOW, a 1.5D transient isothermal numerical model, to investigate the dynamics of lava extrusion at Semeru. Petrologic observations from tephra and ballistic samples collected at the summit help us constrain the initial conditions of the system. Preliminary model runs produced periodic lava extrusion and pulses of gas release at the vent, with a cycle period on the order of hours, even though a steady magma supply rate was prescribed at the bottom of the conduit. Enhanced shallow permeability implemented in the model appears to create a dense plug in the shallow subsurface, which in turn plays a critical role in creating and controlling the observed periodic behavior. We measured SO2 fluxes just above the vent, using a custom UV imaging system. The device consists of two high-sensitivity CCD cameras with narrow UV filters centered at 310 and 330 nm, and a USB2000+ spectrometer for calibration and distance correction. The method produces high-frequency flux series with an accurate determination of the wind speed and plume geometry. The model results, when combined with gas measurements, and measurements of sulfur in both the groundmass and melt inclusions in eruptive products, could be used to create a volatile budget of the system. Furthermore, a well-calibrated model of the system will ultimately allow the characteristic periodicity and corresponding gas flux to be used as a proxy for magma supply rate.

  16. Governing transitions: Cases and insights from two periods in the history of the UK gas industry

    International Nuclear Information System (INIS)

    Arapostathis, Stathis; Carlsson-Hyslop, Anna; Pearson, Peter J G; Thornton, Judith; Gradillas, Maria; Laczay, Scott; Wallis, Suzanne

    2013-01-01

    The paper aims to inform historically the analyses of future sociotechnical transition pathways in the electricity sector, particularly those developed by the Transition Pathways to a Low Carbon Economy project. It also aims to inform the theoretical approach to transitions by focusing on key decisions at ‘branching points’ that led to transitions in the UK gas energy services regime, which occurred under different governance patterns. The first historical case study covers the market-led transformation of the manufactured gas regime from 1877 to 1914, which developed the end-uses of gas beyond lighting to include cooking, and extended access to working class consumers. The second case study covers the period from 1948 to 1977, historically reconstructing the transition from town gas to natural gas. This state-led and coordinated conversion to natural gas was preceded by a period of destabilisation of the manufactured gas regime, the co-existence of several niche technologies and the hybridisation of the key actors and technological infrastructures of the incumbent regime. Comparing the cases provides insights for future energy service transitions by addressing the significance of power, trust and networking in the decision making processes involved in the governance of energy transitions. - Highlights: ► Historical work is useful in understanding socio-technical energy transitions. ► Different governance modes have led to transitions with different characteristics. ► Gas regimes operating under market and state ‘logics’ took decisions differently. ► Decisions at key branching points led to path dependency, affecting later decisions. ► Agency, governance and trust were important elements in the transitions analysed.

  17. Multi-period natural gas market modeling Applications, stochastic extensions and solution approaches

    Science.gov (United States)

    Egging, Rudolf Gerardus

    This dissertation develops deterministic and stochastic multi-period mixed complementarity problems (MCP) for the global natural gas market, as well as solution approaches for large-scale stochastic MCP. The deterministic model is unique in the combination of the level of detail of the actors in the natural gas markets and the transport options, the detailed regional and global coverage, the multi-period approach with endogenous capacity expansions for transportation and storage infrastructure, the seasonal variation in demand and the representation of market power according to Nash-Cournot theory. The model is applied to several scenarios for the natural gas market that cover the formation of a cartel by the members of the Gas Exporting Countries Forum, a low availability of unconventional gas in the United States, and cost reductions in long-distance gas transportation. 1 The results provide insights in how different regions are affected by various developments, in terms of production, consumption, traded volumes, prices and profits of market participants. The stochastic MCP is developed and applied to a global natural gas market problem with four scenarios for a time horizon until 2050 with nineteen regions and containing 78,768 variables. The scenarios vary in the possibility of a gas market cartel formation and varying depletion rates of gas reserves in the major gas importing regions. Outcomes for hedging decisions of market participants show some significant shifts in the timing and location of infrastructure investments, thereby affecting local market situations. A first application of Benders decomposition (BD) is presented to solve a large-scale stochastic MCP for the global gas market with many hundreds of first-stage capacity expansion variables and market players exerting various levels of market power. The largest problem solved successfully using BD contained 47,373 variables of which 763 first-stage variables, however using BD did not result in

  18. Multi-Period Natural Gas Market Modeling. Applications, Stochastic Extensions and Solution Approaches

    International Nuclear Information System (INIS)

    Egging, R.G.

    2010-11-01

    This dissertation develops deterministic and stochastic multi-period mixed complementarity problems (MCP) for the global natural gas market, as well as solution approaches for large-scale stochastic MCP. The deterministic model is unique in the combination of the level of detail of the actors in the natural gas markets and the transport options, the detailed regional and global coverage, the multi-period approach with endogenous capacity expansions for transportation and storage infrastructure, the seasonal variation in demand and the representation of market power according to Nash-Cournot theory. The model is applied to several scenarios for the natural gas market that cover the formation of a cartel by the members of the Gas Exporting Countries Forum, a low availability of unconventional gas in the United States, and cost reductions in long-distance gas transportation. The results provide insights in how different regions are affected by various developments, in terms of production, consumption, traded volumes, prices and profits of market participants. The stochastic MCP is developed and applied to a global natural gas market problem with four scenarios for a time horizon until 2050 with nineteen regions and containing 78,768 variables. The scenarios vary in the possibility of a gas market cartel formation and varying depletion rates of gas reserves in the major gas importing regions. Outcomes for hedging decisions of market participants show some significant shifts in the timing and location of infrastructure investments, thereby affecting local market situations. A first application of Benders decomposition (BD) is presented to solve a large-scale stochastic MCP for the global gas market with many hundreds of first-stage capacity expansion variables and market players exerting various levels of market power. The largest problem solved successfully using BD contained 47,373 variables of which 763 first-stage variables, however using BD did not result in

  19. Gasbuggy, New Mexico, Hydrologic and Natural Gas Sampling and Analysis Results for 2009

    International Nuclear Information System (INIS)

    2009-11-01

    The U.S. Department of Energy (DOE) Office of Legacy Management conducted hydrologic and natural gas sampling for the Gasbuggy, New Mexico, site on June 16, and 17, 2009. Hydrologic sampling consists of collecting water samples from water wells and surface water locations. Natural gas sampling consists of collecting both gas samples and samples of produced water from gas production wells. The water well samples were analyzed for gamma-emitting radionuclides and tritium. Surface water samples were analyzed for tritium. Water samples from gas production wells were analyzed for gamma-emitting radionuclides, gross alpha, gross beta, and tritium. Natural gas samples were analyzed for tritium and carbon-14. Water samples were analyzed by ALS Laboratory Group in Fort Collins, Colorado, and natural gas samples were analyzed by Isotech Laboratories in Champaign, Illinois. Concentrations of tritium and gamma-emitting radionuclides in water samples collected in the vicinity of the Gasbuggy site continue to demonstrate that the sample locations have not been impacted by detonation-related contaminants. Results from the sampling of natural gas from producing wells demonstrate that the gas wells nearest the Gasbuggy site are not currently impacted by detonation-related contaminants. Annual sampling of the gas production wells nearest the Gasbuggy site for gas and produced water will continue for the foreseeable future. The sampling frequency of water wells and surface water sources in the surrounding area will be reduced to once every 5 years. The next hydrologic sampling event at water wells, springs, and ponds will be in 2014.

  20. Effects of gas periodic stimulation on key enzyme activity in gas double-dynamic solid state fermentation (GDD-SSF).

    Science.gov (United States)

    Chen, Hongzhang; Shao, Meixue; Li, Hongqiang

    2014-03-05

    The heat and mass transfer have been proved to be the important factors in air pressure pulsation for cellulase production. However, as process of enzyme secretion, the cellulase formation has not been studied in the view of microorganism metabolism and metabolic key enzyme activity under air pressure pulsation condition. Two fermentation methods in ATPase activity, cellulase productivity, weight lose rate and membrane permeability were systematically compared. Results indicated that gas double-dynamic solid state fermentation had no obviously effect on cell membrane permeability. However, the relation between ATPase activity and weight loss rate was linearly dependent with r=0.9784. Meanwhile, the results also implied that gas periodic stimulation had apparently strengthened microbial metabolism through increasing ATPase activity during gas double-dynamic solid state fermentation, resulting in motivating the production of cellulase by Trichoderma reesei YG3. Therefore, the increase of ATPase activity would be another crucial factor to strengthen fermentation process for cellulase production under gas double-dynamic solid state fermentation. Copyright © 2013 Elsevier Inc. All rights reserved.

  1. Wuchereria bancrofti in Tanzania: microfilarial periodicity and effect of blood sampling time on microfilarial intensities

    DEFF Research Database (Denmark)

    Simonsen, Poul Erik; Niemann, L.; Meyrowitsch, Dan Wolf

    1997-01-01

    The circadian periodicity of Wuchereria bancrofti microfilarial (mf) intensities in peripheral blood was analysed in a group of infected individuals from an endemic community in north-eastern Tanzania. The mf density was quantified at two-hourly intervals for 24 hours. A clear nocturnal periodic...... of blood sampling before peak time is discussed, and the importance of taking sampling time into consideration when analysing data from epidemiological studies is emphasized. A simple method is devised which can be used to adjust for the influence of time on mf intensities, in studies where accurate...... information on mf intensities is necessary, and where it is impossible to obtain all samples at peak time....

  2. Comparative study of the characteristics of some suction devices for gas sampling applications

    International Nuclear Information System (INIS)

    Donguy, R.; Drouet, J.

    1959-06-01

    Gas sampling (used to determine the characteristics of dusts or aerosols contained in a gas) needs a suction device. In order to select the right device and the right conditions of use, the characteristics and performances of various suction devices (helicoidal and centrifugal aspirators, air pumps, volumetric pumps) have been experimentally measured: flow rate, head loss, sampling volume and duration, aerosol and dust concentration, gas density, nature of the gas, suction circuit configuration, etc

  3. Synthesis of Nanoparticles in a Pulsed-Periodic Gas Discharge and Their Potential Applications

    Science.gov (United States)

    Ivanov, V. V.; Efimov, A. A.; Myl'nikov, D. A.; Lizunova, A. A.

    2018-03-01

    Conditions for the synthesis of three types nanoparticles (SnO2, Al2O3, and Ag) with typical sizes in the range of 4 to 10 nm and a performance of 0.4 g/h are employed in a pulsed-periodic gas discharge in an atmosphere of air. Spherical Ge nanoparticles with a characteristic size of 13 nm are synthesized by these means for the first time with a performance of around 10 mg/h. The specific energy consumption in the synthesis of nanoparticles is for these materials in the range of 2000 to 5000 kW h/kg. The prospects for using tinoxide nanoparticles in sensor components and jets of silver nanoparticles for aerosol printing are discussed. The merits and demerits of the pulsed gas-discharge method among other gas-phase approaches to the synthesis of nanoparticles are analyzed for the current level of development.

  4. Distributions of crystals and gas bubbles in reservoir ice during growth period

    Directory of Open Access Journals (Sweden)

    Zhi-jun Li

    2011-06-01

    Full Text Available In order to understand the dominant factors of the physical properties of ice in ice thermodynamics and mechanics, in-situ observations of ice growth and decay processes were carried out. Two samplings were conducted in the fast and steady ice growth stages. Ice pieces were used to observe ice crystals and gas bubbles in ice, and to measure the ice density. Vertical profiles of the type and size of ice crystals, shape and size of gas bubbles, and gas bubble content, as well as the ice density, were obtained. The results show that the upper layer of the ice pieces is granular ice and the lower layer is columnar ice; the average crystal size increases with the ice depth and remains steady in the fast and steady ice growth stages; the shape of gas bubbles in the upper layer of ice pieces is spherical with higher total content, and the shape in the middle and lower layers is cylinder with lower total content; the gas bubble size and content vary with the ice growth stage; and the ice density decreases with the increase of the gas bubble content.

  5. Gas liquid sampling for closed canisters in KW Basin - test plan

    International Nuclear Information System (INIS)

    Pitkoff, C.C.

    1995-01-01

    Test procedures for the gas/liquid sampler. Characterization of the Spent Nuclear Fuel, SNF, sealed in canisters at KW-Basin is needed to determine the state of storing SNF wet. Samples of the liquid and the gas in the closed canisters will be taken to gain characterization information. Sampling equipment has been designed to retrieve gas and liquid from the closed canisters in KW basin. This plan is written to outline the test requirements for this developmental sampling equipment

  6. Evaluation of the Frequency for Gas Sampling for the High Burnup Confirmatory Data Project

    Energy Technology Data Exchange (ETDEWEB)

    Stockman, Christine T. [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States); Alsaed, Halim A. [Idaho National Lab. (INL), Idaho Falls, ID (United States); Bryan, Charles R. [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States); Marschman, Steven C. [Idaho National Lab. (INL), Idaho Falls, ID (United States); Scaglione, John M. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

    2015-05-01

    This report provides a technically based gas sampling frequency strategy for the High Burnup (HBU) Confirmatory Data Project. The evaluation of: 1) the types and magnitudes of gases that could be present in the project cask and, 2) the degradation mechanisms that could change gas compositions culminates in an adaptive gas sampling frequency strategy. This adaptive strategy is compared against the sampling frequency that has been developed based on operational considerations.

  7. Exact dynamics of a one dimensional Bose gas in a periodic time-dependent harmonic trap

    Science.gov (United States)

    Scopa, Stefano; Unterberger, Jéremie; Karevski, Dragi

    2018-05-01

    We study the unitary dynamics of a 1D gas of hard-core bosons trapped into a harmonic potential which varies periodically in time with frequency . Such periodic systems can be classified into orbits of different monodromies corresponding to two different physical situations, namely the case in which the bosonic cloud remains stable during the time-evolution and the case where it turns out to be unstable. In the present work we derive in the large particle number limit exact results for the stroboscopic evolution of the energy and particle densities in both physical situations.

  8. Magnetoresistance calculations for a two-dimensional electron gas with unilateral short-period strong modulation

    Czech Academy of Sciences Publication Activity Database

    Výborný, Karel; Smrčka, Ludvík

    2002-01-01

    Roč. 66, č. 20 (2002), s. 205318-1 - 205318-8 ISSN 0163-1829 R&D Projects: GA ČR GA202/01/0754 Institutional research plan: CEZ:AV0Z1010914 Keywords : magnetoresistance * short-period superlattices * two-dimensional electron gas Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 3.327, year: 2002

  9. The non-proliferation experiment and gas sampling as an on-site inspection activity: A progress report

    International Nuclear Information System (INIS)

    Carrigan, C.R.

    1994-03-01

    The Non-proliferation Experiment (NPE) is contributing to the development of gas sampling methods and models that may be incorporated into future on-site inspection (OSI) activities. Surface gas sampling and analysis, motivated by nuclear test containment studies, have already demonstrated the tendency for the gaseous products of an underground nuclear test to flow hundreds of meters to the surface over periods ranging from days to months. Even in the presence of a uniform sinusoidal pressure variation, there will be a net flow of cavity gas toward the surface. To test this barometric pumping effect at Rainier Mesa, gas bottles containing sulfur hexaflouride and 3 He were added to the pre-detonation cavity for the 1 kt chemical explosives test. Pre-detonation measurements of the background levels of both gases were obtained at selected sites on top of the mesa. The background levels of both tracers were found to be at or below mass spectrographic/gas chromatographic sensitivity thresholds in the parts-per-trillion range. Post-detonation, gas chromatographic analyses of samples taken during barometric pressure lows from the sampling sites on the mesa indicate the presence of significant levels (300--600 ppt) of sulfur hexaflouride. However, mass spectrographic analyses of gas samples taken to date do not show the presence of 3 He. To explain these observations, several possibilities are being explored through additional sampling/analysis and numerical modeling. For the NPE, the detonation point was approximately 400 m beneath the surface of Rainier Mesa and the event did not produce significant fracturing or subsidence on the surface of the mesa. Thus, the NPE may ultimately represent an extreme, but useful example for the application and tuning of cavity gas detection techniques

  10. Values Education in Ottoman Empire in the Second Constitutional Period: A Sample Lesson

    Science.gov (United States)

    Oruc, Sahin; Ilhan, Genc Osman

    2015-01-01

    Values education holds a significant place in an education environment and many studies are carried out about this new subject area. The aim of this study is to define how the subject of "values education" is handled in a sample lesson designed in the period of Constitution II in the Ottoman Empire. In this study, the lesson plan in the…

  11. Draft evaluation of the frequency for gas sampling for the high burnup confirmatory data project

    Energy Technology Data Exchange (ETDEWEB)

    Stockman, Christine T. [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States); Alsaed, Halim A. [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States); Bryan, Charles R. [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)

    2015-03-26

    This report fulfills the M3 milestone M3FT-15SN0802041, “Draft Evaluation of the Frequency for Gas Sampling for the High Burn-up Storage Demonstration Project” under Work Package FT-15SN080204, “ST Field Demonstration Support – SNL”. This report provides a technically based gas sampling frequency strategy for the High Burnup (HBU) Confirmatory Data Project. The evaluation of: 1) the types and magnitudes of gases that could be present in the project cask and, 2) the degradation mechanisms that could change gas compositions culminates in an adaptive gas sampling frequency strategy. This adaptive strategy is compared against the sampling frequency that has been developed based on operational considerations. Gas sampling will provide information on the presence of residual water (and byproducts associated with its reactions and decomposition) and breach of cladding, which could inform the decision of when to open the project cask.

  12. On-line sample treatment - Capillary gas chromatography

    NARCIS (Netherlands)

    Goosens, EC; de Jong, D; de Jong, GJ; Brinkman, UAT

    Sample pretreatment is often the bottleneck of a trace level analytical procedure. In order to increase performance, increasing attention is therefore being devoted to combining sample pretreatment on-line with the separation technique that has to be used. In the present review, a variety of

  13. Revisiting random walk based sampling in networks: evasion of burn-in period and frequent regenerations.

    Science.gov (United States)

    Avrachenkov, Konstantin; Borkar, Vivek S; Kadavankandy, Arun; Sreedharan, Jithin K

    2018-01-01

    In the framework of network sampling, random walk (RW) based estimation techniques provide many pragmatic solutions while uncovering the unknown network as little as possible. Despite several theoretical advances in this area, RW based sampling techniques usually make a strong assumption that the samples are in stationary regime, and hence are impelled to leave out the samples collected during the burn-in period. This work proposes two sampling schemes without burn-in time constraint to estimate the average of an arbitrary function defined on the network nodes, for example, the average age of users in a social network. The central idea of the algorithms lies in exploiting regeneration of RWs at revisits to an aggregated super-node or to a set of nodes, and in strategies to enhance the frequency of such regenerations either by contracting the graph or by making the hitting set larger. Our first algorithm, which is based on reinforcement learning (RL), uses stochastic approximation to derive an estimator. This method can be seen as intermediate between purely stochastic Markov chain Monte Carlo iterations and deterministic relative value iterations. The second algorithm, which we call the Ratio with Tours (RT)-estimator, is a modified form of respondent-driven sampling (RDS) that accommodates the idea of regeneration. We study the methods via simulations on real networks. We observe that the trajectories of RL-estimator are much more stable than those of standard random walk based estimation procedures, and its error performance is comparable to that of respondent-driven sampling (RDS) which has a smaller asymptotic variance than many other estimators. Simulation studies also show that the mean squared error of RT-estimator decays much faster than that of RDS with time. The newly developed RW based estimators (RL- and RT-estimators) allow to avoid burn-in period, provide better control of stability along the sample path, and overall reduce the estimation time. Our

  14. Estimating the residential demand function for natural gas in Seoul with correction for sample selection bias

    International Nuclear Information System (INIS)

    Yoo, Seung-Hoon; Lim, Hea-Jin; Kwak, Seung-Jun

    2009-01-01

    Over the last twenty years, the consumption of natural gas in Korea has increased dramatically. This increase has mainly resulted from the rise of consumption in the residential sector. The main objective of the study is to estimate households' demand function for natural gas by applying a sample selection model using data from a survey of households in Seoul. The results show that there exists a selection bias in the sample and that failure to correct for sample selection bias distorts the mean estimate, of the demand for natural gas, downward by 48.1%. In addition, according to the estimation results, the size of the house, the dummy variable for dwelling in an apartment, the dummy variable for having a bed in an inner room, and the household's income all have positive relationships with the demand for natural gas. On the other hand, the size of the family and the price of gas negatively contribute to the demand for natural gas. (author)

  15. Comparing and contrasting Holocene and Eemian warm periods with greenhouse-gas-induced warming

    International Nuclear Information System (INIS)

    MacCracken, M.C.; Kutzbach, J.

    1990-01-01

    Periods of the past that are estimated to have been warmer than present are of great potential interest for comparison with simulations of future climates associated with greenhouse-gas-induced warming. Certain features of the climates of the mid-Holocene and Eemian periods, both interglacial maxima, are described. The simulated climatic responses to both types of forcing, in terms of land/ocean and latitudinal averages, are also compared. The zonal average and annual (or seasonal) average radiation fluxes associated with the different-from-present orbital conditions that existed for those interglacials are compared to the radiation flux associated with CO 2 -induced warming. There are some similarities but also significant differences in the two types of radiation flux perturbations, and there are both similarities and differences in the simulated climatic responses

  16. Data compilation report: Gas and liquid samples from K West Basin fuel storage canisters

    International Nuclear Information System (INIS)

    Trimble, D.J.

    1995-01-01

    Forty-one gas and liquid samples were taken from spent fuel storage canisters in the K West Basin during a March 1995 sampling campaign. (Spent fuel from the N Reactor is stored in sealed canisters at the bottom of the K West Basin.) A description of the sampling process, gamma energy analysis data, and quantitative gas mass spectroscopy data are documented. This documentation does not include data analysis

  17. 40 CFR 86.509-90 - Exhaust gas sampling system.

    Science.gov (United States)

    2010-07-01

    ... have an accuracy and precision of ±1 °C (1.8 °F). (3) The pressure gauges shall have an accuracy and... of the test by more than ±5 percent. (The volumetric sample flow rate shall be varied inversely with...

  18. A novel method for fission product noble gas sampling

    International Nuclear Information System (INIS)

    Jain, S.K.; Prakash, Vivek; Singh, G.K.; Vinay, Kr.; Awsthi, A.; Bihari, K.; Joyson, R.; Manu, K.; Gupta, Ashok

    2008-01-01

    Noble gases occur to some extent in the Earth's atmosphere, but the concentrations of all but argon are exceedingly low. Argon is plentiful, constituting almost 1 % of the air. Fission Product Noble Gases (FPNG) are produced by nuclear fission and large parts of FPNG is produced in Nuclear reactions. FPNG are b-j emitters and contributing significantly in public dose. During normal operation of reactor release of FPNG is negligible but its release increases in case of fuel failure. Xenon, a member of FPNG family helps in identification of fuel failure and its extent in PHWRs. Due to above reasons it becomes necessary to assess the FPNG release during operation of NPPs. Presently used methodology of assessment of FPNG, at almost all power stations is Computer based gamma ray spectrometry. This provides fission product Noble gases nuclide identification through peak search of spectra. The air sample for the same is collected by grab sampling method, which has inherent disadvantages. An alternate method was developed at Rajasthan Atomic Power Station (RAPS) - 3 and 4 for assessment of FPNG, which uses adsorption phenomena for collection of air samples. This report presents details of sampling method for FPNG and noble gases in different systems of Nuclear Power Plant. (author)

  19. Computer automated mass spectrometer for isotope analysis on gas samples

    International Nuclear Information System (INIS)

    Pamula, A.; Kaucsar, M.; Fatu, C.; Ursu, D.; Vonica, D.; Bendea, D.; Muntean, F.

    1998-01-01

    A low resolution, high precision instrument was designed and realized in the mass spectrometry laboratory of the Institute of Isotopic and Molecular Technology, Cluj-Napoca. The paper presents the vacuum system, the sample inlet system, the ion source, the magnetic analyzer and the ion collector. The instrument is almost completely automated. There are described the analog-to-digital conversion circuits, the local control microcomputer, the automation systems and the performance checking. (authors)

  20. Dissociation behavior of pellet shaped mixed gas hydrate samples that contain propane as a guest

    International Nuclear Information System (INIS)

    Kawamura, Taro; Sakamoto, Yasuhide; Ohtake, Michika; Yamamoto, Yoshitaka; Komai, Takeshi; Haneda, Hironori; Yoon, Ji-Ho; Ohga, Kotaro

    2006-01-01

    The dissociation kinetics of mixed gas hydrates that contain propane as a guest molecule have been investigated. The mixed gas hydrates used in this work were artificially prepared using the binary gas mixture of methane-propane and the ternary gas mixture of methane-ethane-propane. The crystal structures and the guest compositions of the mixed hydrates were clearly identified by using Raman spectroscopy and gas chromatography. The dissociation rates of the gas hydrates observed under several isothermal and isobaric conditions were discussed with an analytical model. The isobaric conditions were achieved by pressurizing with mixed gases using buffer cylinders, which had similar compositions to those of the initial gases used for synthesizing each hydrate sample. Interestingly, the calculated result agreed well with the experimentally observed results only when the composition of the vapor phase was assumed to be identical with that of the hydrate phase instead of the bulk (equilibrium) gas composition

  1. Studies on radioimmunoassay diagnosis of cow pregnancy at an early period by milk sample communication

    International Nuclear Information System (INIS)

    Wu Meiwen

    1986-01-01

    Cow pregancy was diagnosed at an early period by milk sample communication and radioimmunoassay (RIA). Liquid milk samples were converted into solid forms on filter paper and mailed to the laboratory from appointed locations, and concentrations of progesterone in milk samples were then determined by RIA method. Milks were sampled 19 and 23 days after mating. Criterion used for the judgement of cow pregnancy was as follows: When the progesterone content in milk was 5 ng/ml or less, the cow was not pregnant; when progesterone content was between 5-11 ng/ml, it was doubtful; when progesterone content was 11 ng/ml or more, it was pregnant. According to this criterion, among 215 cows, 131 were pregnant, 73 were not pregnant, and 11 were doubtful. The results were further checked by palpation 3 months after inseminations. The unpregnancy and pregnancy accuracies were 97.6% and 89.2%, respectively. Forther milk samples were collected on 44 days for above cows that had been diagnosed on 19 and 23 days showing pregnancy to diagnose embryo forming. Among 91 cows, 74 had embryo. 7 had none, and the other 10 were doubtful. The embryo and unembryo accuracies were 94.6% and 100% respectively checking by palpation 3 months after inseminations

  2. One-Way Flow of a Rarefied Gas Induced in a Circular Pipe with a Periodic Temperature Distribution

    National Research Council Canada - National Science Library

    Aoki, K

    2000-01-01

    The steady behavior of a rarefied gas in a circular pipe with a saw-like temperature distribution increasing and decreasing periodically in the direction of the pipe axis is investigated numerically...

  3. Measuring modulated luminescence using non-modulated stimulation: Ramping the sample period

    DEFF Research Database (Denmark)

    Poolton, N.R.J.; Bøtter-Jensen, L.; Andersen, C.E.

    2003-01-01

    . Directly analogous results to LM-OSL can, however, be achieved with non-modulated excitation sources, by ramping the sample period (RSP) of luminescence detection. RSP-OSL has the distinct advantage over LM-OSL in that, since the excitation remains at full power, data accumulation times (that can...... be considerable) can be reduced by typically 50%. RSP methods are universally applicable and can be employed, for example, where the excitation source is constant heat, rather than light: here, iso-thermal decay of phosphorescence becomes recorded as a sequence of peaks, corresponding to de-trapping of charge...

  4. Off-Gas Analysis During the Vitrification of Hanford Radioactive Waste Samples

    International Nuclear Information System (INIS)

    Ha, B.C.; Ferrara, D.M.; Crawford, C.L.; Choi, A.S.; Bibler, N.E.

    1998-01-01

    This paper describes the off-gas analysis of samples collected during the radioactive vitrification experiments. Production and characterization of the Hanford waste-containing LAW and HAW glasses are presented in related reports from this conference

  5. Hazard categorization of 100 K West fuel canister gas and liquid sampling

    International Nuclear Information System (INIS)

    Alwardt, L.D.

    1994-01-01

    This report documents the determination that the activities associated with the 100 K West fuel canister gas and liquid sampling are classified as Hazard Category Other (consequences are below criteria for Category 3)

  6. GAS AND COAL EXTRACTIVE INDUSTRY DURING THE SOCIALIST INDUSTRIALIZATION PERIOD (1948-1989

    Directory of Open Access Journals (Sweden)

    MARIUS BULEARCA

    2015-12-01

    Full Text Available This article shows that since 1949 the extractive industry has undergone a strong process of restructuring when enterprises were nationalized and a strict control over all components of the economy was established. The new leadership of the country had the intention of developing the industrial sector as well, basically laying the foundations of the new Romanian economy where the industrial sector economy would bring considerable income. This program will lead to the development of the energy sector in Romania also, thus contributing to a great extent to the development and consolidation of coal and gas extraction. Despite of all the economic and social development achieved during the period 1950-1989, at the end of it, Romania ranked a marginal position in the European countries hierarchy since between its level of development and the market economy developed countries large gaps in respect to the main economic and social indicators occurred.

  7. Unreviewed safety question evaluation of 100 K West fuel canister gas and liquid sampling

    International Nuclear Information System (INIS)

    Alwardt, L.D.

    1995-01-01

    The purpose of this report is to provide the basis for answers to an Unreviewed Safety Question (USQ) safety evaluation for the gas and liquid sampling activities associated with the fuel characterization program at the 100 K West (KW) fuel storage basin. The scope of this safety evaluation is limited to the movement of canisters between the main storage basin, weasel pit, and south loadout pit transfer channel (also known as the decapping station); gas and liquid sampling of fuel canisters in the weasel pit; mobile laboratory preliminary sample analysis in or near the 105 KW basin building; and the placement of sample containers in an approved shipping container. It was concluded that the activities and potential accident consequences associated with the gas and liquid sampling of 100 KW fuel canisters are bounded by the current safety basis documents and do not constitute an Unreviewed Safety Question

  8. 14CO2 analysis of soil gas: Evaluation of sample size limits and sampling devices

    Science.gov (United States)

    Wotte, Anja; Wischhöfer, Philipp; Wacker, Lukas; Rethemeyer, Janet

    2017-12-01

    Radiocarbon (14C) analysis of CO2 respired from soils or sediments is a valuable tool to identify different carbon sources. The collection and processing of the CO2, however, is challenging and prone to contamination. We thus continuously improve our handling procedures and present a refined method for the collection of even small amounts of CO2 in molecular sieve cartridges (MSCs) for accelerator mass spectrometry 14C analysis. Using a modified vacuum rig and an improved desorption procedure, we were able to increase the CO2 recovery from the MSC (95%) as well as the sample throughput compared to our previous study. By processing series of different sample size, we show that our MSCs can be used for CO2 samples of as small as 50 μg C. The contamination by exogenous carbon determined in these laboratory tests, was less than 2.0 μg C from fossil and less than 3.0 μg C from modern sources. Additionally, we tested two sampling devices for the collection of CO2 samples released from soils or sediments, including a respiration chamber and a depth sampler, which are connected to the MSC. We obtained a very promising, low process blank for the entire CO2 sampling and purification procedure of ∼0.004 F14C (equal to 44,000 yrs BP) and ∼0.003 F14C (equal to 47,000 yrs BP). In contrast to previous studies, we observed no isotopic fractionation towards lighter δ13C values during the passive sampling with the depth samplers.

  9. Thermal modeling of core sampling in flammable gas waste tanks. Part 1: Push-mode sampling

    International Nuclear Information System (INIS)

    Unal, C.; Stroh, K.; Pasamehmetoglu, K.O.

    1997-01-01

    The radioactive waste stored in underground storage tanks at Hanford site is routinely being sampled for waste characterization purposes. The push- and rotary-mode core sampling is one of the sampling methods employed. The waste includes mixtures of sodium nitrate and sodium nitrite with organic compounds that can produce violent exothermic reactions if heated above 160 C during core sampling. A self-propagating waste reaction would produce very high temperatures that eventually result in failure of the tank and radioactive material releases to environment. A two-dimensional thermal model based on a lumped finite volume analysis method is developed. The enthalpy of each node is calculated from the first law of thermodynamics. A flash temperature and effective contact area concept were introduced to account the interface temperature rise. No maximum temperature rise exceeding the critical value of 60 C was found in the cases studied for normal operating conditions. Several accident conditions are also examined. In these cases it was found that the maximum drill bit temperature remained below the critical reaction temperature as long as a 30 scfm purge flow is provided the push-mode drill bit during sampling in rotary mode. The failure to provide purge flow resulted in exceeding the limiting temperatures in a relatively short time

  10. Recent developments on field gas extraction and sample preparation methods for radiokrypton dating of groundwater

    Science.gov (United States)

    Yokochi, Reika

    2016-09-01

    Current and foreseen population growths will lead to an increased demand in freshwater, large quantities of which is stored as groundwater. The ventilation age is crucial to the assessment of groundwater resources, complementing the hydrological model approach based on hydrogeological parameters. Ultra-trace radioactive isotopes of Kr (81 Kr and 85 Kr) possess the ideal physical and chemical properties for groundwater dating. The recent advent of atom trap trace analyses (ATTA) has enabled determination of ultra-trace noble gas radioisotope abundances using 5-10 μ L of pure Kr. Anticipated developments will enable ATTA to analyze radiokrypton isotope abundances at high sample throughput, which necessitates simple and efficient sample preparation techniques that are adaptable to various sample chemistries. Recent developments of field gas extraction devices and simple and rapid Kr separation method at the University of Chicago are presented herein. Two field gas extraction devices optimized for different sampling conditions were recently designed and constructed, aiming at operational simplicity and portability. A newly developed Kr purification system enriches Kr by flowing a sample gas through a moderately cooled (138 K) activated charcoal column, followed by a gentle fractionating desorption. This simple process uses a single adsorbent and separates 99% of the bulk atmospheric gases from Kr without significant loss. The subsequent two stages of gas chromatographic separation and a hot Ti sponge getter further purify the Kr-enriched gas. Abundant CH4 necessitates multiple passages through one of the gas chromatographic separation columns. The presented Kr separation system has a demonstrated capability of extracting Kr with > 90% yield and 99% purity within 75 min from 1.2 to 26.8 L STP of atmospheric air with various concentrations of CH4. The apparatuses have successfully been deployed for sampling in the field and purification of groundwater samples.

  11. Method to make accurate concentration and isotopic measurements for small gas samples

    Science.gov (United States)

    Palmer, M. R.; Wahl, E.; Cunningham, K. L.

    2013-12-01

    Carbon isotopic ratio measurements of CO2 and CH4 provide valuable insight into carbon cycle processes. However, many of these studies, like soil gas, soil flux, and water head space experiments, provide very small gas sample volumes, too small for direct measurement by current constant-flow Cavity Ring-Down (CRDS) isotopic analyzers. Previously, we addressed this issue by developing a sample introduction module which enabled the isotopic ratio measurement of 40ml samples or smaller. However, the system, called the Small Sample Isotope Module (SSIM), does dilute the sample during the delivery with inert carrier gas which causes a ~5% reduction in concentration. The isotopic ratio measurements are not affected by this small dilution, but researchers are naturally interested accurate concentration measurements. We present the accuracy and precision of a new method of using this delivery module which we call 'double injection.' Two portions of the 40ml of the sample (20ml each) are introduced to the analyzer, the first injection of which flushes out the diluting gas and the second injection is measured. The accuracy of this new method is demonstrated by comparing the concentration and isotopic ratio measurements for a gas sampled directly and that same gas measured through the SSIM. The data show that the CO2 concentration measurements were the same within instrument precision. The isotopic ratio precision (1σ) of repeated measurements was 0.16 permil for CO2 and 1.15 permil for CH4 at ambient concentrations. This new method provides a significant enhancement in the information provided by small samples.

  12. Short-period volcanic gas precursors to phreatic eruptions: Insights from Poás Volcano, Costa Rica

    Science.gov (United States)

    de Moor, Maarten; Aiuppa, Alessandro; Pacheco, Javier; Avard, Geoffroy; Kern, Christoph; Liuzzo, Marco; Martinez, Maria; Giudice, Gaetano; Fischer, Tobias P.

    2016-01-01

    Volcanic eruptions involving interaction with water are amongst the most violent and unpredictable geologic phenomena on Earth. Phreatic eruptions are exceptionally difficult to forecast by traditional geophysical techniques. Here we report on short-term precursory variations in gas emissions related to phreatic blasts at Poás volcano, Costa Rica, as measured with an in situ multiple gas analyzer that was deployed at the edge of the erupting lake. Gas emitted from this hyper-acid crater lake approaches magmatic values of SO2/CO2 1–6 days prior to eruption. The SO2 flux derived from magmatic degassing through the lake is measureable by differential optical absorption spectrometry (sporadic campaign measurements), which allows us to constrain lake gas output and input for the major gas species during eruptive and non-eruptive periods. We can further calculate power supply to the hydrothermal system using volatile mass balance and thermodynamics, which indicates that the magmatic heat flux into the shallow hydrothermal system increases from ∼27 MW during quiescence to ∼59 MW during periods of phreatic events. These transient pulses of gas and heat from the deeper magmatic system generate both phreatic eruptions and the observed short-term changes in gas composition, because at high gas flux scrubbing of sulfur by the hydrothermal system is both kinetically and thermodynamically inhibited whereas CO2gas is always essentially inert in hyperacid conditions. Thus, the SO2/CO2 of lake emissions approaches magmatic values as gas and power supply to the sub-limnic hydrothermal system increase, vaporizing fluids and priming the hydrothermal system for eruption. Our results suggest that high-frequency real-time gas monitoring could provide useful short-term eruptive precursors at volcanoes prone to phreatic explosions.

  13. Concurrent Lactic and Volatile Fatty Acid Analysis of Microbial Fermentation Samples by Gas Chromatography with Heat Pre-treatment.

    Science.gov (United States)

    Darwin; WipaCharles; Cord-Ruwisch, Ralf

    2018-01-01

    Organic acid analysis of fermentation samples can be readily achieved by gas chromatography (GC), which detects volatile organic acids. However, lactic acid, a key fermentation acid is non-volatile and can hence not be quantified by regular GC analysis. However the addition of periodic acid to organic acid samples has been shown to enable lactic acid analysis by GC, as periodic acid oxidizes lactic acid to the volatile acetaldehyde. Direct GC injection of lactic acid standards and periodic acid generated inconsistent and irreproducible peaks, possibly due to incomplete lactic acid oxidation to acetaldehyde. The described method is developed to improve lactic acid analysis by GC by using a heat treated derivatization pre-treatment, such that it becomes independent of the retention time and temperature selection of the GC injector. Samples containing lactic acid were amended by periodic acid and heated in a sealed test tube at 100°C for at least 45 min before injecting it to the GC. Reproducible and consistent peaks of acetaldehyde were obtained. Simultaneous determination of lactic acid, acetone, ethanol, butanol, volatile fatty acids could also be accomplished by applying this GC method, enabling precise and convenient organic acid analysis of biological samples such as anaerobic digestion and fermentation processes. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  14. Natural gas to start long period of growth during next 3 years

    International Nuclear Information System (INIS)

    Anon.

    1993-01-01

    Pressures are building worldwide to increase consumption of natural gas. During the past decade, worldwide marketed production of natural gas has moved up much faster than oil and coal production. Gas output increased from 51.8 tcf in 1982 to 72.1 tcf in 1992. This 39.2% production increase compares with gains of 13.7% for oil and 15.2% for coal. The natural gas share of worldwide energy consumption moved up from 20.1% in 1982 to 22.8% in 1992. The biggest change was in the C.I.S. and East Europe, where the gas share of total energy use rose from 28.8% in 1982 to 41.3% in 1992. In the OECD, the gas share of total energy use rose from 21.1% in 1982 to 21.5% in 1992. The natural gas industry was well-developed by 1982 in many industrial countries. In the developing world, gas provided 10.4% of total energy in 1982 and 12.5% in 1992. The paper discusses production trends, gas trade trends, natural gas prices, gas reserves, drilling shifts, and the demand outlook

  15. NG09 And CTBT On-Site Inspection Noble Gas Sampling and Analysis Requirements

    Science.gov (United States)

    Carrigan, Charles R.; Tanaka, Junichi

    2010-05-01

    A provision of the Comprehensive Test Ban Treaty (CTBT) allows on-site inspections (OSIs) of suspect nuclear sites to determine if the occurrence of a detected event is nuclear in origin. For an underground nuclear explosion (UNE), the potential success of an OSI depends significantly on the containment scenario of the alleged event as well as the application of air and soil-gas radionuclide sampling techniques in a manner that takes into account both the suspect site geology and the gas transport physics. UNE scenarios may be broadly divided into categories involving the level of containment. The simplest to detect is a UNE that vents a significant portion of its radionuclide inventory and is readily detectable at distance by the International Monitoring System (IMS). The most well contained subsurface events will only be detectable during an OSI. In such cases, 37 Ar and radioactive xenon cavity gases may reach the surface through either "micro-seepage" or the barometric pumping process and only the careful siting of sampling locations, timing of sampling and application of the most site-appropriate atmospheric and soil-gas capturing methods will result in a confirmatory signal. The OSI noble gas field tests NG09 was recently held in Stupava, Slovakia to consider, in addition to other field sampling and analysis techniques, drilling and subsurface noble gas extraction methods that might be applied during an OSI. One of the experiments focused on challenges to soil-gas sampling near the soil-atmosphere interface. During withdrawal of soil gas from shallow, subsurface sample points, atmospheric dilution of the sample and the potential for introduction of unwanted atmospheric gases were considered. Tests were designed to evaluate surface infiltration and the ability of inflatable well-packers to seal out atmospheric gases during sample acquisition. We discuss these tests along with some model-based predictions regarding infiltration under different near

  16. Gas and liquid sampling for closed canisters in KW Basin - Work Plan

    International Nuclear Information System (INIS)

    Pitkoff, C.C.

    1995-01-01

    Work Plan for the design and fabrication of gas/liquid sampler for closed canister sampling in KW Basin. This document defines the tasks associated with the design, fabrication, assembly, and acceptance testing equipment necessary for gas and liquid sampling of the Mark I and Mark II canisters in the K-West basin. The sampling of the gas space and the remaining liquid inside the closed canisters will be used to help understand any changes to the fuel elements and the canisters. Specifically, this work plan will define the scope of work and required task structure, list the technical requirements, describe design configuration control and verification methodologies, detail quality assurance requirements, and present a baseline estimate and schedule

  17. [Recent advances in analysis of petroleum geological samples by comprehensive two-dimensional gas chromatography].

    Science.gov (United States)

    Gao, Xuanbo; Chang, Zhenyang; Dai, Wei; Tong, Ting; Zhang, Wanfeng; He, Sheng; Zhu, Shukui

    2014-10-01

    Abundant geochemical information can be acquired by analyzing the chemical compositions of petroleum geological samples. The information obtained from the analysis provides scientifical evidences for petroleum exploration. However, these samples are complicated and can be easily influenced by physical (e. g. evaporation, emulsification, natural dispersion, dissolution and sorption), chemical (photodegradation) and biological (mainly microbial degradation) weathering processes. Therefore, it is very difficult to analyze the petroleum geological samples and they cannot be effectively separated by traditional gas chromatography/mass spectrometry. A newly developed separation technique, comprehensive two-dimensional gas chromatography (GC x GC), has unique advantages in complex sample analysis, and recently it has been applied to petroleum geological samples. This article mainly reviews the research progres- ses in the last five years, the main problems and the future research about GC x GC applied in the area of petroleum geology.

  18. Six-month low level chlorine dioxide gas inhalation toxicity study with two-week recovery period in rats

    Directory of Open Access Journals (Sweden)

    Akamatsu Akinori

    2012-02-01

    Full Text Available Abstract Background Chlorine dioxide (CD gas has a potent antimicrobial activity at extremely low concentration and may serve as a new tool for infection control occupationally as well as publicly. However, it remains unknown whether the chronic exposure of CD gas concentration effective against microbes is safe. Therefore, long-term, low concentration CD gas inhalation toxicity was studied in rats as a six-month continuous whole-body exposure followed by a two-week recovery period, so as to prove that the CD gas exposed up to 0.1 ppm (volume ratio is judged as safe on the basis of a battery of toxicological examinations. Methods CD gas at 0.05 ppm or 0.1 ppm for 24 hours/day and 7 days/week was exposed to rats for 6 months under an unrestrained condition with free access to chow and water in a chamber so as to simulate the ordinary lifestyle in human. The control animals were exposed to air only. During the study period, the body weight as well as the food and water consumptions were recorded. After the 6-month exposure and the 2-week recovery period, animals were sacrificed and a battery of toxicological examinations, including biochemistry, hematology, necropsy, organ weights and histopathology, were performed. Results Well regulated levels of CD gas were exposed throughout the chamber over the entire study period. No CD gas-related toxicity sign was observed during the whole study period. No significant difference was observed in body weight gain, food and water consumptions, and relative organ weight. In biochemistry and hematology examinations, changes did not appear to be related to CD gas toxicity. In necropsy and histopathology, no CD gas-related toxicity was observed even in expected target respiratory organs. Conclusions CD gas up to 0.1 ppm, exceeding the level effective against microbes, exposed to whole body in rats continuously for six months was not toxic, under a condition simulating the conventional lifestyle in human.

  19. Thermal modeling of core sampling in flammable gas waste tanks. Part 2: Rotary-mode sampling

    International Nuclear Information System (INIS)

    Unal, C.; Poston, D.; Pasamehmetoglu, K.O.; Witwer, K.S.

    1997-01-01

    The radioactive waste stored in underground storage tanks at Hanford site includes mixtures of sodium nitrate and sodium nitrite with organic compounds. The waste can produce undesired violent exothermic reactions when heated locally during the rotary-mode sampling. Experiments are performed varying the downward force at a maximum rotational speed of 55 rpm and minimum nitrogen purge flow of 30 scfm. The rotary drill bit teeth-face temperatures are measured. The waste is simulated with a low thermal conductivity hard material, pumice blocks. A torque meter is used to determine the energy provided to the drill string. The exhaust air-chip temperature as well as drill string and drill bit temperatures and other key operating parameters were recorded. A two-dimensional thermal model is developed. The safe operating conditions were determined for normal operating conditions. A downward force of 750 at 55 rpm and 30 scfm nitrogen purge flow was found to yield acceptable substrate temperatures. The model predicted experimental results reasonably well. Therefore, it could be used to simulate abnormal conditions to develop procedures for safe operations

  20. Semi-annual report for the unconventional gas recovery program, period ending September 30, 1980

    Energy Technology Data Exchange (ETDEWEB)

    Manilla, R.D. (ed.)

    1980-11-01

    Progress is reported in research on methane recovery from coalbeds, eastern gas shales, western gas sands, and geopressured aquifers. In the methane from coalbeds project, data on information evaluation and management, resource and site assessment and characterization, model development, instrumentation, basic research, and production technology development are reported. In the methane from eastern gas shales project, data on resource characterization and inventory, extraction technology, and technology testing and verification are presented. In the western gas sands project, data on resource assessments, field tests and demonstrations and project management are reported. In the methane from geopressured aquifers project, data on resource assessment, supporting research, field tests and demonstrations, and technology transfer are reported.

  1. Groundwater-quality data in 12 GAMA study units: Results from the 2006–10 initial sampling period and the 2008–13 trend sampling period, California GAMA Priority Basin Project

    Science.gov (United States)

    Mathany, Timothy M.

    2017-03-09

    The Priority Basin Project (PBP) of the Groundwater Ambient Monitoring and Assessment (GAMA) program was developed in response to the Groundwater Quality Monitoring Act of 2001 and is being conducted by the U.S. Geological Survey in cooperation with the California State Water Resources Control Board. From 2004 through 2012, the GAMA-PBP collected samples and assessed the quality of groundwater resources that supply public drinking water in 35 study units across the State. Selected sites in each study unit were sampled again approximately 3 years after initial sampling as part of an assessment of temporal trends in water quality by the GAMA-PBP. Twelve of the study units, initially sampled during 2006–11 (initial sampling period) and sampled a second time during 2008–13 (trend sampling period) to assess temporal trends, are the subject of this report.The initial sampling was designed to provide a spatially unbiased assessment of the quality of untreated groundwater used for public water supplies in the 12 study units. In these study units, 550 sampling sites were selected by using a spatially distributed, randomized, grid-based method to provide spatially unbiased representation of the areas assessed (grid sites, also called “status sites”). After the initial sampling period, 76 of the previously sampled status sites (approximately 10 percent in each study unit) were randomly selected for trend sampling (“trend sites”). The 12 study units sampled both during the initial sampling and during the trend sampling period were distributed among 6 hydrogeologic provinces: Coastal (Northern and Southern), Transverse Ranges and Selected Peninsular Ranges, Klamath, Modoc Plateau and Cascades, and Sierra Nevada Hydrogeologic Provinces. For the purposes of this trend report, the six hydrogeologic provinces were grouped into two hydrogeologic regions based on location: Coastal and Mountain.The groundwater samples were analyzed for a number of synthetic organic

  2. Greenhouse gas emissions in Europe: a retrospective trend analysis for the period 1990-2008

    Energy Technology Data Exchange (ETDEWEB)

    Borgan, A.; Gugele, B.; Haider, S. (Umweltbundesamt, Vienna (Austria)) (and others)

    2011-10-15

    This report presents a retrospective overview of the greenhouse gas (GHG) emission trends in Europe from 1990 to 2008, with a particular focus on the underpinning drivers and the influence of EU policies. The analysis is based on the combination of decomposition analyses to identify the respective influence of each identified driver and an overview of the main EU policies and their likely effects on these drivers. The period covered by the analysis stops in 2008. As a result, the analysis avoids the effects of the recent economic crisis on GHG emissions. This reinforces the conclusion on long-term emission drivers. The report covers the EU-27 and presents results for the other EEA member countries (Iceland, Liechtenstein, Norway, Switzerland and Turkey) and Croatia (EU candidate country together with Turkey) as far as data is available. The results can be summarized as: 1) Overall GHG emission trends. EU GHG emissions were reduced between 1990 and 2008. Most of the reductions took place in the 1990s, but emissions have also been decreasing every year from 2003 until the last year considered in this report, 2008. 2) Predominant drivers. For the most part, the GHG emission trends observed in the EU between 1990 and 2008 resulted from economic factors. However, EU policies, some of which were not directly targeting GHG emissions, as well as national policies by some front runner countries, also played a role in these trends. 3) Impacts of EU policies. Between 2000 and 2008, emission trends were more directly targeted by a range of energy and climate policies, e.g. the implementation of the European Climate Change programme. However, the steady increase in energy demand during this period - particularly electricity - outweighed the considerable EU-wide savings generated by energy efficiency improvements and the development of renewable energy. 4) Co-benefits. Taking example from the positive benefits on GHG emissions that resulted from the implementation of non

  3. Use of the Keele injector for sample introduction for gas chromatographic analysis of vinclozolin in lettuces.

    Science.gov (United States)

    Shim, J H; Lee, Y S; Kim, M R; Lee, C J; Kim, I S

    2003-10-10

    We examined a Keele injector for sample introduction for gas chromatographic analysis of vinclozolin treated in lettuces. Samples in milligram quantity were introduced into a glass tube in a Keele injector at a gas chromatograph injection port. The glass tube was then crushed to allow the sample to carry onto a capillary column in a normal manner. The standard calibration curve for quantitative detection of vinclozolin was obtained by determining vinclozolin spiked in samples at variable concentrations. The calibration curve showed a linear response to vinclozolin ranging from 0.05 to 1.0 microg/g, giving a slope value of 174.8, the y-intercept value of -2.8146 and the mean r2-value of 0.9994. Limit of quantification for vinclozolin was 0.05 microg/g by this method, comparable to 0.01 microg/g by a normal injector. When samples treated previously with vinclozolin were determined by the Keele injector, vinclozolin was found to be about 30% lower as compared to a normal method, suggesting about 70% recovery of the spiked vinclozolin by the Keele injector. From these results, the Keele injector was suggested to be potential for sample introduction in gas chromatographic analysis of vinclozolin in lettuce samples.

  4. Critique of Hanford Waste Vitrification Plant off-gas sampling requirements

    International Nuclear Information System (INIS)

    Goles, R.W.

    1996-03-01

    Off-gas sampling and monitoring activities needed to support operations safety, process control, waste form qualification, and environmental protection requirements of the Hanford Waste Vitrification Plant (HWVP) have been evaluated. The locations of necessary sampling sites have been identified on the basis of plant requirements, and the applicability of Defense Waste Processing Facility (DWPF) reference sampling equipment to these HWVP requirements has been assessed for all sampling sites. Equipment deficiencies, if present, have been described and the bases for modifications and/or alternative approaches have been developed

  5. Optimal sampling period of the digital control system for the nuclear power plant steam generator water level control

    International Nuclear Information System (INIS)

    Hur, Woo Sung; Seong, Poong Hyun

    1995-01-01

    A great effort has been made to improve the nuclear plant control system by use of digital technologies and a long term schedule for the control system upgrade has been prepared with an aim to implementation in the next generation nuclear plants. In case of digital control system, it is important to decide the sampling period for analysis and design of the system, because the performance and the stability of a digital control system depend on the value of the sampling period of the digital control system. There is, however, currently no systematic method used universally for determining the sampling period of the digital control system. Generally, a traditional way to select the sampling frequency is to use 20 to 30 times the bandwidth of the analog control system which has the same system configuration and parameters as the digital one. In this paper, a new method to select the sampling period is suggested which takes into account of the performance as well as the stability of the digital control system. By use of the Irving's model steam generator, the optimal sampling period of an assumptive digital control system for steam generator level control is estimated and is actually verified in the digital control simulation system for Kori-2 nuclear power plant steam generator level control. Consequently, we conclude the optimal sampling period of the digital control system for Kori-2 nuclear power plant steam generator level control is 1 second for all power ranges. 7 figs., 3 tabs., 8 refs. (Author)

  6. Sample collection and preparation of biofluids and extracts for gas chromatography-mass spectrometry.

    Science.gov (United States)

    Emwas, Abdul-Hamid M; Al-Talla, Zeyad A; Kharbatia, Najeh M

    2015-01-01

    To maximize the utility of gas chromatography-mass spectrometry (GC-MS) in metabonomics research, all stages of the experimental design should be standardized, including sample collection, storage, preparation, and sample separation. Moreover, the prerequisite for any GC-MS analysis is that a compound must be volatile and thermally stable if it is to be analyzed using this technique. Since many metabolites are nonvolatile and polar in nature, they are not readily amenable to analysis by GC-MS and require initial chemical derivatization of the polar functional groups in order to reduce the polarity and to increase the thermal stability and volatility of the analytes. In this chapter, an overview is presented of the optimum approach to sample collection, storage, and preparation for gas chromatography-mass spectrometry-based metabonomics with particular focus on urine samples as example of biofluids.

  7. Irradiation test of HAFM and tag gas samples at the standard neutron field of 'YAYOI'

    International Nuclear Information System (INIS)

    Iguchi, Tetsuo

    1997-03-01

    To check the accuracy of helium accumulation neutron fluence monitors (HAFM) as new technique for fast reactor neutron dosimetry and the applicability of tag gas activation analysis to fast reactor failed fuel detection, their samples were irradiated at the standard neutron field of the fast neutron source reactor 'YAYOI' (Nuclear Engineering Research Laboratory, University of Tokyo). Since October in 1996, the HAFM samples such as 93% enriched boron (B) powders of 1 mg and natural B powders of 10 mg contained in vanadium (V) capsule were intermittently irradiated at the reactor core center (Glory hole: Gy) and/or under the leakage neutron field from the reactor core (Fast column: FC). In addition, new V capsules filled with enriched B of 40 mg and Be of 100 mg, respectively, were put into an experimental hole through the blanket surrounding the core. These neutron fields were monitored by the activation foils consisting of Fe, Co, Ni, Au, 235 U, 237 Np etc., mainly to confirm the results obtained from 1995's preliminary works. In particular, neutron flux distributions in the vicinity of irradiated samples were measured in more detail. At the end of March in 1997, the irradiated neutron fluence have reached the goal necessary to produce the detectable number of He atoms more than ∼10 13 in each HAFM sample. Six kinds of tag gas samples, which are the mixed gases of isotopically adjusted Xe and Kr contained in SUS capsules, were separately irradiated three times at Gy under the neutron fluence of ∼10 16 n/cm 2 in average. After irradiation, γ-ray spectra were measured for each sample. Depending on the composition of tag gas mixtures, the different patterns of γ-ray peak spectra from 79 Kr, 125 Xe, etc. produced through tag gas activation were able to be clearly identified. These experimental data will be very useful for the benchmark test of tag gas activation calculation applied to the fast reactor failed fuel detection. (author)

  8. A pyrolysis/gas chromatographic method for the determination of hydrogen in solid samples

    Science.gov (United States)

    Carr, R. H.; Bustin, R.; Gibson, E. K.

    1987-01-01

    A method is described for the determination of hydrogen in solid samples. The sample is heated under vacuum after which the evolved gases are separated by gas chromatography with a helium ionization detector. The system is calibrated by injecting known amounts of hydrogen, as determined manometrically. The method, which is rapid and reliable, was checked for a variety of lunar soils; the limit of detection is about 10 ng of hydrogen.

  9. Gas-chromatographic quantitative determination of argon in air samples, by elimination of oxigen

    International Nuclear Information System (INIS)

    Sofronie, E.

    1982-08-01

    A method of gas-chromatographic quantitative determination of argon in air samples, by elimination of oxygen, is presented. Experiments were carried out in a static system. Conditions for the application of the method in dynamic systems are specified. Sensibility of the method: 5 10 -4 cm 3 Ar per cm 3 of air. (author)

  10. Tank 241-B-103 headspace gas and vapor characterization results for samples collected in February 1995

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-01-01

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

  11. Tank 241-BX-104 headspace gas and vapor characterization results for samples collected in December 1994

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-01-01

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

  12. Tank 241-U-203 headspace gas and vapor characterization results for samples collected in August 1995

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-09-01

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

  13. Tank 241-C-106 headspace gas and vapor characterization results for samples collected in February 1994

    International Nuclear Information System (INIS)

    Hackaby, J.L.; Bratzel, D.R.

    1995-01-01

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

  14. Tank 241-S-111 headspace gas and vapor characterization results for samples collected in March 1995

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-09-01

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

  15. Tank 241-U-103 headspace gas and vapor characterization results for samples collected in February 1995

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-01-01

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

  16. Tank 241-SX-106 headspace gas and vapor characterization results for samples collected in March 1995

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-09-01

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

  17. Tank 241-TX-105 headspace gas and vapor characterization results for samples collected in December 1995

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-01-01

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

  18. Tank 241-C-102 headspace gas and vapor characterization results for samples collected in August 1994

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-09-01

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

  19. Tank 241-BY-112 headspace gas and vapor characterization results for samples collected in November 1994

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-01-01

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

  20. Tank 241-T-111 headspace gas and vapor characterization results for samples collected in January 1995

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-09-01

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

  1. Tank 241-SX-103 headspace gas and vapor characterization results for samples collected in March 1995

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-09-01

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

  2. Tank 241-TY-104 headspace gas and vapor characterization results for samples collected in April 1995

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-09-01

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

  3. Tank 241-C-110 headspace gas and vapor characterization results for samples collected in August 1994

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-09-01

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

  4. Tank 241-C-101 headspace gas and vapor characterization results for samples collected in September 1994

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-09-01

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

  5. Tank 241-C-107 headspace gas and vapor characterization results for samples collected in September 1994

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-01-01

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

  6. Tank 241-C-104 headspace gas and vapor characterization results for samples collected in March 1994

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-01-01

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

  7. Hemoglobin in samples with leukocytosis can be measured on ABL 700 series blood gas analyzers

    NARCIS (Netherlands)

    Scharnhorst, V.; Laar, van der P.D.; Vader, H.

    2003-01-01

    To compare lactate, bilirubin and Hemoglobin F concentrations obtained on ABL 700 series blood gas analyzers with those from laboratory methods. Pooled neonatal plasma, cord blood and adult plasma samples were used for comparison of bilirubin, hemoglobin F and lactate concentrations respectively.

  8. Assessment of long-term gas sampling design at two commercial manure-belt layer barns.

    Science.gov (United States)

    Chai, Li-Long; Ni, Ji-Qin; Chen, Yan; Diehl, Claude A; Heber, Albert J; Lim, Teng T

    2010-06-01

    Understanding temporal and spatial variations of aerial pollutant concentrations is important for designing air quality monitoring systems. In long-term and continuous air quality monitoring in large livestock and poultry barns, these systems usually use location-shared analyzers and sensors and can only sample air at limited number of locations. To assess the validity of the gas sampling design at a commercial layer farm, a new methodology was developed to map pollutant gas concentrations using portable sensors under steady-state or quasi-steady-state barn conditions. Three assessment tests were conducted from December 2008 to February 2009 in two manure-belt layer barns. Each barn was 140.2 m long and 19.5 m wide and had 250,000 birds. Each test included four measurements of ammonia and carbon dioxide concentrations at 20 locations that covered all operating fans, including six of the fans used in the long-term sampling that represented three zones along the lengths of the barns, to generate data for complete-barn monitoring. To simulate the long-term monitoring, gas concentrations from the six long-term sampling locations were extracted from the 20 assessment locations. Statistical analyses were performed to test the variances (F-test) and sample means (t test) between the 6- and 20-sample data. The study clearly demonstrated ammonia and carbon dioxide concentration gradients that were characterized by increasing concentrations from the west to east ends of the barns following the under-cage manure-belt travel direction. Mean concentrations increased from 7.1 to 47.7 parts per million (ppm) for ammonia and from 2303 to 3454 ppm for carbon dioxide from the west to east of the barns. Variations of mean gas concentrations were much less apparent between the south and north sides of the barns, because they were 21.2 and 20.9 ppm for ammonia and 2979 and 2951 ppm for carbon dioxide, respectively. The null hypotheses that the variances and means between the 6- and 20

  9. Krypton and xenon in Apollo 14 samples - Fission and neutron capture effects in gas-rich samples

    Science.gov (United States)

    Drozd, R.; Hohenberg, C.; Morgan, C.

    1975-01-01

    Gas-rich Apollo 14 breccias and trench soil are examined for fission xenon from the decay of the extinct isotopes Pu-244 and I-129, and some samples have been found to have an excess fission component which apparently was incorporated after decay elsewhere and was not produced by in situ decay. Two samples have excess Xe-129 resulting from the decay of I-129. The excess is correlated at low temperatures with excess Xe-128 resulting from neutron capture on I-127. This neutron capture effect is accompanied by related low-temperature excesses of Kr-80 and Kr-82 from neutron capture on the bromine isotopes. Surface correlated concentrations of iodine and bromine are calculated from the neutron capture excesses.

  10. Are symptom features of depression during pregnancy, the postpartum period and outside the peripartum period distinct? Results from a nationally representative sample using item response theory (IRT).

    Science.gov (United States)

    Hoertel, Nicolas; López, Saioa; Peyre, Hugo; Wall, Melanie M; González-Pinto, Ana; Limosin, Frédéric; Blanco, Carlos

    2015-02-01

    Whether there are systematic differences in depression symptom expression during pregnancy, the postpartum period and outside these periods (i.e., outside the peripartum period) remains debated. The aim of this study was to use methods based on item response theory (IRT) to examine, after equating for depression severity, differences in the likelihood of reporting DSM-IV symptoms of major depressive episode (MDE) in women of childbearing age (i.e., aged 18-50) during pregnancy, the postpartum period and outside the peripartum period. We conducted these analyses using a large, nationally representative sample of women of childbearing age from the United States (n = 11,256) who participated in the second wave of the National Epidemiologic Survey on Alcohol and Related Conditions (NESARC). The overall 12-month prevalence of all depressive criteria (except for worthlessness/guilt) was significantly lower in pregnant women than in women of childbearing age outside the peripartum period, whereas the prevalence of all symptoms (except for "psychomotor symptoms") was not significantly different between the postpartum and the nonperipartum group. There were no clinically significant differences in the endorsement rates of symptoms of MDE by pregnancy status when equating for levels of depression severity. This study suggests that the clinical presentation of depressive symptoms in women of childbearing age does not differ during pregnancy, the postpartum period and outside the peripartum period. These findings do not provide psychometric support for the inclusion of the peripartum onset specifier for major depressive disorder in the DSM-5. © 2014 Wiley Periodicals, Inc.

