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Sample records for on-line gas chromatographic

  1. On-line gas chromatographic analysis of airborne particles

    Science.gov (United States)

    Hering, Susanne V [Berkeley, CA; Goldstein, Allen H [Orinda, CA

    2012-01-03

    A method and apparatus for the in-situ, chemical analysis of an aerosol. The method may include the steps of: collecting an aerosol; thermally desorbing the aerosol into a carrier gas to provide desorbed aerosol material; transporting the desorbed aerosol material onto the head of a gas chromatography column; analyzing the aerosol material using a gas chromatograph, and quantizing the aerosol material as it evolves from the gas chromatography column. The apparatus includes a collection and thermal desorption cell, a gas chromatograph including a gas chromatography column, heated transport lines coupling the cell and the column; and a quantization detector for aerosol material evolving from the gas chromatography column.

  2. On-line gas chromatographic studies of rutherfordium (Element 104), hahnium (Element 105), and homologs

    International Nuclear Information System (INIS)

    Kadkhodayan, B.

    1993-05-01

    Gas-phase isothermal chromatogaphy is a method by which volatile compounds of different chemical elements can be separated according to their volatilities. The technique, coupled with theoretical modeling of the processes occurring in the chromatogaphy column, provides accurate determination of thermodynamic properties (e.g., adsorption enthalpies) for compounds of elements, such as the transactinides, which can only be produced on an atom-at-a-time basis. In addition, the chemical selectivity of the isothermal chromatogaphy technique provides the decontamination from interfering activities necessary for the determination of the nuclear decay properties of isotopes of the transactinide elements. Volatility measurements were performed on chloride species of Rf and its group 4 homologs, Zr and Hf, as well as Ha and its group 5 homologs, Nb and Ta. Adsorption enthalpies were calculated for all species using a Monte Carlo code simulation based on a microscopic model for gas thermochromatography in open columns with laminar flow of the carrier gas. Preliminary results are presented for Zr- and Nb-bromides

  3. Dual liquid and gas chromatograph system

    Science.gov (United States)

    Gay, D.D.

    A chromatographic system is described that utilizes one detection system for gas chromatographic and micro-liquid chromatographic determinations. The detection system is a direct-current, atmospheric-pressure, helium plasma emission spectrometer. The detector utilizes a nontransparent plasma source unit which contains the plasma region and two side-arms which receive effluents from the micro-liquid chromatograph and the gas chromatograph. The dual nature of this chromatographic system offers: (1) extreme flexibility in the samples to be examined; (2) extreme low sensitivity; (3) element selectivity; (4) long-term stability; (5) direct correlation of data from the liquid and gas samples; (6) simpler operation than with individual liquid and gas chromatographs, each with different detection systems; and (7) cheaper than a commercial liquid chromatograph and a gas chromatograph.

  4. A Quantitative Gas Chromatographic Ethanol Determination.

    Science.gov (United States)

    Leary, James J.

    1983-01-01

    Describes a gas chromatographic experiment for the quantitative determination of volume percent ethanol in water ethanol solutions. Background information, procedures, and typical results are included. Accuracy and precision of results are both on the order of two percent. (JN)

  5. Optimization of the gas chromatographic separations

    International Nuclear Information System (INIS)

    Gasco Sanchez, L.

    1973-01-01

    A review and a critical study on the optimization of the gas chromatographic separations are made. After dealing with the fundamental gas chromatographic equations, some methods of expressing column performances are discussed: performance indices, performance parameters, resolution and effective plate number per unit time. This is completed with a comparative study on performances of various types of columns. Moreover, optimization methods for operating chromatographic conditions are extensively dealt with: as resolution optimization, separation time, and normalization techniques for the time of analysis in order to achieve the maximum resolution at constant time. Finally, some others non operating parameters such as: selectivity of stationary phases, column preparation and optimization methods by means of computers are studied. (Author) 68 refs

  6. GAS CHROMATOGRAPHIC AND SPECTROSCOPIC ANALYSIS OF ...

    African Journals Online (AJOL)

    Peroxyformic acid prepared in-situ was employed for epoxidation of canola oil in the presence of toluene. Gas chromatographic analysis of the product revealed the following species: C16:0; C18:0; C18:1; C18:2; C18:3; monoepoxy C18:0; monoepoxy C18:1; monoepoxy C18:2; diepoxy C18:0; diepoxy C18:1 and triepoxy ...

  7. A Small-Scale Low-Cost Gas Chromatograph

    Science.gov (United States)

    Gros, Natasa; Vrtacnik, Margareta

    2005-01-01

    The design and application of a small-scale portable gas chromatograph for learning of the basic concepts of chromatography is described. The apparatus consists of two basic separable units, which includes a chromatographic unit and an electronic unit.

  8. Simple gas chromatographic method for furfural analysis.

    Science.gov (United States)

    Gaspar, Elvira M S M; Lopes, João F

    2009-04-03

    A new, simple, gas chromatographic method was developed for the direct analysis of 5-hydroxymethylfurfural (5-HMF), 2-furfural (2-F) and 5-methylfurfural (5-MF) in liquid and water soluble foods, using direct immersion SPME coupled to GC-FID and/or GC-TOF-MS. The fiber (DVB/CAR/PDMS) conditions were optimized: pH effect, temperature, adsorption and desorption times. The method is simple and accurate (RSDfurfurals will contribute to characterise and quantify their presence in the human diet.

  9. The gas-chromatographic and gas-chromatographic-mass-spectrometric identification of halogen-containing organic compounds

    Science.gov (United States)

    Gidaspov, B. V.; Zenkevich, I. G.; Rodin, A. A.

    1989-09-01

    The problem of identifying halogen-containing organic compounds in their gas-chromatographic and gas-chromatographic-mass-spectrometric (GC-MS) determination in different materials has been examined. Particular attention has been paid not to the complete characterisation of methods for carrying out this analysis but to the most important problem of increasing the selectivity at the stages of sampling, separation, and interpretation of the gas-chromatographic and GC-MS information. The bibliography contains 292 references.

  10. Gas-Chromatographic Determination Of Water In Freon PCA

    Science.gov (United States)

    Melton, Donald M.

    1994-01-01

    Gas-chromatographic apparatus measures small concentrations of water in specimens of Freon PCA. Testing by use of apparatus faster and provides greater protection against accidental contamination of specimens by water in testing environment. Automated for unattended operation. Also used to measure water contents of materials, other than Freon PCA. Innovation extended to development of purgeable sampling accessory for gas chromatographs.

  11. Operational experience of water quality improvement accompanied by monitoring with on-line ion chromatograph

    International Nuclear Information System (INIS)

    Kobayashi, M.; Maeda, K.; Hashimoto, H.; Ishibe, T.; Usui, N.; Osumi, K.; Ishigure, K.

    1997-01-01

    Hamaoka Unit No.1 (BWR 540 MWe) of Chubu Electric Power Company, Inc. had experienced fuel failures caused by fuel cladding corrosion at the cycle 11 in 1990. This cladding corrosion was considered to be caused by a combination of cladding material susceptibility to corrosion and anomalous reactor water quality. Based on the intensive investigations on the causes of anomalous reactor water quality, several countermeasures were proposed to improve the reactor water quality for the subsequent cycles operation. As the results of countermeasures, reactor water quality of Hamaoka Unit No.1 in the cycle 12 became much better than that of any other previous cycles and neither failure nor accelerated corrosion was found in the subsequent annual inspection. As one of the countermeasures for water quality improvement, an on-line ion chromatograph has been installed on Hamaoka Unit No.1 to reinforce reactor water quality monitoring, that has enabled us to identify ion species in reactor water and to evaluate reactor water behaviour in detail. (author). 3 refs, 8 figs, 2 tab

  12. Operational experience of water quality improvement accompanied by monitoring with on-line ion chromatograph

    Energy Technology Data Exchange (ETDEWEB)

    Kobayashi, M; Maeda, K [Toshiba Corp., Yokohama (Japan); Hashimoto, H; Ishibe, T [Chubu Electric Power Co. Inc., Nagoya (Japan); Usui, N [Hitachi Engineering Co. Ltd., Ibaraki (Japan); Osumi, K [Hitachi Ltd., Hitachi (Japan); Ishigure, K [Tokyo Univ. (Japan)

    1997-02-01

    Hamaoka Unit No.1 (BWR 540 MWe) of Chubu Electric Power Company, Inc. had experienced fuel failures caused by fuel cladding corrosion at the cycle 11 in 1990. This cladding corrosion was considered to be caused by a combination of cladding material susceptibility to corrosion and anomalous reactor water quality. Based on the intensive investigations on the causes of anomalous reactor water quality, several countermeasures were proposed to improve the reactor water quality for the subsequent cycles operation. As the results of countermeasures, reactor water quality of Hamaoka Unit No.1 in the cycle 12 became much better than that of any other previous cycles and neither failure nor accelerated corrosion was found in the subsequent annual inspection. As one of the countermeasures for water quality improvement, an on-line ion chromatograph has been installed on Hamaoka Unit No.1 to reinforce reactor water quality monitoring, that has enabled us to identify ion species in reactor water and to evaluate reactor water behaviour in detail. (author). 3 refs, 8 figs, 2 tab.

  13. Pyrolysis gas chromatographic atomic emission detection for sediments, coals and other petrochemical precursors

    Energy Technology Data Exchange (ETDEWEB)

    Seeley, J.A.; Zeng, Y.D.; Uden, P.C.; Eglinton, T.I.; Ericson, I. (Massachusetts University, Amherst, MA (USA). Dept. of Chemistry)

    1992-09-01

    On-line flash pyrolysis coupled to a capillary gas chromatograph for the characterization of marine sediments, coals and other heterogeneous solid samples is described. A helium microwave-induced plasma is used for chromatographic detection by atomic emission spectrometry. Simultaneous multi-element detection is achieved with a photodiode array detector. The optical path of the gas chromatographic atomic emission detector is purged with helium, allowing simultaneous, sensitive detection of atomic emission from sulfur 181 nm, phosphorous 186 nm, arsenic 189 nm, selenium 196 nm and carbon 193 nm. Several sediment and coal samples have been analysed for their carbon, nitrogen, sulfur, oxygen, phosphorous, arsenic and selenium content. Qualitative information indicating the occurrence and distribution of these elements in the samples can be used to gauge the relative stage of diagenetic evolution of the samples and provide information on their depositional environment. In some instances the chromatographic behaviour of the compounds produced upon pyrolysis is improved through on-line alkylation. This on-line derivatization is achieved by adding liquid reagents to the pyrolysis probe or by adding liquid reagents to the pyrolysis probe or by adding solid reagents either to the solid sample or by packing the reagent in the injection port of the chromatograph.

  14. On-line ultrasonic gas entrainment monitor

    International Nuclear Information System (INIS)

    Day, C.K.; Pedersen, H.N.

    1978-01-01

    Apparatus employing ultrasonic energy for detecting and measuring the quantity of gas bubbles present in liquids being transported through pipes is described. An ultrasonic transducer is positioned along the longitudinal axis of a fluid duct, oriented to transmit acoustic energy radially of the duct around the circumference of the enclosure walls. The back-reflected energy is received centrally of the duct and interpreted as a measure of gas entrainment. One embodiment employs a conical reflector to direct the transmitted acoustic energy radially of the duct and redirect the reflected energy back to the transducer for reception. A modified embodiment employs a cylindrical ultrasonic transducer for this purpose

  15. Continuous determination of volatile products in anaerobic fermenters by on-line capillary gas chromatography

    International Nuclear Information System (INIS)

    Diamantis, V.; Melidis, P.; Aivasidis, A.

    2006-01-01

    Bio-ethanol and biogas produced during the anaerobic conversion of organic compounds has been a subject of great interest since the oil crisis of the 1970s. In ethanol fermentation and anaerobic treatment of wastewaters, end-product (ethanol) and intermediate-products (short-chain fatty acids, SCFA) cause inhibition that results in reduced process efficiency. Control of these constituents is of utmost importance for bioreactor optimization and process stability. Ethanol and SCFA can be detected with precision by capillary gas chromatography usually conducted in off-line measurements. In this work, an on-line monitoring and controlling system was developed and connected to the fermenter via an auto-sampling equipment, which could perform the feeding, filtration and dilution of the sample and final injection into the gas chromatograph through an automation-based programmed procedure. The sample was continuously pumped from the recycle stream of the bioreactor and treated using a microfiltration unit. The concentrate was returned to the reactor while the permeate was quantitatively mixed with an internal standard solution. The system comprised of a gas chromatograph with the flow cell and one-shot sampler and a PC with the appropriate software. The on-line measurement of ethanol and SCFA, directly from the liquid phase of an ethanol fermenter and a high-rate continuous mode anaerobic digester, was accomplished by gas chromatography. Also, this monitoring and controlling system was proved to be effective in the continuous fermentation of alcohol-free beer

  16. On-line optimal control improves gas processing

    International Nuclear Information System (INIS)

    Berkowitz, P.N.; Papadopoulos, M.N.

    1992-01-01

    This paper reports that the authors' companies jointly funded the first phase of a gas processing liquids optimization project that has the specific purposes to: Improve the return of processing natural gas liquids, Develop sets of control algorithms, Make available a low-cost solution suitable for small to medium-sized gas processing plants, Test and demonstrate the feasibility of line control. The ARCO Willard CO 2 gas recovery processing plant was chosen as the initial test site to demonstrate the application of multivariable on-line optimal control. One objective of this project is to support an R ampersand D effort to provide a standardized solution to the various types of gas processing plants in the U.S. Processes involved in these gas plants include cryogenic separations, demethanization, lean oil absorption, fractionation and gas treating. Next, the proposed solutions had to be simple yet comprehensive enough to allow an operator to maintain product specifications while operating over a wide range of gas input flow and composition. This had to be a supervisors system that remained on-line more than 95% of the time, and achieved reduced plant operating variability and improved variable cost control. It took more than a year to study various gas processes and to develop a control approach before a real application was finally exercised. An initial process for C 2 and CO 2 recoveries was chosen

  17. Gas-chromatographic separation of hydrogen isotopic mixtures

    International Nuclear Information System (INIS)

    Preda, Anisoara; Bidica, Nicolae

    2005-01-01

    Full text: Gas chromatographic separation of hydrogen isotopes have been reported in the literature since late of 1950's. Gas chromatography is primarily an analytical method, but because of its properties it may be used in many other fields with excellent results. A simple method is proposed for the gas-chromatographic analysis of complex gas mixtures containing hydrogen isotopes; the method is based on the substantial difference in the thermal conductivity of these isotopes. One of the main disadvantages of the conventional gas chromatography is the long retention times required for the analysis of hydrogen gas mixtures while the column is operated at very low temperature. The method described in this paper was based on using a capillary molecular sieve 5A column operated for this kind of separation at 173 K. The carrier gas was Ne and the detector was TCD. In the paper chromatograms for various carrier flow rates and various hydrogen isotope mixtures are presented. (authors)

  18. Evaluation of pesticide adsorption in gas chromatographic injector and column

    Directory of Open Access Journals (Sweden)

    Gevany Paulino de Pinho

    2012-01-01

    Full Text Available Components in complex matrices can cause variations in chromatographic response during analysis of pesticides by gas chromatography. These variations are related to the competition between analytes and matrix components for adsorption sites in the chromatographic system. The capacity of the pesticides chlorpyrifos and deltamethrin to be adsorbed in the injector and chromatographic column was evaluated by constructing three isotherms and changing the column heating rate to 10 and 30 ºC min-1. By using ANCOVA to compare the slope of calibration graphs, results showed that the higher the injector temperature (310 ºC the lower the pesticide adsorption. Also, deltamethrin influenced the adsorption of chlorpyrifos on the column chromatographic.

  19. Gas chromatographic analysis of volatiles in fluid and gas inclusions

    Science.gov (United States)

    Andrawes, F.; Holzer, G.; Roedder, E.; Gibson, E.K.; Oro, John

    1984-01-01

    Most geological samples and some synthetic materials contain fluid inclusions. These inclusions preserve for us tiny samples of the liquid and/or the gas phase that was present during formation, although in some cases they may have undergone significant changes from the original material. Studies of the current composition of the inclusions provide data on both the original composition and the change since trapping.These inclusions are seldom larger than 1 millimeter in diameter. The composition varies from a single major compound (e.g., water) in a single phase to a very complex mixture in one or more phases. The concentration of some of the compounds present may be at trace levels.We present here some analyses of inclusions in a variety of geological samples, including diamonds. We used a sample crusher and a gas chromatography—mass spectrometry (GC—MS) system to analyze for organic and inorganic volatiles present as major to trace constituents in inclusions. The crusher is a hardened stainless-steel piston cylinder apparatus with tungsten carbide crusing surfaces, and is operated in a pure helium atmosphere at a controlled temperature.Samples ranging from 1 mg to 1 g were crushed and the released volatiles were analyzed using multi-chromatographic columns and detectors, including the sensitive helium ionization detector. Identification of the GC peaks was carried out by GC—MS. This combination of procedures has been shown to provide geochemically useful information on the process involved in the history of the samples analyzed.

  20. On-line sodium and cover as purity monitors gas operating tools at EBR-II

    International Nuclear Information System (INIS)

    Smith, C.R.F.; Richardson, W.J.; Holmes, J.T.

    1976-01-01

    Plugging temperature indicators, electrochemical oxygen meters and hydrogen diffusion meters are the on-line sodium purity monitors now in use at EBR-II. On-line gas chromatographs are used to monitor helium, hydrogen, oxygen and nitrogen impurities in the argon cover gases. Monitors for tritium-in-sodium and for hydrocarbons-in-cover gas have been developed and are scheduled for installation in the near future. An important advantage of on-line monitors over the conventional grab-sampling techniques is the speed of response to changing reactor conditions. This helps us to identify the source of the impurity, whether the cause may be transient or constant, and take corrective action as necessary. The oxygen meter is calibrated monthly against oxygen in sodium determined by the vanadium wire equilibration method. The other instruments either do not require calibration or are self-calibrating. The ranges, sensitivity and response times of all of the on-line purity monitors has proven satisfactory under EBR-II operating conditions

  1. Gas chromatographic column for the Viking 1975 molecular analysis experiment

    Science.gov (United States)

    Novotny, M.; Hayes, J. M.; Bruner, F.; Simmonds, P. G.

    1975-01-01

    A gas chromatographic column has been developed for use in the remote analysis of the Martian surface. The column, which utilizes a liquid-modified organic adsorbent (Tenax) as the stationary phase, provides efficient transmission and resolution of nanogram quantities of organic materials in the presence of millionfold excesses of water and carbon dioxide.

  2. Gas chromatographic determination of impurities of inorganic compounds

    International Nuclear Information System (INIS)

    Drugov, Yu.S.

    1985-01-01

    Methods of concentration, separation, detection in gas chromatographic determination of impurities of inorganic compounds including low-boiling gases, reactive gases, organometallic compounds, free metals, anions, etc. are reviewed. Methods of reaction gas chromatography for determining reactive gases, water, anions, metal chelates are considered in detail as well as methods of reaction-sorption concentration and reaction gas extraction. The application of gas chromatograpny ior anaiysis of water and atmosphere contamination, for determination of impurities in highly pure solid substances and gases is described

  3. Transformation kinetics of chlorinated ethenes by Methylosinus trichosporium OB3b and detection of unstable epoxides by on-line gas chromatography

    NARCIS (Netherlands)

    van Hylckama Vlieg, Johan. E.T.; Koning, Wim de; Janssen, Dick B.

    A rapid and accurate method for the determination of transformation kinetics of volatile organic substrates was developed. Concentrations were monitored by on-line gas chromatographic analysis of the headspace of well-mixed incubation mixtures. With this method, the kinetics of transformation of a

  4. A Gas Chromatographic System for the Detection of Ethylene Gas Using Ambient Air as a Carrier Gas.

    Science.gov (United States)

    Zaidi, Nayyer Abbas; Tahir, Muhammad Waseem; Vellekoop, Michael J; Lang, Walter

    2017-10-07

    Ethylene gas is a naturally occurring gas that has an influence on the shelf life of fruit during their transportation in cargo ships. An unintentional exposure of ethylene gas during transportation results in a loss of fruit. A gas chromatographic system is presented here for the detection of ethylene gas. The gas chromatographic system was assembled using a preconcentrator, a printed 3D printed gas chromatographic column, a humidity sensor, solenoid valves, and an electrochemical ethylene gas sensor. Ambient air was used as a carrier gas in the gas chromatographic system. The flow rate was fixed to 10 sccm. It was generated through a mini-pump connected in series with a mass flow controller. The metal oxide gas sensor is discussed with its limitation in ambient air. The results show the chromatogram obtained from metal oxide gas sensor has low stability, drifts, and has uncertain peaks, while the chromatogram from the electrochemical sensor is stable and precise. Furthermore, ethylene gas measurements at higher ppb concentration and at lower ppb concentration were demonstrated with the electrochemical ethylene gas sensor. The system separates ethylene gas and humidity. The chromatograms obtained from the system are stable, and the results are 1.2% repeatable in five similar measurements. The statistical calculation of the gas chromatographic system shows that a concentration of 2.3 ppb of ethylene gas can be detected through this system.

  5. Gas chromatographic method fr determination of carbon in metallic uranium

    International Nuclear Information System (INIS)

    Nikol'skij, V.A.; Markov, V.K.; Evseeva, T.I.; Cherstvenkova, E.P.

    1983-01-01

    Gas chromatographic device to determine carbon in metal uranium is developed. Burnout unite, permitting to load in the burnout tube simultaneously quite a few (up to 20) weight amounts of materials to be burned is a characteristic feature of the device. As a result amendments for control experiment and determination limit are decreased. The time of a single determination is also reduced. Conditions of carbon burn out from metal uranium are studied and temperature and time of complete extraction of carbon in the form of dioxide from weight amount into gaseous phase are established

  6. Temperature Control of Gas Chromatograph Based on Switched Delayed System Techniques

    Directory of Open Access Journals (Sweden)

    Xiao-Liang Wang

    2014-01-01

    Full Text Available We address the temperature control problem of the gas chromatograph. We model the temperature control system of the gas chromatograph into a switched delayed system and analyze the stability by common Lyapunov functional technique. The PI controller parameters can be given based on the proposed linear matrix inequalities (LMIs condition and the designed controller can make the temperature of gas chromatograph track the reference signal asymptotically. An experiment is given to illustrate the effectiveness of the stability criterion.

  7. Gas chromatographic isolation technique for compound-specific radiocarbon analysis

    International Nuclear Information System (INIS)

    Uchida, M.; Kumamoto, Y.; Shibata, Y.; Yoneda, M.; Morita, M.; Kawamura, K.

    2002-01-01

    Full text: We present here a gas chromatographic isolation technique for the compound-specific radiocarbon analysis of biomarkers from the marine sediments. The biomarkers of fatty acids, hydrocarbon and sterols were isolated with enough amount for radiocarbon analysis using a preparative capillary gas chromatograph (PCGC) system. The PCGC systems used here is composed of an HP 6890 GC with FID, a cooled injection system (CIS, Gerstel, Germany), a zero-dead-volume effluent splitter, and a cryogenic preparative collection device (PFC, Gerstel). For AMS analysis, we need to separate and recover sufficient quantity of target individual compounds (>50 μgC). Yields of target compounds from C 14 n-alkanes to C 40 to C 30 n-alkanes and approximately that of 80% for higher molecular weights compounds more than C 30 n-alkanes. Compound specific radiocarbon analysis of organic compounds, as well as compound-specific stable isotope analysis, provide valuable information on the origins and carbon cycling in marine system. Above PCGC conditions, we applied compound-specific radiocarbon analysis to the marine sediments from western north Pacific, which showed the possibility of a useful chronology tool for estimating the age of sediment using organic matter in paleoceanographic study, in the area where enough amounts of planktonic foraminifera for radiocarbon analysis by accelerator mass spectrometry (AMS) are difficult to obtain due to dissolution of calcium carbonate. (author)

  8. Gas chromatographic measurement in water-steam circuits

    International Nuclear Information System (INIS)

    Zschetke, J.; Nieder, R.

    1984-01-01

    A gas chromatographic technique for measurements in water-steam circuits, which has been well known for many years, has been improved by design modifications. A new type of equipment developed for special measuring tasks on nuclear engineering plant also has a general application. To date measurements have been carried out on the ''Otto Hahn'' nuclear powered ship, on the KNK and AVR experimental nuclear power plants at Karlsruhe and Juelich respectively and on experimental boiler circuits. The measurements at the power plants were carried out under different operating conditions. In addition measurements during the alkali operating mode and during combined cycle operation were carried out on the AVR reactor. It has been possible to draw new conclusion from the many measurements undertaken. (orig.) [de

  9. 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

  10. Mars Solar Balloon Landed Gas Chromatograph Mass Spectrometer

    Science.gov (United States)

    Mahaffy, P.; Harpold, D.; Niemann, H.; Atreya, S.; Gorevan, S.; Israel, G.; Bertaux, J. L.; Jones, J.; Owen, T.; Raulin, F.

    1999-01-01

    A Mars surface lander Gas Chromatograph Mass Spectrometer (GCMS) is described to measure the chemical composition of abundant and trace volatile species and isotope ratios for noble gases and other elements. These measurements are relevant to the study of atmospheric evolution and past climatic conditions. A Micromission plan is under study where a surface package including a miniaturized GCMS would be delivered to the surface by a solar heated hot air balloon based system. The balloon system would be deployed about 8 km above the surface of Mars, wherein it would rapidly fill with Martian atmosphere and be heated quickly by the sun. The combined buoyancy and parachuting effects of the solar balloon result in a surface package impact of about 5 m/sec. After delivery of the package to the surface, the balloon would ascend to about 4 km altitude, with imaging and magnetometry data being taken for the remainder of the daylight hours as the balloon is blown with the Martian winds. Total atmospheric entry mass of this mission is estimated to be approximately 50 kg, and it can fit as an Ariane 5 piggyback payload. The GCMS would obtain samples directly from the atmosphere at the surface and also from gases evolved from solid phase material collected from well below the surface with a Sample Acquisition and Transport Mechanism (SATM). The experiment envisioned in the Mars Micromission described would obtain samples from a much greater depth of up to one meter below the surface, and would search for organic molecules trapped in ancient stratified layers well below the oxidized surface. Insitu instruments on upcoming NASA missions working in concert with remote sensing measurement techniques have the potential to provide a more detailed investigation of mineralogy and the extent of simple volatiles such as CO2 and H2O in surface and subsurface solid phase materials. Within the context of subsequent mission opportunities such as those provided by the Ariane 5 piggyback

  11. Characterisation of wax works of art by gas chromatographic procedures.

    Science.gov (United States)

    Regert, M; Langlois, J; Colinart, S

    2005-10-14

    To identify the various natural and synthetic substances used by sculptors at the end of the 19th century, several contemporary reference samples were investigated by high temperature gas chromatography (HT GC) and HT GC-MS. Using specific chromatographic conditions and minimising sample preparation, we could separate, detect and identify a wide range of biomolecular markers covering a great variety of molecular weights and volatilities, with a minimum amount of sample, in a single run. Beeswax, spermaceti, carnauba, candellila and Japan waxes as well as pine resin derivatives, animal fats, paraffin, ozokerite and stearin, used as additives in wax works of art, were chemically investigated. In the case of low volatile compounds, transbutylation was performed. The structure of long-chain esters of spermaceti was elucidated for the first time by HT GC-MS analysis. Such a method was then carried out on 10 samples collected on a statuette of Junon by Antoine-Louis Barye (Louvre Museum, Paris, France) and on a sculpture by Aimé-Jules Dalou (Musée de la Révolution Française, Vizille, France). The analytical results obtained provide new data on the complex recipes elaborated by sculptors at the end of the 19th century.

  12. Recent Advances in Water Analysis with Gas Chromatograph Mass Spectrometers

    Science.gov (United States)

    MacAskill, John A.; Tsikata, Edem

    2014-01-01

    We report on progress made in developing a water sampling system for detection and analysis of volatile organic compounds in water with a gas chromatograph mass spectrometer (GCMS). Two approaches are described herein. The first approach uses a custom water pre-concentrator for performing trap and purge of VOCs from water. The second approach uses a custom micro-volume, split-splitless injector that is compatible with air and water. These water sampling systems will enable a single GC-based instrument to analyze air and water samples for VOC content. As reduced mass, volume, and power is crucial for long-duration, manned space-exploration, these water sampling systems will demonstrate the ability of a GCMS to monitor both air and water quality of the astronaut environment, thereby reducing the amount of required instrumentation for long duration habitation. Laboratory prototypes of these water sampling systems have been constructed and tested with a quadrupole ion trap mass spectrometer as well as a thermal conductivity detector. Presented herein are details of these water sampling system with preliminary test results.

  13. The behaviour of radionuclides in gas adsorption chromatographic processes with superimposed chemical reactions (chlorides)

    International Nuclear Information System (INIS)

    Eichler, B.

    1996-01-01

    Thermochemical relationships are derived describing the gas adsorption chromatographic transport of carrier-free radionuclides. Especially, complex adsorption processes such as dissociative, associative and substitutive adsorption are dealt with. The comparison of experimental with calculated data allows the determination of the type of adsorption reaction, which is the basis of the respective gas chromatographic process. The behaviour of carrier-free radionuclides of elements Pu, Ce, Ru, Co and Cr in thermochromatographic experiments with chlorinating carrier gases can be described as dissociative adsorption of chlorides in higher oxidation states. The gas adsorption chromatographic transport of Zr with oxygen and chlorine containing carrier gas is shown to be a substitutive adsorption process. The consequences of superimposed chemical reactions on the interpretation of results and the conception of gas adsorption chromatographic experiments with carrier-free radionuclides in isothermal columns and in temperature gradient tubes is discussed. (orig.)

  14. On-line non-contact gas analysis

    DEFF Research Database (Denmark)

    Fateev, Alexander; Clausen, Sønnik

    , and good agreement has been found for NO (e.g. deviations of 1-5% for NO at 1200 °C). Practical highresolution measurements at the AVV2 boiler are analysed, and detection limits for the NO are discussed. The developed tools and results will be used in the future projects, e.g. fast measurements of the gas...

  15. On-line gas chemistry experiments with trans actinide elements

    International Nuclear Information System (INIS)

    Turler, A.; Gaguller, B.; Jost, D.T.

    1993-01-01

    The latest achievements in the gas phase chemistry studies of elements 104 and 105 and their lighter homologs are reviewed. Experimental techniques employed in the studies are described. Experimental data on chlorides and bromides of the groups 4, 5 elements and elements 104, 105 are compared with their theoretically predicted chemical properties. 45 refs

  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. Gas chromatographic analysis of simmondsins and simmondsin ferulates in jojoba meal.

    Science.gov (United States)

    Van Boven, M; Holser, R; Cokelaere, M; Flo, G; Decuypere, E

    2000-09-01

    A capillary gas chromatographic method was developed for the simultaneous determination of simmondsins and simmondsin ferulates in jojoba meal, in detoxified jojoba meal, in jojoba meal extracts, and in animal food mixtures.

  18. Separation and determination of high-carbon alcohols using method of column chromatographic and gas-chromatographic analysis

    International Nuclear Information System (INIS)

    Kang Zhongrong; Li Biping; Zeng Yongchang

    1988-01-01

    This paper describes the separation and determination of high-carbon alcohols from amine extractant by using the method of column chromatography of aluminium oxide and gas-chromatographic analysis. The total conent of high-carbon alcohols is determined by the method of column chromatography, while the components of the high-carbon alcohols and their relative contents are determined by the method of gas-chromatography. A simple reliable and practical method is provided for the analysis of high-carbon alcohol from the amine extractant in this paper

  19. Gas chromatographic determination of yohimbine in commercial yohimbe products.

    Science.gov (United States)

    Betz, J M; White, K D; der Marderosian, A H

    1995-01-01

    The bark of Pausinystalia yohimbe [K. Schumann] Pierre (Rubiaceae), long valued as an aphrodisiac in West Africa, recently has been promoted in the United States as a dietary supplement alternative to anabolic steroids for enhancement of athletic performance. As the number of yohimbe products on the retail market increases, concerns about their safety are raised because of the reported toxicity of yohimbine (the major alkaloid of the plant). Although plant materials are usually identified microscopically, we were unable to identify them in many of the products, because as their labels indicated, the products were mixtures of various botanicals or were bark extracts and contained little or no plant material. A method for extraction and capillary gas chromatographic (GC) separation of the alkaloids of P. yohimbe was, therefore, developed and used to analyze a number of commercial yohimbe products. The method involved solvent extraction and partitioning in chloroform-water followed by separation on a methyl silicone capillary GC column (N-P detection). Comparisons of chromatograms of extracts of authentic bark with those of commercial products indicated that, although many products contained measurable quantities of the alkaloid yohimbine, they were largely devoid of the other alkaloids previously reported in this species. Concentrations of yohimbine in the commercial products ranged from < 0.1 to 489 ppm, compared with 7089 ppm in the authentic material. Authentic bark has been reported to contain up to 6% total alkaloids, 10-15% of which are yohimbine. The possible presence of undeclared diluents in the products was indicated by peaks in product chromatograms but not in those of authentic bark.

  20. ALICE TPC gas system is the first of the LHC experiments to be put on line

    CERN Document Server

    Maximilien Brice

    2006-01-01

    Picture 01 : the Physics Department's DT1 gas systems team in their laboratory. Picture 02 : Chilo Garabatos (ALICE) and Stefan Haider (PH-DT1-GS) in front of the gas system for the ALICE TPC which has just been put on line.

  1. Different reactivities of amphetamines with N-methyl-bis(trifluoroacetamide) in heated gas chromatographic injectors.

    Science.gov (United States)

    Hidvégi, E; Hideg, Zs; Somogyi, G P

    2008-03-01

    A fast gas chromatographic mass spectrometric method has been developed earlier for the determination of amphetamine derivatives in human serum and urine. For derivatization, N-methyl-bis(trifluoroacetamide) (MBTFA) was used. Derivatization was performed using an on-line mode, since 1 microl of MBTFA and 1 microl sample extract, dissolved in toluene were injected simultaneously. In this study, the reactivity of the several amphetamine type analytes with MBTFA was investigated. MBTFA used for flash derivatization was applied undiluted on the one hand and diluted 4--4096-fold with acetonitrile on the other hand. Studying several amphetamines in the test sample spiked at the same concentrations we found that they could be divided into 3 groups based on relative target ion peak areas as a function of MBTFA dilution. Group 1, containing only primary amines showed an early increase of the relative peak areas if we increased MBTFA concentration, where group 2 (mainly N-methyl secondary amines) showed that relative peak areas started to increase intensively at higher MBTFA concentrations. Finally, MDEA as an N-ethyl secondary amine, representing group 3, showed significant increase if only slightly diluted MBTFA was used as a flash reagent. This phenomenon can be explained mainly with the less and less reactivity of amine groups in the case of groups 2 and 3, compared to group 1. These findings could help to optimise analytical methods involving flash derivatization processes.

  2. Natural gas large volumes measurement: going for on-line custody transfer; Medicao de grandes volumes de gas natural: rumo a transferencia de custodia on-line

    Energy Technology Data Exchange (ETDEWEB)

    Mercon, Eduardo G.; Frisoli, Caetano [PETROBRAS Transporte S.A. (TRANSPETRO), Rio de Janeiro, RJ (Brazil)

    2005-07-01

    This paper describes the structure of the natural gas flow measurement process in TRANSPETRO, and comments features and performance of existing or under-implantation equipment and systems, reviewing best practices and technology in use. This process runs through three interrelated segments: data flow measurement, strictly speaking; data transfer and acquisition; and data flow measurement certification (data consolidation to invoice). Initially, the work makes an approach to the data flow measurement segment, evaluating technical features of flow meters, and describing configurations and functions of the operating gas flow computers in TRANSPETRO's custody transfer stations. In this part it will also be presented the implantation of TRANSPETRO's system for gas chromatography data input on-line to flow computers. Further, in data transfer and acquisition, SCADA system technical aspects will be evaluated, considering communications protocols and programmable logic controllers functions in remote terminal units, and discussing their places in the measurement process. Additionally, TRANSPETRO's experience in data measurement certification tools is in discussion, as well as new upcoming tools and their potential features, from what new practices will be suggested. Finally, all the work has been conceived and carried out always aiming to the state-of-the-art technology in gas flow measurement: on-line custody transfer. (author)

  3. Research on technology of online gas chromatograph for SF6 decomposition products

    Science.gov (United States)

    Li, L.; Fan, X. P.; Zhou, Y. Y.; Tang, N.; Zou, Z. L.; Liu, M. Z.; Huang, G. J.

    2017-12-01

    Sulfur hexafluoride (SF6) decomposition products were qualitatively and quantitatively analyzed by several gas chromatographs in the laboratory. Test conditions and methods were selected and optimized to minimize and eliminate the SF6’ influences on detection of other trace components. The effective separation and detection of selected characteristic gases were achieved. And by comparison among different types of gas chromatograph, it was found that GPTR-S101 can effectively separate and detect SF6 decomposition products and has best the best detection limit and sensitivity. On the basis of GPTR-S101, online gas chromatograph for SF6decomposition products (GPTR-S201) was developed. It lays the foundation for further online monitoring and diagnosis of SF6.

  4. Determination of hexachlorocyclohexane pesticide residues in wool fat by a combined high-performance liquid chromatographic-gas-liquid chromatographic method

    International Nuclear Information System (INIS)

    Ali, S.L.

    1978-01-01

    Beta- and gamma-hexachlorocyclohexane residues were determined in twelve wool fat samples by using a combined high-performance liquid chromatographic (HPLC)-gas-liquid chromatographic (GLC) method. After extraction and chromatographic clean-up on a silca-gel column, the sample was further purified by HPLC on a reversed-phase C-18 column with methanol as the mobile phase. The final determination was effected by GLC with a 1-mCi nickel-63 electron-capture detector. The analytical method was checked by addition of carbon-14-labelled lindane and measurement of the radioactivity in a liquid scintillation counter. (Auth.)