  11. THEORETICAL GAS CONCENTRATIONS ACHIEVING 100% FILL OF THE VITREOUS CAVITY IN THE POSTOPERATIVE PERIOD: A Gas Eye Model Study.

    Science.gov (United States)

    Williamson, Tom H; Guillemaut, Jean-Yves; Hall, Sheldon K; Hutter, Joseph C; Goddard, Tony

    2017-12-11

    To determine the concentrations of different gas tamponades in air to achieve 100% fill of the vitreous cavity postoperatively and to examine the influence of eye volume on these concentrations. A mathematical model of the mass transfer dynamics of tamponade and blood gases (O2, N2, and CO2) when injected into the eye was used. Mass transfer surface areas were calculated from published anatomical data. The model has been calibrated from published volumetric decay and composition results for three gases sulphahexafluoride (SF6), hexafluoroethane (C2F6), or perfluoropropane (C3F8). The concentrations of these gases (in air) required to achieve 100% fill of the vitreous cavity postoperatively without an intraocular pressure rise were determined. The concentrations were calculated for three volumes of the vitreous cavity to test whether ocular size influenced the results. A table of gas concentrations was produced. In a simulation of pars plana vitrectomy operations in which an 80% to 85% fill of the vitreous cavity with gas was achieved at surgery, the concentrations of the 3 gases in air to achieve 100% fill postoperatively were 10% to 13% for C3F8, 12% to 15% for C2F6, and 19% to 25% for SF6. These were similar to the so-called "nonexpansive" concentrations used in the clinical setting. The calculations were repeated for three different sizes of eye. Aiming for an 80% fill at surgery and 100% postoperatively, an eye with a 4-mL vitreous cavity required 24% SF6, 15% C2F6, or 13% C3F8; 7.2 mL required 25% SF6, 15% C2F6, or 13% C3F8; and 10 mL required 25% SF6, 16% C2F6, or 13% C3F8. When using 100% gas (e.g., used in pneumatic retinopexy), to achieve 100% fill postoperatively, the minimum vitreous cavity fill at surgery was 43% for SF6, 29% for C2F6, and 25% for C3F8 and was only minimally changed by variation in the size of the eye. A table has been produced, which could be used for surgical innovation in gas usage in the vitreous cavity. It provides concentrations

  12. Work Sampling Study of an Engineering Professor during a Regular Contract Period

    Science.gov (United States)

    Brink, Jan; McDonald, Dale B.

    2015-01-01

    Work sampling is a technique that has been employed in industry and fields such as healthcare for some time. It is a powerful technique, and an alternative to conventional stop watch time studies, used by industrial engineers to focus upon random work sampling observations. This study applies work sampling to the duties performed by an individual…

  13. Improved methodology to assess modification and completion of landfill gas management in the aftercare period

    International Nuclear Information System (INIS)

    Morris, Jeremy W.F.; Crest, Marion; Barlaz, Morton A.; Spokas, Kurt A.; Åkerman, Anna; Yuan, Lei

    2012-01-01

    Highlights: ► Performance-based evaluation of landfill gas control system. ► Analytical framework to evaluate transition from active to passive gas control. ► Focus on cover oxidation as an alternative means of passive gas control. ► Integrates research on long-term landfill behavior with practical guidance. - Abstract: Municipal solid waste landfills represent the dominant option for waste disposal in many parts of the world. While some countries have greatly reduced their reliance on landfills, there remain thousands of landfills that require aftercare. The development of cost-effective strategies for landfill aftercare is in society’s interest to protect human health and the environment and to prevent the emergence of landfills with exhausted aftercare funding. The Evaluation of Post-Closure Care (EPCC) methodology is a performance-based approach in which landfill performance is assessed in four modules including leachate, gas, groundwater, and final cover. In the methodology, the objective is to evaluate landfill performance to determine when aftercare monitoring and maintenance can be reduced or possibly eliminated. This study presents an improved gas module for the methodology. While the original version of the module focused narrowly on regulatory requirements for control of methane migration, the improved gas module also considers best available control technology for landfill gas in terms of greenhouse gas emissions, air quality, and emissions of odoriferous compounds. The improved module emphasizes the reduction or elimination of fugitive methane by considering the methane oxidation capacity of the cover system. The module also allows for the installation of biologically active covers or other features designed to enhance methane oxidation. A methane emissions model, CALMIM, was used to assist with an assessment of the methane oxidation capacity of landfill covers.

  14. Improved methodology to assess modification and completion of landfill gas management in the aftercare period

    Energy Technology Data Exchange (ETDEWEB)

    Morris, Jeremy W.F., E-mail: jmorris@geosyntec.com [Geosyntec Consultants, 10220 Old Columbia Road, Suite A, Columbia, MD 21046 (United States); Crest, Marion, E-mail: marion.crest@suez-env.com [Suez Environnement, 38 rue du President Wilson, 78230 Le Pecq (France); Barlaz, Morton A., E-mail: barlaz@ncsu.edu [Department of Civil, Construction, and Environmental Engineering, Campus Box 7908, North Carolina State University, Raleigh, NC 27695-7908 (United States); Spokas, Kurt A., E-mail: kurt.spokas@ars.usda.gov [United States Department of Agriculture - Agricultural Research Service, 1991 Upper Buford Circle, 439 Borlaug Hall, St. Paul, MN 55108 (United States); Akerman, Anna, E-mail: anna.akerman@sita.fr [SITA France, Tour CB 21, 16 Place de l' Iris, 92040 Paris La Defense Cedex (France); Yuan, Lei, E-mail: lyuan@geosyntec.com [Geosyntec Consultants, 10220 Old Columbia Road, Suite A, Columbia, MD 21046 (United States)

    2012-12-15

    Highlights: Black-Right-Pointing-Pointer Performance-based evaluation of landfill gas control system. Black-Right-Pointing-Pointer Analytical framework to evaluate transition from active to passive gas control. Black-Right-Pointing-Pointer Focus on cover oxidation as an alternative means of passive gas control. Black-Right-Pointing-Pointer Integrates research on long-term landfill behavior with practical guidance. - Abstract: Municipal solid waste landfills represent the dominant option for waste disposal in many parts of the world. While some countries have greatly reduced their reliance on landfills, there remain thousands of landfills that require aftercare. The development of cost-effective strategies for landfill aftercare is in society's interest to protect human health and the environment and to prevent the emergence of landfills with exhausted aftercare funding. The Evaluation of Post-Closure Care (EPCC) methodology is a performance-based approach in which landfill performance is assessed in four modules including leachate, gas, groundwater, and final cover. In the methodology, the objective is to evaluate landfill performance to determine when aftercare monitoring and maintenance can be reduced or possibly eliminated. This study presents an improved gas module for the methodology. While the original version of the module focused narrowly on regulatory requirements for control of methane migration, the improved gas module also considers best available control technology for landfill gas in terms of greenhouse gas emissions, air quality, and emissions of odoriferous compounds. The improved module emphasizes the reduction or elimination of fugitive methane by considering the methane oxidation capacity of the cover system. The module also allows for the installation of biologically active covers or other features designed to enhance methane oxidation. A methane emissions model, CALMIM, was used to assist with an assessment of the methane oxidation

  15. Design of a radioactive gas sampling system for NESHAP compliance measurements of 41Ar

    International Nuclear Information System (INIS)

    Newton, G.J.; McDonald, M.J.; Ghanbari, F.; Hoover, M.D.; Barr, E.B.

    1994-01-01

    United States Department of Energy facilities are required to comply with the U.S. Environmental Protection Agency, National Emission Standard for Hazardous Air Pollutants (NESHAP) 40 CFR, part 61, subpart H. Compliance generally requires confirmatory measurements of emitted radionuclides. Although a number of standard procedures exist for extractive sampling of particle-associated radionuclides, sampling approaches for radioactive gases are less defined. Real-time, flow-through sampling of radioactive gases can be done when concentrations are high compared to interferences from background radiation. Cold traps can be used to collect and concentrate condensible effluents in applications where cryogenic conditions can be established and maintained. Commercially available gas-sampling cylinders can be used to capture grab samples of contaminated air under ambient or compressed conditions, if suitable sampling and control hardware are added to the cylinders. The purpose of the current study was to develop an efficient and compact set of sampling and control hardware for use with commercially available gas-sampling cylinders, and to demonstrate its use in NESHAP compliance testing of 41 Ar at two experimental research reactors

  16. Reducing the sampling periods required in protocols for establishing ammonia emissions from pig fattening buildings using measurements and modelling

    NARCIS (Netherlands)

    Mosquera Losada, J.; Ogink, N.W.M.

    2011-01-01

    Ammonia (NH(3)) emission factors for animal housing systems in the Netherlands are based on measurements using standardised measurement protocols. Both the original Green Label (GL) protocol and the newly developed multi-site sampling protocol are based on year-round sampling periods. The objective

  17. Development of a new method for hydrogen isotope analysis of trace hydrocarbons in natural gas samples

    Directory of Open Access Journals (Sweden)

    Xibin Wang

    2016-12-01

    Full Text Available A new method had been developed for the analysis of hydrogen isotopic composition of trace hydrocarbons in natural gas samples by using solid phase microextraction (SPME combined with gas chromatography-isotope ratio mass spectrometry (GC/IRMS. In this study, the SPME technique had been initially introduced to achieve the enrichment of trace content of hydrocarbons with low abundance and coupled to GC/IRMS for hydrogen isotopic analysis. The main parameters, including the equilibration time, extraction temperature, and the fiber type, were systematically optimized. The results not only demonstrated that high extraction yield was true but also shows that the hydrogen isotopic fractionation was not observed during the extraction process, when the SPME device fitted with polydimethylsiloxane/divinylbenzene/carbon molecular sieve (PDMS/DVB/CAR fiber. The applications of SPME-GC/IRMS method were evaluated by using natural gas samples collected from different sedimentary basins; the standard deviation (SD was better than 4‰ for reproducible measurements; and also, the hydrogen isotope values from C1 to C9 can be obtained with satisfying repeatability. The SPME-GC/IRMS method fitted with PDMS/DVB/CAR fiber is well suited for the preconcentration of trace hydrocarbons, and provides a reliable hydrogen isotopic analysis for trace hydrocarbons in natural gas samples.

  18. Glass bottle sampling solid phase microextraction gas chromatography mass spectrometry for breath analysis of drug metabolites.

    Science.gov (United States)

    Lu, Yan; Niu, Wenqi; Zou, Xue; Shen, Chengyin; Xia, Lei; Huang, Chaoqun; Wang, Hongzhi; Jiang, Haihe; Chu, Yannan

    2017-05-05

    Breath analysis is a non-invasive approach which may be applied to disease diagnosis and pharmacokinetic study. In the case of offline analysis, the exhaled gas needs to be collected and the sampling bag is often used as the storage vessel. However, the sampling bag usually releases some extra compounds, which may interfere with the result of the breath test. In this study, a novel breath sampling glass bottle was developed with a syringe needle sampling port for solid phase microextraction (SPME). Such a glass bottle scarcely liberates compounds and can be used to collect exhaled gas for ensuing analysis by gas chromatography-mass spectrometry (GC-MS). The glass bottle sampling SPME-GC-MS analysis was carried out to investigate the breath metabolites of myrtol, a multicompound drug normally used in the treatment of bronchitis and sinusitis. Four compounds, α-pinene, 2,3-dehydro-1,8-cineole, d-limonene and 1,8-cineole were found in the exhaled breath of all eight volunteers who had taken the myrtol. While for other ten subjects who had not used the myrtol, these compounds were undetectable. In the SPME-GC-MS analysis of the headspace of myrtol, three compounds were detected including α-pinene, d-limonene and 1,8-cineole. Comparing the results of breath and headspace analysis, it indicates that 2,3-dehydro-1,8-cineole in the breath is the metabolite of 1,8-cineole. It is the first time that this metabolite was identified in human breath. The study demonstrates that the glass bottle sampling SPME-GC-MS method is applicable to exhaled gas analysis including breath metabolites investigation of drugs like myrtol. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. Evaluation Of Gas Diffusion Through Plastic Materials Used In Experimental And Sampling Equipment

    DEFF Research Database (Denmark)

    Kjeldsen, Peter

    1993-01-01

    . Calculations show that diffusion of oxygen through plastic tubing and reactors into anoxic water can be a serious problem for a series of plastic materials. Comparison of the method for turbulent and laminar flow in tubings shows that the difference is insignificant for most cases. Calculations show also......Plastic materials are often used in experimental and sampling equipment. Plastics are not gas tight, since gases are able to diffuse through the walls of tubing and containers made of plastic. Methods for calculating the significance of gas diffusion through the walls of containers and the walls...... of tubings for both turbulent and laminar flow conditions is presented. A more complex model for diffusion under laminar flow conditions is developed. A comprehensive review on gas diffusion coefficients for the main gases (O2, N2, CO2, CH4 etc.) and for a long range of plastic materials is also presented...

  20. Sampling and chemical analysis of smoke gas components from the SP Industry Calorimeter

    Energy Technology Data Exchange (ETDEWEB)

    Maansson, M.; Blomqvist, P.; Isaksson, I.; Rosell, L.

    1995-12-31

    This report describes the sampling and chemical analyses of smoke gas components for combustion performed in the SP Industry Calorimeter, where continuous measurements of oxygen, carbon dioxide and carbon monoxide are an integrated part of the Calorimeter system. On-line measurements of nitrogen oxides and total amounts of unburnt hydrocarbons were performed. Hydrogen cyanide, hydrogen chloride and ammonia in the smoke were sampled and absorbed in impinger bottles and subsequently analyzed using wet chemical techniques. An adsorbent sampling system was designed to allow the identification and quantitative analysis of individual organic compounds in the smoke. Gas chromatography was utilized with a mass spectrometric detector for the identification and a FID for quantification of the total amounts as well as individual components. A procedure for cleaning the smoke gas duct in between the combustion experiments was designed and found to be effective. The materials studied were Nylon 66, polypropylene, polystyrene (with and without fire retardant), PVC, and chlorobenzene. A total of 19 large-scale tests were carried out. The mass of sample burnt ranged from 20 kg to 125 kg in an experiment. 14 refs, 11 tabs

  1. A passive method for the determination of the equilibrium factor between radon gas and its short period progeny

    International Nuclear Information System (INIS)

    Lopez, Fabio O.; Canoba, Analia C.

    2001-01-01

    Due to the radiological importance of 222 Rn gas and its progeny of short period it is extremely necessary to count with an adequate methodology for the determination of its concentration in the different atmospheres in which human activity is developed. In this work a method was developed to determine the concentration of 222 Rn gas and the equilibrium factor between the concentration of the gas and its descendants, by means of a single device that has two Makrofol passive tracks detector. This device is completely passive and integrating, conditions that make it very appropriate to be used in any atmospheres in which human activity is developed, for example in houses, schools, places of work, underground mines, etc. (author)

  2. The Gas Sampling Interval Effect on V˙O2peak Is Independent of Exercise Protocol.

    Science.gov (United States)

    Scheadler, Cory M; Garver, Matthew J; Hanson, Nicholas J

    2017-09-01

    There is a plethora of gas sampling intervals available during cardiopulmonary exercise testing to measure peak oxygen consumption (V˙O2peak). Different intervals can lead to altered V˙O2peak. Whether differences are affected by the exercise protocol or subject sample is not clear. The purpose of this investigation was to determine whether V˙O2peak differed because of the manipulation of sampling intervals and whether differences were independent of the protocol and subject sample. The first subject sample (24 ± 3 yr; V˙O2peak via 15-breath moving averages: 56.2 ± 6.8 mL·kg·min) completed the Bruce and the self-paced V˙O2max protocols. The second subject sample (21.9 ± 2.7 yr; V˙O2peak via 15-breath moving averages: 54.2 ± 8.0 mL·kg·min) completed the Bruce and the modified Astrand protocols. V˙O2peak was identified using five sampling intervals: 15-s block averages, 30-s block averages, 15-breath block averages, 15-breath moving averages, and 30-s block averages aligned to the end of exercise. Differences in V˙O2peak between intervals were determined using repeated-measures ANOVAs. The influence of subject sample on the sampling effect was determined using independent t-tests. There was a significant main effect of sampling interval on V˙O2peak (first sample Bruce and self-paced V˙O2max P sample Bruce and modified Astrand P sampling intervals followed a similar pattern for each protocol and subject sample, with 15-breath moving average presenting the highest V˙O2peak. The effect of manipulating gas sampling intervals on V˙O2peak appears to be protocol and sample independent. These findings highlight our recommendation that the clinical and scientific community request and report the sampling interval whenever metabolic data are presented. The standardization of reporting would assist in the comparison of V˙O2peak.

  3. Comparison of tree coring and soil gas sampling for screening of contaminated sites

    DEFF Research Database (Denmark)

    Nielsen, Mette Algreen; Stalder, Marcel; Riis, Charlotte

    and then identify high risk areas. The uptake of BTEX into trees varies to a greater extent with the tree species and the site conditions than chlorinated solvents, which lead to greater uncertainty. Both methods have their advantages and disadvantages. Hence, the methods supplement each other. Based on results......Site characterization is often time consuming and a financial burden for the site owners, which raises a demand for rapid and inexpensive (pre)screening methods. Phytoscreening by tree coring has shown to be a useful tool to detect subsurface contamination, especially of chlorinated solvents...... suitable as initial screening methods for site characterization. The aim of this study is to compare tree coring and soil gas sampling to evaluate to which extent tree coring may supplement or substitute soil gas sampling as a site contaminant screening tool. And where both methods are feasible, evaluate...

  4. Development of gas-sampling device for 13N monitoring system

    International Nuclear Information System (INIS)

    Zhao Lihong; Gong Xueyu

    2003-01-01

    The 13 N monitoring system is used in the monitoring of the rate of leakage of the primary coolant circuit in nuclear power stations. The author introduces a gas-sampling device of the 13 Nmonitoring system. It is with a close-loop flow control system with intelligent control of Single Chip Micyoco (SCM), and has the ability to monitor and replace the filter paper automatically, to increase the automation of the device and stable operation in long time

  5. A Numerical Investigation on the Effect of Gas Pressure on the Water Saturation of Compacted Bentonite-Sand Samples

    Directory of Open Access Journals (Sweden)

    Jiang-Feng Liu

    2017-01-01

    Full Text Available In deep geological disposal for high-level radioactive waste, the generated gas can potentially affect the sealing ability of bentonite buffers. There is a competition between water and gas: the former provides sealing by swelling bentonite, and the latter attempts to desaturate the bentonite buffer. Thus, this study focused on numerically modelling the coupling effects of water and gas on the water saturation and sealing efficiency of compacted bentonite-sand samples. Different gas pressures were applied to the top surface of an upper sample, whereas the water pressure on the bottom side of the lower sample was maintained at 4 MPa. The results indicated that gas pressure did not significantly affect the saturation of the bentonite-sand sample until 2 MPa. At 2 MPa, the degree of water saturation of the upper sample was close to 1.0. As the gas pressure increased, this influence was more apparent. When the gas pressure was 6 MPa or higher, it was difficult for the upper sample to become fully saturated. Additionally, the lower sample was desaturated due to the high gas pressure. This indicated that gas pressure played an important role in the water saturation process and can affect the sealing efficiency of bentonite-based buffer materials.

  6. Physiologically available cyanide (PAC) in manufactured gas plant waste and soil samples

    International Nuclear Information System (INIS)

    Magee, B.; Taft, A.; Ratliff, W.; Kelley, J.; Sullivan, J.; Pancorbo, O.

    1995-01-01

    Iron-complexed cyanide compounds, such as ferri-ferrocyanide (Prussian Blue), are wastes associated with former manufactured gas plant (MGP) facilities. When tested for total cyanide, these wastes often show a high total cyanide content. Because simple cyanide salts are acutely toxic, cyanide compounds can be the subject of concern. However, Prussian Blue and related species are known to have a low order of human and animal toxicity. Toxicology data on complexed cyanides will be presented. Another issue regarding Prussian Blue and related species is that the total cyanide method does not accurately represent the amount of free cyanide released from these cyanide species. The method involves boiling the sample in an acidic solution under vacuum to force the formation of HCN gas. Thus, Prussian Blue, which is known to be low in toxicity, cannot be properly evaluated with current methods. The Massachusetts Natural Gas Council initiated a program with the Massachusetts Department of Environmental Protection to develop a method that would define the amount of cyanide that is able to be converted into hydrogen cyanide under the pH conditions of the stomach. It is demonstrated that less than 1% of the cyanide present in Prussian Blue samples and soils from MGP sites can be converted to HCN under the conditions of the human stomach. The physiologically available cyanide method has been designed to be executed at a higher temperature for one hour. It is shown that physiologically available cyanide in MGP samples is < 5--15% of total cyanide

  7. Effect of gas heating on the generation of an ultrashort avalanche electron beam in the pulse-periodic regime

    Science.gov (United States)

    Baksht, E. Kh.; Burachenko, A. G.; Lomaev, M. I.; Sorokin, D. A.; Tarasenko, V. F.

    2015-07-01

    The generation of an ultrashort avalanche electron beam (UAEB) in nitrogen in the pulse-periodic regime is investigated. The gas temperature in the discharge gap of the atmospheric-pressure nitrogen is measured from the intensity distribution of unresolved rotational transitions ( C 3Π u , v' = 0) → ( B 3Π g , v″ = 0) in the nitrogen molecule for an excitation pulse repetition rate of 2 kHz. It is shown that an increase in the UAEB current amplitude in the pulse-periodic regime is due to gas heating by a series of previous pulses, which leads to an increase in the reduced electric field strength as a result of a decrease in the gas density in the zone of the discharge formation. It is found that in the pulse-periodic regime and the formation of the diffuse discharge, the number of electrons in the beam increases by several times for a nitrogen pressure of 9 × 103 Pa. The dependences of the number of electrons in the UAEB on the time of operation of the generator are considered.

  8. Optimizing detection of noble gas emission at a former UNE site: sample strategy, collection, and analysis

    Science.gov (United States)

    Kirkham, R.; Olsen, K.; Hayes, J. C.; Emer, D. F.

    2013-12-01

    Underground nuclear tests may be first detected by seismic or air samplers operated by the CTBTO (Comprehensive Nuclear-Test-Ban Treaty Organization). After initial detection of a suspicious event, member nations may call for an On-Site Inspection (OSI) that in part, will sample for localized releases of radioactive noble gases and particles. Although much of the commercially available equipment and methods used for surface and subsurface environmental sampling of gases can be used for an OSI scenario, on-site sampling conditions, required sampling volumes and establishment of background concentrations of noble gases require development of specialized methodologies. To facilitate development of sampling equipment and methodologies that address OSI sampling volume and detection objectives, and to collect information required for model development, a field test site was created at a former underground nuclear explosion site located in welded volcanic tuff. A mixture of SF-6, Xe127 and Ar37 was metered into 4400 m3 of air as it was injected into the top region of the UNE cavity. These tracers were expected to move towards the surface primarily in response to barometric pumping or through delayed cavity pressurization (accelerated transport to minimize source decay time). Sampling approaches compared during the field exercise included sampling at the soil surface, inside surface fractures, and at soil vapor extraction points at depths down to 2 m. Effectiveness of various sampling approaches and the results of tracer gas measurements will be presented.

  9. Appropriate xenon-inhalation time in xenon-enhanced CT using the end-tidal gas-sampling method

    Energy Technology Data Exchange (ETDEWEB)

    Asada, Hideo; Furuhata, Shigeru; Onozuka, Satoshi; Uchida, Koichi; Fujii, Koji; Suga, Sadao; Kawase, Takeshi; Toya, Shigeo; Shiga, Hayao

    1988-12-01

    For the end-tidal gas-sampling method of xenon-enhanced CT (Xe-CT), the respective functional images of K, lambda, and the regional cerebral blood flow (rCBF) were studied and compared using the data at 7-, 10-, 15- and 25-minute inhalations. The most appropriate inhalation time of xenon gas was evaluated in 14 clinical cases. An end-tidal xenon curve which represents the arterial xenon concentration was monitored with a xenon analyzer; the xenon concentration was gradually increased to a level of 50% by using a xenon inhalator with a closed circuit to prevent the overestimation of the xenon concentration sampled from the mask. Serial CT scans were taken over a period of 25 minutes of inhalation. The functional images of K, lambda, and rCBF were calculated for serial CT scans for 7, 10, 15 and 25 minutes using Fick's equation. Those various images and absolute values were then compared. The rCBF value of a 15-minute inhalation was approximately 15% greater than that of 25 minutes, while the values of K, lambda, rCBF from a 15-minute inhalation were significantly correlated to those from 25 minutes. The regression line made it possible to estimate 25-minute inhalation values from those of 15 minutes. In imaging, the rCBF mapping of the 15-minute inhalation was found to be more reliable than that of 25 minutes. This study suggests that the minimal time of xenon inhalation is 15 minutes for the end-tidal gas-sampling method. A longer inhalation may be necessary for the estimation of rCBF in the low-flow area, such as the white matter or the pathological region.

  10. Analytical Values for Mushroom Compost, Poultry Deep Litter and Poultry Slurry Samples over a 5 Year Period 1978-82

    OpenAIRE

    Gormley, T. R. (Thomas Ronan); Staunton, L.

    1984-01-01

    Data are presented on the analysis of mushroom compost, poultry deep litter and poultry slurry samples over the period 1978-82. There was no difference in the dry matter (DM) content of compost samples between years either at time of filling or spawning, with mean values of 32 and 29%, respectively. The DM values were highest in the April-September period. Nitrogen (N) values were not different on an annual or quarterly basis, with means of 2.21 and 1.99%, on a DM basis, at spawning and filli...

  11. Analysis of Frankincense in Archaeological Samples by Gas Chromatography-Mass Spectrometry

    International Nuclear Information System (INIS)

    Mathe, C.; Archier, P.; Vieillescazes, C.; Connan, J.; Mouton, M.

    2007-01-01

    Four archaeological samples, unearthed from Qana in Yemen were analysed by analytical technique, currently applied in the field of petroleum geochemistry, and by gas chromatography coupled with a mass spectrometer (GC-MS). Sample no 1286 comes from a burned warehouse and samples no 964, 963 and 962 from the central sanctuary. These specimens were probably exposed to a heating source. In each case olibanum resin was identified according to the presence of their chemical markers corresponding to α-, β-boswellic and lupeolic acids (3α-hydroxy-olean-12-en-24-oic, 3α-hydroxy-urs-12-en-24-oic and 3α-hydroxy-lup-20(29)en-24-oic acids) and their respective O-acetyled derivatives (3α- O-acetyl -olean-12-en-24-oic, 3α-O-acetyl-urs-12-en-24-oic and 3α-O-acetyl-lup-20(29)-en-24-oic acids). Concerning the thermal degradation state of samples, the GC-MS results are in agreement with the geochemical ones. Sample no 1286 and 964 correspond to ageing incense which has not undergone any heating action and are consequently relatively well preserved. Lastly, samples no 963 and 962 are thermally degraded resins and their gross composition data permits to conclude that sample no 963 is only partially burnt while sample no 962 has been much more degraded

  12. Gas and Isotope Geochemistry of 81 Steam Samples from Wells in The Geysers Geothermal Field, Sonoma and Lake Counties, California

    Science.gov (United States)

    Lowenstern, Jacob B.; Janik, Cathy J.; Fahlquist, Lynne; Johnson, Linda S.

    1999-01-01

    geothermal field, the carbon-isotopic composition of CO2 is consistent with derivation of carbon from Franciscan metasedimentary rocks. NH3 concentrations are high in most Geysers well fluids, and are 2-3 orders of magnitude greater than would be expected in a the gas phase exhibiting homogeneous equilibrium at normal reservoir temperatures and pressures. Evidently, NH3 is flushed from the Franciscan host rocks at a rate that exceeds the reaction rate for NH3 breakdown. Many wells show clear influence by fluids from reinjection wells where steam condensate has been pumped back into the geothermal reservoir. Six wells were resampled over the time period of this study. One of these six wells was strongly affected by a nearby injection well. Three of the six resampled wells showed some signs of decreasing liquid/ steam within the geothermal reservoir, consistent with 'drying out' of the reservoir due to steam withdrawal. However, two wells exhibited little change. Analyses of gases from five surface manifestations (fumaroles and bubbling pools) are roughly similar to the deeper geothermal samples in both chemical and isotopic composition, but are lower in soluble gases that dissolve in groundwater during transit toward the surface.

  13. Gas chromatographic/mass spectrometric determination of carbon isotope composition in unpurified samples: methamphetamine example.

    Science.gov (United States)

    Low, I A; Liu, R H; Legendre, M G; Piotrowski, E G; Furner, R L

    1986-10-01

    A gas chromatograph/quadrupole mass spectrometer system, operated in electron impact/selected ion monitoring mode, is used to determine the intensity ratio of the m/z 59 and the m/z 58 ions of the [C3H8N]+ fragment derived from methamphetamine samples synthesized with varying amounts of 13C-labeled methylamine. Crude products are introduced into the gas chromatograph without prior cleanup. The ratios measured were in excellent agreement with those calculated. A change in 0.25% use of 13C-methylamine is sufficient for product differentiation. The feasibility of using isotope labeling and subsequent mass spectrometric isotope ratio measurement as the basis of a compound tracing mechanism is discussed. Specifically, if methamphetamine samples manufactured from legal sources are asked to incorporate distinct 13C compositions, their sources can be traced when samples are diverted into illegal channels. Samples derived from illicit preparations can also be traced if the manufacturers of a precursor (methylamine in this case) incorporate distinct 13C compositions in their products.

  14. Chemical and physical characteristics of tar samples from selected Manufactured Gas Plant (MGP) sites

    International Nuclear Information System (INIS)

    Ripp, J.; Taylor, B.; Mauro, D.; Young, M.

    1993-05-01

    A multiyear, multidisciplinary project concerning the toxicity of former Manufactured Gas Plant (MGP) tarry residues was initiated by EPRI under the Environmental Behavior of Organic Substances (EBOS) Program. This report concerns one portion of that work -- the collection and chemical characterization of tar samples from several former MGP sites. META Environmental, Inc. and Atlantic Environmental Services, Inc. were contracted by EPRI to collect several samples of tarry residues from former MGP sites with varied historical gas production processes and from several parts of the country. The eight tars collected during this program were physically very different. Some tars were fluid and easily pumped from existing wells, while other tars were thicker, semi-solid, or solid. Although care was taken to collect only tar, the nature of the residues at several sites made it impossible not to collect other material, such as soil, gravel, and plant matter. After the samples were collected, they were analyzed for 37 organic compounds, 8 metals, and cyanide. In addition, elemental analysis was performed on the tar samples for carbon, hydrogen, oxygen, sulfur and nitrogen content and several physical/chemical properties were determined for each tar. The tars were mixed together in different batches and distributed to researchers for use in animal toxicity studies. The results of this work show that, although the tars were produced from different processes and stored in different manners, they had some chemical similarities. All of the tars, with the exception of one unusual solid tar, contained similar relative abundances of polycyclic aromatic hydrocarbons (PAHs)

  15. The Behaviour of Gas Bubble during Rest Period of Pulse-Activated Electrolysis Hydrogen Production

    Directory of Open Access Journals (Sweden)

    Vilasmongkolchai Thanet

    2016-01-01

    Full Text Available The pulse-activated electrolyzer has been developed and used for several years. With the capability of enhancing the efficiency of an electrolytic process and easy operation, this technique becomes an interesting process for hydrogen production. Unfortunately during electrolytic reaction, the creation of bubbles becomes a reaction inhibitor and consumes energy. This paper aims to study the proper rest period that gives the bubble free rise-off the solution without additional bubble created. The mathematical method and acoustic emission method were used for investigation of bubble’s rising velocity. The result shows that the variation of rest period on pulse-activated makes production efficiency enhanced. For the practicality of use and set control parameters, duty cycle and frequency were demonstrated instead of rest period.

  16. Periodic motions and chaos for a damped mobile piston system in a high pressure gas cylinder with P control

    International Nuclear Information System (INIS)

    Wang, Donghua; Huang, Jianzhe

    2017-01-01

    In this paper, the complex motions for a moving piston in a closed gas cylinder will be analyzed using the discrete implicit maps method. The strong nonlinearity of such system will be observed due to the large quadratic and cubic stiffness. Period-1 motions which contain high order of harmonic components will be presented. The periodic motions will be discretized into multiple continuous mappings, and such mapping can be analyzed via Newton–Raphson iteration. The stability analysis will be given and the analytic conditions for the saddle-node and period-doubling bifurcation will be determined. From the semi-analytic solution route, the possible motions without considering the impact of the piston with the end wall of the cylinder will be obtained analytically. The scheme to reduce the vibration of the piston can be obtained through the parameter studies.

  17. THE IMPORTANCE OF THE STANDARD SAMPLE FOR ACCURATE ESTIMATION OF THE CONCENTRATION OF NET ENERGY FOR LACTATION IN FEEDS ON THE BASIS OF GAS PRODUCED DURING THE INCUBATION OF SAMPLES WITH RUMEN LIQUOR

    Directory of Open Access Journals (Sweden)

    T ŽNIDARŠIČ

    2003-10-01

    Full Text Available The aim of this work was to examine the necessity of using the standard sample at the Hohenheim gas test. During a three year period, 24 runs of forage samples were incubated with rumen liquor in vitro. Beside the forage samples also the standard hay sample provided by the Hohenheim University (HFT-99 was included in the experiment. Half of the runs were incubated with rumen liquor of cattle and half with the rumen liquor of sheep. Gas produced during the 24 h incubation of standard sample was measured and compared to a declared value of sample HFT-99. Beside HFT-99, 25 test samples with known digestibility coefficients determined in vivo were included in the experiment. Based on the gas production of HFT-99, it was found that donor animal (cattle or sheep did not significantly affect the activity of rumen liquor (41.4 vs. 42.2 ml of gas per 200 mg dry matter, P>0.1. Neither differences between years (41.9, 41.2 and 42.3 ml of gas per 200 mg dry matter, P>0.1 were significant. However, a variability of about 10% (from 38.9 to 43.7 ml of gas per 200 mg dry matter was observed between runs. In the present experiment, the gas production in HFT-99 was about 6% lower than the value obtained by the Hohenheim University (41.8 vs. 44.43 ml per 200 mg dry matter. This indicates a systematic error between the laboratories. In the case of twenty-five test samples, correction on the basis of the standard sample reduced the average difference of the in vitro estimates of net energy for lactation (NEL from the in vivo determined values. It was concluded that, due to variation between runs and systematical differences in rumen liquor activity between two laboratories, the results of Hohenheim gas test have to be corrected on the basis of standard sample.

  18. A Hybrid Algorithm for Period Analysis from Multiband Data with Sparse and Irregular Sampling for Arbitrary Light-curve Shapes

    Science.gov (United States)

    Saha, Abhijit; Vivas, A. Katherina

    2017-12-01

    Ongoing and future surveys with repeat imaging in multiple bands are producing (or will produce) time-spaced measurements of brightness, resulting in the identification of large numbers of variable sources in the sky. A large fraction of these are periodic variables: compilations of these are of scientific interest for a variety of purposes. Unavoidably, the data sets from many such surveys not only have sparse sampling, but also have embedded frequencies in the observing cadence that beat against the natural periodicities of any object under investigation. Such limitations can make period determination ambiguous and uncertain. For multiband data sets with asynchronous measurements in multiple passbands, we wish to maximally use the information on periodicity in a manner that is agnostic of differences in the light-curve shapes across the different channels. Given large volumes of data, computational efficiency is also at a premium. This paper develops and presents a computationally economic method for determining periodicity that combines the results from two different classes of period-determination algorithms. The underlying principles are illustrated through examples. The effectiveness of this approach for combining asynchronously sampled measurements in multiple observables that share an underlying fundamental frequency is also demonstrated.

  19. [Determination of buprofezin, methamidophos, acephate, and triazophos residues in Chinese tea samples by gas chromatography].

    Science.gov (United States)

    Zhang, Shuiba; Yi, Jun; Ye, Jianglei; Zheng, Wenhui; Cai, Xueqin; Gong, Zhenbin

    2004-03-01

    A method has been developed for the simultaneous determination of buprofezin, methamidophos, acephate and triazophos residues in Chinese tea samples. The pesticide residues were extracted from tea samples with a mixture of ethyl acetate and n-hexane (50:50, v/v) at 45 degrees C. The extracts were subsequently treated with a column packed with 40 mg of active carbon by gradient elution with ethyl acetate and n-hexane. Buprofenzin and the three organophosphorus pesticides were analyzed by gas chromatography using a DB-210 capillary column and a nitrogen-phosphorus detector. The recoveries for spiked standards were 73.4%-96.9%. The relative standard deviations were all within 4.63%. The limits of quantitation (3sigma) in the tea samples were about 7.0-12.0 microg/kg.

  20. Method and apparatus for transport, introduction, atomization and excitation of emission spectrum for quantitative analysis of high temperature gas sample streams containing vapor and particulates without degradation of sample stream temperature

    Science.gov (United States)

    Eckels, David E.; Hass, William J.

    1989-05-30

    A sample transport, sample introduction, and flame excitation system for spectrometric analysis of high temperature gas streams which eliminates degradation of the sample stream by condensation losses.

  1. Testing odorants recovery from a novel metallized fluorinated ethylene propylene gas sampling bag.

    Science.gov (United States)

    Zhu, Wenda; Koziel, Jacek A; Cai, Lingshuang; Wright, Donald; Kuhrt, Fred

    2015-12-01

    Industry-standard Tedlar bags for odor sample collection from confined animal feeding operations (CAFOs) have been challenged by the evidence of volatile organic compound (VOC) losses and background interferences. Novel impermeable aluminum foil with a thin layer of fluorinated ethylene propylene (FEP) film on the surface that is in contact with a gas sample was developed to address this challenge. In this research, Tedlar and metallized FEP bags were compared for (a) recoveries of four characteristic CAFO odorous VOCs (ethyl mercaptan, butyric acid, isovaleric acid and p-cresol) after 30 min and 24 hr sample storage time and for (b) chemical background interferences. All air sampling and analyses were performed with solid-phase microextraction (SPME) followed by gas chromatography-mass spectroscopy (GC-MS). Mean target gas sample recoveries from metallized FEP bags were 25.9% and 28.0% higher than those in Tedlar bags, for 30 min and 24 hr, respectively. Metallized FEP bags demonstrated the highest p-cresol recoveries after 30-min and 24-hr storage, 96.1±44.5% and 44.8±10.2%, respectively, among different types of sampling bags reported in previous studies. However, a higher variability was observed for p-cresol recovery with metallized FEP bags. A 0% recovery of ethyl mercaptan was observed with Tedlar bags after 24-hr storage, whereas an 85.7±7.4% recovery was achieved with metallized FEP bags. Recoveries of butyric and isovaleric acids were similar for both bag types. Two major impurities in Tedlar bags' background were identified as N,N-dimethylacetamide and phenol, while backgrounds of metallized FEP bags were significantly cleaner. Reusability of metallized FEP bags was tested. Caution is advised when using polymeric materials for storage of livestock-relevant odorous volatile organic compounds. The odorants loss with storage time confirmed that long-term storage in whole-air form is ill advised. A focused short-term odor sample containment should be

  2. Advertising Intellection in Ottoman Empire Period end Sample of Tanin Newspaper between 1908 and 1909 Years

    Directory of Open Access Journals (Sweden)

    Ayşe Hanife KOCAKAYA

    2016-06-01

    Full Text Available Advertising that has become an indispensable element of today’s conditions has also become a frequently used tool of goods and services the companies utilized. With the advances in technology, the number of companies that commercialises their goods has been steadily increasing day by day. That fact that advertising has become such a significant sector of the industry; has provided this sector with the opportunity to contact a lot of people all at the same time. That is why; advertising is special among the marketing and the media tools. The Tanin newspaper discussed in this article began to be broadcast towards the end of the Ottoman Empire. The newspaper that began to be published in the late Ottoman and the early Turkish Republic eras came to the fore as a political organ rather than the advertisements of the publication. The number of Tanin newspaper published during the years 1908-1909 were examined in this article. The newspaper had published many advertisements and covered many brands in the issues that were published during this period,The newspaper that encountered various obstacles during its life of publication bears importance by being, established by the Committee of Union and Progress members as well

  3. Operability test report for core sample truck number one flammable gas modifications

    International Nuclear Information System (INIS)

    Akers, J.C.

    1997-01-01

    This report primarily consists of the original test procedure used for the Operability Testing of the flammable gas modifications to Core Sample Truck No. One. Included are exceptions, resolutions, comments, and test results. This report consists of the original, completed, test procedure used for the Operability Testing of the flammable gas modifications to the Push Mode Core Sample Truck No. 1. Prior to the Acceptance/Operability test the truck No. 1 operations procedure (TO-080-503) was revised to be more consistent with the other core sample truck procedures and to include operational steps/instructions for the SR weather cover pressurization system. A draft copy of the operations procedure was used to perform the Operability Test Procedure (OTP). A Document Acceptance Review Form is included with this report (last page) indicating the draft status of the operations procedure during the OTP. During the OTP 11 test exceptions were encountered. Of these exceptions four were determined to affect Acceptance Criteria as listed in the OTP, Section 4.7 ACCEPTANCE CRITERIA

  4. Gas chromatographic determination of cholesterol from food samples using extraction/saponification method

    International Nuclear Information System (INIS)

    Ali, Z.M.; Soomro, A.S.A.

    2007-01-01

    A simple and fast one-step extraction/saponification with Na/OH/KOH (Ethanolic, Sodium Hydroxide/Potassium Hydroxide was compared and validated for determination of cholesterol from locally available 10 edible oil and egg samples. The importance of the use of edible oils and eggs in routine diet is unquestionable, but presence of cholesterol is considered as a risk factor for coronary heart disease and hypertension. The lowering of cholesterol level in order to reduce the risk is widely accepted. The cholesterol in the edible oil and eggs was determined by gas chromatography, through elution from the column (2x3 mm i.d) packed with 3% OV-I01, on Chromosorb G/'NAW 80-100 mesh size at 250-300C with programmed heating rate of 3 degree C/min. Nitrogen gas flow rate was 40 ml/min. The cholesterol samples were run under the conditions after selective extraction in diethyl ether. The calibration was linear within 50-500 IJg/ml concentration range. The amount of cholesterol detected were from 12.92-18.05 mg/g in edible oil and 117.54-143.42 mg/g in egg samples with RSD 1.3-2.7%. (author)

  5. The Atmospheric Scanning Electron Microscope with open sample space observes dynamic phenomena in liquid or gas.

    Science.gov (United States)

    Suga, Mitsuo; Nishiyama, Hidetoshi; Konyuba, Yuji; Iwamatsu, Shinnosuke; Watanabe, Yoshiyuki; Yoshiura, Chie; Ueda, Takumi; Sato, Chikara

    2011-12-01

    Although conventional electron microscopy (EM) requires samples to be in vacuum, most chemical and physical reactions occur in liquid or gas. The Atmospheric Scanning Electron Microscope (ASEM) can observe dynamic phenomena in liquid or gas under atmospheric pressure in real time. An electron-permeable window made of pressure-resistant 100 nm-thick silicon nitride (SiN) film, set into the bottom of the open ASEM sample dish, allows an electron beam to be projected from underneath the sample. A detector positioned below captures backscattered electrons. Using the ASEM, we observed the radiation-induced self-organization process of particles, as well as phenomena accompanying volume change, including evaporation-induced crystallization. Using the electrochemical ASEM dish, we observed tree-like electrochemical depositions on the cathode. In silver nitrate solution, we observed silver depositions near the cathode forming incidental internal voids. The heated ASEM dish allowed observation of patterns of contrast in melting and solidifying solder. Finally, to demonstrate its applicability for monitoring and control of industrial processes, silver paste and solder paste were examined at high throughput. High resolution, imaging speed, flexibility, adaptability, and ease of use facilitate the observation of previously difficult-to-image phenomena, and make the ASEM applicable to various fields. Copyright © 2011 Elsevier B.V. All rights reserved.

  6. Properties of samples containing natural gas hydrate from the JAPEX/JNOC/GSC Mallik 2L-38 gas hydrate research well, determined using Gas Hydrate And Sediment Test Laboratory Instrument (GHASTLI)

    Science.gov (United States)

    Winters, W.J.

    1999-01-01

    As part of an ongoing laboratory study, preliminary acoustic, strength, and hydraulic conductivity results are presented from a suite of tests conducted on four natural-gas-hydrate-containing samples from the Mackenzie Delta JAPEX/JNOC/GSC Mallik 2L-38 gas hydrate research well. The gas hydrate samples were preserved in pressure vessels during transport from the Northwest Territories to Woods Hole, Massachusetts, where multistep tests were performed using GHASTLI (Gas Hydrate And Sediment Test Laboratory Instrument), which recreates pressure and temperature conditions that are stable for gas hydrate. Properties and changes in sediment behaviour were measured before, during, and after controlled gas hydrate dissociation. Significant amounts of gas hydrate occupied the sample pores and substantially increased acoustic velocity and shear strength.

  7. Gas dispersion concentration of trace inorganic contaminants from fuel gas and analysis using head-column field-amplified sample stacking capillary electrophoresis.

    Science.gov (United States)

    Yang, Jianmin; Li, Hai-Fang; Li, Meilan; Lin, Jin-Ming

    2012-08-21

    The presence of inorganic elements in fuel gas generally accelerates the corrosion and depletion of materials used in the fuel gas industry, and even leads to serious accidents. For identification of existing trace inorganic contaminants in fuel gas in a portable way, a highly efficient gas-liquid sampling collection system based on gas dispersion concentration is introduced in this work. Using the constructed dual path gas-liquid collection setup, inorganic cations and anions were simultaneously collected from real liquefied petroleum gas (LPG) and analyzed by capillary electrophoresis (CE) with indirect UV absorbance detection. The head-column field-amplified sample stacking technique was applied to improve the detection limits to 2-25 ng mL(-1). The developed collection and analytical methods have successfully determined existing inorganic contaminants in a real LPG sample in the range of 4.59-138.69 μg m(-3). The recoveries of cations and anions with spiked LPG samples were between 83.98 and 105.63%, and the relative standard deviations (RSDs) were less than 7.19%.

  8. Use of the small gas proportional counters for the carbon-14 measurement of very small samples

    International Nuclear Information System (INIS)

    Sayre, E.V.; Harbottle, G.; Stoenner, R.W.; Otlet, R.L.; Evans, G.V.

    1981-01-01

    Two recent developments are: the first is the mass-spectrometric separation of 14 C and 12 C ions, followed by counting of the 14 C, while the second is the extension of conventional proportional counter operation, using CO 2 as counting gas, to very small counters and samples. Although the second method is slow (months of counting time are required for 10 mg of carbon) it does not require operator intervention and many samples may be counted simultaneously. Also, it costs only a fraction of the capital expense of an accelerator installation. The development, construction and operation of suitable small counters are described, and results of three actual dating studies involving milligram scale carbon samples will be given. None of these could have been carried out if conventional, gram-sized samples had been needed. New installations, based on the use of these counters, are under construction or in the planning stages. These are located at Brookhaven Laboratory, the National Bureau of Standards (USA) and Harwell (UK). The Harwell installation, which is in advanced stages of construction, will be described in outline. The main significance of the small-counter method is, that although it will not suffice to measure the smallest (much less than 10 mg) or oldest samples, it will permit existing radiocarbon laboratories to extend their capability considerably, in the direction of smaller samples, at modest expense

  9. Radioactivity measurements of soil samples in the Republic of Serbia for the period 1999-2001

    International Nuclear Information System (INIS)

    Eremic Savkovic, M.; Pantelic, G.; Javorina, L.; Tanaskovic, I.; Vuletic, V.

    2002-01-01

    The soil is the basic environment of migration of radionuclides into plants, from which they reach the people and animals through food. The type of soil affects the distribution of radionuclides in the soil itself and their transfer into plants, respectively. Systemic testing of radioactivity of soils is performed on specific locations in the Federal Republic of Yugoslavia, in particular time periods according to methods defined by regulations. As result of NATO aggression and use of ammunition with depleted uranium in 1999, the existing radioactivity monitoring program of Yugoslavia was modified. Besides measurement of activity of artificial radionuclides, that were present in living environment after Chernobyl accident in 1986, the testing of activity of natural radionuclides, especially of uranium, was carried out as well. Uranium in Serbia derives from natural sources, considering the geological composition of rocks and geochemical composition of soil, and their concentrations as well as the concentrations of its descendants represent the significant component of natural sources of ionizing irradiation. In Serbia, the major uranium sources are igneous, carbonic and sedimentary rocks, and granite. According to perennial geological investigation of uranium in our country, several geological regions have been found to have uranium in higher or lower concentration. The uranium concentration in these regions ranged from 0.003g/t for ultra basic rocks to 3.5g/t for igneous, sedimentary rocks and granite. One of considerable uranium sources is specific technological procedure in industry such as production and combustion of coal in thermal plants, production of phosphate mineral fertilizers, production of phosphoric acid, phosphoric plaster, etc

  10. Gas sampling calorimeter studies in proportional, saturated avalanche, and streamer modes

    International Nuclear Information System (INIS)

    Atac, M.; Bedeschi, F.; Yoh, J.; Morse, R.; Procario, M.

    1982-01-01

    Recently, satisfactory new results were obtained at SLAC from gas sampling calorimeters running in the saturated avalanche mode within the energy range of 1.5 to 17.5 GeV. To study the higher energy behavior of this mode, more tests were carried out in the M4 beamline at Fermilab. This paper contains results obtained from the MAC prototype electromagnetic and hadronic calorimeters running in the proportional, saturated avalanche, and the streamer regions for energies between 12 and 150 GeV

  11. Fast derivatization of fatty acids in different meat samples for gas chromatography analysis.

    Science.gov (United States)

    Figueiredo, Ingrid Lima; Claus, Thiago; Oliveira Santos Júnior, Oscar; Almeida, Vitor Cinque; Magon, Thiago; Visentainer, Jesuí Vergilio

    2016-07-22

    In order to analyze the composition of fatty acids employing gas chromatography as the separation method, a derivatization of lipids using esterification and transesterification reactions is needed. The methodologies currently available are time consuming and use large amounts of sample and reagents. Thus, this work proposes a new procedure to carry out the derivatization of fatty acids without the need for prior extraction of lipids. The use of small amounts of sample (100mg) allows the analysis to be performed in specific parts of animals, in most cases without having them slaughtered. Another benefit is the use of small amounts of reagents (only 2mL of NaOH/Methanol and H2SO4/Methanol). The use of an experimental design procedure (Design Expert software) allows the optimization of the alkaline and acid reaction times. The procedure was validated for five minutes in both steps. The method was validated for bovine fat, beef, chicken, pork, fish and shrimp meats. The results for the merit figures of accuracy (from 101.07% to 109.18%), precision (RSDintra-day (from 0.65 to 3.93%), RSDinter-day (from 1.57 to 5.22%)), linearity (R(2)=0.9864) and robustness confirmed that the new method is satisfactory within the linear range of 2-30% of lipids in the sample. Besides the benefits of minimizing the amount of samples and reagents, the procedure enables gas chromatography sample preparation in a very short time compared with traditional procedures. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. Acute and chronic toxicity of sediment samples from Guanabara Bay (RJ during the rainy period

    Directory of Open Access Journals (Sweden)

    Luciane Alves Maranho

    2010-06-01

    Full Text Available Guanabara Bay is a marine-estuarine environment of high ecological and socio-economic importance, subject to a variety of environmental impacts. Sediment is the eventual repository for most substances introduced into water bodies and may, therefore, provide an integrated measure of the environmental quality, which can be assessed by many different approaches. In this project, the quality of sediments from Guanabara Bay was evaluated by the ecotoxicological approach: whole-sediment toxicity tests, using Tiburonella viscana, and porewater, elutriate and sediment-water interface chronic toxicity tests, using embryos of Lytechinus variegatus, were applied. Sediments were collected at 14 sampling stations, distributed across the bay. Chronic tests showed significant toxicity in most of the sediment samples. Sediments from stations 1, 2, 3, 6, 8, 10, 11, 12 and 15 showed acute toxicity as well. The results of the different tests were well correlated, and their integration showed that the sediments analyzed were considered unsuitable for aquatic life, resulting in the environmental degradation of Guanabara Bay. In this context, the control of pollution sources and multi-purpose management are required to improve the environmental quality.A Baía de Guanabara é um ambiente marinho-estuarino de grande relevância ecológica e sócio-econômica, e sujeita a uma ampla gama de impactos ambientais. O sedimento é o principal destino para a maioria das substâncias introduzidas nos corpos d'água, podendo fornecer uma medida integrada da qualidade ambiental, a qual pode ser avaliada por várias abordagens. Neste projeto, a qualidade de sedimentos da Baía de Guanabara foi por uma abordagem ecotoxicológica, por meio de testes de toxicidade aguda de sedimento integral, utilizando Tiburonella viscana, e testes de toxicidade crônica de água intersticial, elutriato e interface sedimento-água, utilizando embriões de Lytechinus variegatus. Os sedimentos foram

  13. Radioactivity measurements of soil samples in the Region Vranje (Bratoselce Village) for the period 2001-2004

    International Nuclear Information System (INIS)

    Eremic-savkovic, M.; Pantelic, G.; Tanaskovic, I.; Vuletic, V.; Javorina, L.

    2006-01-01

    Systematic examination of radioactive contamination of soil samples was established at the Institute for Occupational and Radiological Health. With the bombing of our country (Spring 1999) the monitoring of radioactivity has changed. We also measured the activities of uranium and it descendants. This paper presents the results of radioactivity monitoring of the soil in small area 700 m near village Bratoselce in region Vranje during the period 2001 - 2004. From 2001 to 2004, we collected different samples from this fenced area as well as outside this area assuming not to be contaminated, before, during and after decontamination. Some soil samples were made as a mix of small samples from a large area of location. Other samples were taken at the points formerly designated as contaminated or from shell-craters seen on the fenced area surface. All samples were analyzed by gamma spectrometry and measurements of alpha and beta activity. On the basis of measurements of soil activities, analysis of 238 U and 235 U, as well as in comparison with natural activity ratio being 21.4, it may be concluded that depleted uranium contamination was present both in the fenced area and outside it, because this ratio in the samples of soil was found to be 34 to 73. Natural activity in soil samples was slightly higher in relation to mean soil activity in Serbia. (authors)

  14. Identifying intimate partner violence (IPV) during the postpartum period in a Greek sample.

    Science.gov (United States)

    Vivilaki, Victoria G; Dafermos, Vassilis; Daglas, Maria; Antoniou, Evagelia; Tsopelas, Nicholas D; Theodorakis, Pavlos N; Brown, Judith B; Lionis, Christos

    2010-12-01

    Research has highlighted the wide impact of intimate partner violence (IPV) and the public health role of community health professionals in detection of victimized women. The purpose of this study was to identify postpartum emotional and physical abuse and to validate the Greek version of the Women Abuse Screening Tool (WAST) along with its sensitivity and specificity. Five hundred seventy-nine mothers within 12 weeks postpartum were recruited from the perinatal care registers of the Maternity Departments of two public hospitals in Athens, Greece. Participants were randomly selected by clinic or shift. The WAST and the Partner Violence Screen (PVS) surveys were administered in random order to the mothers from September 2007 to January 2008. The WAST was compared with the PVS as a criterion standard. Agreement between the screening instruments was examined. The psychometric measurements that were performed included: two independent sample t tests, reliability coefficients, explanatory factor analysis using a Varimax rotation, and Principal Components Method. Confirmatory analysis-also called structural equation modeling-of principal components was conducted by Linear Structural Relations. A receiver operating characteristic (ROC) analysis was carried out to evaluate the global functioning of the scale. Two hundred four (35.6%) of the mothers screened were identified as experiencing IPV. Scores on the WAST correlated well with those on the PVS; the internal consistency of the WAST Greek version-tested using Cronbach's alpha coefficient-was found to be 0.926 and that of Guttman's split-half coefficient was 0.924. Our findings confirm the multidimensionality of the WAST, demonstrating a two-factor structure. The area under ROC curve (AUC) was found to be 0.824, and the logistic estimate for the threshold score of 0/1 fitted the model sensitivity at 99.7% and model specificity at 64.4%. Our data confirm the validity of the Greek version of the WAST in identifying IPV

  15. A novel approach to process carbonate samples for radiocarbon measurements with helium carrier gas

    Energy Technology Data Exchange (ETDEWEB)

    Wacker, L., E-mail: wacker@phys.ethz.ch [Laboratory of Ion Beam Physics, ETH Zurich, 8093 Zurich (Switzerland); Fueloep, R.-H. [Institute of Geology and Mineralogy, University of Cologne, 50674 Cologne (Germany); Hajdas, I. [Laboratory of Ion Beam Physics, ETH Zurich, 8093 Zurich (Switzerland); Molnar, M. [Laboratory of Ion Beam Physics, ETH Zurich, 8093 Zurich (Switzerland); Institute of Nuclear Research, Hungarian Academy of Sciences, 4026 Debrecen (Hungary); Rethemeyer, J. [Institute of Geology and Mineralogy, University of Cologne, 50674 Cologne (Germany)

    2013-01-15

    Most laboratories prepare carbonates samples for radiocarbon analysis by acid decomposition in evacuated glass tubes and subsequent reduction of the evolved CO{sub 2} to graphite in self-made reduction manifolds. This process is time consuming and labor intensive. In this work, we have tested a new approach for the preparation of carbonate samples, where any high-vacuum system is avoided and helium is used as a carrier gas. The liberation of CO{sub 2} from carbonates with phosphoric acid is performed in a similar way as it is often done in stable isotope ratio mass spectrometry where CO{sub 2} is released with acid in septum sealed tube under helium atmosphere. The formed CO{sub 2} is later flushed in a helium flow by means of a double-walled needle mounted from the tubes to the zeolite trap of the automated graphitization equipment (AGE). It essentially replaces the elemental analyzer normally used for the combustion of organic samples. The process can be fully automated from sampling the released CO{sub 2} in the septum-sealed tubes with a commercially available auto-sampler to the graphitization with the automated graphitization. The new method yields in low sample blanks of about 50000 years. Results of processed reference materials (IAEA-C2, FIRI-C) are in agreement with their consensus values.

  16. Electrostatic modulation of periodic potentials in a two-dimensional electron gas: From antidot lattice to quantum dot lattice

    Energy Technology Data Exchange (ETDEWEB)

    Goswami, Srijit; Aamir, Mohammed Ali; Shamim, Saquib; Ghosh, Arindam [Department of Physics, Indian Institute of Science, Bangalore 560 012 (India); Siegert, Christoph; Farrer, Ian; Ritchie, David A. [Cavendish Laboratory, University of Cambridge, J.J. Thomson Avenue, Cambridge CB3 0HE (United Kingdom); Pepper, Michael [Department of Electrical and Electronic Engineering, University College, London WC1E 7JE (United Kingdom)

    2013-12-04

    We use a dual gated device structure to introduce a gate-tuneable periodic potential in a GaAs/AlGaAs two dimensional electron gas (2DEG). Using only a suitable choice of gate voltages we can controllably alter the potential landscape of the bare 2DEG, inducing either a periodic array of antidots or quantum dots. Antidots are artificial scattering centers, and therefore allow for a study of electron dynamics. In particular, we show that the thermovoltage of an antidot lattice is particularly sensitive to the relative positions of the Fermi level and the antidot potential. A quantum dot lattice, on the other hand, provides the opportunity to study correlated electron physics. We find that its current-voltage characteristics display a voltage threshold, as well as a power law scaling, indicative of collective Coulomb blockade in a disordered background.

  17. Electrostatic modulation of periodic potentials in a two-dimensional electron gas: From antidot lattice to quantum dot lattice

    International Nuclear Information System (INIS)

    Goswami, Srijit; Aamir, Mohammed Ali; Shamim, Saquib; Ghosh, Arindam; Siegert, Christoph; Farrer, Ian; Ritchie, David A.; Pepper, Michael

    2013-01-01

    We use a dual gated device structure to introduce a gate-tuneable periodic potential in a GaAs/AlGaAs two dimensional electron gas (2DEG). Using only a suitable choice of gate voltages we can controllably alter the potential landscape of the bare 2DEG, inducing either a periodic array of antidots or quantum dots. Antidots are artificial scattering centers, and therefore allow for a study of electron dynamics. In particular, we show that the thermovoltage of an antidot lattice is particularly sensitive to the relative positions of the Fermi level and the antidot potential. A quantum dot lattice, on the other hand, provides the opportunity to study correlated electron physics. We find that its current-voltage characteristics display a voltage threshold, as well as a power law scaling, indicative of collective Coulomb blockade in a disordered background

  18. Next Generation Offline Approaches to Trace Gas-Phase Organic Compound Speciation: Sample Collection and Analysis

    Science.gov (United States)

    Sheu, R.; Marcotte, A.; Khare, P.; Ditto, J.; Charan, S.; Gentner, D. R.

    2017-12-01

    Intermediate-volatility and semi-volatile organic compounds (I/SVOCs) are major precursors to secondary organic aerosol, and contribute to tropospheric ozone formation. Their wide volatility range, chemical complexity, behavior in analytical systems, and trace concentrations present numerous hurdles to characterization. We present an integrated sampling-to-analysis system for the collection and offline analysis of trace gas-phase organic compounds with the goal of preserving and recovering analytes throughout sample collection, transport, storage, and thermal desorption for accurate analysis. Custom multi-bed adsorbent tubes are used to collect samples for offline analysis by advanced analytical detectors. The analytical instrumentation comprises an automated thermal desorption system that introduces analytes from the adsorbent tubes into a gas chromatograph, which is coupled with an electron ionization mass spectrometer (GC-EIMS) and other detectors. In order to optimize the collection and recovery for a wide range of analyte volatility and functionalization, we evaluated a variety of commercially-available materials, including Res-Sil beads, quartz wool, glass beads, Tenax TA, and silica gel. Key properties for optimization include inertness, versatile chemical capture, minimal affinity for water, and minimal artifacts or degradation byproducts; these properties were assessed with a diverse mix of traditionally-measured and functionalized analytes. Along with a focus on material selection, we provide recommendations spanning the entire sampling-and-analysis process to improve the accuracy of future comprehensive I/SVOC measurements, including oxygenated and other functionalized I/SVOCs. We demonstrate the performance of our system by providing results on speciated VOCs-SVOCs from indoor, outdoor, and chamber studies that establish the utility of our protocols and pave the way for precise laboratory characterization via a mix of detection methods.

  19. Evaluation and application of static headspace-multicapillary column-gas chromatography-ion mobility spectrometry for complex sample analysis.

    Science.gov (United States)

    Denawaka, Chamila J; Fowlis, Ian A; Dean, John R

    2014-04-18

    An evaluation of static headspace-multicapillary column-gas chromatography-ion mobility spectrometry (SHS-MCC-GC-IMS) has been undertaken to assess its applicability for the determination of 32 volatile compounds (VCs). The key experimental variables of sample incubation time and temperature have been evaluated alongside the MCC-GC variables of column polarity, syringe temperature, injection temperature, injection volume, column temperature and carrier gas flow rate coupled with the IMS variables of temperature and drift gas flow rate. This evaluation resulted in six sets of experimental variables being required to separate the 32 VCs. The optimum experimental variables for SHS-MCC-GC-IMS, the retention time and drift time operating parameters were determined; to normalise the operating parameters, the relative drift time and normalised reduced ion mobility for each VC were determined. In addition, a full theoretical explanation is provided on the formation of the monomer, dimer and trimer of a VC. The optimum operating condition for each VC calibration data was obtained alongside limit of detection (LOD) and limit of quantitation (LOQ) values. Typical detection limits ranged from 0.1ng bis(methylthio)methane, ethylbutanoate and (E)-2-nonenal to 472ng isovaleric acid with correlation coefficient (R(2)) data ranging from 0.9793 (for the dimer of octanal) through to 0.9990 (for isobutyric acid). Finally, the developed protocols were applied to the analysis of malodour in sock samples. Initial work involved spiking an inert matrix and sock samples with appropriate concentrations of eight VCs. The average recovery from the inert matrix was 101±18% (n=8), while recoveries from the sock samples were lower, that is, 54±30% (n=8) for sock type 1 and 78±24% (n=6) for sock type 2. Finally, SHS-MCC-GC-IMS was applied to sock malodour in a field trial based on 11 volunteers (mixed gender) over a 3-week period. By applying the SHS-MCC-GC-IMS database, four VCs were

  20. Steady Secondary Flows Generated by Periodic Compression and Expansion of an Ideal Gas in a Pulse Tube

    Science.gov (United States)

    Lee, Jeffrey M.