  5. Measurement of water absorption capacity in wheat flour by a headspace gas chromatographic technique.

    Science.gov (United States)

    Xie, Wei-Qi; Yu, Kong-Xian; Gong, Yi-Xian

    2018-04-17

    The purpose of this work is to introduce a new method for quantitatively analyzing water absorption capacity in wheat flour by a headspace gas chromatographic technique. This headspace gas chromatographic technique was based on measuring the water vapor released from a series of wheat flour samples with different contents of water addition. According to the different trends between the vapor and wheat flour phase before and after the water absorption capacity in wheat flour, a turning point (corresponding to water absorption capacity in wheat flour) can be obtained by fitting the data of the water gas chromatography peak area from different wheat flour samples. The data showed that the phase equilibrium in the vial can be achieved in 25 min at desired temperature (35°C). The relative standard deviation of the reaction headspace gas chromatographic technique in water absorption capacity determination was within 3.48%, the relative differences has been determined by comparing the water absorption capacity obtained from this new analytical technique with the data from the reference technique (i.e., the filtration method), which are less than 8.92%. The new headspace gas chromatographic method is automated, accurate and be a reliable tool for quantifying water absorption capacity in wheat flour in both laboratory research and mill applications. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Optimization of the gas chromatographic separations; Optimacion de las separaciones cromatograficas en fase gaseosa

    Energy Technology Data Exchange (ETDEWEB)

    Gasco Sanchez, L

    1973-07-01

    A review and a critical study on the optimization of the gas chromatographic separations are made. After dealing with the fundamental gas chromatographic equations, some methods of expressing column performances are discussed: performance indices, performance parameters, resolution and effective plate number per unit time. This is completed with a comparative study on performances of various types of columns. Moreover, optimization methods for operating chromatographic conditions are extensively dealt with: as resolution optimization, separation time, and normalization techniques for the time of analysis in order to achieve the maximum resolution at constant time. Finally, some others non operating parameters such as: selectivity of stationary phases, column preparation and optimization methods by means of computers are studied. (Author) 68 refs.

  7. Large scale gas chromatographic demonstration system for hydrogen isotope separation

    International Nuclear Information System (INIS)

    Cheh, C.H.

    1988-01-01

    A large scale demonstration system was designed for a throughput of 3 mol/day equimolar mixture of H,D, and T. The demonstration system was assembled and an experimental program carried out. This project was funded by Kernforschungszentrum Karlsruhe, Canadian Fusion Fuel Technology Projects and Ontario Hydro Research Division. Several major design innovations were successfully implemented in the demonstration system and are discussed in detail. Many experiments were carried out in the demonstration system to study the performance of the system to separate hydrogen isotopes at high throughput. Various temperature programming schemes were tested, heart-cutting operation was evaluated, and very large (up to 138 NL/injection) samples were separated in the system. The results of the experiments showed that the specially designed column performed well as a chromatographic column and good separation could be achieved even when a 138 NL sample was injected

  8. Multiplex gas chromatography: an alternative concept for gas chromatographic analysis of planetary atmospheres

    Science.gov (United States)

    Valentin, J. R.

    1989-01-01

    Gas chromatography (GC) is a powerful technique for analyzing gaseous mixtures. Applied to the earth's atmosphere, GC can be used to determine the permanent gases--such as carbon dioxide, nitrogen, and oxygen--and to analyze organic pollutants in air. The U.S. National Aeronautics and Space Administration (NASA) has used GC in spacecraft missions to Mars (the Viking Biology Gas Exchange Experiment [GEX] and the Viking Gas Chromatograph-Mass Spectrometer [GC-MS]) and to Venus (the Pioneer Venus Gas Chromatograph [PVGC] on board the Pioneer Venus sounder probe) for determining the atmospheric constituents of these two planets. Even though conventional GC was very useful in the Viking and Pioneer missions, spacecraft constraints and limitations intrinsic to the technique prevented the collection of more samples. With the Venus probe, for instance, each measurement took a relatively long time to complete (10 min), and successive samples could not be introduced until the previous samples had left the column. Therefore, while the probe descended through the Venusian atmosphere, only three samples were acquired at widely separated altitudes. With the Viking mission, the sampling rate was not a serious problem because samples were acquired over a period of one year. However, the detection limit was a major disadvantage. The GC-MS could not detect simple hydrocarbons and simple alcohols below 0.1 ppm, and the GEX could not detect them below 1 ppm. For more complex molecules, the detection limits were at the parts-per-billion level for both instruments. Finally, in both the Viking and Pioneer missions, the relatively slow rate of data acquisition limited the number of analyses, and consequently, the amount of information returned. Similar constraints are expected in future NASA missions. For instance, gas chromatographic instrumentation is being developed to collect and analyze organic gases and aerosols in the atmosphere of Titan (one of Saturn's satellites). The Titan

  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. Gas chromatographic studies of the relative retention of the sulfur isotopes in carbonyl sulfide, carbon disulfide, and sulfur dioxide

    International Nuclear Information System (INIS)

    Fetzer, J.C.; Rogers, L.B.

    1980-01-01

    A precision gas chromatograph, coupled to a quadrupole mass spectrometer and an on-line computer, was used to study the fractionation on Porasil A of the 32 S/ 34 S isotopic pair in a variety of sulfur-containing molecules. Carbonyl sulfide (COS) yielded an average α value of 1.00074 +- 0.00017 (standard deviation) for the temperature range 25 0 C to 75 0 C. The carbon disulfide (CS 2 ) value was 1.00069 +- 0.00023 for the range 53 0 C to 103 0 C, and that for sulfur dioxide (SO 2 ) was 1.00090 +- 0.00018 for the range 62 0 C to 112 0 C. Differential thermodynamic data have been reported. A Porapak Q column showed no fractionation of this isotopic pair in these three molecules

  11. Improvement of gas chromatographic analysis for organic acids and ...

    African Journals Online (AJOL)

    Yomi

    2010-08-27

    Aug 27, 2010 ... short retention time and fair recognition peak of the compounds were obtained under the ... GC for acid and solvent analysis from ABE fermentation ... FID was kept at 230°C. Nitrogen gas was used as a carrier gas at a.

  12. Simple gas chromatographic system for analysis of microbial respiratory gases

    Science.gov (United States)

    Carle, G. C.

    1972-01-01

    Dual column ambient temperature system, consisting of pair of capillary columns, microbead thermistor detector and micro gas-sampling valve, is used in remote life-detection equipment for space experiments. Performance outweighs advantage gained by utilizing single-column systems to reduce weight, conserve carrier gas and operate at lower power levels.

  13. Acrylamide analysis in food by liquid chromatographic and gas chromatographic methods.

    Science.gov (United States)

    Elbashir, Abdalla A; Omar, Mei M Ali; Ibrahim, Wan Aini Wan; Schmitz, Oliver J; Aboul-Enein, Hassan Y

    2014-01-01

    Acrylamide (AA) is a compound classified as carcinogenic to humans by the International Agency for Research on Cancer. It was first discovered to be present in certain heated processed food by the Swedish National Food Administration (SNFA) and University of Stockholm in early 2002. The major pathway for AA formation in food is the Maillard reaction between reducing sugar and the amino acid asparagine at high temperature. Since the discovery of AA's presence in food, many analytical methods have been developed for determination of AA contents in different food matrices. Also, several studies have been conducted to develop extraction procedures for AA from difficult food matrices. AA is a small, highly polar molecule, which makes its extraction and analysis challenging. Many articles and reviews have been published dealing with AA in food. The aim of the review is to discuss AA formation in food, the factors affecting AA formation and removal, AA exposure assessment, AA extraction and cleanup from food samples, and analytical methods used in AA determination, such as high-performance liquid chromatography (HPLC) and gas chromatography (GC). Special attention is given to sample extraction and cleanup procedures and analytical techniques used for AA determination.

  14. Pyrolysis-gas chromatographic method for kerogen typing

    Energy Technology Data Exchange (ETDEWEB)

    Larter, S.R.; Douglas, A.G.

    1980-01-01

    The classification of kerogens according to their type and rank is important for the definition of any kerogen assemblage. Whereas optical methods of rank determination are well known, vitrinite reflectance and spore coloration being the most widely accepted chemical methods for typing kerogens are less developed. In this work we show that pyrograms, produced by pyrolyzing microgram quantities of solvent-extracted kerogens, enable not only their characterization in terms of a chromatographic fingerprint but also the production of a numerical type index determined as the ratio of m(+p)-xylene/n-octene (oct-1-ene) in the pyrogram. This index appears to be a close function of kerogen type. Type 3 kerogens (Tissot et al., 1974), including vitrinite, provide a high type index and have pyrolysates dominated by aromatic and phenolic compounds whereas type 1 kerogens provide an aliphatic-rich pyrolysate and consequently a low type index. The type index described here correlates well with microscopic and elemental analysis data and the pyrogram fingerprint provides an additional level of characterization not attainable with other current typing techniques.

  15. Non-chromatographic speciation analysis of mercury by flow injection on-line preconcentration in combination with chemical vapor generation atomic fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Wu Hong [School of Chemistry and Chemical Engineering, State Key Laboratory of Coordination Chemistry and Key Laboratory of MOE for Life Science, Nanjing University, Nanjing 210093 (China); Department of Chemistry, Xuzhou Normal University, Xuzhou 221116 (China); Jin Yan [School of Chemistry and Chemical Engineering, State Key Laboratory of Coordination Chemistry and Key Laboratory of MOE for Life Science, Nanjing University, Nanjing 210093 (China); Han Weiying [School of Chemistry and Chemical Engineering, State Key Laboratory of Coordination Chemistry and Key Laboratory of MOE for Life Science, Nanjing University, Nanjing 210093 (China); Miao, Qiang [School of Chemistry and Chemical Engineering, State Key Laboratory of Coordination Chemistry and Key Laboratory of MOE for Life Science, Nanjing University, Nanjing 210093 (China); Bi Shuping [School of Chemistry and Chemical Engineering, State Key Laboratory of Coordination Chemistry and Key Laboratory of MOE for Life Science, Nanjing University, Nanjing 210093 (China)]. E-mail: bisp@nju.edu.cn

    2006-07-15

    A novel non-chromatographic approach for direct speciation of mercury, based on the selective retention inorganic mercury and methylmercury on the inner wall of a knotted reactor by using ammonium diethyl dithiophosphate and dithizone as complexing agents respectively, was developed for flow injection on-line sorption preconcentration coupled with chemical vapor generation non-dispersive atomic fluorescence spectrometry. With the sample pH kept at 2.0, the preconcentration of inorganic mercury on the inner walls of the knotted reactor was carried out based on the exclusive retention of Hg-DDP complex in the presence of methylmercury via on-line merging the sample solution with ammonium diethyl dithiophosphate solution, and selective preconcentration methylmercury was achieved with dithizone instead of ammonium diethyl dithiophosphate. A 15% (v/v) HCl was introduced to elute the retained mercury species and merge with KBH{sub 4} solution for atomic fluorescence spectrometry detection. Under the optimal experimental conditions, the sample throughputs of inorganic mercury and methylmercury were 30 and 20 h{sup -1} with the enhancement factors of 13 and 24. The detection limits were found to be 3.6 ng l{sup -1} for Hg{sup 2+} and 2.0 ng l{sup -1} for CH{sub 3}Hg{sup +}. The precisions (RSD) for the 11 replicate measurements of each 0.2 {mu}g l{sup -1} of Hg{sup 2+} and CH{sub 3}Hg{sup +} were 2.2% and 2.8%, respectively. The developed method was validated by the analysis of certified reference materials (simulated natural water, rice flour and pork) and by recovery measurements on spiked samples, and was applied to the determination of inorganic mercury and methylmercury in biological and environmental water samples.

  16. Non-chromatographic speciation analysis of mercury by flow injection on-line preconcentration in combination with chemical vapor generation atomic fluorescence spectrometry

    International Nuclear Information System (INIS)

    Wu Hong; Jin Yan; Han Weiying; Miao, Qiang; Bi Shuping

    2006-01-01

    A novel non-chromatographic approach for direct speciation of mercury, based on the selective retention inorganic mercury and methylmercury on the inner wall of a knotted reactor by using ammonium diethyl dithiophosphate and dithizone as complexing agents respectively, was developed for flow injection on-line sorption preconcentration coupled with chemical vapor generation non-dispersive atomic fluorescence spectrometry. With the sample pH kept at 2.0, the preconcentration of inorganic mercury on the inner walls of the knotted reactor was carried out based on the exclusive retention of Hg-DDP complex in the presence of methylmercury via on-line merging the sample solution with ammonium diethyl dithiophosphate solution, and selective preconcentration methylmercury was achieved with dithizone instead of ammonium diethyl dithiophosphate. A 15% (v/v) HCl was introduced to elute the retained mercury species and merge with KBH 4 solution for atomic fluorescence spectrometry detection. Under the optimal experimental conditions, the sample throughputs of inorganic mercury and methylmercury were 30 and 20 h -1 with the enhancement factors of 13 and 24. The detection limits were found to be 3.6 ng l -1 for Hg 2+ and 2.0 ng l -1 for CH 3 Hg + . The precisions (RSD) for the 11 replicate measurements of each 0.2 μg l -1 of Hg 2+ and CH 3 Hg + were 2.2% and 2.8%, respectively. The developed method was validated by the analysis of certified reference materials (simulated natural water, rice flour and pork) and by recovery measurements on spiked samples, and was applied to the determination of inorganic mercury and methylmercury in biological and environmental water samples

  17. Evaluation of serpentine ore as a nuclear shielding material using gas chromatographic techniques

    International Nuclear Information System (INIS)

    Singh, B.N.; Unnikrishnan, E.K.; Kumar, Sangita D.

    2007-01-01

    Serpentine ore mixed with cement has been recognized as a candidate shielding material for use in nuclear reactors because of its many desirable properties. Therefore the assessment of serpentine ore for release of volatile gases during exposure to elevated temperatures, irradiation and changes in chemical composition, is essential. The present paper deals with the studies on the serpentine ores using gas chromatography and combustion gas chromatographic techniques. (author)

  18. On-Line Enrichment Monitor for UF{sub 6} Gas Centrifuge Enrichment Plant

    Energy Technology Data Exchange (ETDEWEB)

    Ianakiev, K. D.; Boyer, B.; Favalli, A.; Goda, J. M.; Hill, T.; Keller, C.; Lombardi, M.; Paffett, M.; MacArthur, D. W.; McCluskey, C.; Moss, C. E.; Parker, R.; Smith, M. K.; Swinhoe, M. T. [Los Alamos National Laboratory, Los Alamos (United States)

    2012-06-15

    This paper is a continuation of the Advanced Enrichment Monitoring Technology for UF{sub 6} Gas Centrifuge Enrichment Plant (GCEP) work, presented in the 2010 IAEA Safeguards Symposium. Here we will present the system architecture for a planned side-by-side field trial test of passive (186-keV line spectroscopy and pressure-based correction for UF{sub 6} gas density) and active (186-keV line spectroscopy and transmission measurement based correction for UF{sub 6} gas density) enrichment monitoring systems in URENCO's enrichment plant in Capenhurst. Because the pressure and transmission measurements of UF{sub 6} are complementary, additional information on the importance of the presence of light gases and the UF{sub 6} gas temperature can be obtained by cross-correlation between simultaneous measurements of transmission, pressure and 186-keV intensity. We will discuss the calibration issues and performance in the context of accurate, on-line enrichment measurement. It is hoped that a simple and accurate on-line enrichment monitor can be built using the UF{sub 6} gas pressure provided by the Operator, based on online mass spectrometer calibration, assuming a negligible (a small fraction of percent) contribution of wall deposits. Unaccounted-for wall deposits present at the initial calibration will lead to unwanted sensitivity to changes in theUF{sub 6} gas pressure and thus to error in the enrichment results. Because the accumulated deposits in the cascade header pipe have been identified as an issue for Go/No Go measurements with the Cascade Header Enrichment Monitor (CHEM) and Continuous Enrichment Monitor (CEMO), it is important to explore their effect. Therefore we present the expected uncertainty on enrichment measurements obtained by propagating the errors introduced by deposits, gas density, etc. and will discuss the options for a deposit correction during initial calibration of an On-Line Enrichment Monitor (OLEM).

  19. An on-line gas control system using an artificial intelligence language: PROLOG II

    International Nuclear Information System (INIS)

    Lai, C.

    1990-01-01

    An application of Artificial Intelligence to a real physics experiment is presented. This allows comparison with classical programming techniques. The PROLOG language appears as a convenient on-line language, easily interfaced to the low level service routines, for which algorithmic languages can still be used. Steering modules have been written for a gas acquisition and analysis program, and for a control system with graphic human interface. This system includes safety rules and automatic action sequences

  20. Physicochemical, thin layer and gas-liquid chromatographic ...

    African Journals Online (AJOL)

    DELL

    2012-05-22

    May 22, 2012 ... PEG (3 m × 3 mm I. D.) was used for gas chromatography. Physicochemical analysis ... subjected to thin layer chromatography on plates (20 × 20 cm) having 0.25 mm thick silica gel ..... Headspace solid- phase microextraction ...

  1. Gas Chromatographic-Mass Spectrometric Analysis of Essential Oil ...

    African Journals Online (AJOL)

    Purpose: To analyze the essential oil composition of the flower of Jasminum officinale L. var. grandifloroum L. (Jasminum grandiflorum) by gas chromatography-mass spectrometry (GC-MS). Methods: The optimum GC-MS conditions used for the analysis were 250 oC inlet temperature, 150 oC MSD detector temperature, ...

  2. On-line gas mixing and multi-channel distribution system

    International Nuclear Information System (INIS)

    Kalmani, S.D.; Mondal, N.K.; Satyanarayana, B.; Verma, P.; Joshi, Avinash

    2009-01-01

    In this presentation, we describe a mass-flow controller based on-line gas mixing unit with the multi-channel distribution system. We highlight different aspects such as requirement, design, calibration, control and operation of this system. This unit has the capability to mix up to four different input gases and distribute over 16 output channels. Output in individual channels is controlled accurately by using capillary-based system. At present, we are using this gas mixing unit for prototype of iron calorimeter (ICAL) detector of India-based Neutrino Observatory (INO).

  3. TBP degradation products. Separation and gas-chromatographic determination

    International Nuclear Information System (INIS)

    Kuada, T.A.; Alem, C.M.; Matsuda, H.T.; Araujo, B.F. de; Araujo, J.A de.

    1991-11-01

    A separation method for di butylphosphate, mono butylphosphate and phosphoric acid as degradation products in organic and aqueous streams of the process containing variable amounts of actinides and fission products is described. The products were separated by extraction and after methylation the final determination was carried out by gas chromatography. TPP was used as internal standard and 5 to 500 mg/L concentration range was determined with 1 to 10% deviation depending on the concentration of organo phosphates. (author)

  4. Adsorption and gas-chromatographic properties of tungsten selenide

    International Nuclear Information System (INIS)

    Gavrilova, T.B.; Kiselev, A.V.; Roshchina, T.M.

    1988-01-01

    Method of gas chromatography was used to investigate the surface properties of a series of tungsten selenide WSe 2 samples as well as to determine the role of geometrical and electronic structure of adsorbate molecules and their orientation with respect to the surface during adsorption on WSe 2 . Thermodynamic characteristics of hydrocarbon C 6 -C 10 adsorption at surface occupation close to the zero one were determined. Correlation of the values of thermodynamic characteristics of saturated and aromatic hydrocarbon adsorption enabled to refer WSe 2 to nonspecific adsorbents. It is noted that the main role during hydrocarbon adsorption on WSe 2 is played by nonpolar basic facets, occupied by selenium atoms

  5. Gas chromatographic analysis of extractive solvent in reprocessing plants

    International Nuclear Information System (INIS)

    Marlet, B.

    1984-01-01

    Operation of a reprocessing plant using the Purex process is recalled and analytical controls for optimum performance are specified. The aim of this thesis is the development of analytical methods using gas chromatography required to follow the evolution of the extraction solvent during spent fuel reprocessing. The solvent at different concentrations, is analysed along the reprocessing lines in organic or aqueous phases. Solvent degradation interferes with extraction and decomposition products are analysed. The solvent becomes less and less efficient, also it is distilled and quality is checked. Traces of solvent should also be checked in waste water. Analysis are made as simple as possible to facilitate handling of radioactive samples [fr

  6. Increasing of MERARG experimental performances: on-line fission gas release measurement by mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Pontillon, Y.; Capdevila, H.; Clement, S. [CEA, DEN, DEC, SA3C, LAMIR, F-13108 Saint Paul lez Durance, (France); Guigues, E.; Janulyte, A.; Zerega, Y.; Andre, J. [Aix-Marseille Universite, LISA EA 4672, 13397 MARSEILLE cedex 20, (France)

    2015-07-01

    The MERARG device - implemented at the LECASTAR Hot Laboratory, at the CEA Cadarache - allows characterizing nuclear fuels with respect to the behaviour of fission gases during thermal transients representative of normal or off normal operating nuclear power plant conditions. The fuel is heated in order to extract a part or the total gas inventory it contains. Fission Gas Release (FGR) is actually recorded by mean of both on-line gamma spectrometry station and micro gas chromatography. These two devices monitor the quantity and kinetics of fission gas release rate. They only address {sup 85}Kr radioactive isotope and the elemental quantification of Kr, Xe and He (with a relatively low detection limit in the latter case, typically 5-10 ppm). In order to better estimate the basic mechanisms that promote fission gas release from irradiated nuclear fuels, the CEA fuel study department decided to improve its experimental facility by modifying MERARG to extend the studies of gamma emitter fission gases to all gases (including Helium) with a complete isotopic distribution capability. To match these specifications, a Residual Gas Analyser (RGA) has been chosen as mass spectrometer. This paper presents a review of the main aspects of the qualification/calibration phase of the RGA type analyser. In particular, results recorded over three mass ranges 1-10 u, 80-90 u and 120-140 u in the two classical modes of MERARG, i.e. on-line and off-line measurements are discussed. Results obtained from a standard gas bottle show that the quantitative analysis at a few ppm levels can be achieved for all isotopes of Kr and Xe, as well as masses 2 and 4 u. (authors)

  7. Chromatographic measurement of hydrogen isotopic and permanent gas impurities in tritium

    International Nuclear Information System (INIS)

    Warner, D.K.; Kinard, C.; Bohl, D.C.

    1976-01-01

    This paper describes a gas chromatograph that was designed for dedicated analysis of hydrogen isotopic and permanent gas impurities in tritium and tritium-deuterium mixtures. The instrument that was developed substantially improved the accuracy and precision of hydrogen isotopic analysis in the 20 ppM to one mole percent range as compared with other analytical methods. Several unique design features of the instrument were required due to the radiation and isotopic exchange properties of the tritium in the samples; descriptions of these features are presented along with details of the complete chromatographic system. The experimental procedures used to calibrate the detector and statistically evaluate its performance are given, and the sources of analytical error are cited. The limitations of the present system are also discussed

  8. Detection of irradiated fruits and vegetables by gas-chromatographic methods and electron spin-resonance

    Energy Technology Data Exchange (ETDEWEB)

    Farag, S.E.A. (National Centre for Radiation Research and Technology, Cairo (Egypt))

    1993-01-01

    Gas chromatographic methods detected some hydrocarbons esp. 17:1, 16:2, 15:0 and 14:1 in irradiated, Avocado, Papaya, Mangoes with 0.75, 1.5, 3.0 kGy and Apricot with 0.5 and 3.0 kGy. The detection of hydrocarbons was clearly at high doses but the low doses need more sensitive conditions using Liquid-Liquid-Gas chromatographic method as used here. Using Electron Spin-Resonance, produce a specific signal from irradiated onion (dried leaves) as well as apricot (hard coat of kernels) after some weeks of irradiation process but not clear with the other foodstuffs. (orig.)

  9. Gas chromatographic determination of calcium propionate added as preservative to bread.

    Science.gov (United States)

    Lamkin, W M; Unruh, N C; Pomeranz, Y

    1987-01-01

    A simple and rapid gas chromatographic procedure was developed for determining low concentrations of propionate added as a preservative to bread. A bread sample to be analyzed was ground in a meat grinder with a 3 mm hole plate and finely divided by rubbing through a No. 8 sieve. The propionate was then extracted into 0.050M formic acid in a blender at low speed for 5 min, and an aliquot of a filtrate was analyzed directly by gas chromatography. Chromatographic separation was accomplished on a Carbopack C column coated with 0.3% (w/w) Carbowax 20M and 0.1% (w/w) phosphoric acid. Less than 0.2 ppm propionic acid could be detected in the aqueous extract. Over the range of 0.03-0.23% calcium propionate, average relative error was -1.20% with an average coefficient of variation of 2.02%.

  10. Detection of radiation-induced hydrocarbons in Camembert irradiated before and after the maturing process-comparison of florisil column chromatography and on-line coupled liquid chromatography-gas chromatography

    International Nuclear Information System (INIS)

    Schulzki, G.; Spiegelberg, A.; Bögl, K.W.; Schreiber, G.A.

    1995-01-01

    The influence of the maturing process on the detection of radiation-induced volatile hydrocarbons in the fat of Camembert has been investigated. Two analytical methods for separation of the hydrocarbon fraction from the lipid were applied: Florisil column chromatography with subsequent gas chromatographic-mass spectrometric (GC-MS) determination as well as on-line coupled liquid chromatography-GC-MS. The maturing process had no influence on the detection of radiation-induced volatiles. Comparable results were achieved with both analytical methods. However, preference is given to the more effective on-line coupled LC-GC method

  11. Multidimensional High-Resolution Gas Chromatographic Investigations of Hydrocarbon Fuels and Various Turbine Engine Fuel Precursors.

    Science.gov (United States)

    1985-08-01

    time were spurious transits observed during the recording of the chromatographic output data. *Packaged gas purification filters supplied by Alltech ... Alltech ) that were needed for these unusual installations. When the column diameters were small and of comparable size, the assembly attach- ments at...into an MDGC system has definite advantages as separations can be made faster and with greater detectability. However, specific precautions must be

  12. The adaptive internet application for interpretation of the transformer oil gas chromatographic analysis results

    Directory of Open Access Journals (Sweden)

    Polužanski Vladimir

    2015-01-01

    Full Text Available This paper describes an adaptive Internet application for the interpretation of the transformer oil gas chromatographic analysis results. The first version of the application is developed by following an evolutionary software development concept. The most important software development risks and the appropriate solutions are described. An open-source web framework named Bootstrap is used for an application implementation. The application is developed by using ASP.NET and MS SQL server.

  13. 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.

  14. On-line valve monitoring at the Ormen Lange gas plant

    Energy Technology Data Exchange (ETDEWEB)

    Greenlees, R.; Hale, S. [Score Atlanta Inc., Kennesaw, Georgia (United States)

    2011-07-01

    The purpose of this presentation is to discuss replacing time and labor intensive nuclear outage activities with on line condition monitoring solutions, primarily the periodic verification of MOV functionality discussed in USNRC Generic Letter 96.05. This regulation requires that MOV age related performance degradations are properly identified and accounted for, causing utilities to have to retest valves periodically for the duration of the plants operating license. AECL designed CANDU reactors have a world class performance and safety record, with typical average annual capacity factors of 90%. The CANDU reactor design has the ability to refuel on line, as a result (a) it can be a challenge scheduling all required valve testing into limited duration outage work windows, (b) at multi unit sites, Unit 0 valves can be difficult to test because they are rarely ever out of service, (c) deuterium-oxide (heavy water) moderator is expensive to manufacture, as a result, effective through valve leakage monitoring is essential. These three factors alone make CANDU sites the most suitable candidates for on line valve monitoring systems. Nuclear industry regulations have been instrumental in the development of 'at the valve' diagnostic systems, but diagnostic testing has not typically been utilized to the same degree in other less regulated industries. However, that trend is changing, and the move toward valve diagnostics and condition monitoring has moved fastest in the offshore oil and gas industry on the Norwegian side of the North Sea. The Ormen Lange plant, located on Nyhamna Island on the west coast of Norway, operated by Shell, is one of the worlds most advanced gas processing plants. A stated maintenance goal for the plant is that 70% of the maintenance budget and spend should be based on the results of on line condition monitoring, utilizing monitoring systems equipped with switch sensing, strain gages, hydraulic and pneumatic pressure transducers and

  15. On-line valve monitoring at the Ormen Lange gas plant

    International Nuclear Information System (INIS)

    Greenlees, R.; Hale, S.

    2011-01-01

    The purpose of this presentation is to discuss replacing time and labor intensive nuclear outage activities with on line condition monitoring solutions, primarily the periodic verification of MOV functionality discussed in USNRC Generic Letter 96.05. This regulation requires that MOV age related performance degradations are properly identified and accounted for, causing utilities to have to retest valves periodically for the duration of the plants operating license. AECL designed CANDU reactors have a world class performance and safety record, with typical average annual capacity factors of 90%. The CANDU reactor design has the ability to refuel on line, as a result (a) it can be a challenge scheduling all required valve testing into limited duration outage work windows, (b) at multi unit sites, Unit 0 valves can be difficult to test because they are rarely ever out of service, (c) deuterium-oxide (heavy water) moderator is expensive to manufacture, as a result, effective through valve leakage monitoring is essential. These three factors alone make CANDU sites the most suitable candidates for on line valve monitoring systems. Nuclear industry regulations have been instrumental in the development of 'at the valve' diagnostic systems, but diagnostic testing has not typically been utilized to the same degree in other less regulated industries. However, that trend is changing, and the move toward valve diagnostics and condition monitoring has moved fastest in the offshore oil and gas industry on the Norwegian side of the North Sea. The Ormen Lange plant, located on Nyhamna Island on the west coast of Norway, operated by Shell, is one of the worlds most advanced gas processing plants. A stated maintenance goal for the plant is that 70% of the maintenance budget and spend should be based on the results of on line condition monitoring, utilizing monitoring systems equipped with switch sensing, strain gages, hydraulic and pneumatic pressure transducers and acoustic leakage

  16. On-Line Fission Gas Release Monitoring System in the High Flux Reactor Petten

    International Nuclear Information System (INIS)

    Laurie, M.; Fuetterer, M. A.; Appelman, K.H.; Lapetite, J.-M.; Marmier, A.; Knol, S.; Best, J.

    2013-06-01

    For HTR fuel irradiation tests in the HFR Petten a specific installation was designed and installed dubbed the 'Sweep Loop Facility' (SLF). The SLF is tasked with three functions, namely temperature control by gas mixture technique, surveillance of safety parameters (temperature, pressure, radioactivity etc.) and analysis of fission gas release for three individual capsules in two separate experimental rigs. The SLF enables continuous and independent surveillance of all gas circuits. The release of volatile fission products (FP) from the in-pile experiments is monitored by continuous gas purging. The fractional release of these FP, defined as the ratio between release rate of a gaseous fission isotope (measured) to its instantaneous birth rate (calculated), is a licensing-relevant test for HTR fuel. The developed gamma spectrometry station allows for higher measurement frequencies, thus enabling follow-up of rapid and massive release transients. The designed stand-alone system was tested and fully used through the final irradiation period of the HFR-EU1 experiment which was terminated on 18 February 2010. Its robustness allowed the set up to be used as extra safety instrumentation. This paper describes the gas activity measurement technique based on HPGe gamma spectrometry and illustrates how qualitative and quantitative analysis of volatile FP can be performed on-line. (authors)

  17. Characteristics of a gas-jet transport system for an on-line isotope separator

    International Nuclear Information System (INIS)

    Kawade, K.; Yamamoto, H.; Amano, H.; Hanada, M.; Katoh, T.; Okano, K.; Kawase, Y.; Fujiwara, I.

    1982-01-01

    Basic characteristics of a gas-jet transport system for an on-line isotope separator have been investigated using a 252 Cf source and a 235 U fission source. The transport efficiency of fission products through a capillary has been measured to be about 60% for the 235 U fission source. The sweep-out time of fission products through a target chamber and the transit time through a capillary have been measured for He, N 2 and CO 2 gases at several pressures. The measured sweep-out times have been almost equal to the exchange over time of the gas. The transit times have been found to be reasonably predicted by calculations. The transport system has been incorporated into the KUR-ISOL and is used for the study of short-lived nuclei. (orig.)

  18. Gas-liquid chromatographic determination of resmethrin in corn, cornmeal, flour, and wheat.

    Science.gov (United States)

    Simonaitis, R A; Cail, R S

    1975-09-01

    A gas-liquid chromatographic (GLC) method was developed for the determination of residues of resmethrin ((5-benzyl-3-furyl)methyl cis-trans-(+/-)-2,2-dimethyl-3-(2-methylpropenyl)-cyclopropanecarboxylate) in corn, cornmeal, flour, and wheat. The commodity, fortified with resmethrin, was extracted by tumbling with pentane and transferred to acetonitrile, the fat was partitioned off, and the sample was chromatographed with 3% ethyl acetate in pentane on Florisil containing 0.5% water. The resmethrin residue was determined by GLC with a flame ionization detector. The results were compared with known standards that had undergone the same cleanup procedures. The method was sensitive to concentrations of resmethrin to 0.2 ppm, recoveries averaged 83%, and reproducibility was good.

  19. New method for evaluating irreversible adsorption and stationary phase bleed in gas chromatographic capillary columns.

    Science.gov (United States)

    Wright, Bob W; Wright, Cherylyn W

    2012-10-26

    A novel method is described for the evaluation of irreversible adsorption and column bleed in gas chromatographic (GC) columns using a tandem GC approach. This work specifically determined the degree of irreversible adsorption behavior of specific sulfur and phosphorous containing test probe compounds at levels ranging from approximately 50 picograms (pg) to 1 nanogram (ng) on selected gas chromatographic columns. This method does not replace existing evaluation methods that characterize reversible adsorption but provides an additional tool. The test compounds were selected due to their ease of adsorption and their importance in the specific trace analytical detection methodology being developed. Replicate chromatographic columns with 5% phenylmethylpolysiloxane (PMS), polyethylene glycol (wax), trifluoropropylpolysiloxane (TFP), or 78% cyanopropylpolysiloxane stationary phases from a variety of vendors were evaluated. As expected, the results demonstrate that the different chromatographic phases exhibit differing degrees of irreversible adsorption behavior. The results also indicate that all manufacturers do not produce equally inert columns nor are columns from a given manufacturer identical. The wax-coated columns for the test probes used were more inert as a group than 5% PMS coated columns, and they were more reproducibly manufactured. Both TFP and 78% cyanopropylpolysiloxane columns displayed superior inertness to the test compounds compared to either 5% PMS- or wax-coated columns. Irreversible adsorption behavior was characterized for a limited range of stationary phase film thicknesses. In addition, the method was shown effective for characterizing column bleed and methods to remove bleed components. This method is useful in screening columns for demanding applications and to obtain diagnostic information related to improved preparation methods. Copyright © 2012 Elsevier B.V. All rights reserved.

  20. Headspace gas chromatographic method for the measurement of difluoroethane in blood.

    Science.gov (United States)

    Broussard, L A; Broussard, A; Pittman, T; Lafferty, D; Presley, L

    2001-01-01

    To develop a gas chromatographic assay for the analysis of difluoroethane, a volatile substance, in blood and to determine assay characteristics including linearity, limit of quantitation, precision, and specificity. Referral toxicology laboratory Difluoroethane, a colorless, odorless, highly flammable gas used as a refrigerant blend component and aerosol propellant, may be abused via inhalation. A headspace gas chromatographic procedure for the identification and quantitation of difluoroethane in blood is presented. A methanolic stock standard prepared from pure gaseous difluoroethane was used to prepare whole blood calibrators. Quantitation of difluoroethane was performed using a six-point calibration curve and an internal standard of 1-propanol. The assay is linear from 0 to 115 mg/L including a low calibrator at 4 mg/L, the limit of quantitation. Within-run coefficients of variation at mean concentrations of 13.8 mg/L and 38.5 mg/L were 5.8% and 6.8% respectively. Between-run coefficients of variation at mean concentrations of 15.9 mg/L and 45.7 mg/L were 13.4% and 9.8% respectively. Several volatile substances were tested as potential interfering compounds with propane having a retention time identical to that of difluoroethane. This method requires minimal sample preparation, is rapid and reproducible, can be modified for the quantitation of other volatiles, and could be automated using an automatic sampler/injector system.

  1. Optimum yields of dibenzylbutyrolactone-type lignans from Cynareae fruits, during their ripening, germination and enzymatic hydrolysis processes, determined by on-line chromatographic methods.

    Science.gov (United States)

    Szokol-Borsodi, Lilla; Sólyomváry, Anna; Molnár-Perl, Ibolya; Boldizsár, Imre

    2012-01-01

    Dibenzylbutyrolactone-type lignans are the physiologically active constituents of the achene fruits of Cynareae. These lignans occur in glycoside/aglycone forms: in the highest quantity of the arctiin/arctigenin, matairesinoside/matairesinol and tracheloside/trachelogenin pairs found in the fruits of Arctium lappa L., Centaurea scabiosa L. and Cirsium arvense (L.) Scop. To optimise the extraction yield of the arctiin/arctigenin, matairesinoside/matairesinol and tracheloside/trachelogenin glycoside/aglycone pairs, from the fruits of Arctium lappa, Centaurea scabiosa and Cirsium arvense, under the ripening, germination and enzymatic hydrolysis processes of the fruits. Identification and quantification of lignans were performed with on-line gas chromatography-mass spectrometry (GC-MS) and with high performance liquid chromatography (HPLC), both with UV and mass selective detections (HPLC-UV/MS). As novelties to the field it was confirmed that: (i) the unripe fruits provide a high amount of lignans, similar to the ripe fruit; (ii) the fruits of Arctium lappa and Cirsium arvense do have glycosidase activity to hydrolyse their lignan glycosides into free lignans; (iii) the glycosidase of Centaurea scabiosa fruit becomes activated under its germination process only; and (iv) the overwhelming part of the fruits lignan contents (80-94%) in all three species are accumulated in the embryo. The best sources of (i) lignan aglycones are the enzyme-hydrolysed embryos, separating spontaneously during the germination process, and (ii) lignan glycosides are the unripe fruits. Copyright © 2012 John Wiley & Sons, Ltd.

  2. Gas chromatographic sensing on an optical fiber by mode-filtered light detection.

    Science.gov (United States)

    Bruckner, C A; Synovec, R E

    1996-06-01

    A chemical sensor for gas phase measurements is reported which combines the principles of chemical separation and fiber optic detection. The analyzer incorporates an annular column Chromatographic sensor, constructed by inserting a polymer-clad optical fiber into a silica capillary. Light from a helium-neon laser is launched down the fiber, producing a steady intensity distribution within the fiber, but a low background of scattered light. When sample vapor is introduced to the sensor, and an analyte-rich volume interacts with the polymer cladding, Chromatographic retention is observed simultaneously with a change in the local refractive index of the cladding. An increase in cladding refractive index (RI) causes light to be coupled out of the fiber, with detection at a right-angle to the annular column length to provide optimum S/N ratio. This detection mechanism is called mode-filtered light detection. We report a gas Chromatographic separation on a 3.1 m annular column (320 microm i.d. silica tube, 228 microm o.d. fiber with a 12 microm fluorinated silicone clad) of methane, benzene, butanone and chlorobenzene in 6 min. The annular column length was reduced to 22 cm to function as a sensor, with selected organic vapors exhibiting unique retention times and detection selectivity. The detection selectivity is determined by the analyte RI and the partition coefficient into the cladding. The calculated limit of detection (LOD) for benzene vapor is 0.03% by volume in nitrogen, and several chlorinated species had LOD values less than 1%. For binary mixtures of organic vapors, the detected response appears to be the linear combination of the two organic standards, suggesting that the annular column may be useful as a general approach for designing chemical sensors that incorporate separation and optical detection principles simultaneously.

  3. A system for accurate on-line measurement of total gas consumption or production rates in microbioreactors

    NARCIS (Netherlands)

    van Leeuwen, Michiel; Heijnen, Joseph J.; Gardeniers, Johannes G.E.; Oudshoorn, Arthur; Noorman, Henk; Visser, Jan; van der Wielen, Luuk A.M.; van Gulik, Walter M.

    2009-01-01

    A system has been developed, based on pressure controlled gas pumping, for accurate measurement of total gas consumption or production rates in the nmol/min range, applicable for on-line monitoring of bioconversions in microbioreactors. The system was validated by carrying out a bioconversion with

  4. 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.

  5. A Gas Chromatographic Method for the Determination of Bicarbonate and Dissolved Gases

    Directory of Open Access Journals (Sweden)

    John H. Loughrin

    2017-11-01

    Full Text Available A gas chromatographic method for the rapid determination of aqueous carbon dioxide and its speciation into solvated carbon dioxide and bicarbonate is presented. One-half mL samples are injected through a rubber septum into 20-mL vials that are filled with 9.5 mL of 0.1 N HCl. A one mL portion of the headspace is withdrawn and injected onto a gas chromatograph equipped with a thermal conductivity detector. Using the dimensionless Henry's constant for carbon dioxide and an adaptation of the Henderson-Hasselbalch equation, carbon dioxide in the samples can be categorized among solvated, bicarbonate, and carbonate forms. Natural water samples as well as wastewater from a municipal sewage treatment plant and a swine rearing operation were analyzed by this method and the results compared favorably to those obtained by titration. Samples stored for up to 5 weeks showed no significant changes in carbon dioxide concentrations. In addition, using flame ionization and electron capture detectors, methane and nitrous oxide concentrations in the samples were also measured.

  6. Application of Gas Chromatographic analysis to RPC detectors in the ATLAS experiment at CERN-LHC

    CERN Document Server

    De Asmundis, R

    2007-01-01

    Starting from 2007 a large number (1200) Resistive Plate Chambers (RPC) detectors will be used as muon trigger detectors in the ATLAS Experiment at CERN-LHC accelerator. RPC are gaseous detector in which the quality and the stability of the gas mixture as well as the design of the gas supplying system, play a fundamental role in their functioning. RPC are foreseen to work more than ten years in the high radiation environment of ATLAS and the gas mixture acts really as a "lifeguard" for the detectors. For this reason a great attention has been devoted to the gas studies in order to optimize RPC performance, robustness and reliability in a high radiation environment. In this paper we describe the work done to decide how to supply and control in an optimal way the gas to the detectors, in order to ensure their best performance for a long time. The activity, based on Gas Chromatographic (GC) analysis, has been carried on a sample of final RPC working in radiation conditions much more intense than those foreseen f...

  7. Detection system for a gas chromatograph. [. cap alpha. -methylnaphthalene,. beta. -methylnapthalene

    Science.gov (United States)

    Hayes, J.M.; Small, G.J.

    1982-04-26

    A method and apparatus are described for the quantitative analysis of vaporizable compounds, and in particular of polycyclic aromatic hydrocarbons which may be induced to fluoresce. The sample to be analyzed is injected into a gas chromatography column and is eluted through a narrow orifice into a vacuum chamber. The free expansion of the eluted sample into the vacuum chamber creates a supersonic molecular beam in which the sample molecules are cooled to the extent that the excited vibrational and rotational levels are substantially depopulated. The cooled molecules, when induced to fluoresce by laser excitation, give greatly simplified spectra suitable for analytical purposes. The laser induced fluorimetry provides great selectivity, and the gas chromatograph provides quantitative transfer of the sample to the molecular beam. 3 figures, 2 tables.

  8. Qualification of an Agilent Technologies 7890A gas chromatograph used in the biotechnology industry

    International Nuclear Information System (INIS)

    Alvarez Gonzalez, Alberto; Tambara Hernandez, Yanet; Alvarez Gil, Felix

    2014-01-01

    The drug manufacture is governed by strict international standards that guarantee reproducibility and consistency of results. The qualification of the instruments used in the productive processes, as well as in the characterization of products and their quality control are prerequisites to the validation of any analytical technique using them. One of the instrumental techniques used in the biotechnical industry is Gas Chromatography. A standard of pure caffeine was used for analysis in addition to a HP-5 30 m x 0,32 mm d.i. and 0,33 μm thick film column was used in a Gas Chromatograph coupled with a Flame Ionization Detector. For the testing of the different modules involved in the analysis (injector, column, oven and detector), an experimental design was made to estimate several parameters

  9. Gas chromatographic determination of Di-n-butyl phosphate in radioactive lean organic solvent of FBTR carbide fuel reprocessing

    International Nuclear Information System (INIS)

    Velavendan, P.; Ganesh, S.; Pandey, N.K.; Kamachi Mudali, U.; Natarajan, R.

    2011-01-01

    In the present work Di-n- butyl phosphate (DBP) a degraded product of Tri-n-butyl phosphate (TBP) formed by acid hydrolysis and radiolysis in the PUREX process was analyzed. Lean organic streams of different fuel burn-up FBTR carbide fuel reprocessing solution was determined by standard Gas Chromatographic technique. The method involves the conversion of non-volatile Di-n-butyl phosphate into volatile and stable derivatives by the action of diazomethane and then determined by Gas Chromatograph (GC). A calibration graph was made for DBP concentration range of 200-2000 ppm with correlation coefficient of 0.99587 and RSD 1.2 %. (author)

  10. Investigation of gas discharge ion sources for on-line mass separation

    International Nuclear Information System (INIS)

    Kirchner, R.

    1976-03-01

    The development of efficient gas discharge ion sources with axial beam extraction for on-line mass separation is described. The aim of the investigation was to increase the ion source temperature, the lifetime and the ionisation yield in comparison to present low-pressure are discharge ion sources and to reduce the ion current density from usually 1 to 100 mA/cm 3 . In all ion sources the pressure range below the minimal ignition pressure of the arc discharge was investigated. As a result an ion source was developed which works at small changes in geometry and in electric device of a Nielsen source with high ionization yield (up to 50% for xenon) stabil and without ignition difficulties up to 10 -5 Torr. At a typical pressure of 3 x 10 -5 Torr ion current and ion current density are about 1 μA and 0.1 mA/cm 3 respectively besides high yield and a great emission aperture (diameter 1.2 mm). (orig.) [de

  11. Measurement method for benzene, toluene, and xylene in the atmosphere by the gas chromatographic method

    Energy Technology Data Exchange (ETDEWEB)

    Shiroyama, H

    1975-08-01

    The chromatographic method for measuring benzene, toluene, and xylene (three isomers) in the atmosphere was evaluated using the Varian model 2740-10 gas chromatograph. As a solvent, n-hexane was most suitable, and the detection limit was improved by increasing the purity of n-hexane. The calibration curves were prepared, the recovery rate was calculated (76.0-99.4 percent), and the correlation coefficient was obtained from regression curves (r equals 0.97-0.99). Samples collected at a naphtha cracking plant, an aluminum smelting mill, a pharmaceutical plant, a carbon electrode manufacturing plant, a plywood manufacturing plant, a plastic bathtub manufacturing plant, and along a major highway were analyzed. All three substances were detected in all samples with the concentration of toluene high compared to the other two. Among xylene isomers, the concentration of p-xylene was always the lowest while m- and o-xylene varied from place to place. In the atmosphere along the highway, the benzene, toluene, and xylene determined were 0.01-0.09 ppM. No benzene, toluene, and xylene were detected in atmospheric samples used as controls.

  12. Gas chromatographic determination of residual hydrazine and morpholine in boiler feed water and steam condensates

    International Nuclear Information System (INIS)

    Vatsala, S.; Bansal, V.; Tuli, D.K.; Rai, M.M.; Jain, S.K.; Srivastava, S.P.; Bhatnagar, A.K.

    1994-01-01

    Hydrazine, an oxygen scavenger in boiler water, was derivatised to the corresponding acetone azine and determined at the ng ml -1 level by gas chromatography. Morpholine, a corrosion inhibitor used in steam boilers, was estimated either directly (if >2.0 μg ml -1 ) or by quantitative preconcentration (0.1 ng-2.0 μg ml -1 ). To obtain symmetrical peaks for these amines, the column packing was coated with KOH. Use of a nitrogen-specific detector improved accuracy of estimation of hydrazine and morpholine, giving a RSD of 1.9-3.6%. Chromatographic analysis of these amines in boiler feed water and steam condensate samples collected from boilers servicing a pertroleum refinery is described. Environmental safety regulations calls for monitoring of hydrazine and the methods developed can easily be adapted for this purpose. (orig.)

  13. Use of adsorption and gas chromatographic techniques in estimating biodegradation of indigenous crude oils

    International Nuclear Information System (INIS)

    Kokub, D.; Allahi, A.; Shafeeq, M.; Khalid, Z.M.; Malik, K.A.; Hussain, A.

    1993-01-01

    Indigenous crude oils could be degraded and emulsified upto varying degree by locally isolated bacteria. Degradation and emulsification was found to be dependent upon the chemical composition of the crude oils. Tando Alum and Khashkheli crude oils were emulsified in 27 and 33 days of incubation respectively. While Joyamair crude oil and not emulsify even mainly due to high viscosity of this oil. Using adsorption chromatographic technique, oil from control (uninoculated) and bio degraded flasks was fractioned into the deasphaltened oil containing saturate, aromatic, NSO (nitrogen, sulphur, oxygen) containing hydrocarbons) and soluble asphaltenes. Saturate fractions from control and degraded oil were further analysed by gas liquid chromatography. From these analyses, it was observed that saturate fraction was preferentially utilized and the crude oils having greater contents of saturate fraction were better emulsified than those low in this fraction. Utilization of various fractions of crude oils was in the order saturate> aromatic> NSO. (author)

  14. Gas Chromatographic Mass Spectrometric Determination of Myo-inositol in Humans Utilizing a Deuterated Internal Standard

    DEFF Research Database (Denmark)

    Andersen, Jan Rud; Larsen, Elfinn; Harbo, Helge

    1982-01-01

    The isotopic dilution technique was used for determining the content of myo-inositol in human urine, plasma and haemolysed erythrocyte samples. A deuterated myo-inositol, synthesized from inosose-2 by base-catalysed exchange of hydrogens by deuterium, followed by reduction of the inosose with 2H2......, was added as internal standard to the samples at an early stage in the analytical procedure. After separation and derivatization to the hexa-acetate, the gas chromatographic mass spectrometric analysis was carried out. A 25 m fused silica capillary column coated with methyl silicone was used, and the ions...... selected for monitoring were m/z 210 and m/z 214, which are characteristic and abundant fragment ions from unlabelled and hexadeuterated myo-inositolhexa-acetate, respectively. Calibration curves from water, urine, plasma and haemolysed erythrocytes show parallel, linear responses in the ratio between...

  15. Determination and discrimination of biodiesel fuels by gas chromatographic and chemometric methods

    Science.gov (United States)

    Milina, R.; Mustafa, Z.; Bojilov, D.; Dagnon, S.; Moskovkina, M.

    2016-03-01

    Pattern recognition method (PRM) was applied to gas chromatographic (GC) data for a fatty acid methyl esters (FAME) composition of commercial and laboratory synthesized biodiesel fuels from vegetable oils including sunflower, rapeseed, corn and palm oils. Two GC quantitative methods to calculate individual fames were compared: Area % and internal standard. The both methods were applied for analysis of two certified reference materials. The statistical processing of the obtained results demonstrates the accuracy and precision of the two methods and allows them to be compared. For further chemometric investigations of biodiesel fuels by their FAME-profiles any of those methods can be used. PRM results of FAME profiles of samples from different vegetable oils show a successful recognition of biodiesels according to the feedstock. The information obtained can be used for selection of feedstock to produce biodiesels with certain properties, for assessing their interchangeability, for fuel spillage and remedial actions in the environment.

  16. Modified molecular sieves: stationary phase for the gas chromatographic separation of hydrogen isotopes

    International Nuclear Information System (INIS)

    Pushpa, K.K.; Annaji Rao, K.; Iyer, R.M.

    1993-01-01

    Gas chromatographic separation of hydrogen isotopes on different molecular sieves at liquid nitrogen temperature has been investigated. Normal molecular sieves 5A, 13X and AW500 are not satisfactory for the purpose both in the partially dehydrated as well as totally dehydrated state. Molecular sieve 4A in partially dehydrated state separated H 2 and D 2 while H 2 and HD are not well resolved. Iron exchanged or coated molecular sieves 4A, 5A, 13X and AW500 in the partially dehydrated state separated the isotopic mixtures H 2 , HD, D 2 and H 2 , HT, T 2 . The resolution varied depending on the amount of iron content and the residual moisture in the molecular sieves. Good separations were obtained on 15% Fe coated molecular sieve 5A and 5% Fe coated molecular sieve 4A. (author). 18 refs., 6 figs., 3 tabs

  17. Headspace solid-phase microextraction procedures for gas chromatographic analysis of biological fluids and materials.

    Science.gov (United States)

    Mills, G A; Walker, V

    2000-12-01

    Solid-phase microextraction (SPME) is a new solventless sample preparation technique that is finding wide usage. This review provides updated information on headspace SPME with gas chromatographic separation for the extraction and measurement of volatile and semivolatile analytes in biological fluids and materials. Firstly the background to the technique is given in terms of apparatus, fibres used, extraction conditions and derivatisation procedures. Then the different matrices, urine, blood, faeces, breast milk, hair, breath and saliva are considered separately. For each, methods appropriate for the analysis of drugs and metabolites, solvents and chemicals, anaesthetics, pesticides, organometallics and endogenous compounds are reviewed and the main experimental conditions outlined with specific examples. Then finally, the future potential of SPME for the analysis of biological samples in terms of the development of new devices and fibre chemistries and its coupling with high-performance liquid chromatography is discussed.

  18. On the ability of the Viking gas chromatograph-mass spectrometer to detect organic matter.

    Science.gov (United States)

    Biemann, Klaus

    2007-06-19

    A recent paper by Navarro-Gonzalez et al. [Navarro-Gonzalez R, Navarro KF, de la Rosa J, Iniguez E, Molina P, Miranda LD, Morales P, Cienfuegos E, Coll P, Raulin F, et al. (2006) Proc Natl Acad Sci USA 103:16089-16094] claims to show that the Viking GCMS (gas chromatograph-mass spectrometer) experiment, which carried out a search for organic matter at the surface of Mars in 1976, "may have been blind to low levels of organics." To rebut this assertion, the Viking experiment, test data, and results on Mars are reviewed, and the fallacies in the design, execution, and interpretation of the new experiments presented by Navarro-Gonzalez et al. are critically examined.

  19. Formation of hydrocarbons in irradiated Brazilian beans: gas chromatographic analysis to detect radiation processing

    International Nuclear Information System (INIS)

    Villavicencio, A.L.C.H.; Mancini-Filho, J.; Hartmann, M.; Ammon, J.; Delincee, H.

    1997-01-01

    Radiation processing of beans, which are a major source of dietary protein in Brazil, is a valuable alternative to chemical fumigation to combat postharvest losses due to insect infestation. To ensure free consumer choice, irradiated food will be labeled as such, and to enforce labeling, analytical methods to detect the irradiation treatment in the food product itself are desirable. In two varieties of Brazilian beans, Carioca and Macacar beans, the radiolytic formation of hydrocarbons formed after alpha and beta cleavage, with regard to the carbonyl group in triglycerides, have been studied. Using gas chromatographic analysis of these radiolytic hydrocarbons, different yields per precursor fatty acid are observed for the two types of beans. However, the typical degradation pattern allows the identification of the irradiation treatment in both bean varieties, even after 6 months of storage

  20. Volatile hexafluoroacetylacetonates for the isolation and gas-chromatographic determination of trace metals. Pt. 1

    International Nuclear Information System (INIS)

    Hellmuth, K.H.; Mirzai, H.

    1985-01-01

    The optimization of the extraction of metal cations [Sc(III), Cr(III), Mn(II), Fe(III), Co(II), Cu(II), Zn(II), Y(III), Ag(I), Cd(II), La(IIII), Ce(III), Eu(III), Yb(III), Hg(II), Pb(II), Th(IV), U(IV, VI) and Am(III)] in the form of mixed-ligand complexes with hexafluoroacetylacetone and neutral donators with nitrogen atoms or P=O-groups is described. The thermal and gas-chromatographic characteristics of the extracted volatile compounds are reported. Optimal results were achieved using tri-n-butyl-phosphine oxide as donator. (orig.) [de

  1. Determination and discrimination of biodiesel fuels by gas chromatographic and chemometric methods

    Directory of Open Access Journals (Sweden)

    Milina R.

    2016-03-01

    Full Text Available Pattern recognition method (PRM was applied to gas chromatographic (GC data for a fatty acid methyl esters (FAME composition of commercial and laboratory synthesized biodiesel fuels from vegetable oils including sunflower, rapeseed, corn and palm oils. Two GC quantitative methods to calculate individual fames were compared: Area % and internal standard. The both methods were applied for analysis of two certified reference materials. The statistical processing of the obtained results demonstrates the accuracy and precision of the two methods and allows them to be compared. For further chemometric investigations of biodiesel fuels by their FAME-profiles any of those methods can be used. PRM results of FAME profiles of samples from different vegetable oils show a successful recognition of biodiesels according to the feedstock. The information obtained can be used for selection of feedstock to produce biodiesels with certain properties, for assessing their interchangeability, for fuel spillage and remedial actions in the environment.

  2. On-line system on the base of the ELEKTRONIKA D3-28 microcomputer for gas filling

    International Nuclear Information System (INIS)

    Artemov, A.A.; Baranchuk, N.S.; Livitskij, M.M.; Platonov, V.P.; Chernyak, V.Ya.

    1989-01-01

    On-line system for gas filling on the base of SNA-1 pressure controller, ELEKTRONIKA D3-28 microcomputer and interface device and program for information exchange within the system are described. The system is designed for on-line measurement of gas pressure and filling and is used during operation without pumping out. Volume of vacuum chamber is 0.8 m 3 , pressure of filled-out gas (nitrogen) is 1 atm. The system enables to change pressure up to 0.1 Torr with 1x10 -4 Torr accuracy. Actuation time of g as filling-on system is determined with program control and depends on pressure measurement. Minimal actuation time of gas filling-on system is determined with program control and depends on pressure measurement. Minimal actuation time is 12 ms

  3. Detection of radiation-induced hydrocarbons in irradiated fish and prawns by means of on-line coupled liquid chromatography-gas chromatography

    International Nuclear Information System (INIS)

    Schulzki, G.; Spiegelberg, A.; Bogl, K.W.; Schreiberg, G.A.

    1997-01-01

    Radiation-induced hydrocarbons were analyzed in a fatty (halibut) and a lean fish (cod) as well as in a prawn species by on-line coupled liquid chromatography (LC) -gas chromatography (GC) combined with mass spectrometry. In irradiated halibut which is known to contain mainly saturated and monounsaturated fatty acids, all expected radiolytic alkanes, alkenes, and alkadienes could be detected. The yields of the C(n-1) and C(n-2:1) hydrocarbons were comparable to those found in irradiated lipids of terrestrial animals and plants. However, in cod and prawns which contain high levels of polyunsaturated fatty acids (PUFA), the C(n-1) hydrocarbons were found in concentrations which were up to 10 times higher whereas the C(n-2:1) products were again comparable to those of terrestrial animals and plants. The identification of radiation-induced hydrocarbons in fish lipids was achieved by transfer of the hydrocarbons from the LC column to the gas chromatographic column in fractions differing in their degree of unsaturation. For the first time, radiation-induced hydrocarbons with more than four double bonds generated from polyunsaturated fatty acids (20:4 omega 6 and 20:5 omega 3) could be identified

  4. Thermal soil desorption for total petroleum hydrocarbon testing on gas chromatographs

    International Nuclear Information System (INIS)

    Mott, J.

    1995-01-01

    Testing for total petroleum hydrocarbons (TPH) is one of the most common analytical tests today. A recent development in chromatography incorporates Thermal Soil Desorption technology to enable analyses of unprepared soil samples for volatiles such as BTEX components and semi-volatiles such as diesel, PCBs, PAHs and pesticides in the same chromatogram, while in the field. A gas chromatograph is the preferred method for determining TPH because the column in a GC separates the individual hydrocarbons compounds such as benzene and toluene from each other and measures each individually. A GC analysis will determine not only the total amount of hydrocarbon, but also whether it is gasoline, diesel or another compound. TPH analysis with a GC is typically conducted with a Flame Ionization Detector (FID). Extensive field and laboratory testing has shown that incorporation of a Thermal Soil Desorber offers many benefits over traditional analytical testing methods such as Headspace, Solvent Extraction, and Purge and Trap. This paper presents the process of implementing Thermal Soil Desorption in gas chromatography, including procedures for, and advantages of faster testing and analysis times, concurrent volatile and semi-volatile analysis, minimized sample manipulation, single gas (H 2 ) operation, and detection to the part-per billion levels

  5. A purge-and-trap capillary column gas chromatographic method for the measurement of halocarbons in water and air

    Energy Technology Data Exchange (ETDEWEB)

    Happell, J.D.; Wallace, D.W.R.; Wills, K.D.; Wilke, R.J.; Neill, C.C.

    1996-06-01

    This report describes an automated, accurate, precise and sensitive capillary column purge- and -trap method capable of quantifying CFC-12, CFC-11, CFC-113, CH{sub 3}CCL{sub 3}, and CCL{sub 4} during a single chromatographic analysis in either water or gas phase samples.

  6. Abnormal tyrosine and phenylalanine metabolism in patients with tyrosyluria and phenylketonuria; gas-liquid chromatographic analysis of urinary metabolites

    NARCIS (Netherlands)

    Wadman, S.K.; Heiden, C. van der; Ketting, D.; Sprang, F.J. van

    Gas-liquid chromatographic methods have been developed for the analysis of: urinary phenylalanine metabolites (I) in patients with phenylketonuria, tyrosine metabolites (II) in patients with a disturbed tyrosine metabolism at the level of p-hydroxyphenylpyruvate hydroxylase, and homogentisic acid in

  7. Chromatographic separation and continuously referenced, on-line monitoring of creatine kinase isoenzymes by use of an immobilized-enzyme microreactor

    International Nuclear Information System (INIS)

    Denton, M.S.; Bostick, W.D.; Dinsmore, S.R.; Mrochek, J.E.

    1978-01-01

    We describe a new concept in continuously referenced monitoring of the isoenzyme activities of creatine kinase (EC 2.7.3.2) after liquid-chromatographic separation. After separation on a diethylaminoethyl-Sephacel column, the three isoenzymes of creatine kinase undergo a series of upled enzyme reactions, ultimately resulting in the formation of ultraviolet-detectable NADPH. A major advantage of this detection system is the immobilized-enzyme microreactor (2 x 17 mm), which may be removed and stored refrigerated when not in use. A split-stream configuration allows self-blanking of endogenous ultraviolet-absorbing constituents in authentic sera samples, which would otherwise make definitive diagnosis and quantitation difficult or impossible. This detection system is applicable to the automated analysis of creatine kinase isoenzymes in the clinical laboratory. 5 figures; 42 references

  8. On-Line Digital Computer Applications in Gas Chromatography, An Undergraduate Analytical Experiment

    Science.gov (United States)

    Perone, S. P.; Eagleston, J. F.

    1971-01-01

    Presented are some descriptive background materials and the directions for an experiment which provides an introduction to on-line computer instrumentation. Assumes students are familiar with the Purdue Real-Time Basic (PRTB) laboratory computer system. (PR)

  9. Autonomous gas chromatograph system for Thermal Enhanced Vapor Extraction System (TEVES) proof of concept demonstration

    International Nuclear Information System (INIS)

    Peter, F.J.; Laguna, G.R.

    1996-09-01

    An autonomous gas chromatograph system was designed and built to support the Thermal Enhanced Vapor Extraction System (TEVES) demonstration. TEVES is a remediation demonstration that seeks to enhance an existing technology (vacuum extraction) by adding a new technology (soil heating). A pilot scale unit was set up at one of the organic waste disposal pits at the Sandia National Laboratories Chemical Waste Landfill (CWL) in Tech Area 3. The responsibility for engineering a major part of the process instrumentation for TEVES belonged to the Manufacturing Control Subsystems Department. The primary mission of the one-of-a-kind hardware/software system is to perform on-site gas sampling and analysis to quantify a variety of volatile organic compounds (VOCs) from various sources during TEVES operations. The secondary mission is to monitor a variety of TEVES process physical parameters such as extraction manifold temperature, pressure, humidity, and flow rate, and various subsurface pressures. The system began operation in September 1994 and was still in use on follow-on projects when this report was published

  10. A Gas Chromatographic Continuous Emissions Monitoring System for the Determination of VOCs and HAPs.

    Science.gov (United States)

    Coleman, William M; Gordon, Bert M

    1996-01-01

    This article describes a new gas chromatography-based emissions monitoring system for measuring volatile organic compounds (VOCs) and hazardous air pollutants (HAPs). The system is composed of a dual-column gas chromatograph equipped with thermal conductivity detectors, in which separation is optimized for fast chromatography. The system has the necessary valving for stream selection, which allows automatic calibration of the system at predetermined times and successive measurement of individual VOCs before and after a control device. Nine different VOCs (two of which are HAPs), plus methane (CH4) and carbon dioxide (CO2) are separated and quantified every two minutes. The accuracy and precision of this system has been demonstrated to be greater than 95%. The system employs a mass flow measurement device and also calculates and displays processed emission data, such as control device efficiency and total weight emitted during given time periods. Two such systems have been operational for one year in two separate gravure printing facilities; minimal upkeep is required, about one hour per month. One of these systems, used before and after a carbon adsorber, has been approved by the pertinent local permitting authority.

  11. Authentication of commercial spices based on the similarities between gas chromatographic fingerprints.

    Science.gov (United States)

    Matsushita, Takaya; Zhao, Jing Jing; Igura, Noriyuki; Shimoda, Mitsuya

    2018-06-01

    A simple and solvent-free method was developed for the authentication of commercial spices. The similarities between gas chromatographic fingerprints were measured using similarity indices and multivariate data analyses, as morphological differentiation between dried powders and small spice particles was challenging. The volatile compounds present in 11 spices (i.e. allspice, anise, black pepper, caraway, clove, coriander, cumin, dill, fennel, star anise, and white pepper) were extracted by headspace solid-phase microextraction, and analysed by gas chromatography-mass spectrometry. The largest 10 peaks were selected from each total ion chromatogram, and a total of 65 volatiles were tentatively identified. The similarity indices (i.e. the congruence coefficients) were calculated using the data matrices of the identified compound relative peak areas to differentiate between two sets of fingerprints. Where pairs of similar fingerprints produced high congruence coefficients (>0.80), distinctive volatile markers were employed to distinguish between these samples. In addition, hierarchical cluster analysis and principal component analysis were performed to visualise the similarity among fingerprints, and the analysed spices were grouped and characterised according to their distinctive major components. This method is suitable for screening unknown spices, and can therefore be employed to evaluate the quality and authenticity of various spices. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

  12. Assessment of corrosion in the flue gas cleaning system using on-line monitoring

    DEFF Research Database (Denmark)

    Montgomery, Melanie; Vendelbo Nielsen, Lars; Berggreen Petersen, Michael

    2015-01-01

    Amager unit 1 is a 350 MW multifuel suspension-fired plant commissioned in 2009 to fire biomass (straw and wood pellets). Increasing corrosion problems in the flue gas cleaning system were observed in the gas-gas preheater (GAFO), the booster fan and flue gas ducts. Chlorine containing corrosion ...

  13. On-line stable isotope measurements during plant and soil gas exchange

    International Nuclear Information System (INIS)

    Yakir, D.

    2001-01-01

    Recent techniques for on-line stable isotope measurements during plant and soil exchange of CO 2 and/or water vapor are briefly reviewed. For CO 2 , these techniques provide means for on-line measurements of isotopic discrimination during CO 2 exchange by leaves in the laboratory and in the field, of isotopic discrimination during soil respiration and during soil-atmosphere CO 2 exchange, and of isotopic discrimination in O 2 during plant respiration. For water vapor, these techniques provide means to measure oxygen isotopic composition of water vapor during leaf transpiration and for the analysis of sub microliter condensed water vapor samples. Most of these techniques involve on-line sampling of CO 2 and water vapor from a dynamic, intact soil or plant system. In the laboratory, these systems also allow on-line isotopic analysis by continuous-flow isotope ratio mass spectrometry. The information obtained with these on-line techniques is becoming increasingly valuable, and often critical, for ecophysiologial research and in the study of biosphere-atmosphere interactions. (author)

  14. Characterization of crude oils and petroleum products: (I Elution liquid chromatographic separation and gas chromatographic analysis of crude oils and petroleum products

    Directory of Open Access Journals (Sweden)

    E.O. Odebunmi

    2002-12-01

    Full Text Available Some physical and chemical properties of samples of light, medium and heavy Nigerian crude oils and petroleum products including gasoline, kerosene and engine oil have been measured and are reported in this paper. The crude oils and petroleum products have also been characterized by fractional distillation and elution liquid chromatography. The fractions obtained from elution liquid chromatography were analyzed using gas chromatography (GC. The GC fractions were identified by comparing the retention time of peaks in the unknown samples with those of components of calibration standard mixtures. The importance of the physico-chemical properties and the significance of the fractional distillation and chromatographic separation methods to industrial process operations have been discussed.

  15. Supercritical fluid extraction-capillary gas chromatography: on-line coupling with a programmed temperature vaporizer

    NARCIS (Netherlands)

    Houben, R.J.; Janssen, J.G.M.; Leclercq, P.A.; Rijks, J.A.; Cramers, C.A.M.G.

    1990-01-01

    A simple and versatile system is described for the on-line coupling of SFE to capillary GC. The interfacing consists of a programmed temperature vaporizer (PTV) injector. With this injector it is possible to combine solute trapping, elimination of a high flow of extraction fluid, and quantitative

  16. Chromatographic efficiency of polar capillary columns applied for the analysis of fatty acid methyl esters by gas chromatography.

    Science.gov (United States)

    Waktola, Habtewold D; Mjøs, Svein A

    2018-04-01

    The chromatographic efficiency that could be achieved in temperature-programmed gas chromatography was compared for four capillary columns that are typically applied for analysis of fatty acid methyl esters (FAME). Three different carrier gases, hydrogen, helium and nitrogen, were applied. For each experiment, the carrier gas velocities and the temperature rates were varied with a full 9 × 3 design, with nine levels on the carrier gas velocity and temperature rates of 1, 2 or 3°C/min. Response surface methodology was used to create models of chromatographic efficiency as a function of temperature rate and carrier gas velocity. The chromatographic efficiency was defined as the inverse of peak widths measured in retention index units. The final results were standardized so that the efficiencies that could be achieved within a certain time frame, defined by the retention time of the last compound in the chromatogram, could be compared. The results show that there were clear differences in the efficiencies that could be achieved with the different columns and that the efficiency decreased with increasing polarity of the stationary phase. The differences can be explained by higher resistance to mass transfer in the stationary phase in the most polar columns. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Gas chromatographic determination with electron capture detection of residual ethylene oxide in intraocular lenses

    Energy Technology Data Exchange (ETDEWEB)

    Kikuchi, H.; Nakamura, A.; Tsuji, K.

    1988-01-01

    A sensitive method is described to determine trace quantities of ethylene oxide (EO) in EO-sterilized intraocular lenses (IOLs). An IOL is dipped in ethanol containing 0.25 ppm propylene oxide (PO) in a 4 mL vial, 2 drops of freshly distilled hydrobromic acid is added through a septum, and the mixture is warmed at 50/sup 0/C for 24 h. It is then neutralized by vigorous shaking with sodium bicarbonate, dehydrated with anhydrous sodium sulfate, and filtered. The filtrate is injected into a gas chromatograph with electron-capture detection, and the peak height ratio of ethylene bromohydrin/propylene bromohydrin is measured. EO residue is calculated from the calibration curve obtained through a similar procedure with the standard EO/PO solutions. The limit of determination is 0.04 ..mu..g/lens (ca 2.0 ppm). When EO residue levels were determined for IOLs sampled at 3 different aeration periods after stabilization, the authors found that 9 days of aeration was necessary to meet the US Food and Drug Administration proposed limit for EO residue in IOLs.

  18. Chromatographic analysis of methylglyoxal and other α-dicarbonyls using gas-diffusion microextraction.

    Science.gov (United States)

    Santos, Christiane M; Valente, Inês M; Gonçalves, Luís M; Rodrigues, José A

    2013-12-07

    Many α-dicarbonyl compounds such as methylglyoxal, diacetyl and pentane-2,3-dione are important quality markers of processed foods. They are produced by enzymatic and chemical processes, the Maillard reaction is the most known chemical route for α-dicarbonyl formation. In the case of methylglyoxal, there are obstacles to be overcome when analysing this compound due to its high reactivity, low volatility and low concentration. The use of extraction techniques based on the volatilization of methylglyoxal (like solid-phase microextraction) showed to be ineffective for the methylglyoxal extraction from aqueous solutions. Therefore, derivatization is typically applied to increase analyte's volatility. In this work a new methodology for the extraction and analysis of methylglyoxal and also diacetyl and pentane-2,3-dione from selected food matrices is presented. It is based on a gas-diffusion microextraction step followed by high performance liquid chromatographic analysis. It was successfully applied to port wines, black tea and soy sauce. Methylglyoxal, diacetyl and pentane-2,3-dione were quantified in the following concentration ranges: 0.24-1.74 mg L(-1), 0.1-1.85 mg L(-1) and 0.023-0.15 mg L(-1), respectively. The main advantages over existing methodologies are its simplicity in terms of sample handling, not requiring any chemical modification of the α-dicarbonyls prior to the extraction, low reagent consumption and short time of analysis.

  19. Gas chromatographic isolation of individual compounds from complex matrices for radiocarbon dating.

    Science.gov (United States)

    Eglinton, T I; Aluwihare, L I; Bauer, J E; Druffel, E R; McNichol, A P

    1996-03-01

    This paper describes the application of a novel, practical approach for isolation of individual compounds from complex organic matrices for natural abundance radiocarbon measurement. This is achieved through the use of automated preparative capillary gas chromatography (PCGC) to separate and recover sufficient quantities of individual target compounds for (14)C analysis by accelerator mass spectrometry (AMS). We developed and tested this approach using a suite of samples (plant lipids, petroleums) whose ages spanned the (14)C time scale and which contained a variety of compound types (fatty acids, sterols, hydrocarbons). Comparison of individual compound and bulk radiocarbon signatures for the isotopically homogeneous samples studied revealed that Δ(14)C values generally agreed well (±10%). Background contamination was assessed at each stage of the isolation procedure, and incomplete solvent removal prior to combustion was the only significant source of additional carbon. Isotope fractionation was addressed through compound-specific stable carbon isotopic analyses. Fractionation of isotopes during isolation of individual compounds was minimal (radiocarbon measurements. The addition of carbon accompanying derivatization of functionalized compounds (e.g., fatty acids and sterols) prior to chromatographic separation represents a further source of potential error. This contribution can be removed using a simple isotopic mass balance approach. Based on these preliminary results, the PCGC-based approach holds promise for accurately determining (14)C ages on compounds specific to a given source within complex, heterogeneous samples.

  20. Gas Chromatographic Determination of Fatty Acids in Oils with Regard to the Assessment of Fire Hazard

    Science.gov (United States)

    Bartošová, Alica; Štefko, Tomáš

    2017-06-01

    The aim of the paper was to study and research the application of processing gas chromatographic method for the rapid and accurate determination of the composition of different types of oils, such as substances with the possibility of an adverse event spontaneous combustion or self-heating. Tendency to spontaneous combustion is chemically characterized mainly by the amount of unsaturated fatty acids, which have one or more double bonds in their molecule. Vegetable oils essentially consist of the following fatty acids: palmitic, stearic, oleic, linoleic, and linoleic. For the needs of assessment, the fire hazard must be known, in which the double bond is present, as well as their number in a molecule. As an analytical method, GCMS was used for determination of oils content. Three types of oil were used - rapeseed, sunflower, and coconut oil. Owing to the occurrence of linoleic acid C18:2 (49.8 wt.%) and oleic acid C18:1 (43.3 wt.%) with double bonds, sunflower oil is the most prone to self-heating. The coconut and rapeseed oils contain double bond FAME in lesser amount, and their propensity to self-heating is relatively low.

  1. Capillary gas chromatographic analysis of nerve agents using large volume injections. Final report

    Energy Technology Data Exchange (ETDEWEB)

    Deinum, T.; Nieuwenhuy, C.

    1994-11-01

    The procedure developed at TNO-Prins Maurits Laboratory (TNO-PML) for the verification of intact organophosphorus chemical warfare agents in water samples was improved. The last step in this procedure, the laborious and non-reproducible transfer of an ethyl acetate extract onto a Tenax-adsorption tube followed by thermal desorption of the Tenax-tube, was replaced by large volume injection of the extract onto a capillary gas chromatographic system. The parameters controlling the injection of a large volume of an extract (200 ul) were investigated and optimized. As ethyl acetate caused severe problems, potential new solvents were evaluated. With the improved procedure, the nerve agents sarin, tabun, soman, diisopropyl fluorophosphate (DFP) and VX could be determined in freshly prepared water samples at pg/ml (ppt) levels. The fate of the nerve agents under study in water at two pH`s (4.8 and 6) was investigated. For VX, the pH should be adjusted before extraction. Moreover, it is worthwhile to acidify water samples to diminish hydrolysis.

  2. Automatic on-line monitoring of atmospheric volatile organic compounds: Gas chromatography-mass spectrometry and gas chromatography-flame ionization detection as complementary systems

    International Nuclear Information System (INIS)

    Blas, Maite de; Navazo, Marino; Alonso, Lucio; Durana, Nieves; Iza, Jon

    2011-01-01

    Traditionally air quality networks have been carrying out the continuous, on-line measurement of volatile organic compounds (VOC) in ambient air with GC-FID. In this paper some identification and coelution problems observed while using this technique in long-term measurement campaigns are described. In order to solve these problems a GC-MS was set up and operated simultaneously with a GC-FID for C 2 -C 11 VOCs measurement. There are few on-line, unattended, long term measurements of atmospheric VOCs performed with GC-MS. In this work such a system has been optimized for that purpose, achieving good repeatability, linearity, and detection limits of the order of the GC-FID ones, even smaller in some cases. VOC quantification has been made by using response factors, which is not frequent in on-line GC-MS. That way, the identification and coelution problems detected in the GC-FID, which may led to reporting erroneous data, could be corrected. The combination of GC-FID and GC-MS as complementary techniques for the measurement of speciated VOCs in ambient air at sub-ppbv levels is proposed. Some results of the measurements are presented, including concentration values for some compounds not found until now on public ambient air VOC databases, which were identified and quantified combining both techniques. Results may also help to correct previously published VOC data with wrongly identified compounds by reprocessing raw chromatographic data.