    1999-01-01

    This study establishes a consistent set of differential equations for use in describing the steady secondary flows generated by periodic compression and expansion of an ideal gas in pulse tubes. Also considered is heat transfer between the gas and the tube wall of finite thickness. A small-amplitude series expansion solution in the inverse Strouhal number is proposed for the two-dimensional axisymmetric mass, momentum and energy equations. The anelastic approach applies when shock and acoustic energies are small compared with the energy needed to compress and expand the gas. An analytic solution to the ordered series is obtained in the strong temperature limit where the zeroth-order temperature is constant. The solution shows steady velocities increase linearly for small Valensi number and can be of order I for large Valensi number. A conversion of steady work flow to heat flow occurs whenever temperature, velocity or phase angle gradients are present. Steady enthalpy flow is reduced by heat transfer and is scaled by the Prandtl times Valensi numbers. Particle velocities from a smoke-wire experiment were compared with predictions for the basic and orifice pulse tube configurations. The theory accurately predicted the observed steady streaming.

  1. Poly-use multi-level sampling system for soil-gas transport analysis in the vadose zone.

    Science.gov (United States)

    Nauer, Philipp A; Chiri, Eleonora; Schroth, Martin H

    2013-10-01

    Soil-gas turnover is important in the global cycling of greenhouse gases. The analysis of soil-gas profiles provides quantitative information on below-ground turnover and fluxes. We developed a poly-use multi-level sampling system (PMLS) for soil-gas sampling, water-content and temperature measurement with high depth resolution and minimal soil disturbance. It is based on perforated access tubes (ATs) permanently installed in the soil. A multi-level sampler allows extraction of soil-gas samples from 20 locations within 1 m depth, while a capacitance probe is used to measure volumetric water contents. During idle times, the ATs are sealed and can be equipped with temperature sensors. Proof-of-concept experiments in a field lysimeter showed good agreement of soil-gas samples and water-content measurements compared with conventional techniques, while a successfully performed gas-tracer test demonstrated the feasibility of the PMLS to determine soil-gas diffusion coefficients in situ. A field application of the PMLS to quantify oxidation of atmospheric CH4 in a field lysimeter and in the forefield of a receding glacier yielded activity coefficients and soil-atmosphere fluxes well in agreement with previous studies. With numerous options for customization, the presented tool extends the methodological choices to investigate soil-gas transport in the vadose zone.

  2. Method and apparatus maintaining multi-component sample gas constituents in vapor phase during sample extraction and cooling

    Science.gov (United States)

    Farthing, William Earl; Felix, Larry Gordon; Snyder, Todd Robert

    2009-12-15

    An apparatus and method for diluting and cooling that is extracted from high temperature and/or high pressure industrial processes. Through a feedback process, a specialized, CFD-modeled dilution cooler is employed along with real-time estimations of the point at which condensation will occur within the dilution cooler to define a level of dilution and diluted gas temperature that results in a gas that can be conveyed to standard gas analyzers that contains no condensed hydrocarbon compounds or condensed moisture.

  3. Method and apparatus for maintaining multi-component sample gas constituents in vapor phase during sample extraction and cooling

    Science.gov (United States)

    Farthing, William Earl [Pinson, AL; Felix, Larry Gordon [Pelham, AL; Snyder, Todd Robert [Birmingham, AL

    2008-02-12

    An apparatus and method for diluting and cooling that is extracted from high temperature and/or high pressure industrial processes. Through a feedback process, a specialized, CFD-modeled dilution cooler is employed along with real-time estimations of the point at which condensation will occur within the dilution cooler to define a level of dilution and diluted gas temperature that results in a gas that can be conveyed to standard gas analyzers that contains no condensed hydrocarbon compounds or condensed moisture.

  4. k0-INAA for APM samples collected in period of June 2004 - March 2005 and some marine certified reference materials

    International Nuclear Information System (INIS)

    Dung, Ho Manh; Vu, Cao Dong; Y, Truong; Sy, Nguyen Thi

    2006-01-01

    The airborne particulate matter (APM) samples have been collected in 2004 using two types of polycarbonate membrane filter PM 2.5 and PM 2.5-10 at two sites of industrial (Ho Chi Mihn City) and rural (Dateh) regions in south of Vietnam. Three marine certified reference materials have been selected to establish a k0-NAA procedure for marine samples. The concentration of trace multi-element in the samples has been determined by the k 0 -INAA procedure using K o -DALAT software developed in Dalat NRI. About 28 elements in 224 APM samples collected at two areas of Dateh and HCMC of Vietnam in period from June, 2004 to March, 2005 were presented in report. The statistical analysis was applied to the data set to investigate the pollution source at sampling sites. The results proved that the k 0 -NAA on the Dalat research reactor is a reliable and effective analytical technique for characterization of trace multi-element in APM and marine samples for air and marine environmental pollution study in Vietnam. (author)

  5. THE CHEMICAL COMPOSITION AND VARIOUS SAMPLES PREPARATION METHODS FOR In Vitro GAS TEST OF TWO TROPICAL FEEDS

    Directory of Open Access Journals (Sweden)

    J. Daryatmo

    2015-04-01

    Full Text Available A 3x2 factorial experimental design was conducted to evaluate the chemical composition ofSesbania grandiflora (SG and Manihot esculenta Crantz (MEC leaves and to measure the effects ofpreparation and drying methods on the in vitro gas production in the presence and absence of PEG. Thecollected samples were divided into three groups: One group was fresh samples (F. The second groupwas oven-dried at 55°C for 48h (OD and the last group was freeze-dried at –40°C for 72h (FD. Resultsshowed that the mean value of gas production from fresh SG and MEC samples were not significantlyhigher (P<0.05 than from FD and OD samples. In SG and MEC, the mean value of gas production ofFD was not significant compared to OD samples (P>0.05. Gas production from samples added withPEG were higher (P<0.05 than without PEG. In conclusion, the preparation and drying methods of feedsamples could affect the volume of gas production. The addition of PEG in SG and MEC resulted inhigher gas production volumes.

  6. Two-dimensional gas chromatography-online hydrogenation for improved characterization of petrochemical samples.

    Science.gov (United States)

    Potgieter, H; Bekker, R; Govender, A; Rohwer, E

    2016-05-06

    The Fischer-Tropsch (FT) process produces a variety of hydrocarbons over a wide carbon number range and during subsequent product workup a large variety of synthetic fuels and chemicals are produced. The complexity of the product slate obtained from this process is well documented and the high temperature FT (HT-FT) process products are spread over gas, oil and water phases. The characterization of these phases is very challenging even when using comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC×GC-TOFMS). Despite the increase in separation power, peak co-elution still occurs when samples containing isomeric compounds are analysed by comprehensive two dimensional GC. The separation of isomeric compounds with the same double bond equivalents is especially difficult since these compounds elute in a similar position on the GC×GC chromatogram and have identical molecular masses and similar fragmentation patterns in their electron ionization (EI) mass spectra. On-line hydrogenation after GC×GC separation is a possible way to distinguish between these isomeric compounds since the number of rings and alkene double bonds can be determined from the mass spectra of the compounds before and after hydrogenation. This paper describes development of a GC×GC method with post column hydrogenation for the determination of the backbone of cyclic/olefinic structures enabling us to differentiate between classes like dienes and cyclic olefins in complex petrochemical streams. Copyright © 2016 Elsevier B.V. All rights reserved.

  7. Systematic comparison of static and dynamic headspace sampling techniques for gas chromatography.

    Science.gov (United States)

    Kremser, Andreas; Jochmann, Maik A; Schmidt, Torsten C

    2016-09-01

    Six automated, headspace-based sample preparation techniques were used to extract volatile analytes from water with the goal of establishing a systematic comparison between commonly available instrumental alternatives. To that end, these six techniques were used in conjunction with the same gas chromatography instrument for analysis of a common set of volatile organic carbon (VOC) analytes. The methods were thereby divided into three classes: static sampling (by syringe or loop), static enrichment (SPME and PAL SPME Arrow), and dynamic enrichment (ITEX and trap sampling). For PAL SPME Arrow, different sorption phase materials were also included in the evaluation. To enable an effective comparison, method detection limits (MDLs), relative standard deviations (RSDs), and extraction yields were determined and are discussed for all techniques. While static sampling techniques exhibited sufficient extraction yields (approx. 10-20 %) to be reliably used down to approx. 100 ng L(-1), enrichment techniques displayed extraction yields of up to 80 %, resulting in MDLs down to the picogram per liter range. RSDs for all techniques were below 27 %. The choice on one of the different instrumental modes of operation (aforementioned classes) was thereby the most influential parameter in terms of extraction yields and MDLs. Individual methods inside each class showed smaller deviations, and the least influences were observed when evaluating different sorption phase materials for the individual enrichment techniques. The option of selecting specialized sorption phase materials may, however, be more important when analyzing analytes with different properties such as high polarity or the capability of specific molecular interactions. Graphical Abstract PAL SPME Arrow during the extraction of volatile analytes from the headspace of an aqueous sample.

  8. Simultaneous determination of organophosphorous insecticides in bean samples by gas chromatography - flame photometric detection

    Directory of Open Access Journals (Sweden)

    Keyller Bastos Borges

    2014-02-01

    Full Text Available The indiscriminate use of organophosphorous pesticides (OPPs in crops may leave residues in food and may cause poisoning in the applicators. A method was developed for the determination of five OPPs in bean samples by Gas Chromatography-Flame Photometric Detection (GC-FPD. Validation parameters comprised linearity between 0.24 and 8.56 μg g-1 (r = 0.9985 for diazinon; 0.23 and 8.14 μg g-1 (r = 0.9959 for methyl parathion; 0.28 and 10.25 μg g-1 (r = 0.9987 for methyl pirimiphos; 0.52 and 18.87 μg g-1 (r = 0.9955 for malathion; 0.86 and 13.67 μg g-1 (r = 0.9919 for ethion. The limits of quantification (equal to those of detection were the lowest rates of ranges mentioned above for each compound. The extraction method showed approximately 95% recovery, with CV% < 15%. Although twenty-eight bean samples obtained in the southern region of the state of Minas Gerais,Brazil, were analyzed, they failed to match any of the OPPs under analysis. The absence of OPPs in the samples could be due to the degradation that occurred between the use of OPPs and bean commercialization, levels below the detection /quantification limits and the non-use of OPPs in bean cultivation.

  9. A sampling-based Bayesian model for gas saturation estimationusing seismic AVA and marine CSEM data

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Jinsong; Hoversten, Michael; Vasco, Don; Rubin, Yoram; Hou,Zhangshuan

    2006-04-04

    We develop a sampling-based Bayesian model to jointly invertseismic amplitude versus angles (AVA) and marine controlled-sourceelectromagnetic (CSEM) data for layered reservoir models. The porosityand fluid saturation in each layer of the reservoir, the seismic P- andS-wave velocity and density in the layers below and above the reservoir,and the electrical conductivity of the overburden are considered asrandom variables. Pre-stack seismic AVA data in a selected time windowand real and quadrature components of the recorded electrical field areconsidered as data. We use Markov chain Monte Carlo (MCMC) samplingmethods to obtain a large number of samples from the joint posteriordistribution function. Using those samples, we obtain not only estimatesof each unknown variable, but also its uncertainty information. Thedeveloped method is applied to both synthetic and field data to explorethe combined use of seismic AVA and EM data for gas saturationestimation. Results show that the developed method is effective for jointinversion, and the incorporation of CSEM data reduces uncertainty influid saturation estimation, when compared to results from inversion ofAVA data only.

  10. Vapor and gas sampling of single-shell tank 241-B-102 using the in situ vapor sampling system

    International Nuclear Information System (INIS)

    Lockrem, L.L.

    1997-01-01

    The Vapor Issue Resolution Program tasked the Vapor Team (the team) to collect representative headspace samples from Hanford Site single-shell tank (SST) 241-B-102. This document presents sampling data resulting from the April 18, 1996 sampling of SST 241-B-102. Analytical results will be presented in a separate report issued by Pacific Northwest National Laboratory (PNNL), which supplied and analyzed the sampling media. The team, consisting of Sampling and Mobile Laboratories (SML) and Special Analytical Studies (SAS) personnel, used the vapor sampling system (VSS) to collect representative samples of the air, gases, and vapors from the headspace of SST 241-B-102 with sorbent traps and SUMMA canisters

  11. Phase identification of quasi-periodic flow measured by particle image velocimetry with a low sampling rate

    International Nuclear Information System (INIS)

    Pan, Chong; Wang, Hongping; Wang, Jinjun

    2013-01-01

    This work mainly deals with the proper orthogonal decomposition (POD) time coefficient method used for extracting phase information from quasi-periodic flow. The mathematical equivalence between this method and the traditional cross-correlation method is firstly proved. A two-dimensional circular cylinder wake flow measured by time-resolved particle image velocimetry within a range of Reynolds numbers is then used to evaluate the reliability of this method. The effect of both the sampling rate and Reynolds number on the identification accuracy is finally discussed. It is found that the POD time coefficient method provides a convenient alternative for phase identification, whose feasibility in low-sampling-rate measurement has additional advantages for experimentalists. (paper)

  12. Application of end-tidal carbon dioxide monitoring via distal gas samples in ventilated neonates.

    Science.gov (United States)

    Jin, Ziying; Yang, Maoying; Lin, Ru; Huang, Wenfang; Wang, Jiangmei; Hu, Zhiyong; Shu, Qiang

    2017-08-01

    Previous research has suggested correlations between the end-tidal partial pressure of carbon dioxide (P ET CO 2 ) and the partial pressure of arterial carbon dioxide (PaCO 2 ) in mechanically ventilated patients, but both the relationship between P ET CO 2 and PaCO 2 and whether P ET CO 2 accurately reflects PaCO 2 in neonates and infants are still controversial. This study evaluated remote sampling of P ET CO 2 via an epidural catheter within an endotracheal tube to determine the procedure's clinical safety and efficacy in the perioperative management of neonates. Abdominal surgery was performed under general anesthesia in 86 full-term newborns (age 1-30 days, weight 2.55-4.0 kg, American Society of Anesthesiologists class I or II). The infants were divided into 2 groups (n = 43 each), and carbon dioxide (CO 2 ) gas samples were collected either from the conventional position (the proximal end) or a modified position (the distal end) of the epidural catheter. The P ET CO 2 measured with the new method was significantly higher than that measured with the traditional method, and the difference between P ET CO 2 and PaCO 2 was also reduced. The accuracy of P ET CO 2 measured increased from 78.7% to 91.5% when the modified sampling method was used. The moderate correlation between P ET CO 2 and PaCO 2 by traditional measurement was 0.596, which significantly increased to 0.960 in the modified sampling group. Thus, the P ET CO 2 value was closer to that of PaCO 2 . P ET CO 2 detected via modified carbon dioxide monitoring had a better accuracy and correlation with PaCO 2 in neonates. Copyright © 2017. Published by Elsevier B.V.

  13. A membrane inlet mass spectrometry system for noble gases at natural abundances in gas and water samples.

    Science.gov (United States)

    Visser, Ate; Singleton, Michael J; Hillegonds, Darren J; Velsko, Carol A; Moran, Jean E; Esser, Bradley K

    2013-11-15

    Noble gases dissolved in groundwater can reveal paleotemperatures, recharge conditions, and precise travel times. The collection and analysis of noble gas samples are cumbersome, involving noble gas purification, cryogenic separation and static mass spectrometry. A quicker and more efficient sample analysis method is required for introduced tracer studies and laboratory experiments. A Noble Gas Membrane Inlet Mass Spectrometry (NG-MIMS) system was developed to measure noble gases at natural abundances in gas and water samples. The NG-MIMS system consists of a membrane inlet, a dry-ice water trap, a carbon-dioxide trap, two getters, a gate valve, a turbomolecular pump and a quadrupole mass spectrometer equipped with an electron multiplier. Noble gases isotopes (4)He, (22)Ne, (38)Ar, (84)Kr and (132)Xe are measured every 10 s. The NG-MIMS system can reproduce measurements made on a traditional noble gas mass spectrometer system with precisions of 2%, 8%, 1%, 1% and 3% for He, Ne, Ar, Kr and Xe, respectively. Noble gas concentrations measured in an artificial recharge pond were used to monitor an introduced xenon tracer and to reconstruct temperature variations to within 2 °C. Additional experiments demonstrated the capability to measure noble gases in gas and in water samples, in real time. The NG-MIMS system is capable of providing analyses sufficiently accurate and precise for introduced noble gas tracers at managed aquifer recharge facilities, groundwater fingerprinting based on excess air and noble gas recharge temperature, and field and laboratory studies investigating ebullition and diffusive exchange. Copyright © 2013 John Wiley & Sons, Ltd.

  14. Vapor and gas sampling of single-shell tank 241-S-106 using the in situ vapor sampling system

    International Nuclear Information System (INIS)

    Lockrem, L.L.

    1997-01-01

    The Vapor Issue Resolution Program tasked the Vapor Team (VT) to collect representative headspace samples from Hanford Site single-shell tank (SST) 241-S-106. This document presents In Situ vapor Sampling System (ISVS) data resulting from the June 13, 1996 sampling of SST 241-S-106. Analytical results will be presented in separate reports issued by the Pacific Northwest National Laboratory (PNNL) which'supplied and analyzed the sample media

  15. Vapor and gas sampling of single-shell tank 241-U-104 using the in situ vapor sampling system

    International Nuclear Information System (INIS)

    Lockrem, L.L.

    1997-01-01

    The Vapor Issue.Resolution Program tasked the Vapor Team (VT) to collect representative headspace samples from Hanford Site single-shell tank (SST) 241-U-104. This document presents In Situ Vapor Sampling System (ISVS) data resulting from the July 16, 1996 sampling of SST 241-U-104. Analytical results will be presented in separate reports issued by the Pacific Northwest National Laboratory (PNNL) which supplied and analyzed the sample media

  16. Vapor and gas sampling of single-shell tank 241-BX-110 using the in situ vapor sampling system

    International Nuclear Information System (INIS)

    Lockrem, L.L.

    1997-01-01

    The Vapor Issue Resolution Program tasked the Vapor Team (the team) to collect representative headspace samples from Hanford Site single-shell tank (SST) 241-BX-110. This document presents sampling data resulting from the April 30, 1996 sampling of SST 241-BX-110. Analytical results will be presented in a separate report issued by Pacific Northwest National Laboratory (PNNL), which supplied and analyzed the sampling media

  17. Vapor and gas sampling of single-shell tank 241-S-103 using the in situ vapor sampling system

    International Nuclear Information System (INIS)

    Lockrem, L.L.

    1997-01-01

    The Vapor Issue Resolution Program tasked the Vapor Team (VT) to collect representative headspace samples from Hanford Site single-shell tank (SST) 241-S-103. This document presents In Situ Vapor Sampling System (ISVS) data resulting from the June 12, 1996 sampling of SST 241-S-103. Analytical results will be presented in separate reports issued by the Pacific Northwest National Laboratory (PNNL) which supplied and analyzed the sample media

  18. ANALYSIS AND IDENTIFICATION SPIKING CHEMICAL COMPOUNDS RELATED TO CHEMICAL WEAPON CONVENTION IN UNKNOWN WATER SAMPLES USING GAS CHROMATOGRAPHY AND GAS CHROMATOGRAPHY ELECTRON IONIZATION MASS SPECTROMETRY

    Directory of Open Access Journals (Sweden)

    Harry Budiman

    2010-06-01

    Full Text Available The identification and analysis of chemical warfare agents and their degradation products is one of important component for the implementation of the convention. Nowadays, the analytical method for determination chemical warfare agent and their degradation products has been developing and improving. In order to get the sufficient analytical data as recommended by OPCW especially in Proficiency Testing, the spiking chemical compounds related to Chemical Weapon Convention in unknown water sample were determined using two different techniques such as gas chromatography and gas chromatography electron-impact ionization mass spectrometry. Neutral organic extraction, pH 11 organic extraction, cation exchanged-methylation, triethylamine/methanol-silylation were performed to extract the chemical warfare agents from the sample, before analyzing with gas chromatography. The identification of chemical warfare agents was carried out by comparing the mass spectrum of chemicals with mass spectrum reference from the OPCW Central Analytical Database (OCAD library while the retention indices calculation obtained from gas chromatography analysis was used to get the confirmation and supported data of  the chemical warfare agents. Diisopropyl methylphosphonate, 2,2-diphenyl-2-hydroacetic acid and 3-quinuclidinol were found in unknown water sample. Those chemicals were classified in schedule 2 as precursor or reactant of chemical weapons compound in schedule list of Chemical Weapon Convention.   Keywords: gas chromatography, mass spectrometry, retention indices, OCAD library, chemical warfare agents

  19. Friends of hot Jupiters. I. A radial velocity search for massive, long-period companions to close-in gas giant planets

    Energy Technology Data Exchange (ETDEWEB)

    Knutson, Heather A.; Ngo, Henry; Johnson, John Asher [Division of Geological and Planetary Sciences, California Institute of Technology, Pasadena, CA 91125 (United States); Fulton, Benjamin J.; Howard, Andrew W. [Institute for Astronomy, University of Hawaii at Manoa, Honolulu, HI (United States); Montet, Benjamin T.; Kao, Melodie; Hinkley, Sasha; Morton, Timothy D.; Muirhead, Philip S. [Cahill Center for Astronomy and Astrophysics, California Institute of Technology, 1200 East California Boulevard, MC 249-17, Pasadena, CA 91125 (United States); Crepp, Justin R. [Department of Physics, University of Notre Dame, Notre Dame, IN (United States); Bakos, Gaspar Á. [Department of Astrophysical Sciences, Princeton University, Princeton, NJ (United States); Batygin, Konstantin, E-mail: hknutson@caltech.edu [Harvard-Smithsonian Center for Astrophysics, Cambridge, MA (United States)

    2014-04-20

    In this paper we search for distant massive companions to known transiting gas giant planets that may have influenced the dynamical evolution of these systems. We present new radial velocity observations for a sample of 51 planets obtained using the Keck HIRES instrument, and find statistically significant accelerations in fifteen systems. Six of these systems have no previously reported accelerations in the published literature: HAT-P-10, HAT-P-22, HAT-P-29, HAT-P-32, WASP-10, and XO-2. We combine our radial velocity fits with Keck NIRC2 adaptive optics (AO) imaging data to place constraints on the allowed masses and orbital periods of the companions responsible for the detected accelerations. The estimated masses of the companions range between 1-500 M {sub Jup}, with orbital semi-major axes typically between 1-75 AU. A significant majority of the companions detected by our survey are constrained to have minimum masses comparable to or larger than those of the transiting planets in these systems, making them candidates for influencing the orbital evolution of the inner gas giant. We estimate a total occurrence rate of 51% ± 10% for companions with masses between 1-13 M {sub Jup} and orbital semi-major axes between 1-20 AU in our sample. We find no statistically significant difference between the frequency of companions to transiting planets with misaligned or eccentric orbits and those with well-aligned, circular orbits. We combine our expanded sample of radial velocity measurements with constraints from transit and secondary eclipse observations to provide improved measurements of the physical and orbital characteristics of all of the planets included in our survey.

  20. Pluri annual indicative plan of the investments in the gas sector; Plan indicatif pluriannuel des investissements dans le secteur du gaz Periode 2006-2015

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2007-03-15

    This indicative plan constitutes the first report to the Parliament. It is a prospective document for the period 2006-2015 containing: a forecast of the gas demand increase, a description of main investments decided in matter of gas infrastructures, a diagnostic concerning the adequation between the supplying capacities in natural gas and the national needs, a series of recommendations on the State tools to guarantee the national supplying security and on the investment. The four parts deal with the stakes and perspectives of the national natural gas supplying, the demand evolution, the offer evolution and the equilibrium offer. (A.L.B.)

  1. Dimerization Products of Chloroprene are Background Contaminants Emitted from ALTEF (Polyvinylidene Difluoride) Gas Sampling Bags.

    Science.gov (United States)

    Kwak, Jae; Fan, Maomian; Martin, Jennifer A; Ott, Darrin K; Grigsby, Claude C

    2017-01-01

    Gas sampling bags have been used for collecting air samples. Tedlar bags are most commonly used, but bleed background chemicals such as N,N-dimethylacetamide and phenol. It is often necessary to remove the contaminant by flushing the bags with pure nitrogen or air. In this study, we identified four chloroprene dimerization products as background contaminants emitted from ALTEF bags that are made of a proprietary polyvinylidene difluoride (PVDF). No monomer chloroprene was detected in the bags analyzed. All of the dimers gradually increased once bags were filled with nitrogen due to diffusion from the bag surface. Flushing the bags with nitrogen reduced their concentrations, but was not effective for removing the contaminants. When the bags that had been flushed with nitrogen 5 times were left for 24 h, they increased again, indicating that the dimers were constantly emitted from the ALTEF bag surface. To our knowledge, these compounds have never been demonstrated in ALTEF or other PVDF bags. Our finding indicates that ALTEF might be incorporated with Neoprene (chloroprene-based polymer) during its manufacturing process.

  2. Position-specific 13C distributions within propane from experiments and natural gas samples

    Science.gov (United States)

    Piasecki, Alison; Sessions, Alex; Lawson, Michael; Ferreira, A. A.; Santos Neto, E. V.; Ellis, Geoffrey S.; Lewan, Michael D.; Eiler, John M.

    2018-01-01

    Site-specific carbon isotope measurements of organic compounds potentially recover information that is lost in a conventional, 'bulk' isotopic analysis. Such measurements are useful because isotopically fractionating processes may have distinct effects at different molecular sites, and thermodynamically equilibrated populations of molecules tend to concentrate heavy isotopes in one molecular site versus another. Most recent studies of site-specific 13C in organics use specialized Nuclear Magnetic Resonance (NMR) techniques or complex chemical degradations prior to mass spectrometric measurements. Herein we present the first application of a new mass spectrometric technique that reconstructs the site-specific carbon isotope composition of propane based on measurements of the 13C/12C ratios of two or more fragment ions that sample different proportions of the terminal and central carbon sites. We apply this method to propane from laboratory experiments and natural gas samples to explore the relationships between site-specific carbon isotope composition, full-molecular δ13C, thermal maturity, and variation in organic matter precursors. Our goal is to advance the understanding of the sources and histories of short-chain alkanes within geologic systems. Our findings suggest that propane varies in its site-specific carbon isotope structure, which is correlated with increasing thermal maturity, first increasing in terminal position δ13C and then increasing in both center and terminal position δ13C. This pattern is observed in both experimental and natural samples, and is plausibly explained by a combination of site-specific, temperature-dependent isotope effects associated with conversion of different precursor molecules (kerogen, bitumen, and/or oil) to propane, differences in site-specific isotopic contents of those precursors, and possibly distillation of reactive components of those precursors with increasing maturity. We hypothesize that the largest changes in

  3. Position-specific 13C distributions within propane from experiments and natural gas samples

    Science.gov (United States)

    Piasecki, Alison; Sessions, Alex L.; Lawson, Michael; Ferreira, A.A.; Santos Neto, E. V.; Ellis, Geoffrey S.; Lewan, Michael; Eilers, J.M.

    2018-01-01

    Site-specific carbon isotope measurements of organic compounds potentially recover information that is lost in a conventional, ‘bulk’ isotopic analysis. Such measurements are useful because isotopically fractionating processes may have distinct effects at different molecular sites, and thermodynamically equilibrated populations of molecules tend to concentrate heavy isotopes in one molecular site versus another. Most recent studies of site-specific 13C in organics use specialized Nuclear Magnetic Resonance (NMR) techniques or complex chemical degradations prior to mass spectrometric measurements. Herein we present the first application of a new mass spectrometric technique that reconstructs the site-specific carbon isotope composition of propane based on measurements of the 13C/12C ratios of two or more fragment ions that sample different proportions of the terminal and central carbon sites. We apply this method to propane from laboratory experiments and natural gas samples to explore the relationships between site-specific carbon isotope composition, full-molecular δ13C, thermal maturity, and variation in organic matter precursors. Our goal is to advance the understanding of the sources and histories of short-chain alkanes within geologic systems. Our findings suggest that propane varies in its site-specific carbon isotope structure, which is correlated with increasing thermal maturity, first increasing in terminal position δ13C and then increasing in both center and terminal position δ13C. This pattern is observed in both experimental and natural samples, and is plausibly explained by a combination of site-specific, temperature-dependent isotope effects associated with conversion of different precursor molecules (kerogen, bitumen, and/or oil) to propane, differences in site-specific isotopic contents of those precursors, and possibly distillation of reactive components of those precursors with increasing maturity. We hypothesize that the largest changes in

  4. Bringing a needle to a laser fight: comparing greenhouse gas sampling methods with gas chromatography and fourier transform infrared spectroscopy

    Science.gov (United States)

    As scientists, producers, policymakers, and the general public become more concerned about impacts of climate change, there is an increasing need to understand and quantify greenhouse gas emissions from agricultural practices, which often feed into global, multi-institution databases. Current best p...

  5. Innovative method for carbon dioxide determination in human postmortem cardiac gas samples using headspace-gas chromatography–mass spectrometry and stable labeled isotope as internal standard

    International Nuclear Information System (INIS)

    Varlet, V.; Smith, F.; Froidmont, S. de; Dominguez, A.; Rinaldi, A.; Augsburger, M.; Mangin, P.; Grabherr, S.

    2013-01-01

    Graphical abstract: -- Highlights: •We developed a method for CO 2 analysis in cardiac samples and quantification by 13 CO 2 . •This method was fully validated by accuracy profile. •We have applied this method to perform CO 2 precise quantification for forensic applications. •Context of the death could be documented following CO 2 concentrations. -- Abstract: A novel approach to measure carbon dioxide (CO 2 ) in gaseous samples, based on a precise and accurate quantification by 13 CO 2 internal standard generated in situ is presented. The main goal of this study was to provide an innovative headspace-gas chromatography–mass spectrometry (HS-GC–MS) method applicable in the routine determination of CO 2 . The main drawback of the GC methods discussed in the literature for CO 2 measurement is the lack of a specific internal standard necessary to perform quantification. CO 2 measurement is still quantified by external calibration without taking into account analytical problems which can often occur considering gaseous samples. To avoid the manipulation of a stable isotope-labeled gas, we have chosen to generate in situ an internal labeled standard gas ( 13 CO 2 ) on the basis of the stoichiometric formation of CO 2 by the reaction of hydrochloric acid (HCl) with sodium hydrogen carbonate (NaH 13 CO 3 ). This method allows a precise measurement of CO 2 concentration and was validated on various human postmortem gas samples in order to study its efficiency

  6. A policy of routine umbilical cord blood gas analysis decreased missing samples from high-risk births.

    Science.gov (United States)

    Ahlberg, M; Elvander, C; Johansson, S; Cnattingius, S; Stephansson, O

    2017-01-01

    This study compared obstetric units practicing routine or selective umbilical cord blood gas analysis, with respect to the risk of missing samples in high-risk deliveries and in infants with birth asphyxia. This was a Swedish population-based cohort study that used register data for 155 235 deliveries of live singleton infants between 2008 and 2014. Risk ratios and 95% confidence intervals were calculated to estimate the association between routine and selective umbilical cord blood gas sampling strategies and the risk of missing samples. Selective sampling increased the risk ratios when routine sampling was used as the reference, with a value of 1.0, and these were significant in high-risk deliveries and birth asphyxia. The risk ratios for selective sampling were large-for-gestational age (9.07), preterm delivery at up to 36 weeks of gestation (8.24), small-for-gestational age (7.94), two or more foetal scalp blood samples (5.96), an Apgar score of less than seven at one minute (2.36), emergency Caesarean section (1.67) and instrumental vaginal delivery (1.24). Compared with routine sampling, selective umbilical cord blood gas sampling significantly increased the risks of missing samples in high-risk deliveries and in infants with birth asphyxia. ©2016 Foundation Acta Paediatrica. Published by John Wiley & Sons Ltd.

  7. Preparation of {sup 183,184}Re samples for modelling a rapid gas phase chemistry of Nielsbohrium (Ns), element 107

    Energy Technology Data Exchange (ETDEWEB)

    Eichler, R.; Gaeggeler, H.W.; Eichler, B.; Tuerler, A. [Paul Scherrer Inst. (PSI), Villigen (Switzerland)

    1997-09-01

    Chemical gas phase reactions of the heavier group 7 elements in the system O{sub 2}/H{sub 2}O are presumably best suited for a separation of Nielsbohrium from the lighter transactinides. We expect a higher reaction velocity using the more reactive gas system O{sub 3}/H{sub 2}O{sub 2}. For the experimental verification of this idea we prepared {sup 183}Re/{sup 184}Re samples for thermochromatography experiments with both gas systems. (author) 8 refs.

  8. U.S. Geological Survey Noble Gas Laboratory’s standard operating procedures for the measurement of dissolved gas in water samples

    Science.gov (United States)

    Hunt, Andrew G.

    2015-08-12

    This report addresses the standard operating procedures used by the U.S. Geological Survey’s Noble Gas Laboratory in Denver, Colorado, U.S.A., for the measurement of dissolved gases (methane, nitrogen, oxygen, and carbon dioxide) and noble gas isotopes (helium-3, helium-4, neon-20, neon-21, neon-22, argon-36, argon-38, argon-40, kryton-84, krypton-86, xenon-103, and xenon-132) dissolved in water. A synopsis of the instrumentation used, procedures followed, calibration practices, standards used, and a quality assurance and quality control program is presented. The report outlines the day-to-day operation of the Residual Gas Analyzer Model 200, Mass Analyzer Products Model 215–50, and ultralow vacuum extraction line along with the sample handling procedures, noble gas extraction and purification, instrument measurement procedures, instrumental data acquisition, and calculations for the conversion of raw data from the mass spectrometer into noble gas concentrations per unit mass of water analyzed. Techniques for the preparation of artificial dissolved gas standards are detailed and coupled to a quality assurance and quality control program to present the accuracy of the procedures used in the laboratory.

  9. Sampling and Analysis of the Headspace Gas in 3013 Type Plutonium Storage Containers at Los Alamos National Laboratory

    International Nuclear Information System (INIS)

    Jackson, Jay M.; Berg, John M.; Hill, Dallas D.; Worl, Laura A.; Veirs, Douglas K.

    2012-01-01

    Department of Energy (DOE) sites have packaged approximately 5200 3013 containers to date. One of the requirements specified in DOESTD-3013, which specifies requirements for packaging plutonium bearing materials, is that the material be no greater than 0.5 weight percent moisture. The containers are robust, nested, welded vessels. A shelf life surveillance program was established to monitor these cans over their 50 year design life. In the event pressurization is detected by radiography, it will be necessary to obtain a head space gas sample from the pressurized container. This technique is also useful to study the head space gas in cans selected for random destructive evaluation. The atmosphere is sampled and the hydrogen to oxygen ratio is measured to determine the effects of radiolysis on the moisture in the container. A system capable of penetrating all layers of a 3013 container assembly and obtaining a viable sample of the enclosed gas and an estimate of internal pressure was designed.

  10. Cluster chemical ionization for improved confidence level in sample identification by gas chromatography/mass spectrometry.

    Science.gov (United States)

    Fialkov, Alexander B; Amirav, Aviv

    2003-01-01

    Upon the supersonic expansion of helium mixed with vapor from an organic solvent (e.g. methanol), various clusters of the solvent with the sample molecules can be formed. As a result of 70 eV electron ionization of these clusters, cluster chemical ionization (cluster CI) mass spectra are obtained. These spectra are characterized by the combination of EI mass spectra of vibrationally cold molecules in the supersonic molecular beam (cold EI) with CI-like appearance of abundant protonated molecules, together with satellite peaks corresponding to protonated or non-protonated clusters of sample compounds with 1-3 solvent molecules. Like CI, cluster CI preferably occurs for polar compounds with high proton affinity. However, in contrast to conventional CI, for non-polar compounds or those with reduced proton affinity the cluster CI mass spectrum converges to that of cold EI. The appearance of a protonated molecule and its solvent cluster peaks, plus the lack of protonation and cluster satellites for prominent EI fragments, enable the unambiguous identification of the molecular ion. In turn, the insertion of the proper molecular ion into the NIST library search of the cold EI mass spectra eliminates those candidates with incorrect molecular mass and thus significantly increases the confidence level in sample identification. Furthermore, molecular mass identification is of prime importance for the analysis of unknown compounds that are absent in the library. Examples are given with emphasis on the cluster CI analysis of carbamate pesticides, high explosives and unknown samples, to demonstrate the usefulness of Supersonic GC/MS (GC/MS with supersonic molecular beam) in the analysis of these thermally labile compounds. Cluster CI is shown to be a practical ionization method, due to its ease-of-use and fast instrumental conversion between EI and cluster CI, which involves the opening of only one valve located at the make-up gas path. The ease-of-use of cluster CI is analogous

  11. Materials processing issues for non-destructive laser gas sampling (NDLGS)

    Energy Technology Data Exchange (ETDEWEB)

    Lienert, Thomas J [Los Alamos National Laboratory

    2010-12-09

    The Non-Destructive Laser Gas Sampling (NDLGS) process essentially involves three steps: (1) laser drilling through the top of a crimped tube made of 304L stainles steel (Hammar and Svennson Cr{sub eq}/Ni{sub eq} = 1.55, produced in 1985); (2) gas sampling; and (3) laser re-welding of the crimp. All three steps are performed in a sealed chamber with a fused silica window under controlled vacuum conditions. Quality requirements for successful processing call for a hermetic re-weld with no cracks or other defects in the fusion zone or HAZ. It has been well established that austenitic stainless steels ({gamma}-SS), such as 304L, can suffer from solidification cracking if their Cr{sub eq}/Ni{sub eq} is below a critical value that causes solidification to occur as austenite (fcc structure) and their combined impurity level (%P+%S) is above {approx}0.02%. Conversely, for Cr{sub eq}/Ni{sub eq} values above the critical level, solidification occurs as ferrite (bcc structure), and cracking propensity is greatly reduced at all combined impurity levels. The consensus of results from studies of several researchers starting in the late 1970's indicates that the critical Cr{sub eq}/Ni{sub eq} value is {approx}1.5 for arc welds. However, more recent studies by the author and others show that the critical Cr{sub eq}/Ni{sub eq} value increases to {approx}1 .6 for weld processes with very rapid thermal cycles, such as the pulsed Nd:YAG laser beam welding (LBW) process used here. Initial attempts at NDLGS using pulsed LBW resulted in considerable solidification cracking, consistent with the results of work discussed above. After a brief introduction to the welding metallurgy of {gamma}-SS, this presentation will review the results of a study aimed at developing a production-ready process that eliminates cracking. The solution to the cracking issue, developed at LANL, involved locally augmenting the Cr content by applying either Cr or a Cr-rich stainless steel (ER 312) to the top

  12. Enhancing the Frequency Adaptability of Periodic Current Controllers with a Fixed Sampling Rate for Grid-Connected Power Converters

    DEFF Research Database (Denmark)

    Yang, Yongheng; Zhou, Keliang; Blaabjerg, Frede

    2016-01-01

    Grid-connected power converters should employ advanced current controllers, e.g., Proportional Resonant (PR) and Repetitive Controllers (RC), in order to produce high-quality feed-in currents that are required to be synchronized with the grid. The synchronization is actually to detect...... of the resonant controllers and by approximating the fractional delay using a Lagrange interpolating polynomial for the RC, respectively, the frequency-variation-immunity of these periodic current controllers with a fixed sampling rate is improved. Experiments on a single-phase grid-connected system are presented...... the instantaneous grid information (e.g., frequency and phase of the grid voltage) for the current control, which is commonly performed by a Phase-Locked-Loop (PLL) system. Hence, harmonics and deviations in the estimated frequency by the PLL could lead to current tracking performance degradation, especially...

  13. Alternative sorptive extraction method for gas chromatography determination of halogenated anisoles in water and wine samples

    International Nuclear Information System (INIS)

    Montes, R.; Rodriguez, I.; Rubi, E.; Bollain, M.H.; Cela, R.

    2007-01-01

    An alternative sorptive microextraction method for the determination of five halogenated anisoles in water and wine matrices is proposed. Analytes were concentrated in an inexpensive and disposable piece of bulk polydimethylsiloxane (PDMS), desorbed with a small volume of organic solvent, and determined by gas chromatography with electron-capture detection (GC-ECD) or tandem mass spectrometry (GC-MS/MS). The influence of several factors on the efficiency of extraction and desorption steps was investigated in detail and the observed behaviour justified on the basis of thermodynamics and kinetics of the solid-phase microextraction technique. Under optimised conditions, analytes were first extracted in the headspace (HS) mode, at room temperature, for 2.5 h and then desorbed with 1 mL of n-pentane. This extract was further evaporated to 50 μL. The overall extraction yield of the procedure ranged from 40 to 55% and the limits of quantification remained between 0.5 and 20 ng L -1 , depending on the compound considered and the detection technique. Precision and linearity of the method were excellent for all species with both GC-ECD and GC-MS/MS detection. Matrix effects were evaluated with different water and wine samples; moreover, the suitability of the PDMS sorbent for storage of analytes, under different conditions, was demonstrated

  14. Alternative sorptive extraction method for gas chromatography determination of halogenated anisoles in water and wine samples

    Energy Technology Data Exchange (ETDEWEB)

    Montes, R. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Instituto de Investigacion y Analisis Alimentario, Universidad de Santiago de Compostela, Santiago de Compostela 15782 (Spain); Rodriguez, I. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Instituto de Investigacion y Analisis Alimentario, Universidad de Santiago de Compostela, Santiago de Compostela 15782 (Spain)], E-mail: qnisaac@usc.es; Rubi, E.; Bollain, M.H.; Cela, R. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Instituto de Investigacion y Analisis Alimentario, Universidad de Santiago de Compostela, Santiago de Compostela 15782 (Spain)

    2007-09-05

    An alternative sorptive microextraction method for the determination of five halogenated anisoles in water and wine matrices is proposed. Analytes were concentrated in an inexpensive and disposable piece of bulk polydimethylsiloxane (PDMS), desorbed with a small volume of organic solvent, and determined by gas chromatography with electron-capture detection (GC-ECD) or tandem mass spectrometry (GC-MS/MS). The influence of several factors on the efficiency of extraction and desorption steps was investigated in detail and the observed behaviour justified on the basis of thermodynamics and kinetics of the solid-phase microextraction technique. Under optimised conditions, analytes were first extracted in the headspace (HS) mode, at room temperature, for 2.5 h and then desorbed with 1 mL of n-pentane. This extract was further evaporated to 50 {mu}L. The overall extraction yield of the procedure ranged from 40 to 55% and the limits of quantification remained between 0.5 and 20 ng L{sup -1}, depending on the compound considered and the detection technique. Precision and linearity of the method were excellent for all species with both GC-ECD and GC-MS/MS detection. Matrix effects were evaluated with different water and wine samples; moreover, the suitability of the PDMS sorbent for storage of analytes, under different conditions, was demonstrated.

  15. A Principle Component Analysis of Galaxy Properties from a Large, Gas-Selected Sample

    Directory of Open Access Journals (Sweden)

    Yu-Yen Chang

    2012-01-01

    concluded that this is in conflict with the CDM model. Considering the importance of the issue, we reinvestigate the problem using the principal component analysis on a fivefold larger sample and additional near-infrared data. We use databases from the Arecibo Legacy Fast Arecibo L-band Feed Array Survey for the gas properties, the Sloan Digital Sky Survey for the optical properties, and the Two Micron All Sky Survey for the near-infrared properties. We confirm that the parameters are indeed correlated where a single physical parameter can explain 83% of the variations. When color (g-i is included, the first component still dominates but it develops a second principal component. In addition, the near-infrared color (i-J shows an obvious second principal component that might provide evidence of the complex old star formation. Based on our data, we suggest that it is premature to pronounce the failure of the CDM model and it motivates more theoretical work.

  16. Low volume sampling device for mass spectrometry analysis of gas formation in nickel-metalhydride (NiMH) batteries

    International Nuclear Information System (INIS)

    Kruesemann, P.V.E.; Mank, A.J.G.; Belfadhel-Ayeb, A.; Notten, P.H.L.

    2006-01-01

    Rechargeable nickel-metalhydride (NiMH) batteries have major advantages with respect to environmental friendliness and energy density compared to other battery systems. Research on thermodynamics and reaction kinetics is required to study the behaviour of these batteries, especially under severe operating conditions such as overcharging and (over)discharging. During these processes several reactions take place resulting in the formation of oxygen and hydrogen gas. Hence, the recombination processes should be well controlled to guarantee that the partial oxygen and hydrogen pressure inside the battery are kept low. Mass spectrometry is one of the analytical techniques capable of measuring the composition of gases released inside the battery during the charge and discharge processes. However, the sample gas needs to be withdrawn from the battery during the experiment. The gas consumption must be kept to a minimum otherwise the equilibrium inside the battery will be disturbed. A bench-top quadrupole mass spectrometer with a standard capillary by-pass inlet cannot be used for this purpose as its gas consumption is in the 1-10 ml/min range. In this paper, a new gas inlet device is presented that reduces gas consumption to a value <50 μl/h. The use of a capillary by-pass splitter and a discontinuous sampling procedure allow mass spectrometry to be used as a gas analysis tool in many applications in which small amounts of sample gas are involved. Experiments with standard AA-size NiMH batteries show that hydrogen release dominates during (over)charging at increased charging rates. Beside mass spectrometry, evolved gases are also analysed using Raman spectroscopy. Although some differences are observed, the results of similar experiments show a good agreement

  17. Design review report for rotary mode core sample truck (RMCST) modifications for flammable gas tanks, preliminary design

    International Nuclear Information System (INIS)

    Corbett, J.E.

    1996-02-01

    This report documents the completion of a preliminary design review for the Rotary Mode Core Sample Truck (RMCST) modifications for flammable gas tanks. The RMCST modifications are intended to support core sampling operations in waste tanks requiring flammable gas controls. The objective of this review was to validate basic design assumptions and concepts to support a path forward leading to a final design. The conclusion reached by the review committee was that the design was acceptable and efforts should continue toward a final design review

  18. A Gas-Spring-Loaded X-Y-Z Stage System for X-ray Microdiffraction Sample Manipulation

    International Nuclear Information System (INIS)

    Shu Deming; Cai Zhonghou; Lai, Barry

    2007-01-01

    We have designed and constructed a gas-spring-loaded x-y-z stage system for x-ray microdiffraction sample manipulation at the Advanced Photon Source XOR 2-ID-D station. The stage system includes three DC-motor-driven linear stages and a gas-spring-based heavy preloading structure, which provides antigravity forces to ensure that the stage system keeps high-positioning performance under variable goniometer orientation. Microdiffraction experiments with this new stage system showed significant sample manipulation performance improvement

  19. Early action to reduce greenhouse gas emissions before the commitment period of the Kyoto protocol: advantages and disadvantages.

    Science.gov (United States)

    Michaelowa, A; Rolfe, C

    2001-09-01

    Current "business as usual" projections suggest greenhouse gas emissions from industrialized nations will grow substantially over the next decade. However, if it comes into force, the Kyoto Protocol will require industrialized nations to reduce emissions to an average of 5% below 1990 levels in the 2008-2012 period. Taking early action to close this gap has a number of advantages. It reduces the risks of passing thresholds that trigger climate change "surprises." Early action also increases future generations' ability to choose greater levels of climate protection, and it leads to faster reductions of other pollutants. From an economic sense, early action is important because it allows shifts to less carbon-intensive technologies during the course of normal capital stock turnover. Moreover, many options for emission reduction have negative costs, and thus are economically worthwhile, because of paybacks in energy costs, healthcare costs, and other benefits. Finally, early emission reductions enhance the probability of successful ratification and lower the risk of noncompliance with the protocol. We discuss policy approaches for the period prior to 2008. Disadvantages of the current proposals for Credit for Early Action are the possibility of adverse selection due to problematic baseline calculation methods as well as the distributionary impacts of allocating a part of the emissions budget already before 2008. One simple policy without drawbacks is the so-called baseline protection, which removes the disincentive to early action due to the expectation that businesses may, in the future, receive emission rights in proportion to past emissions. It is particularly important to adopt policies that shift investment in long-lived capital stock towards less carbon-intensive technologies and to encourage innovation and technology development that will reduce future compliance costs.

  20. Protocol for Measuring the Thermal Properties of a Supercooled Synthetic Sand-water-gas-methane Hydrate Sample.

    Science.gov (United States)

    Muraoka, Michihiro; Susuki, Naoko; Yamaguchi, Hiroko; Tsuji, Tomoya; Yamamoto, Yoshitaka

    2016-03-21

    Methane hydrates (MHs) are present in large amounts in the ocean floor and permafrost regions. Methane and hydrogen hydrates are being studied as future energy resources and energy storage media. To develop a method for gas production from natural MH-bearing sediments and hydrate-based technologies, it is imperative to understand the thermal properties of gas hydrates. The thermal properties' measurements of samples comprising sand, water, methane, and MH are difficult because the melting heat of MH may affect the measurements. To solve this problem, we performed thermal properties' measurements at supercooled conditions during MH formation. The measurement protocol, calculation method of the saturation change, and tips for thermal constants' analysis of the sample using transient plane source techniques are described here. The effect of the formation heat of MH on measurement is very small because the gas hydrate formation rate is very slow. This measurement method can be applied to the thermal properties of the gas hydrate-water-guest gas system, which contains hydrogen, CO2, and ozone hydrates, because the characteristic low formation rate of gas hydrate is not unique to MH. The key point of this method is the low rate of phase transition of the target material. Hence, this method may be applied to other materials having low phase-transition rates.

  1. System for δ13C-CO2 and xCO2 analysis of discrete gas samples by cavity ring-down spectroscopy

    Science.gov (United States)

    Dickinson, Dane; Bodé, Samuel; Boeckx, Pascal

    2017-11-01

    A method was devised for analysing small discrete gas samples (50 mL syringe) by cavity ring-down spectroscopy (CRDS). Measurements were accomplished by inletting 50 mL syringed samples into an isotopic-CO2 CRDS analyser (Picarro G2131-i) between baseline readings of a reference air standard, which produced sharp peaks in the CRDS data feed. A custom software script was developed to manage the measurement process and aggregate sample data in real time. The method was successfully tested with CO2 mole fractions (xCO2) ranging from 20 000 ppm and δ13C-CO2 values from -100 up to +30 000 ‰ in comparison to VPDB (Vienna Pee Dee Belemnite). Throughput was typically 10 samples h-1, with 13 h-1 possible under ideal conditions. The measurement failure rate in routine use was ca. 1 %. Calibration to correct for memory effects was performed with gravimetric gas standards ranging from 0.05 to 2109 ppm xCO2 and δ13C-CO2 levels varying from -27.3 to +21 740 ‰. Repeatability tests demonstrated that method precision for 50 mL samples was ca. 0.05 % in xCO2 and 0.15 ‰ in δ13C-CO2 for CO2 compositions from 300 to 2000 ppm with natural abundance 13C. Long-term method consistency was tested over a 9-month period, with results showing no systematic measurement drift over time. Standardised analysis of discrete gas samples expands the scope of application for isotopic-CO2 CRDS and enhances its potential for replacing conventional isotope ratio measurement techniques. Our method involves minimal set-up costs and can be readily implemented in Picarro G2131-i and G2201-i analysers or tailored for use with other CRDS instruments and trace gases.

  2. Analysis of s-triazine herbicides in model systems and samples of groundwater by gas and liquid chromatography

    Directory of Open Access Journals (Sweden)

    Kostadinović Ljiljana

    2010-01-01

    Full Text Available In this paper, residues of s-triazine herbicides (Simazine, Atrazine, Amethrine, Promethrine and Azyprothrine have been determined in samples of model systems and real groundwater samples by gas-chromatography and high performance liquid chromatography. S-triazine herbicides were isolated from water samples by chloroform-methanol mixture (1:1, followed by purification of extract on the Al2O3 column. Gas-chromatographic determination the residues of s-triazines is performed on parallel capilar columns ULTRA I and ULTRA II, using specific NP detector. Liquid-chromatographic determination the s-triazines was performed on the column TSK ODS-120 A 5 mm 'LKB', using the mobile phase methanol-water (60:40. Total concentration of s-triazines in samples of Danube water was 3.54 mg dm-3. .

  3. Appropriate xenon-inhalation speed in xenon-enhanced CT using the end-tidal gas-sampling method

    International Nuclear Information System (INIS)

    Suga, Sadao; Toya, Shigeo; Kawase, Takeshi; Koyama, Hideki; Shiga, Hayao

    1986-01-01

    This report describes some problems when end-tidal xenon gas is substituted for the arterial xenon concentration in xenon-enhanced CT. The authors used a newly developed xenon inhalator with a xenon-gas-concentration analyzer and performed xenon-enhanced CT by means of the ''arterio-venous shunt'' method and the ''end-tidal gas-sampling'' method simultaneously. By the former method, the arterial build-up rate (K) was obtained directly from the CT slices of a blood circuit passing through the phantom. By the latter method, it was calculated from the xenon concentration of end-tidal gas sampled from the mask. The speed of xenon supply was varied between 0.6 - 1.2 L/min. in 11 patients with or without a cerebral lesion. The results revealed that rapid xenon inhalation caused a discrepancy in the arterial K between the ''shunt'' method and the ''end-tidal'' method. This discrepancy may be responsible for the mixing of inhalated gas and expired gas in respiratory dead space, such as the nasal cavity or the mask. The cerebral blood flow was underestimated because of the higher arterial K in the latter method. Too much slow inhalation, however, was timewasting, and it increased the body motion in the subanesthetic state. Therefore, an inhalation speed of the arterial K of as much as 0.2 was ideal to represent the end-tidal xenon concentration for the arterial K in the ''end-tidal gas-sampling'' method. When attention is given to this point, this method may offer a reliable absolute value in xenon-enhanced CT. (author)

  4. Development of septum-free injector for gas chromatography and its application to the samples with a high boiling point.

    Science.gov (United States)

    Ito, Hiroshi; Hayakawa, Kazuichi; Yamamoto, Atsushi; Murase, Atsushi; Hayakawa, Kazumi; Kuno, Minoru; Inoue, Yoshinori

    2006-11-03

    A novel apparatus with a simple structure has been developed for introducing samples into the vaporizing chamber of a gas chromatograph. It requires no septum due to the gas sealing structure over the carrier gas supply line. The septum-free injector made it possible to use injection port temperatures as high as 450 degrees C. Repetitive injection of samples with boiling points below 300 degrees C resulted in peak areas with relative standard deviations between 1.25 and 3.28% (n=5) and good linearity (r(2)>0.9942) for the calibration curve. In the analysis of polycyclic aromatic hydrocarbons and a base oil, the peak areas of components with high boiling points increased as the injection port temperature was increased to 450 degrees C.

  5. An X-Ray/SDSS Sample: Observational Characterization of The Outflowing Gas

    Science.gov (United States)

    Perna, Michele; Brusa, M.; Lanzuisi, G.; Mignoli, M.

    2016-10-01

    Powerful ionised AGN-driven outflows, commonly detected both locally and at high redshift, are invoked to contribute to the co-evolution of SMBH and galaxies through feedback phenomena. Our recent works (Brusa+2015; 2016; Perna+2015a,b) have shown that the XMM-COSMOS targets with evidence of outflows collected so far ( 10 sources) appear to be associated with low X-ray kbol corrections (Lbol /LX ˜ 18), in spite of their spread in obscuration, in the locations on the SFR-Mstar diagram, in their radio emission. A higher statistical significance is required to validate a connection between outflow phenomena and a X-ray loudness. Moreover, in order to validate their binding nature to the galaxy fate, it is crucial to correctly determine the outflow energetics. This requires time consuming integral field spectroscopic (IFS) observations, which are, at present, mostly limited to high luminosity objectsThe study of SDSS data offers a complementary strategy to IFS efforts. I will present physical and demographic characterization of the AGN-galaxy system during the feedback phase obtained studying a sample of 500 X-ray/SDSS AGNs, at zdispersion) and X-ray properties (intrinsic X-ray luminosity, obscuration and X-ray kbol correction), to determine what drives ionised winds. Several diagnostic line ratios have been used to infer the physical properties of the ionised outflowing gas. The knowledge of these properties can reduce the actual uncertainties in the outflow energetics by a factor of ten, pointing to improve our understanding of the AGN outflow phenomenon and its impact on galaxy evolution.

  6. Analyses of Gas, Steam and Water Samples Collected in and Around Lassen Volcanic National Park, California, 1975-2002

    Science.gov (United States)

    Janik, Cathy J.; Bergfeld, D.

    2010-01-01

    This report contains physical and chemical data from gas, steam, and water samples collected between July 1975 and September 2002 from locations in and around Lassen Volcanic National Park, California. Data are compiled as tables in Excel spreadsheets and are organized by locale. Most data are keyed to 1 of 107 site codes that are shown on local- and regional-scale maps. Brief descriptions of terminology, sampling, and analytical methods are provided.

  7. Tank 241-TY-103 headspace gas and vapor characterization results for samples collected in August 1994 and April 1995

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-09-01

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

  8. Tank 241-TX-118 headspace gas and vapor characterization results for samples collected in September 1994 and December 1994

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-01-01

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

  9. Tank 241-C-108 headspace gas and vapor characterization results for samples collected in July 1993 and August 1994

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-09-01

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

  10. Tank 241-BY-107 headspace gas and vapor characterization results for samples collected in March 1994 and October 1994

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-09-01

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

  11. Tank 241-BY-104 headspace gas and vapor characterization results for samples collected in April 1994 and June 1994

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-09-01

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

  12. Tank 241-BY-106 headspace gas and vapor characterization results for samples collected in May 1994 and July 1994

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-09-01

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

  13. Tank 241-C-112 headspace gas and vapor characterization results for samples collected in June 1994 and August 1994

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-09-01

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

  14. Tank 241-BY-103 headspace gas and vapor characterization results for samples collected in May 1994 and November 1994

    International Nuclear Information System (INIS)

    Bratzel, D.R.

    1995-01-01

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

  15. Tank 241-C-109 headspace gas and vapor characterization results for samples collected in August 1994. Revision 2

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-09-01

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

  16. Tank 241-C-111 headspace gas and vapor characterization results for samples collected in August 1993 and September 1994

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-09-01

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

  17. Tank 241-BY-108 headspace gas and vapor characterization results for samples collected in March 1994 and October 1994

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-09-01

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

  18. Tank 241-BY-110 Headspace Gas and Vapor Characterization Results for Samples Collected in November 1994. Revision 2

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-09-01

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

  19. Tank 241-C-105 headspace gas and vapor characterization results for samples collected in February 1994. Revision 1

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-09-01

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

  20. Tank 241-BY-111 headspace gas and vapor characterization results for samples collected in May 1994 and November 1994

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-01-01

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

  1. Tank 241-TY-101 headspace gas and vapor characterization results for samples collected in August 1994 and April 1995

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-09-01

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

  2. Innovative method for carbon dioxide determination in human postmortem cardiac gas samples using headspace-gas chromatography–mass spectrometry and stable labeled isotope as internal standard

    Energy Technology Data Exchange (ETDEWEB)

    Varlet, V., E-mail: vincent.varlet@chuv.ch [Toxicology and Forensic Chemistry Unit, University Center of Legal Medicine Lausanne – Geneva, CH-1011 Lausanne (Switzerland); Smith, F. [Toxicology and Forensic Chemistry Unit, University Center of Legal Medicine Lausanne – Geneva, CH-1011 Lausanne (Switzerland); Froidmont, S. de; Dominguez, A.; Rinaldi, A. [Forensic Medicine Unit, University Center of Legal Medicine Lausanne – Geneva, CH-1011 Lausanne (Switzerland); Augsburger, M. [Toxicology and Forensic Chemistry Unit, University Center of Legal Medicine Lausanne – Geneva, CH-1011 Lausanne (Switzerland); Mangin, P.; Grabherr, S. [Forensic Medicine Unit, University Center of Legal Medicine Lausanne – Geneva, CH-1011 Lausanne (Switzerland)

    2013-06-19

    Graphical abstract: -- Highlights: •We developed a method for CO{sub 2} analysis in cardiac samples and quantification by {sup 13}CO{sub 2}. •This method was fully validated by accuracy profile. •We have applied this method to perform CO{sub 2} precise quantification for forensic applications. •Context of the death could be documented following CO{sub 2} concentrations. -- Abstract: A novel approach to measure carbon dioxide (CO{sub 2}) in gaseous samples, based on a precise and accurate quantification by {sup 13}CO{sub 2} internal standard generated in situ is presented. The main goal of this study was to provide an innovative headspace-gas chromatography–mass spectrometry (HS-GC–MS) method applicable in the routine determination of CO{sub 2}. The main drawback of the GC methods discussed in the literature for CO{sub 2} measurement is the lack of a specific internal standard necessary to perform quantification. CO{sub 2} measurement is still quantified by external calibration without taking into account analytical problems which can often occur considering gaseous samples. To avoid the manipulation of a stable isotope-labeled gas, we have chosen to generate in situ an internal labeled standard gas ({sup 13}CO{sub 2}) on the basis of the stoichiometric formation of CO{sub 2} by the reaction of hydrochloric acid (HCl) with sodium hydrogen carbonate (NaH{sup 13}CO{sub 3}). This method allows a precise measurement of CO{sub 2} concentration and was validated on various human postmortem gas samples in order to study its efficiency.

  3. Sensitivity of hepatitis C virus core antigen and antibody combination assays in a global panel of window period samples

    Science.gov (United States)

    Laperche, Syria; Nubling, C. Micha; Stramer, Susan L.; Brojer, Ewa; Grabarczyk, Piotr; Yoshizawa, Hiroshi; Kalibatas, Vytenis; El Elkyabi, Magdy; Moftah, Faten; Girault, Annie; van Drimmelen, Harry; Busch, Michael P.; Lelie, Nico

    2016-01-01

    BACKGROUND Hepatitis C virus (HCV) antigen and antibody combination assays have been launched as a cost-effective alternative to nucleic acid testing (NAT) for reducing the antibody-negative window period (WP). Later, a HCV antigen chemiluminescence immunoassay (CLIA) became available. STUDY DESIGN AND METHODS A panel composed of 337 HCV NAT–yield samples that were characterized for viral load (VL) and genotype was used to compare the sensitivity of two combination enzyme-linked immunosorbent assays (Monolisa, Bio-Rad; and Murex, formerly Abbott) and a HCV antigen CLIA (Abbott). Analytic sensitivity was compared with HCV RNA detection using Ultrio (Grifols) by testing serial dilutions of 10 genotype (gt)1 to gt4 samples. RESULTS HCV antigen CLIA detected 92.4% of samples, whereas Monolisa and Murex detected 38.3 and 47.5%, respectively. In the HCV RNA VL range of 105 to 107 IU/mL, Monolisa and Murex detected 38% to 56% of gt1, 85% to 78% of gt2, and 21% to 37% of gt3. The overall geometric mean 50% limit of detection (range) of Ultrio on gt1 to gt4 dilution series was 3.5 (1.2–7.7) copies/mL, compared to 3.3 × 106 (4.4 × 105-2.7 × 107), 3.4 × 106 (2.2 × 105–4.2 × 107), and 2728 (415–7243) copies/mL for Monolisa, Murex, and HCV antigen CLIA, respectively. CONCLUSION Analytical sensitivity of NAT was on average 1 million- and 780-fold higher than combination assays and HCV antigen CLIA, respectively. Relative sensitivities of combination assays differed for genotypes with Murex being more sensitive for gt1 and gt3 and Monolisa more sensitive for gt2. Although being less sensitive than NAT, combination assays could be considered in resource-limited settings since they detect 38% to 47% of seronegative WP donations. PMID:26013970

  4. What justifies the lack of alignment between natural gas and crude oil prices in the period 2006-2007; O que justifica o deslocamento entre os precos do gas natural e do petroleo no periodo 2006-2007

    Energy Technology Data Exchange (ETDEWEB)

    Abreu, Ana Lucia Vahia de; Pinelli, Marcelo Santos

    2008-07-01

    The objective of the work is to show that the mismatch between Brent and Henry Hub in the period 2006-2007 is mainly due to the local characteristics of natural gas market. After the beginning of 2008, the price of Henry Hub is increasing and returning to the long term relationship (nonlinear) with Brent. Even with local features, the natural gas market tends to be a market of tradable goods. (author.

  5. A simple method for the measurement of radioactivity of samples separated by gas chromatography

    International Nuclear Information System (INIS)

    Farkas, T.