  3. Gas chromatographic simulated distillation-mass spectrometry for the determination of the boiling point distributions of crude oils

    Science.gov (United States)

    Roussis; Fitzgerald

    2000-04-01

    The coupling of gas chromatographic simulated distillation with mass spectrometry for the determination of the distillation profiles of crude oils is reported. The method provides the boiling point distributions of both weight and volume percent amounts. The weight percent distribution is obtained from the measured total ion current signal. The total ion current signal is converted to weight percent amount by calibration with a reference crude oil of a known distillation profile. Knowledge of the chemical composition of the crude oil across the boiling range permits the determination of the volume percent distribution. The long-term repeatability is equivalent to or better than the short-term repeatability of the currently available American Society for Testing and Materials (ASTM) gas chromatographic method for simulated distillation. Results obtained by the mass spectrometric method are in very good agreement with results obtained by conventional methods of physical distillation. The compositional information supplied by the method can be used to extensively characterize crude oils.

  4. Implementation of a fully automated process purge-and-trap gas chromatograph at an environmental remediation site

    International Nuclear Information System (INIS)

    Blair, D.S.; Morrison, D.J.

    1997-01-01

    The AQUASCAN, a commercially available, fully automated purge-and-trap gas chromatograph from Sentex Systems Inc., was implemented and evaluated as an in-field, automated monitoring system of contaminated groundwater at an active DOE remediation site in Pinellas, FL. Though the AQUASCAN is designed as a stand alone process analytical unit, implementation at this site required additional hardware. The hardware included a sample dilution system and a method for delivering standard solution to the gas chromatograph for automated calibration. As a result of the evaluation the system was determined to be a reliable and accurate instrument. The AQUASCAN reported concentration values for methylene chloride, trichloroethylene, and toluene in the Pinellas ground water were within 20% of reference laboratory values

  5. Derivative spectrum chromatographic method for the determination of trimethoprim in honey samples using an on-line solid-phase extraction technique.

    Science.gov (United States)

    Uchiyama, Kazuhisa; Kondo, Mari; Yokochi, Rika; Takeuchi, Yuri; Yamamoto, Atsushi; Inoue, Yoshinori

    2011-07-01

    A simple, selective and rapid analytical method for determination of trimethoprim (TMP) in honey samples was developed and validated. This method is based on a SPE technique followed by HPLC with photodiode array detection. After dilution and filtration, aliquots of 500 μL honey samples were directly injected to an on-line SPE HPLC system. TMP was extracted on an RP SPE column, and separated on a hydrophilic interaction chromatography column during HPLC analysis. At the first detection step, the noise level of the photodiode array data was reduced with two-dimensional equalizer filtering, and then the smoothed data were subjected to derivative spectrum chromatography. On the second-derivative chromatogram at 254 nm, the limit of detection and the limit of quantification of TMP in a honey sample were 5 and 10 ng/g, respectively. The proposed method showed high accuracy (60-103%) with adequate sensitivity for TMP monitoring in honey samples. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Direct coupling of a dense (supercritical) gas chromatograph to a mass spectrometer using a supersonic molecular beam interface

    International Nuclear Information System (INIS)

    Randall, L.G.; Wahrhaftig, A.L.

    1981-01-01

    A detecting mass spectrometer has been successfully coupled to a dense gas (supercritical fluid) chromatograph to produce an instrument (DGC/MS) that may be an alternative to high performance liquid chromatograph/mass spectrometer instruments (HPLC/MS) and gas chromatograph/mass spectrometer instruments (GC/MS) for analysis of involatile and/or thermally labile compounds. The mobile phase in DGC is a gas held at temperatures above the critical temperature and at pressures sufficient to obtain nearly liquid-like densities. DGC combines advantages of GC and HPLC: rapid separations, moderate operating temperatures, and analysis of involatile compounds. An advantage unique to DGC is the solvent power dependence upon pressure. While several groups have studied DGC, its development has been limited by the lack of a sensitive and selective detector. Hence, work has been directed towards the design and construction of a DGC/MS resulting in a trial instrument capable of chromatographic pressures of at least 300 atm and temperatures from 10 0 to 60 0 C. The DGC/MS coupling has been accomplished by the use of a supersonic molecular beam interface. This application of molecular beam formation appears to be unique in its requirements of a large pressure ratio (approx.10 8 ), low flow rates, and low final pressures. The authors outline characteristics of supersonic jets and molecular beams pertinent to the design of such an instrument. The interface which uses pumping speeds of 2400 and 1200 l/s in the beam forming chambers is described in detail, while the other components: the detecting mass spectrometer, the dense gas supply, and the DGC: are briefly described. Preliminary work with this instrument has established the feasibility of DGC/MS as an analytical technique and further development is recommended

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

    Science.gov (United States)

    Bluemlein, Katharina; Raab, Andrea; Feldmann, Jörg

    2009-01-01

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

  8. Domestic Preparedness Program: Evaluation of the Agilent Gas Chromatograph - Flame Photometric Detector/Mass Selective Detector (GC-FPD/MSD) System Against Chemical Warfare Agents Summary Report

    National Research Council Canada - National Science Library

    Longworth, Terri

    2003-01-01

    This report characterizes the chemical warfare agent (CWA) detection potential of the commercially available Agilent gas chromatograph-flame photometric detector/mass selective detector (GC-FPD/MSD...

  9. The gas-phase on-line production of phosphoryl halides, Pox3 and their identification by infrared spectroscopy

    International Nuclear Information System (INIS)

    Allaf, A.W.

    1998-01-01

    A new route has been devised, leading to the production of Pox 3 molecules where X=F, Br and I by an on-line process using phosphoryl chloride, POCL 3 as a starting material passed over heated sodium fluoride, NaF, potassium bromide, KBr and potassium iodide, K1 at 535 Centigrade, 690 Centigrade and 480 Centigrade, respectively. The low resolution gas-phase fourier transform infrared spectra reported for the first time showed strong bands centered at 1411.6, 1322.9, 1300.8 and 1285 cm - 1, assigned to Ε 1 (a 1 ), the O = P stretching fundamental of POF 3 , POCL 3 , POBR 3 and POI 3 , respectively. Attempts were made to prepare POCL 2 and POBr 2 , by an on-line process using POCL 3 again but passed over heated sodium and potassium bromide for POCL 2 and POBr 2 . (author). 3 refs., 2 figs., 1 tab

  10. The gas-phase on-line production of vanadium oxytrihalides, VOX3 and their identification by infrared spectroscopy

    International Nuclear Information System (INIS)

    Zidan, M. D.; Allaf, A. W.

    2001-01-01

    A new route has been devised, leading to the production of VOX 3 molecules where X=F, Br and I by an on-line process using vanadium oxytrichloride, VOCl 3 as a starting compound passed over the following heated salts NaF, KBr and KI at 375, 700 and 550 centigrade, respectively. The products have been characterized by the IR spectra of their vapors. the low resolution gas phase on-line Fourier transform infrared spectra reported for the first time show strong bands with PQR type structure, centered at 1058, 1035, 1030 and 1025 cm -1 to the υ 1 (a 1 ), the O=V stretching fundamental mode of VOF 3 , VOCl 3 , VOBr 3 and VOI 3 , respectively. (Author)

  11. Structural assessment procedure of corroding submarine gas pipelines using on-line inspection data

    International Nuclear Information System (INIS)

    Nordin Yahaya

    2000-01-01

    This paper presents 'the alternative approach of overall procedure in the assessment of corroded pipelines using data gathered by the on-line inspection device. The methodology adopts a generalised approach of analysing pipeline inspection data and a prediction of the structural reliability due to the deteriorating corrosion environment. The whole assessment methodology is divided into four separate stages; 1 to IV. Stages 1 and 11 are the initial procedure prior to the actual analysis of the inspection data. The scope of this paper is concerted into the procedure to be taken in Stage 111 where the stage is sub-divided into 3 major steps; Part A, B and C. These procedures are Part A (statistical and probabilistic analysis of the inspection data) and Part B (the application of extreme value statistics) and C (reliability assessment). Stage IV (risk assessment) is the final step in the procedure where the consequences of failure are evaluated. The proposed risk-based assessment procedure is more systematic and reliable to account for a huge amount of collected data usually obtained in an on-line inspection using the intelligent devices. The outcomes of this risk-based methodology can be very useful in the decision-making process by the operation management. This in turn will produce an efficient inspection, repair and maintenance program and enhanced the optimised return in investment. (author)

  12. Basic studies of a gas-jet-coupled ion source for on-line isotope separation

    International Nuclear Information System (INIS)

    Anderl, R.A.; Novick, V.J.; Greenwood, R.C.

    1980-01-01

    A hollow-cathode ion source was used in a gas-jet-coupled configuration to produce ion beams of fission products transported to it from a 252 Cf fission source. Solid aerosols of NaCl and Ag were used effectively as activity carriers in the gas-jet system. Flat-plate skimmers provided an effective coupling of the ion source to the gas jet. Ge(Li) spectrometric measurements of the activity deposited on an ion-beam collector relative to that deposited on a pre-skimmer collector were used to obtain separation efficiencies ranging from 0.1% to > 1% for Sr, Y, Tc, Te, Cs, Ba, Ce, Pr, Nd and Sm. The use of CCl 4 as a support gas resulted in a significant enhancement of the alkaline-earth and rare-earth separation efficiencies

  13. Utilization of on-line corrosion monitoring in the flue gas cleaning system

    DEFF Research Database (Denmark)

    Montgomery, Melanie; Nielsen, Lars V.; Petersen, Michael B.

    2015-01-01

    fan. The corrosion rates measured with respect to time were correlated to plant data such as load, temperature, gas composition, water content as well as change in the fuel used. From these results it is clear that many shutdowns/start-ups influence corrosion and therefore cause decreased lifetime...

  14. 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.

  15. Development of new process network for gas chromatograph and analyzers connected with SCADA system and Digital Control Computers at Cernavoda NPP Unit 1

    International Nuclear Information System (INIS)

    Deneanu, Cornel; Popa Nemoiu, Dragos; Nica, Dana; Bucur, Cosmin

    2007-01-01

    The continuous monitoring of gas mixture concentrations (deuterium/ hydrogen/oxygen/nitrogen) accumulated in 'Moderator Cover Gas', 'Liquid Control Zone' and 'Heat Transport D 2 O Storage Tank Cover Gas', as well as the continuous monitoring of Heavy Water into Light Water concentration in 'Boilers Steam', 'Boilers Blown Down', 'Moderator heat exchangers', and 'Recirculated Water System', sensing any leaks of Cernavoda NPP U1 led to requirement of developing a new process network for gas chromatograph and analyzers connected to the SCADA system and Digital Control Computers of Cernavoda NPP Unit 1. In 2005 it was designed and implemented the process network for gas chromatograph which connected the gas chromatograph equipment to the SCADA system and Digital Control Computers of the Cernavoda NPP Unit 1. Later this process network for gas chromatograph has been extended to connect the AE13 and AE14 Fourier Transform Infrared (FTIR) analyzers with either. The Gas Chromatograph equipment measures with best accuracy the mixture gases (deuterium/ hydrogen/oxygen/nitrogen) concentration. The Fourier Transform Infrared (FTIR) AE13 and AE14 Analyzers measure the Heavy Water into Light Water concentration in Boilers Steam, Boilers BlownDown, Moderator heat exchangers, and Recirculated Water System, monitoring and signaling any leaks. The Gas Chromatograph equipment and Fourier Transform Infrared (FTIR) AE13 and AE14 Analyzers use the new OPC (Object Link Embedded for Process Control) technologies available in ABB's VistaNet network for interoperability with automation equipment. This new process network has interconnected the ABB chromatograph and Fourier Transform Infrared analyzers with plant Digital Control Computers using new technology. The result was an increased reliability and capability for inspection and improved system safety

  16. On-line mass spectrometry measurement of fission gas release from nuclear fuel submitted to thermal transients

    International Nuclear Information System (INIS)

    Guigues, E.; Janulyte, A.; Zerega, Y.; Pontillon, Y.

    2013-06-01

    The work presented in this paper has been performed in the framework of a joint research program between Aix-Marseille University and CEA Cadarache. The aim is to develop a mass spectrometer (MS) device for the MERARG facility. MERARG is devoted to the study of fission gas release measurement, from nuclear fuels submitted to annealing tests in high activity laboratory such as LECA-STAR, thanks to gamma spectrometry. The mass spectrometer will then extend the measurement capability from the γ-emitters gases to all the gases involved in the release in order to have a better understanding of the fission gas release dynamics from fuel during thermal transients. Furthermore, the mass spectrometer instrument combines the capabilities and performances of both on-line (for release kinetic) and off-line implementations (for delayed accurate analysis of capacities containing total release gas). The paper deals with two main axes: (1) the modelling of gas sampling inlet device and its performance and (2) the first MS qualification/calibration results. The inlet device samples the gas and also adapts the pressure between MERARG sweeping line at 1.2 bar and mass spectrometer chamber at high vacuum. It is a two-stage device comprising a capillary at inlet, an intermediate vacuum chamber, a molecular leak inlet and a two-stage pumping device. Pressure drops, conductance and throughputs are estimated both for mass spectrometer operation and for exhaust gas recovery. Possible gas segregation is also estimated and device modification is proposed to attain a more accurate calibration. First experimental results obtained from a standard gas bottle show that the quantitative analysis at a few ppm level can be achieved for all isotopes of Kr and Xe, as well as masses 2 and 4 u. (authors)

  17. Multi Parameter Flow Meter for On-Line Measurement of Gas Mixture Composition

    Directory of Open Access Journals (Sweden)

    Egbert van der Wouden

    2015-04-01

    Full Text Available In this paper we describe the development of a system and model to analyze the composition of gas mixtures up to four components. The system consists of a Coriolis mass flow sensor, density, pressure and thermal flow sensor. With this system it is possible to measure the viscosity, density, heat capacity and flow rate of the medium. In a next step the composition can be analyzed if the constituents of the mixture are known. This makes the approach universally applicable to all gasses as long as the number of components does not exceed the number of measured properties and as long as the properties are measured with a sufficient accuracy. We present measurements with binary and ternary gas mixtures, on compositions that range over an order of magnitude in value for the physical properties. Two platforms for analyses are presented. The first platform consists of sensors realized with MEMS fabrication technology. This approach allows for a system with a high level of integration. With this system we demonstrate a proof of principle for the analyses of binary mixtures with an accuracy of 10%. In the second platform we utilize more mature steel sensor technology to demonstrate the potential of this approach. We show that with this technique, binary mixtures can be measured within 1% and ternary gas mixtures within 3%.

  18. Systematization of by-product plant. (1) Development of on-line analyzers for treatment of gas liquor

    Energy Technology Data Exchange (ETDEWEB)

    Matsumura, Susumu; Taketomi, Hirofumi; Ohashi, Shigeru [Nippon Kokan K.K., Tokyo (Japan)

    1988-04-07

    As a part of systematization of absorption and refinery processing installation for coke oven gas, on-line analyzers for gas liquor treatment with activated sludge were developed and established. A T-NH{sub 3} analyzer using a potential difference titration method was equipped to control NH{sub 3} which had a bad influence upon activated sludge. The oxygen intake rate is measured with an activity measuring instrument in order to get the activity condition of bacteria. The SCN concentration of precipitator outlet solution is measured with an SCN(thiocyanogen) measuring instrument so that conditions of bacteria can be seized. An absorptiometry with ferric chloride is used to analyze it. For a COD measuring instrument, precipitator outlet solution is used and analysis with the JIS method is entirely automated. As a transparency measuring instrument, a color-difference colorimeter is used instead of the former instrument made of glass. According to the collected data, charged coal conditions, and operating conditions of coke oven, the process computer does the calculation for optimization and indicates operation control guidances to the operator. Automated on -line analyzers are useful to save a great deal of labor and contribute to the control and stabilization of operations. 9 figs., 1 tab.

  19. Gas Chromatograph Method Optimization Trade Study for RESOLVE: 20-meter Column v. 8-meter Column

    Science.gov (United States)

    Huz, Kateryna

    2014-01-01

    RESOLVE is the payload on a Class D mission, Resource Prospector, which will prospect for water and other volatile resources at a lunar pole. The RESOLVE payload's primary scientific purpose includes determining the presence of water on the moon in the lunar regolith. In order to detect the water, a gas chromatograph (GC) will be used in conjunction with a mass spectrometer (MS). The goal of the experiment was to compare two GC column lengths and recommend which would be best for RESOLVE's purposes. Throughout the experiment, an Inficon Fusion GC and an Inficon Micro GC 3000 were used. The Fusion had a 20m long column with 0.25mm internal diameter (Id). The Micro GC 3000 had an 8m long column with a 0.32mm Id. By varying the column temperature and column pressure while holding all other parameters constant, the ideal conditions for testing with each column length in their individual instrument configurations were determined. The criteria used for determining the optimal method parameters included (in no particular order) (1) quickest run time, (2) peak sharpness, and (3) peak separation. After testing numerous combinations of temperature and pressure, the parameters for each column length that resulted in the most optimal data given my three criteria were selected. The ideal temperature and pressure for the 20m column were 95 C and 50psig. At this temperature and pressure, the peaks were separated and the retention times were shorter compared to other combinations. The Inficon Micro GC 3000 operated better at lower temperature mainly due to the shorter 8m column. The optimal column temperature and pressure were 70 C and 30psig. The Inficon Micro GC 3000 8m column had worse separation than the Inficon Fusion 20m column, but was able to separate water within a shorter run time. Therefore, the most significant tradeoff between the two column lengths was peak separation of the sample versus run time. After performing several tests, it was concluded that better

  20. On-line gamma spectroscopy measuring station for cover gas monitoring at KNK II

    International Nuclear Information System (INIS)

    Hoffmann, G.; Letz, K.D.

    1980-02-01

    An automated Ge-γ-spectrometer was developed for cover gas monitoring at KNK II which, by the gamma spectra measured, is to allow the following statements to be made on fuel cladding failure: Type, size, variation with time and subsequent development of the failure. In this report the hardware and software will be explained. Besides, an instruction manual was written for the measuring station, which allows to operate it without detailed knowledge of the manuals for the individual hardware components. (orig.) 891 HP/orig. 892 MKO [de

  1. A low thermal mass fast gas chromatograph and its implementation in fast gas chromatography mass spectrometry with supersonic molecular beams.

    Science.gov (United States)

    Fialkov, Alexander B; Moragn, Mati; Amirav, Aviv

    2011-12-30

    A new type of low thermal mass (LTM) fast gas chromatograph (GC) was designed and operated in combination with gas chromatography mass spectrometry (GC-MS) with supersonic molecular beams (SMB), including GC-MS-MS with SMB, thereby providing a novel combination with unique capabilities. The LTM fast GC is based on a short capillary column inserted inside a stainless steel tube that is resistively heated. It is located and mounted outside the standard GC oven on its available top detector port, while the capillary column is connected as usual to the standard GC injector and supersonic molecular beam interface transfer line. This new type of fast GC-MS with SMB enables less than 1 min full range temperature programming and cooling down analysis cycle time. The operation of the fast GC-MS with SMB was explored and 1 min full analysis cycle time of a mixture of 16 hydrocarbons in the C(10)H(22) up to C(44)H(90) range was achieved. The use of 35 mL/min high column flow rate enabled the elution of C(44)H(90) in less than 45 s while the SMB interface enabled splitless acceptance of this high flow rate and the provision of dominant molecular ions. A novel compound 9-benzylazidanthracene was analyzed for its purity and a synthetic chemistry process was monitored for the optimization of the chemical reaction yield. Biodiesel was analyzed in jet fuel (by both GC-MS and GC-MS-MS) in under 1 min as 5 ppm fatty acid methyl esters. Authentic iprodion and cypermethrin pesticides were analyzed in grapes extract in both full scan mode and fast GC-MS-MS mode in under 1 min cycle time and explosive mixture including TATP, TNT and RDX was analyzed in under 1 min combined with exhibiting dominant molecular ion for TATP. Fast GC-MS with SMB is based on trading GC separation for speed of analysis while enhancing the separation power of the MS via the enhancement of the molecular ion in the electron ionization of cold molecules in the SMB. This paper further discusses several features of

  2. Development of an on-line low gas pressure cell for laser ablation-ICP-mass spectrometry

    International Nuclear Information System (INIS)

    Hirata, Takafumi

    2007-01-01

    An on-line low gas pressure cell device has been developed for elemental analysis using laser ablation-ICP-mass spectrometry (LA-ICPMS). Ambient gas in the sample cell was evacuated by a constant-flow diaphragm pump, and the pressure of the sample cell was controlled by changing the flow rate of He-inlet gas. The degree of sample re-deposition around the ablation pit could be reduced when the pressure of the ambient gas was lower than 50 kPa. Produced sample aerosol was drawn and taken from the outlet of the diaphragm pump, and directly introduced into the ICP ion source. The flow rate of He gas controls not only the gas pressure in the sample cell, but also the transport efficiency of the sample particles from the cell to the ICP, and the gas flow rate must be optimized to maximize the signal intensity of the analytes. The flow rates of the He carrier and Ar makeup gas were tuned to maximize the signal intensity of the analytes, and in the case of 238 U from the NIST SRM610 glass material, the signal intensity could be maximized with gas flow rates of 0.4 L/min for He and 1.2 L/min for Ar. The resulting gas pressure in the cell was 30-35 kPa. Using the low gas pressure cell device, the stability in the signal intensities and the resulting precision in isotopic ratio measurements were evaluated. The signal intensity profile of 63 Cu obtained by laser ablation from a metallic sample (NIST SRM976) demonstrated that typical spikes in the transient signal, which can become a large source of analytical error, were no longer found. The resulting precision in the 65 Cu/ 63 Cu ratio measurements was 2-3% (n=10, 2SD), which was half on the level obtained by laser ablation under atmospheric pressure (6-10%). The newly developed low-pressure cell device provides easier optimization of the operational conditions, together with smaller degrees of sample re-deposition and better stability in the signal intensity, even from a metallic sample. (author)

  3. An automated multidimensional preparative gas chromatographic system for isolation and enrichment of trace amounts of xenon from ambient air.

    Science.gov (United States)

    Larson, Tuula; Östman, Conny; Colmsjö, Anders

    2011-04-01

    The monitoring of radioactive xenon isotopes is one of the principal methods for the detection of nuclear explosions in order to identify clandestine nuclear testing. In this work, a miniaturized, multiple-oven, six-column, preparative gas chromatograph was constructed in order to isolate trace quantities of radioactive xenon isotopes from ambient air, utilizing nitrogen as the carrier gas. The multidimensional chromatograph comprised preparative stainless steel columns packed with molecular sieves, activated carbon, and synthetic carbon adsorbents (e.g., Anasorb®-747 and Carbosphere®). A combination of purification techniques--ambient adsorption, thermal desorption, back-flushing, thermal focusing, and heart cutting--was selectively optimized to produce a well-defined xenon peak that facilitated reproducible heart cutting and accurate quantification. The chromatographic purification of a sample requires approximately 4 h and provides complete separation of xenon from potentially interfering components (such as water vapor, methane, carbon dioxide, and radon) with recovery and accuracy close to 100%. The preparative enrichment process isolates and concentrates a highly purified xenon gas fraction that is suitable for subsequent ultra-low-level γ-, ß/γ-spectroscopic or high-resolution mass spectrometric measurement (e.g., to monitor the gaseous fission products of nuclear explosions at remote locations). The Xenon Processing Unit is a free-standing, relatively lightweight, and transportable system that can be interfaced to a variety of sampling and detection systems. It has a relatively inexpensive, rugged, and compact modular (19-inch rack) design that provides easy access to all parts for maintenance and has a low power requirement.

  4. On-line fast response device and method for measuring dissolved gas in a fluid

    Science.gov (United States)

    Tutu, Narinder Kumar [Manorville, NY

    2011-01-11

    A method and device for the measurement of dissolved gas within a fluid. The fluid, substantially a liquid, is pumped into a pipe. The flow of the fluid is temporally restricted, creating one or more low pressure regions. A measurement indicative of trapped air is taken before and after the restriction. The amount of dissolved air is calculated from the difference between the first and second measurements. Preferably measurements indicative of trapped air is obtained from one or more pressure transducers, capacitance transducers, or combinations thereof. In the alternative, other methods such as those utilizing x-rays or gamma rays may also be used to detect trapped air. Preferably, the fluid is a hydraulic fluid, whereby dissolved air in the fluid is detected.

  5. Automated-process gas-chromatograph system for use in accelerated corrosion testing of HTGR core-support posts

    International Nuclear Information System (INIS)

    Harper, R.E.; Herndon, P.G.

    1982-01-01

    An automated-process gas chromatograph is the heart of a gaseous-impurities-analysis system developed for the Oak Ridge National Laboratory Core Support Performance Test, at which graphite core-support posts for high-temperature gas-cooled fission reactors are being subjected to accelerated corrosion tests under tightly controlled conditions of atmosphere and temperature. Realistic estimation of in-core corrosion rates is critically dependent upon the accurate measurement of low concentrations of CO, CO 2 , CH 4 , H 2 , and O 2 in the predominantly helium atmosphere. In addition, the capital and labor investment associated with each test puts a premium upon the reliability of the analytical system, as excessive downtime or failure to obtain accurate data would result in unacceptable costs and schedule delays. After an extensive survey of available measurement techniques, gas chromatography was chosen for reasons of accuracy, flexibility, good-performance record, and cost

  6. In situ derivatization and hollow fiber membrane microextraction for gas chromatographic determination of haloacetic acids in water

    International Nuclear Information System (INIS)

    Varanusupakul, Pakorn; Vora-adisak, Narongchai; Pulpoka, Bancha

    2007-01-01

    An alternative method for gas chromatographic determination of haloacetic acids (HAAs) in water using direct derivatization followed by hollow fiber membrane liquid-phase microextraction (HF-LPME) has been developed. The method has improved the sample preparation step according to the conventional US EPA Method 552.2 by combining the derivatization and the extraction into one step prior to determination by gas chromatography electron captured detector (GC-ECD). The HAAs were derivatized with acidic methanol into their methyl esters and simultaneously extracted with supported liquid hollow fiber membrane in headspace mode. The derivatization was attempted directly in water sample without sample evaporation. The HF-LPME was performed using 1-octanol as the extracting solvent at 55 deg. C for 60 min with 20% Na 2 SO 4 . The linear calibration curves were observed for the concentrations ranging from 1 to 300 μg L -1 with the correlation coefficients (R 2 ) being greater than 0.99. The method detection limits of most analytes were below 1 μg L -1 except DCAA and MCAA that were 2 and 18 μg L -1 , respectively. The recoveries from spiked concentration ranged from 97 to 109% with %R.S.D. less than 12%. The method was applied for determination of HAAs in drinking water and tap water samples. The method offers an easy one step high sample throughput sample preparation for gas chromatographic determination of haloacetic acids as well as other contaminants in water

  7. Incident at university research facility - melt down of gas chromatograph evaporation block and failure of a passive safety barrier

    DEFF Research Database (Denmark)

    Jensen, Niels; Jørgensen, Sten Bay

    2014-01-01

    Two incidents are described highlighting the importance of process hazard analysis in university laboratories. In the first incident, an online gas chromatograph (GC) was being developed. A complete meltdown of the heating blog was experienced during testing because the PC had failed to turn off...... the heating of the evaporation circuit. There had been no design review of the GC, nor any code review of the software controlling the GC. Neither had there been any management of change review for the introduction of the GC in the pilot plant environment, and so the GC had been introduced without any...

  8. 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.

  9. On-line component ratio measurement of oil/gas/water mixtures using an admittance sensor

    Energy Technology Data Exchange (ETDEWEB)

    Andersen, J A

    1984-01-01

    The operator of a production platform is primarily interested in which types of fluids a well is producing and how quickly these different components are being produced. The component ratio and production rate of a well vary during the life of a field. To optimize production, measurement of each well's output is thus desirable. Current designs for subsea production systems lack means of continuously measuring three-component flows. A new method of component ratio measurement is described. The fraction of oil, gas and water flowing between two insulated electrode plates is determined by measuring both the electrical conductance and suseptance across the sensor. A preliminary evaluation of the new measurement system has been performed using a process oil/ water/air mixture. The method is not limited to small pipe diameters. The only possible limitation is that for low velocities in very large pipe diameters an in-line mixer may be required. Advantages of this new system are that real-time measurement of void fraction and water content is possible if a non-intrusive rugged sensor is used, and there are no range limitations, as each component may be measured for any given concentration. 4 references.

  10. A gas chromatograph system for semi-continuous greenhouse gas measurements at Puy de Dôme station, Central France

    Science.gov (United States)

    Lopez, M.; Schmidt, M.; Ramonet, M.; Bonne, J.-L.; Colomb, A.; Kazan, V.; Laj, P.; Pichon, J.-M.

    2015-03-01

    Three years of greenhouse gases measurements, obtained using a gas chromatograph (GC) system located at the Puy de Dôme station at 1465 m a.s.l. in Central France are presented. The GC system was installed in 2010 at Puy de Dôme and was designed for automatic and accurate semi-continuous measurements of atmospheric carbon dioxide, methane, nitrous oxide and sulfur hexafluoride mole fractions. We present in detail the instrumental set up and the calibration strategy, which together allow the GC to reach repeatabilities of 0.1 μmol mol-1, 1.2, 0.3 nmol mol-1 and 0.06 pmol mol-1 for CO2, CH4, N2O and SF6, respectively. Comparisons of the atmospheric time series with those obtained using other instruments shown that the GC system meets the World Meteorological Organization recommendations. The analysis of the three-year atmospheric time series revealed how the planetary boundary layer height drives the mole fractions observed at a mountain site such as Puy de Dôme where air masses alternate between the planetary boundary layer and the free troposphere. Accurate long-lived greenhouse gases measurements collocated with 222Rn measurements as an atmospheric tracer, allowed us to determine the CO2, CH4 and N2O emissions in the catchment area of the station. The derived CO2 surface flux revealed a clear seasonal cycle with net uptake by plant assimilation in the spring and net emission caused by the biosphere and burning of fossil fuel during the remainder of the year. We calculated a mean annual CO2 flux of 1150 t(CO2) km-2. The derived CH4 and N2O emissions in the station catchment area were 5.6 t(CH4) km-2 yr-1 and 1.5 t(N2O) km-2 yr-1, respectively. Our derived annual CH4 flux is in agreement with the national French inventory, whereas our derived N2O flux is five times larger than the same inventory.

  11. The gas-phase on-line production of phosphoryl halides, Pox sub 3 and their identification by infrared spectroscopy

    International Nuclear Information System (INIS)

    Allaf, A.W.

    1999-01-01

    A new route has been devised, leading to the production of Pox sub 3 molecules where X=F, Br and I by an on-line process using phosphoryl chloride, POCI sub 3 as a starting material passed over heated sodium fluoride, NaF, potassium bromide, KBr and potassium iodide, K1 at 535 Centigrade, 690 Centigrade and 480 Centigrade, respectively. The low resolution gas-phase fourier transform infrared spectra reported for the first time showed strong bands centered at 1411.6, 1322.9, 1300.8 and 1285 cm sup - 1, assigned to EPSILON sub 1 (a sub 1), the O = P stretching fundamental of POF sub 3 , POCI sub 3 , POBr sub 3 and POI sub 3 , respectively. Attempts were made to prepare POCI sub 2 and POBr sub 2 , by an on-line process using POCI sub 3 again but passed over heated sodium and potassium bromide for POCI sub 2 and POBr sub 2. (author)

  12. A single gas chromatograph for accurate atmospheric mixing ratio measurements of CO2, CH4, N2O, SF6 and CO

    NARCIS (Netherlands)

    van der Laan, S.; Neubert, R. E. M.; Meijer, H. A. J.; Simpson, W.R.

    2009-01-01

    We present an adapted gas chromatograph capable of measuring simultaneously and semi-continuously the atmospheric mixing ratios of the greenhouse gases CO2, CH4, N2O and SF6 and the trace gas CO with high precision and long-term stability. The novelty of our design is that all species are measured

  13. In-line gas chromatographic apparatus for measuring the hydrophobic micropore volume (HMV) and contaminant transformation in mineral micropores

    International Nuclear Information System (INIS)

    Cheng Hefa; Reinhard, Martin

    2010-01-01

    Desorption of hydrophobic organic compounds from micropores is characteristically slow compared to surface adsorption and partitioning. The slow-desorbing mass of a hydrophobic probe molecule can be used to calculate the hydrophobic micropore volume (HMV) of microporous solids. A gas chromatographic apparatus is described that allows characterization of the sorbed mass with respect to the desorption rate. The method is demonstrated using a dealuminated zeolite and an aquifer sand as the model and reference sorbents, respectively, and trichloroethylene (TCE) as the probe molecule. A glass column packed with the microporous sorbent is coupled directly to a gas chromatograph that is equipped with flame ionization and electron capture detectors. Sorption and desorption of TCE on the sorbent was measured by sampling the influent and effluent of the column using a combination of switching and injection valves. For geosorbents, the HMV is quantified based on Gurvitsch's rule from the mass of TCE desorbed at a rate that is characteristic for micropores. Instrumental requirements, design considerations, hardware details, detector calibration, performance, and data analysis are discussed along with applications. The method is novel and complements traditional vacuum gravimetric and piezometric techniques, which quantify the total pore volume under vacuum conditions. The HMV is more relevant than the total micropore volume for predicting the fate and transport of organic contaminants in the subsurface. Sorption in hydrophobic micropores strongly impacts the mobility of organic contaminants, and their chemical and biological transformations. The apparatus can serve as a tool for characterizing microprous solids and investigating contaminant-solid interactions.

  14. Proposal for data acquisition system of gas chromatograph and natural gas transfer custody via web; Proposta para um sistema de aquisicao de dados de cromatografia e medicao fiscal de gas natural via web

    Energy Technology Data Exchange (ETDEWEB)

    Santana, Jose Paulo C.; Guimaraes, Marcelo F.; Zeitoune, Rafael J. [PETROBRAS, Rio de Janeiro, RJ (Brazil)

    2005-07-01

    In this paper, is presented a proposal of a Chromatograph and Transfer Custody Measurement Data Acquisition System through Web, complementary to the SCADA System, responsible for control and monitoring PETROBRAS Gas Pipelines, intended to comply with the requirements of the Gerencias de Qualidade e Medicao (MQD) and Planejamento Integrado da Logistica (PCL) from PETROBRAS Gas e Energia, regarding the evaluation of the quality of the natural gas that is being commercialized, as well as its billing. (author)

  15. Preliminary studies of using preheated carrier gas for on-line membrane extraction of semivolatile organic compounds.

    Science.gov (United States)

    Liu, Xinyu; Pawliszyn, Janusz

    2007-04-01

    In this paper, we present results for the on-line determination of semivolatile organic compounds (SVOCs) in air using membrane extraction with a sorbent interface-ion mobility spectrometry (MESI-IMS) system with a preheated carrier (stripping) gas. The mechanism of the mass transfer of SVOCs across a membrane was initially studied. In comparison with the extraction of volatile analytes, the mass transfer resistance that originated from the slow desorption from the internal membrane surface during the SVOC extraction processes should be taken into account. A preheated carrier gas system was therefore built to facilitate desorption of analytes from the internal membrane surface. With the benefit of a temperature gradient existing between the internal and external membrane surfaces, an increase in the desorption rate of a specific analyte at the internal surface and the diffusion coefficient within the membrane could be achieved while avoiding a decrease of the distribution constant on the external membrane interface. This technique improved both the extraction rate and response times of the MESI-IMS system for the analysis of SVOCs. Finally, the MESI-IMS system was shown to be capable of on-site measurement by monitoring selected polynuclear aromatic hydrocarbons emitted from cigarette smoke.

  16. A multiphase flow meter for the on-line determination of the flow rates of oil, water and gas

    International Nuclear Information System (INIS)

    Roach, G.J.; Watt, J.S.

    1997-01-01

    Multiphase mixtures of crude oil, formation water and gas are carried in pipelines from oil wells to production facilities. Multiphase flow meters (MFMs) are being developed to determine the flow rates of each component of the heterogeneous mixture in the pipeline. CSIRO Minerals has developed and field tested a gamma-ray MFM for the on-line determination of the flow rates of heterogeneous mixtures of oil, water and gas in pipelines. It consists of two specialised gamma-ray transmission gauges, and pressure and temperature sensors, mounted on the pipeline carrying the full flow of the production stream. The MFM separately measures liquids and gas flow rates, and the volume ratio of water and liquids (water cut). The MFM has been trialled at three offshore production facilities in Australia. In each, the MFM was mounted on the pipeline between the test manifold and the test separator. The multiphase streams from the various wells feeding to the platform were sequentially routed past the MFM. The MFM and test separator outputs were compared using regression analysis. The flow rates of oil, water and gas were each determined to relative errors in the range of 5-10% . The MFM has been in routine use on the West Kingfish platform in the Bass Strait since November 1994. The MFM was recently tested over a wide range of flow conditions at a Texaco flow facility near Houston. Water cut, based on pre-trial calibration, was determined to 2% rms over the range 0-100% water cut. The liquids and gas flow results were interpreted based on slip correlations obtained from comparison of the MFM and Texaco flows. Using these, the relative errors were respectively 6.6% for liquid flow, 6.2% for gas, 8% for oil and 8% for water. The MFM is licensed to Kvaerner FSSL of Aberdeen. Kvaerner will supply the gamma-ray MFM for both platform and subsea use. Technology transfer commenced in December 1996, and Kvaerner completed the manufacture of the first MFM in August 1997

  17. In situ derivatization and hollow fiber membrane microextraction for gas chromatographic determination of haloacetic acids in water

    Energy Technology Data Exchange (ETDEWEB)

    Varanusupakul, Pakorn [Chromatography and Separation Research Unit, Department of Chemistry, Faculty of Science, Chulalongkorn University, Phayathai Road, Patumwan, Bangkok 10330 (Thailand)], E-mail: pakorn.v@chula.ac.th; Vora-adisak, Narongchai; Pulpoka, Bancha [Chromatography and Separation Research Unit, Department of Chemistry, Faculty of Science, Chulalongkorn University, Phayathai Road, Patumwan, Bangkok 10330 (Thailand)

    2007-08-15

    An alternative method for gas chromatographic determination of haloacetic acids (HAAs) in water using direct derivatization followed by hollow fiber membrane liquid-phase microextraction (HF-LPME) has been developed. The method has improved the sample preparation step according to the conventional US EPA Method 552.2 by combining the derivatization and the extraction into one step prior to determination by gas chromatography electron captured detector (GC-ECD). The HAAs were derivatized with acidic methanol into their methyl esters and simultaneously extracted with supported liquid hollow fiber membrane in headspace mode. The derivatization was attempted directly in water sample without sample evaporation. The HF-LPME was performed using 1-octanol as the extracting solvent at 55 deg. C for 60 min with 20% Na{sub 2}SO{sub 4}. The linear calibration curves were observed for the concentrations ranging from 1 to 300 {mu}g L{sup -1} with the correlation coefficients (R{sup 2}) being greater than 0.99. The method detection limits of most analytes were below 1 {mu}g L{sup -1} except DCAA and MCAA that were 2 and 18 {mu}g L{sup -1}, respectively. The recoveries from spiked concentration ranged from 97 to 109% with %R.S.D. less than 12%. The method was applied for determination of HAAs in drinking water and tap water samples. The method offers an easy one step high sample throughput sample preparation for gas chromatographic determination of haloacetic acids as well as other contaminants in water.

  18. A gas/liquid chromatographic-mass spectrometric method for the rapid screening of 250 pesticides in aqueous matrices

    Energy Technology Data Exchange (ETDEWEB)

    Chandramouli, B.; Harvan, D.; Brittain, S.; Hass, R. [Eno River Labs, LLC. Durham, NC (United States)

    2004-09-15

    Pesticide residues in food present a potentially serious and significant cause for concern. Many pesticides have been associated with significant health effects to the nervous and endocrine systems and some have been deemed carcinogenic. There are many well-established techniques for pesticide analysis. However, commercial pesticide methods have traditionally only been available for specific pesticide families, such as chlorinated pesticides or herbicides, and at detection limits ranging from 0.05 ppb to 1 ppm in aqueous matrices. Techniques that can quickly screen for the presence/absence of pesticide residues in food matrices are critical in ensuring the safety of food and water. This paper outlines a combined Gas Chromatographic-High Resolution Mass Spectrometric (GC-HRMS) and Liquid Chromatographic Tandem Mass Spectrometric (LC-MS/MS) screening assay for 250 pesticides that was developed for use in water, and soda samples at screening levels ranging from 0.1-5 ppb. The pesticides selected have been identified by the European Union as being of concern and the target of possible legislation. The list encompasses a variety of pesticide classes and compound groupings.

  19. Equations for nickel-chromium wire heaters of column transfer lines in gas chromatographic-electroantennographic detection (GC-EAD).

    Science.gov (United States)

    Byers, John A

    2004-05-30

    Heating of chromatographic columns, transfer lines, and other devices is often required in neuroscience research. For example, volatile compounds passing through a capillary column of a gas chromatograph (GC) can be split, with half exiting the instrument through a heated transfer line to an insect antenna or olfactory sensillum for electroantennographic detector (GC-EAD) recordings. The heated transfer line is used to prevent condensation of various chemicals in the capillary that would otherwise occur at room temperature. Construction of such a transfer line heater is described using (80/20%) nickel-chromium heating wire wrapped in a helical coil and powered by a 120/220 V ac rheostat. Algorithms were developed in a computer program to estimate the voltage at which a rheostat should be set to obtain the desired heater temperature for a specific coil. The coil attributes (radius, width, number of loops, or length of each loop) are input by the user, as well as AWG size of heating wire and desired heater temperature. The program calculates total length of wire in the helix, resistance of the wire, amperage used, and the voltage to set the rheostat. A discussion of semiochemical isolation methods using the GC-EAD and bioassays is presented.

  20. Gas-chromatographic separation of hydrogen isotopes mixtures on capillary molecular sieve 5 A column at 173 K

    International Nuclear Information System (INIS)

    Bidica, N.; Preda, A.; Stanciu, V.

    2002-01-01

    Analysis of a gas mixture of hydrogen species, is not too easy because the differences in their physical-chemical properties are very small; the most different are their masses, and consequently most common analytical method appear to be the mass-spectrometry. However, the impossibility to distinguish between two ions (atomic or molecular) with the same mass renders this method as unapplicable. Another problem is the decay of tritium with production of 3 He. These disadvantages of mass-spectrometry have made that other analytical methods, like gas chromatography, to be considered and developed. Thus, there are many papers about various chromatographic columns especially prepared for hydrogen species separation but the preparation and treatment of these columns are very difficult to reproduce. Besides these, there are two other main disadvantages: column operating temperature is very low and long retention times for hydrogen species (more than half an hour) are required. However, the gas-chromatography method still remains an appropriate one. The method described in this paper was based on using a capillary molecular sieve 5A column which has been operated for this kind of separation. The retention times were relatively short, about 8-9 minutes. The carrier gas was Ne and the detector - TCD. In the paper chromatograms for various carrier flow rates and various hydrogen isotope mixtures are presented. The results demonstrated a quite good efficiency for H 2 , HD, D 2 and a not very good one for orthoH 2 -paraH 2 . (authors)

  1. In-line gas chromatographic apparatus for measuring the hydrophobic micropore volume (HMV) and contaminant transformation in mineral micropores.

    Science.gov (United States)

    Cheng, Hefa; Reinhard, Martin

    2010-07-15

    Desorption of hydrophobic organic compounds from micropores is characteristically slow compared to surface adsorption and partitioning. The slow-desorbing mass of a hydrophobic probe molecule can be used to calculate the hydrophobic micropore volume (HMV) of microporous solids. A gas chromatographic apparatus is described that allows characterization of the sorbed mass with respect to the desorption rate. The method is demonstrated using a dealuminated zeolite and an aquifer sand as the model and reference sorbents, respectively, and trichloroethylene (TCE) as the probe molecule. A glass column packed with the microporous sorbent is coupled directly to a gas chromatograph that is equipped with flame ionization and electron capture detectors. Sorption and desorption of TCE on the sorbent was measured by sampling the influent and effluent of the column using a combination of switching and injection valves. For geosorbents, the HMV is quantified based on Gurvitsch's rule from the mass of TCE desorbed at a rate that is characteristic for micropores. Instrumental requirements, design considerations, hardware details, detector calibration, performance, and data analysis are discussed along with applications. The method is novel and complements traditional vacuum gravimetric and piezometric techniques, which quantify the total pore volume under vacuum conditions. The HMV is more relevant than the total micropore volume for predicting the fate and transport of organic contaminants in the subsurface. Sorption in hydrophobic micropores strongly impacts the mobility of organic contaminants, and their chemical and biological transformations. The apparatus can serve as a tool for characterizing microporous solids and investigating contaminant-solid interactions. 2010 Elsevier B.V. All rights reserved.

  2. In-line gas chromatographic apparatus for measuring the hydrophobic micropore volume (HMV) and contaminant transformation in mineral micropores

    Energy Technology Data Exchange (ETDEWEB)

    Cheng Hefa [State Key Laboratory of Organic Geochemistry, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou 510640 (China); Reinhard, Martin, E-mail: reinhard@stanford.edu [Department of Civil and Environmental Engineering, Stanford University, Stanford, CA 94305-4020 (United States)

    2010-07-15

    Desorption of hydrophobic organic compounds from micropores is characteristically slow compared to surface adsorption and partitioning. The slow-desorbing mass of a hydrophobic probe molecule can be used to calculate the hydrophobic micropore volume (HMV) of microporous solids. A gas chromatographic apparatus is described that allows characterization of the sorbed mass with respect to the desorption rate. The method is demonstrated using a dealuminated zeolite and an aquifer sand as the model and reference sorbents, respectively, and trichloroethylene (TCE) as the probe molecule. A glass column packed with the microporous sorbent is coupled directly to a gas chromatograph that is equipped with flame ionization and electron capture detectors. Sorption and desorption of TCE on the sorbent was measured by sampling the influent and effluent of the column using a combination of switching and injection valves. For geosorbents, the HMV is quantified based on Gurvitsch's rule from the mass of TCE desorbed at a rate that is characteristic for micropores. Instrumental requirements, design considerations, hardware details, detector calibration, performance, and data analysis are discussed along with applications. The method is novel and complements traditional vacuum gravimetric and piezometric techniques, which quantify the total pore volume under vacuum conditions. The HMV is more relevant than the total micropore volume for predicting the fate and transport of organic contaminants in the subsurface. Sorption in hydrophobic micropores strongly impacts the mobility of organic contaminants, and their chemical and biological transformations. The apparatus can serve as a tool for characterizing microprous solids and investigating contaminant-solid interactions.

  3. Gas chromatographic-mass spectrometric analysis of biomarkers related to folate and cobalamin status in human serum after dimercaptopropanesulfonate reduction and heptafluorobutyl chloroformate derivatization

    Czech Academy of Sciences Publication Activity Database

    Šimek, Petr; Hušek, Petr; Zahradníčková, Helena

    2008-01-01

    Roč. 80, č. 15 (2008), s. 5776-5782 ISSN 0003-2700 R&D Projects: GA ČR GA303/06/1674 Institutional research plan: CEZ:AV0Z50070508 Keywords : biomarkers * gas chromatographic * chloroformate derivatization Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 5.712, year: 2008

  4. 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

  5. Comparison of radioimmunoassay and gas chromatographic mass spectrometric assay for d-amphetamine

    International Nuclear Information System (INIS)

    Powers, K.H.; Ebert, M.H.

    1979-01-01

    Quantification of low levels of psychotropic drugs (10 -7 to 10 -9 g ml -1 ) in small volumes of plasma requires sensitive and accurate methods. Validation of these methods is best achieved by comparing results obtained using several techniques. In this study, amphetamine levels in plasma were measured using gas chromatography mass spectrometry and radioimmunoassay. Correlation of the results obtained by the two methods was found to be positive and high (R = 0.9822). The average coefficient of variation between assays for gas chromatography mass spectrometry was 5.8% and for radioimmunoassay was 12.3%, while the average coefficient of variation within assays for gas chromatography mass spectrometry was 4.9% and for radioimmunoassay 6.9%. Although gas chromatography mass spectrometry was 1.9 times more sensitive than radioimmunoassay, for most purposes, the convenience of the radioimmunoassay method outweighs the technical superiority of gas chromatography mass spectrometry. (author)

  6. Effects of γ-irradiation on caprolactam level from multilayer PA-6 films for food packaging: Development and validation of a gas chromatographic method

    International Nuclear Information System (INIS)

    Araujo, Henrique Peres; Felix, Juliana Silva; Manzoli, Jose Eduardo; Padula, Marisa; Monteiro, Magali

    2008-01-01

    A gas chromatographic method to determine caprolactam in multilayer PA-6 films used for meat foodstuffs and cheese was developed and validated. A wide linear range (0.8-400 μg/ml), RSD≤4.1% and recovery higher than 90.0% were obtained for the chromatographic system, while precision and accuracy of the method showed RSD≤3.8%, recovery from 95.5-100.0% and LOQ of 32 μg/g. Irradiated (3, 7 and 12 kGy) and non-irradiated commercial films were analyzed. Most of them increased caprolactam levels with the increase of irradiation doses

  7. Effects of {gamma}-irradiation on caprolactam level from multilayer PA-6 films for food packaging: Development and validation of a gas chromatographic method

    Energy Technology Data Exchange (ETDEWEB)

    Araujo, Henrique Peres; Felix, Juliana Silva [Department of Food and Nutrition, School of Pharmaceutical Science, Sao Paulo State University, PO Box 502, 14801-902 Araraquara, SP (Brazil); Manzoli, Jose Eduardo [Nuclear and Energetic Research Institute (IPEN), Sao Paulo, SP (Brazil); Padula, Marisa [Packaging Technology Center/Food Technology Institute (CETEA/ITAL), Campinas, SP (Brazil); Monteiro, Magali [Department of Food and Nutrition, School of Pharmaceutical Science, Sao Paulo State University, PO Box 502, 14801-902 Araraquara, SP (Brazil)], E-mail: monteiro@fcfar.unesp.br

    2008-07-15

    A gas chromatographic method to determine caprolactam in multilayer PA-6 films used for meat foodstuffs and cheese was developed and validated. A wide linear range (0.8-400 {mu}g/ml), RSD{<=}4.1% and recovery higher than 90.0% were obtained for the chromatographic system, while precision and accuracy of the method showed RSD{<=}3.8%, recovery from 95.5-100.0% and LOQ of 32 {mu}g/g. Irradiated (3, 7 and 12 kGy) and non-irradiated commercial films were analyzed. Most of them increased caprolactam levels with the increase of irradiation doses.

  8. Chromatographic separations of stereoisomers

    Energy Technology Data Exchange (ETDEWEB)

    Souter, R.W.

    1985-01-01

    This text covers both diastereomers and enantiomers; describes techniques for GC, HPLC, and other chromatographic methods; and tabulates results of various applications by both techniques and compound class. It provides current knowledge about separation mechanisms and interactions of asymmetric molecules, as well as experimental and commercial materials such as columns, instruments, and derivatization reagents. The contents also include stereoisomer separations by gas chromatography. Stereoisomer separations by high-performance liquid chromatography. Stereoisomer separations by other chromatographic techniques.

  9. Gas Chromatographic Determination of Methyl Salicylate in Rubbing Alcohol: An Experiment Employing Standard Addition.

    Science.gov (United States)

    Van Atta, Robert E.; Van Atta, R. Lewis

    1980-01-01

    Provides a gas chromatography experiment that exercises the quantitative technique of standard addition to the analysis for a minor component, methyl salicylate, in a commercial product, "wintergreen rubbing alcohol." (CS)

  10. On-line monitoring of trace compounds in the flue gas of an incineration pilot plant: Formation of polycyclic aromatic hydrocarbons

    International Nuclear Information System (INIS)

    Heger, H. J.; Zimmermann, R.; Dorfner, R.; Kettrup, A.; Boesl, U.

    1998-01-01

    Laser mass spectrometry is applied for on-line analysis of PAHs from a complex flue gas matrix in the combustion chamber of an incineration plant. Process monitoring of industrial processes can be performed. New insights into the formation of toxic combustion byproducts are possible

  11. Quantitative analysis of higher hydrocarbons in natural gas using coupled solid-phase extraction / supercritiacal fluid extraction with on-line GC analysis

    NARCIS (Netherlands)

    Janssen, J.G.M.; Cramers, C.A.M.G.; Meulen-Kuijk, van der L.; Smit, A.L.C.; Sandra, P.; Devos, G.

    1993-01-01

    Characterisation of natural gas with respect to the hydrocarbon content is a challenging analytical problem due to the extremely low concentrations and the complexity of the matrix. In this publication a method is described for fully on-line preconcentration and analysis of n-nonane and higher

  12. Data correlation in on-line solid-phase extraction-gas chromatography-atomic emission/mass spectrometric detection of unknown microcontaminants

    NARCIS (Netherlands)

    Hankemeier, Th.; Rozenbrand, J.; Abhadur, M.; Vreuls, J.J.; Brinkman, U.A.Th.

    1998-01-01

    A procedure is described for the (non-target) screening of hetero-atom-containing compounds in tap and waste water by correlating data obtained by gas chromatography (GC) using atomic emission (AED) and mass selective (MS) detection. Solid-phase extraction (SPE) was coupled on-line to both GC

  13. Experience with an on-line computer for controlling and optimizing the gas supply and the application of various peak-load supply plants of a public utility

    Energy Technology Data Exchange (ETDEWEB)

    Poll, J [Technische Werke der Stadt Stuttgart A.G. (Germany, F.R.)

    1977-02-01

    The computer system has the following tasks: 1) On-line control; 2) supply of an information system; 3) performance of a gas marketing forecast; 4) background computations. Measured data are compiled, processed, monitored, recorded, prepared, and stored. The process is controlled by about a dozen programmes, the remaining tasks are taken over by 22 programmes. The system has proved a success.

  14. Evaluation of highly polar ionic liquid gas chromatographic column for the determination of the fatty acids in milk fat.

    Science.gov (United States)

    Delmonte, Pierluigi; Fardin-Kia, Ali Reza; Kramer, John K G; Mossoba, Magdi M; Sidisky, Len; Tyburczy, Cynthia; Rader, Jeanne I

    2012-04-13

    The SLB-IL111, a new ionic liquid capillary column for gas chromatography available from Supelco Inc., was recently shown to provide enhanced separation of unsaturated geometric and positional isomers of fatty acid (FAs) when it was compared to cyanopropylsiloxane (CPS) columns currently recommended for the analysis of fatty acid methyl esters (FAMEs). A 200 m SLB-IL111 capillary column, operated under a combined temperature and eluent flow gradient, was successfully used to resolve most of the FAs contained in milk fat in a single 80 min chromatographic separation. The selected chromatographic conditions provided a balanced, simultaneous separation of short-chain (from 4:0), long-chain polyunsaturated fatty acids (PUFAs), and most of the unsaturated FA positional/geometric isomers contained in milk fat. Among the monounsaturated fatty acids (MUFAs), these conditions separated t11-18:1 and t10-18:1 FAs, the two most abundant trans fatty acids (t-FA) contained in most dairy products. These t-FAs reportedly have different biological activities. The conjugated linoleic acid (CLA) isomers commonly found in dairy products were separated from each other, including t7,c9-18:2 from c9,t11-18:2, which eliminated the need for their complementary silver ion HPLC analysis. The application of the SLB-IL111 column provided a complementary elution profile of FAMEs to those obtained by CPS columns, allowing for a more comprehensive FA analysis of total milk fat. The FAMEs were identified by the use of available reference materials, previously synthesized and characterized reference mixtures, and prior separations of the milk fat FAMEs by silver ion chromatography based on the number/geometry of double bonds. Published by Elsevier B.V.

  15. Determination of trihalomethanes in waters by ionic liquid-based single drop microextraction/gas chromatographic/mass spectrometry.

    Science.gov (United States)

    Aguilera-Herrador, Eva; Lucena, Rafael; Cárdenas, Soledad; Valcárcel, Miguel

    2008-10-31

    A simple, rapid, solventless method for the determination of trihalomethanes (THMs) (chloroform, bromodichloromethane, dibromochloromethane and bromoform) in water samples is presented. The analytes are extracted from the headspace of the aqueous matrix into a 2 microL drop of the ionic liquid 1-octyl-3-methyl-imidazolium hexafluorophosphate working at 30 degrees C for 30 min. The separation and detection of the target compounds is accomplished by gas chromatography/mass spectrometry owing to the use of an interface that efficiently transfers the analytes extracted in the ionic liquid drop to the gas chromatograph while preventing the ionic liquid from entering the column. The detection limits obtained are below the values compelled by the legislation, ranging from 0.5 microg L(-1) for chloroform and bromodichloromethane to 0.9 microg L(-1) for dibromochloromethane. The use of ionic liquid in the extraction procedure avoids the use of organic solvents and leads to relative standard deviations that range from 3.1% to 4.8%.

  16. Gas chromatographic analysis of dimethyltryptamine and beta-carboline alkaloids in ayahuasca, an Amazonian psychoactive plant beverage.

    Science.gov (United States)

    Pires, Ana Paula Salum; De Oliveira, Carolina Dizioli Rodrigues; Moura, Sidnei; Dörr, Felipe Augusto; Silva, Wagner Abreu E; Yonamine, Mauricio

    2009-01-01

    Ayahuasca is obtained by infusing the pounded stems of Banisteriopsis caapi in combination with the leaves of Psychotria viridis. P. viridis is rich in the psychedelic indole N,N-dimethyltryptamine, whereas B. caapi contains substantial amounts of beta-carboline alkaloids, mainly harmine, harmaline and tetrahydroharmine, which are monoamine-oxidase inhibitors. Because of differences in composition in ayahuasca preparations, a method to measure their main active constituents is needed. To develop a gas chromatographic method for the simultaneous determination of dimethyltryptamine and the main beta-carbolines found in ayahuasca preparations. The alkaloids were extracted by means of solid phase extraction (C(18)) and detected by gas chromatography with nitrogen/phosphorous detector. The lower limit of quantification (LLOQ) was 0.02 mg/mL for all analytes. The calibration curves were linear over a concentration range of 0.02-4.0 mg/mL (r(2 )> 0.99). The method was also precise (RSD ayahuasca was developed and validated. The method can be useful to estimate administered doses in animals and humans for further pharmacological and toxicological investigations of ayahuasca. Copyright (c) 2009 John Wiley & Sons, Ltd.

  17. Gas-liquid chromatographic determination of aniline metabolites of substituted urea and carbamate herbicides in aqueous solution.

    Science.gov (United States)

    Hargesheimer, E E; Coutts, R T; Pasutto, F M

    1981-07-01

    A simple gas-liquid chromatographic (GLC) method has been developed which provides sensitivity and specificity for the analysis of complex mixtures of the commonly occurring herbicide metabolites aniline, 3-chloroaniline, 4-chloroaniline, 4-bromoaniline, and 3-chloro-4-methylaniline. All of these anilines react with acetic anhydride directly in basified aqueous solution. Further reaction of the acetylated anilines with trifluoroacetic anhydride gave diacyl derivatives which were readily resolved by gas chromatography. The structures of the N-acetylated and N-trifluoroacetylated derivatives of benzylamine (internal standard) and the anilines were confirmed by GLC-mass spectrometry. In distilled water the minimum detectable concentrations of aniline and the substituted anilines, using electron capture GLC, are 0.1 nmole/100 mL and 0.05 nmole/100 mL, respectively. The detection limit for the anilines is 1 nmole/100 mL distilled water, using GLC with flame ionization detection. The technique was applied to the determination of anilines added to urine samples obtained from the general population.

  18. Gas chromatograph study of bitumen from oil shale of Amman Formation (upper cretaceous), NW Jordan

    International Nuclear Information System (INIS)

    Darwish, H.; Mustafa, H.

    1997-01-01

    The extractable organic matter of seven outcrop samples of Amman Formation Oil Shale have been analysed by Gas Chromatography (GC). The bitumen is rich in heterocompounds contents (> 60 wt%). Gas chromatograms show a predominance of iosprenoids, specially phytane over n-alkanes, and low carbon preference index (CPI). This indicates that the organic matter is immature, and its origin is mainly of marine organisms. These rocks could be possible source rocks due to the high content of hydrocarbon. (authors). 22 refs., 4 figs. 3 tabs

  19. Environmental Technology Verification Report. Field Portable Gas Chromatograph/Mass Spectrometer. Viking Instruments Corporation SpectraTrak (Trademark) 672

    National Research Council Canada - National Science Library

    Enfield, Wayne

    1997-01-01

    .... This self-contained, field transportable system, whose design has been adapted from laboratory technology, uses a contained, chromatographic column and accompanying mass spectrometer to provide...

  20. A mobile automatic gas chromatograph system to measure CO2, CH4 and N2O fluxes from soil in the field

    International Nuclear Information System (INIS)

    Silvola, J.; Martikainen, P.; Nykaenen, H.

    1992-01-01

    A caravan has been converted into mobile laboratory for measuring fluxes of CO 2 , CH 4 and N 2 O from the soil in the field. The caravan was equipped with a gas chromatograph fitted with TC-, FI- and EC-detectors, and a PC controlled data logger. The gas collecting chambers can be used up to 50 m from the caravan. The closing and opening of the chambers, as well as the flows of sample gases from chambers to the gas chromatograph. is pneumatically regulated. Simultaneous recordings of temperature, light intensity and the depth of water table are made. The system has been used for two months in 1992, and some preliminary results are presented

  1. Large-volume injection in gas chromatographic trace analysis using temperature-programmable (PTV) injectors

    NARCIS (Netherlands)

    Mol, J.G.J.; Janssen, J.G.M.; Cramers, C.A.M.G.; Brinkman, U.A.T.

    1996-01-01

    The use of programmed-temperature vaporising (PTV) injectors for large-volume injection in capillary gas chromatography is briefly reviewed. The principles and optimisation of large-volume PTV injection are discussed. Guidelines are given for selection of the PTV conditions and injection mode for

  2. High-resolution gas chromatographic analysis of polycyclic aromatic hydrocarbons and aliphatic hydrocarbons

    International Nuclear Information System (INIS)

    Perez, M.; Gonzalez, D.

    1988-01-01

    A study of the analysis by gas chromatography of aromatic polycyclic hydrocarbons and aliphatic hydrocarbons is presented. The separation has been carried out by glass and fused silica capillary column in two different polar stationary phases OV-1 and SE-54. The limitation and the advantages of the procedure are discussed in terms of separation, sensitivity and precision. (Author) 20 refs

  3. A technique for rapid source apportionment applied to ambient organic aerosol measurements from a thermal desorption aerosol gas chromatograph (TAG

    Directory of Open Access Journals (Sweden)

    Y. Zhang

    2016-11-01

    Full Text Available We present a rapid method for apportioning the sources of atmospheric organic aerosol composition measured by gas chromatography–mass spectrometry methods. Here, we specifically apply this new analysis method to data acquired on a thermal desorption aerosol gas chromatograph (TAG system. Gas chromatograms are divided by retention time into evenly spaced bins, within which the mass spectra are summed. A previous chromatogram binning method was introduced for the purpose of chromatogram structure deconvolution (e.g., major compound classes (Zhang et al., 2014. Here we extend the method development for the specific purpose of determining aerosol samples' sources. Chromatogram bins are arranged into an input data matrix for positive matrix factorization (PMF, where the sample number is the row dimension and the mass-spectra-resolved eluting time intervals (bins are the column dimension. Then two-dimensional PMF can effectively do three-dimensional factorization on the three-dimensional TAG mass spectra data. The retention time shift of the chromatogram is corrected by applying the median values of the different peaks' shifts. Bin width affects chemical resolution but does not affect PMF retrieval of the sources' time variations for low-factor solutions. A bin width smaller than the maximum retention shift among all samples requires retention time shift correction. A six-factor PMF comparison among aerosol mass spectrometry (AMS, TAG binning, and conventional TAG compound integration methods shows that the TAG binning method performs similarly to the integration method. However, the new binning method incorporates the entirety of the data set and requires significantly less pre-processing of the data than conventional single compound identification and integration. In addition, while a fraction of the most oxygenated aerosol does not elute through an underivatized TAG analysis, the TAG binning method does have the ability to achieve molecular level

  4. Gas--liquid chromatographic determination of total inorganic iodine in milk

    International Nuclear Information System (INIS)

    Bakker, H.J.

    1977-01-01

    Total inorganic iodine in milk is determined by conversion to iodobutanone, which is quantitated by gas-liquid chromatography and electron capture detection. As little as 10 μg/L can be determined. The thyroid-active iodine content of milk can be determined rapidly with a relative standard deviation of 1.9%. Average recoveries for added iodide and iodine were 95.5 and 94.6%, respectively

  5. 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.

  6. A low-power pressure-and temperature-programmed separation system for a micro gas chromatograph.

    Energy Technology Data Exchange (ETDEWEB)

    Sacks, Richard D. (University of Michigan, Ann Arbor, MI); Robinson, Alex Lockwood (Advanced Sensor Technologies, Albuquerque, NM); Lambertus, Gordon R. (University of Michigan, Ann Arbor, MI); Potkay, Joseph A. (University of Michigan, Ann Arbor, MI); Wise, Kensall D. (University of Michigan, Ann Arbor, MI)

    2006-10-01

    This thesis presents the theory, design, fabrication and testing of the microvalves and columns necessary in a pressure- and temperature-programmed micro gas chromatograph ({micro}GC). Two microcolumn designs are investigated: a bonded Si-glass column having a rectangular cross section and a vapor-deposited silicon oxynitride (Sion) column having a roughly circular cross section. Both microcolumns contain integrated heaters and sensors for rapid, controlled heating. The 3.2 cm x 3.2 cm, 3 m-long silicon-glass column, coated with a non-polar polydimethylsiloxane (PDMS) stationary phase, separates 30 volatile organic compounds (VOCs) in less than 6 min. This is the most efficient micromachined column reported to date, producing greater than 4000 plates/m. The 2.7 mm x 1.4 mm Sion column eliminates the glass sealing plate and silicon substrate using deposited dielectrics and is the lowest power and fastest GC column reported to date; it requires only 11 mW to raise the column temperature by 100 C and has a response time of 11s and natural temperature ramp rate of 580 C/min. A 1 m-long PDMS-coated Sion microcolumn separates 10 VOCs in 52s. A system-based design approach was used for both columns.

  7. A novel headspace gas chromatographic method for in situ monitoring of monomer conversion during polymerization in an emulsion environment.

    Science.gov (United States)

    Chai, Xin-Sheng; Zhong, Jin-Feng; Hu, Hui-Chao

    2012-05-18

    This paper describes a novel multiple-headspace extraction/gas chromatographic (MHE-GC) technique for monitoring monomer conversion during a polymerization reaction in a water-based emulsion environment. The polymerization reaction of methyl methacrylate (MMA) in an aqueous emulsion is used as an example. The reaction was performed in a closed headspace sample vial (as a mini-reactor), with pentane as a tracer. In situ monitoring of the vapor concentration of the tracer, employing a multiple headspace extraction (sampling) scheme, coupled to a GC, makes it possible to quantitatively follow the conversion of MMA during the early stages of polymerization. Data on the integrated amount of the tracer vapor released from the monomer droplet phase during the polymerization is described by a mathematic equation from which the monomer conversion can be calculated. The present method is simple, automated and economical, and provides an efficient tool in the investigation of the reaction kinetics and effects of the reaction conditions on the early stage of polymerization. Copyright © 2012 Elsevier B.V. All rights reserved.

  8. Interlaboratory tests to identify irradiation treatment of various foods via gas chromatographic detection of hydrocarbons, ESR spectroscopy and TL analysis

    Energy Technology Data Exchange (ETDEWEB)

    Schreiber, G.A.; Helle, N.; Schulzki, G.; Linke, B.; Spiegelberg, A.; Mager, M.; Boegl, K.W. [BgVV - Federal Inst. for Health Protection of Consumers and Veterinary Medicine, Berlin (Germany)

    1996-12-31

    The gas chromatographic (GC) analysis of radiation-induced volatile hydrocarbons (HC) and 2-alkylcyclobutanones, the ESR spectroscopic detection of radiation-specific radicals and the thermoluminescence (TL) analysis of silicate mineral are the most important methods for identification of irradiated foods. After successful performance in interlaboratory studies on meat products, fish, spices, herbs and shells of nuts, all or some of these methods have been approved by national authorities in Germany and the United Kingdom. Recently, draft European Standards have been elaborated for approval by member states of the European Committee for Standardization (CEN). Several research laboratories have shown that these methods can be applied to various foods not yet tested in collaborative studies. However, for an effective application in food control it is necessary to prove their suitability in interlaboratory studies. Therefore, in 1993/94, various interlaboratory tests were organised by the BgVV. In an ESR spectroscopic test, shrimps and paprika powder were examined. Shrimps were also the subject of examination in a TL test. Finally, GC detection of radiation-induced hydrocarbons in the fat fraction of foods was used in another test to identify irradiated Camembert, avocado, papaya and mango. In the following paper, results of the interlaboratory tests are summarised. Detailed reports are published by this institute. (author).

  9. Interlaboratory tests to identify irradiation treatment of various foods via gas chromatographic detection of hydrocarbons, ESR spectroscopy and TL analysis

    International Nuclear Information System (INIS)

    Schreiber, G.A.; Helle, N.; Schulzki, G.; Linke, B.; Spiegelberg, A.; Mager, M.; Boegl, K.W.

    1996-01-01

    The gas chromatographic (GC) analysis of radiation-induced volatile hydrocarbons (HC) and 2-alkylcyclobutanones, the ESR spectroscopic detection of radiation-specific radicals and the thermoluminescence (TL) analysis of silicate mineral are the most important methods for identification of irradiated foods. After successful performance in interlaboratory studies on meat products, fish, spices, herbs and shells of nuts, all or some of these methods have been approved by national authorities in Germany and the United Kingdom. Recently, draft European Standards have been elaborated for approval by member states of the European Committee for Standardization (CEN). Several research laboratories have shown that these methods can be applied to various foods not yet tested in collaborative studies. However, for an effective application in food control it is necessary to prove their suitability in interlaboratory studies. Therefore, in 1993/94, various interlaboratory tests were organised by the BgVV. In an ESR spectroscopic test, shrimps and paprika powder were examined. Shrimps were also the subject of examination in a TL test. Finally, GC detection of radiation-induced hydrocarbons in the fat fraction of foods was used in another test to identify irradiated Camembert, avocado, papaya and mango. In the following paper, results of the interlaboratory tests are summarised. Detailed reports are published by this institute. (author)

  10. Gas chromatographic analysis of reactive carbonyl compounds formed from lipids upon UV-irradiation

    International Nuclear Information System (INIS)

    Dennis, K.J.; Shibamoto, T.

    1990-01-01

    Peroxidation of lipids produces carbonyl compounds; some of these, e.g., malonaldehyde and 4-hydroxynonenal, are genotoxic because of their reactivity with biological nucleophiles. Analysis of the reactive carbonyl compounds is often difficult. The methylhydrazine method developed for malonaldehyde analysis was applied to simultaneously measure the products formed from linoleic acid, linolenic acid, arachidonic acid, and squalene upon ultraviolet-irradiation (UV-irradiation). The photoreaction products, saturated monocarbonyl, alpha,beta-unsaturated carbonyls, and beta-dicarbonyls, were derivatized with methylhydrazine to give hydrazones, pyrazolines, and pyrazoles, respectively. The derivatives were analyzed by gas chromatography and gas chromatography-mass spectrometry. Lipid peroxidation products identified included formaldehyde, acetaldehyde, acrolein, malonaldehyde, n-hexanal, and 4-hydroxy-2-nonenal. Malonaldehyde levels formed upon 4 hr of irradiation were 0.06 micrograms/mg from squalene, 2.4 micrograms/mg from linolenic acid, and 5.7 micrograms/mg from arachidonic acid. Significant levels of acrolein (2.5 micrograms/mg) and 4-hydroxy-2-nonenal (0.17 micrograms/mg) were also produced from arachidonic acid upon 4 hr irradiation

  11. 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)

  12. Potential for Measurement of Trace Volatile Organic Compounds in Closed Environments Using Gas Chromatograph/Differential Mobility Spectrometer

    Science.gov (United States)

    Limero, Thomas; Cheng, Patti

    2007-01-01

    For nearly 3.5 years, the Volatile Organic Analyzer (VOA) has routinely analyzed the International Space Station (ISS) atmosphere for a target list of approximately 20 volatile organic compounds (VOCs). Additionally, an early prototype of the VOA collected data aboard submarines in two separate trials. Comparison of the data collected on ISS and submarines showed a surprising similarity in the atmospheres of the two environments. Furthermore, in both cases it was demonstrated that the VOA data can detect hardware issues unrelated to crew health. Finally, it was also clear in both operations that the VOA s size and resource consumption were major disadvantages that would restrict its use in the future. The VOA showed the value of measuring VOCs in closed environments, but it had to be shrunk if it was to be considered for future operations in these environments that are characterized by cramped spaces and limited resources. The Sionex Microanalyzer is a fraction of the VOA s size and this instrument seems capable of maintaining or improving upon the analytical performance of the VOA. The two design improvements that led to a smaller, less complex instrument are the Microanalyzer s use of recirculated air as the gas chromatograph s carrier gas and a micromachined detector. Although the VOA s ion mobility spectrometer and the Microanalyzer s differential mobility spectrometer (DMS) are related detector technologies, the DMS was more amenable to micromachining. This paper will present data from the initial assessment of the Microanalyzer. The instrument was challenged with mixtures that simulated the VOCs typically detected in closed-environment atmospheres.

  13. Technical Note: Precise quantitative measurements of total dissolved inorganic carbon from small amounts of seawater using a gas chromatographic system

    Directory of Open Access Journals (Sweden)

    T. Hansen

    2013-10-01

    Full Text Available Total dissolved inorganic carbon (CT is one of the most frequently measured parameters used to calculate the partial pressure of carbon dioxide in seawater. Its determination has become increasingly important because of the rising interest in the biological effects of ocean acidification. Coulometric and infrared detection methods are currently favored in order to precisely quantify CT. These methods however are not sufficiently validated for CT measurements of biological experiments manipulating seawater carbonate chemistry with an extended CT measurement range (~1250–2400 μmol kg–1 compared to natural open ocean seawater (~1950–2200 μmol kg−1. The requirement of total sample amounts between 0.1–1 L seawater in the coulometric- and infrared detection methods potentially exclude their use for experiments working with much smaller volumes. Additionally, precise CT analytics become difficult with high amounts of biomass (e.g., phytoplankton cultures or even impossible in the presence of planktonic calcifiers without sample pre-filtration. Filtration however, can alter CT concentration through gas exchange induced by high pressure. Addressing these problems, we present precise quantification of CT using a small, basic and inexpensive gas chromatograph as a CT analyzer. Our technique is able to provide a repeatability of ±3.1 μmol kg−1, given by the pooled standard deviation over a CT range typically applied in acidification experiments. 200 μL of sample is required to perform the actual CT measurement. The total sample amount needed is 12 mL. Moreover, we show that sample filtration is applicable with only minor alteration of the CT. The method is simple, reliable and with low cumulative material costs. Hence, it is potentially attractive for all researchers experimentally manipulating the seawater carbonate system.

  14. Evaluation of a portable gas chromatograph with photoionization detector under variations of VOC concentration, temperature, and relative humidity.

    Science.gov (United States)

    Soo, Jhy-Charm; Lee, Eun Gyung; LeBouf, Ryan F; Kashon, Michael L; Chisholm, William; Harper, Martin

    2018-04-01

    The objective of this present study was to evaluate the performance of a portable gas chromatograph-photoionization detector (GC-PID), under various test conditions to determine if it could be used in occupational settings. A mixture of 7 volatile organic compounds (VOCs)-acetone, ethylbenzene, methyl isobutyl ketone, toluene, m-xylene, p-xylene, and o-xylene-was selected because its components are commonly present in paint manufacturing industries. A full-factorial combination of 4 concentration levels (exposure scenarios) of VOC mixtures, 3 different temperatures (25°C, 30°C, and 35°C), and 3 relative humidities (RHs; 25%, 50%, and 75%) was conducted in a full-size controlled environmental chamber. Three repetitions were conducted for each test condition allowing for estimation of accuracy. Time-weighted average exposure data were collected using solid sorbent tubes (Anasorb 747, SKC Inc.) as the reference sampling medium. Calibration curves of Frog-4000 using the dry gases showed R 2 > 0.99 for all analytes except for toluene (R 2 = 0.97). Frog-4000 estimates within a test condition showed good consistency for the performance of repeated measurement. However, there was ∼41-64% reduction in the analysis of polar acetone with 75% RH relative to collection at 25% RH. Although Frog-4000 results correlated well with solid sorbent tubes (r = 0.808-0.993, except for toluene) most of the combinations regardless of analyte did not meet the <25% accuracy criterion recommended by NIOSH. The effect of chromatographic co-elution can be seen with m, p-xylene when the results are compared to the sorbent tube sampling technique with GC-flame ionization detector. The results indicated an effect of humidity on the quantification of the polar compounds that might be attributed to the pre-concentrator placed in the selected GC-PID. Further investigation may resolve the humidity effect on sorbent trap with micro GC pre-concentrator when water vapor is present. Although this

  15. Pyrolysis gas chromatographic study of homo polymers and copolymers of chlorotrifluoroethylene and styrene

    International Nuclear Information System (INIS)

    Rizvi, M.; Munir, A.