    1981-01-01

    Gas chromatographs with flame ionization detector can be used to determine the radioactivity ( 14 C) of separated peaks. After a suitable change in the detector output the combustion product 14 CO 2 can be trapped by hyamine hydroxyde and measured by liquid scintigraphy. 90% of peak activity can be collected and measured, thus the method can be applied to determine the distribution and specific radioactivity of the components separated by gas chromatography. (author)

  6. High Pressure Atmospheric Sampling Inlet System for Venus or the Gas Giants, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — Thorleaf Research, Inc. proposes to develop a miniaturized high pressure atmospheric sampling inlet system for sample acquisition in extreme planetary environments,...

  7. A high-throughput headspace gas chromatographic technique for the determination of nitrite content in water samples.

    Science.gov (United States)

    Zhang, Shu-Xin; Peng, Rong; Jiang, Ran; Chai, Xin-Sheng; Barnes, Donald G

    2018-02-23

    This paper reports on a high-throughput headspace gas chromatographic method (HS-GC) for the determination of nitrite content in water sample, based on GC measurement of cyclohexene produced from the reaction between nitrite and cyclamate in a closed vial. The method has a relative standard deviation of water samples. In short, the present HS-GC method is simple, accurate, and sensitive, and it is very suitable to be used in the batch sample testing. Copyright © 2018 Elsevier B.V. All rights reserved.

  8. Gas

    International Nuclear Information System (INIS)

    1996-01-01

    The French government has decided to modify the conditions of extension of local natural gas authorities to neighbouring districts. The European Union is studying the conditions of internal gas market with the objective of more open markets although considering public service requirements

  9. Sampling

    CERN Document Server

    Thompson, Steven K

    2012-01-01

    Praise for the Second Edition "This book has never had a competitor. It is the only book that takes a broad approach to sampling . . . any good personal statistics library should include a copy of this book." —Technometrics "Well-written . . . an excellent book on an important subject. Highly recommended." —Choice "An ideal reference for scientific researchers and other professionals who use sampling." —Zentralblatt Math Features new developments in the field combined with all aspects of obtaining, interpreting, and using sample data Sampling provides an up-to-date treat

  10. Is Young Adulthood a Critical Period for Suicidal Behavior among Sexual Minorities? Results from a US National Sample.

    Science.gov (United States)

    Fish, Jessica N; Rice, Cara E; Lanza, Stephanie T; Russell, Stephen T

    2018-03-29

    The developmental timing of suicide-related disparities between heterosexuals and sexual minorities (i.e., lesbian/gay and bisexual (LGB) people) is an understudied area that has critical prevention implications. In addition to developmentally situated experiences that shape risk for suicidality in the general population, sexual minorities also experience unique social stressors (e.g., anti-LGB stigma) that may alter their risk for suicidal behavior at different ages. Using a nationally representative US sample of adults, we assessed age-varying rates of suicidal behavior among heterosexuals and sexual minorities ages 18 to 60 and the age-varying association between anti-LGB discrimination and suicidal behavior. We also tested whether these age-varying prevalences and associations differed for men and women and for sexual minorities who did and did not endorse a sexual minority identity. Results indicate a critical period for suicide behavior risk for sexual minorities during young adulthood, with the highest rates of risk at age 18 followed by a steady decline until the early 40s. Disparities were particularly robust for sexual minorities who identified as lesbian, gay, or bisexual. This pattern was present for both men and women, though sexual minority women in their 30s were more likely to report suicidal behavior than heterosexuals and sexual minority men. Sexual minorities who experienced anti-LGB discrimination were more likely to report suicidal behavior, but the significance of this association was limited to those under 30. The effect of discrimination on suicidal behavior was stronger among young adult sexual minority men, relative to sexual minority women, but was present for a wider age range for sexual minority women (until age 30) relative to sexual minority men (until age 25).

  11. Hepatitis C genotype distribution in patient and blood donor samples in South Africa for the period 2008-2012.

    Science.gov (United States)

    Prabdial-Sing, N; Chirwa, T; Thaver, J; Smuts, H; Vermeulen, M; Suchard, M; Puren, A J

    2016-11-01

    There are limited molecular epidemiological studies of hepatitis C at a national level in South Africa. The introduction of newer treatment modalities for hepatitis C requires knowledge of the genotypes as these may have different prognostic and therapeutic implications. This retrospective study describes genotype distributions of patients attending specialist clinics and a blood donor group studied during the period 2008-2012 in South Africa. Residual samples from diagnostic viral load testing from specialist clinics in South Africa (n=941) and from the South African National Blood Service (n=294) were analysed quantitatively by real-time PCR and genotyped using the Versant line probe assay or sequencing. Genotype 1 was predominant in blood donors (34%), whilst genotype 5a was prevalent in patients (36%). In the blood donor group, genotype 4 was detected for the first time. Genotype 2 was rare in the patient group and not detected in blood donors. Genotype 1 was the predominant genotype in the younger age groups (less than 30 years), whereas genotype 5a was found at higher proportions in the older age groups for both the patient and blood donor groups, comprising more than 60% of genotypes in those older than 50 years. Genotypes 1 and 5 were at highest proportions across all provinces compared to other genotypes. In blood donors, genotype 1 was predominant among Caucasians (43%) and genotype 5a among Blacks (54%). Such information is required for planning the impact on the health sector with regard to newly emerging therapies for hepatitis C and burden of disease. © 2016 John Wiley & Sons Ltd.

  12. Effects of dry period length on production, cash flows and greenhouse gas emissions of the dairy herd: A dynamic stochastic simulation model.

    Directory of Open Access Journals (Sweden)

    Akke Kok

    Full Text Available Shortening or omitting the dry period of dairy cows improves metabolic health in early lactation and reduces management transitions for dairy cows. The success of implementation of these strategies depends on their impact on milk yield and farm profitability. Insight in these impacts is valuable for informed decision-making by farmers. The aim of this study was to investigate how shortening or omitting the dry period of dairy cows affects production and cash flows at the herd level, and greenhouse gas emissions per unit of milk, using a dynamic stochastic simulation model. The effects of dry period length on milk yield and calving interval assumed in this model were derived from actual performance of commercial dairy cows over multiple lactations. The model simulated lactations, and calving and culling events of individual cows for herds of 100 cows. Herds were simulated for 5 years with a dry period of 56 (conventional, 28 or 0 days (n = 50 herds each. Partial cash flows were computed from revenues from sold milk, calves, and culled cows, and costs from feed and rearing youngstock. Greenhouse gas emissions were computed using a life cycle approach. A dry period of 28 days reduced milk production of the herd by 3.0% in years 2 through 5, compared with a dry period of 56 days. A dry period of 0 days reduced milk production by 3.5% in years 3 through 5, after a dip in milk production of 6.9% in year 2. On average, dry periods of 28 and 0 days reduced partial cash flows by €1,249 and €1,632 per herd per year, and increased greenhouse gas emissions by 0.7% and 0.5%, respectively. Considering the potential for enhancing cow welfare, these negative impacts of shortening or omitting the dry period seem justifiable, and they might even be offset by improved health.

  13. Analysis of the tritium gas sample by gas chromatography. one of the basic steps in the fuel cycle of the ITER

    International Nuclear Information System (INIS)

    Szuecs, Z.

    2006-01-01

    Complete text of publication follows. The international consortium (EU, USA, Russia, Japan, South Korea, China and India) signed a formal agreement to build the International Thermonuclear Experimental Reactor (ITER) on November 21, 2006. The official objective of ITER is to 'demonstrate the scientific and technological feasibility of fusion energy for peaceful purposes'. The deuterium-tritium fusion process releases roughly three times much energy as uranium 235 fission and millions of times more energy than a chemical reaction such as the burning of coal or hydrocarbons. It is the goal of a fusion power plant to harness this energy to produce electricity. The Atomki recognized this perspective trend at time and it was involved into the fusion research by the Hungarian Fusion Association from September 2005. This short communication is referring about the cooperation, which was realized between the Atomki and the Tritium Laboratory Karlsruhe (TLK) in field of the analysis of the tritium gas samples from spring of 2006. The tritium is one of the main important fuel materials for the fusion reactor. As a radioactive gas it needs special attention for its handling and analysis. In the TLK has been developed gas-chromatographic technology for checking of the tritium gas sampling, origin from the different parts of the Tritium Plant. However this method is already 14 years old and the old staff was changed 2 years ago, loosed some important knowhow at the same time. Therefore was necessary to check the system and to carry out some important maintenance. All of them are summarized in the following 4 points: 1. The continuously increasing of the retention time of the Porapack Q column created the question: Nor the resin phase of the column already damaged or the resin works properly and any other effect (leak on the pipe system or in the valves or in pressure regulators, changing of the inlet and outlet pressure and the changing of the ratio of the flow rates) occurs

  14. Changes According to Incubation Periods in Some Microbiological Characteristics at Soil Samples of Some Soil Series from the Gelemen Agricultural Administration

    OpenAIRE

    KARA, Emine Erman

    1998-01-01

    Changes according to incubation periods in some microbiological characteristics at soil samples of soil series from Gelemen Agricultural Administraction were investigated in this study. The results show that bacteria, actinomycet had values in the first periods of incubation (30ºC and field capacity) and in the following periods increased. However, fungus population changed depending upon series properties and reached maximum values 24th and 32th days after the beginning of incubation. During...

  15. Augmented switching linear dynamical system model for gas concentration estimation with MOX sensors in an open sampling system.

    Science.gov (United States)

    Di Lello, Enrico; Trincavelli, Marco; Bruyninckx, Herman; De Laet, Tinne

    2014-07-11

    In this paper, we introduce a Bayesian time series model approach for gas concentration estimation using Metal Oxide (MOX) sensors in Open Sampling System (OSS). Our approach focuses on the compensation of the slow response of MOX sensors, while concurrently solving the problem of estimating the gas concentration in OSS. The proposed Augmented Switching Linear System model allows to include all the sources of uncertainty arising at each step of the problem in a single coherent probabilistic formulation. In particular, the problem of detecting on-line the current sensor dynamical regime and estimating the underlying gas concentration under environmental disturbances and noisy measurements is formulated and solved as a statistical inference problem. Our model improves, with respect to the state of the art, where system modeling approaches have been already introduced, but only provided an indirect relative measures proportional to the gas concentration and the problem of modeling uncertainty was ignored. Our approach is validated experimentally and the performances in terms of speed of and quality of the gas concentration estimation are compared with the ones obtained using a photo-ionization detector.

  16. Versatile, ultra-low sample volume gas analyzer using a rapid, broad-tuning ECQCL and a hollow fiber gas cell

    Science.gov (United States)

    Kriesel, Jason M.; Makarem, Camille N.; Phillips, Mark C.; Moran, James J.; Coleman, Max L.; Christensen, Lance E.; Kelly, James F.

    2017-05-01

    We describe a versatile mid-infrared (Mid-IR) spectroscopy system developed to measure the concentration of a wide range of gases with an ultra-low sample size. The system combines a rapidly-swept external cavity quantum cascade laser (ECQCL) with a hollow fiber gas cell. The ECQCL has sufficient spectral resolution and reproducibility to measure gases with narrow features (e.g., water, methane, ammonia, etc.), and also the spectral tuning range needed to measure volatile organic compounds (VOCs), (e.g., aldehydes, ketones, hydrocarbons), sulfur compounds, chlorine compounds, etc. The hollow fiber is a capillary tube having an internal reflective coating optimized for transmitting the Mid-IR laser beam to a detector. Sample gas introduced into the fiber (e.g., internal volume = 0.6 ml) interacts strongly with the laser beam, and despite relatively modest path lengths (e.g., L 3 m), the requisite quantity of sample needed for sensitive measurements can be significantly less than what is required using conventional IR laser spectroscopy systems. Example measurements are presented including quantification of VOCs relevant for human breath analysis with a sensitivity of 2 picomoles at a 1 Hz data rate.

  17. Versatile, ultra-low sample volume gas analyzer using a rapid, broad-tuning ECQCL and a hollow fiber gas cell

    Energy Technology Data Exchange (ETDEWEB)

    Kriesel, Jason M.; Makarem, Camille N.; Phillips, Mark C.; Moran, James J.; Coleman, Max; Christensen, Lance; Kelly, James F.

    2017-05-05

    We describe a versatile mid-infrared (Mid-IR) spectroscopy system developed to measure the concentration of a wide range of gases with an ultra-low sample size. The system combines a rapidly-swept external cavity quantum cascade laser (ECQCL) with a hollow fiber gas cell. The ECQCL has sufficient spectral resolution and reproducibility to measure gases with narrow features (e.g., water, methane, ammonia, etc.), and also the spectral tuning range needed to measure volatile organic compounds (VOCs), (e.g., aldehydes, ketones, hydrocarbons), sulfur compounds, chlorine compounds, etc. The hollow fiber is a capillary tube having an internal reflective coating optimized for transmitting the Mid-IR laser beam to a detector. Sample gas introduced into the fiber (e.g., internal volume = 0.6 ml) interacts strongly with the laser beam, and despite relatively modest path lengths (e.g., L ~ 3 m), the requisite quantity of sample needed for sensitive measurements can be significantly less than what is required using conventional IR laser spectroscopy systems. Example measurements are presented including quantification of VOCs relevant for human breath analysis with a sensitivity of ~2 picomoles at a 1 Hz data rate.

  18. Determination of Organic Pollutants in Small Samples of Groundwaters by Liquid-Liquid Extraction and Capillary Gas Chromatography

    DEFF Research Database (Denmark)

    Harrison, I.; Leader, R.U.; Higgo, J.J.W.

    1994-01-01

    A method is presented for the determination of 22 organic compounds in polluted groundwaters. The method includes liquid-liquid extraction of the base/neutral organics from small, alkaline groundwater samples, followed by derivatisation and liquid-liquid extraction of phenolic compounds after neu...... neutralisation. The extracts were analysed by capillary gas chromatography. Dual detection by flame Ionisation and electron capture was used to reduce analysis time....

  19. Atmospheric Gas Tracers in Groundwater: Theory, Sampling. Measurement and Interpretation; Yeraltisuyunda Atmosferik Gaz Izleyiciler: Kuram, Oernekleme, Oelcuem ve Yorum

    Energy Technology Data Exchange (ETDEWEB)

    Bayari, C S [Hacettepe University, Ankara(Turkey)

    2002-07-01

    Some of the atmospheric gasses posses features that are sought in an environmental tracer of hydrogeologic interest. Among these, chlorofluorocarbons, sulfur hegzafluoride, carbon tetrachloride, methyl chloroform, krypton-85 etc. have found increasing use in groundwater age dating studies during the last ten years. This paper explains the theory of their use as tracer and discusses the major concerns as related to their sampling and analyses. Factors affecting their applicability and the approach to interpret tracer gas data is briefly outlined.

  20. Gas sampling method for determining pollutant concentrations in the flame zone of two swirl-can combustor modules

    Science.gov (United States)

    Duerr, R. A.

    1975-01-01

    A gas sampling probe and traversing mechanism were developed to obtain detailed measurements of gaseous pollutant concentrations in the primary and mixing regions of combustors in order to better understand how pollutants are formed. The gas sampling probe was actuated by a three-degree-of-freedom traversing mechanism and the samples obtained were analyzed by an on-line gas analysis system. The pollutants in the flame zone of two different swirl-can combustor modules were measured at an inlet-air temperature of 590 K, pressure of 6 atmospheres, and reference velocities of 23 and 30 meters per second at a fuel-air ratio of 0.02. Typical results show large spatial gradients in the gaseous pollutant concentration close to the swirl-can module. Average concentrations of unburned hydrocarbons and carbon monoxide decrease rapidly in the downstream wake regions of each module. By careful and detailed probing, the effect of various module design features on pollutant formation can be assessed. The techniques presently developed seem adequate to obtain the desired information.

  1. A safety assessment of rotary mode core sampling in flammable gas single shell tanks: Hanford Site, Richland, Washington

    Energy Technology Data Exchange (ETDEWEB)

    Raymond, R.E.

    1996-04-15

    This safety assessment (SA) addresses each of the required elements associated with the installation, operation, and removal of a rotary-mode core sampling (RMCS) device in flammable-gas single-shell tanks (SSTs). The RMCS operations are needed in order to retrieve waste samples from SSTs with hard layers of waste for which push-mode sampling is not adequate for sampling. In this SA, potential hazards associated with the proposed action were identified and evaluated systematically. Several potential accident cases that could result in radiological or toxicological gas releases were identified and analyzed and their consequences assessed. Administrative controls, procedures and design changes required to eliminate or reduce the potential of hazards were identified. The accidents were analyzed under nine categories, four of which were burn scenarios. In SSTS, burn accidents result in unacceptable consequences because of a potential dome collapse. The accidents in which an aboveground burn propagates into the dome space were shown to be in the ``beyond extremely unlikely`` frequency category. Given the unknown nature of the gas-release behavior in the SSTS, a number of design changes and administrative controls were implemented to achieve these low frequencies. Likewise, drill string fires and dome space fires were shown to be very low frequency accidents by taking credit for the design changes, controls, and available experimental and analytical data. However, a number of Bureau of Mines (BOM) tests must be completed before some of the burn accidents can be dismissed with high confidence. Under the category of waste fires, the possibility of igniting the entrapped gases and the waste itself were analyzed. Experiments are being conducted at the BOM to demonstrate that the drill bit is not capable of igniting the trapped gas in the waste. Laboratory testing and thermal analysis demonstrated that, under normal operating conditions, the drill bit will not create high

  2. A safety assessment of rotary mode core sampling in flammable gas single shell tanks: Hanford Site, Richland, Washington

    International Nuclear Information System (INIS)

    Raymond, R.E.

    1996-01-01

    This safety assessment (SA) addresses each of the required elements associated with the installation, operation, and removal of a rotary-mode core sampling (RMCS) device in flammable-gas single-shell tanks (SSTs). The RMCS operations are needed in order to retrieve waste samples from SSTs with hard layers of waste for which push-mode sampling is not adequate for sampling. In this SA, potential hazards associated with the proposed action were identified and evaluated systematically. Several potential accident cases that could result in radiological or toxicological gas releases were identified and analyzed and their consequences assessed. Administrative controls, procedures and design changes required to eliminate or reduce the potential of hazards were identified. The accidents were analyzed under nine categories, four of which were burn scenarios. In SSTS, burn accidents result in unacceptable consequences because of a potential dome collapse. The accidents in which an aboveground burn propagates into the dome space were shown to be in the ''beyond extremely unlikely'' frequency category. Given the unknown nature of the gas-release behavior in the SSTS, a number of design changes and administrative controls were implemented to achieve these low frequencies. Likewise, drill string fires and dome space fires were shown to be very low frequency accidents by taking credit for the design changes, controls, and available experimental and analytical data. However, a number of Bureau of Mines (BOM) tests must be completed before some of the burn accidents can be dismissed with high confidence. Under the category of waste fires, the possibility of igniting the entrapped gases and the waste itself were analyzed. Experiments are being conducted at the BOM to demonstrate that the drill bit is not capable of igniting the trapped gas in the waste. Laboratory testing and thermal analysis demonstrated that, under normal operating conditions, the drill bit will not create high

  3. Direct sample introduction-gas chromatography-mass spectrometry for the determination of haloanisole compounds in cork stoppers.

    Science.gov (United States)

    Cacho, J I; Nicolás, J; Viñas, P; Campillo, N; Hernández-Córdoba, M

    2016-12-02

    A solventless analytical method is proposed for analyzing the compounds responsible for cork taint in cork stoppers. Direct sample introduction (DSI) is evaluated as a sample introduction system for the gas chromatography-mass spectrometry (GC-MS) determination of four haloanisoles (HAs) in cork samples. Several parameters affecting the DSI step, including desorption temperature and time, gas flow rate and other focusing parameters, were optimized using univariate and multivariate approaches. The proposed method shows high sensitivity and minimises sample handling, with detection limits of 1.6-2.6ngg -1 , depending on the compound. The suitability of the optimized procedure as a screening method was evaluated by obtaining decision limits (CCα) and detection capabilities (CCβ) for each analyte, which were found to be in 6.9-11.8 and 8.7-14.8ngg -1 , respectively, depending on the compound. Twenty-four cork samples were analysed, and 2,4,6-trichloroanisole was found in four of them at levels between 12.6 and 53ngg -1 . Copyright © 2016 Elsevier B.V. All rights reserved.

  4. The challenge of multi-parameter hydrochemical, gas-physical, and isotopic analyses of in-situ clay pore water and samples from in-situ clay experiments

    International Nuclear Information System (INIS)

    Eichinger, L.; Lorenz, G.D.; Eichinger, F.; Wechner, S.; Voropaev, A.

    2012-01-01

    Document available in extended abstract form only. Within the research framework of natural clay rocks used as barriers for radioactive waste confinement comprehensive analyses are mandatory to determine the chemical and isotopic composition of natural pore water and therein dissolved gases as well as samples from distinct in-situ and lab experiments. Based on the natural conditions pore waters from low permeable argillaceous rocks can be sampled only in small amounts over long time periods. Often those samples are primarily influenced by processes of the exploration and exploitation such as the contamination by drilling fluid and disinfection fluid or cement-water interactions. Sophisticated equipment for circulation experiments allows the sampling of gas and water in the original state in steel and peek cells. The challenge though is to optimise the lab equipment and measurement techniques in a way that the physical-chemical conditions of the water can be analysed in the original state. The development of special micro measuring cells enables the analyses of physical parameters like redox potential under very slow through-flow conditions. Additional analyses can follow subsequently without wasting any drop of the precious pore water. The gas composition is measured in equilibrated gas phases above water phases after emptying a defined volume by inert gas or through manual pressure. The analytical challenge is to obtain an extensive set of parameters which is considered representative for the in-situ conditions using only a few millilitres of water. The parameter analysis includes the determination of the composition of the water, the isotopic compositions of the water and the dissolved constituents as well as their gas concentrations and isotopic signatures. So far the smallest sample volume needed for an analysis of a full set of parameters including the gas composition was 9 ml of water. Obviously, the analysis requires a highly sophisticated infrastructure and

  5. Large-volume constant-concentration sampling technique coupling with surface-enhanced Raman spectroscopy for rapid on-site gas analysis.

    Science.gov (United States)

    Zhang, Zhuomin; Zhan, Yisen; Huang, Yichun; Li, Gongke

    2017-08-05

    In this work, a portable large-volume constant-concentration (LVCC) sampling technique coupling with surface-enhanced Raman spectroscopy (SERS) was developed for the rapid on-site gas analysis based on suitable derivatization methods. LVCC sampling technique mainly consisted of a specially designed sampling cell including the rigid sample container and flexible sampling bag, and an absorption-derivatization module with a portable pump and a gas flowmeter. LVCC sampling technique allowed large, alterable and well-controlled sampling volume, which kept the concentration of gas target in headspace phase constant during the entire sampling process and made the sampling result more representative. Moreover, absorption and derivatization of gas target during LVCC sampling process were efficiently merged in one step using bromine-thiourea and OPA-NH 4 + strategy for ethylene and SO 2 respectively, which made LVCC sampling technique conveniently adapted to consequent SERS analysis. Finally, a new LVCC sampling-SERS method was developed and successfully applied for rapid analysis of trace ethylene and SO 2 from fruits. It was satisfied that trace ethylene and SO 2 from real fruit samples could be actually and accurately quantified by this method. The minor concentration fluctuations of ethylene and SO 2 during the entire LVCC sampling process were proved to be gas targets from real samples by SERS. Copyright © 2017 Elsevier B.V. All rights reserved.

  6. Analytical Method for Carbon and Oxygen Isotope of Small Carbonate Samples with the GasBench Ⅱ-IRMS Device

    Directory of Open Access Journals (Sweden)

    LIANG Cui-cui

    2015-01-01

    Full Text Available An analytical method for measuring carbon and oxygen isotopic compositions of trace amount carbonate (>15 μg was established by Delta V Advantage isotope Ratio MS coupled with GasBench Ⅱ. Different trace amount (5-50 μg carbonate standard samples (IAEA-CO-1 were measured by GasBench Ⅱ with 12 mL and 3.7 mL vials. When the weight of samples was less than 40 μg and it was acidified in 12 mL vials, most standard deviations of the δ13C and δ18O were more than 0.1‰, which couldn’t satisfied high-precision measurements. When the weight of samples was greater than 15 μg and it was acidified in 3.7 mL vials, standard deviations for the δ13C and δ18O were 0.01‰-0.07‰ and 0.01‰-0.08‰ respectively, which satisfied high-precision measurements. Therefore, small 3.7 mL vials were used to increase the concentration of carbon dioxide in headspace, carbonate samples even less as 15 μg can be analyzed routinely by a GasBench Ⅱ continuous-flow IRMS. Meanwhile, the linear relationship between sample’s weight and peak’s area was strong (R2>0.993 2 and it can be used to determine the carbon content of carbonate samples.

  7. Hydrogen sulfide measurement by headspace-gas chromatography-mass spectrometry (HS-GC-MS): application to gaseous samples and gas dissolved in muscle.

    Science.gov (United States)

    Varlet, Vincent; Giuliani, Nicole; Palmiere, Cristian; Maujean, Géraldine; Augsburger, Marc

    2015-01-01

    The aim of our study was to present a new headspace-gas chromatography-mass spectrometry (HS-GC-MS) method applicable to the routine determination of hydrogen sulfide (H(2)S) concentrations in biological and gaseous samples. The primary analytical drawback of the GC/MS methods for H(2)S measurement discussed in the literature was the absence of a specific H(2)S internal standard required to perform quantification. Although a deuterated hydrogen sulfide (D(2)S) standard is currently available, this standard is not often used because this standard is expensive and is only available in the gas phase. As an alternative approach, D(2)S can be generated in situ by reacting deuterated chloride with sodium sulfide; however, this technique can lead to low recovery yield and potential isotopic fractionation. Therefore, N(2)O was chosen for use as an internal standard. This method allows precise measurements of H(2)S concentrations in biological and gaseous samples. Therefore, a full validation using accuracy profile based on the β-expectation tolerance interval is presented. Finally, this method was applied to quantify H(2)S in an actual case of H(2)S fatal intoxication. © The Author 2014. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  8. Identification of control parameters for the sulfur gas storability with bag sampling methods

    Science.gov (United States)

    Air samples containing sulfur compounds are often collected and stored in sample bags prior to analyses. The storage stability of six gaseous sulfur compounds (H2S, CH3SH, DMS, CS2, DMDS and SO2) was compared between two different bag materials (polyvinyl fluoride (PVF) and polyester aluminum (PEA))...

  9. 40 CFR 92.114 - Exhaust gas and particulate sampling and analytical system.

    Science.gov (United States)

    2010-07-01

    ... transport sample to analyzers. (I) Temperature sensor. A temperature sensor (T1) to measure the NO2 to NO... feet (1.22 m) from the exhaust duct. (iii) The sample transport system from the engine exhaust duct to.... (A) For diesel fueled and biodiesel fueled locomotives and engines, the wall temperature of the HC...

  10. Development and evaluation of a gas chromatographic method for the determination of triazine herbicides in natural water samples

    Science.gov (United States)

    Steinheimer, T.R.; Brooks, M.G.

    1984-01-01

    A multi-residue method is described for the determination of triazine herbicides in natural water samples. The technique uses solvent extraction followed by gas chromatographic separation and detection employing nitrogen-selective devices. Seven compounds can be determined simultaneously at a nominal detection limit of 0.1 ??g/L in a 1-litre sample. Three different natural water samples were used for error analysis via evaluation of recovery efficiencies and estimation of overall method precision. As an alternative to liquid-liquid partition (solvent extraction) for removal of compounds of interest from water, solid-phase extraction (SPE) techniques employing chromatographic grade silicas with chemically modified surfaces have been examined. SPE is found to provide rapid and efficient concentration with quantitative recovery of some triazine herbicides from natural water samples. Concentration factors of 500 to 1000 times are obtained readily by the SPE technique.A multi-residue method is described for the determination of triazine herbicides in natural water samples. The technique uses solvent extraction followed by gas chromatographic separation and detection employing nitrogen-selective devices. Seven compounds can be determined simultaneously at a nominal detection limit of 0. 1 mu g/L in a 1-litre sample. As an alternative to liquid-liquid partition (solvent extraction) for removal of compounds of interest from water, solid-phase extraction (SPE) techniques employing chromatographic grade silicas with chemically modified surfaces have been examined. SPE is found to provide rapid and efficient concentration with quantitative recovery of some triazine herbicides from natural water samples. Concentration factors of 500 to 1000 times are obtained readily by the SPE technique.

  11. Application of model MTS5 dew-point meter in gas sampling and analyzing system of HTR-10

    International Nuclear Information System (INIS)

    Zhu Jiang; Li Zhihui

    2010-01-01

    The feature of humidity detector to measure the content of water in pure helium of main loop of reactor was discussed, and the circumstances using Al 2 O 3 moisture sensor to measure the content of water in helium on-line were introduced. During those few years, the dew-point meter has sufficed to measure the content of water in the helium gas during the running of the reactor. On the other hand, excursion can happen when the instrument running. Demarcate must be made periodically to improve the veracity of the meter. (authors)

  12. Prediction of Repair Work Duration for Gas Transport Systems Based on Small Data Samples

    DEFF Research Database (Denmark)

    Lesnykh, Valery; Litvin, Yuri; Kozin, Igor

    2016-01-01

    Prediction of the duration of a repair and maintenance project of a gas transport system is an important part of planning activities. There exist numerous sources of uncertainties that may result in time overruns possibly leading to multiple negative consequences. Our experience in planning...... this work suggests that accepting the stochastic nature of the project duration is a constructive step towards the preparedness to contingencies and defining penalties for repair companies. To support this approach, one needs to construct probability distributions of the durations of the projects...

  13. Abundances of Volatile - Bearing Species from Evolved Gas Analysis of Samples from the Rocknest Aeolian Bedform in Gale Crater

    Science.gov (United States)

    Archer, P. D., Jr.; Franc, H. B.; Sutter, B.; McAdam, A.; Ming, D. W.; Morris, R. V.; Mahaffy, P. R.

    2013-01-01

    The Sample Analysis at Mars (SAM) instrument suite on board the Mars Science Laboratory (MSL) recently ran four samples from an aeolian bedform named Rocknest. SAM detected the evolution of H2O, CO2, O2, and SO2, indicative of the presence of multiple volatile bearing species (Fig 1). The Rocknest bedform is a windblown deposit selected as representative of both the windblown material in Gale crater as well as the globally-distributed martian dust. Four samples of Rocknest material were analyzed by SAM, all from the fifth scoop taken at this location. The material delivered to SAM passed through a 150 m sieve and is assumed to have been well mixed during the sample acquisition/preparation/handoff process. SAM heated the Rocknest samples to approx.835 C at a ramp rate of 35 C/min with a He carrier gas flow rate of apprx.1.5 standard cubic centimeters per minute and at an oven pressure of 30 mbar [1]. Evolved gases were detected by a quadrupole mass spectrometer (QMS). This abstract presents the molar abundances of H2O, CO2, O2, and SO2 as well as their concentration in rocknest samples using an estimated sample mass.

  14. 40 CFR 89.421 - Exhaust gas analytical system; CVS bag sample.

    Science.gov (United States)

    2010-07-01

    ... the measurement of carbon monoxide and carbon dioxide, and a chemiluminescence detector (CLD) (or HCLD... following requirements: (1) The CLD (or HCLD) requires that the nitrogen dioxide present in the sample be...

  15. 40 CFR 91.423 - Exhaust gas analytical system; CVS grab sample.

    Science.gov (United States)

    2010-07-01

    ... carbon dioxide, and a chemiluminescence detector (CLD) (or heated CLD (HCLD)) for the measurement of...) The CLD (or HCLD) requires that the nitrogen dioxide present in the sample be converted to nitric...

  16. 40 CFR 90.423 - Exhaust gas analytical system; CVS grab sample.

    Science.gov (United States)

    2010-07-01

    ... measurement of carbon monoxide and carbon dioxide, and a chemiluminescence detector (CLD) (or heated CLD (HCLD... following requirements: (1) The CLD (or HCLD) requires that the nitrogen dioxide present in the sample be...

  17. Gas and liquid sampling for closed canisters in K-West basins - functional design criteria

    International Nuclear Information System (INIS)

    Pitkoff, C.C.

    1994-01-01

    The purpose of this document is to provide functions and requirements for the design and fabrication of equipment for sampling closed canisters in the K-West basin. The samples will be used to help determine the state of the fuel elements in closed canisters. The characterization information obtained will support evaluation and development of processes required for safe storage and disposition of Spent Nuclear Fuel (SNF) materials

  18. Planck/SDSS Cluster Mass and Gas Scaling Relations for a Volume-Complete redMaPPer Sample

    Science.gov (United States)

    Jimeno, Pablo; Diego, Jose M.; Broadhurst, Tom; De Martino, I.; Lazkoz, Ruth

    2018-04-01

    Using Planck satellite data, we construct Sunyaev-Zel'dovich (SZ) gas pressure profiles for a large, volume-complete sample of optically selected clusters. We have defined a sample of over 8,000 redMaPPer clusters from the Sloan Digital Sky Survey (SDSS), within the volume-complete redshift region 0.100 trend towards larger break radius with increasing cluster mass. Our SZ-based masses fall ˜16% below the mass-richness relations from weak lensing, in a similar fashion as the "hydrostatic bias" related with X-ray derived masses. Finally, we derive a tight Y500-M500 relation over a wide range of cluster mass, with a power law slope equal to 1.70 ± 0.07, that agrees well with the independent slope obtained by the Planck team with an SZ-selected cluster sample, but extends to lower masses with higher precision.

  19. Noble Gas Sampling and Detection Methods for On-Site Inspections in Support of CTBT

    International Nuclear Information System (INIS)

    Wieslander, J.S.E.

    2015-01-01

    The On-Site Inspections (OSI) constitutes the final verification measure under the CTBT, and are conducted to verify States Parties' compliance with the Comprehensive Nuclear-Test-Ban Treaty (CTBT). An on-site inspection is launched to establish whether or not a nuclear explosion has been carried out and during such an inspection, facts might also be gathered to identify a possible violator of the Treaty. The Treaty lists all activities and techniques that are permitted and one of these is the environmental sampling of noble gases (NG) in the air and underground, which can be deployed at any time during an OSI. The CTBT relevant isotopes are Xe-133, 133m, 131m, 135 and Ar-37. The samples are primarily to be analyzed on-site, although the treaty also allows off-site analysis in designated laboratories if necessary. Stringent procedures ensure the security, integrity and confidentiality of the samples throughout the sampling and analysis process — all taking place in the field. Over the past decade the techniques for NG sampling, processing and analysis of both atmospheric and subsoil NG samples have been developed further in order to fit to the conditions and requirements during an OSI. This has been a major international effort with a global set of collaborators. Especially during the past three years the efforts intensified in order to finalize the scientific and technical developments for the Integrated Field Exercise, November 2014 (IFE14). This presentation will provide an overview of the current status of the OSI NG sampling regime and the OSI NG Field Laboratory to be deployed in IFE14, together with more technical descriptions of methods and equipment as well as a short discussion on potential future developments and alternative applications as applicable. (author)

  20. Monitoring and groundwater/gas sampling in sands densified with explosives

    Directory of Open Access Journals (Sweden)

    Carlos A. Vega-Posada

    2014-01-01

    Full Text Available Este manuscrito presenta los resultados de un estudio de densificación de suelos en campo utilizando explosivos y realizado en un relleno sanitario localizado en Carolina de Sur, Estados Unidos; este estudio se realizó con el objeto de determinar los tipos de gases que se liberan y sus respectivas concentraciones in situ después del proceso de densificación. Se utilizó un sistema de sonda BAT para recolectar las muestras de aguas subterráneas y de gas en la mitad del estrato en estudio, así como para medir la evolución de las presiones del agua durante y después de la detonación de las cargas explosivas. Adicionalmente, se hicieron mediciones topográficas a través del eje central longitudinal de la zona de estudio después de cada explosión para medir la magnitud y la efectividad de esta técnica de densificación en depósitos de arena sueltas. Los resultados de este estudio mostraron que: a el sistema de sonda BAT puede ser una técnica confiable para recolectar muestra de agua subterránea y gas en campo antes y después de la explosión; b la masa de suelo afectada por la detonación de los explosivos licuó por un periodo de 6 horas, mientras el esfuerzo vertical efectivo alcanzó sus valores iniciales después de 3 días; y c se observaron deformaciones verticales significativas en el área de estudio después de cada explosión, lo cual indica que la masa de suelo fue exitosamente densificada.

  1. A safety equipment list for rotary mode core sampling systems operation in single shell flammable gas tanks; TOPICAL

    International Nuclear Information System (INIS)

    SMALLEY, J.L.

    1999-01-01

    This document identifies all interim safety equipment to be used for rotary mode core sampling of single-shell flammable gas tanks utilizing Rotary Mode Core Sampling systems (RMCS). This document provides the safety equipment for RMCS trucks HO-68K-4600, HO-68K-4647, trucks three and four respectively, and associated equipment. It is not intended to replace or supersede WHC-SD-WM-SEL-023, (Kelly 1991), or WHC-SD-WM-SEL-032, (Corbett 1994), which classifies 80-68K-4344 and HO-68K-4345 respectively. The term ''safety equipment'' refers to safety class (SC) and safety significant (SS) equipment, where equipment refers to structures, systems and components (SSC's). The identification of safety equipment in this document is based on the credited design safety features and analysis contained in the Authorization Basis (AB) for rotary mode core sampling operations in single-shell flammable gas tanks. This is an interim safety classification since the AB is interim. This document will be updated to reflect the final RMCS equipment safety classification designations upon completion of a final AB which will be implemented with the release of the Final Safety Analysis Report (FSAR)

  2. Low temperature X-ray diffraction studies of natural gas hydrate samples from the Gulf of Mexico

    Energy Technology Data Exchange (ETDEWEB)

    Rawn, C.J. [Oak Ridge National Laboratory, Oak Ridge, TN (United States). Materials Science and Technology Div.; Sassen, R. [Texas A and M Univ., College Station, TX (United States). Geochemical and Environmental Research Group; Ulrich, S.M.; Phelps, T.J. [Oak Ridge National Laboratory, Oak Ridge, TN (United States). Biosciences Div.; Chakoumakos, B.C. [Oak Ridge National Laboratory, Oak Ridge, TN (United States). Neutron Scattering Science Div.; Payzant, E.A. [Oak Ridge National Laboratory, Oak Ridge, TN (United States). Center for Nanophase Materials Science

    2008-07-01

    Quantitative studies of natural clathrate hydrates are hampered by the difficulties associated with obtaining pristine samples for the sea floor without comprising their integrity. This paper discussed X-ray power diffraction studies conducted to measure natural gas hydrate samples obtained from the Green Canyon in the Gulf of Mexico. Data on the hydrate deposits were initially collected in 2002. The X-ray diffraction data were collected in order to examine the structure 2 (s2) gas hydrates as functions of temperature and time. A diffractometer with a theta-theta goniometer modified with a helium closed cycle refrigerator and temperature controller was used. Aragonite, quartz and halite phases were determined in the decomposed sample. Refined phase fractions for both the ice and the s2 hydrate were obtained as a function of temperature. Results of the study demonstrated that the amount of hydrates decreased with increasing temperatures and amounts of time. Large pieces of the hydrate showed heterogenous ice content. Dissociation rates were higher at lower temperatures. It was concluded that unusual trends observed for the smaller lattice parameter of the hydrates resulted from the formation of ice layers that acted as barriers to the released gases and caused increased isostatic pressures around the hydrate core. 9 refs., 6 figs.

  3. A safety equipment list for rotary mode core sampling systems operation in single shell flammable gas tanks

    International Nuclear Information System (INIS)

    SMALLEY, J.L.

    1999-01-01

    This document identifies all interim safety equipment to be used for rotary mode core sampling of single-shell flammable gas tanks utilizing Rotary Mode Core Sampling systems (RMCS). This document provides the safety equipment for RMCS trucks HO-68K-4600, HO-68K-4647, trucks three and four respectively, and associated equipment. It is not intended to replace or supersede WHC-SD-WM-SEL-023, (Kelly 1991), or WHC-SD-WM-SEL-032, (Corbett 1994), which classifies 80-68K-4344 and HO-68K-4345 respectively. The term ''safety equipment'' refers to safety class (SC) and safety significant (SS) equipment, where equipment refers to structures, systems and components (SSC's). The identification of safety equipment in this document is based on the credited design safety features and analysis contained in the Authorization Basis (AB) for rotary mode core sampling operations in single-shell flammable gas tanks. This is an interim safety classification since the AB is interim. This document will be updated to reflect the final RMCS equipment safety classification designations upon completion of a final AB which will be implemented with the release of the Final Safety Analysis Report (FSAR)

  4. Development and application of a sampling method for the determination of reactive halogen species in volcanic gas emissions

    Science.gov (United States)

    Rüdiger, Julian; Bobrowski, Nicole; Liotta, Marcello; Hoffmann, Thorsten

    2017-04-01

    Volcanoes are a potential large source of several reactive atmospheric trace gases including sulfur and halogen containing species. Besides the importance for atmospheric chemistry, the detailed knowledge of halogen chemistry in volcanic plumes can help to get insights into subsurface processes. In this study a gas diffusion denuder sampling method, using a 1,3,5-trimethoxybenzene (1,3,5-TMB) coating for the derivatization of reactive halogen species (RHS), was characterized by dilution chamber experiments. The coating proved to be suitable to collect selectively gaseous bromine species with oxidation states (OS) of +1 or 0 (such as Br2, BrCl, BrO(H) and BrONO2), while being ignorant to HBr (OS -1). The reaction of 1,3,5-TMB with reactive bromine species gives 1-bromo-2,4,6-trimethoxybenzene (1-bromo-2,4,6-TMB) - other halogens give corresponding products. Solvent elution of the derivatized analytes and subsequent analysis with gas chromatography mass spectrometry gives detection limits of 10 ng or less for Br2, Cl2, and I2. In 2015 the method was applied on volcanic gas plumes at Mt. Etna (Italy) giving reactive bromine mixing ratios from 0.8 ppbv to 7.0 ppbv. Total bromine mixing ratios of 4.7 ppbv to 27.5 ppbv were obtained by simultaneous alkaline trap sampling (by a Raschig-tube) followed by analysis with ion chromatography and inductively coupled plasma mass spectrometry. This leads to the first results of in-situ measured reactive bromine to total bromine ratios, spanning a range between 12±1 % and 36±2 %. Our finding is in an agreement with previous model studies, which imply values < 44 % for plume ages < 1 minute, which is consistent with the assumed plume age at the sampling sites.

  5. Methodological Comparison between a Novel Automatic Sampling System for Gas Chromatography versus Photoacoustic Spectroscopy for Measuring Greenhouse Gas Emissions under Field Conditions

    Directory of Open Access Journals (Sweden)

    Alexander J. Schmithausen

    2016-10-01

    Full Text Available Trace gases such as nitrous oxide (N2O, methane (CH4, and carbon dioxide (CO2 are climate-related gases, and their emissions from agricultural livestock barns are not negligible. Conventional measurement systems in the field (Fourier transform infrared spectroscopy (FTIR; photoacoustic system (PAS are not sufficiently sensitive to N2O. Laser-based measurement systems are highly accurate, but they are very expensive to purchase and maintain. One cost-effective alternative is gas chromatography (GC with electron capture detection (ECD, but this is not suitable for field applications due to radiation. Measuring samples collected automatically under field conditions in the laboratory at a subsequent time presents many challenges. This study presents a sampling designed to promote laboratory analysis of N2O concentrations sampled under field conditions. Analyses were carried out using PAS in the field (online system and GC in the laboratory (offline system. Both measurement systems showed a good correlation for CH4 and CO2 concentrations. Measured N2O concentrations were near the detection limit for PAS. GC achieved more reliable results for N2O in very low concentration ranges.

  6. Determination of Physicals, Chemical, Biologicals and Radioactivity Parameters of Sediments and Water Samples of Seropan River of First Period

    International Nuclear Information System (INIS)

    Tri Rusmanto; Agus Taftazani

    2007-01-01

    Seropan river water quality as residential water resources can be controlled by physical, chemical, and biological parameters. The water quality with the parameters of temperature, suspended solid (SS), gross β radioactivity, hardwater, COD, BOD, Escherichia Coli have been experimentally conducted. The sediment and water samples have been taken at February and August 2006. Measurement result of Seropan river water quality showed that the temperature was 28°C, maximum SS was 48 mg/L, maximum pH was 6.8 maximum hardwater was 257.49 mg/L, maximum COD was 8 mg/L, maximum BOD was 4.9 mg/L, maximum bacteria E. coli > 2400 mpn/100 mL, maximum water gross β was 0.9071 Bq/L. All the parameters were lower than maximum permissible for water condition that decided by Governor of Yogyakarta Special Province No/214/Kpts/1991 and Public Health Minister of Republic of Indonesia Number 907/Menkes/SK/VlI/2002. Sediment sample can not be evaluated because it was not included yet in the river water quality natural radionuclides gamma transmitter identified in river water samples were Tl-208 and K-40. More element detected in sediment samples, they were, Tl-208, Ac-228, Ra-226, Pb-212, Pb-214, Bi-214, Ac-228, Ac-228 and of K-40. (author)

  7. System for δ13C–CO2 and xCO2 analysis of discrete gas samples by cavity ring-down spectroscopy

    Directory of Open Access Journals (Sweden)

    D. Dickinson

    2017-11-01

    Full Text Available A method was devised for analysing small discrete gas samples (50 mL syringe by cavity ring-down spectroscopy (CRDS. Measurements were accomplished by inletting 50 mL syringed samples into an isotopic-CO2 CRDS analyser (Picarro G2131-i between baseline readings of a reference air standard, which produced sharp peaks in the CRDS data feed. A custom software script was developed to manage the measurement process and aggregate sample data in real time. The method was successfully tested with CO2 mole fractions (xCO2 ranging from  <  0.1 to  >  20 000 ppm and δ13C–CO2 values from −100 up to +30 000 ‰ in comparison to VPDB (Vienna Pee Dee Belemnite. Throughput was typically 10 samples h−1, with 13 h−1 possible under ideal conditions. The measurement failure rate in routine use was ca. 1 %. Calibration to correct for memory effects was performed with gravimetric gas standards ranging from 0.05 to 2109 ppm xCO2 and δ13C–CO2 levels varying from −27.3 to +21 740 ‰. Repeatability tests demonstrated that method precision for 50 mL samples was ca. 0.05 % in xCO2 and 0.15 ‰ in δ13C–CO2 for CO2 compositions from 300 to 2000 ppm with natural abundance 13C. Long-term method consistency was tested over a 9-month period, with results showing no systematic measurement drift over time. Standardised analysis of discrete gas samples expands the scope of application for isotopic-CO2 CRDS and enhances its potential for replacing conventional isotope ratio measurement techniques. Our method involves minimal set-up costs and can be readily implemented in Picarro G2131-i and G2201-i analysers or tailored for use with other CRDS instruments and trace gases.

  8. 40 CFR 86.1310-90 - Exhaust gas sampling and analytical system; diesel engines.

    Science.gov (United States)

    2010-07-01

    ... avoid moisture condensation. A filter pair loading of 1 mg is typically proportional to a 0.1 g/bhp-hr..., the temperatures where condensation of water in the exhaust gases could occur. This may be achieved by... sampling zone in the primary dilution tunnel and as required to prevent condensation at any point in the...

  9. Gas chromatographic-mass spectrometric characterisation of plant gums in samples from painted works of art.

    Science.gov (United States)

    Bonaduce, Ilaria; Brecoulaki, Hariclia; Colombini, Maria Perla; Lluveras, Anna; Restivo, Vincenzo; Ribechini, Erika

    2007-12-21

    This paper presents an analytical GC-MS procedure to study the chemical composition of plant gums, determining aldoses and uronic acids in one step. The procedure is based on the silylation of aldoses and uronic acids, released from plant gums by microwave assisted hydrolysis, and previously converted into the corresponding diethyl-dithioacetals and diethyl-dithioacetal lactones. Using this method only one peak for each compound is obtained, thus providing simple and highly reproducible chromatograms. The analytical procedure was optimised using reference samples of raw plant gums (arabic, karaya, ghatti, guar, locust bean and tragacanth, cherry, plum and peach gums), commercial watercolours and paint layers prepared according to ancient recipes at the Opificio delle Pietre Dure of Florence (Italy). To identify gum media in samples of unknown composition, a decisional schema for the gum identification and the principal component analysis of the relative sugar percentage contents were employed. The procedure was used to study samples collected from wall paintings from Macedonian tombs (4th-3rd centuries bc) and from the Mycenaean "Palace of Nestor" (13th century bc) in Pylos, Greece. The presence of carbohydrates was ascertained and plant gum binders (fruit and a mixture of tragacanth and fruit tree gums) were identified in some of the samples.

  10. An all-glass solid sampling device for open tubular columns in gas chromatography

    NARCIS (Netherlands)

    Cox, T.P.H.; vd Berg, P.M.J.

    1972-01-01

    An all-glass system for direct sample-introduction of high-boiling compounds onto open tubular columns is described. The standard deviation for quantitative measurements is less than 2.7%. The loss in resolving power of capillary columns, due to this injection system is negligible. The system is

  11. Widely tunable Sampled Grating Distributed Bragg Reflector Quantum Cascade laser for gas spectroscopy applications

    Science.gov (United States)

    Diba, Abdou Salam

    Since the advent of semiconductor lasers, the development of tunable laser sources has been subject of many efforts in industry and academia arenas. This interest towards broadly tunable lasers is mainly due to the great promise they have in many applications ranging from telecommunication, to environmental science and homeland security, just to name a few. After the first demonstration of quantum cascade laser (QCL) in the early nineties, QCL has experienced a rapid development, so much so that QCLs are now the most reliable and efficient laser source in the Mid-IR range covering between 3 microm to 30 microm region of the electromagnetic spectrum. QCLs have almost all the desirable characteristics of a laser for spectroscopy applications such as narrow spectral linewidth ideal for high selectivity measurement, high power enabling high sensitivity sensing and more importantly they emit in the finger-print region of most of the trace gases and large molecules. The need for widely tunable QCLs is now more pressing than ever before. A single mode quantum cascade laser (QCL) such as a distributed feedback (DFB) QCL, is an ideal light source for gas sensing in the MIR wavelength range. Despite their performance and reliability, DFB QCLs are limited by their relatively narrow wavelength tuning range determined by the thermal rollover of the laser. An external cavity (EC) QCL, on the other hand, is a widely tunable laser source, and so far is the choice mid-infrared single frequency light sources for detecting multiple species/large molecules. However, EC QCLs can be complex, bulky and expensive. In the quest for finding alternative broadly wavelength tunable sources in the mid-infrared, many monolithic tunable QCLs are recently proposed and fabricated, including SG-DBR, DFB-Arrays, Slot-hole etc. and they are all of potentially of interest as a candidate for multi-gas sensing and monitoring applications, due to their large tuning range (>50 cm-1), and potentially low

  12. Gas tax/public transit annual expenditure report pursuant to the agreement on the transfer of federal gas tax revenue and the agreement on the transfer of public transit funds for the period April 1, 2006 to March 31, 2007

    International Nuclear Information System (INIS)

    Binnie, B.; Taylor, R.; Gibson, B.

    2007-09-01

    Federal funding initiatives for local infrastructure and capacity building was discussed with particular reference to the unique partnerships between the Canada-British Columbia Agreement on the transfer of federal gas tax revenues and the Canada-British Columbia agreement on the transfer of funds for public transit. The agreements reflect the nature of intergovernmental relations in British Columbia where the Union of British Columbia Municipalities (UBCM) works together with both federal and provincial governments to promote sustainable communities. This report identified the initiatives that are underway in communities across British Columbia as they begin to implement Gas Tax and Public Transit funded projects. These projects span a broad range of eligible project categories. The leadership role taken by local governments in the province to reduce greenhouse gas emissions was highlighted. Some of the 141 projects reported in 2007 were highlighted in this report, including improvement to public transit in the District of Saanich; TransLink bus replacement and expansion; cycling and pedestrian infrastructure; improvements to local roads and bridges; alternative energy retrofits; collection of solid waste; improvement to water systems; stormwater and wastewater treatment; capacity building; watershed protection; and water acquisition strategies. Of the projects reported, 33 per cent anticipated gas tax spending in more than 1 year, indicating either payment of capital costs as they are incurred during a construction period that spans beyond a single year, or use of gas tax funding towards the debt servicing costs related to the eligible project. tabs., figs

  13. Flow rate and source reservoir identification from airborne chemical sampling of the uncontrolled Elgin platform gas release

    Science.gov (United States)

    Lee, James D.; Mobbs, Stephen D.; Wellpott, Axel; Allen, Grant; Bauguitte, Stephane J.-B.; Burton, Ralph R.; Camilli, Richard; Coe, Hugh; Fisher, Rebecca E.; France, James L.; Gallagher, Martin; Hopkins, James R.; Lanoiselle, Mathias; Lewis, Alastair C.; Lowry, David; Nisbet, Euan G.; Purvis, Ruth M.; O'Shea, Sebastian; Pyle, John A.; Ryerson, Thomas B.

    2018-03-01

    An uncontrolled gas leak from 25 March to 16 May 2012 led to evacuation of the Total Elgin wellhead and neighbouring drilling and production platforms in the UK North Sea. Initially the atmospheric flow rate of leaking gas and condensate was very poorly known, hampering environmental assessment and well control efforts. Six flights by the UK FAAM chemically instrumented BAe-146 research aircraft were used to quantify the flow rate. The flow rate was calculated by assuming the plume may be modelled by a Gaussian distribution with two different solution methods: Gaussian fitting in the vertical and fitting with a fully mixed layer. When both solution methods were used they compared within 6 % of each other, which was within combined errors. Data from the first flight on 30 March 2012 showed the flow rate to be 1.3 ± 0.2 kg CH4 s-1, decreasing to less than half that by the second flight on 17 April 2012. δ13CCH4 in the gas was found to be -43 ‰, implying that the gas source was unlikely to be from the main high pressure, high temperature Elgin gas field at 5.5 km depth, but more probably from the overlying Hod Formation at 4.2 km depth. This was deemed to be smaller and more manageable than the high pressure Elgin field and hence the response strategy was considerably simpler. The first flight was conducted within 5 days of the blowout and allowed a flow rate estimate within 48 h of sampling, with δ13CCH4 characterization soon thereafter, demonstrating the potential for a rapid-response capability that is widely applicable to future atmospheric emissions of environmental concern. Knowledge of the Elgin flow rate helped inform subsequent decision making. This study shows that leak assessment using appropriately designed airborne plume sampling strategies is well suited for circumstances where direct access is difficult or potentially dangerous. Measurements such as this also permit unbiased regulatory assessment of potential impact, independent of the emitting

  14. USAGE OF PRESSURE OSCILLATIONS OF FLUCTUATING GAS FLOW FOR HANDLING OF 40X HARDENED STEEL SAMPLES

    Directory of Open Access Journals (Sweden)

    E. E. Il'ina

    2016-07-01

    Full Text Available Subject of Research. The paper deals with experience in the use of advanced technology of aeroacoustic treatment of materials for impact toughness improvement of the 40X type constructional steel samples. The method is based on the influence of pulsating air stream with oscillating shock-wave structures on the sample. As a result, the so-called Maxwell's waves are generated in the sample, that can lead to a beneficial transformation in the micro- and substructure and also in the phase structure of hardened steels. Obtained changes may be enough to improve impact toughness and decrease the residual stresses that arise in the course of previous treatments. Distortion of components decreases in this case, and failure probability becomes lower at the further treatment and operation. The advantage of technology is elimination of the additional heat treatment, for example, of the relaxation annealing that serves to reduce the residual stresses. This can be useful, particularly, for the preservation of high hardness and wear resistance, obtained by hardening and low-temperature tempering (about 200 ° C, as the relaxation annealing has typically a higher temperature and will result in their reduction. The toughness increase of the samples is assumed as an indicator of the positive impact of the considered treatment. Main Results. We have defined characteristics and modes of experimental acoustic transducer implementing the aeroacoustic processing. Experiments have been carried out on the impact assessment of aeroacoustic effects on the toughness of widely used 40X type steel. The obtained results enable to suggest that the application of aeroacoustic treatment for samples hardened by heat treatment leads to the toughness increasing of the investigated material. In this case an increased value of hardness obtained after heat treatment is maintained. Practical Relevance. The results supplement previously obtained experimental data for aeroacoustic

  15. Effects of dry period length on production, cash flows and greenhouse gas emissions of the dairy herd

    NARCIS (Netherlands)

    Kok, Akke; Middelaar, van Corina E.; Mostert, Pim F.; Knegsel, van Ariëtte T.M.; Kemp, Bas; Boer, de Imke J.M.; Hogeveen, Henk

    2017-01-01

    Shortening or omitting the dry period of dairy cows improves metabolic health in early lactation and reduces management transitions for dairy cows. The success of implementation of these strategies depends on their impact on milk yield and farm profitability. Insight in these impacts is valuable

  16. Full evaporation dynamic headspace and gas chromatography-mass spectrometry for uniform enrichment of odor compounds in aqueous samples.

    Science.gov (United States)

    Ochiai, Nobuo; Sasamoto, Kikuo; Hoffmann, Andreas; Okanoya, Kazunori

    2012-06-01

    A method for analysis of a wide range of odor compounds in aqueous samples at sub-ng mL⁻¹ to μg mL⁻¹ levels was developed by full evaporation dynamic headspace (FEDHS) and gas chromatography-mass spectrometry (GC-MS). Compared to conventional DHS and headspace solid phase microextraction (HS-SPME), FEDHS provides more uniform enrichment over the entire polarity range for odor compounds in aqueous samples. FEDHS at 80°C using 3 L of purge gas allows complete vaporization of 100 μL of an aqueous sample, and trapping and drying it in an adsorbent packed tube, while providing high recoveries (85-103%) of the 18 model odor compounds (water solubility at 25°C: log0.54-5.65 mg L⁻¹, vapor pressure at 25°C: 0.011-3.2 mm Hg) and leaving most of the low volatile matrix behind. The FEDHS-GC-MS method showed good linearity (r²>0.9909) and high sensitivity (limit of detection: 0.21-5.2 ng mL⁻¹) for the model compounds even with the scan mode in the conventional MS. The feasibility and benefit of the method was demonstrated with analyses of key odor compounds including hydrophilic and less volatile characteristics in beverages (whiskey and green tea). In a single malt whiskey sample, phenolic compounds including vanillin could be determined in the range of 0.92-5.1 μg mL⁻¹ (RSDfuraneol, indole, maltol, and pyrazine congeners) were determined in the range of 0.21-110 ng mL⁻¹ (RSD<10%, n=6). Copyright © 2012 Elsevier B.V. All rights reserved.

  17. Large-volume constant-concentration sampling technique coupling with surface-enhanced Raman spectroscopy for rapid on-site gas analysis

    Science.gov (United States)

    Zhang, Zhuomin; Zhan, Yisen; Huang, Yichun; Li, Gongke

    2017-08-01

    In this work, a portable large-volume constant-concentration (LVCC) sampling technique coupling with surface-enhanced Raman spectroscopy (SERS) was developed for the rapid on-site gas analysis based on suitable derivatization methods. LVCC sampling technique mainly consisted of a specially designed sampling cell including the rigid sample container and flexible sampling bag, and an absorption-derivatization module with a portable pump and a gas flowmeter. LVCC sampling technique allowed large, alterable and well-controlled sampling volume, which kept the concentration of gas target in headspace phase constant during the entire sampling process and made the sampling result more representative. Moreover, absorption and derivatization of gas target during LVCC sampling process were efficiently merged in one step using bromine-thiourea and OPA-NH4+ strategy for ethylene and SO2 respectively, which made LVCC sampling technique conveniently adapted to consequent SERS analysis. Finally, a new LVCC sampling-SERS method was developed and successfully applied for rapid analysis of trace ethylene and SO2 from fruits. It was satisfied that trace ethylene and SO2 from real fruit samples could be actually and accurately quantified by this method. The minor concentration fluctuations of ethylene and SO2 during the entire LVCC sampling process were proved to be samples were achieved in range of 95.0-101% and 97.0-104% respectively. It is expected that portable LVCC sampling technique would pave the way for rapid on-site analysis of accurate concentrations of trace gas targets from real samples by SERS.

  18. Human exposure to unconventional natural gas development: A public health demonstration of periodic high exposure to chemical mixtures in ambient air.

    Science.gov (United States)

    Brown, David R; Lewis, Celia; Weinberger, Beth I

    2015-01-01

    Directional drilling and hydraulic fracturing of shale gas and oil bring industrial activity into close proximity to residences, schools, daycare centers and places where people spend their time. Multiple gas production sources can be sited near residences. Health care providers evaluating patient health need to know the chemicals present, the emissions from different sites and the intensity and frequency of the exposures. This research describes a hypothetical case study designed to provide a basic model that demonstrates the direct effect of weather on exposure patterns of particulate matter smaller than 2.5 microns (PM2.5) and volatile organic chemicals (VOCs). Because emissions from unconventional natural gas development (UNGD) sites are variable, a short term exposure profile is proposed that determines 6-hour assessments of emissions estimates, a time scale needed to assist physicians in the evaluation of individual exposures. The hypothetical case is based on observed conditions in shale gas development in Washington County, Pennsylvania, and on estimated emissions from facilities during gas development and production. An air exposure screening model was applied to determine the ambient concentration of VOCs and PM2.5 at different 6-hour periods of the day and night. Hourly wind speed, wind direction and cloud cover data from Pittsburgh International Airport were used to calculate the expected exposures. Fourteen months of daily observations were modeled. Higher than yearly average source terms were used to predict health impacts at periods when emissions are high. The frequency and intensity of exposures to PM2.5 and VOCs at a residence surrounded by three UNGD facilities was determined. The findings show that peak PM2.5 and VOC exposures occurred 83 times over the course of 14 months of well development. Among the stages of well development, the drilling, flaring and finishing, and gas production stages produced higher intensity exposures than the

  19. Gas-Cooled Thermal Reactor Program. Annual technical progress report for the period ending September 30, 1981

    International Nuclear Information System (INIS)

    1982-03-01

    This report provides descriptions and results of the technical effort during FY81 on the Gas-Cooled Thermal Reactor Program. The FY81 work was organized according to the Work Breakdown Structure (WBS) for the National HTGR Program, and fell within five of the WBS tasks. The work on Market Definition and Development (WBS 03) was associated with estimating product costs for HTGR systems and their alternatives, projecting markets and market penetrations for these systems, and providing costs and market input to application analyses and component design. The Plant Technology (WBS 13) effort was mainly in the development of the systems dynamic computer code, STAR, for the transient analysis of HTGR's in reformer applications. The analysis of pebble bed reactors (PBR) was performed under Technology Transfer (WBS 15). The effort on components and systems within the nuclear heat source for reforming plants was performed under High Temperature Nuclear Heat Source (WBS 42)

  20. An analytical method for trifluoroacetic Acid in water and air samples using headspace gas chromatographic determination of the methyl ester.

    Science.gov (United States)

    Zehavi, D; Seiber, J N

    1996-10-01

    An analytical method has been developed for the determination of trace levels of trifluoroacetic acid (TFA), an atmospheric breakdown product of several of the hydrofluorocarbon (HFC) and hydrochlorofluorocarbon (HCFC) replacements for the chlorofluorocarbon (CFC) refrigerants, in water and air. TFA is derivatized to the volatile methyl trifluoroacetate (MTFA) and determined by automated headspace gas chromatography (HSGC) with electron-capture detection or manual HSGC using GC/MS in the selected ion monitoring (SIM) mode. The method is based on the reaction of an aqueous sample containing TFA with dimethyl sulfate (DMS) in concentrated sulfuric acid in a sealed headspace vial under conditions favoring distribution of MTFA to the vapor phase. Water samples are prepared by evaporative concentration, during which TFA is retained as the anion, followed by extraction with diethyl ether of the acidified sample and then back-extraction of TFA (as the anion) in aqueous bicarbonate solution. The extraction step is required for samples with a relatively high background of other salts and organic materials. Air samples are collected in sodium bicarbonate-glycerin-coated glass denuder tubes and prepared by rinsing the denuder contents with water to form an aqueous sample for derivatization and analysis. Recoveries of TFA from spiked water, with and without evaporative concentration, and from spiked air were quantitative, with estimated detection limits of 10 ng/mL (unconcentrated) and 25 pg/mL (concentrated 250 mL:1 mL) for water and 1 ng/m(3) (72 h at 5 L/min) for air. Several environmental air, fogwater, rainwater, and surface water samples were successfully analyzed; many showed the presence of TFA.