    1993-01-01

    Polymer degradation reactions have always been important for the development of thermally stable polymers. Among different available techniques, pyrolysis gas chromatography (PGC) has been used frequently to establish thermal stability and the plausible mechanism of degradation reactions. In the present work, homo polymers of chlorotrifluoroethylene (CTFE) and styrene and their copolymers were studied by PGC/IR for separation and identification of degraded products and to understand the degradation mechanism. Besides monomers, C/sub 2/H/sub 4/, C/sub 2/H/sub 2/, SiF/sub 4/, C/sub 6/H/sub 6/ C/sub 3/F/sub 5/Cl, C/sub 7/H sub 8/, C/sub 8/H/sub 10/ are the observed pyrolysis products. Mechanism for different degradation reactions have also been studied. (author)

  16. Headspace Solid Phase Micro Extraction Gas Chromatographic Determination of Fenthion in Human Serum

    Directory of Open Access Journals (Sweden)

    Kyriaki Machera

    2008-05-01

    Full Text Available A simple and effective analytical procedure was developed for the determination of fenthion residues in human serum samples. The sample treatment was performed using the headspace solid-phase micro extraction with polyacrylate fiber, which has the advantage to require low amount of serum (1 mL without tedious pre-treatment. The quantification of fenthion was carried out by gas chromatography-mass spectrometry and the recoveries ranged from 79 to 104% at two spiking levels for 6 replicates. Detection and quantification limits were calculated as 1.51 and 4.54 ng/mL of serum respectively. Two fenthion metabolites − fenoxon and fenthion–sulfoxide − were also identified.

  17. Liquid chromatographic analysis of a formulated ester from a gas-turbine engine test

    Science.gov (United States)

    Jones, W. R., Jr.; Morales, W.

    1983-01-01

    Size exclusion chromatography (SEC) utilizing mu-Bondagel and mu-Styragel columns with a tetrahydrofuran mobile phase was used to determine the chemical degradation of lubricant samples from a gas-turbine engine test. A MIL-L-27502 candidate, ester-based lubricant was run in a J57-29 engine at a bulk oil temperature of 216 C. In general, the analyses indicated a progressive loss of primary ester, additive depletion, and formation of higher molecular weight material. An oil sample taken at the conclusion of the test showed a reversal of this trend because of large additions of new oil. The high-molecular-weight product from the degraded ester absorbed strongly in the ultraviolet region at 254 nanometers. This would indicate the presence of chromophoric groups. An analysis of a similar ester lubricant from a separate high-temperature bearing test yielded qualitatively similar results.

  18. Gas chromatographic study of degradation phenomena concerning building and cultural heritage materials

    International Nuclear Information System (INIS)

    Metaxa, E.; Agelakopoulou, T.; Bassiotis, I.; Karagianni, Ch.; Roubani-Kalantzopoulou, F.

    2009-01-01

    Air pollution influences all aspects of social and economical life nowadays. In order to investigate the impact of air pollution on materials of works of art, the method of Reversed Flow-Inverse Gas Chromatography has been selected. The presence of various atmospheric pollutants is studied on marbles, oxides-building materials and samples of authentic statues from the Greek Archaeological Museums of Kavala and of Philippi. The method leads to the determination of several physicochemical quantities and the characterization of the heterogeneous surfaces of these solids. Moreover, the influence of a second pollutant (synergistic effect) is examined. The structure, the properties and the behavior of the materials are examined by X-Ray Diffraction, Scanning Electron Microscopy and Raman Spectroscopy. Therefore, the precise measurement of the above mentioned quantities form the scientific basis for elucidation of the mechanism of the whole phenomenon of the degradation, thus providing a scientific platform to conservation procedures.

  19. Novel preconcentration technique for on-line coupling to high-speed narrow-bore capillary gas chromatography: sample enrichment by equilibrium (ab)sorption, I: Principles and theoretical aspects

    NARCIS (Netherlands)

    Pham Tuan, H.; Janssen, J.G.M.; Cramers, C.A.M.G.

    1997-01-01

    In recent years, there has been substantial progress in the field of high-speed narrow-bore capillary gas chromatography (GC) in general, and in the development of (trans)portable gas chromatographs for fast and accurate analysis in field applications in particular. Due to the limited

  20. 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),

  1. Determination of Profenofos Pesticidal Residue in Lettuce (Lactuca sativa L. by Gas Chromatographic Method

    Directory of Open Access Journals (Sweden)

    Yohannes Alen

    2015-05-01

    Full Text Available The determination of profenofos pesticidal residue in the lettuce (Lactuca sativa L. by using gas chromatography using flame photometric detector (FPD had been investigated. The lettuce was collected from Padang Luar area, Agam distric, West Sumatera. Sample for determination of profenofos residue divided into three groups: unwashed (A, washed with water (B, and washed with detergent (C. Maceration with sonication was used for the extraction using ethylacetateas a solvent. The results showed that profenofos pesticide residue in sample A, B and C were 0.204, 0.080 and 0.061 ppm, respectively. These profenofos pesticidal residue are over than the Maximum Residue Limits (MRL that established by The Japan Food Chemical Research Foundation (0.05 ppm even though World Health Organization (WHO has not established Maximum Residue Limits (MRL profenofos on lettuce. Based on the statistical analysis one-way method (Anova using SPSS 20.0 showed that there was a significant concentrations difference between lettuce A from lettuce B and lettuce C with p < 0.05.

  2. Gas chromatographic determination of purines and pyrimidines from DNA using ethyl chloroformate as derivatizing reagent

    International Nuclear Information System (INIS)

    Brohi, R.O.Z.; Khuhawar, M.Y.; Laghari, A.J.; Channa, A.

    2016-01-01

    An analytical method has been proposed for the separation and determination of guanine, adenine, cytosine, thymine and uracil by gas chromatography (GC) following precolumn derivatization using ethyl chloroformate. The GC separation was achieved from HP-5 (30 m x 0.32 rnrn id) column with layer thickness 0.25 microm. The linear calibrations were observed within 0.5-50.0 micro mole/L for each of the compound and limits of detection were within 0.1-0.17 micro mol/L. The derivatization, separation and quantitation was repeatable with intra (n=5) and inter (n=5) variation in terms of peak height/peak area and retention time with relative standard deviation (RSD) within 4.70-6.43%. The method was applied for the analysis of isolated DNA from human blood and plant leaves after acid hydrolysis. The concentration of thymine, adenine, cytosine and guanine in blood samples were observed within 0.602-2.135 micro mol/L of each compounds with RSD 2.60- 6.00%. The recovery of the nucleobases by standard addition was calculated within 98-108% with RSD 2.5-7.8%. (author)

  3. Gas Chromatographic Determination of Purines and Pyrimidines from DNA Using Ethyl Chloroformate as Derivatizing Reagent

    Directory of Open Access Journals (Sweden)

    Rafi O. Zaman Brohi

    2016-06-01

    Full Text Available An analytical method has been proposed for the separation and determination of guanine, adenine, cytosine, thymine and uracil by gas chromatography (GC following precolumn derivatization using ethyl chloroformate. The GC separation was achieved from HP-5 (30 m × 0.32 mm id column with layer thickness 0.25 µm. The linear calibrations were observed within 0.5-50.0 µmol/L for each of the compound and limits of detection were within 0.1-0.17 µmol/L. The derivatization, separation and quantitation was repeatable with intra (n=5 and inter (n=5 variation in terms of peak height/peak area and retention time with relative standard deviation (RSD within 4.70-6.43%. The method was applied for the analysis of isolated DNA from human blood and plant leaves after acid hydrolysis. The concentration of thymine, adenine, cytosine and guanine in blood samples were observed within 0.602-2.135 µmol/L of each compounds with RSD 2.60-6.00%. The recovery of the nucleobases by standard addition was calculated within 98-108% with RSD 2.5-7.8%.

  4. π-Extended triptycene-based material for capillary gas chromatographic separations.

    Science.gov (United States)

    Yang, Yinhui; Wang, Qinsi; Qi, Meiling; Huang, Xuebin

    2017-10-02

    Triptycene-based materials feature favorable physicochemical properties and unique molecular recognition ability that offer good potential as stationary phases for capillary gas chromatography (GC). Herein, we report the investigation of utilizing a π-extended triptycene material (denoted as TQPP) for GC separations. As a result, the TQPP capillary column exhibited high column efficiency of 4030 plates m -1 and high-resolution performance for a wide range of analytes, especially structural and positional isomers. Interestingly, the TQPP stationary phase showed unique shape selectivity for alkanes isomers and preferential retention for analytes with halogen atoms and H-bonding nature mainly through their halogen-bonding and H-bonding interactions. In addition, the TQPP column had good repeatability and reproducibility with the RSD values of 0.02-0.34% for run-to-run, 0.09-0.80% for day-to-day and 1.4-5.2% for column-to-column, respectively, and favorable thermal stability up to 280 °C. This work demonstrates the promising future of triptycene-based materials as a new class of stationary phases for GC separations. Copyright © 2017 Elsevier B.V. All rights reserved.

  5. Gas chromatographic/mass spectrometric characterization of dromostanolone metabolites in human urine

    International Nuclear Information System (INIS)

    Kim, Tae Wook; Choi, Man Ho; Jung, Byung Hwa; Chung, Bong Chul

    1998-01-01

    The metabolism of dromostanolone (2α-methyl-5α-androstan-17β-ol-3-one) was studied in three adult volunteers after oral dose of 20 mg. Solvent extracts of urine obtained after enzyme hydrolysis were derivatized with MSTFA/TMCS and MSTFA/TMIS. The structures of intact drug and its metabolites were determined by gas chromatography/mass spectrometry (GC/MS) in electron impact (EI) mode. The major metabolite (2α-methyl-5α-androstan-3α-ol-17-one), its 3β-epimer, parent compound, and several hydroxylated metabolites including intact drug were detected by comparing total ion chromatograms of control urine with that of the administered sample. Two epimers of 2α-methyl-5α-androstan-3, 17β-diol were detected using selected ion monitoring. The maximum excretion of dromostanolone and 2α-methyl-5α-androstan-3α-ol-17-one was reached in 6.2-15 hr. The half-life of intact dromostanolone was 5.3 hr. About 3.0% of the administered amount was found to be excreted within 95 hr as unchanged form

  6. Characterization of Atypical Off-Flavor Compounds in Natural Cork Stoppers by Multidimensional Gas Chromatographic Techniques.

    Science.gov (United States)

    Slabizki, Petra; Fischer, Claus; Legrum, Charlotte; Schmarr, Hans-Georg

    2015-09-09

    Natural cork stoppers with sensory deviations other than the typical cork taint were subgrouped according to their sensory descriptions and compared with unaffected control cork stoppers. The assessment of purge and trap extracts obtained from corresponding cork soaks was performed by heart-cut multidimensional gas chromatography-olfactometry (MDGC-O). The identification of compounds responsible for atypical cork taint detected in MDGC-O was further supported with additional multidimensional GC analysis in combination with mass spectrometric detection. Geosmin and 2-methylisoborneol were mainly found in cork stoppers described as moldy and cellarlike; 3-isopropyl-2-methoxypyrazine and 3-isobutyl-2-methoxypyrazine were found in cork stoppers described with green attributes. Across all cork subgroups, the impact compound for typical cork taint, 2,4,6-trichloroanisole (TCA), was present and is therefore a good marker for cork taint in general. Another potent aroma compound, 3,5-dimethyl-2-methoxypyrazine (MDMP), was also detected in each subgroup, obviously playing an important role with regard to the atypical cork taint. Sensory deviations possibly affecting the wine could be generated by MDMP and its presence should thus be monitored in routine quality control.

  7. Gas chromatographic quantitative analysis of the gaseous emissions and carbon balance in the alcoholic fermentation

    Directory of Open Access Journals (Sweden)

    C. Chon

    1997-06-01

    ln order to try to answer to this question, methods able to analyse simultaneously and quantitatively the liquid phase, the gaseous emissions and the biomass are needed. Recently, we have shown that under suitable defined conditions 13C NMR spectroscopy allows the quantitative measurement of at least eight components present at a concentration up to 5 x 10-3M (glycerol, glucose, butandiols, tartric, malic, lactic, citric and succinic acids in a short time (one hour with a precision of about 3 p. cent. The measurements of the ethanol concentrations and of the amount of carbon transferred in the biomass are easily achieved using respectively ebullioscopic and standard combustion techniques. We are now able to extend these results and to show that, by using gas chromatography in a continuous dynamic mode and under a sweep of air at the head space of the fermentor, it is possible to measure quantitatively the mixture of volatile substances (composed mainly of air, carbon dioxide, ethanol and water emanating from an alcoholic fermentation. The results obtained, when correlated with quantitative 13C NMR spectroscopy on the medium components permits the total balance sheet of the carbon transfers occuring during the fermentation process betwcen the liquid and the gaseous phases to be established. Our results indicate that the losses of ethanol during the fermentation process conducted under an air flow at the head space of the fermentor, may reach about 10 p. cent of the theoretical maximal amount of ethanol produced. The experiments presented here could explain the ethanol losses observed during some vinification processes conducted in open tanks.

  8. Antioxidant and Antiangiogenic Properties, and Gas Chromatographic-Time of Flight Analysis of Sonchus arvensis Leaves Extracts

    International Nuclear Information System (INIS)

    Itam, A.; Shah, A. M.; Majid, A.; Ismail, Z.

    2015-01-01

    Sonchus arvensis L. (Asteraceae) is one of the medicinal herbs used in traditional medicines, in which the leaf extract was used as a diuretic, lithotriptic and antiurolithiasis agent. The leaves of S. arvensis reported contain several compounds, including a variety of flavonoids, terpenoids and sterol, even this plant also contain silica and potassium. Flavonoids are secondary metabolite compound which have ability as antioxidant. In this study, the aims are to determine of antioxidants and antiangiogenic properties, and phytoconstituents quantitative of aqueous and methanol extracts of S. arvensis leaves. The antioxidant properties were studied using 1,1-Diphenyl-2-picrylhydrazyl (DPPH) free radical, xanthine oxidase and beta-carotene-linoleate models system. Furthermore, the antiangiogenic property was evaluated using ex vivo rat aorta ring assay. Quantitative determination of extracts phytoconstituents were carried out by using Gas Chromatographic-Time of Flight (GC-TOF) mass spectrophotometric methods. The results showed that the aqueous and methanol extracts have ability as antioxidant which is antioxidant activities of aqueous extracts on DPPH radical and inhibition of xanthine oxidase activity are higher than that of methanol extracts. Meanwhile antioxidant activity using beta-carotene-linoleate model system of S. arvensis aqueous extract is lower than that of methanol extracts. Nevertheless, the differences of these antioxidant activities are not significant. Antiangiogenic property of aqueous extract is also higher than that of methanol extract which is measured at 100 meu g mL/sup -1/ of extracts. This indicates that there is correlation between antioxidant activity and antiangigenic property, exhibiting that this plant possesses the potential to prevent or cure the diseases that related to angiogenesis such as cancer. (author)

  9. Gas chromatographic-mass spectrometric analysis of di(2-ethylhexyl) phthalate and its metabolites in hepatic microsomal incubations

    Energy Technology Data Exchange (ETDEWEB)

    Pietrogrande, M.C.; Rossi, D.; Paganetto, G

    2003-03-17

    A method is reported for the determination of di(2-ethylhexyl) phthalate (DEHP) and its metabolites in in vitro metabolism studies. Gas chromatography-mass spectrometry (GC-MS) analysis allows separation of 18 by-products of DEHP metabolism. On the basis of retention time and specific mass spectra m/z values, three classes of compounds can be identified: (i) alcohols as hydrolysis product; (ii) acids produced by alcohol oxidation; (iii) compounds retaining phthalic moiety. The chromatogram can also be acquired in SIM mode at m/z 149 resulting in 13 well-separated chromatographic peaks: from retention time and mass spectra it can be inferred that the main peaks correspond to mono(2-ethylhexyl) phthalate (MEHP) and ({omega}-1)-hydroxyl-MEHP. The kinetics of DEHP metabolism was studied using an S9 Aroclor-induced liver fraction as in vitro model and following incubation assay after 20, 40, 60 and 90 min. The composition of incubation mixtures can be quantitatively evaluated from selected ion monitoring chromatograms at m/z 149: the by-product concentration increases during the incubation time, as a consequence of DEHP degradation. During the incubation test a significant conversion of DEHP into MEHP is observed: a conversion yield of 10, 13, 16 and 20% of the original DEHP is obtained after 20, 40, 60 and 90 min, respectively. The metabolic conversion of DEHP to MEHP explains the endocrine-disrupting activity of the original DEHP; moreover, it has been demonstrated that MEHP and its ({omega}-1)-oxidation metabolite induce peroxisome proliferation. This result strengthens the suggestion that the study of DEHP metabolic pathway is fundamental to better understanding its toxicological behavior.

  10. On-line liquid chromatography-gas chromatography: A novel approach for the analysis of phytosterol oxidation products in enriched foods.

    Science.gov (United States)

    Scholz, Birgit; Wocheslander, Stefan; Lander, Vera; Engel, Karl-Heinz

    2015-05-29

    A novel methodology for the automated qualitative and quantitative determination of phytosterol oxidation products in enriched foods via on-line liquid chromatography-gas chromatography (LC-GC) was established. The approach is based on the LC pre-separation of acetylated phytosterols and their corresponding oxides using silica as stationary phase and a mixture of n-hexane/methyl tert-butyl ether/isopropanol as eluent. Two LC-fractions containing (i) 5,6-epoxy- and 7-hydroxyphytosterols, and (ii) 7-ketophytosterols are transferred on-line to the GC for the analysis of their individual compositions on a medium polar trifluoropropylmethyl polysiloxane capillary column. Thus, conventionally employed laborious off-line purification and enrichment steps can be avoided. Validation data, including recovery, repeatability, and reproducibility of the method, were elaborated using an enriched margarine as example. The margarine was subjected to a heating procedure in order to exemplarily monitor the formation of phytosterol oxidation products. Quantification was performed using on-line LC-GC-FID, identification of the analytes was based on on-line LC-GC-MS. The developed approach offers a new possibility for the reliable and fast analysis of phytosterol oxidation products in enriched foods. Copyright © 2015 Elsevier B.V. All rights reserved.

  11. Dopant-assisted negative photoionization Ion mobility spectrometry coupled with on-line cooling inlet for real-time monitoring H2S concentration in sewer gas.

    Science.gov (United States)

    Peng, Liying; Jiang, Dandan; Wang, Zhenxin; Hua, Lei; Li, Haiyang

    2016-06-01

    Malodorous hydrogen sulfide (H2S) gas often exists in the sewer system and associates with the problems of releasing the dangerous odor to the atmosphere and causing sewer pipe to be corroded. A simple method is in demand for real-time measuring H2S level in the sewer gas. In this paper, an innovated method based on dopant-assisted negative photoionization ion mobility spectrometry (DANP-IMS) with on-line semiconductor cooling inlet was put forward and successfully applied for the real-time measurement of H2S in sewer gas. The influence of moisture was effectively reduced via an on-line cooling method and a non-equilibrium dilution with drift gas. The limits of quantitation for the H2S in ≥60% relative humidity air could be obtained at ≤79.0ng L(-1) with linear ranges of 129-2064ng L(-1). The H2S concentration in a sewer manhole was successfully determined while its product ions were identified by an ion-mobility time-of-fight mass spectrometry. Finally, the correlation between sewer H2S concentration and the daily routines and habits of residents was investigated through hourly or real-time monitoring the variation of sewer H2S in manholes, indicating the power of this DANP-IMS method in assessing the H2S concentration in sewer system. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. Total OH reactivity measurements using a new fast Gas Chromatographic Photo-Ionization Detector (GC-PID

    Directory of Open Access Journals (Sweden)

    V. Sinha

    2012-12-01

    Full Text Available The primary and most important oxidant in the atmosphere is the hydroxyl radical (OH. Currently OH sinks, particularly gas phase reactions, are poorly constrained. One way to characterize the overall sink of OH is to measure directly the ambient loss rate of OH, the total OH reactivity. To date, direct measurements of total OH reactivity have been either performed using a Laser-Induced Fluorescence (LIF system ("pump-and-probe" or "flow reactor" or the Comparative Reactivity Method (CRM with a Proton-Transfer-Reaction Mass Spectrometer (PTR-MS. Both techniques require large, complex and expensive detection systems. This study presents a feasibility assessment for CRM total OH reactivity measurements using a new detector, a Gas Chromatographic Photoionization Detector (GC-PID. Such a system is smaller, more portable, less power consuming and less expensive than other total OH reactivity measurement techniques.

    Total OH reactivity is measured by the CRM using a competitive reaction between a reagent (here pyrrole with OH alone and in the presence of atmospheric reactive molecules. The new CRM method for total OH reactivity has been tested with parallel measurements of the GC-PID and the previously validated PTR-MS as detector for the reagent pyrrole during laboratory experiments, plant chamber and boreal field studies. Excellent agreement of both detectors was found when the GC-PID was operated under optimum conditions. Time resolution (60–70 s, sensitivity (LOD 3–6 s−1 and overall uncertainty (25% in optimum conditions for total OH reactivity were similar to PTR-MS based total OH reactivity measurements. One drawback of the GC-PID system was the steady loss of sensitivity and accuracy during intensive measurements lasting several weeks, and a possible toluene interference. Generally, the GC-PID system has been shown to produce closely comparable results to the PTR-MS and thus in suitable environments (e.g. forests it

  13. Immunological screening of drugs of abuse and gas chromatographic-mass spectrometric confirmation of opiates and cocaine in hair.

    Science.gov (United States)

    Segura, J; Stramesi, C; Redón, A; Ventura, M; Sanchez, C J; González, G; San, L; Montagna, M

    1999-03-05

    The work presents an analytical strategy to detect drugs of abuse in hair. It involves two sequential steps: a screening by a simple enzyme-linked immunosorbent assay (ELISA) methodology to detect opiates, cocaine and its metabolites, and benzodiacepines, followed by confirmation of opiates and cocaine metabolites in positive samples by gas chromatography coupled to mass spectrometry (GC-MS). In the same GC-MS run other drugs for substitution therapy (e.g. methadone and its main metabolite) can also be detected. After a double washing of hair samples with dichloromethane, hair specimens were cut into small pieces and 10 mg samples were incubated in 2 ml of methanol-trifluoroacetic acid (9:1) mixture, overnight at 37 degrees C. Aliquots of the extract were then evaporated, reconstituted in buffer and analysed according to the ELISA procedure. Confirmation involved solid-phase extraction of another fraction of the extract kept at -20 degrees C, derivatization with heptafluorobutyric anhydride and hexafluoroisopropanol and detection of cocaine, benzoylecgonine, ecgonine methylester, cocaethylene, morphine, codeine, 6-monoacetylmorphine, methadone and 2-ethylidene-1.5-dimethyl-3,3-diphenylpirrolidine (methadone metabolite) by selective ion monitoring after gas chromatographic separation. During the development of the method it was verified that no more than 10% of cocaine, opiates and benzodiacepines were lost when dichloromethane was used to wash real samples. The results also confirmed the increase of extractability power of TFA when it was added to methanol: the recovery for the analytes (cocaine and its metabolites and opiates) added to methanol-TFA alone was of the order of 90% except for benzoylecgonine (75%), and the recovery for the analytes added to methanol-TFA extract of drug-free hair was about 90% for all analytes except for benzoylecgonine and 6-MAM (around 70%). Regarding the stability of labile compounds, only small amounts of ecgonine methylester (2

  14. On-line determination of iodine in nuclear fuel reprocessing off-gas streams by a combination of laser-induced fluorimetry and laser photoacoustic spectroscopy

    International Nuclear Information System (INIS)

    Kuno, Yusuke; Sato, Souichi; Masui, Jinichi

    1992-01-01

    The on-line determination of molecular iodine and organic iodides in nuclear fuel reprocessing off-gas streams containing high concentrations of NO x gas was studied. Ultraviolet radiation is used to convert organic iodides into molecular iodine. The approximate concentration of iodine before and after the photochemical conversion in the presence of NO x gas was first determined by laser-induced fluorimetry. NO 2 was determined by photoacoustic spectroscopy, correcting the acoustic signal due to iodine by using the approximate iodine concentration. NO was determined from the concentrations of NO 2 before and after the photoirradiation based on the photochemical fraction changes of NO and NO 2 . The quenching of the fluorimetry due to NO and NO 2 was finally corrected with the NO and NO 2 concentrations obtained. The detection limit of the proposed method is 10 nl 1 -1 . 7 figs., 2 tabs., 11 refs

  15. 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

  16. Detection and on-line prediction of leak magnitude in a gas pipeline using an acoustic method and neural network data processing

    Directory of Open Access Journals (Sweden)

    R. B. Santos

    2014-03-01

    Full Text Available Considering the importance of monitoring pipeline systems, this work presents the development of a technique to detect gas leakage in pipelines, based on an acoustic method, and on-line prediction of leak magnitude using artificial neural networks. On-line audible noises generated by leakage were obtained with a microphone installed in a 60 m long pipeline. The sound noises were decomposed into sounds of different frequencies: 1 kHz, 5 kHz and 9 kHz. The dynamics of these noises in time were used as input to the neural model in order to determine the occurrence and the leak magnitude. The results indicated the great potential of the technique and of the developed neural network models. For all on-line tests, the models showed 100% accuracy in leak detection, except for a small orifice (1 mm under 4 kgf/cm² of nominal pressure. Similarly, the neural network models could adequately predict the magnitude of the leakages.

  17. A multiresidue method by high performance liquid chromatography-based fractionation and gas chromatographic determination of trace levels of pesticides in air and water.

    Science.gov (United States)

    Seiber, J N; Glotfelty, D E; Lucas, A D; McChesney, M M; Sagebiel, J C; Wehner, T A

    1990-01-01

    A multiresidue analytical method is described for pesticides, transformation products, and related toxicants based upon high performance liquid chromatographic (HPLC) fractionation of extracted residue on a Partisil silica gel normal phase column followed by selective-detector gas chromatographic (GC) determination of components in each fraction. The HPLC mobile phase gradient (hexane to methyl t-butyl ether) gave good chromatographic efficiency, resolution, reproducibility and recovery for 61 test compounds, and allowed for collection in four fractions spanning polarities from low polarity organochlorine compounds (fraction 1) to polar N-methylcarbamates and organophosphorus oxons (fraction 4). The multiresidue method was developed for use with air samples collected on XAD-4 and related trapping agents, and water samples extracted with methylene chloride. Detection limits estimated from spiking experiments were generally 0.3-1 ng/m3 for high-volume air samples, and 0.01-0.1 microgram/L for one-liter water samples. Applications were made to determination of pesticides in fogwater and air samples.

  18. Electrochemical reduction of phthalide at carbon cathodes in dimethylformamide: Effects of supporting electrolyte and gas chromatographic injector-port chemistry on the product distribution

    International Nuclear Information System (INIS)

    Pasciak, Erick M.; Hochstetler, Spencer E.; Mubarak, Mohammad S.; Evans, Dennis H.; Peters, Dennis G.

    2013-01-01

    Highlights: • Reduction of phthalide gives a radical-anion that undergoes ring-opening in 3.5 s. • Phthalide reduction gives 2-methylbenzoate esters with electrolyte-derived moieties. • Electrolysis of phthalide affords products that depend on the method of analysis. • Upon reduction, phthalide undergoes deuteration in the presence of deuterium oxide. -- Abstract: Cyclic voltammetry and controlled-potential (bulk) electrolysis have been used to investigate the direct reduction of phthalide at carbon electrodes in dimethylformamide (DMF) containing 0.10 M tetramethylammonium perchlorate (TMAP) or tetra-n-butylammonium perchlorate (TBAP). Cyclic voltammograms recorded with a glassy carbon electrode exhibit a single cathodic peak and a corresponding anodic peak that arise, respectively, from one-electron reduction of phthalide to generate a radical-anion intermediate and from reoxidation of the intermediate. At a scan rate of 100 mV s −1 , quasi-reversible behavior is observed (due to ring-opening of the radical-anion), whereas fully reversible behavior is seen at 5 V s −1 or higher. Digital simulation of cyclic voltammograms indicates that the lifetime of the radical-anion is 3.5 s. Bulk electrolysis of phthalide at a reticulated vitreous carbon cathode affords products that depend on the procedure used to analyze the catholyte. Direct injection of catholyte into a gas chromatograph shows phthalide and a 2-methylbenzoate ester bearing an alkyl moiety from the supporting-electrolyte cation. However, if the catholyte is partitioned between diethyl ether and aqueous hydrochloric acid before gas chromatographic analysis, phthalide and 2-methylbenzoic acid are observed. Thermally induced reactions that occur in the injector port of the gas chromatograph are responsible for the formation of the 2-methylbenzoate ester as well as for the phthalide found in all electrolyzed solutions

  19. Thermal Boundary Layer Effects on Line-of-Sight Tunable Diode Laser Absorption Spectroscopy (TDLAS) Gas Concentration Measurements.

    Science.gov (United States)

    Qu, Zhechao; Werhahn, Olav; Ebert, Volker

    2018-06-01

    The effects of thermal boundary layers on tunable diode laser absorption spectroscopy (TDLAS) measurement results must be quantified when using the line-of-sight (LOS) TDLAS under conditions with spatial temperature gradient. In this paper, a new methodology based on spectral simulation is presented quantifying the LOS TDLAS measurement deviation under conditions with thermal boundary layers. The effects of different temperature gradients and thermal boundary layer thickness on spectral collisional widths and gas concentration measurements are quantified. A CO 2 TDLAS spectrometer, which has two gas cells to generate the spatial temperature gradients, was employed to validate the simulation results. The measured deviations and LOS averaged collisional widths are in very good agreement with the simulated results for conditions with different temperature gradients. We demonstrate quantification of thermal boundary layers' thickness with proposed method by exploitation of the LOS averaged the collisional width of the path-integrated spectrum.

  20. An on-line push/pull perfusion-based hollow-fiber liquid-phase microextraction system for high-performance liquid chromatographic determination of alkylphenols in water samples.

    Science.gov (United States)

    Chao, Yu-Ying; Jian, Zhi-Xuan; Tu, Yi-Ming; Wang, Hsaio-Wen; Huang, Yeou-Lih

    2013-06-07

    In this study, we employed a novel on-line method, push/pull perfusion hollow-fiber liquid-phase microextraction (PPP-HF-LPME), to extract 4-tert-butylphenol, 2,4-di-tert-butylphenol, 4-n-nonylphenol, and 4-n-octylphenol from river and tap water samples; we then separated and quantified the extracted analytes through high-performance liquid chromatography (HPLC). Using this approach, we overcame the problem of fluid loss across the porous HF membrane to the donor phase, permitting on-line coupling of HF-LPME to HPLC. In our PPP-HF-LPME system, we used a push/pull syringe pump as the driving source to perfuse the acceptor phase, while employing a heating mantle and an ultrasonic probe to accelerate mass transfer. We optimized the experimental conditions such as the nature of the HF supported intermediary phase and the acceptor phase, the composition of the donor and acceptor phases, the sample temperature, and the sonication conditions. Our proposed method provided relative standard deviations of 3.1-6.2%, coefficients of determination (r(2)) of 0.9989-0.9998, and limits of detection of 0.03-0.2 ng mL(-1) for the analytes under the optimized conditions. When we applied this method to analyses of river and tap water samples, our results confirmed that this microextraction technique allows reliable monitoring of alkylphenols in water samples.

  1. An integrated methodological approach to the computer-assisted gas chromatographic screening of basic drugs in biological fluids using nitrogen selective detection.

    Science.gov (United States)

    Dugal, R; Massé, R; Sanchez, G; Bertrand, M J

    1980-01-01

    This paper presents the methodological aspects of a computerized system for the gas-chromatographic screening and primary identification of central nervous system stimulants and narcotic analgesics (including some of their respective metabolites) extracted from urine. The operating conditions of a selective nitrogen detector for optimized analytical functions are discussed, particularly the effect of carrier and fuel gas on the detector's sensitivity to nitrogen-containing molecules and discriminating performance toward biological matrix interferences. Application of simple extraction techniques, combined with rapid derivatization procedures, computer data acquisition, and reduction of chromatographic data are presented. Results show that this system approach allows for the screening of several drugs and their metabolites in a short amount of time. The reliability and stability of the system have been tested by analyzing several thousand samples for doping control at major international sporting events and for monitoring drug intake in addicts participating in a rehabilitation program. Results indicate that these techniques can be used and adapted to many different analytical toxicology situations.

  2. Simultaneous derivatisation and preconcentration of parabens in food and other matrices by isobutyl chloroformate and dispersive liquid-liquid microextraction followed by gas chromatographic analysis.

    Science.gov (United States)

    Jain, Rajeev; Mudiam, Mohana Krishna Reddy; Chauhan, Abhishek; Ch, Ratnasekhar; Murthy, R C; Khan, Haider A

    2013-11-01

    A simple, rapid and economical method has been proposed for the quantitative determination of parabens (methyl, ethyl, propyl and butyl paraben) in different samples (food, cosmetics and water) based on isobutyl chloroformate (IBCF) derivatisation and preconcentration using dispersive liquid-liquid microextraction in single step. Under optimum conditions, solid samples were extracted with ethanol (disperser solvent) and 200 μL of this extract along with 50 μL of chloroform (extraction solvent) and 10 μL of IBCF was rapidly injected into 2 mL of ultra-pure water containing 150 μL of pyridine to induce formation of a cloudy state. After centrifugation, 1 μL of the sedimented phase was analysed using gas chromatograph-flame ionisation detector (GC-FID) and the peaks were confirmed using gas chromatograph-positive chemical ionisation-mass spectrometer (GC-PCI-MS). Method was found to be linear over the range of 0.1-10 μg mL(-1) with square of correlation coefficient (R(2)) in the range of 0.9913-0.9992. Limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.029-0.102 μg mL(-1) and 0.095-0.336 μg mL(-1) with a signal to noise ratio of 3:1 and 10:1, respectively. Copyright © 2013 Elsevier Ltd. All rights reserved.

  3. On-Line Fuel Failure Monitor for Fuel Testing and Monitoring of Gas Cooled Very High Temperature Reactors

    International Nuclear Information System (INIS)

    Hawari, Ayman I.; Bourham, Mohamed A.

    2010-01-01

    Very High Temperature Reactors (VHTR) utilize the TRISO microsphere as the fundamental fuel unit in the core. The TRISO microsphere (∼ 1-mm diameter) is composed of a UO2 kernel surrounded by a porous pyrolytic graphite buffer, an inner pyrolytic graphite layer, a silicon carbide (SiC) coating, and an outer pyrolytic graphite layer. The U-235 enrichment of the fuel is expected to range from 4%-10% (higher enrichments are also being considered). The layer/coating system that surrounds the UO2 kernel acts as the containment and main barrier against the environmental release of radioactivity. To understand better the behavior of this fuel under in-core conditions (e.g., high temperature, intense fast neutron flux, etc.), the US Department of Energy (DOE) is launching a fuel testing program that will take place at the Advanced Test Reactor (ATR) located at Idaho National Laboratory (INL). During this project North Carolina State University (NCSU) researchers will collaborate with INL staff for establishing an optimized system for fuel monitoring for the ATR tests. In addition, it is expected that the developed system and methods will be of general use for fuel failure monitoring in gas cooled VHTRs.

  4. Towards the interaction between calcium carbide and water during gas-chromatographic determination of trace moisture in ultra-high purity ammonia.

    Science.gov (United States)

    Trubyanov, Maxim M; Mochalov, Georgy M; Suvorov, Sergey S; Puzanov, Egor S; Petukhov, Anton N; Vorotyntsev, Ilya V; Vorotyntsev, Vladimir M

    2018-05-16

    The current study focuses on the processes involved during the flow conversion of water into acetylene in a calcium carbide reaction cell for the trace moisture analysis of ammonia by reaction gas chromatography. The factors negatively affecting the reproducibility and the accuracy of the measurements are suggested and discussed. The intramolecular reaction of the HOCaCCH intermediate was found to be a side reaction producing background acetylene during the contact of wet ammonia gas with calcium carbide. The presence of the HOCaCCH intermediate among the reaction products is confirmed by an FTIR spectral study of calcium carbide powder exposed to wet gas. The side reaction kinetics is evaluated experimentally and its influence on the results of the gas chromatographic measurements is discussed in relation to the determination of the optimal operating parameters for ammonia analysis. The reaction gas chromatography method for the trace moisture measurements in an ammonia matrix was experimentally compared to an FTIR long-path length gas cell technique to evaluate the accuracy limitations and the resource intensity. Copyright © 2018 Elsevier B.V. All rights reserved.

  5. Gas chromatography-mass spectrometric analysis of products from on-line pyrolysis/silylation of plant gums used as binding media

    Science.gov (United States)

    Chiantore, Oscar; Riedo, Chiara; Scalarone, Dominique

    2009-07-01

    Plant gums are complex polysaccharides used in the field of cultural heritage especially as binding media. Classification of polysaccharides may be achieved on the basis of monosaccharides composition after cleavage of glycosidic bond. Characterization of plant gums in works of art is complicated by the necessity of to use a method minimally invasive and requiring a small mount of sample. Pyrolisys is an useful method to obtain polysaccharides decomposition and generally pyrolysis products can be identified by the use of gas chromatography-mass spectrometry. This paper describes a method where two plant gums, arabic and tragacanth, were pyrolized in presence of silylating agents (HMDS e BSTFA alone and with TMCS as catalyst) using an on-line Py-GC/MS apparatus. Some characteristic trimethylsilyl derivatives of monosaccharides were identified on the basis of mass spectra. The presence of characteristic pyrolysis products of sugars allows to distinguish the two gums.

  6. Epoxidized soy bean oil migrating from the gaskets of lids into food packed in glass jars. Analysis by on-line liquid chromatography-gas chromatography.

    Science.gov (United States)

    Fankhauser-Noti, Anja; Fiselier, Katell; Biedermann-Brem, Sandra; Grob, Koni

    2005-08-05

    The migration of epoxidized soy bean oil (ESBO) from the gasket in the lids of glass jars into foods, particularly those rich in edible oil, often far exceeds the legal limit (60 mg/kg). ESBO was determined through a methyl ester isomer of diepoxy linoleic acid. Transesterification occurred directly in the homogenized food. From the extracted methyl esters, the diepoxy components were isolated by normal-phase LC and transferred on-line to gas chromatography with flame ionization detection using the on-column interface in the concurrent solvent evaporation mode. The method involves verification elements to ensure the reliability of the results for every sample analyzed. The detection limit is 2-5 mg/kg, depending on the food. Uncertainty of the procedure is below 10%.

  7. A rapid gas chromatographic injection-port derivatization method for the tandem mass spectrometric determination of patulin and 5-hydroxymethylfurfural in fruit juices.