  1. Gas treatment of Cr(VI)-contaminated sediment samples from the North 60's pits of the chemical waste landfill

    International Nuclear Information System (INIS)

    Thornton, E.C.; Amonette, J.E.

    1997-12-01

    Twenty sediment samples were collected at depths ranging from 5 to 100 ft (1.5 to 30 m) beneath a metal-contaminated plating-waste site and extensively characterized for Cr(VI) content and environmental availability. Three samples were selected for treatment with diluted gas mixtures with the objective of converting Cr(VI) to Cr(III), which is relatively nontoxic and immobile. These tests were designed to provide information needed to evaluate the potential application of gas injection as an in situ remediation technique. Gas treatment was performed in small columns (4.9-cm ID, 6.4- to 13.9-cm long) using 100 ppm (μL L -1 ) H 2 S or ethylene mixtures in N 2 . Treatment progress during the tests involving H 2 S was assessed by monitoring the breakthrough of H 2 S. Evaluation of H 2 S treatment efficacy included (1) water-leaching of treated and untreated columns for ten days, (2) repetitive extraction of treated and untreated subsamples by water, 0.01 M phosphate (pH 7) or 6 M HCl solutions, and (3) Cr K-edge X-ray absorption near-edge structure (XANES) spectroscopy of treated and untreated subsamples. Results of the water-leaching studies showed that the H 2 S treatment decreased Cr(VI) levels in the column effluent by 90% to nearly 100%. Repetitive extractions by water and phosphate solutions echoed these results, and the extraction by HCl released only 35-40% as much Cr in the treated as in the untreated samples. Analysis by XANES spectroscopy showed that a substantial portion of the Cr in the samples remained as Cr(VI) after treatment, even though it was not available to the water and phosphate extracting solutions. These results suggest that this residual Cr(VI) is present in low solubility phases such as PbCrO 4 or sequestered in unreacted grain interiors under impermeable coatings formed during H 2 S treatment. However, this fraction is essentially immobile and thus unavailable to the environment

  2. Evolved Gas Measurements Planned for the Lower Layers of the Gale Crater Mound with the Sample Analysis at Mars Instrument Suite

    Science.gov (United States)

    Mahaffy, P. R.; Franz, H.; McAdam, A.; Conrad, P. G.; Brunner, A.; Cabane, M.; Webster, C. R.

    2011-12-01

    The lower mound strata of Gale Crater provide a diverse set of chemical environments for exploration by the varied tools of the Curiosity Rover of the Mars Science Laboratory (MSL) Mission. Orbital imaging and spectroscopy clearly reveal distinct layers of hydrated minerals, sulfates, and clays with abundant evidence of a variety of fluvial processes. The three instruments of the MSL Sample Analysis at Mars (SAM) investigation, the Quadrupole Mass Spectrometer (QMS), the Tunable Laser Spectrometer (TLS), and the Gas Chromatograph (GC) are designed to analyze either atmospheric gases or volatiles thermally evolved or chemically extracted from powdered rock or soil. The presence or absence of organic compounds in these layers is of great interest since such an in situ search for this type of record has not been successfully implemented since the mid-70s Viking GCMS experiments. However, regardless of the outcome of the analysis for organics, the abundance and isotopic composition of thermally evolved inorganic compounds should also provide a rich data set to complement the mineralogical and elemental information provided by other MSL instruments. In addition, these evolved gas analysis (EGA) experiments will help test sedimentary models proposed by Malin and Edgett (2000) and then further developed by Milliken et al (2010) for Gale Crater. In the SAM EGA experiments the evolution temperatures of H2O, CO2, SO2, O2, or other simple compounds as the samples are heated in a helium stream to 1000C provides information on mineral types and their associations. The isotopic composition of O, H, C, and S can be precisely determined in several evolved compounds and compared with the present day atmosphere. Such SAM results might be able to test mineralogical evidence of changing sedimentary and alteration processes over an extended period of time. For example, Bibring et al (2006) have suggested such a major shift from early nonacidic to later acidic alteration. We will

  3. Evolved Gas Measurements Planned for the Lower Layers of the Gale Crater Mound with the Sample Analysis at Mars Instrument Suite

    Science.gov (United States)

    Mahaffy, Paul; Brunner, Anna; McAdam, Amy; Franz, Heather; Conrad, Pamela; Webster, Chris; Cabane, Michel

    2009-01-01

    The lower mound strata of Gale Crater provide a diverse set of chemical environments for exploration by the varied tools of the Curiosity Rover of the Mars Science Laboratory (MSL) Mission. Orbital imaging and spectroscopy clearly reveal distinct layers of hydrated minerals, sulfates, and clays with abundant evidence of a variety of fluvial processes. The three instruments of the MSL Sample Analysis at aMars (SAM) investigation, the Quadrupole Mass Spectrometer (QMS), the Tunable Laser Spectrometer (TLS), and the Gas Chromatograph (GC) are designed to analyze either atmospheric gases or volatiles thermally evolved or chemically extracted from powdered rock or soil. The presence or absence of organic compounds in these layers is of great interest since such an in situ search for this type of record has not been successfully implemented since the mid-60s Viking GCMS experiments. However, regardless of the outcome of the analysis for organics, the abundance and isotopic composition of thermally evolved inorganic compounds should also provide a rich data set to complement the mineralogical and elemental information provided by other MSL instruments. In addition, these evolved gas analysis (EGA) experiments will help test sedimentary models proposed by Malin and Edgett (2000) and then further developed by Milliken et al (2010) for Gale Crater. In the SAM EGA experiments the evolution temperatures of H2O, CO2, SO2, O2, or other simple compounds as the samples are heated in a helium stream to 1000 C provides information on mineral types and their associations. The isotopic composition of O, H, C, and S can be precisely determined in several evolved compounds and compared with the present day atmosphere. Such SAM results might be able to test mineralogical evidence of changing sedimentary and alteration processes over an extended period of time. For example, Bibring et al (2006) have suggested such a major shift from early nonacidic to later acidic alteration. We will

  4. MEASUREMENT OF PYRETHROID RESIDUES IN ENVIRONMENTAL AND FOOD SAMPLES BY ENHANCED SOLVENT EXTRACTION/SUPERCRITICAL FLUID EXTRACTION COUPLED WITH GAS CHROMATOGRAPHY-TANDEM MASS SPECTROMETRY

    Science.gov (United States)

    The abstract summarizes pyrethorid methods development research. It provides a summary of sample preparation and analytical techniques such as supercritical fluid extraction, enhance solvent extraction, gas chromatography and tandem mass spectrometry.

  5. Potential denitrification in arable soil samples at winter temperatures - measurements by 15N gas analysis

    International Nuclear Information System (INIS)

    Lippold, H.; Foerster, I.; Matzel, W.

    1989-01-01

    In samples from the plough horizon of five soils taken after cereal harvest, denitrification was measured as volatilization of N 2 and N 2 O from 15 N nitrate in the absence of O 2 . Nitrate contents lower than 50 ppm N (related to soil dry matter) had only a small effect on denitrification velocity in four of the five soils. In a clay soil dependence on nitrate concentration corresponded to a first-order reaction. Available C was no limiting factor. Even at zero temperatures remarkable N amounts (on average 0.2 ppm N per day) were still denitrified. The addition of daily turnover rates in relation to soil temperatures prevailing from December to March revealed potential turnovers in the 0-to-30-cm layer of the soils to average 28 ± 5 ppm N. (author)

  6. New Frontiers Science at Venus from Orbit plus Atmospheric Gas Sampling

    Science.gov (United States)

    Smrekar, Suzanne; Dyar, Melinda; Hensley, Scott; Helbert, Joern; VOX Science and Engineering Teams

    2017-10-01

    Venus remains the most Earth-like body in terms of size, composition, surface age, and insulation. Venus Origins Explorer (VOX) determines how Earth’s twin diverged, and enables breakthroughs in our understanding of rocky planet evolution and habitability. At the time of the Decadal Survey the ability to map mineralogy from orbit (Helbert et al.) and present-day radar techniques to detect active deformation were not fully appreciated. VOX leverages these methods and in-situ noble gases to answer New Frontiers science objectives:1. Atmospheric physics/chemistry: noble gases and isotopes to constrain atmospheric sources, escape processes, and integrated volcanic outgassing; global search for current volcanically outgassed water.2. Past hydrological cycles: global tessera composition to determine the role of volatiles in crustal formation.3. Crustal physics/chemistry: global crustal mineralogy/chemistry, tectonic processes, heat flow, resolve the catastrophic vs. equilibrium resurfacing debate, active geologic processes and possible crustal recycling.4. Crustal weathering: surface-atmosphere weathering reactions from redox state and the chemical equilibrium of the near-surface atmosphere.5. Atmospheric properties/winds: map cloud particle modes and their temporal variations, and track cloud-level winds in the polar vortices.6. Surface-atmosphere interactions: chemical reactions from mineralogy; weathering state between new, recent and older flows; possible volcanically outgassed water.VOX’s Atmosphere Sampling Vehicle (ASV) dips into and samples the well-mixed atmosphere, using Venus Original Constituents Experiment (VOCE) to measure noble gases. VOX’s orbiter carries the Venus Emissivity Mapper (VEM) and the Venus Interferometric Synthetic Aperture Radar (VISAR), and maps the gravity field using Ka-band tracking.VOX is the logical next mission to Venus because it delivers: 1) top priority atmosphere, surface, and interior science; 2) key global data for

  7. Determination of thiobencarb in water samples by gas chromatography using a homogeneous liquid-liquid microextraction via flotation assistance procedure

    Directory of Open Access Journals (Sweden)

    H.A. Mashayekhi

    2013-09-01

    Full Text Available Homogeneous liquid-liquid microextraction via flotation assistance (HLLME-FA coupled with gas chromatography-flame ionization detection (GC-FID was applied for the extraction and determination of thiobencarb in water samples. In this study, a special extraction cell was designed to facilitate collection of the low-density solvent extraction. No centrifugation was required in this procedure. The water sample solution was added into the extraction cell which contained an appropriate mixture of toluene (as an extraction solvent and acetone (as a homogeneous solvent. By using air flotation, the organic solvent was collected at the conical part of the designed cell. The effect of the different parameters on the efficiency of extraction such as type and volume of extraction and homogeneous solvents, ionic strength and extraction time were studied and optimized. Under the optimal conditions, linearity of the method was in the range of 1.0-200 µg L-1. The relative standard deviations in the real samples varied from 7.8-11.7 % (n = 3. The proposed method was successfully applied to analysis of thiobencarb in the water samples and satisfactory results were obtained.DOI: http://dx.doi.org/10.4314/bcse.v27i3.4

  8. Solid-phase microextraction for gas chromatographic/mass spectrometric analysis of dimethoate in human biological samples.

    Science.gov (United States)

    Gallardo, E; Barroso, M; Margalho, C; Cruz, A; Vieira, D N; López-Rivadulla, M

    2006-01-01

    A new, simple and rapid procedure for the determination of dimethoate in urine and blood samples was developed using direct immersion solid-phase microextraction and gas chromatography/mass spectrometry. This technique required only 0.1 mL of sample, and ethion was used as internal standard. Two types of coated fibre were compared (100 microm polydimethylsiloxane, and 65 microm Carbowax/divinylbenzene). Other parameters, such as extraction temperature, adsorption and desorption time, salt addition, agitation and pH, were optimized to enhance the sensitivity of the method. Limits of detection (LODs) and quantitation (LOQs) were 50 and 100 ng/mL for urine and 200 and 500 ng/mL for blood, respectively. The method was found to be linear between the LOQ and 40 microg/mL for urine, and between the LOQ and 50 microg/mL for blood, with correlation coefficients ranging from 0.9923-0.9996. Precision (intra- and interday) and accuracy were in conformity with the criteria normally accepted in bioanalytical method validation. The mean absolute recoveries of dimethoate were 1.24 and 0.50% for urine and blood, respectively. Because of its simplicity and the fact that small volumes of sample are used, the described method can be successfully used in the diagnosis of poisoning by this pesticide, namely in those situations where the sample volume is limited, as frequently occurs in forensic toxicology. Copyright 2006 John Wiley & Sons, Ltd.

  9. Quantitative analysis of detailed lignin monomer composition by pyrolysis-gas chromatography combined with preliminary acetylation of the samples.

    Science.gov (United States)

    Sonoda, T; Ona, T; Yokoi, H; Ishida, Y; Ohtani, H; Tsuge, S

    2001-11-15

    Detailed quantitative analysis of lignin monomer composition comprising p-coumaryl, coniferyl, and sinapyl alcohol and p-coumaraldehyde, coniferaldehyde, and sinapaldehyde in plant has not been studied from every point mainly because of artifact formation during the lignin isolation procedure, partial loss of the lignin components inherent in the chemical degradative methods, and difficulty in the explanation of the complex spectra generally observed for the lignin components. Here we propose a new method to quantify lignin monomer composition in detail by pyrolysis-gas chromatography (Py-GC) using acetylated lignin samples. The lignin acetylation procedure would contribute to prevent secondary formation of cinnamaldehydes from the corresponding alcohol forms during pyrolysis, which are otherwise unavoidable in conventional Py-GC process to some extent. On the basis of the characteristic peaks on the pyrograms of the acetylated sample, lignin monomer compositions in various dehydrogenative polymers (DHP) as lignin model compounds were determined, taking even minor components such as cinnamaldehydes into consideration. The observed compositions by Py-GC were in good agreement with the supplied lignin monomer contents on DHP synthesis. The new Py-GC method combined with sample preacetylation allowed us an accurate quantitative analysis of detailed lignin monomer composition using a microgram order of extractive-free plant samples.

  10. Mosquitoes of the Caatinga: 2. Species from periodic sampling of bromeliads and tree holes in a dry Brazilian forest.

    Science.gov (United States)

    Marteis, Letícia Silva; Natal, Delsio; Sallum, Maria Anice Mureb; Medeiros-Sousa, Antônio Ralph; Corte, Roseli La

    2017-07-01

    The Caatinga is a dry tropical forest, located in the Brazilian semiarid region and rich in phytotelmata. This study investigated the culicid fauna of phytotelmata of the caatinga by sampling for 19 consecutive months aquatic immatures from tree holes and bromeliads. A total of 127L of water was taken from the plants, containing 6764 immature culicids of 16 species, of which 11 (69%) are undescribed and respond to 90% of the total abundance of the specimens collected. Epiphytic bromeliads harbor a large number of immature Culicidae, although terrestrial bromeliads are the most abundant and widely distributed in the region. The richness of culicid species was similar between terrestrial and epiphytic bromeliads and lower in habitats represented by tree hole phytotelmata. There was no similarity in the composition of culicid species that developed in bromeliads or tree holes. Temperature and humidity were the environmental parameters most strongly associated with the proportion of positive plants. The Caatinga has a great number of endemic species that remain unknown to science and many additional culicid species may await discovery from there. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Determination of 2-Octanone in Biological Samples Using Liquid–Liquid Microextractions Followed by Gas Chromatography–Flame Ionization Detectio

    Directory of Open Access Journals (Sweden)

    Abolghasem Jouyban, Maryam Abbaspour, Mir Ali Farajzadeh, Maryam Khoubnasabjafari

    2017-06-01

    Full Text Available Background: Analysis of chemicals in biological fluids is required in many areas of medical sciences. Rapid, highly efficient, and reliable dispersive and air assisted liquid–liquid microextraction methods followed by gas chromatography-flame ionization detection were developed for the extraction, preconcentration, and determination of 2-octanone in human plasma and urine samples. Methods: Proteins of plasma samples are precipitated by adding methanol and urine sample is diluted with water prior to performing the microextraction procedure. Fine organic solvent droplets are formed by repeated suction and injection of the mixture of sample solution and extraction solvent into a test tube with a glass syringe. After extraction, phase separation is performed by centrifuging and the enriched analyte in the sedimented organic phase is determined by the separation system. The main factors influencing the extraction efficiency including extraction solvent type and volume, salt addition, pH, and extraction times are investigated. Results: Under the optimized conditions, the proposed method showed good precision (relative standard deviation less than 7%. Limit of detection and lower limit of quantification for 2-octanone were obtained in the range of 0.1–0.5 µg mL−1. The linear ranges were 0.5-500 and 0.5-200 µg mL−1 in plasma and urine, respectively (r2 ≥ 0.9995. Enrichment factors were in the range of 13-37. Good recoveries (55–86% were obtained for the spiked samples. Conclusion: Preconcentration methods coupled with GC analysis were developed and could be used to monitor 2-octanone in biological samples.

  12. Chemometric deconvolution of gas chromatographic unresolved conjugated linoleic acid isomers triplet in milk samples.

    Science.gov (United States)

    Blasko, Jaroslav; Kubinec, Róbert; Ostrovský, Ivan; Pavlíková, Eva; Krupcík, Ján; Soják, Ladislav

    2009-04-03

    A generally known problem of GC separation of trans-7;cis-9; cis-9,trans-11; and trans-8,cis-10 CLA (conjugated linoleic acid) isomers was studied by GC-MS on 100m capillary column coated with cyanopropyl silicone phase at isothermal column temperatures in a range of 140-170 degrees C. The resolution of these CLA isomers obtained at given conditions was not high enough for direct quantitative analysis, but it was, however, sufficient for the determination of their peak areas by commercial deconvolution software. Resolution factors of overlapped CLA isomers determined by the separation of a model CLA mixture prepared by mixing of a commercial CLA mixture and CLA isomer fraction obtained by the HPLC semi-preparative separation of milk fatty acids methyl esters were used to validate the deconvolution procedure. Developed deconvolution procedure allowed the determination of the content of studied CLA isomers in ewes' and cows' milk samples, where dominant isomer cis-9,trans-11 is eluted between two small isomers trans-7,cis-9 and trans-8,cis-10 (in the ratio up to 1:100).

  13. Characteristics of volcanic gas correlated to the eruption activity; Case study in the Merapi Volcano, periods of 1990-1994

    Directory of Open Access Journals (Sweden)

    Priatna Priatna

    2014-06-01

    Full Text Available http://dx.doi.org/10.17014/ijog.vol2no4.20074Volcanic gases, collected from Gendol and Woro solfatara fields, the summit of Merapi Volcano during 1990-1994, show an increase in chemical composition of H , CO, CO , SO , and HCl prior to the volcanic events, on the contrary to the drastic decreasing water vapour. The carbon/sulfur ratio of the volcanic gases lies between 1.5 and 5.7 which means that they were derived from the fresh magma. The Apparent Equilibrium Temperature (AET which is calculated from chemical compositions of volcanic gases using reaction of SO +3H = H S+2H O showed an increasing value prior to the volcanic events. The Merapi activities lasted during August 1990 to November 1994 showed a significant increase in ratio SO /H S prior to the November 1994 pyroclastic flow. The isotopic composition of volcanic gas condensates indicates that water vapour in Gendol is directly derived from the fresh magma. On the other hand, the contamination and cooling by the subsurface water occurred around the Woro field at a shallow part. 

  14. Evolved Gas Analyses of the Murray Formation in Gale Crater, Mars: Results of the Curiosity Rover's Sample Analysis at Mars (SAM) Instrument

    Science.gov (United States)

    Sutter, B.; McAdam, A. C.; Rampe, E. B.; Thompson, L. M.; Ming, D. W.; Mahaffy, P. R.; Navarro-Gonzalez, R.; Stern, J. C.; Eigenbrode, J. L.; Archer, P. D.

    2017-01-01

    The Sample Analysis at Mars (SAM) instrument aboard the Mars Science Laboratory rover has analyzed 13 samples from Gale Crater. All SAM-evolved gas analyses have yielded a multitude of volatiles (e.g., H2O, SO2, H2S, CO2, CO, NO, O2, HCl) [1- 6]. The objectives of this work are to 1) Characterize recent evolved SO2, CO2, O2, and NO gas traces of the Murray formation mudstone, 2) Constrain sediment mineralogy/composition based on SAM evolved gas analysis (SAM-EGA), and 3) Discuss the implications of these results relative to understanding the geological history of Gale Crater.

  15. Evolved Gas Analyses of Sedimentary Materials in Gale Crater, Mars: Results of the Curiosity Rover's Sample Analysis at Mars (SAM) Instrument from Yellowknife Bay to the Stimson Formation

    Science.gov (United States)

    Sutter, B.; McAdam, A. C.; Rampe, E. B.; Ming, D. W.; Mahaffy, P. R.; Navarro-Gonzalez, R.; Stern, J. C.; Eigenbrode, J. L.; Archer, P. D.

    2016-01-01

    The Sample Analysis at Mars (SAM) instrument aboard the Mars Science Laboratory rover has analyzed 10 samples from Gale Crater. All SAM evolved gas analyses have yielded a multitude of volatiles (e.g, H2O, SO2, H2S, CO2, CO, NO, O2, HC1). The objectives of this work are to 1) Characterize the evolved H2O, SO2, CO2, and O2 gas traces of sediments analyzed by SAM through sol 1178, 2) Constrain sediment mineralogy/composition based on SAM evolved gas analysis (SAM-EGA), and 3) Discuss the implications of these results releative to understanding the geochemical history of Gale Crater.

  16. A study on the separation and extraction of polycyclic aromatic hydrocarbons in water sample by gas chromatography/mass spectrometry

    International Nuclear Information System (INIS)

    Lee, Won; Hong, Jee Eun; Park, Song Ja; Pyo, Hee Soo; Kim, In Hwan

    1998-01-01

    The separation and sample extraction methods of 19 polycyclic aromatic hydrocarbons (PAH S ) in water samples were investigated by gas chromatography/mass spectrometry (GC/MS) and some ex-traction methods involved liquid-liquid extraction, disk extraction and solid-phase extraction methods. The separation of 19 PAH s was possible by partial variation of oven temperature of GC/MS in temperature range 80∼310.deg.C. Extraction procedures of PAH s in water samples were somewhat modified and com-pared as extraction recoveries and the simplicity of methods. Extraction recoveries of PAH s were 71.3∼109.5% by liquid-liquid extraction method. By using disk extraction, good extraction recoveries (80.7∼94.9%) were obtained in case of C 1 8 disk extraction method by filtration. And extraction recoveries of PAH s by C 1 8 solid-phase were in the range of 51.8∼77.9%. Method detection limits (S/N=5) of 19 PAH s were in the range of 0.25∼6.25 ppb by liquid-liquid extraction and solid-phase extraction and 0.05∼1.25 ppb by disk extraction methods

  17. Periodic DFT study of acidic trace atmospheric gas molecule adsorption on Ca- and Fe-doped MgO(001) surface basic sites.

    Science.gov (United States)

    Baltrusaitis, Jonas; Hatch, Courtney; Orlando, Roberto

    2012-08-02

    The electronic properties of undoped and Ca- or Fe-doped MgO(001) surfaces, as well as their propensity toward atmospheric acidic gas (CO2, SO2, and NO2) uptake was investigated with an emphasis on gas adsorption on the basic MgO oxygen surface sites, O(surf), using periodic density functional theory (DFT) calculations. Adsorption energy calculations show that MgO doping will provide stronger interactions of the adsorbate with the O(surf) sites than the undoped MgO for a given adsorbate molecule. Charge transfer from the iron atom in Fe-doped MgO(001) to NO2 was shown to increase the binding interaction between adsorbate by an order of magnitude, when compared to that of undoped and Ca-doped MgO(001) surfaces. Secondary binding interactions of adsorbate oxygen atoms were observed with surface magnesium sites at distances close to those of the Mg-O bond within the crystal. These interactions may serve as a preliminary step for adsorption and facilitate further adsorbate transformations into other binding configurations. Impacts on global atmospheric chemistry are discussed as these adsorption phenomena can affect atmospheric gas budgets via altered partitioning and retention on mineral aerosol surfaces.

  18. Distribution of Gas Phase Polycyclic Aromatic Hydrocarbons (PAHs in Selected Indoor and Outdoor Air Samples of Malaysia: a Case Study in Serdang, Selangor and Bachang, Malacca

    Directory of Open Access Journals (Sweden)

    Haris Hafizal Abd Hamid

    2017-07-01

    Full Text Available Distribution of 10 polycyclic aromatic hydrocarbons (PAHs in the gas phase of air from selected indoor and outdoor areas of Selangor and Malacca, Malaysia has been investigated. A locally designed Semi Permeable Membrane Device (SPMD was applied for passive air sampling for 37 days at selected locations. Cleanup was carried out with Gas Purge - Micro Syringe Extraction (GP-MSE and the final analysis was using Gas Chromatography-Mass Spectrometry (GC-MS. In this study, 6 indoor and 12 outdoor locations were selected for air sampling. A total of 10 compounds of PAHs (Ʃ10PAHs were determined in the range of 0.218 ng/m3 - 1.692 ng/m3 and 0.378 ng/m3 - 1.492 ng/m3 in outdoor and indoor samples respectively. In the outdoor samples, locations such as near a petrol station and heavy traffic showed the maximum levels of Ʃ10PAHs, while rooftop samples showed the lowest Ʃ10PAHs. The distribution of gas phase Ʃ10PAHs was influenced by vehicular emission. Low molecular weight (LMW compounds (2-3 rings were dominant in all samples (>70% indicating that SPMD has successfully sampled the gas phase of the air.

  19. Drought-induced defoliation and long periods of near-zero gas exchange play a key role in accentuating metabolic decline of Scots pine.

    Science.gov (United States)

    Poyatos, Rafael; Aguadé, David; Galiano, Lucía; Mencuccini, Maurizio; Martínez-Vilalta, Jordi

    2013-10-01

    Drought-induced defoliation has recently been associated with the depletion of carbon reserves and increased mortality risk in Scots pine (Pinus sylvestris). We hypothesize that defoliated individuals are more sensitive to drought, implying that potentially higher gas exchange (per unit of leaf area) during wet periods may not compensate for their reduced photosynthetic area. We measured sap flow, needle water potentials and whole-tree hydraulic conductance to analyse the drought responses of co-occurring defoliated and nondefoliated Scots pines in northeast Spain during typical (2010) and extreme (2011) drought conditions. Defoliated Scots pines showed higher sap flow per unit leaf area during spring, but were more sensitive to summer drought, relative to nondefoliated pines. This pattern was associated with a steeper decline in soil-to-leaf hydraulic conductance with drought and an enhanced sensitivity of canopy conductance to soil water availability. Near-homeostasis in midday water potentials was observed across years and defoliation classes, with minimum values of -2.5 MPa. Enhanced sensitivity to drought and prolonged periods of near-zero gas exchange were consistent with low levels of carbohydrate reserves in defoliated trees. Our results support the critical links between defoliation, water and carbon availability, and their key roles in determining tree survival and recovery under drought. © 2013 The Authors. New Phytologist © 2013 New Phytologist Trust.

  20. Reliability of Serum Metabolites over a Two-Year Period: A Targeted Metabolomic Approach in Fasting and Non-Fasting Samples from EPIC

    Science.gov (United States)

    Achaintre, David; Sacerdote, Carlotta; Vineis, Paolo; Key, Timothy J.; Onland Moret, N. Charlotte; Scalbert, Augustin; Rinaldi, Sabina; Ferrari, Pietro

    2015-01-01

    Objective Although metabolic profiles have been associated with chronic disease risk, lack of temporal stability of metabolite levels could limit their use in epidemiological investigations. The present study aims to evaluate the reliability over a two-year period of 158 metabolites and compare reliability over time in fasting and non-fasting serum samples. Methods Metabolites were measured with the AbsolueIDQp180 kit (Biocrates, Innsbruck, Austria) by mass spectrometry and included acylcarnitines, amino acids, biogenic amines, hexoses, phosphatidylcholines and sphingomyelins. Measurements were performed on repeat serum samples collected two years apart in 27 fasting men from Turin, Italy, and 39 non-fasting women from Utrecht, The Netherlands, all participating in the European Prospective Investigation into Cancer and Nutrition (EPIC) study. Reproducibility was assessed by estimating intraclass correlation coefficients (ICCs) in multivariable mixed models. Results In fasting samples, a median ICC of 0.70 was observed. ICC values were fasting samples, the median ICC was 0.54. ICC values were fasting as compared to fasting samples, with a statistically significant difference for 19–36% of acylcarnitines, phosphatidylcholines and sphingomyelins. Conclusion A single measurement per individual may be sufficient for the study of 73% and 52% of the metabolites showing ICCs >0.50 in fasting and non-fasting samples, respectively. ICCs were higher in fasting samples that are preferable to non-fasting. PMID:26274920

  1. Random-effects linear modeling and sample size tables for two special crossover designs of average bioequivalence studies: the four-period, two-sequence, two-formulation and six-period, three-sequence, three-formulation designs.

    Science.gov (United States)

    Diaz, Francisco J; Berg, Michel J; Krebill, Ron; Welty, Timothy; Gidal, Barry E; Alloway, Rita; Privitera, Michael

    2013-12-01

    Due to concern and debate in the epilepsy medical community and to the current interest of the US Food and Drug Administration (FDA) in revising approaches to the approval of generic drugs, the FDA is currently supporting ongoing bioequivalence studies of antiepileptic drugs, the EQUIGEN studies. During the design of these crossover studies, the researchers could not find commercial or non-commercial statistical software that quickly allowed computation of sample sizes for their designs, particularly software implementing the FDA requirement of using random-effects linear models for the analyses of bioequivalence studies. This article presents tables for sample-size evaluations of average bioequivalence studies based on the two crossover designs used in the EQUIGEN studies: the four-period, two-sequence, two-formulation design, and the six-period, three-sequence, three-formulation design. Sample-size computations assume that random-effects linear models are used in bioequivalence analyses with crossover designs. Random-effects linear models have been traditionally viewed by many pharmacologists and clinical researchers as just mathematical devices to analyze repeated-measures data. In contrast, a modern view of these models attributes an important mathematical role in theoretical formulations in personalized medicine to them, because these models not only have parameters that represent average patients, but also have parameters that represent individual patients. Moreover, the notation and language of random-effects linear models have evolved over the years. Thus, another goal of this article is to provide a presentation of the statistical modeling of data from bioequivalence studies that highlights the modern view of these models, with special emphasis on power analyses and sample-size computations.

  2. Determination of Volatile Compounds in Four Commercial Samples of Japanese Green Algae Using Solid Phase Microextraction Gas Chromatography Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Masayoshi Yamamoto

    2014-01-01

    Full Text Available Green algae are of great economic importance. Seaweed is consumed fresh or as seasoning in Japan. The commercial value is determined by quality, color, and flavor and is also strongly influenced by the production area. Our research, based on solid phase microextraction gas chromatography mass spectrometry (SPME-GC-MS, has revealed that volatile compounds differ intensely in the four varieties of commercial green algae. Accordingly, 41 major volatile compounds were identified. Heptadecene was the most abundant compound from Okayama (Ulva prolifera, Tokushima (Ulva prolifera, and Ehime prefecture (Ulva linza. Apocarotenoids, such as ionones, and their derivatives were prominent volatiles in algae from Okayama (Ulva prolifera and Tokushima prefecture (Ulva prolifera. Volatile, short chained apocarotenoids are among the most potent flavor components and contribute to the flavor of fresh, processed algae, and algae-based products. Benzaldehyde was predominant in seaweed from Shizuoka prefecture (Monostroma nitidum. Multivariant statistical analysis (PCA enabled simple discrimination of the samples based on their volatile profiles. This work shows the potential of SPME-GC-MS coupled with multivariant analysis to discriminate between samples of different geographical and botanical origins and form the basis for development of authentication methods of green algae products, including seasonings.

  3. Determination of volatile compounds in four commercial samples of Japanese green algae using solid phase microextraction gas chromatography mass spectrometry.

    Science.gov (United States)

    Yamamoto, Masayoshi; Baldermann, Susanne; Yoshikawa, Keisuke; Fujita, Akira; Mase, Nobuyuki; Watanabe, Naoharu

    2014-01-01

    Green algae are of great economic importance. Seaweed is consumed fresh or as seasoning in Japan. The commercial value is determined by quality, color, and flavor and is also strongly influenced by the production area. Our research, based on solid phase microextraction gas chromatography mass spectrometry (SPME-GC-MS), has revealed that volatile compounds differ intensely in the four varieties of commercial green algae. Accordingly, 41 major volatile compounds were identified. Heptadecene was the most abundant compound from Okayama (Ulva prolifera), Tokushima (Ulva prolifera), and Ehime prefecture (Ulva linza). Apocarotenoids, such as ionones, and their derivatives were prominent volatiles in algae from Okayama (Ulva prolifera) and Tokushima prefecture (Ulva prolifera). Volatile, short chained apocarotenoids are among the most potent flavor components and contribute to the flavor of fresh, processed algae, and algae-based products. Benzaldehyde was predominant in seaweed from Shizuoka prefecture (Monostroma nitidum). Multivariant statistical analysis (PCA) enabled simple discrimination of the samples based on their volatile profiles. This work shows the potential of SPME-GC-MS coupled with multivariant analysis to discriminate between samples of different geographical and botanical origins and form the basis for development of authentication methods of green algae products, including seasonings.

  4. Separation and screening of short-chain chlorinated paraffins in environmental samples using comprehensive two-dimensional gas chromatography with micro electron capture detection.

    Science.gov (United States)

    Xia, Dan; Gao, Lirong; Zhu, Shuai; Zheng, Minghui

    2014-11-01

    Short-chain chlorinated paraffins (SCCPs) are highly complex technical mixtures with thousands of isomers and numerous homologs. They are classified as priority candidate persistent organic pollutants under the Stockholm Convention for their persistence, bioaccumulation, and toxicity. Analyzing SCCPs is challenging because of the complexity of the mixtures. Chromatograms of SCCPs acquired using one-dimensional (1D) gas chromatography (GC) contain a large characteristic "peak" with a broad and unresolved profile. Comprehensive two-dimensional GC (GC×GC) shows excellent potential for separating complex mixtures. In this study, GC×GC coupled with micro electron capture detection (μECD) was used to separate and screen SCCPs. The chromatographic parameters, including the GC column types, oven temperature program, and modulation period, were systematically optimized. The SCCP congeners were separated into groups using a DM-1 column connected to a BPX-50 column. The SCCP congeners in technical mixtures were separated according to the number of chlorine substituents for a given carbon chain length and according to the number of carbon atoms plus chlorine atoms for different carbon chain lengths. A fish tissue sample was analyzed to illustrate the feasibility of the GC×GC-μECD method in analyzing biological samples. Over 1,500 compounds were identified in the fish extract, significantly more than were identified using 1D GC. The detection limits for five selected SCCP congeners were between 1 and 5 pg/L using the GC×GC method, and these were significantly lower than those achieved using 1D GC. This method is a good choice for analysis of SCCPs in environmental samples, exhibiting good separation and good sensitivity.

  5. Distribution of Parasites Detected in Stool Samples of Patients Admitted to Our Parasitology Laboratory during a Three-Year Period between 2012 and 2014.

    Science.gov (United States)

    Selek, Mehmet Burak; Bektöre, Bayhan; Karagöz, Ergenekon; Baylan, Orhan; Özyurt, Mustafa

    2016-09-01

    Parasitic diseases are among the major public health issues worldwide. A number of tests are available for diagnosis, but the sentivity and specifity of these tests are assumed to be insufficient. Nevertheless, the most common diagnostic method is microscopic examination. In this study, we aimed to introduce the distribution of parasites detected in stool samples of patients admitted to our laboratory on the basis of parameters such as, age, and gender during a 3-year period between 2012 and 2014. In total, 6757 stool samples were included in the study. After macroscopic examination, wet mounts of all samples were examined under a light microscope using ×100 and ×400 magnification lenses. Wet mounts were prepared with physiological saline and Lugol's iodine. Parasites were detected in 3.7% (252) of the samples, while no parasites were detected in 96.3% (6505) of the samples. The distribution of intestinal parasites was as follows: Blastocystis hominis (63.5%), Giardia intestinalis (26.2%), Taenia sp. (4.8%), Enterobius vermicularis (2.4%), Entamoeba histolytica/dispar (1.6%), and Hymenolepis nana (1.6%). When the burden of intestinal parasites on public health is considered, they are still a major health issue in Turkey. The frequency of parasitic diseases can be reduced by the education of individuals and implementation of effective diagnostic methods, treatments, and preventive measures.

  6. Measurement of large asymptotic reactor periods from about 103 to 4.104 sec) to determine reactivity effects of small samples

    International Nuclear Information System (INIS)

    Grinevich, F.A.; Evchuk, A.I.; Klimentov, V.B.; Tyzh, A.V.; Churkin, Yu.I.; Yaroshevich, O.I.

    1977-01-01

    All investigation programs on fast reactor physics include measurements of low reactivity values (1-0.01)x10 -5 ΔK/K. An application of the pile oscillator technique for the purpose requires a special critical assembly for an installation of the oscillator. Thus it is of interest to develop relatively simple methods. In particular, one of such methods is the asymptotic period method which is widely used for low reactivity measurements. The description of the method and equipment developed for low reactivity measurements according to the measurements of the steady-state reactor period is presented. The equipment has been tested on the BTS-2 fast-thermal critical assembly. Measurement results on the reactivity effects of small samples in the fast zone centre are given. It is shown that the application of the method of measuring long steady-state periods and developed and tested equipment enables the reactivity of (1+-0.02)x10 -5 ΔK/K to be determined at the critical assembly power of 5 to 10 Wt. The disadvantage of the method presented is the time lost on reaching the steady-state period which results in greater sensitivity of the method to reactivity drifts

  7. Psychostimulant use among college students during periods of high and low stress: an interdisciplinary approach utilizing both self-report and unobtrusive chemical sample data.

    Science.gov (United States)

    Moore, David R; Burgard, Daniel A; Larson, Ramsey G; Ferm, Mikael

    2014-05-01

    This study quantified psychostimulant use patterns over periods of high and low stress from both self-report measures and chemical wastewater analyses and identified possible predictors of psychostimulant abuse on a college campus. Self-report data were collected at three times of varying stress levels throughout one college semester: during the first week of school (N=676), midterms (N=468), and shortly before final exams (N=400). Campus wastewater samples were collected over 72-hour periods during the same time frames as the surveys. The metabolites of Adderall and Ritalin were quantified through solid phase extraction and liquid chromatography-tandem mass spectrometry (LC-MS/MS). Samples were normalized with creatinine. Evidence was found to suggest an increase in psychostimulant use during periods of stress, with significant differences found from self-report data between the first week and midterms and from chemical data between these same two assessment periods as well as between the first week of classes and finals. Key predictors of lifetime non-prescriptive psychostimulant use included self-reported procrastination and poor time-management, use of other substances (especially nicotine/tobacco, alcohol, and cocaine), and students' perception of non-prescriptive psychostimulant use as normative on campus. The findings shed further light on psychostimulant use patterns among college students, particularly as a function of stress; the study also highlights the benefit of utilizing an interdisciplinary approach that uses both subjective and objective empirical data. The results have implications for prevention/intervention programs on college campuses designed to reduce stress and facilitate healthier coping. Copyright © 2014 Elsevier Ltd. All rights reserved.

  8. Multiscale CT-Based Computational Modeling of Alveolar Gas Exchange during Artificial Lung Ventilation, Cluster (Biot and Periodic (Cheyne-Stokes Breathings and Bronchial Asthma Attack

    Directory of Open Access Journals (Sweden)

    Andrey Golov

    2017-02-01

    Full Text Available An airflow in the first four generations of the tracheobronchial tree was simulated by the 1D model of incompressible fluid flow through the network of the elastic tubes coupled with 0D models of lumped alveolar components, which aggregates parts of the alveolar volume and smaller airways, extended with convective transport model throughout the lung and alveolar components which were combined with the model of oxygen and carbon dioxide transport between the alveolar volume and the averaged blood compartment during pathological respiratory conditions. The novel features of this work are 1D reconstruction of the tracheobronchial tree structure on the basis of 3D segmentation of the computed tomography (CT data; 1D−0D coupling of the models of 1D bronchial tube and 0D alveolar components; and the alveolar gas exchange model. The results of our simulations include mechanical ventilation, breathing patterns of severely ill patients with the cluster (Biot and periodic (Cheyne-Stokes respirations and bronchial asthma attack. The suitability of the proposed mathematical model was validated. Carbon dioxide elimination efficiency was analyzed in all these cases. In the future, these results might be integrated into research and practical studies aimed to design cyberbiological systems for remote real-time monitoring, classification, prediction of breathing patterns and alveolar gas exchange for patients with breathing problems.

  9. Evaluation of volatile profiles obtained for minimally-processed pineapple fruit samples during storage by headspace-solid phase microextraction gas chromatography-mass spectrometry

    Directory of Open Access Journals (Sweden)

    Francielle Crocetta TURAZZI

    Full Text Available Abstract This paper describes the application of the solid-phase microextraction (SPME technique for the determination and monitoring of the volatile profile of minimally-processed pineapple fruit stored at various temperatures (-12 °C, 4 °C and 25 °C for different periods (1, 4 and 10 days. The SPME fiber coating composed of Car/PDMS presented the best performance. The optimal extraction conditions obtained through a Doehlert design were 60 min at 35 °C. The profiles for the volatile compounds content of the fruit at each stage of storage were determined by gas chromatography-mass spectrometry (GC-MS. The variation in the volatile profile over time was greater when the fruit samples were stored at 25 °C and at -12 °C compared to 4 °C. Thus, according to the volatile profiles associated with the storage conditions evaluated in this study, packaged pineapple retains best its fresh fruit aroma when stored at 4 °C.

  10. Analysis of pharmaceutical and other organic wastewater compounds in filtered and unfiltered water samples by gas chromatography/mass spectrometry

    Science.gov (United States)

    Zaugg, Steven D.; Phillips, Patrick J.; Smith, Steven G.

    2014-01-01

    Research on the effects of exposure of stream biota to complex mixtures of pharmaceuticals and other organic compounds associated with wastewater requires the development of additional analytical capabilities for these compounds in water samples. Two gas chromatography/mass spectrometry (GC/MS) analytical methods used at the U.S. Geological Survey National Water Quality Laboratory (NWQL) to analyze organic compounds associated with wastewater were adapted to include additional pharmaceutical and other organic compounds beginning in 2009. This report includes a description of method performance for 42 additional compounds for the filtered-water method (hereafter referred to as the filtered method) and 46 additional compounds for the unfiltered-water method (hereafter referred to as the unfiltered method). The method performance for the filtered method described in this report has been published for seven of these compounds; however, the addition of several other compounds to the filtered method and the addition of the compounds to the unfiltered method resulted in the need to document method performance for both of the modified methods. Most of these added compounds are pharmaceuticals or pharmaceutical degradates, although two nonpharmaceutical compounds are included in each method. The main pharmaceutical compound classes added to the two modified methods include muscle relaxants, opiates, analgesics, and sedatives. These types of compounds were added to the original filtered and unfiltered methods largely in response to the tentative identification of a wide range of pharmaceutical and other organic compounds in samples collected from wastewater-treatment plants. Filtered water samples are extracted by vacuum through disposable solid-phase cartridges that contain modified polystyrene-divinylbenzene resin. Unfiltered samples are extracted by using continuous liquid-liquid extraction with dichloromethane. The compounds of interest for filtered and unfiltered sample

  11. Exploiting gas diffusion for non-invasive sampling in flow analysis: determination of ethanol in alcoholic beverages

    Directory of Open Access Journals (Sweden)

    Simone Vicente

    2006-03-01

    Full Text Available A tubular gas diffusion PTFE membrane is exploited for non-invasive sampling in flow analysis, aiming to develop an improved spectrophotometric determination of ethanol in alcoholic beverages. The probe is immersed into the sample, allowing ethanol to diffuse through the membrane. It is collected into the acceptor stream (acidic dichromate solution, leading to formation of Cr(III, monitored at 600 nm. The analytical curve is linear up to 50% (v/v ethanol, baseline drift is Uma membrana tubular de PTFE permeável a espécies gasosas foi empregada como sonda em sistemas de análises em fluxo visando a proposta de uma estratégia de amostragem não invasiva. Como aplicação, foi selecionada a determinação espectrofotométrica de etanol em bebidas alcoólicas. A sonda é imersa na amostra, permitindo que o analito se difunda através desta e seja coletado pelo fluxo aceptor (solução ácida de dicromato, levando à formação de Cr(III, o qual é monitorado a 600 nm. Linearidade da curva analítica é verificada até 50,0% (v/v de etanol (r > 0,998; n = 8, derivas de linha base são menores do que 0,005 absorbância durante períodos de 4 horas de operação e a velocidade analítica é de 30 h-1 o que corresponde a 0.6 mmol K2Cr2O7 por determinação. Os resultados são precisos (d.p.r. < 2% e concordantes com aqueles obtidos por um método oficial.

  12. Removal of gas phase low-concentration toluene over Mn, Ag and Ce modified HZSM-5 catalysts by periodical operation of adsorption and non-thermal plasma regeneration.

    Science.gov (United States)

    Wang, Wenzheng; Wang, Honglei; Zhu, Tianle; Fan, Xing

    2015-07-15

    Ag/HZSM-5, Mn/HZSM-5, Ce/HZSM-5, Ag-Mn/HZSM-5 and Ce-Mn/HZSM-5 were prepared by impregnation method. Both their adsorption capacity and catalytic activity were investigated for the removal of gas phase low-concentration toluene by periodical operation of adsorption and non-thermal plasma regeneration. Results show that catalysts loaded with Ag (Ag/HZSM-5 and Ag-Mn/HZSM-5) had larger adsorption capacity for toluene than the other catalysts. And Ag-Mn/HZSM-5 displayed the best catalytic performance for both toluene oxidation by non-thermal plasma and byproducts suppression. On the other hand, the deactivated catalyst can be fully regenerated by calcining in air stream when its adsorption capacity and catalytic activity of the Ag-Mn/HZSM-5 catalyst was found to be decreased after 10 cycles of periodical adsorption and non-thermal regeneration. Copyright © 2015. Published by Elsevier B.V.

  13. A novel method for the determination of adsorption partition coefficients of minor gases in a shale sample by headspace gas chromatography.

    Science.gov (United States)

    Zhang, Chun-Yun; Hu, Hui-Chao; Chai, Xin-Sheng; Pan, Lei; Xiao, Xian-Ming

    2013-10-04

    A novel method has been developed for the determination of adsorption partition coefficient (Kd) of minor gases in shale. The method uses samples of two different sizes (masses) of the same material, from which the partition coefficient of the gas can be determined from two independent headspace gas chromatographic (HS-GC) measurements. The equilibrium for the model gas (ethane) was achieved in 5h at 120°C. The method also involves establishing an equation based on the Kd at higher equilibrium temperature, from which the Kd at lower temperature can be calculated. Although the HS-GC method requires some time and effort, it is simpler and quicker than the isothermal adsorption method that is in widespread use today. As a result, the method is simple and practical and can be a valuable tool for shale gas-related research and applications. Copyright © 2013 Elsevier B.V. All rights reserved.

  14. On the role of the gas environment, electron-dose-rate, and sample on the image resolution in transmission electron microscopy

    DEFF Research Database (Denmark)

    Ek, Martin; Jespersen, Sebastian Pirel Fredsgaard; Damsgaard, Christian Danvad

    2016-01-01

    on the electron-dose-rate. In this article, we demonstrate that both the total and areal electron-dose-rates work as descriptors for the dose-rate-dependent resolution and are related through the illumination area. Furthermore, the resolution degradation was observed to occur gradually over time after......The introduction of gaseous atmospheres in transmission electron microscopy offers the possibility of studying materials in situ under chemically relevant environments. The presence of a gas environment can degrade the resolution. Surprisingly, this phenomenon has been shown to depend...... initializing the illumination of the sample and gas by the electron beam. The resolution was also observed to be sensitive to the electrical conductivity of the sample. These observations can be explained by a charge buildup over the electron-illuminated sample area, caused by the beam–gas–sample interaction...

  15. Preparation and Loading Process of Single Crystalline Samples into a Gas Environmental Cell Holder for In Situ Atomic Resolution Scanning Transmission Electron Microscopic Observation.

    Science.gov (United States)

    Straubinger, Rainer; Beyer, Andreas; Volz, Kerstin

    2016-06-01

    A reproducible way to transfer a single crystalline sample into a gas environmental cell holder for in situ transmission electron microscopic (TEM) analysis is shown in this study. As in situ holders have only single-tilt capability, it is necessary to prepare the sample precisely along a specific zone axis. This can be achieved by a very accurate focused ion beam lift-out preparation. We show a step-by-step procedure to prepare the sample and transfer it into the gas environmental cell. The sample material is a GaP/Ga(NAsP)/GaP multi-quantum well structure on Si. Scanning TEM observations prove that it is possible to achieve atomic resolution at very high temperatures in a nitrogen environment of 100,000 Pa.

  16. Molecular Characterization of the Gas-Particle Interface of Soot Sampled from a Diesel Engine Using a Titration Method.

    Science.gov (United States)

    Tapia, A; Salgado, M S; Martín, María Pilar; Lapuerta, M; Rodríguez-Fernández, J; Rossi, M J; Cabañas, B

    2016-03-15

    Surface functional groups of two different types of combustion aerosols, a conventional diesel (EN 590) and a hydrotreated vegetable oil (HVO) soot, have been investigated using heterogeneous chemistry (i.e., gas-particle surface reactions). A commercial sample of amorphous carbon (Printex XE2-B) was analyzed as a reference substrate. A Knudsen flow reactor was used to carry out the experiments under molecular flow conditions. The selected gases for the titration experiments were: N(CH3)3 for the identification of acidic sites, NH2OH for the presence of carbonyl groups, CF3COOH and HCl for basic sites of different strength, and O3 and NO2 for reducing groups. Reactivity with N(CH3)3 indicates a lower density of acidic functionalities for Printex XE2-B in relation to diesel and HVO soot. Results for NH2OH experiments indicates that commercial amorphous carbon exhibits a lower abundance of available carbonyl groups at the interface compared to the results from diesel and HVO soot, the latter being the one with the largest abundance of carbonyl functions. Reactions with acids indicate the presence of weak basic oxides on the particle surface that preferentially interact with the strong acid CF3COOH. Finally, reactions with O3 and NO2 reveal that diesel and especially HVO have a significantly higher reactivity with both oxidizers compared to that of Printex XE2-B because they have more reducing sites by roughly a factor of 10 and 30, respectively. The kinetics of titration reactions have also been investigated.

  17. The effect of sample grinding procedures after processing on gas production profiles and end-product formation in expander processed barley and peas

    NARCIS (Netherlands)

    Azarfar, A.; Poel, van der A.F.B.; Tamminga, S.

    2007-01-01

    Grinding is a technological process widely applied in the feed manufacturing industry and is a prerequisite for obtaining representative samples for laboratory procedures (e.g. gas production analysis). When feeds are subjected to technological processes other than grinding (e.g. expander

  18. Evaluation of a gas chromatograph with a novel surface acoustic wave detector (SAW GC) for screening of volatile organic compounds in Hanford waste tank samples

    International Nuclear Information System (INIS)

    Lockrem, L.L.

    1998-01-01

    A novel instrument, a gas chromatograph with a Surface Acoustic Wave Detector (SAW GC), was evaluated for the screening of organic compounds in Hanford tank headspace vapors. Calibration data were developed for the most common organic compounds, and the accuracy and precision were measured with a certified standard. The instrument was tested with headspace samples collected from seven Hanford waste tanks

  19. Selective removal of water in purge and cold-trap capillary gas chromatographic analysis of volatile organic traces in aqueous samples

    NARCIS (Netherlands)

    Noij, T.H.M.; van Es, A.J.J.; Cramers, C.A.M.G.; Rijks, J.A.; Dooper, R.P.M.

    1987-01-01

    The design and features of an on-line purge and cold-trap pre-concentration device for rapid analysis of volatile organic compounds in aqueous samples are discussed. Excessive water is removed from the purge gas by a condenser or a water permeable membrane in order to avoid blocking of the capillary

  20. Trace Analysis in End-Exhaled Air Using Direct Solvent Extraction in Gas Sampling Tubes: Tetrachloroethene in Workers as an Example

    Directory of Open Access Journals (Sweden)

    Chris-Elmo Ziener

    2014-01-01

    Full Text Available Simple and cost-effective analytical methods are required to overcome the barriers preventing the use of exhaled air in routine occupational biological monitoring. Against this background, a new method is proposed that simplifies the automation and calibration of the analytical measurements. End-exhaled air is sampled using valveless gas sampling tubes made of glass. Gaseous analytes are transferred to a liquid phase using a microscale solvent extraction performed directly inside the gas sampling tubes. The liquid extracts are analysed using a gas chromatograph equipped, as usual, with a liquid autosampler, and liquid standards are used for calibration. For demonstration purposes, the method’s concept was applied to the determination of tetrachloroethene in end-exhaled air, which is a biomarker for occupational tetrachloroethene exposure. The method’s performance was investigated in the concentration range 2 to 20 μg tetrachloroethene/L, which corresponds to today’s exposure levels. The calibration curve was linear, and the intra-assay repeatability and recovery rate were sufficient. Analysis of real samples from dry-cleaning workers occupationally exposed to tetrachloroethene and from nonexposed subjects demonstrated the method’s utility. In the case of tetrachloroethene, the method can be deployed quickly, requires no previous experiences in gas analysis, provides sufficient analytical reliability, and addresses typical end-exhaled air concentrations from exposed workers.

  1. Tank 241-BY-105 Headspace Gas and Vapor Characterization Results for Samples Collected in May 1994 and July 1994. Revision 2

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-09-01

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

  2. Comparative study of the characteristics of some suction devices for gas sampling applications; Etude comparative des caracteristiques de quelques dispositifs d'aspiration a l'usage des prelevements de gaz

    Energy Technology Data Exchange (ETDEWEB)

    Donguy, R.; Drouet, J.

    1959-06-15

    Gas sampling (used to determine the characteristics of dusts or aerosols contained in a gas) needs a suction device. In order to select the right device and the right conditions of use, the characteristics and performances of various suction devices (helicoidal and centrifugal aspirators, air pumps, volumetric pumps) have been experimentally measured: flow rate, head loss, sampling volume and duration, aerosol and dust concentration, gas density, nature of the gas, suction circuit configuration, etc.

  3. Aromatic hydrocarbons in produced water from offshore oil and gas production. Test of sample strategy; Aromatiske kulbrinter i produceret vand fra offshore olie- og gas industrien. Test af proevetagningsstrategi

    Energy Technology Data Exchange (ETDEWEB)

    Hansen, A.

    2005-07-01

    In co-operation with the Danish EPA, the National Environmental Research Institute (NERI) has carried out a series of measurements of aromatic hydrocarbons in produced water from an offshore oil and gas production platform in the Danish sector of the North Sea as part of the project 'Testing of sampling strategy for aromatic hydrocarbons in produced water from the offshore oil and gas industry'. The measurements included both volatile (BTEX: benzene, toluene, ethylbenzene and xylenes) and semi-volatile aromatic hydrocarbons: NPD (naphthalenes, phenanthrenes and dibenzothiophenes) and selected PAHs (polycyclic aromatic hydrocarbons). In total, 12 samples of produced water were sampled at the Dan FF production platform located in the North Sea by the operator, Maersk Oil and Gas, as four sets of three parallel samples from November 24 - December 02, 2004. After collection of the last set, the samples were shipped to NERI for analysis. The water samples were collected in 1 L glass bottles that were filled completely (without overfilling) and tightly closed. After sampling, the samples were preserved with hydrochloric acid and cooled below ambient until being shipped off to NERI. Here all samples were analysed in dublicates, and the results show that for BTEX, levels were reduced compared to similar measurements carried out by NERI in 2002 and others. In this work, BTEX levels were approximately 5 mg/L, while similar studies showed levels in the range 0,5 - 35 mg/L. For NPD levels were similar, 0,5 - 1,4 mg/L, while for PAH they seerred elevated; 0,1 - 0,4 mg/L in this work compared to 0,001 - 0,3 mg/L in similar studies. The applied sampling strategy has been tested by performing analysis of variance on the analytical data. The test of the analytical data has shown that the mean values of the three parallel samples collected in series constituted a good estimate of the levels at the time of sampling; thus, the variance between the parallel samples was not

  4. Dynamic terahertz spectroscopy of gas molecules mixed with unwanted aerosol under atmospheric pressure using fibre-based asynchronous-optical-sampling terahertz time-domain spectroscopy

    Science.gov (United States)

    Hsieh, Yi-Da; Nakamura, Shota; Abdelsalam, Dahi Ghareab; Minamikawa, Takeo; Mizutani, Yasuhiro; Yamamoto, Hirotsugu; Iwata, Tetsuo; Hindle, Francis; Yasui, Takeshi

    2016-06-01

    Terahertz (THz) spectroscopy is a promising method for analysing polar gas molecules mixed with unwanted aerosols due to its ability to obtain spectral fingerprints of rotational transition and immunity to aerosol scattering. In this article, dynamic THz spectroscopy of acetonitrile (CH3CN) gas was performed in the presence of smoke under the atmospheric pressure using a fibre-based, asynchronous-optical-sampling THz time-domain spectrometer. To match THz spectral signatures of gas molecules at atmospheric pressure, the spectral resolution was optimized to 1 GHz with a measurement rate of 1 Hz. The spectral overlapping of closely packed absorption lines significantly boosted the detection limit to 200 ppm when considering all the spectral contributions of the numerous absorption lines from 0.2 THz to 1 THz. Temporal changes of the CH3CN gas concentration were monitored under the smoky condition at the atmospheric pressure during volatilization of CH3CN droplets and the following diffusion of the volatilized CH3CN gas without the influence of scattering or absorption by the smoke. This system will be a powerful tool for real-time monitoring of target gases in practical applications of gas analysis in the atmospheric pressure, such as combustion processes or fire accident.

  5. A simple bubbling system for measuring radon (222Rn) gas concentrations in water samples based on the high solubility of radon in olive oil.

    Science.gov (United States)

    Al-Azmi, D; Snopek, B; Sayed, A M; Domanski, T

    2004-01-01

    Based on the different levels of solubility of radon gas in organic solvents and water, a bubbling system has been developed to transfer radon gas, dissolving naturally in water samples, to an organic solvent, i.e. olive oil, which is known to be a good solvent of radon gas. The system features the application of a fixed volume of bubbling air by introducing a fixed volume of water into a flask mounted above the system, to displace an identical volume of air from an air cylinder. Thus a gravitational flow of water is provided without the need for pumping. Then, the flushing air (radon-enriched air) is directed through a vial containing olive oil, to achieve deposition of the radon gas by another bubbling process. Following this, the vial (containing olive oil) is measured by direct use of gamma ray spectrometry, without the need of any chemical or physical processing of the samples. Using a standard solution of 226Ra/222Rn, a lowest measurable concentration (LMC) of radon in water samples of 9.4 Bq L(-1) has been achieved (below the maximum contaminant level of 11 Bq L(-1)).

  6. Thermal and Evolved Gas Analysis of Calcite Under Reduced Operating Pressures: Implications for the 2011 MSL Sample Analysis at Mars (SAM) Instrument

    Science.gov (United States)

    Lauer, H. V. Jr.; Ming, D. W.; Sutter, B.; Mahaffy, P. R.

    2010-01-01

    The Mars Science Laboratory (MSL) is scheduled for launch in 2011. The science objectives for MSL are to assess the past or present biological potential, to characterize the geology, and to investigate other planetary processes that influence habitability at the landing site. The Sample Analysis at Mars (SAM) is a key instrument on the MSL payload that will explore the potential habitability at the landing site [1]. In addition to searching for organic compounds, SAM will have the capability to characterized evolved gases as a function of increasing temperature and provide information on the mineralogy of volatile-bearing phases such as carbonates, sulfates, phyllosilicates, and Fe-oxyhydroxides. The operating conditions in SAM ovens will be maintained at 30 mb pressure with a He carrier gas flowing at 1 sccm. We have previously characterized the thermal and evolved gas behaviors of volatile-bearing species under reduced pressure conditions that simulated operating conditions of the Thermal and Evolved Gas Analyzer (TEGA) that was onboard the 2007 Mars Phoenix Scout Mission [e.g., 2-8]. TEGA ovens operated at 12 mb pressure with a N2 carrier gas flowing at 0.04 sccm. Another key difference between SAM and TEGA is that TEGA was able to perform differential scanning calorimetry whereas SAM only has a pyrolysis oven. The operating conditions for TEGA and SAM have several key parameter differences including operating pressure (12 vs 30 mb), carrier gas (N2 vs. He), and carrier gas flow rate (0.04 vs 1 sccm). The objectives of this study are to characterize the thermal and evolved gas analysis of calcite under SAM operating conditions and then compare it to calcite thermal and evolved gas analysis under TEGA operating conditions.

  7. Compositional simulations of producing oil-gas ratio behaviour in low permeable gas condensate reservoir

    OpenAIRE

    Gundersen, Pål Lee

    2013-01-01

    Master's thesis in Petroleum engineering Gas condensate flow behaviour below the dew point in low permeable formations can make accurate fluid sampling a difficult challenge. The objective of this study was to investigate the producing oil-gas ratio behaviour in the infinite-acting period for a low permeable gas condensate reservoir. Compositional isothermal flow simulations were performed using a single-layer, radial and two-dimensional, gas condensate reservoir model with low permeabili...

  8. Evolved Gas Analysis of Mars Analog Samples from the Arctic Mars Analog Svalbard Expedition: Implications for Analyses by the Mars Science Laboratory

    Science.gov (United States)

    McAdam, A.; Stern, J. C.; Mahaffy, P. R.; Blake, D. F.; Bristow, T.; Steele, A.; Amundsen, H. E. F.

    2012-01-01

    The 2011 Arctic Mars Analog Svalbard Expedition (AMASE) investigated several geologic settings on Svalbard, using methodologies and techniques being developed or considered for future Mars missions, such as the Mars Science Laboratory (MSL). The Sample Analysis at Mars (SAM) instrument suite on MSL consists of a quadrupole mass spectrometer (QMS), a gas chromatograph (GC), and a tunable laser spectrometer (TLS), which analyze gases created by pyrolysis of samples. During AMASE, a Hiden Evolved Gas Analysis-Mass Spectrometer (EGA-MS) system represented the EGA-QMS capability of SAM. Another MSL instrument, CheMin, will use x-ray diffraction (XRD) and x-ray fluorescence (XRF) to perform quantitative mineralogical characterization of samples. Field-portable versions of CheMin were used during AMASE. AMASE 2011 sites spanned a range of environments relevant to understanding martian surface materials, processes and habitability. They included the basaltic Sverrefjell volcano, which hosts carbonate globules, cements and coatings, carbonate and sulfate units at Colletth0gda, Devonian sandstone redbeds in Bockfjorden, altered basaltic lava delta deposits at Mt. Scott Keltie, and altered dolerites and volcanics at Botniahalvoya. Here we focus on SAM-like EGA-MS of a subset of the samples, with mineralogy comparisons to CheMin team results. The results allow insight into sample organic content as well as some constraints on sample mineralogy.

  9. Phase Velocity Estimation of a Microstrip Line in a Stoichiometric Periodically Domain-Inverted LiTaO3 Modulator Using Electro-Optic Sampling Technique

    Directory of Open Access Journals (Sweden)

    Shintaro Hisatake

    2008-01-01

    Full Text Available We estimate the phase velocity of a modulation microwave in a quasi-velocity-matched (QVM electro-optic (EO phase modulator (QVM-EOM using EO sampling which is accurate and the most reliable technique for measuring voltage waveforms at an electrode. The substrate of the measured QVM-EOM is a stoichiometric periodically domain-inverted LiTaO3 crystal. The electric field of a standing wave in a resonant microstrip line (width: 0.5 mm, height: 0.5 mm is measured by employing a CdTe crystal as an EO sensor. The wavelength of the traveling microwave at 16.0801 GHz is determined as 3.33 mm by fitting the theoretical curve to the measured electric field distribution. The phase velocity is estimated as vm=5.35×107 m/s, though there exists about 5% systematic error due to the perturbation by the EO sensor. Relative dielectric constant of εr=41.5 is led as the maximum likelihood value that derives the estimated phase velocity.

  10. Regular drinking may strengthen the beneficial influence of social support on depression: findings from a representative Israeli sample during a period of war and terrorism.

    Science.gov (United States)

    Kane, Jeremy C; Rapaport, Carmit; Zalta, Alyson K; Canetti, Daphna; Hobfoll, Stevan E; Hall, Brian J

    2014-07-01

    Social support is consistently associated with reduced risk of depression. Few studies have investigated how this relationship may be modified by alcohol use, the effects of which may be particularly relevant in traumatized populations in which rates of alcohol use are known to be high. In 2008 a representative sample of 1622 Jewish and Palestinian citizens in Israel were interviewed by phone at two time points during a period of ongoing terrorism and war threat. Two multivariable mixed effects regression models were estimated to measure the longitudinal association of social support from family and friends on depression symptoms. Three-way interaction terms between social support, alcohol use and time were entered into the models to test for effect modification. Findings indicated that increased family social support was associated with less depression symptomatology (p=Social support from friends was also associated with fewer depression symptoms (p=effect of social support was stronger for those who drank alcohol regularly than those who did not drink or drank rarely. These findings suggest that social support is a more important protective factor for depression among regular drinkers than among those who do not drink or drink rarely in the context of political violence. Additional research is warranted to determine whether these findings are stable in other populations and settings. Copyright © 2014 Elsevier Ireland Ltd. All rights reserved.

  11. Use of a holder-vacuum tube device to save on-site hands in preparing urine samples for head-space gas-chromatography, and its application to determine the time allowance for sample sealing.

    Science.gov (United States)

    Kawai, Toshio; Sumino, Kimiaki; Ohashi, Fumiko; Ikeda, Masayuki

    2011-01-01

    To facilitate urine sample preparation prior to head-space gas-chromatographic (HS-GC) analysis. Urine samples containing one of the five solvents (acetone, methanol, methyl ethyl ketone, methyl isobutyl ketone and toluene) at the levels of biological exposure limits were aspirated into a vacuum tube via holder, a device commercially available for venous blood collection (the vacuum tube method). The urine sample, 5 ml, was quantitatively transferred to a 20-ml head-space vial prior to HS-GC analysis. The loaded tubes were stored at +4 ℃ in dark for up to 3 d. The vacuum tube method facilitated on-site procedures of urine sample preparation for HS-GC with no significant loss of solvents in the sample and no need of skilled hands, whereas on-site sample preparation time was significantly reduced. Furthermore, no loss of solvents was detected during the 3-d storage, irrespective of hydrophilic (acetone) or lipophilic solvent (toluene). In a pilot application, high performance of the vacuum tube method in sealing a sample in an air-tight space succeeded to confirm that no solvent will be lost when sealing is completed within 5 min after urine voiding, and that the allowance time is as long as 30 min in case of toluene in urine. The use of the holder-vacuum tube device not only saves hands for transfer of the sample to air-tight space, but facilitates sample storage prior to HS-GC analysis.

  12. Characterization of lipids in complex samples using comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry

    NARCIS (Netherlands)

    Jover, E.; Adahchour, M.; Bayona, J.M.; Vreuls, R.J.J.; Brinkman, U.A.T.

    2005-01-01

    Most lipids are a complex mixture of classes of compounds such as fatty acids, fatty alcohols, diols, sterols and hydroxy acids. In this study, the suitability of comprehensive two-dimensional gas chromatography coupled to a time-of-light mass spectrometer is studied for lipid characterization in

  13. 40 CFR 86.1309-90 - Exhaust gas sampling system; Otto-cycle and non-petroleum-fueled engines.

    Science.gov (United States)

    2010-07-01

    ... exhaust duct excludes the length of pipe representative of the vehicle exhaust pipe) shall be minimized... exhaust manifold, immediately after exhaust aftertreatment systems, or after a length of pipe representative of the vehicle exhaust pipe; or (iv) Partial dilution of the exhaust gas prior to entering the...

  14. On-line combination of liquid chromatography and capillary gas chromatography : preconcentration and analysis of organic compounds in aqueous samples

    NARCIS (Netherlands)

    Noij, T.H.M.; Weiss, E.; Herps, T.; Cruchten, van H.; Rijks, J.A.

    1988-01-01

    This paper describes the design of a new, versatile, and low-cost on-line LC-GC interface that allows the fast and reliable introduction of large sample volumes onto a capillary GC column. The sample introduction procedure consists successively of: evaporation of the entire sample (LC fraction),

  15. Short communication: measurements of methane emissions from feed samples in filter bags or dispersed in the medium in an in vitro gas production system.

    Science.gov (United States)

    Ramin, M; Krizsan, S J; Jančík, F; Huhtanen, P

    2013-07-01

    The objective of this study was to compare methane (CH4) emissions from different feeds when incubated within filter bags for in vitro analysis or directly dispersed in the medium in an automated gas in vitro system. Four different concentrates and 4 forages were used in this study. Two lactating Swedish Red cows were used for the collection of rumen fluid. Feed samples were milled to pass a 1.0-mm screen. Aliquots (0.5 g) of samples were weighed directly in the bottles or within the F 0285 filter bags that were placed in the bottles. Gas samples were taken during 24 and 48 h of incubation, and CH4 concentration was determined. The data were analyzed using a general linear model. Feeds differed significantly in CH4 emission both at 24 and at 48 h of incubation. The interaction between feed and method on methane emission in vitro was significant, indicating that the ranking of feeds was not consistent between the methods. Generally, greater amounts of CH4 were emitted from samples directly dispersed in the medium compared with those incubated within the filter bags, which could be a result of lower microbial activity within the filter bags. The ratio of CH4 to total gas was greater when the feeds were incubated within bags compared with samples directly dispersed in the medium. Incubating samples in filter bags during 48 h of incubation cannot be recommended for determination of CH4 emission of feeds in vitro. Copyright © 2013 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

  16. Theoretical innovation and technical progress will usher in a production period of gas fields with an annual capacity of ten billion cubic meters

    Directory of Open Access Journals (Sweden)

    Zhenwei Gan

    2017-01-01

    Full Text Available Challenged by the increasing complexity of targets and the tense situation of turning losses into profits during the 12th Five-Year Plan, by virtue of technological innovation, Sinopec Southwest Oil & Gas Company proposed the theories of gas exploration in continental clastic rock and marine carbonate rock, and developed the development technologies for reef, channel sandstone and tight sandstone reservoirs. Moreover, it innovatively formed a series of engineering technologies, including intelligent sliding sleeve staged fracturing, blasting–packing–fracturing stimulation, impulse fracturing, and drilling, completion and production technologies for ultra-deep horizontal wells with high sulfur contents. With these innovated theories and improved technologies, great discoveries have been made in the continental clastic rocks and marine carbonate rocks in West Sichuan Basin, the marine shale in South Sichuan Basin, and the marine carbonate rocks in Yuanba area of NE Sichuan Basin, and three 100 billion-m3 class commercial gas reserves zones were discovered. Moreover, two medium- and large-sized gas fields were proved, and three medium- and large-sized gas fields were completely constructed. Both reserves and production reached a new record in history. During the 13th Five-Year Plan, Sinopec Southwest Oil & Gas Company will focus on the exploration and development of deep marine carbonate reservoirs, commercial development of deep shale gas, safe development of gas fields with high sulfur, and enhancement of recovery in mature gas fields. By the end of the 13th Five-Year Plan, it is expected that the annual gas production of (10–12 × 109 m3 will be achieved.

  17. Gas-phase sample introduction techniques for the determination of some non-metals by ICP-AES, MIP-AES AND ICP-MS

    International Nuclear Information System (INIS)

    Nakahara, Taketoshi

    2003-01-01

    Various gas-phase sample introduction methods in analytical atomic spectrometry have been documented for up to 30 elements, but only a few of these methods with less than one-third of the analytes exhibit adequate, competitive performance characteristics. Most attractive are the chemical systems based on (i) reactions in aqueous media, (ii) with fast kinetics of chemical vapor generation and easy stripping off of vapors from solution, (iii) reliable interference control, (iv) with high and reducible chemical yields of volatile products which are (v) readily atomized, excited or ionized in a plasma, so as to provide adequate sensitivity and low limits of detection (LOD). Some significant advantage of gas-phase sample introduction over the widely-used pneumatic nebulization of liquid (solution) samples are (1) high chemical yields and transport efficiency, (2) separation from troublesome matrices, (3) enrichment, (4) automation in flow injection and continuous flow mode, (5) good sample throughput rates, (6) competitive LODs and RSDs, (7) commercially available accessories, (8) economically affordable and (9) speciation potentialities. To the contrary, the major disadvantages and limitations are (1) complex, on line-chemistry involved, (2) specific sample pre-treatment required, (3) effect of oxidation and binding state of analyte, (4) chemical interferences, (5) foaming and aerosol formation, (6) numerous instrumental and chemical parameters for optimization, (7) applicability to a limited number of analytes, (8) limited linear ranges and (9) poor-multi-element capabilities.

  18. AN APPLICATION OF FLOW INJECTION ANALYSIS WITH GAS DIFFUSION AND SPECTROPHOTOMETRIC DETECTION FOR THE MONITORING OF DISSOLVED SULPHIDE CONCENTRATION IN ENVIRONMENTAL SAMPLES

    Directory of Open Access Journals (Sweden)

    Malwina Cykowska

    2014-10-01

    Full Text Available The monitoring of the concentration of sulphide is very important from the environment point of view because of high toxicity of hydrogen sulphide. What is more hydrogen sulphide is an important pollution indicator. In many cases the determination of sulphide is very difficult due to complicated matrix of some environmental samples, which causes that most analytical methods cannot be used. Flow injection analysis allows to avoid matrix problem what makes it suitable for a wide range of applications in analytical laboratories. In this paper determination of dissolved sulphide in environmental samples by gas-diffusion flow injection analysis with spectrophotometric detection was presented. Used gas-diffusion separation ensures the elimination of interferences caused by sample matrix and gives the ability of determination of sulphides in coloured and turbid samples. Studies to optimize the measurement conditions and to determine the value of the validation parameters (e.g. limit of detection, limit of quantification, precision, accuracy were carried out. Obtained results confirm the usefulness of the method for monitoring the concentration of dissolved sulphides in water and waste water. Full automation and work in a closed system greatly reduces time of analysis, minimizes consumption of sample and reagents and increases safety of analyst’s work.

  19. A headspace solid-phase microextraction procedure coupled with gas chromatography-mass spectrometry for the analysis of volatile polycyclic aromatic hydrocarbons in milk samples

    Energy Technology Data Exchange (ETDEWEB)

    Aguinaga, N.; Campillo, N.; Vinas, P.; Hernandez-Cordoba, M. [University of Murcia, Department of Analytical Chemistry, Faculty of Chemistry, Murcia (Spain)

    2008-06-15

    A sensitive and solvent-free method for the determination of ten polycyclic aromatic hydrocarbons, namely, naphthalene, acenaphthylene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benzo[a]anthracene and chrysene, with up to four aromatic rings, in milk samples using headspace solid-phase microextraction and gas chromatography-mass spectrometry detection has been developed. A polydimethylsiloxane-divinylbenzene fiber was chosen and used at 75 C for 60 min. Detection limits ranging from 0.2 to 5 ng L{sup -1} were attained at a signal-to-noise ratio of 3, depending on the compound and the milk sample under analysis. The proposed method was applied to ten different milk samples and the presence of six of the analytes studied in a skimmed milk with vegetal fiber sample was confirmed. The reliability of the procedure was verified by analyzing two different certified reference materials and by recovery studies. (orig.)

  20. FTIR analysis of flue gases - combined in-situ and dry extractive gas sampling; Kombination av in-situ och kallextraktiv roekgasmaetning med FTIR

    Energy Technology Data Exchange (ETDEWEB)

    Andersson, Christer; Soederbom, J [Vattenfall Utveckling AB, Aelvkarleby (Sweden)

    1996-10-01

    Fourier Transform Infra Red (FTIR) spectroscopy is a promising and versatile technique for gas analysis which lately has moved from the laboratory to industrial applications such as emission monitoring of combustion plants. This has been made possible by recent developments of spectrometers and software. The single most important advantage of the FTIR is its capability to simultaneously analyse virtually all gas species of interest in flue gas applications. The project has studied the feasibility of using the technique as a multi-component emission monitoring system. A specific aim was to evaluate different implementations of the technique to flue gas analysis: in-situ, hot/dry and cold extraction or combinations of these. The goal was to demonstrate a system in which gas components that normally require hot extraction (NH{sub 3}, HCl, H{sub 2}O) could instead be measured in-situ. In this way potential sampling artefacts e.g. for ammonia monitoring, can be avoided. The remaining gas components are measured using cold extraction and thereby minimizing interference from water. The latter advantage can be crucial for the accuracy of e.g. NO{sub x} measurements. Prior to the project start in-situ monitoring using FTIR was, a to a large extent, an untried method. The fact that broad band IR radiation can not be guided through optical fibres, presented a major technical obstacle. An `in-situ probe` was developed to serve the purpose. The probe is equipped with a gold plated mirror at the end and is mounted on the support structure of the FTIR-spectrometer. The arrangement proved to be a robust solution without being unnecessary complex or cumbersome to use. 10 refs, 45 figs, 10 tabs

  1. Regular drinking may strengthen the beneficial influence of social support on depression: Findings from a representative Israeli sample during a period of war and terrorism

    Science.gov (United States)

    Kane, Jeremy C.; Rapaport, Carmit; Zalta, Alyson K.; Canetti, Daphna; Hobfoll, Stevan E.; Hall, Brian J.

    2016-01-01

    Background Social support is consistently associated with reduced risk of depression. Few studies have investigated how this relationship may be modified by alcohol use, the effects of which may be particularly relevant in traumatized populations in which rates of alcohol use are known to be high. Methods In 2008 a representative sample of 1622 Jewish and Palestinian citizens in Israel were interviewed by phone at two time points during a period of ongoing terrorism and war threat. Two multivariable mixed effects regression models were estimated to measure the longitudinal association of social support from family and friends on depression symptoms. Three-way interaction terms between social support, alcohol use and time were entered into the models to test for effect modification. Results Findings indicated that increased family social support was associated with less depression symptomatology (p=<.01); this relationship was modified by alcohol use and time (p=<.01). Social support from friends was also associated with fewer depression symptoms (p=<.01) and this relationship was modified by alcohol use and time as well (p=<.01). Stratified analyses in both models revealed that the effect of social support was stronger for those who drank alcohol regularly than those who did not drink or drank rarely. Conclusions These findings suggest that social support is a more important protective factor for depression among regular drinkers than among those who do not drink or drink rarely in the context of political violence. Additional research is warranted to determine whether these findings are stable in other populations and settings. PMID:24838033

  2. Microstructural evolution and mechanical properties of differently heat-treated binder jet printed samples from gas- and water-atomized alloy 625 powders

    International Nuclear Information System (INIS)

    Mostafaei, Amir; Toman, Jakub; Stevens, Erica L.; Hughes, Eamonn T.; Krimer, Yuval L.; Chmielus, Markus

    2017-01-01

    In this study, we investigate the effect of powders resulting from different atomization methods on properties of binder jet printed and heat-treated samples. Air-melted gas atomized (GA) and water atomized (WA) nickel-based alloy 625 powders were used to binder jet print samples for a detailed comparative study on microstructural evolution and mechanical properties. GA printed samples achieved higher sintering density (99.2%) than WA samples (95.0%) due to differences in powder morphology and chemistry. Grain sizes of GA and WA samples at their highest density were 89 ± 21 μm and 88 ± 26 μm, respectively. Mechanical tests were conducted on optimally sintered samples and sintered plus aged samples; aging further improved microstructure and mechanical properties. This study shows that microstructural evolution (densification, and carbide, oxide and intermetallic phase formation) is very different for GA and WA binder jet printed and heat-treated samples. This difference in microstructural evolution results in different mechanical properties with the superior sintered and aged GA specimen reaching a hardness of 327 ± 7 HV_0_._1, yield strength of 394 ± 15 MPa, and ultimate tensile strength of 718 ± 14 MPa which are higher than cast alloy 625 values.

  3. Electrochemical Noise Sensors for Detection of Localized and General Corrosion of Natural Gas Transmission Pipelines. Final Report for the Period July 2001-October 2002

    Energy Technology Data Exchange (ETDEWEB)

    Bullard, Sophie J.; Covino, Jr., Bernard S.; Russell, James H.; Holcomb, Gordon R.; Cramer, Stephen D.; Ziomek-Moroz, Margaret

    2002-12-01

    The U.S. Department of Energy, National Energy Technology Laboratory funded a Natural Gas Infrastructure Reliability program directed at increasing and enhancing research and development activities in topics such as remote leak detection, pipe inspection, and repair technologies and materials. The Albany Research Center (ARC), U.S. Department of Energy was funded to study the use of electrochemical noise sensors for detection of localized and general corrosion of natural gas transmission pipelines. As part of this, ARC entered into a collaborative effort with the corrosion sensor industry to demonstrate the capabilities of commercially available remote corrosion sensors for use with the Nation's Gas Transmission Pipeline Infrastructure needs. The goal of the research was to develop an emerging corrosion sensor technology into a monitor for the type and degree of corrosion occurring at key locations in gas transmission pipelines.

  4. Application of gas geochemistry in the search for different types of uranium deposits. Final report for the period 15 November 1991 - 15 March 1994

    International Nuclear Information System (INIS)

    Chen Guoliang

    1994-10-01

    This paper presents the study of primary and secondary gas halo and application in the search for different types of uranium deposits in China. Through measuring Rn, CO 2 , O 2 and Hg in various deposits of geographical and climatic conditions for the gas geochemical survey. Three comprehensive measuring methods of CO 2 , Rn and 0 2 were thought to be optimum for gas geochemical exploration because of its portability, rapidity, low cost, simple operation and limited interference. Our experimental data can be briefly summarized that higher concentration of CO 2 , Rn and lower concentration of secondary halo in soil show blinded deposits. Our project have finished the study of thermal emanating gas in soil and rock. The methods were confirmed by known deposits and can be used in uranium exploration or environment investigation. 4 refs, 23 figs, 26 tabs

  5. Membrane Assisted Simultaneous Extraction and Derivatization with Triphenylphosphine of Elemental Sulfur in Arabian Crude Samples by Gas Chromatography/Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Ibrahim Al-Zahrani

    2015-01-01

    Full Text Available Determination of trace level elemental sulfur from crude oil samples is a tedious task. Recently, several gas chromatographic methods were reported in which selective triphenylphosphine derivatization of sulfur was used to form triphenylphosphine sulfide. Direct quantitation of elemental sulfur from crude oil requires an efficient sample preparation method. This paper describes how simultaneous extraction derivatization of elemental sulfur was performed for the first time using porous hollow fiber membrane. A thick (0.25 um pore size; 1550 μm wall thickness; and 5500 μm inner diameter hollow fiber membrane filled with triphenylphosphine (dissolved N-methylpyrrolidone is used as a solvent bar. The solvent bar is tumbled freely in the crude oil sample; the elemental sulfur was extracted and derivatized. Finally, the derivatized sulfur was analyzed by gas chromatography/mass spectrometry. Various experimental conditions of solvent bar microextraction (SBME were optimized to achieve higher extraction. The linear range was established between 1 and 50 μg/mL, while a squared regression coefficient was found to be 0.9959 μg/mL. Relative standard deviation (RSD was below 10%. Relative recoveries were calculated for SBME in crude oil samples and were in the range between 98.2% and 101.2%.

  6. Method for sampling and analysis of volatile biomarkers in process gas from aerobic digestion of poultry carcasses using time-weighted average SPME and GC-MS.

    Science.gov (United States)

    Koziel, Jacek A; Nguyen, Lam T; Glanville, Thomas D; Ahn, Heekwon; Frana, Timothy S; Hans van Leeuwen, J

    2017-10-01

    A passive sampling method, using retracted solid-phase microextraction (SPME) - gas chromatography-mass spectrometry and time-weighted averaging, was developed and validated for tracking marker volatile organic compounds (VOCs) emitted during aerobic digestion of biohazardous animal tissue. The retracted SPME configuration protects the fragile fiber from buffeting by the process gas stream, and it requires less equipment and is potentially more biosecure than conventional active sampling methods. VOC concentrations predicted via a model based on Fick's first law of diffusion were within 6.6-12.3% of experimentally controlled values after accounting for VOC adsorption to the SPME fiber housing. Method detection limits for five marker VOCs ranged from 0.70 to 8.44ppbv and were statistically equivalent (p>0.05) to those for active sorbent-tube-based sampling. The sampling time of 30min and fiber retraction of 5mm were found to be optimal for the tissue digestion process. Copyright © 2017 Elsevier Ltd. All rights reserved.

  7. The effect of sequential dual-gas testing on laser-induced breakdown spectroscopy-based discrimination: Application to brass samples and bacterial strains

    International Nuclear Information System (INIS)

    Rehse, Steven J.; Mohaidat, Qassem I.

    2009-01-01

    Four Cu-Zn brass alloys with different stoichiometries and compositions have been analyzed by laser-induced breakdown spectroscopy (LIBS) using nanosecond laser pulses. The intensities of 15 emission lines of copper, zinc, lead, carbon, and aluminum (as well as the environmental contaminants sodium and calcium) were normalized and analyzed with a discriminant function analysis (DFA) to rapidly categorize the samples by alloy. The alloys were tested sequentially in two different noble gases (argon and helium) to enhance discrimination between them. When emission intensities from samples tested sequentially in both gases were combined to form a single 30-spectral line 'fingerprint' of the alloy, an overall 100% correct identification was achieved. This was a modest improvement over using emission intensities acquired in argon gas alone. A similar study was performed to demonstrate an enhanced discrimination between two strains of Escherichia coli (a Gram-negative bacterium) and a Gram-positive bacterium. When emission intensities from bacteria sequentially ablated in two different gas environments were combined, the DFA achieved a 100% categorization accuracy. This result showed the benefit of sequentially testing highly similar samples in two different ambient gases to enhance discrimination between the samples.

  8. Multiwalled carbon nanotubes coated fibers for solid-phase microextraction of polybrominated diphenyl ethers in water and milk samples before gas chromatography with electron-capture detection.

    Science.gov (United States)

    Wang, Jun-Xia; Jiang, Dong-Qing; Gu, Zhi-Yuan; Yan, Xiu-Ping

    2006-12-22

    Determination of polybrominated diphenyl ethers (PBDEs) in environmental samples has raised great concerns due to the widespread use of PBDEs and their potential risk to humans. Solid-phase microextraction (SPME) is a fast, simple, cost-effective, and green sample preparation technique and is widely used for environmental analysis, but reports on the application of SPME for determination of PBDEs are very limited, and only a few publications dealing with commercial SPME fibers are available for extraction of PBDEs. Herein, we report a novel SPME method using multiwalled carbon nanotubes (MWCNTs) as the SPME fiber coating for gas chromatography with electron-capture detection (GC-ECD) of PBDEs in environmental samples. The MWCNTs coating gave much higher enhancement factors (616-1756) than poly (5% dibenzene-95% dimethylsiloxane) coating (139-384) and activated carbon coating (193-423). Thirty-minute extraction of 10 mL of sample solution using the MWCNTs coated fiber for GC-ECD determination yielded the limits of detection of 3.6-8.6 ng L(-1) and exhibited good linearity of the calibration functions (r(2)>0.995). The precision (RSD%, n=4) for peak area and retention time at the 500 ng L(-1) level was 6.9-8.8% and 0.6-0.9%, respectively. The developed method was successfully applied for the analysis of real samples including local river water, wastewater, and milk samples. The recovery of the PBDEs at 500 ng L(-1) spiked in these samples ranged from 90 to 119%. No PBDEs were detected in the river water and skimmed milk samples, whereas in the wastewater sample, 134-215 ng L(-1) of PBDEs were found. The PBDEs were detected in all whole fat milk samples, ranging from 13 to 484 ng L(-1). In a semiskimmed milk sample, only BDE-47 was found at 21 ng L(-1).

  9. The ionisation loss of relativistic charged particles in thin gas samples and its use for particle identification. I

    International Nuclear Information System (INIS)

    Cobb, J.H.; Allison, W.W.M.; Bunch, J.N.

    1976-01-01

    A brief review shows a significant discrepancy between available data and theoretical predictions on the ionisation loss of charged particles in thin gas-filled proportional counters. The discrepancy related both to the increase of the most probable loss at relativistic velocities (relativistic rise) and to the spectrum of such losses at a given velocity (the Landau distribution). The origin of this relativistic rise is discussed in simple terms and related to the phenomena of transition radiation and Cherenkov radiation. It is shown that the failure of the prediction is due to the small number of ionising collisions in a gas. This problem is overcome by using a Monte Carlo method rather than a continuous integral over the spectrum of single collision processes. A specific mode of the atomic form factors is used with a modified Born approximation to yield the differential cross sections needed for the calculation. The new predictions give improved agreement with experiment and are used to investigate the problem of identifying particles of known momenta in the relativistic region. It is shown that by measuring the ionisation loss of each particle several hundred times over 5m or more, kaon, pion and proton separation with good confidence level may be achieved. Many gases are considered and a comparison is made. The results are also compared with the velocity resolution achievable by measuring primary ionisation. (Auth.)

  10. Analysis of Mars Analogue Soil Samples Using Solid-Phase Microextraction, Organic Solvent Extraction and Gas Chromatography/Mass Spectrometry

    Science.gov (United States)

    Orzechowska, G. E.; Kidd, R. D.; Foing, B. H.; Kanik, I.; Stoker, C.; Ehrenfreund, P.

    2011-01-01

    Polycyclic aromatic hydrocarbons (PAHs) are robust and abundant molecules in extraterrestrial environments. They are found ubiquitously in the interstellar medium and have been identified in extracts of meteorites collected on Earth. PAHs are important target molecules for planetary exploration missions that investigate the organic inventory of planets, moons and small bodies. This study is part of an interdisciplinary preparation phase to search for organic molecules and life on Mars. We have investigated PAH compounds in desert soils to determine their composition, distribution and stability. Soil samples (Mars analogue soils) were collected at desert areas of Utah in the vicinity of the Mars Desert Research Station (MDRS), in the Arequipa region in Peru and from the Jutland region of Denmark. The aim of this study was to optimize the solid-phase microextraction (SPME) method for fast screening and determination of PAHs in soil samples. This method minimizes sample handling and preserves the chemical integrity of the sample. Complementary liquid extraction was used to obtain information on five- and six-ring PAH compounds. The measured concentrations of PAHs are, in general, very low, ranging from 1 to 60 ng g(sup -1). The texture of soils is mostly sandy loam with few samples being 100% silt. Collected soils are moderately basic with pH values of 8-9 except for the Salten Skov soil, which is slightly acidic. Although the diverse and variable microbial populations of the samples at the sample sites might have affected the levels and variety of PAHs detected, SPME appears to be a rapid, viable field sampling technique with implications for use on planetary missions.

  11. Determination of benzothiazole and alkylphosphates in water samples from the Great Lakes Drainage Basin by gas chromatography/atomic emission detection

    Energy Technology Data Exchange (ETDEWEB)

    Scott, B.F. [Environment Canada, Burlington, ON (Canada). Wastewater Technology Centre; Sverko, E.; Maguire, R.J. [Environment Canada, Burlington, ON (Canada). Wastewater Technology Centre

    1996-06-01

    Centrifuged water extracts from large receiving water bodies were analyzed for heteroatom-containing compounds. Extracts from aqueous environmental samples were analyzed by gas chromatography/atomic emission detection for P-, S-, and N- containing compounds. The samples exhibited complex chromatographic traces. Benzothiazole, tri-n-butylphosphate, tris(2-chloroethyl)phosphate, tris({beta}-chloroisopropyl)phosphate and two isomers of this last chemical were detected in all archived water extracts collected from permanent sampling stations at Fort Erie, Niagara-on-the-Lake and Wolfe Island. The concentrations of the trialkylphosphates reported in this study were at least four orders of magnitude lower than concentrations of some other trialkylphosphates and triarylphosphates that cause acute toxicity to rainbow trout, water fleas, midge larvae and shrimp. Further work on trialkylphosphates is under way to assess their environmental distribution, their levels in industrial and municipal effluents and their acute and chronic toxicity to aquatic organisms. 32 refs., 3 tabs., 5 figs.

  12. Tank 241-U-104 headspace gas and vapor characterization results from samples collected on July 16, 1996

    International Nuclear Information System (INIS)

    Pool, K.H.; Evans, J.C.; Hayes, J.C.; Mitroshkov, A.V.; Edwards, J.A.; Julya, J.L.; Thornton, B.M.; Fruchter, J.S.; Silvers, K.L.

    1997-08-01

    This report presents the results from analyses of samples taken from the headspace of waste storage tank 241-U-104 (Tank U-104) at the Hanford Site in Washington State. Tank headspace samples collected by Westinghouse Hanford Company (WHC) were analyzed by Pacific Northwest National Laboratory (PNNL) to determine headspace concentrations of selected non-radioactive analytes. Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. Vapor concentrations from sorbent trap samples are based on measured sample volumes provided by WHC. No analytes were determined to be above the immediate notification limits specified by the sampling and analysis plan. None of the flammable constituents were present at concentrations above the analytical instrument detection limits. Total headspace flammability was estimated to be <0.108% of the lower flammability limit. Average measured concentrations of targeted gases, inorganic vapors, and selected organic vapors are provided in a table. A summary of experimental methods, including sampling methodology, analytical procedures, and quality assurance and control methods are presented in Section 2.0. Detailed descriptions of the analytical results are provided in Section 3.0

  13. Packed-Bed Reactor Study of NETL Sample 196c for the Removal of Carbon Dioxide from Simulated Flue Gas Mixture

    Energy Technology Data Exchange (ETDEWEB)

    Hoffman, James S.; Hammache, Sonia; Gray, McMahan L.; Fauth Daniel J.; Pennline, Henry W.

    2012-04-24

    An amine-based solid sorbent process to remove CO2 from flue gas has been investigated. The sorbent consists of polyethylenimine (PEI) immobilized onto silica (SiO2) support. Experiments were conducted in a packed-bed reactor and exit gas composition was monitored using mass spectrometry. The effects of feed gas composition (CO2 and H2O), temperature, and simulated steam regeneration were examined for both the silica support as well as the PEI-based sorbent. The artifact of the empty reactor was also quantified. Sorbent CO2 capacity loading was compared to thermogravimetric (TGA) results to further characterize adsorption isotherms and better define CO2 working capacity. Sorbent stability was monitored by periodically repeating baseline conditions throughout the parametric testing and replacing with fresh sorbent as needed. The concept of the Basic Immobilized Amine Sorbent (BIAS) Process using this sorbent within a system where sorbent continuously flows between the absorber and regenerator was introduced. The basic tenet is to manipulate or control the level of moisture on the sorbent as it travels around the sorbent circulation path between absorption and regeneration stages to minimize its effect on regeneration heat duty.

  14. Development of a sample preparation method for the analysis of current-use pesticides in sediment using gas chromatography.

    Science.gov (United States)

    Wang, Dongli; Weston, Donald P; Ding, Yuping; Lydy, Michael J

    2010-02-01

    Pyrethroid insecticides have been implicated as the cause of sediment toxicity to Hyalella azteca in both agricultural and urban areas of California; however, for a subset of these toxic sediments (approximately 30%), the cause of toxicity remains unidentified. This article describes the analytical method development for seven additional pesticides that are being examined to determine if they might play a role in the unexplained toxicity. A pressurized liquid extraction method was optimized to simultaneously extract diazinon, methyl parathion, oxyfluorfen, dicofol, fenpropathrin, pyraclostrobin, and indoxacarb from sediment, and the extracts were cleaned using a two-step solid-phase extraction procedure. The final extract was analyzed for the target pesticides by gas chromatography/nitrogen-phosphorus detector (GC/NPD), and gas chromatography/electron capture detector (GC/ECD), after sulfur was removed by shaking with copper and cold crystallization. Three sediments were used as reference matrices to assess method accuracy and precision. Method detection limits were 0.23-1.8 ng/g dry sediment using seven replicates of sediment spiked at 1.0 ng/g dry sediment. Recoveries ranged from 61.6 to 118% with relative standard deviations of 2.1-17% when spiked at 5.0 and 50 ng/g dry sediment. The three reference sediments, spiked with 50 ng/g dry weight of the pesticide mixture, were aged for 0.25, 1, 4, 7, and 14 days. Recoveries of the pesticides in the sediments generally decreased with increased aging time, but the magnitude of the decline was pesticide and sediment dependent. The developed method was applied to field-collected sediments from the Central Valley of California.

  15. A Novel UAS Rapid Deployment Platform for Targeted Gas Sampling and Meteorological Soundings at Altitudes up to 2,700 masl

    Science.gov (United States)

    Thomas, Rick M.; Greatwood, Colin; Richardson, Tom; Freer, Jim; MacKenzie, Rob; Brownlow, Rebecca; Lowry, David; Fisher, Rebecca E.; France, James; Nisbet, Euan G.

    2015-04-01

    This research project has developed Unmanned Aerial System (UAS) technologies for intelligent targeting and collection of atmospheric gas samples to investigate the so-called Southern Tropical Methane Anomaly, for which it is necessary to sample air below and above the trade-wind inversion. Air parcels above and below the South Atlantic trade-wind inversion can have markedly different trajectories and, hence, encounter very different methane source regions. The system is intelligent in that high resolution temperature and humidity sensors linked to the ground station characterise the atmospheric profile on the upward flight to ensure the platform targets the appropriate sample elevations on the downward trajectory. This capability has been proven to an altitude of 2,700 metres above sea level (masl; ca. 700 mb) at Ascension Island in the South Atlantic and shown that rapid and repeat deployment and sample collection is achievable. Three novel eight motor multirotor UAS (or octocopter) platforms were developed at Bristol Robotics Laboratory (BRL) using primarily off -the-shelf components with a custom-built main fuselage. Gas sampling and atmospheric sensor systems were designed by the University of Birmingham. Our paper explores the capability of this UAS and provides some initial results from the air sampling campaign conducted in September 2014. Thirty-eight sampling flights were conducted over 12 days and the resulting 47 samples analysed for their CH4 concentration using the high-precision Picarro Cavity Ring Down Spectrometer already installed at Ascension Island. A subset of samples were sent for δ13CCH4 analysis in Egham, UK. The flights were conducted up to an altitude of 2,700m with 2,000m being typical. There were no major incidents although variable zero and high wind situations above the trade wind inversion (typically at 1,800m) both presented unique challenges and required careful flight planning strategies and in flight trajectory changes. As a

  16. Rapid determination of anti-estrogens by gas chromatography/mass spectrometry in urine: Method validation and application to real samples.

    Science.gov (United States)

    Gerace, E; Salomone, A; Abbadessa, G; Racca, S; Vincenti, M

    2012-02-01

    A fast screening protocol was developed for the simultaneous determination of nine anti-estrogenic agents (aminoglutethimide, anastrozole, clomiphene, drostanolone, formestane, letrozole, mesterolone, tamoxifen, testolactone) plus five of their metabolites in human urine. After an enzymatic hydrolysis, these compounds can be extracted simultaneously from urine with a simple liquid-liquid extraction at alkaline conditions. The analytes were subsequently analyzed by fast-gas chromatography/mass spectrometry (fast-GC/MS) after derivatization. The use of a short column, high-flow carrier gas velocity and fast temperature ramping produced an efficient separation of all analytes in about 4 min, allowing a processing rate of 10 samples/h. The present analytical method was validated according to UNI EN ISO/IEC 17025 guidelines for qualitative methods. The range of investigated parameters included the limit of detection, selectivity, linearity, repeatability, robustness and extraction efficiency. High MS-sampling rate, using a benchtop quadrupole mass analyzer, resulted in accurate peak shape definition under both scan and selected ion monitoring modes, and high sensitivity in the latter mode. Therefore, the performances of the method are comparable to the ones obtainable from traditional GC/MS analysis. The method was successfully tested on real samples arising from clinical treatments of hospitalized patients and could profitably be used for clinical studies on anti-estrogenic drug administration.

  17. Rapid determination of anti-estrogens by gas chromatography/mass spectrometry in urine: Method validation and application to real samples

    Directory of Open Access Journals (Sweden)

    E. Gerace

    2012-02-01

    Full Text Available A fast screening protocol was developed for the simultaneous determination of nine anti-estrogenic agents (aminoglutethimide, anastrozole, clomiphene, drostanolone, formestane, letrozole, mesterolone, tamoxifen, testolactone plus five of their metabolites in human urine. After an enzymatic hydrolysis, these compounds can be extracted simultaneously from urine with a simple liquid–liquid extraction at alkaline conditions. The analytes were subsequently analyzed by fast-gas chromatography/mass spectrometry (fast-GC/MS after derivatization. The use of a short column, high-flow carrier gas velocity and fast temperature ramping produced an efficient separation of all analytes in about 4 min, allowing a processing rate of 10 samples/h. The present analytical method was validated according to UNI EN ISO/IEC 17025 guidelines for qualitative methods. The range of investigated parameters included the limit of detection, selectivity, linearity, repeatability, robustness and extraction efficiency. High MS-sampling rate, using a benchtop quadrupole mass analyzer, resulted in accurate peak shape definition under both scan and selected ion monitoring modes, and high sensitivity in the latter mode. Therefore, the performances of the method are comparable to the ones obtainable from traditional GC/MS analysis. The method was successfully tested on real samples arising from clinical treatments of hospitalized patients and could profitably be used for clinical studies on anti-estrogenic drug administration. Keywords: Anti-estrogens, Fast-GC/MS, Urine screening, Validation, Breast cancer

  18. Proposal for the award of a blanket contract for automatic air-sampling systems for fire and gas detection in the LHC experiments

    CERN Document Server

    2004-01-01

    This document concerns the award of a blanket contract for automatic air-sampling systems for fire and gas detection in the LHC experiments. Following a market survey carried out among 119 firms in ten Member States, a call for tenders (IT-2891/ST) was sent on 1 August 2003 to four firms, in three Member States. By the closing date, CERN had received two tenders from one firm and one consortium, in three Member States. The Finance Committee is invited to agree to the negotiation of a blanket contract with ICARE (FR), the lowest bidder, for the supply of automatic air-sampling systems for fire and gas detection in the LHC experiments for a total amount not exceeding 1 750 000 euros (2 714 000 Swiss francs), subject to revision for inflation from 1 January 2007 with options for air-sampling smoke detection systems for electrical racks, for an additional amount of 400 000 euros (620 000 Swiss francs), subject to revision for inflation from 1 January 2007, bringing the total amount to a maximum of 2 150 000 euros...

  19. Sample pretreatment optimization for the analysis of short chain chlorinated paraffins in soil with gas chromatography-electron capture negative ion-mass spectrometry.

    Science.gov (United States)

    Chen, Laiguo; Huang, Yumei; Han, Shuang; Feng, Yongbin; Jiang, Guo; Tang, Caiming; Ye, Zhixiang; Zhan, Wei; Liu, Ming; Zhang, Sukun

    2013-01-25

    Accurately quantifying short chain chlorinated paraffins (SCCPs) in soil samples with gas chromatograph coupled with electron capture negative ionization mass spectrometry (GC-ECNI-MS) is difficult because many other polychlorinated pollutants are present in the sample matrices. These pollutants (e.g., polychlorinated biphenyls (PCBs), organochlorine pesticides (OCPs) and toxaphene) can cause serious interferences during SCCPs analysis with GC-MS. Four main columns packed with different adsorbents, including silica gel, Florisil and alumina, were investigated in this study to determine their performance for separating interfering pollutants from SCCPs. These experimental results suggest that the optimum cleanup procedure uses a silica gel column and a multilayer silica gel-Florisil composite column. This procedure completely separated 22 PCB congeners, 23 OCPs and three toxaphene congeners from SCCPs. However, p,p'-DDD, cis-nonachlor and o,p'-DDD were not completely removed and only 53% of the total toxaphene was removed. This optimized method was successfully and effectively applied for removing interfering pollutants from real soil samples. SCCPs in 17 soil samples from different land use areas within a suburban region were analyzed with the established method. The concentrations of SCCPs in these samples were between 7 and 541 ng g(-1) (mean: 84 ng g(-1)). Similar homologue SCCPs patterns were observed between the soil samples collected from different land use areas. In addition, lower chlorinated (Cl(6/7)) C(10)- and C(11)- SCCPs were the dominant congeners. Copyright © 2012 Elsevier B.V. All rights reserved.

  20. Ultrasound-assisted extraction and solid-phase extraction for the simultaneous determination of five amide herbicides in fish samples by gas chromatography with electron capture detection.

    Science.gov (United States)

    Qu, Zhipeng; Bai, Xiuzhi; Zhang, Ting; Yang, Zhaoguang

    2017-03-01

    An efficient sample extraction and clean-up method was developed for simultaneous determination of five amide herbicides (alachlor, acetochlor, propisochlor, metazachlor, and butachlor) in fish samples. The protocol consisted of ultrasound-assisted solvent extraction and solid-phase extraction clean-up. In detail, aliquots of homogenized fish flesh were thoroughly mixed with 20 mL of n-hexane and then extracted with ultrasonication for 40 min. Each sample was centrifuged and the supernatant was collected for the subsequent clean-up. For the sample preparation, the above supernatant was processed with a C 18 column with 3 mL of dichloromethane/n-hexane (1:1, v/v) as the eluant. Then the samples were analyzed by gas chromatography with electron capture detection. The correlation coefficients of the five calibration curves were 0.9976-0.9998 (n = 3). The limits of detection (S/N = 3, n = 11) and limits of quantification (S/N = 10, n = 11) were 0.19-0.42 and 0.63-1.39 μg/kg, respectively. The recoveries of this method were 71.2-92.6% with good precision (<4.7% relative standard deviations, n = 6). The developed method was successfully applied to monitor the five amide herbicides in fish samples collected from different cities. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Different Analytical Procedures for the Study of Organic Residues in Archeological Ceramic Samples with the Use of Gas Chromatography-mass Spectrometry.

    Science.gov (United States)

    Kałużna-Czaplińska, Joanna; Rosiak, Angelina; Kwapińska, Marzena; Kwapiński, Witold

    2016-01-01

    The analysis of the composition of organic residues present in pottery is an important source of information for historians and archeologists. Chemical characterization of the materials provides information on diets, habits, technologies, and original use of the vessels. This review presents the problem of analytical studies of archeological materials with a special emphasis on organic residues. Current methods used in the determination of different organic compounds in archeological ceramics are presented. Particular attention is paid to the procedures of analysis of archeological ceramic samples used before gas chromatography-mass spectrometry. Advantages and disadvantages of different extraction methods and application of proper quality assurance/quality control procedures are discussed.

  2. 40 CFR 86.109-94 - Exhaust gas sampling system; Otto-cycle vehicles not requiring particulate emission measurements.

    Science.gov (United States)

    2010-07-01

    ... accuracy and precision of ±2 °F (1.1 °C). (3) The pressure gauges shall have an accuracy and precision of... ±5 percent. (The volumetric sample flow rate shall be varied inversely with the square root of the...

  3. Modern sample preparation techniques for gas chromatography-mass spectrometry analysis of environmental markers of chemical warfare agents use

    NARCIS (Netherlands)

    Terzic, O.; de Voogt, P.; Banoub, J.

    2014-01-01

    The chapter introduces problematics of on-site chemical analysis in the investigations of past chemical warfare agents (CWA) events. An overview of primary environmental degradation pathways of CWA leading to formation of chemical markers of their use is given. Conventional and modern sample

  4. Mercury speciation in thawed out and refrozen fish samples by gas chromatography coupled to inductively coupled plasma mass spectrometry and atomic fluorescence spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Krystek, Petra; Ritsema, Rob [National Institute for Public Health and the Environment (RIVM), Laboratory for Analytical Chemistry, Bilthoven (Netherlands)

    2005-01-01

    Different sub-sampling procedures were applied for the determination of mercury species (as total mercury Hg, methylmercury MeHg{sup +} and inorganic mercury Hg{sup 2+}) in frozen fish meat. Analyses were carried out by two different techniques. After the sample material was pre-treated by microwave digestion, atomic fluorescence spectroscopy (AFS) was used for the determination of total Hg. Speciation analysis was performed according to the following procedure: dissolution of sample material in tetramethylammonium hydroxide (TMAH), derivatisation with sodium tetraethylborate (NaBEt{sub 4}), extraction into isooctane and measurement with gas chromatography inductively coupled plasma mass spectrometry (GC-ICPMS) for the identification and quantification of methylmercury (MeHg{sup +}) and inorganic mercury (Hg{sup 2+}). The concentration range of total Hg measured in the shark fillets is between 0.9 and 3.6 {mu}g g{sup -1} thawed out shark fillet. Speciation analysis leads to {>=}94% Hg present as MeHg{sup +}. Homogeneity, storage conditions and stability of analytical species and sample materials have great influence on analytical results. Sub-sampling of half-frozen/partly thawed out fish and analysis lead to significantly different concentrations, which are on average a factor of two lower. (orig.)

  5. The quantification of short-chain chlorinated paraffins in sediment samples using comprehensive two-dimensional gas chromatography with μECD detection.

    Science.gov (United States)

    Muscalu, Alina M; Morse, Dave; Reiner, Eric J; Górecki, Tadeusz

    2017-03-01

    The analysis of persistent organic pollutants in environmental samples is a challenge due to the very large number of compounds with varying chemical and physical properties. Chlorinated paraffins (CPs) are complex mixtures of chlorinated n-alkanes with varying chain lengths (C 10 to C 30 ) and degree of chlorination (30 to 70% by weight). Their physical-chemical properties make these compounds persistent in the environment and able to bioaccumulate in living organisms. Comprehensive two-dimensional gas chromatography (GC × GC) coupled with micro-electron capture detection (μECD) was used to separate and quantify short-chain chlorinated paraffins (SCCP) in sediment samples. Distinct ordered bands were observed in the GC × GC chromatograms pointing to group separation. Using the Classification function of the ChromaTOF software, summary tables were generated to determine total area counts to set up multilevel-calibration curves for different technical mixes. Fortified sediment samples were analyzed by GC × GC-μECD with minimal extraction and cleanup. Recoveries ranged from 120 to 130%. To further validate the proposed method for the analysis of SCCPs, the laboratory participated in interlaboratory studies for the analysis of standards and sediment samples. The results showed recoveries between 75 and 95% and z-score values <2, demonstrating that the method is suitable for the analysis of SCCPs in soil/sediment samples. Graphical abstract Quantification of SCCPs by 2D-GC-μECD.

  6. [Determination of fatty acid esters of chloropropanediols in diet samples by gas chromatography-mass spectrometry coupled with solid-supported liquid-liquid extraction].

    Science.gov (United States)

    Gao, Jie; Liu, Qing; Han, Feng; Miao, Hong; Zhao, Yunfeng; Wu, Yongning

    2014-05-01

    To establish a method for the determination of fatty acid esters of 3-monochloropropane-1, 2-diol (3-MCPD) and 2-monochloropropane-1, 3-diol (2-MCPD) in diet samples by gas chromatography-mass spectrometry (GC-MS) with solid-supported liquid-liquid extraction (SLE). Diet samples were ultrasonically extracted by hexane, followed by ester cleavage reaction with sodium methylate in methanol, and then purified by solid-supported liquid-liquid extraction. (SLE) using diatomaceous earth as the sorbent. After derivatization with heptafluorobutyrylimidazole, the analytes were detected by GC-MS and quantified by the deuterated internal standards. The limits of detection (LODs) of 3-MCPD esters and 2-MCPD esters in different diet samples were 0.002 - 0.005 mg/kg and 0.002 - 0.006 mg/kg. The average recoveries of 3-MCPD esters and 2-MCPD esters at the spiking levels of 0.05 and 0.1 mg/kg in the diet samples were in the range of 65.9% - 104.2% and 75.4% - 118.0%, respectively, with the relative standard deviations in the range of 2.2% - 14.2% and 0.8% - .13.9%. The method is simple, accurate and rugged for the determination of fatty acid esters of 3-MCPD and 2-MCPD in diet samples.

  7. Hollow-fiber-supported liquid phase microextraction with in situ derivatization and gas chromatography-mass spectrometry for determination of chlorophenols in human urine samples.

    Science.gov (United States)

    Ito, Rie; Kawaguchi, Migaku; Honda, Hidehiro; Koganei, Youji; Okanouchi, Noriya; Sakui, Norihiro; Saito, Koichi; Nakazawa, Hiroyuki

    2008-09-01

    A simple and highly sensitive method that involves hollow-fiber-supported liquid phase microextraction (HF-LPME) with in situ derivatization and gas chromatography-mass spectrometry (GC-MS) was developed for the determination of chlorophenols (CPs) such as 2,4-dichlorophenol (DCP), 2,4,6-trichlorophenol (TrCP), 2,3,4,6-tetrachlorophenol (TeCP) and pentachlorophenol (PCP) in human urine samples. Human urine samples were enzymatically de-conjugated with beta-glucuronidase and sulfatase. After de-conjugation, HF-LPME with in situ derivatization was performed. After extraction, 2 microl of extract was carefully withdrawn into a syringe and injected into the GC-MS system. The limits of detection (S/N=3) and quantification (S/N>10) of CPs in the human urine samples are 0.1-0.2 ng ml(-1) and 0.5-1 ng ml(-1), respectively. The calibration curve for CPs is linear with a correlation coefficient of >0.99 in the range of 0.5-500 ng ml(-1) for DCP and TrCP, and of 1-500 ng ml(-1) for TeCP and PCP, respectively. The average recoveries of CPs (n=6) in human urine samples are 81.0-104.0% (R.S.D.: 1.9-6.6%) with correction using added surrogate standards. When the proposed method was applied to human urine samples, CPs were detected at sub-ng ml(-1) level.

  8. Rapid screening of selective serotonin re-uptake inhibitors in urine samples using solid-phase microextraction gas chromatography-mass spectrometry.

    Science.gov (United States)

    Salgado-Petinal, Carmen; Lamas, J Pablo; Garcia-Jares, Carmen; Llompart, Maria; Cela, Rafael

    2005-07-01

    In this paper a solid-phase microextraction-gas chromatography-mass spectrometry (SPME-GC-MS) method is proposed for a rapid analysis of some frequently prescribed selective serotonin re-uptake inhibitors (SSRI)-venlafaxine, fluvoxamine, mirtazapine, fluoxetine, citalopram, and sertraline-in urine samples. The SPME-based method enables simultaneous determination of the target SSRI after simple in-situ derivatization of some of the target compounds. Calibration curves in water and in urine were validated and statistically compared. This revealed the absence of matrix effect and, in consequence, the possibility of quantifying SSRI in urine samples by external water calibration. Intra-day and inter-day precision was satisfactory for all the target compounds (relative standard deviation, RSD, detection limits achieved were detected and tentatively identified.

  9. Reliability of Serum Metabolites over a Two-Year Period : A Targeted Metabolomic Approach in Fasting and Non-Fasting Samples from EPIC

    NARCIS (Netherlands)

    Carayol, Marion; Licaj, Idlir; Achaintre, David; Sacerdote, Carlotta; Vineis, Paolo; Key, Timothy J; Onland Moret, N Charlotte; Scalbert, Augustin; Rinaldi, Sabina; Ferrari, Pietro

    2015-01-01

    OBJECTIVE: Although metabolic profiles have been associated with chronic disease risk, lack of temporal stability of metabolite levels could limit their use in epidemiological investigations. The present study aims to evaluate the reliability over a two-year period of 158 metabolites and compare

  10. High-performance serial block-face SEM of nonconductive biological samples enabled by focal gas injection-based charge compensation.

    Science.gov (United States)

    Deerinck, T J; Shone, T M; Bushong, E A; Ramachandra, R; Peltier, S T; Ellisman, M H

    2018-05-01

    A longstanding limitation of imaging with serial block-face scanning electron microscopy is specimen surface charging. This charging is largely due to the difficulties in making biological specimens and the resins in which they are embedded sufficiently conductive. Local accumulation of charge on the specimen surface can result in poor image quality and distortions. Even minor charging can lead to misalignments between sequential images of the block-face due to image jitter. Typically, variable-pressure SEM is used to reduce specimen charging, but this results in a significant reduction to spatial resolution, signal-to-noise ratio and overall image quality. Here we show the development and application of a simple system that effectively mitigates specimen charging by using focal gas injection of nitrogen over the sample block-face during imaging. A standard gas injection valve is paired with a precisely positioned but retractable application nozzle, which is mechanically coupled to the reciprocating action of the serial block-face ultramicrotome. This system enables the application of nitrogen gas precisely over the block-face during imaging while allowing the specimen chamber to be maintained under high vacuum to maximise achievable SEM image resolution. The action of the ultramicrotome drives the nozzle retraction, automatically moving it away from the specimen area during the cutting cycle of the knife. The device described was added to a Gatan 3View system with minimal modifications, allowing high-resolution block-face imaging of even the most charge prone of epoxy-embedded biological samples. © 2017 The Authors Journal of Microscopy © 2017 Royal Microscopical Society.

  11. Gas chromatography--inductively coupled plasma--time-of-flight mass spectrometry for the speciation analysis of organolead compounds in environmental water samples.

    Science.gov (United States)

    Heisterkamp, M; Adams, F C

    2001-07-01

    The application of inductively coupled plasma--time-of-flight mass spectrometry for the speciation analysis of organolead compounds in environmental waters is described. Construction of the transfer line was achieved by means of a relatively simple and rapid coupling procedure. Derivatization of the ionic lead species was achieved by in-situ propylation with sodium tetrapropylborate; simultaneous extraction of the derivatized compounds in hexane was followed by separation and detection by capillary gas chromatography hyphenated to inductively coupled plasma-time-of-flight mass spectrometry. Detection limits for the different organolead species ranged from 10 to 15 fg (as Pb), corresponding to procedural detection limits between 50 and 75 ng L(-1), on the basis of a 50 mL snow sample, extraction with 200 microL hexane, and subsequent injection of 1 microL of the organic extract on to the column. The accuracy of the system was confirmed by additional analysis of the water samples by capillary gas chromatography coupled with microwave-induced plasma-atomic-emission spectrometry and the analysis of a standard reference material CRM 605 (road dust) with a certified content of trimethyllead.

  12. Multistage plasma initiation process by pulsed CO2 laser irradiation of a Ti sample in an ambient gas (He, Ar, or N2)

    Science.gov (United States)

    Hermann, J.; Boulmer-Leborgne, C.; Mihailescu, I. N.; Dubreuil, B.

    1993-02-01

    New experimental results are reported on plasma initiation in front of a titanium sample irradiated by ir (λ=10.6 μm) laser pulses in an ambient gas (He, Ar, and N2) at pressures ranging from several Torr up to the atmosphere. The plasma is studied by space- and time-resolved emission spectroscopy, while sample vaporization is probed by laser-induced fluorescence spectroscopy. Threshold laser intensities leading to the formation of a plasma in the vapor and in the ambient gases are determined. Experimental results support the model of a vaporization mechanism for the plasma initiation (vaporization-initiated plasma breakdown). The plasma initiation is described by simple numerical criteria based on a two-stage process. Theoretical predictions are found to be in a reasonable agreement with the experiment. This study provides also a clear explanation of the influence of the ambient gas on the laser beam-metal surface energy transfer. Laser irradiation always causes an important vaporization when performed in He, while in the case of Ar or N2, the interaction is reduced in heating and vaporization of some surface defects and impurities.

  13. LANDFILL GAS CONVERSION TO LNG AND LCO{sub 2}. PHASE 1, FINAL REPORT FOR THE PERIOD MARCH 1998-FEBRUARY 1999

    Energy Technology Data Exchange (ETDEWEB)

    COOK,W.J.; NEYMAN,M.; SIWAJEK,L.A.; BROWN,W.R.; VAN HAUWAERT,P.M.; CURREN,E.D.

    1998-02-25

    Process designs and economics were developed to produce LNG and liquid carbon dioxide (CO{sub 2}) from landfill gas (LFG) using the Acrion CO{sub 2} wash process. The patented Acrion CO{sub 2} wash process uses liquid CO{sub 2} to absorb contaminants from the LFG. The process steps are compression, drying, CO{sub 2} wash contaminant removal and CO{sub 2} recovery, residual CO{sub 2} removal and methane liquefaction. Three flowsheets were developed using different residual CO{sub 2} removal schemes. These included physical solvent absorption (methanol), membranes and molecular sieves. The capital and operating costs of the flowsheets were very similar. The LNG production cost was around ten cents per gallon. In parallel with process flowsheet development, the business aspects of an eventual commercial project have been explored. The process was found to have significant potential commercial application. The business plan effort investigated the economics of LNG transportation, fueling, vehicle conversion, and markets. The commercial value of liquid CO{sub 2} was also investigated. This Phase 1 work, March 1998 through February 1999, was funded under Brookhaven National laboratory contract 725089 under the research program entitled ``Liquefied Natural Gas as a Heavy Vehicle Fuel.'' The Phase 2 effort will develop flowsheets for the following: (1) CO{sub 2} and pipeline gas production, with the pipeline methane being liquefied at a peak shaving site, (2) sewage digester gas as an alternate feedstock to LFG and (3) the use of mixed refrigerants for process cooling. Phase 2 will also study the modification of Acrion's process demonstration unit for the production of LNG and a market site for LNG production.

  14. Mobile membrane introduction tandem mass spectrometry for on-the-fly measurements and adaptive sampling of VOCs around oil and gas projects in Alberta, Canada

    Science.gov (United States)

    Krogh, E.; Gill, C.; Bell, R.; Davey, N.; Martinsen, M.; Thompson, A.; Simpson, I. J.; Blake, D. R.

    2012-12-01

    The release of hydrocarbons into the environment can have significant environmental and economic consequences. The evolution of smaller, more portable mass spectrometers to the field can provide spatially and temporally resolved information for rapid detection, adaptive sampling and decision support. We have deployed a mobile platform membrane introduction mass spectrometer (MIMS) for the in-field simultaneous measurement of volatile and semi-volatile organic compounds. In this work, we report instrument and data handling advances that produce geographically referenced data in real-time and preliminary data where these improvements have been combined with high precision ultra-trace VOCs analysis to adaptively sample air plumes near oil and gas operations in Alberta, Canada. We have modified a commercially available ion-trap mass spectrometer (Griffin ICX 400) with an in-house temperature controlled capillary hollow fibre polydimethylsiloxane (PDMS) polymer membrane interface and in-line permeation tube flow cell for a continuously infused internal standard. The system is powered by 24 VDC for remote operations in a moving vehicle. Software modifications include the ability to run continuous, interlaced tandem mass spectrometry (MS/MS) experiments for multiple contaminants/internal standards. All data are time and location stamped with on-board GPS and meteorological data to facilitate spatial and temporal data mapping. Tandem MS/MS scans were employed to simultaneously monitor ten volatile and semi-volatile analytes, including benzene, toluene, ethylbenzene and xylene (BTEX), reduced sulfur compounds, halogenated organics and naphthalene. Quantification was achieved by calibrating against a continuously infused deuterated internal standard (toluene-d8). Time referenced MS/MS data were correlated with positional data and processed using Labview and Matlab to produce calibrated, geographical Google Earth data-visualizations that enable adaptive sampling protocols

  15. Salting-out assisted liquid-liquid extraction combined with gas chromatography-mass spectrometry for the determination of pyrethroid insecticides in high salinity and biological samples.

    Science.gov (United States)

    Niu, Zongliang; Yu, Chunwei; He, Xiaowen; Zhang, Jun; Wen, Yingying

    2017-09-05

    A salting-out assisted liquid-liquid extraction (SALLE) combined with gas chromatography-mass spectrometry (GC-MS) method was developed for the determination of four pyrethroid insecticides (PYRs) in high salinity and biological samples. Several parameters including sample pH, salting-out solution volume and salting-out solution pH influencing the extraction efficiency were systematically investigated with the aid of orthogonal design. The optimal extraction conditions of SALLE were: 4mL of salting-out solution with pH=4 and the sample pH=3. Under the optimum extraction and determination conditions, good responses for four PYRs were obtained in a range of 5-5000ng/mL, with linear coefficients greater than 0.998. The recoveries of the four PYRs ranged from 74% to 110%, with standard deviations ranging from 1.8% to 9.8%. The limits of detection based on a signal-to-noise ratio of 3 were between 1.5-60.6ng/mL. The method was applied to the determination of PYRs in urine, seawater and wastewater samples with a satisfactory result. The results demonstrated that this SALLE-GC-MS method was successfully applied to determine PYRs in high salinity and biological samples. SALLE avoided the need for the elimination of salinity and protein in the sample matrix, as well as clean-up of the extractant. Most of all, no centrifugation or any special apparatus are required, make this a promising method for rapid sample preparation procedure. Copyright © 2017 Elsevier B.V. All rights reserved.

  16. Integrated sampling and analysis unit for the determination of sexual pheromones in environmental air using fabric phase sorptive extraction and headspace-gas chromatography-mass spectrometry.

    Science.gov (United States)

    Alcudia-León, M Carmen; Lucena, Rafael; Cárdenas, Soledad; Valcárcel, Miguel; Kabir, Abuzar; Furton, Kenneth G

    2017-03-10

    This article presents a novel unit that integrates for the first time air sampling and preconcentration based on the use of fabric phase sorptive extraction principles. The determination of Tuta absoluta sexual pheromone traces in environmental air has been selected as analytical problem. For this aim, a novel laboratory-built unit made up of commercial brass elements as holder of the sol-gel coated fabric extracting phase has been designed and optimized. The performance of the integrated unit was evaluated analyzing environmental air sampled in tomato crops. The unit can work under sampling and analysis mode which eliminates any need for sorptive phase manipulation prior to instrumental analysis. In the sampling mode, the unit can be connected to a sampling pump to pass the air through the sorptive phase at a controlled flow-rate. In the analysis mode, it is placed in the gas chromatograph autosampler without any instrumental modification. It also diminishes the risk of cross contamination between sampling and analysis. The performance of the new unit has been evaluated using the main components of the sexual pheromone of Tuta absoluta [(3E,8Z,11Z)-tetradecatrien-1-yl acetate and (3E,8Z)-tetradecadien-1-yl acetate] as model analytes. The limits of detection for both compounds resulted to be 1.6μg and 0.8μg, respectively, while the precision (expressed as relative standard deviation) was better than 3.7%. Finally, the unit has been deployed in the field to analyze a number of real life samples, some of them were found positive. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. Application of acetone acetals as water scavengers and derivatization agents prior to the gas chromatographic analysis of polar residual solvents in aqueous samples.

    Science.gov (United States)

    van Boxtel, Niels; Wolfs, Kris; Van Schepdael, Ann; Adams, Erwin

    2015-12-18

    The sensitivity of gas chromatography (GC) combined with the full evaporation technique (FET) for the analysis of aqueous samples is limited due to the maximum tolerable sample volume in a headspace vial. Using an acetone acetal as water scavenger prior to FET-GC analysis proved to be a useful and versatile tool for the analysis of high boiling analytes in aqueous samples. 2,2-Dimethoxypropane (DMP) was used in this case resulting in methanol and acetone as reaction products with water. These solvents are relatively volatile and were easily removed by evaporation enabling sample enrichment leading to 10-fold improvement in sensitivity compared to the standard 10μL FET sample volumes for a selection of typical high boiling polar residual solvents in water. This could be improved even further if more sample is used. The method was applied for the determination of residual NMP in an aqueous solution of a cefotaxime analogue and proved to be considerably better than conventional static headspace (sHS) and the standard FET approach. The methodology was also applied to determine trace amounts of ethylene glycol (EG) in aqueous samples like contact lens fluids, where scavenging of the water would avoid laborious extraction prior to derivatization. During this experiment it was revealed that DMP reacts quantitatively with EG to form 2,2-dimethyl-1,3-dioxolane (2,2-DD) under the proposed reaction conditions. The relatively high volatility (bp 93°C) of 2,2-DD makes it possible to perform analysis of EG using the sHS methodology making additional derivatization reactions superfluous. Copyright © 2015 Elsevier B.V. All rights reserved.

  18. Gas chromatography/isotope ratio mass spectrometry: analysis of methanol, ethanol and acetic acid by direct injection of aqueous alcoholic and acetic acid samples.

    Science.gov (United States)

    Ai, Guomin; Sun, Tong; Dong, Xiuzhu

    2014-08-15

    Methanol, ethanol, and acetic acid are not easily extracted from aqueous samples and are susceptible to isotope fractionation in gas chromatography/isotope ratio mass spectrometry (GC/IRMS) analysis. Developing a direct dilution GC/IRMS method for aqueous samples, by adjusting the sample concentrations in common solvents to be similar to each other and using a fixed GC split ratio, is very convenient and important because any linearity effects caused by amount-dependent isotope fractionation can be avoided. The suitability of acetonitrile and acetone solvents for the GC/IRMS analysis of pure methanol, ethanol and acetic acid, and commercial liquor and vinegar samples was evaluated using n-hexane and water as control solvents. All the solvents including water were separated from the analyte on a HP-INNOWAX column and were diverted away from the combustion interface. The influence of liquor matrix on the ethanol GC/IRMS analyses was evaluated by adding pure ethanol to liquor samples. Acetonitrile and acetone gave similar δ(13) C values for pure ethanol and pure acetic acid to those obtained in water and n-hexane, and also gave similar δ(13) C values of ethanol in liquor and acetic acid in white vinegar to that obtained in water. For methanol analysis, acetonitrile and refined acetone gave similar δ(13) C values to that obtained in water, but n-hexane was not a suitable solvent. In addition, isotopic fractionation caused by solvent and solute interactions was observed. We recommend using acetonitrile for the GC/IRMS analysis of aqueous alcoholic samples, and acetone for the analysis of aqueous acetic acid samples. This direct dilution method can provide high accurate and precise GC/IRMS analysis of the relative changes in δ(13) C values of methanol, ethanol, and acetic acid. Copyright © 2014 John Wiley & Sons, Ltd.