    Science.gov (United States)

    Marsol-Vall, Alexis; Balcells, Mercè; Eras, Jordi; Canela-Garayoa, Ramon

    2016-07-01

    A novel method consisting of injection-port derivatization coupled to gas chromatography-tandem mass spectrometry is described. The method allows the rapid assessment of 5-hydroxymethylfurfural (HMF) and patulin content in apple and pear derivatives. The chromatographic separation of the compounds was achieved in a short chromatographic run (12.2min) suitable for routine controls of these compounds in the fruit juice industry. The optimal conditions for the injection-port derivatization were at 270°C, 0.5min purge-off, and a 1:2 sample:derivatization reagent ratio (v/v). These conditions represent an important saving in terms of derivatization reagent consumption and sample preparation time. Quality parameters were assessed for the target compounds, giving LOD of 0.7 and 1.6μg/kg and LOQ of 2 and 5μg/kg for patulin and HMF, respectively. These values are below the maximum patulin concentration in food products intended for infants and young children. Repeatability (%RSD n=5) was below 12% for both compounds. In addition, the method linearity ranged between 25 and 1000μg/kg and between 5 and 192μg/kg for HMF and patulin, respectively. Finally, the method was applied to study HMF and patulin content in various fruit juice samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  8. Effects of GC temperature and carrier gas flow rate on on-line oxygen isotope measurement as studied by on-column CO injection.

    Science.gov (United States)

    Chen, Zhi-Gang; Yin, Xi-Jie; Zhou, Youping

    2015-08-01

    Although deemed important to δ 18 O measurement by on-line high-temperature conversion techniques, how the GC conditions affect δ 18 O measurement is rarely examined adequately. We therefore directly injected different volumes of CO or CO-N 2 mix onto the GC column by a six-port valve and examined the CO yield, CO peak shape, CO-N 2 separation, and δ 18 O value under different GC temperatures and carrier gas flow rates. The results show the CO peak area decreases when the carrier gas flow rate increases. The GC temperature has no effect on peak area. The peak width increases with the increase of CO injection volume but decreases with the increase of GC temperature and carrier gas flow rate. The peak intensity increases with the increase of GC temperature and CO injection volume but decreases with the increase of carrier gas flow rate. The peak separation time between N 2 and CO decreases with an increase of GC temperature and carrier gas flow rate. δ 18 O value decreases with the increase of CO injection volume (when half m/z 28 intensity is rate. On average, the δ 18 O value of the injected CO is about 1‰ higher than that of identical reference CO. The δ 18 O distribution pattern of the injected CO is probably a combined result of ion source nonlinearity and preferential loss of C 16 O or oxygen isotopic exchange between zeolite and CO. For practical application, a lower carrier gas flow rate is therefore recommended as it has the combined advantages of higher CO yield, better N 2 -CO separation, lower He consumption, and insignificant effect on δ 18 O value, while a higher-than-60 °C GC temperature and a larger-than-100 µl CO volume is also recommended. When no N 2 peak is expected, a higher GC temperature is recommended, and vice versa. Copyright © 2015 John Wiley & Sons, Ltd. Copyright © 2015 John Wiley & Sons, Ltd.

  9. Gas chromatographic-mass spectrometric determination of hydrophilic compounds in environmental water by solid-phase extraction with activated carbon fiber felt.

    Science.gov (United States)

    Kawata, K; Ibaraki, T; Tanabe, A; Yagoh, H; Shinoda, A; Suzuki, H; Yasuhara, A

    2001-03-09

    Simple gas chromatographic-mass spectrometric determination of hydrophilic organic compounds in environmental water was developed. A cartridge containing activated carbon fiber felt was made by way of trial and was evaluated for solid-phase extraction of the compounds in water. The hydrophilic compounds investigated were acrylamide, N,N-dimethylacetamide, N,N-dimethylformamide, 1,4-dioxane, furfural, furfuryl alcohol, N-nitrosodiethylamine and N-nitrosodimethylamine. Overall recoveries were good (80-100%) from groundwater and river water. The relative standard deviations ranged from 4.5 to 16% for the target compounds. The minimum detectable concentrations were 0.02 to 0.03 microg/l. This method was successfully applied to several river water samples.

  10. Stereometabolism of ethylbenzene in man: gas chromatographic determination of urinary excreted mandelic acid enantiomers and phenylglyoxylic acid and their relation to the height of occupational exposure.

    Science.gov (United States)

    Korn, M; Gfrörer, W; Herz, R; Wodarz, I; Wodarz, R

    1992-01-01

    Ethylbenzene is an important industrial solvent and a key substance in styrene production. Ethylbenzene metabolism leads to the formation of mandelic acid, which occurs in two enantiomeric forms, and phenylglyoxylic acid. To decide which enantiomer is preferably formed, 70 urine samples of exposed workers were taken at the end of shifts and--after 3-pentyl ester derivatisation--gas chromatographically analysed. The R/S ratio of mandelic acid enantiomers in urine amounts to 19:1, which means that R-mandelic acid is a major metabolite and S-mandelic acid is one of the minor urinary metabolites of ethylbenzene in man. The R/S ratio is independent of ambient air concentration of ethylbenzene within the investigated range. Compared to an ethylbenzene monoexposure the height of total mandelic acid excretion is decreased in the case of coexposure to other aromatic solvents.

  11. In situ alcoholysis of triacylglycerols by application of switchable-polarity solvents. A new derivatization procedure for the gas-chromatographic analysis of vegetable oils.

    Science.gov (United States)

    Saliu, Francesco; Orlandi, Marco

    2013-10-01

    We describe a new use of switchable-polarity solvents for the simultaneous derivatization and extraction of triacylglycerols from vegetable oils before gas-chromatographic analysis. Different equimolecular mixtures of the commercially available amidine 1,8-diazabicyclo[5.4.0]undec-7-ene and n-alkyl alcohols were tested. Triolein was used as a model compound. Very good results were achieved by using butanol (recovery of butyl oleate was 89 ± 4%). The procedure was applied for the characterization of the fatty acid profile of different vegetable oils. No statistically significant differences from the results obtained with the application of two traditional methods were evidenced. Moreover, the use of switchable-polarity solvents showed many advantages: owing to the basicity of the amidines, no catalyst was required; the transterification reaction was conducted under mild conditions, one step and in situ; no particular matrix interferences were evidenced; the solvent was recovered.

  12. Chromatographic methods

    International Nuclear Information System (INIS)

    Marhol, M.; Stary, J.

    1975-01-01

    The characteristics are given of chromatographic separation and the methods are listed. Methods and data on materials used in partition, adsorption, precipitation and ion exchange chromatography are listed and conditions are described under which ion partition takes place. Special attention is devoted to ion exchange chromatography where tables are given to show the course of values of the partition coefficients of different ions in dependence on the concentration of agents and the course of equilibrium sorptions on different materials in dependence on the solution pH. A theoretical analysis is given and the properties of the most widely used ion exchangers are listed. Experimental conditions and apparatus used for each type of chromatography are listed. (L.K.)

  13. On-line monitoring of methanol and methyl formate in the exhaust gas of an industrial formaldehyde production plant by a mid-IR gas sensor based on tunable Fabry-Pérot filter technology.

    Science.gov (United States)

    Genner, Andreas; Gasser, Christoph; Moser, Harald; Ofner, Johannes; Schreiber, Josef; Lendl, Bernhard

    2017-01-01

    On-line monitoring of key chemicals in an industrial production plant ensures economic operation, guarantees the desired product quality, and provides additional in-depth information on the involved chemical processes. For that purpose, rapid, rugged, and flexible measurement systems at reasonable cost are required. Here, we present the application of a flexible mid-IR filtometer for industrial gas sensing. The developed prototype consists of a modulated thermal infrared source, a temperature-controlled gas cell for absorption measurement and an integrated device consisting of a Fabry-Pérot interferometer and a pyroelectric mid-IR detector. The prototype was calibrated in the research laboratory at TU Wien for measuring methanol and methyl formate in the concentration ranges from 660 to 4390 and 747 to 4610 ppmV. Subsequently, the prototype was transferred and installed at the project partner Metadynea Austria GmbH and linked to their Process Control System via a dedicated micro-controller and used for on-line monitoring of the process off-gas. Up to five process streams were sequentially monitored in a fully automated manner. The obtained readings for methanol and methyl formate concentrations provided useful information on the efficiency and correct functioning of the process plant. Of special interest for industry is the now added capability to monitor the start-up phase and process irregularities with high time resolution (5 s).

  14. A simple and rapid gas chromatographic method for the determination of dissolved deuterium and nitrogen in heavy water coolant of a nuclear reactor

    International Nuclear Information System (INIS)

    Nair, B.K.S.

    1976-01-01

    A known volume of a heavy water sample is equilibrated with a known volume of pure helium gas at atmospheric pressure in a sample tube. The dissolved gases evolve into the helium and distribute themselves between the gaseous and liquid phases according to their equilibrium partial pressures. These partial pressures of the gases in the equilibrium gas mixture are determined by analysing it gas-chromatographically. From these analytical data and the absorption coefficients of deuterium and nitrogen, their original concentrations in heavy water are calculated. Corrections for the increase in the total pressure of the gaseous phase owing to evolved gases are calculated and found to be negligible. Air contamination during sampling and analysis can be detected by the presence of the oxygen peak in the chromatogram and corrected for. The calculation is facilitated by programming it on an electronic calculator. The method is much simpler and faster than the vacuum method usually applied for this analysis. One determination can be completed in about an hour. The average deviation and standard deviation have been estimated at 0.19 ml/litre heavy water and 0.25 ml/litre heavy water respectively in deuterium, and 0.36 and 0.68 ml/litre in nitrogen. (author)

  15. Gas chromatography-mass spectrometry and high-performance liquid chromatographic analyses of thermal degradation products of common plastics

    NARCIS (Netherlands)

    Pacakova, V.; Leclercq, P.A.

    1991-01-01

    The thermo-oxidation of five commonly used materials, namely low-density polyethylene, retarded polyethylene, paper with a polyethylene foil, a milk package and filled polypropylene, was studied. Capillary gas chromatography and gas chromatography-mass spectrometry were used to analyze the volatile

  16. GEM-AQ, an on-line global multiscale chemical weather modelling system: model description and evaluation of gas phase chemistry processes

    Directory of Open Access Journals (Sweden)

    J. W. Kaminski

    2008-06-01

    Full Text Available Tropospheric chemistry and air quality processes were implemented on-line in the Global Environmental Multiscale weather prediction model. The integrated model, GEM-AQ, was developed as a platform to investigate chemical weather at scales from global to urban. The current chemical mechanism is comprised of 50 gas-phase species, 116 chemical and 19 photolysis reactions, and is complemented by a sectional aerosol module with 5 aerosols types. All tracers are advected using the semi-Lagrangian scheme native to GEM. The vertical transport includes parameterized subgrid-scale turbulence and large scale deep convection. Dry deposition is included as a flux boundary condition in the vertical diffusion equation. Wet deposition of gas-phase species is treated in a simplified way, and only below-cloud scavenging is considered. The emissions used include yearly-averaged anthropogenic, and monthly-averaged biogenic, ocean, soil, and biomass burning emission fluxes, as well as NOx from lightning. In order to evaluate the ability to simulate seasonal variations and regional distributions of trace gases such as ozone, nitrogen dioxide and carbon monoxide, the model was run for a period of five years (2001–2005 on a global uniform 1.5°×1.5° horizontal resolution domain and 28 hybrid levels extending up to 10 hPa. Model results were compared with observations from satellites, aircraft measurement campaigns and balloon sondes. We find that GEM-AQ is able to capture the spatial details of the chemical fields in the middle and lower troposphere. The modelled ozone consistently shows good agreement with observations, except over tropical oceans. The comparison of carbon monoxide and nitrogen dioxide with satellite measurements emphasizes the need for more accurate, year-specific emissions fluxes for biomass burning and anthropogenic sources. Other species also compare well with available observations.

  17. Characterisation of organic compounds in aerosol particles from a finnish forest by on-line coupled supercritical fluid extraction-liquid chromatography-gas chromatography-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Shimmo, Masahiko; Jaentti, Jaana; Hartonen, Kari; Hyoetylaeinen, Tuulia; Riekkola, Marja-Liisa [Laboratory of Analytical Chemistry, Department of Chemistry, University of Helsinki, P.O. Box 55, 00014, Helsinki (Finland); Aalto, Pasi; Kulmala, Markku [Division of Atmospheric Sciences, Department of Physical Sciences, University of Helsinki, P.O. Box 64, 00014, Helsinki (Finland)

    2004-04-01

    During the European Union project Quantification of Aerosol Nucleation in the European Boundary Layer (QUEST), which began in spring 2003, atmospheric aerosol particles were collected in a Finnish Scots pine forest using a high-volume sampler. The organic compounds in the filter samples were then analysed by on-line coupled supercritical fluid extraction-liquid chromatography-gas chromatography-mass spectrometry (SFE-LC-GC-MS). The sample was first extracted by SFE. During LC the extracts were fractionated into three fractions according to polarity. The final separation was carried out by GC-MS. A fraction volume as high as 840 {mu}L was transferred to the GC, using the partial concurrent eluent evaporation technique. The same instrumentation, with an in-situ SFE derivatisation method, was used to analyse organic acids. Major compounds such as n-alkanes and PAH were analysed quantitatively. Their concentrations were lower than those usually observed in urban areas or in other forest areas in Europe. The wind direction was one of the most important factors affecting changes in the daily concentrations of these compounds. Scots pine needles were analysed with the same system to obtain reference data for identification of biogenic compounds in aerosol particles. Other organic compounds found in this study included hopanes, steranes, n-alkanals, n-alkan-2-ones, oxy-PAH, and alkyl-PAH; some biogenic products, including oxidation products of monoterpenes, were also identified. (orig.)

  18. Gas chromatography-mass spectrometry and high-performance liquid chromatographic analyses of thermal degradation products of common plastics

    OpenAIRE

    Pacakova, V.; Leclercq, P.A.

    1991-01-01

    The thermo-oxidation of five commonly used materials, namely low-density polyethylene, retarded polyethylene, paper with a polyethylene foil, a milk package and filled polypropylene, was studied. Capillary gas chromatography and gas chromatography-mass spectrometry were used to analyze the volatile degradation products, while high-performance liquid chromatography was employed to measure polycyclic aromatic hydrocarbons. The results are discussed from the point of view of toxicity of the prod...

  19. [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%.

  20. Chemometric strategy for automatic chromatographic peak detection and background drift correction in chromatographic data.

    Science.gov (United States)

    Yu, Yong-Jie; Xia, Qiao-Ling; Wang, Sheng; Wang, Bing; Xie, Fu-Wei; Zhang, Xiao-Bing; Ma, Yun-Ming; Wu, Hai-Long

    2014-09-12

    Peak detection and background drift correction (BDC) are the key stages in using chemometric methods to analyze chromatographic fingerprints of complex samples. This study developed a novel chemometric strategy for simultaneous automatic chromatographic peak detection and BDC. A robust statistical method was used for intelligent estimation of instrumental noise level coupled with first-order derivative of chromatographic signal to automatically extract chromatographic peaks in the data. A local curve-fitting strategy was then employed for BDC. Simulated and real liquid chromatographic data were designed with various kinds of background drift and degree of overlapped chromatographic peaks to verify the performance of the proposed strategy. The underlying chromatographic peaks can be automatically detected and reasonably integrated by this strategy. Meanwhile, chromatograms with BDC can be precisely obtained. The proposed method was used to analyze a complex gas chromatography dataset that monitored quality changes in plant extracts during storage procedure. Copyright © 2014 Elsevier B.V. All rights reserved.

  1. Capillary gas chromatographic analysis of mycolic acid cleavage products, cellular fatty acids, and alcohols of Mycobacterium xenopi.

    OpenAIRE

    Luquin, M; Lopez, F; Ausina, V

    1989-01-01

    The fatty acids, alcohols, and mycolic acids of 26 strains of Mycobacterium xenopi were studied by capillary gas chromatography and thin-layer chromatography. All strains contained alpha-, keto-, and omega-carboxymycolates. The primary mycolic acid cleavage product was hexacosanoic acid. The fatty acid patterns and, especially, the presence of 2-docosanol are characteristic markers of M. xenopi.

  2. Determination of Diffusion Coefficients and Activation Energy of Selected Organic Liquids using Reversed-Flow Gas Chromatographic Technique

    International Nuclear Information System (INIS)

    Khalisanni Khalid; Rashid Atta Khan; Sharifuddin Mohd Zain

    2012-01-01

    Evaporation of vaporize organic liquid has ecological consequences when the compounds are introduced into both freshwater and marine environments through industrial effluents, or introduced directly into the air from industrial unit processes such as bioreactors and cooling towers. In such cases, a rapid and simple method are needed to measure physicochemical properties of the organic liquids. The Reversed-Flow Gas Chromatography (RF-GC) sampling technique is an easy, fast and accurate procedure. It was used to measure the diffusion coefficients of vapors from liquid into a carrier gas and at the same time to determine the rate coefficients for the evaporation of the respective liquid. The mathematical expression describing the elution curves of the samples peaks was derived and used to calculate the respective parameters for the selected liquid pollutants selected such as methanol, ethanol, 1-propanol, 1-butanol, n-pentane, n-hexane, n-heptane and n-hexadecane, evaporating into the carrier gas of nitrogen. The values of diffusion coefficients found were compared with those calculated theoretically or reported in the literature. The values of evaporation rate were used to determine the activation energy of respective samples using Arrhenius equation. An interesting finding of this work is by using an alternative mathematical analysis based on equilibrium at the liquid-gas interphase, the comparison leads to profound agreement between theoretical values of diffusion coefficients and experimental evidence. (author)

  3. Rapid and simple clean-up and derivatizaton procedure for the gas chromatographic determination of acidic drugs in plasma

    NARCIS (Netherlands)

    Roseboom, H.; Hulshoff, A.

    1979-01-01

    A rapid and simple clean-up and derivatization procedure that can be generally applied to the gas chromatographie (GC) determination of acidic drugs of various chemical and therapeutic classes is described. The drugs are extracted from acidified plasma with chloroform containing 5% of isopropanol,

  4. Gas chromatographic analysis of Tri-N-Octyl-Phosphine oxide (Topo) in D2EHPA-Topo-Kerosene mixtures

    International Nuclear Information System (INIS)

    Perez Garcia, M.

    1973-01-01

    A study about the minimum limit of TOPO, detectable by gas chromatography in an organic phase formed by D2EHPA and kerosene is carried out. The retention time and response factor under the same conditions are also studied. Octacosane has been used as a reference hydrocarbon. (Author) 8 refs

  5. Gas chromatographic quadrupole time-of-flight full scan high resolution mass spectrometric screening of human urine in antidoping analysis

    NARCIS (Netherlands)

    Abushareeda, Wadha; Lyris, Emmanouil; Kraiem, Suhail; Wahaibi, Aisha Al; Alyazidi, Sameera; Dbes, Najib; Lommen, Arjen; Nielen, Michel; Horvatovich, Peter L.; Alsayrafi, Mohammed; Georgakopoulos, Costas

    2017-01-01

    This paper presents the development and validation of a high-resolution full scan (FS) electron impact ionization (EI) gas chromatography coupled to quadrupole Time-of-Flight mass spectrometry (GC/QTOF) platform for screening anabolic androgenic steroids (AAS) in human urine samples. The World

  6. Gas chromatographic quadrupole time-of-flight full scan high resolution mass spectrometric screening of human urine in antidoping analysis

    NARCIS (Netherlands)

    Abushareeda, Wadha; Lyris, Emmanouil; Kraiem, Suhail; Wahaibi, Aisha Al; Alyazidi, Sameera; Dbes, Najib; Lommen, Arjen; Nielen, Michel; Horvatovich, Peter L.; Alsayrafi, Mohammed; Georgakopoulos, Costas

    2017-01-01

    This paper presents the development and validation of a high-resolution full scan (FS) electron impact ionization (EI) gas chromatography coupled to quadrupole Time-of-Flight mass spectrometry (GC/QTOF) platform for screening anabolic androgenic steroids (AAS) in human urine samples. The World

  7. A charge-polarized porous metal-organic framework for gas chromatographic separation of alcohols from water.

    Science.gov (United States)

    Sun, Jian-Ke; Ji, Min; Chen, Cheng; Wang, Wu-Gen; Wang, Peng; Chen, Rui-Ping; Zhang, Jie

    2013-02-25

    A bipyridinium ligand with a charge separated skeleton has been introduced into a metal-organic framework to yield a porous material with charge-polarized pore space, which exhibits selective adsorption for polar guest molecules and can be further used in gas chromatography for the separation of alcohol-water mixtures.

  8. On-line gas chromatography combustion/pyrolysis isotope ratio mass spectrometry (HRGC-C/P-IRMS) of pineapple (Ananas comosus L. Merr.) volatiles.

    Science.gov (United States)

    Preston, Christina; Richling, Elke; Elss, Sandra; Appel, Markus; Heckel, Frank; Hartlieb, Ariane; Schreier, Peter

    2003-12-31

    By use of extracts prepared by liquid-liquid separation of the volatiles from self-prepared juices of pineapple fruits (Ananas comosus) (n = 14) as well as commercial pineapple recovery aromas/water phases (n = 3), on-line capillary gas chromatography-isotope ratio mass spectrometry was employed in the combustion (C) and the pyrolysis (P) modes (HRGC-C/P-IRMS) to determine the delta(13)C(VPDB) and delta(2)H(VSMOW) values of selected pineapple flavor constituents. In addition to methyl 2-methylbutanoate 1, ethyl 2-methylbutanoate 2, methyl hexanoate 3, ethyl hexanoate 4, and 2,5-dimethyl-4-methoxy-3[2H]-furanone 5, each originating from the fruit, the delta(13)C(VPDB) and delta(2)H(VSMOW) data of commercial synthetic 1-5 and "natural" (biotechnologically derived) 1-4 were determined. With delta(13)C(VPDB) data of pineapple volatiles 1-4 varying from -12.8 to -24.4 per thousand, the range expected for CAM metabolism was observed. Compound 5 showed higher depletion from -20.9 to -28.6 per thousand. A similar situation was given for the delta(2)H(VSMOW) values of 3-5 from pineapple ranging from -118 to -191 per thousand, whereas 1 and 2 showed higher depleted values from -184 to -263 per thousand. In nearly all cases, analytical differentiation of 1-5 from pineapple and natural as well as synthetic origin was possible. In general, natural and synthetic 1-5 exhibited delta(13)C(VPDB) data ranging from -11.8 to -32.2 per thousand and -22.7 to -35.9 per thousand, respectively. Their delta(2)H(VSMOW) data were in the range from -242 to -323 per thousand and -49 to -163 per thousand, respectively.

  9. On-line purge-and-trap-gas chromatography with flame ionization detection as an alternative analytical method for dimethyl sulphide trace release from marine algae

    Energy Technology Data Exchange (ETDEWEB)

    Careri, M.; Musci, M.; Bianchi, F.; Mucchino, C. [Parma Univ., Parma (Italy). Dipt. di Chimica Generale ed Inorganica, Chimica Analitica e Chimica Fisica; Azzoni, R.; Viaroli, P. [Parma Univ., Parma (Italy). Dipt. di Scienze Ambientali

    2001-10-01

    The release of dimethyl sulphide (DMS) by the seaweed Ulva spp at trace level was studied in aqueous solutions at different salinities, temperature and light intensities. For this purpose, the purge-and-trap technique combined with gas chromatography-flame ionization detection was used. The analytical method was evaluated in terms of linearity range, limit of detection, precision and accuracy by considering 10% (w/v) and 30% (w/v) synthetic seawater as aqueous matrices. Calculation of the recovery function evidenced a matrix influence. The method of standard addition was then used for an accurate determination of DMS in synthetic seawater reproduction the matrix effect. DMS fluxes were analysed in batch cultures of Ulva spp reproducing the conditions which usually occur in the Sacca di Goro lagoon (Northern Adriatic Sea, Italy). [Italian] Il rilascio di dimetilsolfuro (DMS) in tracce da parte della macroalga Ulva spp e' stato studiato in soluzioni acquose di differente salinita' mediante la tecnica purge-and-trap accoppiata on-line alla gascromatografia con rivelazione a ionizzazione di fiamma (GC-FID). Il metodo analitico e' stato validato in termini di linearita' di risposta, di limite di rivelabilita', precisione e accuratezza considerando come matrice acqua di mare sintetica a diversa salinita' (10%0 m/v e 30%0 m/v). Il calcolo della funzione di recupero ha consentito di verificare la presenza di errori sistematici dovuti all'effetto matrice. Il metodo sviluppato e' stato quindi applicato a matrici ambientali allo scopo di verificare il rilascio di DMS da parte di Ulva spp, operando in condizioni ambientali simili a quelle che si verificano nella Sacca di Goro (Ferrara, Italia).

  10. Analysis of particulate polycyclic aromatic hydrocarbons by on-line coupled supercritical fluid extraction-liquid chromatography-gas chromatography-mass spectrometry

    Science.gov (United States)

    Shimmo, Masahiko; Adler, Heidi; Hyötyläinen, Tuulia; Hartonen, Kari; Kulmala, Markku; Riekkola, Marja-Liisa

    An on-line supercritical fluid extraction-liquid chromatography-gas chromatography-mass spectrometry (SFE-LC-GC-MS) method was developed for the analysis of the particulate polycyclic aromatic hydrocarbons (PAHs). The limits of detection of the system for the quantification standards were in the range of 0.25-0.57 ng, while the limits of determinations for filter samples varied from 0.02 to 0.04 ng m -3 (24 h sampling). The linearity was excellent from 5 to 300 ng ( R2>0.967). The analysis could be carried out in a closed system without tedious manual sample pretreatment and with no risk of errors by contamination or loss of the analytes. The results of the SFE-LC-GC-MS method were comparable with those for Soxhlet and shake-flask extractions with GC-MS. The new method was applied to the analysis of PAHs collected by high-volume filter in the Helsinki area to study the seasonal trend of the concentrations. The individual PAH concentrations varied from 0.015 to more than 1 ng m -3, while total PAH concentrations varied from 0.81 to 5.68 ng m -3. The concentrations were generally higher in winter than in summer. The mass percentage of the total PAHs in total suspended particulates ranged from 2.85×10 -3% in July to 15.0×10 -3% in December. Increased emissions in winter, meteorological conditions, and more serious artefacts during the sampling in summer season may explain the concentration profiles.

  11. 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

  12. An automated method for the analysis of phenolic acids in plasma based on ion-pairing micro-extraction coupled on-line to gas chromatography/mass spectrometry with in-liner derivatisation

    NARCIS (Netherlands)

    Peters, S.; Kaal, E.; Horsting, I.; Janssen, H.-G.

    2012-01-01

    A new method is presented for the analysis of phenolic acids in plasma based on ion-pairing ‘Micro-extraction in packed sorbent’ (MEPS) coupled on-line to in-liner derivatisation-gas chromatography-mass spectrometry (GC-MS). The ion-pairing reagent served a dual purpose. It was used both to improve

  13. Chromatographic and biological aspects of organomercurials

    Energy Technology Data Exchange (ETDEWEB)

    Fishbein, L

    1970-01-01

    A thorough review on the biological and chromatographic aspects of methylmercury, phenylmercurials, and miscellaneous organomercurials is presented. Areas covered include ecology, epidemiology, paper chromatography, thin-layer chromatography, gas chromatography, metabolism and toxicity, and environmental degradation. 183 references.

  14. Method for the routine quantitative gas chromatographic analysis of major free fatty acids in butter and cream.

    Science.gov (United States)

    Woo, A H; Lindsay, R C

    1980-07-01

    A rapid quantiative method was developed for routine analysis of the major, even carbon-numbered free fatty acids in butter and cream. Free fatty acids were isolated directly from intact samples by a modified silicic acid-potassium hydroxide arrestant column and were separated by gas chromatography with a 1.8 m x 2 mm inner diameter glass column packed with 10% neopentyl glycol adipate on 80/100 Chromosorb W. Purified, formic acid-saturated carrier gas was required for minimal peak tailing and extended column life. The accuracy and reproducibility of the mmethod was established through quantitative recovery studies of free fatty acid mixtures, free fatty acids added to butter, and replicate analysis of butter and cream samples.

  15. Determination of polycyclic aromatic hydrocarbons (PAHs). gas chromatographic method; Determinazione degli idrocarburi policiclici aromatici (IPA). Metodo gascaromatografico

    Energy Technology Data Exchange (ETDEWEB)

    Menichini, E; Viviano, G [Istituto Superiore di Sanita` , Rome (Italy). Lab. di Igiene Ambientale

    1997-12-01

    The method enables the determination of 4- to 6- ring PAHs and particularly of carcinogenic PAHs regulated in Italy. This revision is based on the results of a national collaborative study. Sample extract, obtained by a method described in a previous report (Rapporto ISTISAN: 90/33) is cleaned up by thin layer chromatography and analysed by gas chromatography; identification is confirmed by mass spectrometry. An intralaboratory quality control program is described.

  16. Comparison of two validated gas-chromatographic methods for the determination of trihalomethanes in drinking water Comparação de dois métodos cromatográficos validados para a dosagem de trialometanos em água potável

    OpenAIRE

    Maria Yumiko Tominaga; Antonio Flavio Mídio

    2003-01-01

    In this paper the results obtained using two validated gas-chromatographic procedures on drinking water for the determination of trihalomethanes are compared. The volatile compounds, chloroform (CF), bromodichloromethane (BDCM), dibromochloromethane (DBCM) and bromoform (BF) were detected by purge and trap capillary column gas-chromatography with electrolytic conductivity detector ( ELCD) and the simple and rapid gas-chromatographic method by electron capture detector (ECD) after liquid-liqui...

  17. Pulse gas chromatographic study of adsorption of substituted aromatics and heterocyclic molecules on MIL-47 at zero coverage.

    Science.gov (United States)

    Duerinck, Tim; Couck, Sarah; Vermoortele, Frederik; De Vos, Dirk E; Baron, Gino V; Denayer, Joeri F M

    2012-10-02

    The low coverage adsorptive properties of the MIL-47 metal organic framework toward aromatic and heterocyclic molecules are reported in this paper. The effect of molecular functionality and size on Henry adsorption constants and adsorption enthalpies of alkyl and heteroatom functionalized benzene derivates and heterocyclic molecules was studied using pulse gas chromatography. By means of statistical analysis, experimental data was analyzed and modeled using principal component analysis and partial least-squares regression. Structure-property relationships were established, revealing and confirming several trends. Among the molecular properties governing the adsorption process, vapor pressure, mean polarizability, and dipole moment play a determining role.

  18. Comparison of gas chromatographic and gravimetric methods for quantization of total fat and fatty acids in foodstuffs

    Directory of Open Access Journals (Sweden)

    Sabria Aued-Pimentel

    2010-01-01

    Full Text Available Different methods to determine total fat (TF and fatty acids (FA, including trans fatty acids (TFA, in diverse foodstuffs were evaluated, incorporating gravimetric methods and gas chromatography with flame ionization detector (GC/FID, in accordance with a modified AOAC 996.06 method. Concentrations of TF and FA obtained through these different procedures diverged (p< 0.05 and TFA concentrations varied beyond 20 % of the reference values. The modified AOAC 996.06 method satisfied both accuracy and precision, was fast and employed small amounts of low toxicity solvents. Therefore, the results showed that this methodology is viable to be adopted in Brazil for nutritional labeling purposes.

  19. Determination of plant stanols and plant sterols in phytosterol enriched foods with a gas chromatographic-flame ionization detection method: NMKL collaborative study.

    Science.gov (United States)

    Laakso, Päivi H

    2014-01-01

    This collaborative study with nine participating laboratories was conducted to determine the total plant sterol and/or plant stanol contents in phytosterol fortified foods with a gas chromatographic method. Four practice and 12 test samples representing mainly commercially available foodstuffs were analyzed as known replicates. Twelve samples were enriched with phytosterols, whereas four samples contained only natural contents of phytosterols. The analytical procedure consisted of two alternative approaches: hot saponification method, and acid hydrolysis treatment prior to hot saponification. As a result, sterol/stanol compositions and contents in the samples were measured. The amounts of total plant sterols and total plant stanols varying from 0.005 to 8.04 g/100 g product were statistically evaluated after outliers were eliminated. The repeatability RSD (RSDr) varied from 1.34 to 17.13%. The reproducibility RSD (RSDR) ranged from 3.03 to 17.70%, with HorRat values ranging from 0.8 to 2.1. When only phytosterol enriched food test samples are considered, the RSDr ranged from 1.48 to 6.13%, the RSD, ranged from 3.03 to 7.74%, and HorRat values ranged from 0.8 to 2.1. Based on the results of this collaborative study, the study coordinator concludes the method is fit for its purpose.

  20. Comparison of multiple linear regression, partial least squares and artificial neural networks for prediction of gas chromatographic relative retention times of trimethylsilylated anabolic androgenic steroids.

    Science.gov (United States)

    Fragkaki, A G; Farmaki, E; Thomaidis, N; Tsantili-Kakoulidou, A; Angelis, Y S; Koupparis, M; Georgakopoulos, C

    2012-09-21

    The comparison among different modelling techniques, such as multiple linear regression, partial least squares and artificial neural networks, has been performed in order to construct and evaluate models for prediction of gas chromatographic relative retention times of trimethylsilylated anabolic androgenic steroids. The performance of the quantitative structure-retention relationship study, using the multiple linear regression and partial least squares techniques, has been previously conducted. In the present study, artificial neural networks models were constructed and used for the prediction of relative retention times of anabolic androgenic steroids, while their efficiency is compared with that of the models derived from the multiple linear regression and partial least squares techniques. For overall ranking of the models, a novel procedure [Trends Anal. Chem. 29 (2010) 101-109] based on sum of ranking differences was applied, which permits the best model to be selected. The suggested models are considered useful for the estimation of relative retention times of designer steroids for which no analytical data are available. Copyright © 2012 Elsevier B.V. All rights reserved.

  1. 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.

  2. Acidic methanolysis v. alkaline saponification in gas chromatographic characterization of mycobacteria: differentiation between Mycobacterium avium-intracellulare and Mycobacterium gastri.

    Science.gov (United States)

    Larsson, L

    1983-08-01

    Mycobacterium avium-intracellulare and M.gastri were analyzed with capillary gas chromatography after each strain had been subjected to acidic methanolysis or to alkaline saponification followed by methylation. Prominent peaks of myristic, palmitoleic, palmitic, oleic, stearic and tuberculostearic acids were found in the chromatograms of both species, whereas 2-octadecanol and 2-eicosanol were detected only in M. avium-intracellulare. In initial runs, both of the derivatization principles yielded virtually identical chromatograms for a given strain. After repeated injections of extracts from alkaline saponification, however, the alcohol peaks showed pronounced tailing and finally almost disappeared from the chromatograms. This disadvantage, which was not observed when only acid methanolysis was used, could be overcome with trifluoroacetylation. Restored peak shape of the underivatized alcohols could be achieved by washing the cross-linked stationary phase in the capillary tubing with organic solvents. The study demonstrated the importance of conditions which enable separation of 2-octadecanol and 2-eicosanol when gas chromatography is used for species identification of mycobacteria.

  3. Loop system for creating jet fuel vapor standards used in the calibration of infrared spectrophotometers and gas chromatographs.

    Science.gov (United States)

    Reboulet, James; Cunningham, Robert; Gunasekar, Palur G; Chapman, Gail D; Stevens, Sean C

    2009-02-01

    A whole body inhalation study of mixed jet fuel vapor and its aerosol necessitated the development of a method for preparing vapor only standards from the neat fuel. Jet fuel is a complex mixture of components which partitions between aerosol and vapor when aspirated based on relative volatility of the individual compounds. A method was desired which could separate the vapor portion from the aerosol component to prepare standards for the calibration of infrared spectrophotometers and a head space gas chromatography system. A re-circulating loop system was developed which provided vapor only standards whose composition matched those seen in an exposure system. Comparisons of nominal concentrations in the exposure system to those determined by infrared spectrophotometry were in 92-95% agreement. Comparison of jet fuel vapor concentrations determined by infrared spectrophotometry compared to head space gas chromatography yielded a 93% overall agreement in trial runs. These levels of agreement show the loop system to be a viable method for creating jet fuel vapor standards for calibrating instruments.

  4. On-line monitoring of benzene air concentrations while driving in traffic by means of isotopic dilution gas chromatography/mass spectrometry.

    Science.gov (United States)

    Davoli, E; Cappellini, L; Moggi, M; Ferrari, S; Fanelli, R

    1996-01-01

    There is no shortage of information about the average benzene concentrations in urban air, but there is very little about microenvironmental exposure, such as in-vehicle concentrations while driving in various traffic conditions, while refuelling, or while in a parking garage. The main reason for this lack of data is that no analytical instrumentation has been available to measure on-line trace amounts of benzene in such situations. We have recently proposed a highly accurate, high-speed cryofocusing gas chromatography/mass spectrometry (GC/MS) system for monitoring benzene concentrations in air. Accuracy of the analytical data is achieved by enrichment of the air sample before trapping, with a stable isotope permeation tube system. The same principles have been applied to a new instrument, specifically designed for operation on an electric vehicle (Ducato Elettra, Fiat). The zero emission vehicle and the fully transportable, battery-operated GC/MS system provide a unique possibility of monitoring benzene exposure in real everyday situations such as while driving, refuelling, or repairing a car. All power consumptions have been reduced so as to achieve a battery-operated GC/MS system. Liquid nitrogen cryofocusing has been replaced by a packed, inductively heated, graphitized charcoal microtrap. The instrument has been mounted on shock absorbers and installed in the van. The whole system has been tested in both fixed and mobile conditions. The maximum monitoring period without external power supply is 6 h. The full analytical cycle is 4 min, allowing close to real-time monitoring, and the minimum detectable level is 1 microgram/m3 for benzene. In-vehicle monitoring showed that, when recirculation was off and ventilation on, i.e., air from outside the vehicle was blown inside, concentrations varied widely in different driving conditions: moving from a parking lot into normal traffic on an urban traffic condition roadway yielded an increase in benzene concentration

  5. A single gas chromatograph for accurate atmospheric mixing ratio measurements of CO2, CH4, N2O, SF6 and CO

    Directory of Open Access Journals (Sweden)

    H. A. J. Meijer

    2009-09-01

    Full Text Available We present an adapted gas chromatograph capable of measuring simultaneously and semi-continuously the atmospheric mixing ratios of the greenhouse gases CO2, CH4, N2O and SF6 and the trace gas CO with high precision and long-term stability. The novelty of our design is that all species are measured with only one device, making it a very cost-efficient system. No time lags are introduced between the measured mixing ratios. The system is designed to operate fully autonomously which makes it ideal for measurements at remote and unmanned stations. Only a small amount of sample air is needed, which makes this system also highly suitable for flask air measurements. In principle, only two reference cylinders are needed for daily operation and only one calibration per year against international WMO standards is sufficient to obtain high measurement precision and accuracy. The system described in this paper is in use since May 2006 at our atmospheric measurement site Lutjewad near Groningen, The Netherlands at 6°21´ E, 53°24´N, 1 m a.s.l. Results show the long-term stability of the system. Observed measurement precisions at our remote research station Lutjewad were: ±0.04 ppm for CO2, ±0.8 ppb for CH4, ±0.8 ppb for CO, ±0.3 ppb for N2O, and ±0.1 ppt for SF6. The ambient mixing ratios of all measured species as observed at station Lutjewad for the period of May 2007 to August 2008 are presented as well.