  19. Development and operation of an integrated sampling probe and gas analyzer for turbulent mixing studies in complex supersonic flows

    Science.gov (United States)

    Wiswall, John D.

    For many aerospace applications, mixing enhancement between co-flowing streams has been identified as a critical and enabling technology. Due to short fuel residence times in scramjet combustors, combustion is limited by the molecular mixing of hydrogen (fuel) and air. Determining the mixedness of fuel and air in these complex supersonic flowfields is critical to the advancement of novel injection schemes currently being developed at UTA in collaboration with NASA Langley and intended to be used on a future two-stage to orbit (~Mach 16) hypersonic air-breathing vehicle for space access. Expanding on previous work, an instrument has been designed, fabricated, and tested in order to measure mean concentrations of injected helium (a passive scalar used instead of hazardous hydrogen) and to quantitatively characterize the nature of the high-frequency concentration fluctuations encountered in the compressible, turbulent, and high-speed (up to Mach 3.5) complex flows associated with the new supersonic injection schemes. This important high-frequency data is not yet attainable when employing other techniques such as Laser Induced Fluorescence, Filtered Rayleigh Scattering or mass spectroscopy in the same complex supersonic flows. The probe operates by exploiting the difference between the thermodynamic properties of two species through independent massflow measurements and calibration. The probe samples isokinetically from the flowfield's area of interest and the helium concentration may be uniquely determined by hot-film anemometry and internally measured stagnation conditions. The final design has a diameter of 0.25" and is only 2.22" long. The overall accuracy of the probe is 3% in molar fraction of helium. The frequency response of mean concentration measurements is estimated at 103 Hz, while high-frequency hot-film measurements were conducted at 60 kHz. Additionally, the work presents an analysis of the probe's internal mixing effects and the effects of the spatial

  20. Vertical integration of oil groups in gas downstream activities after the deregulation of gas and electricity industries: Determining factors and means of implementation of this strategy. Research report period: October 2000 - September 2003

    International Nuclear Information System (INIS)

    Benadjaoud, Nawel

    2003-12-01

    After a presentation of some characteristics of gas and electric power industries, and an overview of the process and consequences of the general trend of deregulation in these sectors, the author of this research proposes a contribution to the economic analysis of movements of vertical integration of large oil companies and groups in which downstream gas activities and power activities represent a small fraction of their activities. The objectives of this research were then to understand why oil companies are practising vertical integration on the gas sector, and how these oil companies proceed in terms of organisational means to perform this successful movement of vertical integration. The author addresses theoretical concepts as they are analysed in some theories of the firm. The studied questions are then addressed in the case of some major European oil companies through a detailed examination of all their operations related to the gas downstream activities and to electricity activities, and by examining the most used organisational modes for the implementation of such vertical integrations

  1. Forensic Characterization of Liquor Samples by Gas Chromatography-Mass Spectrometry (GC-MS – A Review

    Directory of Open Access Journals (Sweden)

    Praveen K. Yadav

    2017-12-01

    Full Text Available Alcohol is a subject of forensic research across the world. The forensic characterization of alcoholic beverages is required in cases of death and crimes due to alcohol consumption. In many cases, determining the geographic origin becomes a very important part of the investigation. Therefore, it is important to develop more sensitive methods for the analysis of alcoholic beverages. In this review, an attempt has been made to summarize the work accomplished so far in the field of analysis and detection of alcoholic beverages. In this review, various sample preparation techniques for GC-MS analysis of alcoholic beverages have been discussed along with its applications. GC-MS based analysis is less time consuming, more sensitive and more accurate.   Keywords: Forensic Sciences, Alcoholic beverages, Mortality, Analysis, GC-MS

  2. Gas chromatographic determination of 1,1-dimethylhydrazine in water samples by solid-phase microextraction with derivatization

    Directory of Open Access Journals (Sweden)

    Madi Abilev

    2014-10-01

    Full Text Available 1,1-Dimethylhydrazine (1,1-DMH used as a rocket fuel component is highly reactive and unstable compound. It greatly complicates its accurate and express determination in environmental samples. Goal of this work was to develop a method for its express determination in water samples based on solid-phase microextraction with preliminary derivatization. Acetone was selected as reagent for derivatization because during its reaction with 1,1-DMH, volatile and hydrophobic acetone dimethylhydrazone (ADMH was formed. It was established that fiber based on 100-micron polydimethylsiloxane provides the most efficient extraction of ADMH from water at extraction time 2 min. Optimal concentration of acetone was 30 mg/mL. The minimum time for reaction of 1,1-DMH with acetone is 10 minutes. Addition of acids and alkali reduced ADMH response that may be caused by degradation of 1,1-DMH and reduction of derivatization rate. Addition of salt allowed to increase the response of ADMH however made impossible the quantitative determination of 1,1-DMH. Dependence of ADMH response on the concentration of 1,1-DMH at optimized parameters is linear in the concentrations range of 0.1-100 mg/L and can be used for quantitative determination of 1,1-DMH in water. Detection limit of the developed method is 0.02 mg/L. Reproducibility index of the method in the whole range of concentrations did not exceed 7%, accuracy index - 15%. Developed method is simple, inexpensive, accurate, automated and can be recommended for implementation in laboratories conducting environmental monitoring in areas of rocket-carriers fall.

  3. Assessment of pesticide contamination in soil samples from an intensive horticulture area, using ultrasonic extraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Gonçalves, C; Alpendurada, M F

    2005-03-15

    In order to reduce the amount of sample to be collected and the time consumed in the analytical process, a broad range of analytes should be preferably considered in the same analytical procedure. A suitable methodology for pesticide residue analysis in soil samples was developed based on ultrasonic extraction (USE) and gas chromatography-mass spectrometry (GC-MS). For this study, different classes of pesticides were selected, both recent and old persistent molecules: parent compounds and degradation products, namely organochlorine, organophosphorous and pyrethroid insecticides, triazine and acetanilide herbicides and other miscellaneous pesticides. Pesticide residues could be detected in the low- to sub-ppb range (0.05-7.0mugkg(-1)) with good precision (7.5-20.5%, average 13.7% R.S.D.) and extraction efficiency (69-118%, average 88%) for the great majority of analytes. This methodology has been applied in a monitoring program of soil samples from an intensive horticulture area in Póvoa de Varzim, North of Portugal. The pesticides detected in four sampling programs (2001/2002) were the following: lindane, dieldrin, endosulfan, endosulfan sulfate, 4,4'-DDE, 4,4'-DDD, atrazine, desethylatrazine, alachlor, dimethoate, chlorpyrifos, pendimethalin, procymidone and chlorfenvinphos. Pesticide contamination was investigated at three depths and in different soil and crop types to assess the influence of soil characteristics and trends over time.

  4. Mixed-mode solid-phase extraction followed by acetylation and gas chromatography mass spectrometry for the reliable determination of trans-resveratrol in wine samples

    Energy Technology Data Exchange (ETDEWEB)

    Montes, R.; Garcia-Lopez, M. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Instituto de Investigacion y Analisis Alimentario, Universidad de Santiago de Compostela, Santiago de Compostela 15782 (Spain); Rodriguez, I., E-mail: isaac.rodriguez@usc.es [Departamento de Quimica Analitica, Nutricion y Bromatologia, Instituto de Investigacion y Analisis Alimentario, Universidad de Santiago de Compostela, Santiago de Compostela 15782 (Spain); Cela, R. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Instituto de Investigacion y Analisis Alimentario, Universidad de Santiago de Compostela, Santiago de Compostela 15782 (Spain)

    2010-07-12

    This work presents an advantageous analytical procedure for the accurate determination of free trans-resveratrol in red and white wines. The proposed method involves solid-phase extraction (SPE), acetylation of the analyte in aqueous media and further determination by gas chromatography (GC) with mass spectrometry detection (MS). The use of a mixed-mode SPE sorbent provides an improvement in the selectivity of the extraction step; moreover, the presence of several intense ions in the electron impact mass spectra of its acetyl derivative guarantees the unambiguous identification of trans-resveratrol. Considering a sample intake of 10 mL, the method provides a limit of quantification (LOQ) of 0.8 ng mL{sup -1} and linear responses for concentrations up to 2.5 {mu}g mL{sup -1}, referred to wine samples. The average recovery, estimated with samples fortified at different concentrations in the above range, was 99.6% and the inter-day precision stayed below 8%. Trans-resveratrol levels in the analyzed wines varied from 3.4 to 1810 ng mL{sup -1}. Cis-resveratrol was also found in all samples. In most cases, equal or higher responses were measured for this latter form than for the trans-isomer. The reduced form of resveratrol, dihydro-resveratrol, was systematically identified in red wines.

  5. Gas chromatographic-mass spectrometric analysis of urinary volatile organic metabolites: Optimization of the HS-SPME procedure and sample storage conditions.

    Science.gov (United States)

    Živković Semren, Tanja; Brčić Karačonji, Irena; Safner, Toni; Brajenović, Nataša; Tariba Lovaković, Blanka; Pizent, Alica

    2018-01-01

    Non-targeted metabolomics research of human volatile urinary metabolome can be used to identify potential biomarkers associated with the changes in metabolism related to various health disorders. To ensure reliable analysis of urinary volatile organic metabolites (VOMs) by gas chromatography-mass spectrometry (GC-MS), parameters affecting the headspace-solid phase microextraction (HS-SPME) procedure have been evaluated and optimized. The influence of incubation and extraction temperatures and times, coating fibre material and salt addition on SPME efficiency was investigated by multivariate optimization methods using reduced factorial and Doehlert matrix designs. The results showed optimum values for temperature to be 60°C, extraction time 50min, and incubation time 35min. The proposed conditions were applied to investigate urine samples' stability regarding different storage conditions and freeze-thaw processes. The sum of peak areas of urine samples stored at 4°C, -20°C, and -80°C up to six months showed a time dependent decrease over time although storage at -80°C resulted in a slight non-significant reduction comparing to the fresh sample. However, due to the volatile nature of the analysed compounds, more than two cycles of freezing/thawing of the sample stored for six months at -80°C should be avoided whenever possible. Copyright © 2017 Elsevier B.V. All rights reserved.

  6. Application of solid-phase micro extraction for the determination of pesticides in vegetable samples by gas chromatography with an electron capture detector

    International Nuclear Information System (INIS)

    Chai, Mee Kin; Tan, Guan Huat; Kumari, Asha

    2008-01-01

    A solid-phase micro extraction (SPME) method has been developed for the determination of 9 pesticides in 2 vegetables -cucumber and tomato - samples, based on direct immersion mode and subsequent desorption into the injection port of a gas chromatograph with an electron capture detector (GC-ECD). The main factors affecting the SPME process such as extraction time and temperature, desorption time and temperature, the effect of salt addition and fiber depth into the liner were studied and optimized. The analytical procedure proposed consisted of a 30 minute ultrasonic extraction of the target compounds from 1.0 g vegetable samples with 5 mL of distilled water. Then, the samples were filtered and topped up with distilled water to 10 mL. The analytes in this aqueous extract were extracted for 15 minutes with a 100 μm thickness polydimethylsiloxane SPME fiber. Relative standard deviations for triplicate analyses of samples were less than 10 %. The recoveries of the pesticides studied in cucumber and tomato ranged from 52 % to 82 % and the RSD were below 10 %. Therefore, the proposed method is applicable in the analysis of pesticides in vegetable matrices. SPME has been shown to be a simple extraction technique, which has a number of advantages such as solvent free extraction, simplicity and compatibility with the chromatographic analytical system. (author)

  7. The Existence of Heavy Metals such as Pb, Cd, Fe, and Cu in Hair Samples from Gas Station Worker at Yogyakarta Special District

    International Nuclear Information System (INIS)

    Supriyanto, C.; Zainul Kamal; Samin

    2002-01-01

    The monitoring of heavy metals existence such as Pb, Cd, Fe, and Cu in hair samples from gas station worker has been carried out with atomic absorption spectrometry method. The initial preparation of sample were done by immersing them in alcohol over night, after they were dried then they were digested using the teflon bomb digester at the temperature at 150 o C for 3 hours. The content of Pb, Cd, Fe, and Cu in were determined with calibration standard curve method. The content of Pb obtained at hair samples in the range of time at 20 years tend to increase. If it was correlated to the worker who has been working, there was no significant different from the worker who has been working for 20 years there was no significant different. While the content of Cu in sample at range time 20 years showed the significant different if it was correlated to the worker who has been working. The validity of method was tested with CRM Human Hair GBW 07601 from IAEA showed that the content of Fe and Cu were in the certified range of CRM. (author)

  8. Mixed-mode solid-phase extraction followed by acetylation and gas chromatography mass spectrometry for the reliable determination of trans-resveratrol in wine samples

    International Nuclear Information System (INIS)

    Montes, R.; Garcia-Lopez, M.; Rodriguez, I.; Cela, R.

    2010-01-01

    This work presents an advantageous analytical procedure for the accurate determination of free trans-resveratrol in red and white wines. The proposed method involves solid-phase extraction (SPE), acetylation of the analyte in aqueous media and further determination by gas chromatography (GC) with mass spectrometry detection (MS). The use of a mixed-mode SPE sorbent provides an improvement in the selectivity of the extraction step; moreover, the presence of several intense ions in the electron impact mass spectra of its acetyl derivative guarantees the unambiguous identification of trans-resveratrol. Considering a sample intake of 10 mL, the method provides a limit of quantification (LOQ) of 0.8 ng mL -1 and linear responses for concentrations up to 2.5 μg mL -1 , referred to wine samples. The average recovery, estimated with samples fortified at different concentrations in the above range, was 99.6% and the inter-day precision stayed below 8%. Trans-resveratrol levels in the analyzed wines varied from 3.4 to 1810 ng mL -1 . Cis-resveratrol was also found in all samples. In most cases, equal or higher responses were measured for this latter form than for the trans-isomer. The reduced form of resveratrol, dihydro-resveratrol, was systematically identified in red wines.

  9. Development of a radiochemical method for analyzing radon gas in uranium mine atmospheres: covering the period February 3, 1975--March 31, 1976

    Energy Technology Data Exchange (ETDEWEB)

    Stein, L.; Shearer, J.A.; Hohorst, F.A.; Markun, F.

    1977-01-14

    A simplified radiochemical method has been developed for quantitatively analyzing radon gas in underground uranium mines. In this method, a measured volume of air is drawn by a pump through a drying tube and a cartridge containing dioxygenyl hexafluoroantimonate reagent. Radon is captured as a nonvolatile product. After radioactive equilibrium has been established between radon and its short-lived daughters (approximately 4 hours), the gamma-emission of the cartridge is measured with a scintillation counter. The amount of radon is then calculated from the gamma-emission rate. The effect of cartridge geometry, reagent load, and air flow rate upon collection efficiency and counting efficiency is reported.

  10. Development of a radiochemical method for analyzing radon gas in uranium mine atmospheres: covering the period February 3, 1975--March 31, 1976

    International Nuclear Information System (INIS)

    Stein, L.; Shearer, J.A.; Hohorst, F.A.; Markun, F.

    1977-01-01

    A simplified radiochemical method has been developed for quantitatively analyzing radon gas in underground uranium mines. In this method, a measured volume of air is drawn by a pump through a drying tube and a cartridge containing dioxygenyl hexafluoroantimonate reagent. Radon is captured as a nonvolatile product. After radioactive equilibrium has been established between radon and its short-lived daughters (approximately 4 hours), the gamma-emission of the cartridge is measured with a scintillation counter. The amount of radon is then calculated from the gamma-emission rate. The effect of cartridge geometry, reagent load, and air flow rate upon collection efficiency and counting efficiency is reported

  11. Automating data analysis for two-dimensional gas chromatography/time-of-flight mass spectrometry non-targeted analysis of comparative samples.

    Science.gov (United States)

    Titaley, Ivan A; Ogba, O Maduka; Chibwe, Leah; Hoh, Eunha; Cheong, Paul H-Y; Simonich, Staci L Massey

    2018-03-16

    Non-targeted analysis of environmental samples, using comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry (GC × GC/ToF-MS), poses significant data analysis challenges due to the large number of possible analytes. Non-targeted data analysis of complex mixtures is prone to human bias and is laborious, particularly for comparative environmental samples such as contaminated soil pre- and post-bioremediation. To address this research bottleneck, we developed OCTpy, a Python™ script that acts as a data reduction filter to automate GC × GC/ToF-MS data analysis from LECO ® ChromaTOF ® software and facilitates selection of analytes of interest based on peak area comparison between comparative samples. We used data from polycyclic aromatic hydrocarbon (PAH) contaminated soil, pre- and post-bioremediation, to assess the effectiveness of OCTpy in facilitating the selection of analytes that have formed or degraded following treatment. Using datasets from the soil extracts pre- and post-bioremediation, OCTpy selected, on average, 18% of the initial suggested analytes generated by the LECO ® ChromaTOF ® software Statistical Compare feature. Based on this list, 63-100% of the candidate analytes identified by a highly trained individual were also selected by OCTpy. This process was accomplished in several minutes per sample, whereas manual data analysis took several hours per sample. OCTpy automates the analysis of complex mixtures of comparative samples, reduces the potential for human error during heavy data handling and decreases data analysis time by at least tenfold. Copyright © 2018 Elsevier B.V. All rights reserved.

  12. Comparison of Gas Chromatography-Mass Spectrometry and Gas Chromatography-Tandem Mass Spectrometry with Electron Ionization and Negative-Ion Chemical Ionization for Analyses of Pesticides at Trace Levels in Atmospheric Samples

    Directory of Open Access Journals (Sweden)

    Renata Raina

    2008-01-01

    Full Text Available A comparison of detection limits of gas chromatography-mass spectrometry (GC-MS in selected ion monitoring (SIM with gas chromatography-tandem mass spectrometry (GC-MS/MS in selected reaction monitoring (SRM mode with both electron ionization (EI and negative-ion chemical ionization (NCI are presented for over 50 pesticides ranging from organochlorines (OCs, organophosphorus pesticides (OPs and pre-emergent herbicides used in the Canadian prairies (triallate, trifluralin, ethalfluralin. The developed GC-EI/SIM, GC-NCI/SIM, and GC-NCI/SRM are suitable for the determination of pesticides in air sample extracts at concentrations <100 pg µL -1 (< 100 pg m -3 in air. No one method could be used to analyze the range of pre-emergent herbicides, OPs, and OCs investigated. In general GC-NCI/SIM provided the lowest method detection limits (MDLs commonly 2.5-10 pg µL -1 along with best confirmation (<25% RSD of ion ratio, while GC-NCI/SRM is recommended for use where added selectivity or confirmation is required (such as parathion-ethyl, tokuthion, carbofenothion. GC-EI/SRM at concentration < 100 pg µL -1 was not suitable for most pesticides. GC-EI/SIM was more prone to interference issues than NCI methods, but gave good sensitivity (MDLs 1-10 pg µL -1 for pesticides with poor NCI response (OPs: sulfotep, phorate, aspon, ethion, and OCs: alachlor, aldrin, perthane, and DDE, DDD, DDT.

  13. The performance of atmospheric pressure gas chromatography-tandem mass spectrometry compared to gas chromatography-high resolution mass spectrometry for the analysis of polychlorinated dioxins and polychlorinated biphenyls in food and feed samples.

    Science.gov (United States)

    Ten Dam, Guillaume; Pussente, Igor Cabreira; Scholl, Georges; Eppe, Gauthier; Schaechtele, Alexander; van Leeuwen, Stefan

    2016-12-16

    Recently, gas chromatography tandem mass spectrometry (GC-MS/MS) has been added in European Union (EU) legislation as an alternative to magnetic sector high resolution mass spectrometry (HRMS) for the analysis of dioxins and dioxin like polychlorinated biphenyls (dl-PCB) in food and feed. In this study the performance of APGC-MS/MS compared to GC-HRMS is investigated and compared with EU legislation. The study includes the legislative parameters, relative intermediate precision standard deviation (S Rw ,rel), trueness, sensitivity, linear range and ion ratio tolerance. In addition, over 200 real samples of large variety and spanning several orders of magnitude in concentration were analyzed by both techniques and the selectivity was evaluated by comparing chromatograms. The S Rw ,rel and trueness were evaluated using (in-house) reference samples and fulfill to EU legislation, though the S Rw ,rel was better with GC-HRMS. The sensitivity was considerably better than of GC-HRMS while the linear range was similar. Ion ratios were mostly within the tolerable range of ±15%. A (temporary unresolved) systematic deviation in ion ratio was observed for several congeners, yet this did not lead to exceeding of the maximum ion ratio limits. The APGC-MS/MS results for the non-dioxin-like-PCBs (ndl-PCBs) were negatively biased, particularly for PCB138 and 153 in contaminated samples. The selectivity of APGC-MS/MS was lower for several matrices. Particularly for contaminated samples, interfering peaks were observed in the APGC chromatograms of the native compounds (dioxins) and labeled internal standards (PCBs). These can lead to biased results and ultimately to false positive samples. It was concluded that the determination of dioxins and PCBs using APGC-MS/MS meets the requirements set by the European Commission. However, due to generally better selectivity and S Rw ,rel, GC-HRMS is the preferred method for monitoring purposes. Copyright © 2016 Elsevier B.V. All rights

  14. Quantification of short- and medium-chain chlorinated paraffins in environmental samples by gas chromatography quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Gao, Wei; Wu, Jing; Wang, Yawei; Jiang, Guibin

    2016-06-24

    Chlorinated paraffins (CPs) are technical products produced and used in bulk for a number of purposes. However, the analysis of CPs is challenging, as they are complex mixtures of compounds and isomers. We herein report the development of an analytical method for the analysis of short-chain CPs (SCCPs) and medium-chain CPs (MCCPs) using quadrupole time-of-flight high-resolution mass spectrometry (GC-NCI-qTOF-HRMS). This method employs gas chromatography with a chemical ionization source working in negative mode. The linear relationship between chlorination and the CP total response factors was applied to quantify the CP content and the congener group distribution patterns. In a single injection, 24 SCCP formula groups and 24 MCCP formula groups were quantified. Extraction of accurate masses using qTOF-HRMS allowed the SCCPs and MCCPs to be distinguished, with interference from other chemicals (e.g., PCBs) being largely avoided. The SCCP and MCCP detection limits were 24-81ng/mL and 27-170ng/mL, respectively. Comparison of the obtained results with analytical results from gas chromatography coupled with electron capture negative ionization low-resolution mass spectrometry (GC-ECNI-LRMS) indicate that the developed technique is a more accurate and convenient method for the analysis of CPs in samples from a range of matrices. Copyright © 2016 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

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

    2011-04-27

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

  16. The application of headspace gas chromatography coupled to tandem quadrupole mass spectrometry for the analysis of furan in baby food samples.

    Science.gov (United States)

    Pugajeva, Iveta; Rozentale, Irina; Viksna, Arturs; Bartkiene, Elena; Bartkevics, Vadims

    2016-12-01

    Selective methodology employing a tandem quadrupole mass spectrometer coupled to a gas chromatograph with headspace autosampler (HS-GC-MS/MS) was elaborated in this study. Application of the elaborated procedure resulted in a limit of detection of 0.021μgkg(-1) and a limit of quantification of 0.071μgkg(-1). The mean recoveries during in-house validation ranged from 89% to 109%, and coefficients of variation for repeatability ranged from 4% to 11%. The proposed analytical method was applied for monitoring the furan content of 30 commercial baby food samples available on the Latvian retail market. The level of furan found in these samples varied from 0.45 to 81.9μgkg(-1), indicating that infants whose sole diet comprises baby food sold in jars and cans are exposed constantly to furan. Samples containing vegetables and meat had higher levels of furan than those containing only fruits. Copyright © 2016 Elsevier Ltd. All rights reserved.

  17. Performance evaluation of a thermal desorption/gas chromatographic/mass spectrometric method for the characterization of waste tank headspace samples

    International Nuclear Information System (INIS)

    Ma, C.Y.; Skeen, J.T.; Dindal, A.B.; Bayne, C.K.; Jenkins, R.A.

    1997-01-01

    A thermal desorption/gas chromatography/mass spectrometry (TD/GC/MS) method was validated for the determination of volatile organic compounds collected on carbonaceous triple sorbent traps and applied to characterize samples of headspace gases collected from underground nuclear waste storage tanks at the U.S. Department of Energy's Hanford site, in Richland, WA. Method validation used vapor-phase standards generated from 25 target analytes, including alkanes, alkyl alcohols, alkyl ketones, alkylated aromatics, and alkyl nitriles. The target analytes represent a group of compounds identified in one of the most problematic tanks. TD/GC/MS was carried out with modified injectors. Performance was characterized based on desorption efficiency, reproducibility, stability, and linearity of the calibration, method detection limits, preanalytical holding time, and quality control limits for surrogate standard recoveries. Desorption efficiencies were all greater than 82%, and the majority of the analytes (23 out of 25) had reproducibility values less than 24% near the method detection levels. The method was applied to the analysis of a total of 305 samples collected from the headspaces of 48 underground waste storge tanks. Quality control procedures were implemented to monitor sampling and TD/GC/MS method. 33 refs., 2 figs., 4 tabs

  18. Application of enhanced gas chromatography/triple quadrupole mass spectrometry for monitoring petroleum weathering and forensic source fingerprinting in samples impacted by the Deepwater Horizon oil spill.

    Science.gov (United States)

    Adhikari, Puspa L; Wong, Roberto L; Overton, Edward B

    2017-10-01

    Accurate characterization of petroleum hydrocarbons in complex and weathered oil residues is analytically challenging. This is primarily due to chemical compositional complexity of both the oil residues and environmental matrices, and the lack of instrumental selectivity due to co-elution of interferences with the target analytes. To overcome these analytical selectivity issues, we used an enhanced resolution gas chromatography coupled with triple quadrupole mass spectrometry in Multiple Reaction Monitoring (MRM) mode (GC/MS/MS-MRM) to eliminate interferences within the ion chromatograms of target analytes found in environmental samples. This new GC/MS/MS-MRM method was developed and used for forensic fingerprinting of deep-water and marsh sediment samples containing oily residues from the Deepwater Horizon oil spill. The results showed that the GC/MS/MS-MRM method increases selectivity, eliminates interferences, and provides more accurate quantitation and characterization of trace levels of alkyl-PAHs and biomarker compounds, from weathered oil residues in complex sample matrices. The higher selectivity of the new method, even at low detection limits, provides greater insights on isomer and homolog compositional patterns and the extent of oil weathering under various environmental conditions. The method also provides flat chromatographic baselines for accurate and unambiguous calculation of petroleum forensic biomarker compound ratios. Thus, this GC/MS/MS-MRM method can be a reliable analytical strategy for more accurate and selective trace level analyses in petroleum forensic studies, and for tacking continuous weathering of oil residues. Copyright © 2017 Elsevier Ltd. All rights reserved.

  19. Determination of the Three Main Components of the Grapevine Moth Pest Pheromone in Grape-Related Samples by Headspace-Gas Chromatography-Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    María del Carmen Alcudia-León

    2017-10-01

    Full Text Available The grapevine moth (Lobesia botrana is the most significant pest of viticulture. This article reports the development of an analytical method that allows the instrumental determination of the three main pheromone components of the pest ((E,Z-7,9-dodecadien-1-yl acetate, (E,Z-7,9-dodecadien-1-ol and (Z-9-dodecen-1-yl acetate in grape-related samples (must, table grape and wine grape. The combination of headspace, gas chromatography and mass spectrometry provides limits of detection in the range of 60–420 ng/Kg and precision, expressed as a relative standard deviation, better than 8.5%. This analytical approach is rapid and simple and opens a door to the study of the pest incidence on the final products.

  20. Naphthalene, a polycyclic aromatic hydrocarbon, in the fish samples from the Bangsai river of Bangladesh by gas chromatograph–mass spectrometry

    Directory of Open Access Journals (Sweden)

    M. Amzad Hossain

    2014-12-01

    Full Text Available Naphthalene, a polycyclic aromatic hydrocarbon (PAH, was detected and quantified in the selected varieties of fishes collected from the Bangsai river, one of the contaminated rivers located at Savar near the Dhaka Export Processing Zone (DEPZ, Bangladesh, during the period October 2009. Naphthalene, a carcinogenic compound, was analyzed by GC–MS as it was in the mixture of dichloromethane–hexane (1:1 crude extract of the flesh of fish samples collected from the aforesaid river. A suitable and reliable procedure for the extraction of naphthalene from the fish sample has been developed. A multi-layer clean-up (silica gel column was used, followed by glass fiber filter (GFF paper to eliminate the interfering organic compounds as well as the lipids and fat. It was observed that PAHs deposition on the samples takes place in different morphological parts of the biological materials. The PAH, naphthalene, was found in almost all of the fish samples and the concentration of which was in the range 0.030–1.004 μg/g. Recovery studies with fortified samples indicated that the recovery efficiency for naphthalene was about 79.14%. This concentration is within the range of values reported for other comparable regions of the world.

  1. Monitoring radioactive contamination in food, water sediments and other environmental samples in Egypt. Final report for the period 1 October 1992 - 31 July 1996

    International Nuclear Information System (INIS)

    Farouk, M.

    1996-09-01

    A detailed survey for radioactivity content was carried out in the following materials: 1) Raw (from quarries) and finished (e.g., bricks, cement, ceramic tiles) building materials originating in central Egypt; 2) soils and plants (particularly cattle fodder) in upper Egypt, including soil to plant transfer factors; 3) water, bottom sediments and shore sediments from Lake Nasser and its immediate surroundings; 4) water, fish, bottom and shore sediments from the Lake Quaran region; 5) soil, plant, drinking water, bottom and shore sediments from the Sinai Peninsula. The concentrations of the following radionuclides were measured: K-40, Cs-137, Ra-226, Th-232 and U-238. Samples were sealed in Marinelli beakers for 4 weeks to allow complete ingrowth of Rn-222 and daughters. High resolution gamma-ray spectrometry was used to measure K-40 and Cs-137 directly and Ra-226, Th-232 and U-238 indirectly by means of daughter radioactivities. In addition, uranium measurements were also made after chemical decomposition of selected samples by laser fluorimetry and by alpha spectrometry techniques. The results were used for establishing a database of baseline radioactivity levels, for evaluating average doses to the population, for comparison with similar materials from other countries and for determining soil to plant transfer factors which can be used to estimate internal doses to the population. (author). Refs, figs, tabs

  2. Quantification of 4-hydroxy-2,5-dimethyl-3-furanone in fruit samples using solid phase microextraction coupled with gas chromatography-mass spectrometry.

    Science.gov (United States)

    Chen, Yong; Sidisky, Leonard M

    2011-09-23

    Furaneol is an important aroma compound. It is very difficult to extract furaneol from food matrices and separate it on a gas chromatography column due to its high polarity and instability. A new quantitative method was developed to quantify furaneol in aqueous samples by the use of derivatization/solid phase microextraction (SPME) coupled with gas chromatography/mass spectrometry (GC/MS). The derivatization was carried out by reacting pentafluorobenzyl bromide with furaneol in basic solutions at elevated temperatures. The derivative was stable and less polar so that SPME-GC/MS could be applied for extraction, separation and detection. The automated analytical method had a limit of detection (LOD) of 0.5 ng mL(-1), a limit of quantification (LOQ) of 2 ng mL(-1), a repeatability of 9.5%, and a linear range from 2 to 500 ng mL(-1). The method was applied to analyze fruit samples. And it was found that the concentrations of furaneol in tomato ranged from 95 to 173 μg kg(-1), in strawberries ranged from 1663 to 4852 μg kg(-1). The results were verified with a LC procedure. To facilitate analytical method development, some physico-chemical parameters for furaneol were determined in this work. Its solubility in water was determined as 0.315 g mL(-1) (25°C). Its LogD in water and LogP in 0.1 M phosphate buffer were -0.133 and 0.95 (20 °C), respectively. Its pKa was 8.56 (20 °C). Copyright © 2011 Elsevier B.V. All rights reserved.

  3. Implementation of electrochemical, optical and denuder-based sensors and sampling techniques on UAV for volcanic gas measurements: examples from Masaya, Turrialba and Stromboli volcanoes

    Science.gov (United States)

    Rüdiger, Julian; Tirpitz, Jan-Lukas; Maarten de Moor, J.; Bobrowski, Nicole; Gutmann, Alexandra; Liuzzo, Marco; Ibarra, Martha; Hoffmann, Thorsten

    2018-04-01

    Volcanoes are a natural source of several reactive gases (e.g., sulfur and halogen containing species) and nonreactive gases (e.g., carbon dioxide) to the atmosphere. The relative abundance of carbon and sulfur in volcanic gas as well as the total sulfur dioxide emission rate from a volcanic vent are established parameters in current volcano-monitoring strategies, and they oftentimes allow insights into subsurface processes. However, chemical reactions involving halogens are thought to have local to regional impact on the atmospheric chemistry around passively degassing volcanoes. In this study we demonstrate the successful deployment of a multirotor UAV (quadcopter) system with custom-made lightweight payloads for the compositional analysis and gas flux estimation of volcanic plumes. The various applications and their potential are presented and discussed in example studies at three volcanoes encompassing flight heights of 450 to 3300 m and various states of volcanic activity. Field applications were performed at Stromboli volcano (Italy), Turrialba volcano (Costa Rica) and Masaya volcano (Nicaragua). Two in situ gas-measuring systems adapted for autonomous airborne measurements, based on electrochemical and optical detection principles, as well as an airborne sampling unit, are introduced. We show volcanic gas composition results including abundances of CO2, SO2 and halogen species. The new instrumental setups were compared with established instruments during ground-based measurements at Masaya volcano, which resulted in CO2 / SO2 ratios of 3.6 ± 0.4. For total SO2 flux estimations a small differential optical absorption spectroscopy (DOAS) system measured SO2 column amounts on transversal flights below the plume at Turrialba volcano, giving 1776 ± 1108 T d-1 and 1616 ± 1007 T d-1 of SO2 during two traverses. At Stromboli volcano, elevated CO2 / SO2 ratios were observed at spatial and temporal proximity to explosions by airborne in situ measurements. Reactive

  4. Implementation of electrochemical, optical and denuder-based sensors and sampling techniques on UAV for volcanic gas measurements: examples from Masaya, Turrialba and Stromboli volcanoes

    Directory of Open Access Journals (Sweden)

    J. Rüdiger

    2018-04-01

    Full Text Available Volcanoes are a natural source of several reactive gases (e.g., sulfur and halogen containing species and nonreactive gases (e.g., carbon dioxide to the atmosphere. The relative abundance of carbon and sulfur in volcanic gas as well as the total sulfur dioxide emission rate from a volcanic vent are established parameters in current volcano-monitoring strategies, and they oftentimes allow insights into subsurface processes. However, chemical reactions involving halogens are thought to have local to regional impact on the atmospheric chemistry around passively degassing volcanoes. In this study we demonstrate the successful deployment of a multirotor UAV (quadcopter system with custom-made lightweight payloads for the compositional analysis and gas flux estimation of volcanic plumes. The various applications and their potential are presented and discussed in example studies at three volcanoes encompassing flight heights of 450 to 3300 m and various states of volcanic activity. Field applications were performed at Stromboli volcano (Italy, Turrialba volcano (Costa Rica and Masaya volcano (Nicaragua. Two in situ gas-measuring systems adapted for autonomous airborne measurements, based on electrochemical and optical detection principles, as well as an airborne sampling unit, are introduced. We show volcanic gas composition results including abundances of CO2, SO2 and halogen species. The new instrumental setups were compared with established instruments during ground-based measurements at Masaya volcano, which resulted in CO2 ∕ SO2 ratios of 3.6 ± 0.4. For total SO2 flux estimations a small differential optical absorption spectroscopy (DOAS system measured SO2 column amounts on transversal flights below the plume at Turrialba volcano, giving 1776 ± 1108 T d−1 and 1616 ± 1007 T d−1 of SO2 during two traverses. At Stromboli volcano, elevated CO2 ∕ SO2 ratios were observed at spatial and temporal proximity

  5. Correction of estimates of retention in care among a cohort of HIV-positive patients in Uganda in the period before starting ART: a sampling-based approach.

    Science.gov (United States)

    Nyakato, Patience; Kiragga, Agnes N; Kambugu, Andrew; Bradley, John; Baisley, Kathy

    2018-04-20

    The aim of this study was to use a sampling-based approach to obtain estimates of retention in HIV care before initiation of antiretroviral treatment (ART), corrected for outcomes in patients who were lost according to clinic registers. Retrospective cohort study of HIV-positive individuals not yet eligible for ART (CD4 >500). Three urban and three rural HIV care clinics in Uganda; information was extracted from the clinic registers for all patients who had registered for pre-ART care between January and August 2015. A random sample of patients who were lost according to the clinic registers (>3 months late to scheduled visit) was traced to ascertain their outcomes. The proportion of patients lost from care was estimated using a competing risks approach, first based on the information in the clinic records alone and then using inverse probability weights to incorporate the results from tracing. Cox regression was used to determine factors associated with loss from care. Of 1153 patients registered for pre-ART care (68% women, median age 29 years, median CD4 count 645 cells/µL), 307 (27%) were lost according to clinic records. Among these, 195 (63%) were selected for tracing; outcomes were ascertained in 118 (61%). Seven patients (6%) had died, 40 (34%) were in care elsewhere and 71 (60%) were out of care. Loss from care at 9 months was 30.2% (95% CI 27.3% to 33.5%). After incorporating outcomes from tracing, loss from care decreased to 18.5% (95% CI 13.8% to 23.6%). Estimates of loss from HIV care may be too high if based on routine clinic data alone. A sampling-based approach is a feasible way of obtaining more accurate estimates of retention, accounting for transfers to other clinics. © Article author(s) (or their employer(s) unless otherwise stated in the text of the article) 2018. All rights reserved. No commercial use is permitted unless otherwise expressly granted.

  6. Approaches of aroma extraction dilution analysis (AEDA) for headspace solid phase microextraction and gas chromatography-olfactometry (HS-SPME-GC-O): Altering sample amount, diluting the sample or adjusting split ratio?

    Science.gov (United States)

    Feng, Yunzi; Cai, Yu; Sun-Waterhouse, Dongxiao; Cui, Chun; Su, Guowan; Lin, Lianzhu; Zhao, Mouming

    2015-11-15

    Aroma extract dilution analysis (AEDA) is widely used for the screening of aroma-active compounds in gas chromatography-olfactometry (GC-O). In this study, three aroma dilution methods, (I) using different test sample volumes, (II) diluting samples, and (III) adjusting the GC injector split ratio, were compared for the analysis of volatiles by using HS-SPME-AEDA. Results showed that adjusting the GC injector split ratio (III) was the most desirable approach, based on the linearity relationships between Ln (normalised peak area) and Ln (normalised flavour dilution factors). Thereafter this dilution method was applied in the analysis of aroma-active compounds in Japanese soy sauce and 36 key odorants were found in this study. The most intense aroma-active components in Japanese soy sauce were: ethyl 2-methylpropanoate, ethyl 2-methylbutanoate, ethyl 3-methylbutanoate, ethyl 4-methylpentanoate, 3-(methylthio)propanal, 1-octen-3-ol, 2-methoxyphenol, 4-ethyl-2-methoxyphenol, 2-methoxy-4-vinylphenol, 2-phenylethanol, and 4-hydroxy-5-ethyl-2-methyl-3(2H)-furanone. Copyright © 2015. Published by Elsevier Ltd.

  7. Practical and highly sensitive elemental analysis for aqueous samples containing metal impurities employing electrodeposition on indium-tin oxide film samples and laser-induced shock wave plasma in low-pressure helium gas.

    Science.gov (United States)

    Kurniawan, Koo Hendrik; Pardede, Marincan; Hedwig, Rinda; Abdulmadjid, Syahrun Nur; Lahna, Kurnia; Idris, Nasrullah; Jobiliong, Eric; Suyanto, Hery; Suliyanti, Maria Margaretha; Tjia, May On; Lie, Tjung Jie; Lie, Zener Sukra; Kurniawan, Davy Putra; Kagawa, Kiichiro

    2015-09-01

    We have conducted an experimental study exploring the possible application of laser-induced breakdown spectroscopy (LIBS) for practical and highly sensitive detection of metal impurities in water. The spectrochemical measurements were carried out by means of a 355 nm Nd-YAG laser within N2 and He gas at atmospheric pressures as high as 2 kPa. The aqueous samples were prepared as thin films deposited on indium-tin oxide (ITO) glass by an electrolysis process. The resulting emission spectra suggest that concentrations at parts per billion levels may be achieved for a variety of metal impurities, and it is hence potentially feasible for rapid inspection of water quality in the semiconductor and pharmaceutical industries, as well as for cooling water inspection for possible leakage of radioactivity in nuclear power plants. In view of its relative simplicity, this LIBS equipment offers a practical and less costly alternative to the standard use of inductively coupled plasma-mass spectrometry (ICP-MS) for water samples, and its further potential for in situ and mobile applications.

  8. Phylogenetic analysis of G1P[8] and G12P[8] rotavirus A samples obtained in the pre- and post-vaccine periods, and molecular modeling of VP4 and VP7 proteins.

    Science.gov (United States)

    Almeida, Tâmera Nunes Vieira; de Sousa, Teresinha Teixeira; da Silva, Roosevelt Alves; Fiaccadori, Fabíola Souza; Souza, Menira; Badr, Kareem Rady; de Paula Cardoso, Divina das Dôres

    2017-09-01

    Reduction in morbimortality rates for acute gastroenteritis (AGE) by Rotavirus A (RVA) has been observed after the introduction of vaccines, however the agent continues to circulate. The present study described the genomic characterization of the 11 dsRNA segments of two RVA samples G1P[8] obtained in the pre- and post-vaccination periods and one of G12P[8] sample (post-vaccine), compared to Rotarix™ vaccine. Analysis by molecular sequencing of the samples showed that the three samples belonged to genogroup I. In addition, the analysis of VP7 gene revealed that the samples G1 (pre-vaccine), G1 (post-vaccine) and G12 were characterized as lineages II, I and III, respectively. Regarding to VP4 and NSP4 gene it was observed that all samples belonged to lineage III, whereas for VP6 gene, the sample of the pre- and post-vaccine belonged to the lineage IV and I, respectively. Considering the VP7 gene, it was observed high nucleotide and amino acid identity for the two G1 samples when compared to Rotarix™ vaccine and lesser identity for the G12 sample. In relation to antigenic epitope of VP7 greater modifications were observed for the G12 sample in the 7-2 epitope that was confirmed by molecular modeling. On the other hand, for VP4, some changes in the 8-1 and 8-3 antigenic epitopes was observed for the three samples. This data could be interpreted as a low selective pressure exerted by vaccination in relation to G1P[8] samples and lesser protection in relation to G12P[8]. Thus, the continuous monitoring of RVA circulating samples remains important. Copyright © 2017 Elsevier B.V. All rights reserved.

  9. Determination of the analytical performance of a headspace capillary gas chromatographic technique and karl Fischer coulometric titration by system calibration using oil samples containing known amounts of moisture.

    Science.gov (United States)

    Jalbert, J; Gilbert, R; Tétreault, P

    1999-08-01

    Over the past few years, concerns have been raised in the literature about the accuracy of the Karl Fischer (KF) method for assessing moisture in transformer mineral oils. To better understand this issue, the performance of a static headspace capillary gas chromatographic (HS-CGC) technique was compared to that of KF coulometric titration by analyzing moisture in samples containing known amounts of water and various samples obtained from the National Institute of Standards and Technology (NIST). Two modes of adding samples into the KF vessel were used:  direct injection and indirect injection via an azeotropic distillation of the moisture with toluene. Under the conditions used for direct injection, the oil matrix was totally dissolved in the anolyte, which allowed the moisture to be titrated in a single-phase solution rather than in a suspension. The results have shown that when HS-CGC and combined azeotropic distillation/KF titration are calibrated with moisture-in-oil standards, a linear relation is observed over 0-60 ppm H(2)O with a correlation coefficient better than 0.9994 (95% confidence), with the regression line crossing through zero. A similar relation can also be observed when calibration is achieved by direct KF addition of standards prepared with octanol-1, but in this case an intercept of 4-5 ppm is noted. The amount of moisture determined by curve interpolation in NIST reference materials by the three calibrated systems ranges from 13.0 to 14.8 ppm for RM 8506 and 42.5 to 46.4 ppm for RM 8507, and in any case, the results were as high as those reported in the literature with volumetric KF titration. However, titration of various dehydrated oil and solvent samples showed that direct KF titration is affected by a small bias when samples contain very little moisture. The source of error after correction for the large sample volume used for the determination (8 mL) is about 6 ppm for Voltesso naphthenic oil and 4 ppm for toluene, revealing a matrix

  10. [Monitoring of the residue of fosthiazate in water samples using solid-phase extraction coupled with gas chromatography/mass spectrometry].

    Science.gov (United States)

    Zhu, Jing; Zhou, Xin; Fu, Chunmei; Liu, Sankang; Li, Zhangwan

    2004-11-01

    Solid-phase extraction (SPE) coupled with gas chromatography/mass spectrometry (GC/MS) was used to determine the fosthiazate residue in water samples. The water samples were first filtered through cellulose filters (0.45 microm pore size). A 100 mL volume of filtered water, in which 1 mL of methanol has been added, was then passed through a pre-conditioned 3 cm C18 cartridge at a flow-rate of 1.5 mL/min. Elution was performed by 1 mL of methanol. The eluant was finally dried under reduced pressure for solvent evaporation. The volume was quantitatively adjusted to 0.5 mL with methanol. The analysis was carried out on GC/MS. The mass spectrometer was operated in selected ion monitoring (SIM) mode. According to mass spectrum of fosthiazate, three selected ions at m/z of 126, 195, 283, respectively, were monitored for identification and quantification. High sensitivity and selectivity were achieved by using this method. The limit of detection for fosthiazate in water samples was determined to be 56.4 ng/L. The linearity was demonstrated over a wide range of concentrations covering from 0.282 to 141 microg/L. The recoveries were more than 85.5% and the relative standard deviations for the overall procedure were less than 4.42%. The fosthiazate residue was detected in the water samples from a pool near cropland where fosthiazate was used. The results demonstrate the suitability of the SPE-GC/MS approach for the analysis of fosthiazate in water.

  11. Assessment of the mobility of metals and semi-metals in Sepetiba Bay (Rio de Janeiro - Brazil) by analyzing sediments sampled in different periods

    International Nuclear Information System (INIS)

    Cortez, Vinicius D.; Ribeiro, Andreza P.; Figueiredo, Ana M.G.; Santos, Jose O.; Wassermann, Julio C.

    2005-01-01

    In the last three decades, Sepetiba bay, located about 60 km south of the city of Rio de Janeiro, Brazil, has been subjected to increasing pollution impacts. The Sepetiba region has undergone fast industrial expansion leading to high levels of pollution by metals. For the last two decades, an industrial park composed of about 400 industrial plants, basically metallurgical, was established in the Sepetiba Bay basin, releasing its effluents either straight into the bay or through local rivers. Potential toxic elements such as As, Zn, Cr, Pb and Cd have been introduced into the bay through industrial and domestic wastes. In the present paper, instrumental neutron activation analysis (INAA) was applied to determine the elements As, Cr and Zn in sediments from Sepetiba bay, sampled in August 2003, in order to compare to previous results obtained in 1998, for these elements, by Pellegatti et al. (2001). By using a geostatistical model it was possible to evaluate the spatial mobility of As, Cr and Zn in the last six years. The results obtained showed that none of the studied elements showed a significant spatial mobility. This behavior is probably related to geochemical barriers present in Sepetiba bay. (author)

  12. Simultaneous analysis of non-steroidal anti-inflammatory drugs and estrogenic hormones in water and wastewater samples using gas chromatography-mass spectrometry and gas chromatography with electron capture detection

    Energy Technology Data Exchange (ETDEWEB)

    Migowska, Natalia; Caban, Magda; Stepnowski, Piotr; Kumirska, Jolanta, E-mail: kumirska@chem.univ.gda.pl

    2012-12-15

    Non-steroidal anti-inflammatory drugs are the group of pharmaceuticals that is most often found in the environment, whereas estrogenic hormones are considered to be potent endocrine disruptors. However, the fate and persistence of these compounds in the environment are still unclear. In this study we propose two approaches for determining these compounds in environmental water samples: GC-MS using time windows and operating in selected ion-monitoring mode (SIM) and, for the first time, gas chromatography with electron capture detection (GC-ECD). The identification criteria of both methods fulfilled the requirements of Directive 2002/657/EC. The use of time windows improved the sensitivity of GC-MS measurements. In GC-MS analysis the pharmaceuticals were determined as trimethylsilyl, in GC-ECD as pentafluoropropionyl derivatives. The influence of such parameters as the type of reagent, type of solvent, reaction time, reaction temperature and microwave irradiation in a household microwave oven on the efficacy of silylation was investigated. Derivatization using N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) and 1% trimethylchlorosilane (TMCS) in pyridine (1:1, v/v) for 30 min in 60 Degree-Sign C was found to be optimal. Optimization of the solid phase extraction procedure (SPE) confirmed that the application of Oasis HLB cartridges, the acidification of loading samples to pH 2 and the use of methanol as eluent gave the best absolute recoveries (ARs) of the target compounds. The following ARs of all the compounds were achieved: 58.2-106.8% in influent wastewater, 77.8-103.4% in effluent wastewater and 81.2-101.9% in surface water samples. Validation of the SPE-GC-MS method enables 13 pharmaceuticals to be determined with MDLs between 3.3 and 343.6 ng/L, depending on the analytes and matrices. GC-ECD analysis enables the determination of 6 pharmaceuticals in surface water samples with MDLs between 0.7 and 5.4 ng/L. The proposed methods were successfully used for

  13. Simultaneous analysis of non-steroidal anti-inflammatory drugs and estrogenic hormones in water and wastewater samples using gas chromatography–mass spectrometry and gas chromatography with electron capture detection

    International Nuclear Information System (INIS)

    Migowska, Natalia; Caban, Magda; Stepnowski, Piotr; Kumirska, Jolanta

    2012-01-01

    Non-steroidal anti-inflammatory drugs are the group of pharmaceuticals that is most often found in the environment, whereas estrogenic hormones are considered to be potent endocrine disruptors. However, the fate and persistence of these compounds in the environment are still unclear. In this study we propose two approaches for determining these compounds in environmental water samples: GC–MS using time windows and operating in selected ion-monitoring mode (SIM) and, for the first time, gas chromatography with electron capture detection (GC–ECD). The identification criteria of both methods fulfilled the requirements of Directive 2002/657/EC. The use of time windows improved the sensitivity of GC–MS measurements. In GC–MS analysis the pharmaceuticals were determined as trimethylsilyl, in GC–ECD as pentafluoropropionyl derivatives. The influence of such parameters as the type of reagent, type of solvent, reaction time, reaction temperature and microwave irradiation in a household microwave oven on the efficacy of silylation was investigated. Derivatization using N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) and 1% trimethylchlorosilane (TMCS) in pyridine (1:1, v/v) for 30 min in 60 °C was found to be optimal. Optimization of the solid phase extraction procedure (SPE) confirmed that the application of Oasis HLB cartridges, the acidification of loading samples to pH 2 and the use of methanol as eluent gave the best absolute recoveries (ARs) of the target compounds. The following ARs of all the compounds were achieved: 58.2–106.8% in influent wastewater, 77.8–103.4% in effluent wastewater and 81.2–101.9% in surface water samples. Validation of the SPE–GC–MS method enables 13 pharmaceuticals to be determined with MDLs between 3.3 and 343.6 ng/L, depending on the analytes and matrices. GC–ECD analysis enables the determination of 6 pharmaceuticals in surface water samples with MDLs between 0.7 and 5.4 ng/L. The proposed methods were successfully

  14. Cork as a new (green) coating for solid-phase microextraction: determination of polycyclic aromatic hydrocarbons in water samples by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Dias, Adriana Neves; Simão, Vanessa; Merib, Josias; Carasek, Eduardo

    2013-04-15

    A new fiber for solid-phase microextraction (SPME) was prepared employing cork as a coating. The morphology and composition of the cork fiber was evaluated by scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR), respectively. The proposed fiber was used for the determination of polycyclic aromatic hydrocarbons (PAHs) in river water samples by gas chromatography-selected ion monitoring-mass spectrometry (GC-SIM-MS). A central composite design was used for optimization of the variables involved in the extraction of PAHs from water samples. The optimal extraction conditions were extraction time and temperature of 60 min and 80°C, respectively. The detection and quantification limits were 0.03 and 0.1 μg L(-1), respectively. The recovery values were between 70.2 and 103.2% and the RSD was ≤15.7 (n=3). The linear range was 0.1-10 μg L(-1) with r≥0.96 and the fiber-to-fiber reproducibility showed RSD≤18.6% (n=5). The efficiency of the cork fiber was compared with commercially available fibers and good results were achieved, demonstrating the applicability and great potential of cork as a coating for SPME. Copyright © 2013 Elsevier B.V. All rights reserved.

  15. Gas chromatographic determination of polycyclic aromatic hydrocarbons in water and smoked rice samples after solid-phase microextraction using multiwalled carbon nanotube loaded hollow fiber.

    Science.gov (United States)

    Matin, Amir Abbas; Biparva, Pourya; Gheshlaghi, Mohammad

    2014-12-29

    A novel solid-phase microextraction fiber was prepared based on multiwalled carbon nanotubes (MWCNTs) loaded on hollow fiber membrane pores. Stainless steel wire was used as unbreakable support. The major advantages of the proposed fiber are its (a) high reproducibility due to the uniform structure of the hollow fiber membranes, (b) high extraction capacity related to the porous structure of the hollow fiber and outstanding adsorptive characteristics of MWCNTs. The proposed fiber was applied for the microextraction of five representative polycyclic aromatic hydrocarbons (PAHs) from aqueous media (river and hubble-bubble water) and smoked rice samples followed by gas chromatographic determination. Analytical merits of the method, including high correlation coefficients [(0.9963-0.9992) and (0.9982-0.9999)] and low detection limits [(9.0-13.0ngL(-1)) and (40.0-150.0ngkg(-1))] for water and rice samples, respectively, made the proposed method suitable for the ultra-trace determination of PAHs. Copyright © 2014 Elsevier B.V. All rights reserved.

  16. Determination of desipramine in biological samples using liquid-liquid-liquid microextraction combined with in-syringe derivatization, gas chromatography, and nitrogen/phosphorus detection.

    Science.gov (United States)

    Saraji, Mohammad; Mehrafza, Narges; Bidgoli, Ali Akbar Hajialiakbari; Jafari, Mohammad Taghi

    2012-10-01

    A method was established for the determination of desipramine in biological samples using liquid-liquid-liquid microextraction followed by in-syringe derivatization and gas chromatography-nitrogen phosphorus detection. The extraction method was based on the use of two immiscible organic solvents. n-Dodecane was impregnated in the pores of the hollow fiber and methanol was placed inside the lumen of the fiber as the acceptor phase. Acetic anhydride was used as the reagent for the derivatization of the analyte inside the syringe barrel. Parameters that affect the extraction efficiency (composition of donor and acceptor phase, ionic strength, sample temperature, and extraction time) as well as derivatization efficiency (amount of acetic anhydride and reaction time and temperature) were investigated. The limit of detection was 0.02 μg/L with intra and interday RSDs of 2.6 and 7.7%, respectively. The linearity of the method was in the range of 0.2-20 μg/L (r(2) = 0.9986). The method was successfully applied to determine desipramine in human plasma and urine. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Determination of Three Organochlorine Pesticides in Aqueous Samples by Solid-Phase Extraction Based on Natural Nano Diatomite in Packed Syringe Coupled to Gas Chromatography-Mass Spectrometry.

    Science.gov (United States)

    Taghani, Abdollah; Goudarzi, Nasser; Bagherian, Ghadamali; Chamjangali, Mansour Arab

    2017-01-01

    A rapid, simple, and sensitive technique is proposed based on a miniaturized solid-phase extraction method named mictroextraction in a packed syringe coupled with gas chromatography-mass spectrometry for the preconcentration and determination of three organochlorine pesticides. These include hexachlorobenzene, heptachlor and aldrine in aqueous samples. For the first time, the natural nano diatomite is used a sorbent. Based on this technique, 6.0 mg of the nano sorbent is inserted in a syringe between two polypropylene frits. The analytes would be adsorbed on the solid phase, and would subsequently be eluted using organic solvents. The influence of some important parameters, such as the solution pH, type and volume of the organic desorption solvent, and amount of sorbent on the extraction efficiency of the selected pesticides, is investigated. The proposed method shows good linearity in the range of 0.1 - 40.0 μg L -1 , and at low limits of detection in the range of 0.02 - 0.13 μg L -1 using the selected ion-monitoring mode. The reproducibility of this method was found to be in the range of 3.5 - 11.1% for the understudied pesticides. In order to evaluate the matrix effect, the developed method is also applied to the preconcentration and determination of the selected pesticides in different water samples.

  18. Neonatal blood gas sampling methods

    African Journals Online (AJOL)

    You work in a regional neonatal intensive care unit. An 8-day-old ... The baby was born at 28 weeks' gestation with a birth weight of 1. 100 g. ... and arterial blood taken from indwelling arterial lines.2-4 However, even ... tal age of 48 - 72 hours.

  19. Periodicity in the BrO/SO2 molar ratios in the volcanic gas plume of Cotopaxi and its correlation with the Earth tides during the eruption in 2015

    Science.gov (United States)

    Dinger, Florian; Bobrowski, Nicole; Warnach, Simon; Bredemeyer, Stefan; Hidalgo, Silvana; Arellano, Santiago; Galle, Bo; Platt, Ulrich; Wagner, Thomas

    2018-03-01

    We evaluated NOVAC (Network for Observation of Volcanic and Atmospheric Change) gas emission data from the 2015 eruption of the Cotopaxi volcano (Ecuador) for BrO/SO2 molar ratios. The BrO/SO2 molar ratios were very small prior to the phreatomagmatic explosions in August 2015, significantly higher after the explosions, and continuously increasing until the end of the unrest period in December 2015. These observations together with similar findings in previous studies at other volcanoes (Mt. Etna, Nevado del Ruiz, Tungurahua) suggest a possible link between a drop in BrO/SO2 and a future explosion. In addition, the observed relatively high BrO/SO2 molar ratios after December 2015 imply that bromine degassed predominately after sulfur from the magmatic melt. Furthermore, statistical analysis of the data revealed a conspicuous periodic pattern with a periodicity of about 2 weeks in a 3-month time series. While the time series is too short to rule out a chance recurrence of transient geological or meteorological events as a possible origin for the periodic signal, we nevertheless took this observation as a motivation to examine the influence of natural forcings with periodicities of around 2 weeks on volcanic gas emissions. One strong aspirant with such a periodicity are the Earth tides, which are thus central in this study. We present the BrO/SO2 data, analyse the reliability of the periodic signal, discuss a possible meteorological or eruption-induced origin of this signal, and compare the signal with the theoretical ground surface displacement pattern caused by the Earth tides. Our central result is the observation of a significant correlation between the BrO/SO2 molar ratios with the north-south and vertical components of the calculated tide-induced surface displacement with correlation coefficients of 47 and 36 %, respectively. From all other investigated parameters, only the correlation between the BrO/SO2 molar ratios and the relative humidity in the local

  20. Periodicity in the BrO∕SO2 molar ratios in the volcanic gas plume of Cotopaxi and its correlation with the Earth tides during the eruption in 2015

    Directory of Open Access Journals (Sweden)

    F. Dinger

    2018-03-01

    Full Text Available We evaluated NOVAC (Network for Observation of Volcanic and Atmospheric Change gas emission data from the 2015 eruption of the Cotopaxi volcano (Ecuador for BrO∕SO2 molar ratios. The BrO∕SO2 molar ratios were very small prior to the phreatomagmatic explosions in August 2015, significantly higher after the explosions, and continuously increasing until the end of the unrest period in December 2015. These observations together with similar findings in previous studies at other volcanoes (Mt. Etna, Nevado del Ruiz, Tungurahua suggest a possible link between a drop in BrO∕SO2 and a future explosion. In addition, the observed relatively high BrO∕SO2 molar ratios after December 2015 imply that bromine degassed predominately after sulfur from the magmatic melt. Furthermore, statistical analysis of the data revealed a conspicuous periodic pattern with a periodicity of about 2 weeks in a 3-month time series. While the time series is too short to rule out a chance recurrence of transient geological or meteorological events as a possible origin for the periodic signal, we nevertheless took this observation as a motivation to examine the influence of natural forcings with periodicities of around 2 weeks on volcanic gas emissions. One strong aspirant with such a periodicity are the Earth tides, which are thus central in this study. We present the BrO∕SO2 data, analyse the reliability of the periodic signal, discuss a possible meteorological or eruption-induced origin of this signal, and compare the signal with the theoretical ground surface displacement pattern caused by the Earth tides. Our central result is the observation of a significant correlation between the BrO∕SO2 molar ratios with the north–south and vertical components of the calculated tide-induced surface displacement with correlation coefficients of 47 and 36 %, respectively. From all other investigated parameters, only the correlation between the BrO∕SO2 molar

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

    Science.gov (United States)

    Rüdiger, Julian; Bobrowski, Nicole; Hoffmann, Thorsten

    2015-04-01

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

  2. Determination of fragrance allergens in indoor air by active sampling followed by ultrasound-assisted solvent extraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Lamas, J Pablo; Sanchez-Prado, Lucia; Garcia-Jares, Carmen; Llompart, Maria

    2010-03-19

    Fragrances are ubiquitous pollutants in the environment, present in the most of household products, air fresheners, insecticides and cosmetics. Commercial perfumes may contain hundreds of individual fragrance chemicals. In addition to the widespread use and exposure to fragranced products, many of the raw fragrance materials have limited available health and safety data. Because of their nature as artificial fragrances, inhalation should be considered as an important exposure pathway, especially in indoor environments. In this work, a very simple, fast, and sensitive methodology for the analysis of 24 fragrance allergens in indoor air is presented. Considered compounds include those regulated by the EU Directive, excluding limonene; methyl eugenol was also included due to its toxicity. The proposed methodology is based on the use of a very low amount of adsorbent to retain the target compounds, and the rapid ultrasound-assisted solvent extraction (UAE) using a very low volume of solvent which avoids further extract concentration. Quantification was performed by gas chromatography coupled to mass spectrometry (GC-MS). The influence of main factors involved in the UAE step (type of adsorbent and solvent, solvent volume and extraction time) was studied using an experimental design approach to account for possible factor interactions. Using the optimized procedure, 0.2 m(-3) air are sampled, analytes are retained on 25 mg Florisil, from which they are extracted by UAE (5 min) with 2 mL ethyl acetate. Linearity was demonstrated in a wide concentration range. Efficiency of the total sampling-extraction process was studied at several concentration levels (1, 5 and 125 microg m(-3)), obtaining quantitative recoveries, and good precision (RSD<10%). Method detection limits were < or =0.6 microg m(-3). Finally, the proposed method was applied to real samples collected in indoor environments in which several of the target compounds were determined. Copyright 2010 Elsevier B

  3. [Magnetic solid phase extraction combined with gas chromatography-flame photometric detection for the determination of organophosphorus pesticides in juice samples].

    Science.gov (United States)

    Huang, Qian; He, Man; Chen, Beibei; Hu, Bin

    2014-10-01

    A novel method for the determination of organophosphorous pesticides (OPPs) in fresh juice samples was developed. Fe3O4 @ P (St-co-MAA) magnetic microparticles were synthesized and modified with styrene (St) and methacrylic acid (MAA) by coating St and MAA on magnetic particles and characterized by a series of techniques. The results indicated that Fe3 O4 magnetic nanoparticles (MNPs) have been successfully modified with St and MAA. Based on the prepared FeO4 @ P (St-co-MAA) magnetic microparticles, a novel method of magnetic solid phase extraction (MSPE)-gas chromatography (GC)-flame photometric detection (FPD) was developed for the determination of OPPs. The extraction/desorption conditions of MSPE were optimized, and the analytical performance was evaluated under the optimal conditions. The limits of detection (LODs, S/N = 3) for target OPPs were in the range of 0.013-0.305 μg/L with the RSDs (n = 7) ranging from 3.1% to 8.8%. The enrichment factors varied from 406 to 951. The linear ranges were over three orders of magnitudes (R2 > 0.99) and the reproducibilities were 7.4%-14.5% (n = 5). Finally, the proposed MSPE-GC-FPD method was successfully applied to the analysis of the five OPPs in fresh tomato and strawberry juice samples, with the recoveries of target OPPs in the range of 85.4%-118.9% for the spiked samples. The proposed MSPE-GC-FPD method is featured with low cost, fast separation and high enrichment factor.

  4. Chlorinated paraffin analysis by gas chromatography Orbitrap high-resolution mass spectrometry: Method performance, investigation of possible interferences and analysis of fish samples.

    Science.gov (United States)

    Krätschmer, Kerstin; Cojocariu, Cristian; Schächtele, Alexander; Malisch, Rainer; Vetter, Walter

    2018-03-02

    For decades, high quantities of short-chain chlorinated paraffins (SCCP) and medium-chain chlorinated paraffins (MCCP) have been widely used, for instance as plasticizers or flame retardants, leading to global pollution due to unintentional emissions from products or waste. Due to the high complexity of chlorinated paraffins with several thousand congeners there is no consensus on an analytical procedure for SCCPs and MCCPs in food samples. Amongst the multitude of methods currently in use, high-resolution mass spectrometry is particularly valuable for in-depth studies of homologue patterns. Here we analyse SCCPs and MCCPs with gas chromatography coupled to high-resolution Orbitrap mass spectrometry (GC-Orbitrap-HRMS) operated in full-scan acquisition in electron capture negative ion (ECNI) mode at 60,000 and 120,000 resolution (FWHM, m/z 200, equals roughly 30,000 and 60,000 at 5% peak height). Linear dynamic range, selectivity and sensitivity tests confirmed an excellent linearity in a concentration range of 25-15,000 pg/μL with very low limits of detection (LODs) in the low pg/μL range. Spiking experiments with high levels of native mono- and di-ortho-polychlorinated biphenyls (PCBs) and mixtures of MCCP and SCCP standards did not have a negative impact on isotope ratios of the examined homologues. Besides the [M-Cl] - fragment ions used for quantification, the mass spectra of homologues also featured [M-HCl] - ions whose abundance increased with decreasing chlorination degree. In addition, [M-HCl-Cl] - ions were detected with a relative abundance of 5-10%. Three salmon (Salmo salar) samples farmed in Norway showed a consistent CP homologue pattern which differed both from the CP pattern in a sample from Scottish aquaculture and a wild salmon sample. These measurements produce evidence that discretely different CP patterns may exist in different areas of origin. Our results demonstrate that GC/ECNI-Orbitrap-HRMS is well-suited for the analysis of CPs by

  5. Comments on “innovative method for carbon dioxide determination in human postmortem cardiac gas samples using headspace-gas chromatography–mass spectrometry and stable labeled isotope as internal standard” by Varlet et al

    Energy Technology Data Exchange (ETDEWEB)

    Saffaj, T., E-mail: taoufiq.saffaj@usmba.ac.ma [Centre Universitaire Régional d’Interface, Université Sidi Mohamed Ben Abdellah, BP 2626, route d’Imouzzer, Fes Morocco (Morocco); Laboratoire de Chimie Organique Appliquée, Faculté des Sciences et Techniques, BP 2202, route d’Imouzzer, Fes Morocco (Morocco); Ihssane, B. [Laboratoire de Chimie Organique Appliquée, Faculté des Sciences et Techniques, BP 2202, route d’Imouzzer, Fes Morocco (Morocco)

    2014-01-31

    Graphical abstract: -- Highlights: •We comment on the validation results of the method for CO{sub 2} analysis in cardiac samples. •We demonstrate that the total error of the method exceeds the acceptance limits. •We show that the method is not valid according to the new SFSTP guideline. -- Abstract: Varlet et al. recently proposed a headspace-gas chromatography–mass spectrometry (HS-GC–MS) method applicable for the routine determination of CO{sub 2} in gaseous biologic matrices. This developed bioanalytical method was fully validated according to the SFSTP 1997 guidelines using the accuracy profile as a graphical decision-making tool.In this letter, we discuss the validity of HS-GC–MS method based on the newest SFSTP guideline. In particular, we demonstrate by the estimation of the β-expectation tolerance interval that the error total exceeds the acceptance limits (30%) for the second concentration level (0.5 μmol mL{sup −1} vial HS). Furthermore, we show through the risk profile that the probability to have future results inside the ±30% acceptance limits is smaller than 95%.

  6. Cork as a new (green) coating for solid-phase microextraction: Determination of polycyclic aromatic hydrocarbons in water samples by gas chromatography–mass spectrometry

    International Nuclear Information System (INIS)

    Dias, Adriana Neves; Simão, Vanessa; Merib, Josias; Carasek, Eduardo

    2013-01-01

    Highlights: ► Cork as a new coating for solid-phase microextraction was proposed. ► Good results were achieved, demonstrating the applicability of the cork as coating for SPME. ► The efficiency of cork fiber was very similar to commercially available fibers. -- Abstract: A new fiber for solid-phase microextraction (SPME) was prepared employing cork as a coating. The morphology and composition of the cork fiber was evaluated by scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR), respectively. The proposed fiber was used for the determination of polycyclic aromatic hydrocarbons (PAHs) in river water samples by gas chromatography–selected ion monitoring–mass spectrometry (GC–SIM–MS). A central composite design was used for optimization of the variables involved in the extraction of PAHs from water samples. The optimal extraction conditions were extraction time and temperature of 60 min and 80 °C, respectively. The detection and quantification limits were 0.03 and 0.1 μg L −1 , respectively. The recovery values were between 70.2 and 103.2% and the RSD was ≤15.7 (n = 3). The linear range was 0.1–10 μg L −1 with r ≥ 0.96 and the fiber-to-fiber reproducibility showed RSD ≤ 18.6% (n = 5). The efficiency of the cork fiber was compared with commercially available fibers and good results were achieved, demonstrating the applicability and great potential of cork as a coating for SPME

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

    International Nuclear Information System (INIS)

    Habibi, Azza

    2015-01-01

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

  8. Separation and preconcentration of 2,3,7,8-tetrachlorodibenzo-p-dioxin in blood samples by inclusion emulsion membranes and its determination by gas chromatography.

    Science.gov (United States)

    Mokhtari, Bahram; Pourabdollah, Kobra

    2012-10-15

    The nano-mediated preconcentration of 2,3,7,8-tetrachlorodibenzo-p-dioxin from blood samples was reported by inclusion-facilitated emulsion liquid membrane process. The novelty of this study was application of nano-baskets of calixarene and emulsion liquid membranes in selective and efficient preconcentration of 2,3,7,8-tetrachlorodibenzo-p-dioxin. For this aim, four derivatives of p-tert-calix[4]arene bearing different sulfonamide moieties were synthesized and their inclusion-extraction parameters were optimized including calixarenes' scaffold and concentration (3, 4 wt%), diluent type in membrane, phase and treat ratios (0.8 and 0.3), mixing speed (300 rpm), and initial solute concentrations (0.1-10 pg g(-1)). The extraction efficiency was determined by dioxin's concentration using gas chromatography equipped with electron capture detector and the results revealed that in optimized operating conditions, the preconcentration of 2,3,7,8-tetrachlorodibenzo-p-dioxin was improved and the limit of detection decreased. Copyright © 2012 Elsevier B.V. All rights reserved.

  9. Data on the densification during sintering of binder jet printed samples made from water- and gas-atomized alloy 625 powders

    Directory of Open Access Journals (Sweden)

    Amir Mostafaei

    2017-02-01

    Full Text Available Binder jet printing (BJP is a metal additive manufacturing method that manufactures parts with complex geometry by depositing powder layer-by-layer, selectively joining particles in each layer with a polymeric binder and finally curing the binder. After the printing process, the parts still in the powder bed must be sintered to achieve full densification (A. Mostafaei, Y. Behnamian, Y.L. Krimer, E.L. Stevens, J.L. Luo, M. Chmielus, 2016; A. Mostafaei, E. Stevens, E. Hughes, S. Biery, C. Hilla, M. Chmielus, 2016; A. Mostafaei, Y. Behnamian, Y.L. Krimer, E.L. Stevens, J.L. Luo, M. Chmielus, 2016 [1–3]. The collected data presents the characterization of the as-received gas- and water-atomized alloy 625 powders, BJP processing parameters and density of the sintered samples. The effect of sintering temperatures on the microstructure and the relative density of binder jet printed parts made from differently atomized nickel-based superalloy 625 powders are briefly compared in this paper. Detailed data can be found in the original published papers by authors in (A. Mostafaei, J. Toman, E.L. Stevens, E.T. Hughes, Y.L. Krimer, M. Chmielus, 2017 [4].

  10. A solid-phase microextraction-gas chromatographic approach combined with triple quadrupole mass spectrometry for the assay of carbamate pesticides in water samples.

    Science.gov (United States)

    Cavaliere, Brunella; Monteleone, Marcello; Naccarato, Attilio; Sindona, Giovanni; Tagarelli, Antonio

    2012-09-28

    A simple and sensitive method was developed for the quantification of five carbamate pesticides in water samples using solid phase microextraction (SPME) combined with gas chromatography-triple quadrupole mass spectrometry (GC-QqQ-MS). The performance of five SPME fibers was tested in univariate mode whereas the other variables affecting the efficiency of SPME analysis were optimized by the multivariate approach of design of experiment (DoE) and, in particular, a central composite design (CCD) was applied. The optimum working conditions in terms of response values were achieved by performing analysis with polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber in immersion mode for 45min at room temperature with addition of NaCl (10%). The multivariate chemometric approach was also used to explore the chromatographic behavior of the carbamates and to evaluate the importance of each variable investigated. An overall appraisement of results shows that the factor which gave a statistically significant effect on the response was only the injection temperature. Identification and quantification of carbamates was performed by using a gas chromatography-triple quadrupole mass spectrometry (GC-QqQ-MS) system in multiple reaction monitoring (MRM) acquisition. Since the choice of internal standard represented a crucial step in the development of method to achieve good reproducibility and robustness for the entire analytical protocol, three compounds (2,3,5-trimethacarb, 4-bromo-3,5-dimethylphenyl-n-methylcarbamate (BDMC) and carbaryl-d7) were evaluated as internal standards. Both precision and accuracy of the proposed protocol tested at concentration of 0.08, 5 and 3 μg l⁻¹ offered values ranging from 70.8% and 115.7% (except for carbaryl at 3 μg l⁻¹) and from 1.0% and 9.0% for accuracy and precision, respectively. Moreover, LOD and LOQ values ranging from 0.04 to 1.7 ng l⁻¹ and from 0.64 to 2.9 ng l⁻¹, respectively, can be considered very satisfactory. Copyright

  11. Problem Periods

    Science.gov (United States)

    ... ovary syndrome. Read our information on PCOS for teens , and see your doctor if you think you may have PCOS. Major weight loss. Girls who have anorexia will often stop having periods. When to see ...

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

    Science.gov (United States)

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

    2017-05-15

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

  13. Gas and Gas Pains

    Science.gov (United States)

    ... to produce gas. Often, relatively simple changes in eating habits can lessen bothersome gas. Certain digestive system disorders, ... such as soda and beer, increase stomach gas. Eating habits, such as eating too quickly, drinking through a ...

  14. Trace analysis of halogenated hydrocarbons in gaseous samples by on-line enrichment in an adsorption trap, on-column cold-trapping and capillary gas chromatography. I.Method and instrumentation

    NARCIS (Netherlands)

    Noij, T.H.M.; Fabian, P.; Borchers, R.; Janssen, F.; Cramers, C.A.M.G.; Rijks, J.A.

    1987-01-01

    A method is described for the determination of halocarbons in gaseous samples down to the ppt level (1:1012, v/v), consisting of successive on-line sub-ambient enrichment on an adsorbent, on-column cryofocusing, capillary gas chromatography and electron-capture detection. The quantitative aspects of

  15. Analysis of chemical warfare agents in organic liquid samples with magnetic dispersive solid phase extraction and gas chromatography mass spectrometry for verification of the chemical weapons convention.

    Science.gov (United States)

    Singh, Varoon; Purohit, Ajay Kumar; Chinthakindi, Sridhar; Goud, Raghavender D; Tak, Vijay; Pardasani, Deepak; Shrivastava, Anchal Roy; Dubey, Devendra Kumar

    2016-05-27

    A simple, sensitive and low temperature sample preparation method is developed for detection and identification of Chemical Warfare Agents (CWAs) and scheduled esters in organic liquid using magnetic dispersive solid phase extraction (MDSPE) followed by gas chromatography-mass spectrometry analysis. The method utilizes Iron oxide@Poly(methacrylic acid-co-ethylene glycol dimethacrylate) resin (Fe2O3@Poly(MAA-co-EGDMA)) as sorbent. Variants of these sorbents were prepared by precipitation polymerization of methacrylic acid-co-ethylene glycol dimethacrylate (MAA-co-EGDMA) onto Fe2O3 nanoparticles. Fe2O3@poly(MAA-co-EGDMA) with 20% MAA showed highest recovery of analytes. Extractions were performed with magnetic microspheres by MDSPE. Parameters affecting the extraction efficiency were studied and optimized. Under the optimized conditions, method showed linearity in the range of 0.1-3.0μgmL(-1) (r(2)=0.9966-0.9987). The repeatability and reproducibility (relative standard deviations (RSDs) %) were in the range of 4.5-7.6% and 3.4-6.2% respectively for organophosphorous esters in dodecane. Limits of detection (S/N=3/1) and limit of quantification (S/N=10/1) were found to be in the range of 0.05-0.1μgmL(-1) and 0.1-0.12μgmL(-1) respectively in SIM mode for selected analytes. The method was successfully validated and applied to the extraction and identification of targeted analytes from three different organic liquids i.e. n-hexane, dodecane and silicon oil. Recoveries ranged from 58.7 to 97.3% and 53.8 to 95.5% at 3μgmL(-1) and 1μgmL(-1) spiking concentrations. Detection of diethyl methylphosphonate (DEMP) and O-Ethyl S-2-diisopropylaminoethyl methylphosphonothiolate (VX) in samples provided by the Organization for Prohibition of Chemical Weapons Proficiency Test (OPCW-PT) proved the utility of the developed method for the off-site analysis of CWC relevant chemicals. Copyright © 2016 Elsevier B.V. All rights reserved.

  16. Granular Gas in a Periodic Lattice

    Science.gov (United States)

    Dorbolo, S.; Brandenbourger, M.; Damanet, F.; Dister, H.; Ludewig, F.; Terwagne, D.; Lumay, G.; Vandewalle, N.

    2011-01-01

    Glass beads are placed in the compartments of a horizontal square grid. This grid is then vertically shaken. According to the reduced acceleration [image omitted] of the system, the granular material exhibits various behaviours. By counting the number of beads in each compartment after shaking, it is possible to define three regimes. At low…

  17. A new system for the simultaneous measurement of δ{sup 13}C and δ{sup 15}N by IRMS and radiocarbon by AMS on gaseous samples: Design features and performances of the gas handling interface

    Energy Technology Data Exchange (ETDEWEB)

    Braione, Eugenia; Maruccio, Lucio; Quarta, Gianluca; D’Elia, Marisa; Calcagnile, Lucio, E-mail: lucio.calcagnile@unisalento.it

    2015-10-15

    We present the general design features and preliminary performances of a new system for the simultaneous AMS-{sup 14}C and IRMS δ{sup 13}C and δ{sup 15}N measurements on samples with masses in the μg range. The system consists of an elemental analyzer (EA), a gas splitting unit (GSU), a IRMS system, a gas handling interface (GHI) and a sputtering ion source capable of accepting gaseous samples. A detailed description of the system and of the control software supporting unattended operation are presented together with the first performance tests carried out by analyzing samples with masses ranging from 8 μgC to 2.4 mgC. The performances of the system were tested in term of stability of the ion beam extracted from the ion source, precision and accuracy of the results by comparing the measured isotopic ratios with those expected for reference materials.

  18. Radionuclides, Metals, and Hydrocarbons in Oil and Gas Operational Discharges and Environmental Samples Associated with Offshore Production Facilities on the Texas/Louisiana Continental Shelf with an Environmental Assessment of Metals and Hydrocarbons

    International Nuclear Information System (INIS)

    1997-06-01

    This report presents concentrations of radionuclides, metals, and hydrocarbons in samples of produced water and produced sand from oil and gas production platforms located offshore Texas and Louisiana. concentrations in produced water discharge plume / receiving water, ambient seawater, sediment, interstitial water, and marine animal tissue samples collected in the vicinity of discharging platforms and reference sites distant from discharges are also reported and discussed. An environmental risk assessment is made on the basis of the concentration of metals and hydrocarbons determined in the samples

  19. Radionuclides, Metals, and Hydrocarbons in Oil and Gas Operational Discharges and Environmental Samples Associated with Offshore Production Facilities on the Texas/Louisiana Continental Shelf with an Environmental Assessment of Metals and Hydrocarbons.

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1997-06-01

    This report presents concentrations of radionuclides, metals, and hydrocarbons in samples of produced water and produced sand from oil and gas production platforms located offshore Texas and Louisiana. concentrations in produced water discharge plume / receiving water, ambient seawater, sediment, interstitial water, and marine animal tissue samples collected in the vicinity of discharging platforms and reference sites distant from discharges are also reported and discussed. An environmental risk assessment is made on the basis of the concentration of metals and hydrocarbons determined in the samples.

  20. Radionuclides, Metals, and Hydrocarbons in Oil and Gas Operational Discharges and Environmental Samples Associated with Offshore Production Facilities on the Texas/Louisiana Continental Shelf with an Environmental Assessment of Metals and Hydrocarbons

    Energy Technology Data Exchange (ETDEWEB)

    Continental Shelf Associates, Inc.

    1999-08-16

    This report presents concentrations of radionuclides, metals, and hydrocarbons in samples of produced water and produced sand from oil and gas production platforms located offshore Texas and Louisiana. Concentrations in produced water discharge plume/receiving water, ambient seawater, sediment, interstitial water, and marine animal tissue samples collected in the vicinity of discharging platforms and reference sites distant from discharges are also reported and discussed. An environmental risk assessment is made on the basis of the concentrations of metals and hydrocarbons determined in the samples.

  1. SPENT NUCLEAR FUEL (SNF) PROJECT CANISTER STORAGE BUILDING (CSB) MULTI CANISTER OVERPACK (MCO) SAMPLING SYSTEM VALIDATION (OCRWM)

    International Nuclear Information System (INIS)

    BLACK, D.M.; KLEM, M.J.

    2003-01-01

    Approximately 400 Multi-canister overpacks (MCO) containing spent nuclear fuel are to be interim stored at the Canister Storage Building (CSB). Several MCOs (monitored MCOs) are designated to be gas sampled periodically at the CSB sampling/weld station (Bader 2002a). The monitoring program includes pressure, temperature and gas composition measurements of monitored MCOs during their first two years of interim storage at the CSB. The MCO sample cart (CART-001) is used at the sampling/weld station to measure the monitored MCO gas temperature and pressure, obtain gas samples for laboratory analysis and refill the monitored MCO with high purity helium as needed. The sample cart and support equipment were functionally and operationally tested and validated before sampling of the first monitored MCO (H-036). This report documents the results of validation testing using training MCO (TR-003) at the CSB. Another report (Bader 2002b) documents the sample results from gas sampling of the first monitored MCO (H-036). Validation testing of the MCO gas sampling system showed the equipment and procedure as originally constituted will satisfactorily sample the first monitored MCO. Subsequent system and procedural improvements will provide increased flexibility and reliability for future MCO gas sampling. The physical operation of the sampling equipment during testing provided evidence that theoretical correlation factors for extrapolating MCO gas composition from sample results are unnecessarily conservative. Empirically derived correlation factors showed adequate conservatism and support use of the sample system for ongoing monitored MCO sampling

  2. Monitoring gas quality green gas feeding in; Monitoring gaskwaliteit groengasinvoeding

    Energy Technology Data Exchange (ETDEWEB)

    Holstein, J. [DNV KEMA Energy and Sustainability, Arnhem (Netherlands); Polman, E. [Kiwa Technology, Apeldoorn (Netherlands)

    2013-04-15

    Due to the growing number of green gas facilities in the Netherlands more practical knowledge is collected about the production and injection of green gas. Also there was the need to gather data about more practical experiences and knowledge about the gas quality, the performance of gas cleaning and gas treatment systems, as well the integration of green gas in the gas infrastructure. In addition to this, there is a need to get insight in the safety aspects of green gas injection. In order to comply this demand, DNV KEMA en Kiwa Technology measured the quality parameters continuously between June 2012 en January 2013 (three weeks) and discontinuously (gas samples) of green gas at eight production facilities. The measurements have been performed at designated places and are independent from the measurements of the biomethane producer. In order to be sure that the results of DNV KEMA and Kiwa are comparable, a combined measurement program was executed. It results in uniformity for all the measured values: the differences are within the uncertainty level for each component. During the measurement period of three weeks, the gas quality parameters were compared to specifications, written down in the national regulations for the transport and the distribution grid respectively [Dutch] Door het groeiend aantal groengasinvoedingen in Nederland wordt steeds meer praktijkkennis verzameld. Er dient meer praktijkkennis te worden verzameld over de chemische gaskwaliteit, prestaties van de gasreiniging- en gasopwaardering en de wijze van inpassing in de bestaande infrastructuur. Daarnaast is het wenselijk om inzicht te verkrijgen in de veiligheid van groengasinvoeding. Daarop is de groengaskwaliteit op acht locaties over een periode van drie weken continu en discontinu gemeten tussen juni 2012 en januari 2013. De metingen zijn uitgevoerd op een aangewezen plaats door de netbeheerder en staan los van de metingen van de invoeders zelf. Voor het waarborgen van de uniformiteit van

  3. Variation in levels of serum inhibin B, testosterone, estradiol, luteinizing hormone, follicle-stimulating hormone, and sex hormone-binding globulin in monthly samples from healthy men during a 17-month period

    DEFF Research Database (Denmark)

    Andersson, Anna-Maria; Carlsen, Elisabeth; Petersen, Jørgen Holm

    2003-01-01

    To obtain information on the scale of the intraindividual variation in testicular hormone, blood samples for inhibin B determination were collected monthly in 27 healthy male volunteers during a 17-month period. In addition, the traditional reproductive hormones FSH, LH, testosterone, estradiol....... A seasonal variation was observed in LH and testosterone levels, but not in the levels of the other hormones. The seasonal variation in testosterone levels could be explained by the variation in LH levels. The seasonal variation in LH levels seemed to be related to the mean air temperature during the month...... levels in men. The peak levels of both LH and testosterone were observed during June-July, with minimum levels present during winter-early spring. Air temperature, rather than light exposure, seems to be a possible climatic variable explaining the seasonal variation in LH levels....

  4. Variability of matrix effects in liquid and gas chromatography - mass spectrometry analysis of pesticide residues after QuEChERS sample preparation of different food crops

    Science.gov (United States)

    Gas and liquid chromatography (GC and LC) coupled to sophisticated mass spectrometry (MS) instruments are among the most powerful analytical tools currently available to monitor pesticide residues in food, among other applications. However, both GC-MS and LC-MS are susceptible to matrix effects whi...

  5. Derivatisation/solid-phase microextraction followed by gas chromatography-mass spectrometry for the analysis of phenoxy acid herbicides in aqueous samples

    DEFF Research Database (Denmark)

    Nilsson, Torben; Baglio, Daniela; Galdo-Miguez, Isabel

    1998-01-01

    Different combinations of derivatisation and solid-phase microextraction followed by gas chromatography-mass spectrometry were optimised and evaluated for the analysis of phenoxy acid herbicides in water. The most successful derivatisation approach was aqueous-phase derivatisation with benzyl...

  6. 40 CFR 86.1310-2007 - Exhaust gas sampling and analytical system for gaseous emissions from heavy-duty diesel-fueled...

    Science.gov (United States)

    2010-07-01

    ... SAE Recommended Practice J1151, “Methane Measurement Using Gas Chromatography” (1994 SAE Handbook... the filter holder may be adapted, using sound engineering judgment and leak-free construction, to an... shows acceptable variation from the design in 40 CFR part 50, appendix L. Similar variations using sound...

  7. Liquid and gas chromatography coupled to isotope ratio mass spectrometry for the determination of 13C-valine isotopic ratios in complex biological samples

    NARCIS (Netherlands)

    Godin, Jean-Philippe; Breuillé, Denis; Obled, Christiane; Papet, Isabelle; Schierbeek, Henk; Hopfgartner, Gérard; Fay, Laurent-Bernard

    2008-01-01

    On-line gas chromatography-combustion-isotope ratio mass spectrometry (GC-C-IRMS) is commonly used to measure isotopic ratios at natural abundance as well as for tracer studies in nutritional and medical research. However, high-precision (13)C isotopic enrichment can also be measured by liquid

  8. State-of-the-art of NORM nuclide determination in samples from oil and gas production : Validation of potential standardization methods through an interlaboratory test programme

    NARCIS (Netherlands)

    Knaepen, WAI; Bergwerf, W; Lancee, PJF; vanDijk, W; Jansen, JFW; Janssen, RGC; Kiezenberg, WHT; vanSluijs, R; Tijsmans, MH; Voors, PI

    1995-01-01

    Gas and oil companies frequently encounter build-up of Naturally Occurring Radioactive Material (NORM) in their production and processing facilities. In the Netherlands NORM is subject to strict national regulations and, consequently, installations have to be screened on a regular basis. The

  9. The influence of moonlight and lunar periodicity on the efficacy of CDC light trap in sampling Phlebotomus (Larroussius) orientalis Parrot, 1936 and other Phlebotomus sandflies (Diptera: Psychodidae) in Ethiopia.

    Science.gov (United States)

    Gebresilassie, Araya; Yared, Solomon; Aklilu, Essayas; Kirstein, Oscar David; Moncaz, Aviad; Tekie, Habte; Balkew, Meshesha; Warburg, Alon; Hailu, Asrat; Gebre-Michael, Teshome

    2015-02-15

    Phlebotomus orientalis is the main sandfly vector of visceral leishmaniasis in the north and northwest of Ethiopia. CDC light traps and sticky traps are commonly used for monitoring sandfly populations. However, their trapping efficiency is greatly influenced by various environmental factors including moonlight and lunar periodicity. In view of that, the current study assessed the effect of moonlight and lunar periodicity on the performance of light traps in collecting P. orientalis. Trapping of P. orientalis and other Phlebotomus spp. was conducted for 7 months between December 2012 and June 2013 using CDC light traps and sticky traps from peri-domestic and agricultural fields. Throughout the trapping periods, collections of sandfly specimens were carried out for 4 nights per month, totaling 28 trapping nights that coincided with the four lunar phases (viz., first quarter, third quarter, new and full moon) distributed in each month. In total, 13,533 sandflies of eight Phlebotomus species (P. orientalis, P. bergeroti, P. rodhaini, P. duboscqi, P. papatasi, P. martini, P. lesleyae and P. heischi) were recorded. The predominant species was P. orientalis in both trapping sites and by both methods of collection in all lunar phases. A significant difference (P lunar phases. The highest mean number (231.13 ± 36.27 flies/trap/night) of P. orientalis was collected during the new moon phases, when the moonlight is absent. Fewer sandflies were attracted to light traps during a full moon. However, the number of P. orientalis and the other Phlebotomus spp. from sticky traps did not differ in their density among the four lunar phases (P = 0.122). Results of the current study demonstrated that the attraction and trapping efficiency of CDC light traps is largely influenced by the presence moonlight, especially during a full moon. Therefore, sampling of sandflies using light traps to estimate population density and other epidemiological studies in the field should take

  10. Argon cover gas purity control on LMFBR

    Energy Technology Data Exchange (ETDEWEB)

    Maeda, Hiroshi; Kobayashi, Takayoshi [PNC (Japan); Ishiyama, Satoshi [Toshiba (Japan); Motonaga, Tetsuji [Hitachi (Japan)

    1987-07-01

    Various control methods on chemical impurities and radioactive materials (fission products) in the primary argon gas of LMFBRs' have been studied based on experiences in Joyo and results of research and development. These results are reflected on MONJU design. On-line gas chromatographs are installed both in the Primary and in the Secondary Argon Gas Systems in JOYO. Also, chemical analysis has been done by batch sampling in JOYO. Though the rise of impurity concentration had been measured after periodical fuel exchange operation, impurity concentration has been controlled sufficiently under target control limits. In MONJU detailed design, the Rare Gas Removal and Recovery System which consisted of cryogenic distillation equipment had been eliminated and the capacity of Charcoal Beds in the Primary Argon Gas System has been improved to keep the concentration of radioactive materials sufficient low levels. The necessity to control the impurities in fresh argon gas which is supplied to the Primary Argon Gas System is now considered to keep the concentration of Kr and Xe isotopes in specified level, because their isotopes may make background rise for the Tagging Gas Failed Fuel Detection and Location System. Based on various investigations performed on sodium vapor trapping to obtain its detailed characteristics, design specifications and operating conditions of MONJU's Vapor Traps have been decided. To keep the level of radioactivity in gaseous effluents to the environment as low as reasonably achievable, the following means are now adopted in MONJU: the Primary Argon Gas System is composed of a closed recirculating path, but the exhaust gas discharged has different path after the Charcoal Beds; fresh argon gas is blown down to prevent Primary Argon Gas from releasing to the circumference during opening of the primary argon gas boundary, such as fuel exchange operations. (author)

  11. Development of a technique for the efficiency calibration of a HPGe detector for the off gas samples of a nuclear reactor

    International Nuclear Information System (INIS)

    Singh, Sarbjit; Agarwal, Chhavi; Ramaswami, A.; Manchanda, V.K.

    2007-01-01

    Regular monitoring of off gases released to the environment from a nuclear reactor is mandatory. The gaseous fission products are estimated by gamma ray spectrometry using a HPGe detector coupled to a multichannel analyser. In view of the lack of availability of gaseous fission products standards, an indirect method based on the charcoal absorption technique was developed for the efficiency calibration of HPGe detector system using 133B a and 152E u standards. The known activities of 133B a and 152E u are uniformly distributed in a vial having activated charcoal and counted on the HPGe detector system at liquid nitrogen temperature to determine the gamma ray efficiency for the vial having activated charcoal. The ratio of the gamma ray efficiencies of off gas present in the normal vial and the vial having activated charcoal at liquid nitrogen temperature are used to determine the gamma ray efficiency of off gas present in the normal vial. (author)

  12. Use of gas chromatography-olfactometry to identify key odorant compounds in dark chocolate. Comparison of samples before and after conching.

    Science.gov (United States)

    Counet, Christine; Callemien, Delphine; Ouwerx, Caroline; Collin, Sonia

    2002-04-10

    After vacuum distillation and liquid-liquid extraction, the volatile fractions of dark chocolates were analyzed by gas chromatography-olfactometry and gas chromatography-mass spectrometry. Aroma extract dilution analysis revealed the presence of 33 potent odorants in the neutral/basic fraction. Three of these had a strong chocolate flavor: 2-methylpropanal, 2-methylbutanal, and 3-methylbutanal. Many others were characterized by cocoa/praline-flavored/nutty/coffee notes: 2,3-dimethylpyrazine, trimethylpyrazine, tetramethylpyrazine, 3(or 2),5-dimethyl-2(or 3)-ethylpyrazine, 3,5(or 6)-diethyl-2-methylpyrazine, and furfurylpyrrole. Comparisons carried out before and after conching indicate that although no new key odorant is synthesized during the heating process, levels of 2-phenyl-5-methyl-2-hexenal, Furaneol, and branched pyrazines are significantly increased while most Strecker aldehydes are lost by evaporation.

  13. Liquid phase separation of proteins based on electrophoretic effects in an electrospray setup during sample introduction into a gas-phase electrophoretic mobility molecular analyzer (CE–GEMMA/CE–ES–DMA)

    Science.gov (United States)

    Weiss, Victor U.; Kerul, Lukas; Kallinger, Peter; Szymanski, Wladyslaw W.; Marchetti-Deschmann, Martina; Allmaier, Günter

    2014-01-01

    Nanoparticle characterization is gaining importance in food technology, biotechnology, medicine, and pharmaceutical industry. An instrument to determine particle electrophoretic mobility (EM) diameters in the single-digit to double-digit nanometer range receiving increased attention is the gas-phase electrophoretic mobility molecular analyzer (GEMMA) separating electrophoretically single charged analytes in the gas-phase at ambient pressure. A fused-silica capillary is used for analyte transfer to the gas-phase by means of a nano electrospray (ES) unit. The potential of this capillary to separate analytes electrophoretically in the liquid phase due to different mobilities is, at measurement conditions recommended by the manufacturer, eliminated due to elevated pressure applied for sample introduction. Measurements are carried out upon constant feeding of analytes to the system. Under these conditions, aggregate formation is observed for samples including high amounts of non-volatile components or complex samples. This makes the EM determination of individual species sometimes difficult, if not impossible. With the current study we demonstrate that liquid phase electrophoretic separation of proteins (as exemplary analytes) occurs in the capillary (capillary zone electrophoresis, CE) of the nano ES unit of the GEMMA. This finding was consecutively applied for on-line desalting allowing EM diameter determination of analytes despite a high salt concentration within samples. The present study is to our knowledge the first report on the use of the GEMMA to determine EM diameters of analytes solubilized in the ES incompatible electrolyte solutions by the intended use of electrophoresis (in the liquid phase) during sample delivery. Results demonstrate the proof of concept of such an approach and additionally illustrate the high potential of a future on-line coupling of a capillary electrophoresis to a GEMMA instrument. PMID:25109866

  14. Mercury speciation in thawed out and refrozen fish samples by gas chromatography coupled to inductively coupled plasma mass spectrometry and atomic fluorescence spectroscopy

    NARCIS (Netherlands)

    Krystek, Petra; Ritsema, Rob

    Different sub-sampling procedures were applied for the determination of mercury species (as total mercury Hg, methylmercury MeHg+ and inorganic mercury Hg2+) in frozen fish meat. Analyses were carried out by two different techniques. After the sample material was pre-treated by microwave digestion,

  15. Possibilities and limitations of dynamic headspace sampling as a pre-concentration technique for trace analysis of organics by capillary gas chromatography

    NARCIS (Netherlands)

    Curvers, J.M.P.M.; Noij, T.H.M.; Cramers, C.A.M.G.; Rijks, J.A.

    1984-01-01

    The possibilities, the limitations and the quantitative performance of dynamic headspace sampling, in particular closed-loop stripping, were investigated for various classes of organic substances in aqueous samples with concentrations down to the parts per 1012 (ppt) level. The effects of variations

  16. COMPARISON OF IMMUNOASSAY AND GAS CHROMATOGRAPHY/MASS SPECTROMETRY METHODS FOR MEASURING 3,5,6-TRICHLORO-2PYRIDINOL IN MULTIPLE SAMPLE MEDIA

    Science.gov (United States)

    Two enzyme-linked immunosorbent assay (ELISA) methods were evaluated for the determination of 3,5,6-trichloro-2-pyridinol (3,5,6-TCP) in multiple sample media (dust, soil, food, and urine). The dust and soil samples were analyzed by a commercial RaPID immunoassay testing kit. ...

  17. Tank vapor characterization project - Tank 241-U-112 headspace gas and vapor characterization: Results for homogeneity samples collected on December 6, 1996

    Energy Technology Data Exchange (ETDEWEB)

    Sklarew, D.S.; Pool, K.H.; Evans, J.C.; Hayes, J.C. [and others

    1997-09-01

    This report presents the results of analyses of samples taken from the headspace of waste storage tank 241-U-112 (Tank U-112) at the Hanford Site in Washington State. Samples were collected to determine the homogeneity of selected inorganic and organic headspace constitutents. Two risers (Riser 3 and Riser 6) were sampled at three different elevations (Bottom, Middle, and Top) within the tank. Tank headspace samples were collected by SGN Eurisys Service Corporation (SESC) and were analyzed by Pacific Northwest National Laboratory (PNNL) to determine headspace concentrations of selected non-radioactive analytes. Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. Ammonia was determined to be above the immediate notification limit specified by the sampling and analysis plan.

  18. [The elaboration of gas chromatographic method of the determination of N-nitrosamines (N-nitrosodimethylamine, N-nitrosodiethylamine) in biological samples (urine)].

    Science.gov (United States)

    Zaytseva, N V; Ulanova, T S; Nurislamova, T V; Popova, N A

    2014-01-01

    The issues of the elaboration of a method for the determination of N-nitrosamines (N-nitrosodimethylamine, N-nitrosodiethylamine) in urine by means of the method of capillary gas chromatography with the use of a thermionic detector are considered. There were performed investigations on the study of the efficacy of the extraction of N-nitrosamines from the urine by steam distillation and gas chromatographic detection of headspace. With the aim of the maximal recovery of N-nitrosamines from the urine and setting parameters of the extraction two method were used to prepare the bioassay for the analysis the alkalization with potassium hydroxide and the addition of salting out reagent--neutral salts of alkali and alkaline earth metals. During the process of performed studies there was found that the greatest degree of extraction of N-nitrosamines from the urine by the method of headspace analysis is achieved if using the salting-out agent in an amount of 16 g of sodium sulfate and for N-nitrosodimethylamine is 99%, for N-nitrosodiethylamine--100%.

  19. Determination of chlorophenols in landfill leachate using headspace sampling with ionic liquid-coated solid-phase microextraction fibers combined with gas chromatography–mass spectrometry

    International Nuclear Information System (INIS)

    Ho, Tse-Tsung; Chen, Chung-Yu; Li Zuguang; Yang, Thomas Ching-Cherng; Lee, Maw-Rong

    2012-01-01

    Highlights: ► Ionic liquid (IL), ([C 4 MIM][PF 6 ]), was rapid synthesized by microwave radiation. ► Trace chlorophenols in landfill leachate were extract by SPME coated IL. ► The IL-coated SPME-GC/MS method is low-cost, solvent-free and sensitive. - Abstract: A new microextraction technique based on ionic liquid solid-phase microextraction (IL-SPME) was developed for determination of trace chlorophenols (CPs) in landfill leachate. The synthesized ionic liquid, 1-butyl-3-methylimidazolium hexafluorophosphate ([C 4 MIM][PF 6 ]), was coated onto the spent fiber of SPME for extraction of trace CPs. After extraction, the absorbed analytes were desorbed and quantified using gas chromatography–mass spectrometry (GC/MS). The term of the proposed method is as ionic liquid-coated of solid-phase microextraction combined with gas chromatography–mass spectrometry (IL-SPME-GC/MS). No carryover effect was found, and every laboratory-made ionic liquids-coated-fiber could be used for extraction at least eighty times without degradation of efficiency. The chlorophenols studied were 2,4-dichlorophenol (2,4-DP), 2,4,6-trichlorophenol (2,4,6-TCP), 2,3,4,6-tetrachlorophenol (2,3,4,6-TeCP), and pentachlorophenol (PCP). The best results of chlorophenols analysis were obtained with landfill leachate at pH 2, headspace extraction for 4 min, and thermal desorption with the gas chromatograph injector at 240 °C for 4 min. Linearity was observed from 0.1 to 1000 μg L −1 with relative standard deviations (RSD) less than 7% and recoveries were over 87%. The limit of detection (LOD) for pentachlorophenol was 0.008 μg L −1 . The proposed method was tested by analyzing landfill leachate from a sewage farm. The concentrations of chlorophenols were detected to range from 1.1 to 1.4 μg L −1 . The results demonstrate that the IL-SPME-GC/MS method is highly effective in analyzing trace chlorophenols in landfill leachate.

  20. Determination of chlorophenols in landfill leachate using headspace sampling with ionic liquid-coated solid-phase microextraction fibers combined with gas chromatography-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Ho, Tse-Tsung; Chen, Chung-Yu [Department of Chemistry, National Chung Hsing University, Taichung 40227, Taiwan (China); Li Zuguang [Department of Chemistry, National Chung Hsing University, Taichung 40227, Taiwan (China); College of Chemical Engineering and Materials Science, Zhejiang University of Technology, Hangzhou 310014, Zhejiang (China); Yang, Thomas Ching-Cherng [Department of Chemistry, National Kaohsiung Normal University, Kaohsiung 82444, Taiwan (China); Lee, Maw-Rong, E-mail: mrlee@dragon.nchu.edu.tw [Department of Chemistry, National Chung Hsing University, Taichung 40227, Taiwan (China)

    2012-01-27

    Highlights: Black-Right-Pointing-Pointer Ionic liquid (IL), ([C{sub 4}MIM][PF{sub 6}]), was rapid synthesized by microwave radiation. Black-Right-Pointing-Pointer Trace chlorophenols in landfill leachate were extract by SPME coated IL. Black-Right-Pointing-Pointer The IL-coated SPME-GC/MS method is low-cost, solvent-free and sensitive. - Abstract: A new microextraction technique based on ionic liquid solid-phase microextraction (IL-SPME) was developed for determination of trace chlorophenols (CPs) in landfill leachate. The synthesized ionic liquid, 1-butyl-3-methylimidazolium hexafluorophosphate ([C{sub 4}MIM][PF{sub 6}]), was coated onto the spent fiber of SPME for extraction of trace CPs. After extraction, the absorbed analytes were desorbed and quantified using gas chromatography-mass spectrometry (GC/MS). The term of the proposed method is as ionic liquid-coated of solid-phase microextraction combined with gas chromatography-mass spectrometry (IL-SPME-GC/MS). No carryover effect was found, and every laboratory-made ionic liquids-coated-fiber could be used for extraction at least eighty times without degradation of efficiency. The chlorophenols studied were 2,4-dichlorophenol (2,4-DP), 2,4,6-trichlorophenol (2,4,6-TCP), 2,3,4,6-tetrachlorophenol (2,3,4,6-TeCP), and pentachlorophenol (PCP). The best results of chlorophenols analysis were obtained with landfill leachate at pH 2, headspace extraction for 4 min, and thermal desorption with the gas chromatograph injector at 240 Degree-Sign C for 4 min. Linearity was observed from 0.1 to 1000 {mu}g L{sup -1} with relative standard deviations (RSD) less than 7% and recoveries were over 87%. The limit of detection (LOD) for pentachlorophenol was 0.008 {mu}g L{sup -1}. The proposed method was tested by analyzing landfill leachate from a sewage farm. The concentrations of chlorophenols were detected to range from 1.1 to 1.4 {mu}g L{sup -1}. The results demonstrate that the IL-SPME-GC/MS method is highly effective in

  1. Analysis of non-esterified fatty acids in human samples by solid-phase-extraction and gas chromatography/mass spectrometry.

    Science.gov (United States)

    Kopf, Thomas; Schmitz, Gerd

    2013-11-01

    The determination of the fatty acid (FA) profile of lipid classes is essential for lipidomic analysis. We recently developed a GC/MS-method for the analysis of the FA profile of total FAs, i.e. the totality of bound and unbound FAs, in any given biological sample (TOFAs). Here, we present a method for the analysis of non-esterified fatty acids (NEFAs) in biological samples, i.e. the fraction that is present as extractable free fatty acids. Lipid extraction is performed according to Dole using 80/20 2-propanol/n-hexane (v/v), with 0.1% H2SO4. The fatty acid-species composition of this NEFA-fraction is determined as FAME after derivatization with our GC/MS-method on a BPX column (Shimadzu). Validation of the NEFA-method presented was performed in human plasma samples. The validated method has been used with human plasma, cells and tissues, as well as mammalian body fluids and tissue samples. The newly developed solid-phase-extraction (SPE)-GC-MS method allows the rapid separation of the NEFA-fraction from a neutral lipid extract of plasma samples. As a major advantage compared to G-FID-methods, GC-MS allows the use of stable isotope labeled fatty acid precursors to monitor fatty acid metabolism. Copyright © 2013 Elsevier B.V. All rights reserved.

  2. Exposure of unsuspecting workers to deadly atmospheres in below-ground confined spaces and investigation of related whole-air sample composition using adsorption gas chromatography.

    Science.gov (United States)

    Smith, Philip A; Lockhart, Bonnie; Besser, Brett W; Michalski, Michael A R

    2014-01-01

    Hazardous atmospheres in confined spaces may be obvious when a source of air contamination or oxygen (O2) deficiency is recognized. Such is often the case in general industry settings, especially with work processes which create hazardous atmospheres that may be anticipated. Hazards present in active sewers are also well recognized; but the possibility that O2 deficiency or high airborne contaminant concentrations may exist in new construction sewers or storm drains has been repeatedly ignored with deadly results. Low O2 and high carbon dioxide (CO2) concentrations may exist in new construction manholes that have not yet been connected to an active sewer or drain system, and these concentrations have been shown to vary over time. A recent incident is described where workers repeatedly entered such a confined space without incident, but subsequent entry resulted in a fatality and a near-miss for a co-worker rescuer. Additional cases are discussed, with an emphasis placed on elevated CO2 concentrations as a causative factor. A description is provided for the adsorptive gas chromatography whole-air analysis methodology used to quantitatively determine atmospheric conditions present at this type of fatality site or others after an incident, and for the gas chromatography-mass spectrometry method used to provide confirmation of analyte identity with high certainty. Many types of confined spaces may be encountered in addition to the underground varieties discussed, and many possible atmospheric hazards are possible. The definitive whole-air analysis approach described here may be of use and should be considered to investigate many confined space fatality and near-miss cases, and to better understand the causes of dangerous atmosphere conditions that may arise in confined spaces.

  3. Measurement of DNA adducts and strand breaks in dab (Limanda limanda) collected in the field: effects of biotic (age, sex) and abiotic (sampling site and period) factors on the extent of DNA damage

    Energy Technology Data Exchange (ETDEWEB)

    Akcha, F.; Leday, G.; Pfohl-Leszkowicz, A

    2004-08-18

    In the Eastern English Channel, the potential application of the comet assay and post-labelling technique in dab was evaluated for genotoxicity monitoring of the marine environment. The effects of biotic (age, sex) and abiotic (sampling site and period) factors on the extent of DNA lesions were also studied. Female and male dab of two class of size (juvenile and adult) were collected by trawling in different sites in Seine Bay and Somme Bay during September 2001. Single-strand breaks and adducts were, respectively, measured in erythrocytes and the liver. Results obtained for the adult female were compared with those collected during a first cruise in March 2001 [Akcha et al., Mutat Res. 534 (1-2) (2003) 21]. Significant effects of sex and age were demonstrated on the level of strand breaks. Moreover, a significant interaction between age and sex was shown that might indicate the complex influence of other factors on the extent of DNA damage (i.e. reproduction status). In the adult dab, the level of breaks is higher in the male than in the female, whereas the opposite trend was observed for the juvenile. Whatever the sex, the number of DNA breaks is higher in the adult than in the juvenile. For the female dab, significant differences were observed with the comet assay between the Seine Bay and the Somme Bay in March but not in September. This may be due to seasonal variations in the formation of DNA lesions related to variations in lipid content and levels of biotransformation activities and/or to spawning cycles. The presence of genotoxic substances in the study areas was also confirmed by the detection of DNA adducts in each sample analysed. Whereas no effect was shown on the total level of adducts for the tested biotic and abiotic factors, qualitative differences in adduct profiles were observed for each of these factors. For the female dab, comparison of adduct profiles obtained in March and September with one generated by hepatic microsomal activation in dab of

  4. Applicability of solid-phase microextraction combined with gas chromatography atomic emission detection (GC-MIP AED) for the determination of butyltin compounds in sediment samples

    Energy Technology Data Exchange (ETDEWEB)

    Carpinteiro, J.; Rodriguez, I.; Cela, R. [Universidad de Santiago de Compostela, Departamento de Quimica Analitica, Nutricion y Bromatologia, Instituto de Investigacion y Analisis Alimentario, Santiago de Compostela 15782 (Spain)

    2004-11-01

    The performance of solid-phase microextraction (SPME) applied to the determination of butyltin compounds in sediment samples is systematically evaluated. Matrix effects and influence of blank signals on the detection limits of the method are studied in detail. The interval of linear response is also evaluated in order to assess the applicability of the method to sediments polluted with butyltin compounds over a large range of concentrations. Advantages and drawbacks of including an SPME step, instead of the classic liquid-liquid extraction of the derivatized analytes, in the determination of butyltin compounds in sediment samples are considered in terms of achieved detection limits and experimental effort. Analytes were extracted from the samples by sonication using glacial acetic acid. An aliquot of the centrifuged extract was placed on a vial where compounds were ethylated and concentrated on a PDMS fiber using the headspace mode. Determinations were carried out using GC-MIP AED. (orig.)

  5. Thermochemolysis: A New Sample Preparation Approach for the Detection of Organic Components of Complex Macromolecules in Mars Rocks via Gas Chromatography Mass Spectrometry in SAM on MSL

    Science.gov (United States)

    Eugenbrode, J.; Glavin, D.; Dworkin, J.; Conrad, P.; Mahaffy, P.

    2011-01-01

    Organic chemicals, when present in extraterrestrial samples, afford precious insight into past and modern conditions elsewhere in the Solar System . No single technology identifies all molecular components because naturally occurring molecules have different chemistries (e.g., polar vs. non-polar, low to high molecular weight) and interface with the ambient sample chemistry in a variety of modes (i.e., organics may be bonded, absorbed or trapped by minerals, liquids, gases, or other organics). More than 90% of organic matter in most natural samples on Earth and in meteorites is composed of complex macromolecules (e.g. biopolymers, complex biomolecules, humic substances, kerogen) because the processes that tend to break down organic molecules also tend towards complexation of the more recalcitrant components. Thus, methodologies that tap the molecular information contained within macromolecules may be critical to detecting extraterrestrial organic matter and assessing the sources and processes influencing its nature.

  6. Polydimethylsiloxane rod extraction, a novel technique for the determination of organic micropollutants in water samples by thermal desorption-capillary gas chromatography-mass spectrometry.

    Science.gov (United States)

    Montero, L; Popp, P; Paschke, A; Pawliszyn, J

    2004-01-30

    A novel, simple and inexpensive approach to absorptive extraction of organic compounds from environmental samples is presented. It consists of a polydimethylsiloxane rod used as an extraction media, enriched with analytes during shaking, then thermally desorbed and analyzed by GC-MS. Its performance was illustrated and evaluated for the enrichment of sub- to ng/l of selected chlorinated compounds (chlorobenzenes and polychlorinated biphenyls) in water samples. The new approach was compared to the stir bar sorptive extraction performance. A natural ground water sample from Bitterfeld, Germany, was also extracted using both methods, showing good agreement. The proposed approach presented good linearity, high sensitivity, good blank levels and recoveries comparable to stir bars, together with advantages such as simplicity, lower cost and higher feasibility.

  7. A simple air sampling technique for monitoring nitrous oxide pollution

    Energy Technology Data Exchange (ETDEWEB)

    Austin, J C; Shaw, R; Moyes, D; Cleaton-Jones, P E

    1981-01-01

    A simple, inexpensive device for the continuous low-flow sampling of air was devised to permit monitoring of pollution by gaseous anaesthetics. The device consisted of a water-filled Perspex cylinder in which a double-walled flexible-film gas sample collection bag was suspended. Air samples could be aspirated into the collection bag at flow rates of as low as 1 ml min-1 by allowing the water to drain from the cylinder at a controlled rate. The maintenance of sample integrity with aspiration and storage of samples of nitrous oxide in air at concentrations of 1000, 100 and 30 p.p.m. v/v was examined using gas chromatography. The sample bags retained a mean 94% of the nitrous oxide in air samples containing nitrous oxide 25 p.p.m. over a 72-h storage period.

  8. Review of Current Literature and Research on Gas Supersaturation and Gas Bubble Trauma: Special Publication Number 1, 1986.

    Energy Technology Data Exchange (ETDEWEB)

    Colt, John; Bouck, Gerald R.; Fidler, Larry

    1986-12-01

    This report presents recently published information and on-going research on the various areas of gas supersaturation. Growing interest in the effects of chronic gas supersaturation on aquatic animals has been due primarily to heavy mortality of salmonid species under hatchery conditions. Extensive examination of affected animals has failed to consistently identify pathogenic organisms. Water quality sampling has shown that chronic levels of gas supersaturation are commonly present during a significant period of the year. Small marine fish larvae are significantly more sensitive to gas supersaturation than salmonids. Present water quality criteria for gas supersaturation are not adequate for the protection of either salmonids under chronic exposure or marine fish larvae, especially in aquaria or hatcheries. To increase communication between interested parties in the field of gas supersaturation research and control, addresses and telephone numbers of all people responding to the questionnaire are included. 102 refs.

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

    International Nuclear Information System (INIS)

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

    2007-01-01

    Time resolved signals in laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) are studied to determine the influence of experimental parameters on ICP-induced fractionation effects. Differences in sample composition and morphology, i.e., ablating brass, glass, or dust pellets, have a profound effect on the time resolved signal. Helium transport gas significantly decreases large positive signal spikes arising from large particles in the ICP. A binder for pellets also reduces the abundance and amplitude of spikes in the signal. MO + ions also yield signal spikes, but these MO + spikes generally occur at different times from their atomic ion counterparts.

  10. Analysis of microcontaminants in aqueous samples by fully automated on-line solid-phase extraction-gas chromatography-mass selective detection.

    NARCIS (Netherlands)

    Louter, A.J.H.; van Beekvelt, C.A.; Cid Montanes, P.; Slobodník, J.; Vreuls, J.J.; Brinkman, U.A.T.

    1996-01-01

    The trace-level analysis of unknown organic pollutants in water requires the use of fast and sensitive methods which also provide structural information. In the present study, an on-line technique was used which combines sample preparation by means of solid-phase extraction (SPE) on a small

  11. Gas turbine

    International Nuclear Information System (INIS)

    Yang, Ok Ryong

    2004-01-01

    This book introduces gas turbine cycle explaining general thing of gas turbine, full gas turbine cycle, Ericson cycle and Brayton cycle, practical gas turbine cycle without pressure loss, multiaxial type gas turbine cycle and special gas turbine cycle, application of basic theory on a study on suction-cooling gas turbine cycle with turbo-refrigerating machine using the bleed air, and general performance characteristics of the suction-cooling gas turbine cycle combined with absorption-type refrigerating machine.

  12. Validation and assessment of matrix effect and uncertainty of a gas chromatography coupled to mass spectrometry method for pesticides in papaya and avocado samples

    Directory of Open Access Journals (Sweden)

    Norma Susana Pano-Farias

    2017-07-01

    Full Text Available In this paper a method of using the “quick, easy, cheap, effective, rugged, and safe” (QuEChERS extraction and gas chromatography coupled to mass spectrometry detection (GC–MS was developed for the analysis of five frequently applied pesticides in papaya and avocado. The selected pesticides, ametryn, atrazine, carbaryl, carbofuran, and methyl parathion, represent the most commonly used classes (carbamates, organophosphorous, and triazines. Optimum separation achieved the analysis of all pesticides in 0.99. The limits of detection (LOD and quantification (LOQ in papaya ranged from 0.03 mg/kg to 0.35 mg/kg and from 0.06 mg/kg to 0.75 mg/kg, respectively. Meanwhile for avocado, LOD values varied from 0.14 mg/kg to 0.28 mg/kg and LOQ values ranged from 0.22 mg/kg to 0.40 mg/kg. Recoveries obtained for each pesticide in both matrices ranged between 60.6% and 104.3%. The expanded uncertainty of the method was < 26% for all the pesticides in both fruits. Finally, the method was applied to other fruits.

  13. Rapid and sensitive analysis of polychlorinated biphenyls and acrylamide in food samples using ionic liquid-based in situ dispersive liquid-liquid microextraction coupled to headspace gas chromatography.

    Science.gov (United States)

    Zhang, Cheng; Cagliero, Cecilia; Pierson, Stephen A; Anderson, Jared L

    2017-01-20

    A simple and rapid ionic liquid (IL)-based in situ dispersive liquid-liquid microextraction (DLLME) method was developed and coupled to headspace gas chromatography (HS-GC) employing electron capture (ECD) and mass spectrometry (MS) detection for the analysis of polychlorinated biphenyls (PCBs) and acrylamide at trace levels from milk and coffee samples. The chemical structures of the halide-based ILs were tailored by introducing various functional groups to the cations to evaluate the effect of different structural features on the extraction efficiency of the target analytes. Extraction parameters including the molar ratio of IL to metathesis reagent and IL mass were optimized. The effects of HS oven temperature and the HS sample vial volume on the analyte response were also evaluated. The optimized in situ DLLME method exhibited good analytical precision, good linearity, and provided detection limits down to the low ppt level for PCBs and the low ppb level for acrylamide in aqueous samples. The matrix-compatibility of the developed method was also established by quantifying acrylamide in brewed coffee samples. This method is much simpler and faster compared to previously reported GC-MS methods using solid-phase microextraction (SPME) for the extraction/preconcentration of PCBs and acrylamide from complex food samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  14. A sensitive and efficient method for trace analysis of some phenolic compounds using simultaneous derivatization and air-assisted liquid-liquid microextraction from human urine and plasma samples followed by gas chromatography-nitrogen phosphorous detection.

    Science.gov (United States)

    Farajzadeh, Mir Ali; Afshar Mogaddam, Mohammad Reza; Alizadeh Nabil, Ali Akbar

    2015-12-01

    In present study, a simultaneous derivatization and air-assisted liquid-liquid microextraction method combined with gas chromatography-nitrogen phosphorous detection has been developed for the determination of some phenolic compounds in biological samples. The analytes are derivatized and extracted simultaneously by a fast reaction with 1-flouro-2,4-dinitrobenzene under mild conditions. Under optimal conditions low limits of detection in the range of 0.05-0.34 ng mL(-1) are achievable. The obtained extraction recoveries are between 84 and 97% and the relative standard deviations are less than 7.2% for intraday (n = 6) and interday (n = 4) precisions. The proposed method was demonstrated to be a simple and efficient method for the analysis of phenols in biological samples. Copyright © 2015 John Wiley & Sons, Ltd.

  15. Resolving of challenging gas chromatography-mass spectrometry peak clusters in fragrance samples using multicomponent factorization approaches based on polygon inflation algorithm.

    Science.gov (United States)

    Ghaheri, Salehe; Masoum, Saeed; Gholami, Ali

    2016-01-15

    Analysis of fragrance composition is very important for both the fragrance producers and consumers. Unraveling of fragrance formulation is necessary for quality control, competitor and trace analysis. Gas chromatography-mass spectrometry (GC-MS) has been introduced as the most appropriate analytical technique for this type of analysis, which is based on Kovats index and MS database. The most straightforward method to analyze a GC-MS dataset is to integrate those peaks that can be recognized by their mass profiles. But, because of common problems of chromatographic data such as spectral background, baseline offset and specially overlapped peaks, accurate quantitative and qualitative analysis could be failed. Some chemometric modeling techniques such as bilinear multivariate curve resolution (MCR) methods have been introduced to overcome these problems and obtained well resolved chromatographic profiles. The main drawback of these methods is rotational ambiguity or nonunique solution that is represented as area of feasible solutions (AFS). Polygonal inflation algorithm (PIA) is an automatic and simple to use algorithm for numerical computation of AFS. In this study, the extent of rotational ambiguity in curve resolution methods is calculated by MCR-BAND toolbox and the PIA. The ability of the PIA in resolving GC-MS data sets is evaluated by simulated GC-MS data in comparison with other popular curve resolution methods such as multivariate curve resolution alternative least square (MCR-ALS), multivariate curve resolution objective function minimization (MCR-FMIN) by different initial estimation methods and independent component analysis (ICA). In addition, two typical challenging area of total ion chromatogram (TIC) of commercial fragrances with overlapped peaks were analyzed by the PIA to investigate the possibility of peak deconvolution analysis. Copyright © 2015 Elsevier B.V. All rights reserved.

  16. Changes in persistent contaminant concentration and CYP1A1 protein expression in biopsy samples from northern bottlenose whales, Hyperoodon ampullatus, following the onset of nearby oil and gas development

    Energy Technology Data Exchange (ETDEWEB)

    Hooker, Sascha K. [Department of Biology, Dalhousie University, Halifax, Nova Scotia B3H 4J1 (Canada); Sea Mammal Research Unit, University of St Andrews, FIFE KY16 8YG (United Kingdom)], E-mail: s.hooker@st-andrews.ac.uk; Metcalfe, Tracy L.; Metcalfe, Chris D. [Environmental and Resource Studies, Trent University, Peterborough, Ontario K9J 7B8 (Canada); Angell, Carolyn M.; Wilson, Joanna Y.; Moore, Michael J. [Biology Department, Woods Hole Oceanographic Institution, Woods Hole, MA 02543 (United States); Whitehead, Hal [Department of Biology, Dalhousie University, Halifax, Nova Scotia B3H 4J1 (Canada)

    2008-03-15

    A small population of endangered northern bottlenose whales (Hyperoodon ampullatus) inhabits 'The Gully' a Marine Protected Area on the Scotian Shelf, eastern Canada. Amid concerns regarding nearby oil and gas development, we took 36 skin and blubber biopsy samples in 1996-1997 (prior to major development) and 2002-2003 (five years after development began), and three samples from a population in the Davis Strait, Labrador in 2003. These were analysed for cytochrome P4501A1 (CYP1A1) protein expression (n = 36), and for persistent contaminants (n = 23). CYP1A1 showed generally low expression in whales from The Gully, but higher levels during 2003, potentially coincident with recorded oil spills, and higher levels in Davis Strait whales. A range of PCB congeners and organochlorine compounds were detected, with concentrations similar to other North Atlantic odontocetes. Concentrations were higher in whales from The Gully than from the Davis Strait, with significant increases in 4,4'-DDE and trans-nonachlor in 2002-2003 relative to 1996-1997. - Whale contaminants highlight concerns from oil and gas development near a marine protected area.

  17. Changes in persistent contaminant concentration and CYP1A1 protein expression in biopsy samples from northern bottlenose whales, Hyperoodon ampullatus, following the onset of nearby oil and gas development

    International Nuclear Information System (INIS)

    Hooker, Sascha K.; Metcalfe, Tracy L.; Metcalfe, Chris D.; Angell, Carolyn M.; Wilson, Joanna Y.; Moore, Michael J.; Whitehead, Hal

    2008-01-01

    A small population of endangered northern bottlenose whales (Hyperoodon ampullatus) inhabits 'The Gully' a Marine Protected Area on the Scotian Shelf, eastern Canada. Amid concerns regarding nearby oil and gas development, we took 36 skin and blubber biopsy samples in 1996-1997 (prior to major development) and 2002-2003 (five years after development began), and three samples from a population in the Davis Strait, Labrador in 2003. These were analysed for cytochrome P4501A1 (CYP1A1) protein expression (n = 36), and for persistent contaminants (n = 23). CYP1A1 showed generally low expression in whales from The Gully, but higher levels during 2003, potentially coincident with recorded oil spills, and higher levels in Davis Strait whales. A range of PCB congeners and organochlorine compounds were detected, with concentrations similar to other North Atlantic odontocetes. Concentrations were higher in whales from The Gully than from the Davis Strait, with significant increases in 4,4'-DDE and trans-nonachlor in 2002-2003 relative to 1996-1997. - Whale contaminants highlight concerns from oil and gas development near a marine protected area

  18. Review of light water reactor regulatory requirements: Assessment of selected regulatory requirements that may have marginal importance to risk: Postaccident sampling system, Turbine missiles, Combustible gas control, Charcoal filters

    International Nuclear Information System (INIS)

    Scott, W.B.; Jamison, J.D.; Stoetzel, G.A.; Tabatabai, A.S.; Vo, T.V.

    1987-05-01

    In a study commissioned by the Nuclear Regulatory Commission (NRC), Pacific Northwest Laboratory (PNL) evaluated the costs and benefits of modifying regulatory requirements in the areas of the postaccident sampling system, turbine rotor design reviews and inspections, combustible gas control for inerted Boiling Water Reactor (BWR) containments, and impregnated charcoal filters in certain plant ventilation systems. The basic framework for the analyses was that presented in the Regulatory Analysis Guidelines (NUREG/BR-0058) and in the Handbook for Value-Impact Assessment (NUREG/CR-3568). The effects of selected modifications to regulations were evaluated in terms of such factors as public risk and costs to industry and NRC. The results indicate that potential modifications of the regulatory requirements in three of the four areas would have little impact on public risk. In the fourth area, impregnated charcoal filters in buildi