  6. Comparison of gravimetric and gas chromatographic methods for assessing performance of textile materials against liquid pesticide penetration.

    Science.gov (United States)

    Shaw, Anugrah; Abbi, Ruchika

    2004-01-01

    Penetration of liquid pesticides through textile materials is a criterion for determining the performance of protective clothing used by pesticide handlers. The pipette method is frequently used to apply liquid pesticides onto textile materials to measure penetration. Typically, analytical techniques such as Gas Chromatography (GC) are used to measure percentage penetration. These techniques are labor intensive and costly. A simpler gravimetric method was developed, and tests were conducted to compare the gravimetric and GC methods of analysis. Three types of pesticide formulations and 4 fabrics were used for the study. Diluted pesticide formulations were pipetted onto the test specimens and percentage penetration was measured using the 2 methods. For homogeneous formulation, the results of the two methods were fairly comparable. However, due to the filtering action of the textile materials, there were differences in the percentage penetration between the 2 methods for formulations that were not homogeneous.

  7. Evaluation of advanced gas chromatographs for on-site analysis. Final CRADA report for number Y-1295-0374

    Energy Technology Data Exchange (ETDEWEB)

    Wise, M.B.; Guerin, M.R.; Palausky, A.; Merriweather, R. [Lockheed Martin Energy Research, Oak Ridge, TN (United States); Forsberg, R.E. [Mine Safety Appliances-Baseline Industries, Lyons, CO (United States)

    1997-02-21

    The EKHO gas chromatography (GC) is being marketed by Mine Safety Appliances as an instrument for on-site environmental analysis and for process applications. This GC utilizes a unique bundled capillary column produced in Russia that provides very fast analysis and a wide linear dynamic range. Oak Ridge National Laboratory (ORNL) has been involved in a CRADA with Mine Safety Appliances in order to evaluate the analytical performance of the EKHO GC and is suitability for on-site environmental applications. Tests that were performed at ORNL included the analysis of air, water, and soil samples for aromatic hydrocarbons including benzene, toluene, xylene, and ethylbenzene (BTEX). These compounds were selected in order to simulate contamination by gasoline and other petroleum fuels. Performance factors that were studied included the instrument detection limits, the linearity, dynamic range, and precision for replicate samples. Other factors that were evaluated include the ease of set-up and operation.

  8. Measurement of Activity Coefficients of Solvents in Poly ( ethylene oxide ) Using Gas-Chromatographic Method and Correlation by Polymer-ASOG; Poriechirenokishido chu no yobai katsuryo keisu no gasukuromatogurafu ho ni yoru sokutei to Polymer-ASOG ni yoru sokan

    Energy Technology Data Exchange (ETDEWEB)

    Tochigi, K.; Kurita, S.; Ohashi, M. [Yuki Gosei Kogyo Co. LTd., (Japan); Kojima, K. [Nihon University, Tokyo (Japan). Department of Industrial Chemistry

    1997-09-01

    Infinite dilution activity coefficients (353.15-393.15 K) of six solvents (benzene, toluene, p-xylene, cyclohexane, acetone and methylethylketone) and activity coefficient at finite concentrations (353.15 K, 373.15 K) of these solvents in poly (ethylene oxide) are measured using gas-chromatographic method. The experimental data are then correlated by a polymer-ASOG model. 18 refs., 2 figs., 3 tabs.

  9. Evaluation of Pentachlorophenol Residues in Some Hygienic Papers Prepared from Virgin and Secondary Pulp by Electron Capture Gas Chromatographic Method

    Directory of Open Access Journals (Sweden)

    Behrouz Akbari-adergani

    2016-01-01

    Full Text Available In this study, residual amount of pentachlorophenol (PCP as the most important paper preservative, which is extremely hazardous pollutant, was determined in some tissue papers and napkins. Twenty-five samples of two producing hygienic paper factories prepared from virgin and secondary pulp were analyzed for the presence of trace amount of PCP. The analytical procedure involved direct extraction of PCP from hygienic paper and its determination by gas chromatography with electron capture detection. The statistical results for the analysis of all samples revealed that there were significant differences between mean of PCP in hygienic papers prepared from virgin and secondary pulp (P<0.05. This method gave recoveries of 86-98% for hygienic paper made from virgin pulp and 79-92% for hygienic paper made from secondary pulp. The limit of detection (LOD and limit of quantification (LOQ for PCP were 6.3 and 21.0 mg/kg, respectively. The analytical method has the requisite sensitivity, accuracy, precision and specificity to assay PCP in hygienic papers. This study demonstrates a concern with exposition to PCP considering that hygienic paper is largely consumed in the society.

  10. Gas chromatographic sulphur speciation in heavy crude oil using a modified standard D5623 method and microfluidic Deans switching.

    Science.gov (United States)

    Heshka, Nicole E; Choy, Joanne M; Chen, Jinwen

    2017-12-29

    A modification to American Society for Testing and Materials (ASTM) method D5623 is proposed to enable successful and repeatable analysis of heavy crude oil samples. A two-dimensional gas chromatography configuration was implemented, with separation of sulphur compounds occurring on two columns. A Deans switch is used to enable heart-cutting of volatile sulphur compounds onto a DB-Sulfur stationary phase, and separation occurs concurrently with the backflushing of the primary column. The use of a sulphur-selective detector increases selectivity, and 22 volatile sulphur species are quantified in less than 15min, which is almost half the time of the original ASTM method. Samples ranging from light distillation cuts to whole crudes (boiling from 100°C to >750°C) were analyzed with minimal sample preparation. The calculated limit of detection was 0.7mg/kg, repeatability was 3% relative standard deviation (RSD), and a linear range of 1-250mg/kg was obtained, with an R 2 value of 0.994 or better, depending on the compound. Crown Copyright © 2017. Published by Elsevier B.V. All rights reserved.

  11. 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.

  12. Capillary gas chromatographic separation of organic bases using a pH-adjusted basic water stationary phase.

    Science.gov (United States)

    Darko, Ernest; Thurbide, Kevin B

    2016-09-23

    The use of a pH-adjusted water stationary phase for analyzing organic bases in capillary gas chromatography (GC) is demonstrated. Through modifying the phase to typical values near pH 11.5, it is found that various organic bases are readily eluted and separated. Conversely, at the normal pH 7 operating level, they are not. Sodium hydroxide is found to be a much more stable base than ammonium hydroxide for altering the pH due to the higher volatility and evaporation of the latter. In the basic condition, such analytes are not ionized and are observed to produce good peak shapes even for injected masses down to about 20ng. By comparison, analyses on a conventional non-polar capillary GC column yield more peak tailing and only analyte masses of 1μg or higher are normally observed. Through carefully altering the pH, it is also found that the selectivity between analytes can be potentially further enhanced if their respective pKa values differ sufficiently. The analysis of different pharmaceutical and petroleum samples containing organic bases is demonstrated. Results indicate that this approach can potentially offer unique and beneficial selectivity in such analyses. Copyright © 2016 Elsevier B.V. All rights reserved.

  13. Determination of methyl mercury by aqueous phase Eehylation, followed by gas chromatographic separation with cold vapor atomic fluorescence detection

    Science.gov (United States)

    De Wild, John F.; Olsen, Mark L.; Olund, Shane D.

    2002-01-01

    A recent national sampling of streams in the United States revealed low methyl mercury concentrations in surface waters. The resulting median and mean concentrations, calculated from 104 samples, were 0.06 nanograms per liter (ng/L) and 0.15 ng/L, respectively. This level of methyl mercury in surface water in the United States has created a need for analytical techniques capable of detecting sub-nanogram per liter concentrations. In an attempt to create a U.S. Geological Survey approved method, the Wisconsin District Mercury Laboratory has adapted a distillation/ethylation/ gas-phase separation method with cold vapor atomic fluorescence spectroscopy detection for the determination of methyl mercury in filtered and unfiltered waters. This method is described in this report. Based on multiple analyses of surface water and ground-water samples, a method detection limit of 0.04 ng/L was established. Precision and accuracy were evaluated for the method using both spiked and unspiked ground-water and surface-water samples. The percent relative standard deviations ranged from 10.2 to 15.6 for all analyses at all concentrations. Average recoveries obtained for the spiked matrices ranged from 88.8 to 117 percent. The precision and accuracy ranges are within the acceptable method-performance limits. Considering the demonstrated detection limit, precision, and accuracy, the method is an effective means to quantify methyl mercury in waters at or below environmentally relevant concentrations

  14. Development of a gas-liquid chromatographic method for the analysis of fatty acid tryptamides in cocoa products.

    Science.gov (United States)

    Hug, Bernadette; Golay, Pierre-Alain; Giuffrida, Francesca; Dionisi, Fabiola; Destaillats, Frédéric

    2006-05-03

    The determination of the occurrence and level of cocoa shells in cocoa products and chocolate is an important analytical issue. The recent European Union directive on cocoa and chocolate products (2000/36/EC) has not retained the former limit of a maximum amount of 5% of cocoa shells in cocoa nibs (based on fat-free dry matter), previously authorized for the elaboration of cocoa products such as cocoa mass. In the present study, we report a reliable gas-liquid chromatography procedure suitable for the determination of the occurrence of cocoa shells in cocoa products by detection of fatty acid tryptamides (FATs). The precision of the method was evaluated by analyzing nine different samples (cocoa liquors with different ranges of shells) six times (replicate repeatability). The variations of the robust coefficient of variation of the repeatability demonstrated that FAT(C22), FAT(C24), and total FATs are good markers for the detection of shells in cocoa products. The trueness of the method was evaluated by determining the FAT content in two spiked matrices (cocoa liquors and cocoa shells) at different levels (from 1 to 50 mg/100 g). A good relation was found between the results obtained and the spiking (recovery varied between 90 and 130%), and the linearity range was established between 1 and 50 mg/100 g in cocoa products. For total FAT contents of cocoa liquor containing 5% shells, the measurement uncertainty allows us to conclude that FAT is equal to 4.01 +/- 0.8 mg/100 g. This validated method is perfectly suitable to determine shell contents in cocoa products using FAT(C22), FAT(C24), and total FATs as markers. The results also confirmed that cocoa shells contain FAT(C24) and FAT(C22) in a constant ratio of nearly 2:1.

  15. 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.

  16. 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

  17. Microfabricated gas chromatograph for on-site determinations of TCE in indoor air arising from vapor intrusion. 2. Spatial/temporal monitoring.

    Science.gov (United States)

    Kim, Sun Kyu; Burris, David R; Bryant-Genevier, Jonathan; Gorder, Kyle A; Dettenmaier, Erik M; Zellers, Edward T

    2012-06-05

    We demonstrate the use of two prototype Si-microfabricated gas chromatographs (μGC) for continuous, short-term measurements of indoor trichloroethylene (TCE) vapor concentrations related to the investigation of TCE vapor intrusion (VI) in two houses. In the first house, with documented TCE VI, temporal variations in TCE air concentrations were monitored continuously for up to 48 h near the primary VI entry location under different levels of induced differential pressure (relative to the subslab). Concentrations ranged from 0.23 to 27 ppb by volume (1.2-150 μg/m(3)), and concentration trends agreed closely with those determined from concurrent reference samples. The sensitivity and temporal resolution of the measurements were sufficiently high to detect transient fluctuations in concentration resulting from short-term changes in variables affecting the extent of VI. Spatial monitoring showed a decreasing TCE concentration gradient with increasing distance from the primary VI entry location. In the second house, with no TCE VI, spatial profiles derived from the μGC prototype data revealed an intentionally hidden source of TCE within a closet, demonstrating the capability for locating non-VI sources. Concentrations measured in this house ranged from 0.51 to 56 ppb (2.7-300 μg/m(3)), in good agreement with reference method values. This first field demonstration of μGC technology for automated, near-real-time, selective VOC monitoring at low- or subppb levels augurs well for its use in short- and long-term on-site analysis of indoor air in support of VI assessments.

  18. Determination of Trace Anions in Concentrated Hydrogen Peroxide by Direct Injection Ion Chromatography with Conductivity Detection after Pt-Catalyzed On-Line Decomposition

    International Nuclear Information System (INIS)

    Kim, Do Hee; Lee, Bo Kyung; Lee, Dong Soo

    1999-01-01

    A method has been developed for the determination of trace anion impurities in concentrated hydrogen peroxide. The method involves on-line decomposition of hydrogen peroxide, ion chromatographic separation and subsequent suppressed-type conductivity detection. H 2 O 2 is decomposed in Pt-catalyst filled Gore-Tex membrane tubing and the resulting aqueous solution containing analytes is introduced to the injection valve of an ion chromatograph for periodic determinations. The oxygen gas evolving within the membrane tubing escapes freely through the membrane wall causing no problem in ion chromatographic analysis. Decomposition efficiency is above 99.99% at a flow rate of 0.4mL/min for a 30% hydrogen peroxide concentration. Analytes are quantitatively retained. The analysis results for several brands of commercial hydrogen peroxides are reported

  19. Development of a Small, Inexpensive, and Field-deployable Gas Chromatograph for the Automated Collection, Separation, and Analysis of Gas-phase Organic Compounds

    Science.gov (United States)

    Skog, K.; Xiong, F.; Gentner, D. R.

    2017-12-01

    The identification and quantification of gas-phase organic compounds, like volatile organic compounds (VOCs), in the atmosphere relies on separation of complex mixtures and sensitive detection. Gas chromatography (GC) is widely applied, but relies on the need for high-purity compressed gases for separation and, often for detection. We have developed a low-cost, compact GC-based system for the collection and quantitative chemical speciation of complex mixtures of common atmospheric VOCs without the need for compressed high-purity gases or expensive detectors. We present results of lab and field testing against a commercially-available GC system. At optimized linear velocities challenging VOC pairs of similar volatility were resolved within 30 minutes, including n- and i-pentane; n-pentane and isoprene; and ethylbenzene and m/p-xylene. For 5-30 minute samples, we observe ppt-level detection limits for common VOCs such as benzene, toluene, ethylbenzene, xylenes, alpha-pinene, and limonene. We also present results of in-field use for VOC measurements. In all, this instrument is accurate, precise, small, and inexpensive (<$2500). Its lack of compressed gas cylinders make it ideal for field deployment and has been demonstrated to produce similar quality data to available GC technology.

  20. 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

  1. A modified commercial gas chromatograph for the continuous monitoring of the thermal degradation of sunflower oil and off-line solid phase extraction gas-chromatography-mass spectrometry characterization of released volatiles.

    Science.gov (United States)

    Ontañon, I; Sanz, J; Escudero, A; de Marcos, S; Ferreira, V; Galbán, J

    2015-04-03

    A homemade flow cell attached to a commercial Gas Chromatograph equipped with a Flame Ionization Detector (FID) has been designed for the continuous monitoring of volatile compounds released during heating edible oils. Analytical parameters such as mass of sample, temperature and flow rates have been optimized and the obtained results have been compared with the corresponding thermographs from standard TG systems. Results show that under optimum conditions, the profiles of volatiles released upon heating are comparable to the profiles of TG curves, suggesting that the FID based system could be an alternative to TGA. Additionally, volatiles have been retained in a Lichrolut EN(®) resin, eluted and analyzed by Gas Chromatography-Mass Spectrometry. In this case, forty five compounds have been identified (acids, alcohols, alkanes, aldehydes, ketones and furans) and compared with the FID signals, working both in air or nitrogen atmosphere. It has been concluded that the oxidative thermal degradation is prevented in the presence of a nitrogen atmosphere. Copyright © 2015 Elsevier B.V. All rights reserved.

  2. Improved Chromatographic Bioavailability Estimations

    National Research Council Canada - National Science Library

    Dorsey, John

    1996-01-01

    .... Since the inception of reversed phase liquid chromatography there have been many attempts to correlate chromatographic retention with bioavailability and the most often used bulk measure, the octanol...

  3. An aircraft gas chromatograph-mass spectrometer System for Organic Fast Identification Analysis (SOFIA): design, performance and a case study of Asian monsoon pollution outflow

    Science.gov (United States)

    Bourtsoukidis, Efstratios; Helleis, Frank; Tomsche, Laura; Fischer, Horst; Hofmann, Rolf; Lelieveld, Jos; Williams, Jonathan

    2017-12-01

    Volatile organic compounds (VOCs) are important for global air quality and oxidation processes in the troposphere. In addition to ground-based measurements, the chemical evolution of such species during transport can be studied by performing in situ airborne measurements. Generally, aircraft instrumentation needs to be sensitive, robust and sample at higher frequency than ground-based systems while their construction must comply with rigorous mechanical and electrical safety standards. Here, we present a new System for Organic Fast Identification Analysis (SOFIA), which is a custom-built fast gas chromatography-mass spectrometry (GC-MS) system with a time resolution of 2-3 min and the ability to quantify atmospheric mixing ratios of halocarbons (e.g. chloromethanes), hydrocarbons (e.g isoprene), oxygenated VOCs (acetone, propanal, butanone) and aromatics (e.g. benzene, toluene) from sub-ppt to ppb levels. The relatively high time resolution is the result of a novel cryogenic pre-concentration unit which rapidly cools (˜ 6 °C s-1) the sample enrichment traps to -140 °C, and a new chromatographic oven designed for rapid cooling rates (˜ 30 °C s-1) and subsequent thermal stabilization. SOFIA was installed in the High Altitude and Long Range Research Aircraft (HALO) for the Oxidation Mechanism Observations (OMO) campaign in August 2015, aimed at investigating the Asian monsoon pollution outflow in the tropical upper troposphere. In addition to a comprehensive instrument characterization we present an example monsoon plume crossing flight as a case study to demonstrate the instrument capability. Hydrocarbon, halocarbon and oxygenated VOC data from SOFIA are compared with mixing ratios of carbon monoxide (CO) and methane (CH4), used to define the pollution plume. By using excess (ExMR) and normalized excess mixing ratios (NEMRs) the pollution could be attributed to two air masses of distinctly different origin, identified by back-trajectory analysis. This work

  4. 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

  5. A laboratory flow reactor with gas particle separation and on-line MS/MS for product identification in atmospherically important reactions

    Directory of Open Access Journals (Sweden)

    J. F. Bennett

    2009-12-01

    Full Text Available A system to study the gas and particle phase products from gas phase hydrocarbon oxidation is described. It consists of a gas phase photochemical flow reactor followed by a diffusion membrane denuder to remove gases from the reacted products, or a filter to remove the particles. Chemical analysis is performed by an atmospheric pressure chemical ionization (APCI triple quadrupole mass spectrometer. A diffusion membrane denuder is shown to remove trace gases to below detectable limits so the particle phase can be studied. The system was tested by examining the products of the oxidation of m-xylene initiated by HO radicals. Dimethylphenol was observed in both the gas and particle phases although individual isomers could not be identified. Two furanone isomers, 5-methyl-2(3Hfuranone and 3-methyl-2(5Hfuranone were identified in the particulate phase, but the isobaric product 2,5 furandione was not observed. One isomer of dimethyl-nitrophenol was identified in the particle phase but not in the gas phase.

  6. Application of a 1,1,3,3-tetramethylguanidine (TMG)/MeOH-CO2 in situ derivatization procedure for the gas chromatographic characterization of the fatty acid profile in olive oil.

    Science.gov (United States)

    Saliu, F; Anzano, M; Franzetti, A

    2015-03-01

    1,1,3,3-Tetramethylguanidine (TMG), methanol and carbon dioxide were investigated as switchable polarity solvents (SPS) in the simultaneous derivatization and extraction of triacylglycerols for the gas chromatographic (GC) characterization of olive oil. Three commercial olive oils were used as test samples. Results of the developed method did not differ statistically from those provided by reference derivatization procedures. The transesterification reaction was carried out under a very mild condition, one step and in situ, and no particular matrix interferences were evidenced. The method represented the first example of the use of a switchable polarity mixture for the preparation of methyl ester derivatives of fatty acids (FAME).

  7. Argon/UF6 plasma exhaust gas reconstitution experiments using preheated fluorine and on-line diagnostics. [fissioning uranium plasma core reactor design

    Science.gov (United States)

    Roman, W. C.

    1979-01-01

    The feasibility of employing a flowing, high-temperature, pure fluorine/UF6 regeneration system to efficiently convert a large fraction of the effluent plasma exhaust back to pure UF6 was demonstrated. The custom built T.O.F. mass spectrometer sampling system permitted on-line measurements of the UF6 concentration at different locations in the exhaust system. Negligible amounts ( 100 ppm) of UF6 were detected in the axial bypass exhaust duct and the exhaust ducts downstream of the cryogenic trap system used to collect the UF6, thus verifying the overall system efficiency over a range of operating conditions. Use of a porous Monel duct as part of the exhaust duct system, including provision for injection of pure fluorine, provided a viable technique to eliminate uranium compound residue on the inside surface of the exhaust ducts. Typical uranium compound mass deposition per unit area of duct was 2 micron g/sq cm. This porous duct technique is directly applicable to future uranium compound transfer exhaust systems. Throughout these experiments, additional basic data on the corrosion aspects of hot, pressurized UF6/fluorine were also accumulated.

  8. Programmed temperature vaporizing injector to filter off disturbing high boiling and involatile material for on-line high performance liquid chromatography gas chromatography with on-column transfer.

    Science.gov (United States)

    Biedermann, Maurus; Grob, Koni

    2013-03-15

    Insertion of a programmed temperature vaporizing (PTV) injector under conditions of concurrent solvent recondensation (CSR) into the on-line HPLC-GC interface for on-column transfer (such as the retention gap technique with partially concurrent eluent evaporation) enables filtering off high boiling or involatile sample constituents by a desorption temperature adjusted to the required cut-off. Details of this technique were investigated and optimized. Memory effects, observed when transferred liquid was sucked backwards between the transfer line and the wall of the injector liner, can be kept low by a small purge flow rate through the transfer line at the end of the transfer and the release of the liquid through a narrow bore capillary kept away from the liner wall. The column entrance should be within the well heated zone of the injector to prevent losses of solute material retained on the liner wall during the splitless period. The desorption temperature must be maintained until an elevated oven temperature is reached to prevent peak broadening resulting of a cool inlet section in the bottom part of the injector. Copyright © 2013 Elsevier B.V. All rights reserved.

  9. Investigation of parameters affecting the online combination of supercritical fluid extraction with capillary gas chromatography

    NARCIS (Netherlands)

    Lou, X.W.; Janssen, J.G.M.; Cramers, C.A.M.G.

    1996-01-01

    Two different injectors, a split/splitless injector and a programmed temperature vaporizer (PTV) injector were investigated as the interface in on-line supercritical fluid extraction (SFE)-capillary gas chromatography (cGC). The parameters affecting the chromatographic peak shapes as well as the

  10. Potentiometric analytical microsystem based on the integration of a gas-diffusion step for on-line ammonium determination in water recycling processes in manned space missions.

    Science.gov (United States)

    Calvo-López, Antonio; Ymbern, Oriol; Puyol, Mar; Casalta, Joan Manel; Alonso-Chamarro, Julián

    2015-05-18

    The design, construction and evaluation of a versatile cyclic olefin copolymer (COC)-based continuous flow potentiometric microanalyzer to monitor the presence of ammonium ion in recycling water processes for future manned space missions is presented. The microsystem integrates microfluidics, a gas-diffusion module and a detection system in a single substrate. The gas-diffusion module was integrated by a hydrophobic polyvinylidene fluoride (PVDF) membrane. The potentiometric detection system is based on an all-solid state ammonium selective electrode and a screen-printed Ag/AgCl reference electrode. The analytical features provided by the analytical microsystem after the optimization process were a linear range from 0.15 to 500 mg L(-1) and a detection limit of 0.07 ± 0.01 mg L(-1). Nevertheless, the operational features can be easily adapted to other applications through the modification of the hydrodynamic variables of the microfluidic platform. Copyright © 2014 Elsevier B.V. All rights reserved.

  11. Isotope separations using chromatographic methods

    International Nuclear Information System (INIS)

    Leseticky, L.

    1985-01-01

    A survey is given of chromatographic separations of compounds only differing in isotope composition. Isotope effects on physical properties which allow chromatographic separation (vapour tension, adsorption heat, partition coefficient) are very small, with the exception of the simplest molecules. Therefore, separation factors only assume the value of several per cent. From this ensues the necessity of using columns which are specially and very carefully prepared and have a separation efficiency of the order of 10 4 theoretical plates. Briefly discussed is liquid chromatography on ion exchangers which with a varied degree of success was used for separating simple inorganic compounds or ions. Ion exchange chromatography of amino acids labelled with tritium, and chromatography of tritium labelled steroids also provided only a certain degree of separation. A detailed analysis is presented of gas chromatography separation of various deuterium and tritium labelled low-molecular compounds, to which a number of studies has been devoted in the literature. Very promising is the method of complexation gas chromatography based on the reversible formation of a complex of the ligand (the compound being separated) and the compound of the (transition) metal as the steady-state phase. (author)

  12. Chromatographic determination of the relative retention of isotopic species of oxygen in methanol and methan-d3-ol

    International Nuclear Information System (INIS)

    Pauls, R.E.; Mahle, N.H.; Shepard, A.T.; Gaw, J.C.; Rogers, L.B.

    1976-08-01

    A high-precision gas chromatograph was used in conjunction with a quadrupole mass filter and an on-line computer to study the fractionation of oxygen isotopes by Porapak T and glycerol in CH 3 OH and CD 3 OH as a function of temperature. Values of relative retention on the order of 1.002 compared favorably with results for the vapor pressure ratio obtained by classical means. Differences from unity were much smaller for the activity-coefficient ratio than for the vapor-pressure ratio. Differential thermodynamic data were also reported

  13. Simple setup for gas-phase H/D exchange mass spectrometry coupled to electron transfer dissociation and ion mobility for analysis of polypeptide structure on a liquid chromatographic time scale.

    Science.gov (United States)

    Mistarz, Ulrik H; Brown, Jeffery M; Haselmann, Kim F; Rand, Kasper D

    2014-12-02

    Gas-phase hydrogen/deuterium exchange (HDX) is a fast and sensitive, yet unharnessed analytical approach for providing information on the structural properties of biomolecules, in a complementary manner to mass analysis. Here, we describe a simple setup for ND3-mediated millisecond gas-phase HDX inside a mass spectrometer immediately after ESI (gas-phase HDX-MS) and show utility for studying the primary and higher-order structure of peptides and proteins. HDX was achieved by passing N2-gas through a container filled with aqueous deuterated ammonia reagent (ND3/D2O) and admitting the saturated gas immediately upstream or downstream of the primary skimmer cone. The approach was implemented on three commercially available mass spectrometers and required no or minor fully reversible reconfiguration of gas-inlets of the ion source. Results from gas-phase HDX-MS of peptides using the aqueous ND3/D2O as HDX reagent indicate that labeling is facilitated exclusively through gaseous ND3, yielding similar results to the infusion of purified ND3-gas, while circumventing the complications associated with the use of hazardous purified gases. Comparison of the solution-phase- and gas-phase deuterium uptake of Leu-Enkephalin and Glu-Fibrinopeptide B, confirmed that this gas-phase HDX-MS approach allows for labeling of sites (heteroatom-bound non-amide hydrogens located on side-chains, N-terminus and C-terminus) not accessed by classical solution-phase HDX-MS. The simple setup is compatible with liquid chromatography and a chip-based automated nanoESI interface, allowing for online gas-phase HDX-MS analysis of peptides and proteins separated on a liquid chromatographic time scale at increased throughput. Furthermore, online gas-phase HDX-MS could be performed in tandem with ion mobility separation or electron transfer dissociation, thus enabling multiple orthogonal analyses of the structural properties of peptides and proteins in a single automated LC-MS workflow.

  14. On-line filtering

    International Nuclear Information System (INIS)

    Verkerk, C.

    1978-01-01

    Present day electronic detectors used in high energy physics make it possible to obtain high event rates and it is likely that future experiments will face even higher data rates than at present. The complexity of the apparatus increases very rapidly with time and also the criteria for selecting desired events become more and more complex. So complex in fact that the fast trigger system cannot be designed to fully cope with it. The interesting events become thus contaminated with multitudes of uninteresting ones. To distinguish the 'good' events from the often overwhelming background of other events one has to resort to computing techniques. Normally this selection is made in the first part of the analysis of the events, analysis normally performed on a powerful scientific computer. This implies however that many uninteresting or background events have to be recorded during the experiment for subsequent analysis. A number of undesired consequences result; and these constitute a sufficient reason for trying to perform the selection at an earlier stage, in fact ideally before the events are recorded on magnetic tape. This early selection is called 'on-line filtering' and it is the topic of the present lectures. (Auth.)

  15. Chromatographic hydrogen isotope separation

    International Nuclear Information System (INIS)

    Aldridge, F.T.

    1983-01-01

    Intermetallic compounds with the CaCu5 type of crystal structure, particularly LaNiCo and CaNi5, exhibit high separation factors and fast equilibrium times and therefore are useful for packing a chromatographic hydrogen isotope separation column. The addition of an inert metal to dilute the hydride improves performance of the column. A large scale multi-stage chromatographic separation process run as a secondary process off a hydrogen feedstream from an industrial plant which uses large volumes of hydrogen can produce large quantities of heavy water at an effective cost for use in heavy water reactors

  16. Chromatographic hydrogen isotope separation

    International Nuclear Information System (INIS)

    Aldridge, F.T.

    1981-01-01

    Intermetallic compounds with the CaCu5 type of crystal structure , particularly LaNiCo and CaNi5, exhibit high separation factors and fast equilibrium times and therefore are useful for packing a chromatographic hydrogen isotope separation colum. The addition of an inert metal to dilute the hydride improves performance of the column. A large scale mutli-stage chromatographic separation process run as a secondary process off a hydrogen feedstream from an industrial plant which uses large volumes of hydrogen can produce large quantities of heavy water at an effective cost for use in heavy water reactors

  17. On line portal imaging

    International Nuclear Information System (INIS)

    Munro, Peter

    1997-01-01

    Purpose/Objective: The purpose of this presentation is to examine the various imaging devices that have been developed for portal imaging, describe some of the image registration methods that have been developed to determine geometric errors quantitatively, and discuss how portal imaging has been incorporated into clinical practice. Discussion: Verification of patient positioning has always been an important aspect of external beam radiation therapy. Over the past decade many portal imaging devices have been developed by individual investigators and most accelerator manufacturers now offer 'on-line' portal imaging systems. The commercial devices include T.V. camera-based systems, liquid ionisation chamber systems, and shortly, flat panel systems. The characteristics of these imaging systems will be discussed. In addition, other approaches such as the use of kilovoltage x-ray sources, video monitoring, and ultrasound have been proposed for improving patient positioning. Some of the advantages of these approaches will be discussed. One of the major advantages of on-line portal imaging is that many quantitative techniques have been developed to detect errors in patient positioning. The general approach is to register anatomic structures on a portal image with the same structures on a digitized simulator film. Once the anatomic structures have been registered, any discrepancies in the position of the patient can be identified. One problem is finding a common frame of reference for the simulator and portal images, since the location of the radiation field within the pixel matrix may differ for the two images. As a result, a common frame of reference has to be established before the anatomic structures in the images can be registered - generally by registering radiation field edges identified in the simulator and portal images. In addition, distortions in patient geometry or rotations out of the image plane can confound the image registration techniques. Despite the

  18. On line portal imaging

    International Nuclear Information System (INIS)

    Munro, Peter

    1996-01-01

    Purpose/Objective: The purpose of this presentation is to examine the various imaging devices that have been developed for portal imaging; describe some of the image registration methods that have been developed to determine geometric errors quantitatively; discuss some of the ways that portal imaging has been incorporated into routine clinical practice; describe quality assurance procedures for these devices, and discuss the use of portal imaging devices for dosimetry applications. Discussion: Verification of patient positioning has always been an important aspect of external beam radiation therapy. Over the past decade many portal imaging devices have been developed by individual investigators and most accelerator manufacturers now offer 'on-line' portal imaging systems. The commercial devices can be classified into three categories: T.V. camera-based systems, liquid ionisation chamber systems, and amorphous silicon systems. Many factors influence the quality of images generated by these portal imaging systems. These include factors which are unavoidable (e.g., low subject contrast), factors which depend upon the individual imaging device forming the image (e.g., dose utilisation, spatial resolution) as well as factors which depend upon the characteristics of the linear accelerator irradiating the imaging system (x-ray source size, image magnification). The characteristics of individual imaging systems, such as spatial resolution, temporal response, and quantum utilisation will be discussed. One of the major advantages of on-line portal imaging is that many quantitative techniques have been developed to detect errors in patient positioning. The general approach is to register anatomic structures on a portal image with the same structures on a digitized simulator film. Once the anatomic structures have been registered, any discrepancies in the position of the patient can be identified. However, the task is not nearly as straight-forward as it sounds. One problem

  19. On line portal imaging

    International Nuclear Information System (INIS)

    Munro, Peter

    1995-01-01

    Purpose/Objective: The purpose of this presentation is to review the physics of imaging with high energy x-ray beams; examine the various imaging devices that have been developed for portal imaging; describe some of the image registration methods that have been developed to determine errors in patient positioning quantitatively; and discuss some of the ways that portal imaging has been incorporated into routine clinical practice. Verification of patient positioning has always been an important aspect of external beam radiation therapy. Checks of patient positioning have generally been done with film, however, film suffers from a number of drawbacks, such as poor image display and delays due to film development. Over the past decade many portal imaging devices have been developed by individual investigators and most accelerator manufacturers now offer 'on-line' portal imaging systems, which are intended to overcome the limitations of portal films. The commercial devices can be classified into three categories: T.V. camera-based systems, liquid ionisation chamber systems, and amorphous silicon systems. Many factors influence the quality of images generated by these portal imaging systems. These include factors which are unavoidable (e.g., low subject contrast), factors which depend upon the individual imaging device forming the image (e.g., dose utilisation, spatial resolution) as well as factors which depend upon the characteristics of the linear accelerator irradiating the imaging system (x-ray source size, image magnification). The fundamental factors which limit image quality and the characteristics of individual imaging systems, such as spatial resolution, temporal response, and quantum utilisation will be discussed. One of the major advantages of on-line portal imaging is that many quantitative techniques have been developed to detect errors in patient positioning. The general approach is to register anatomic structures on a portal image with the same

  20. Quantification of extra virgin olive oil in dressing and edible oil blends using the representative TMS-4,4'-desmethylsterols gas-chromatographic-normalized fingerprint.

    Science.gov (United States)

    Pérez-Castaño, Estefanía; Sánchez-Viñas, Mercedes; Gázquez-Evangelista, Domingo; Bagur-González, M Gracia

    2018-01-15

    This paper describes and discusses the application of trimethylsilyl (TMS)-4,4'-desmethylsterols derivatives chromatographic fingerprints (obtained from an off-line HPLC-GC-FID system) for the quantification of extra virgin olive oil in commercial vinaigrettes, dressing salad and in-house reference materials (i-HRM) using two different Partial Least Square-Regression (PLS-R) multivariate quantification methods. Different data pre-processing strategies were carried out being the whole one: (i) internal normalization; (ii) sampling based on The Nyquist Theorem; (iii) internal correlation optimized shifting, icoshift; (iv) baseline correction (v) mean centering and (vi) selecting zones. The first model corresponds to a matrix of dimensions 'n×911' variables and the second one to a matrix of dimensions 'n×431' variables. It has to be highlighted that the proposed two PLS-R models allow the quantification of extra virgin olive oil in binary blends, foodstuffs, etc., when the provided percentage is greater than 25%. Copyright © 2017 Elsevier Ltd. All rights reserved.

  1. A custom on-line ultrasonic gas mixture analyzer with simultaneous flowmetry developed for use in the LHC-ATLAS experiment, with wide application in high and low flow gas delivery systems

    International Nuclear Information System (INIS)

    Bates, R.; Bitadze, A.; Battistin, M.; Berry, S.; Berthoud, J.; Bonneau, P.; Botelho- Direito, J.; Bozza, G.; Crespo-Lopez, O.; DiGirolamo, B.; Da Riva, E.; Favre, G.; Godlewski, J.; Lombard, D.; Zwalinski, L.; Bousson, N.; Hallewell, G.; Mathieu, M.; Rozanov, A.; Boyd, G.; Deterre, C.; Doubek, M.; Vacek, V.; Vitek, M.; Degeorge, C.; Katunin, S.; Langevin, N.; McMahon, S.; Nagai, K.; Robinson, D.; Rossi, C.

    2013-06-01

    We describe a combined ultrasonic instrument for continuous gas flow measurement and simultaneous real-time binary gas mixture analysis. In the instrument, sound bursts are transmitted in opposite directions, which may be aligned with the gas flow path or at an angle to it, the latter configuration being the best adapted to high flow rates. Custom electronics based on Microchip R dsPIC and ADuC847 micro-controllers transmits 50 kHz ultrasound pulses and measures transit times in the two directions together with the process gas temperature and pressure. The combined flow measurement and mixture analysis algorithm exploits the phenomenon whereby the sound velocity in a binary gas mixture at known temperature and pressure is a unique function of the molar concentration of the two components. The instrument is central to a possible upgrade to the present ATLAS silicon tracker cooling system in which octafluoro-propane (C 3 F 8 ) evaporative cooling fluid would be replaced by a blend containing up to 25% hexafluoro-ethane (C 2 F 6 ). Such a blend will allow a lower evaporation temperature and will afford the tracker silicon substrates a better safety margin against leakage current-induced thermal runaway caused by cumulative radiation damage as the luminosity profile at the CERN Large Hadron Collider (LHC) increases. The instrument has been developed in two geometries following computational fluid dynamics studies of various mechanical layouts. An instrument with 45 crossing angle has been built in stainless steel and installed for commissioning in the ATLAS silicon tracker evaporative fluorocarbon cooling system. It can be used in gas flows up to 20000 l.min -1 , and has demonstrated a flow resolution of 2.3% of full scale for linear flow velocities up to 10 m.s-1 in preliminary studies with air. Other instruments are currently used to detect low levels of C 3 F 8 vapour leaking into the N 2 environmental gas surrounding the ATLAS silicon tracker. Gas from several

  2. Chromatographic monitoring procedures in laboratory practice

    Energy Technology Data Exchange (ETDEWEB)

    Kaplina, E G; Belova, O I; Lasunina, N A

    1976-01-01

    The Moscow Coke and Chemical Works consist of three plants in combination, viz., the coking plant, the synthetic ammonia plant using coke-oven-gas hydrogen and the oxygen plant. The plant requirements include daily analyses not only of the coke-oven gas but also of a rich gas and an ethylene fraction. The analyses are carried out in VTI-2 apparatus. The analytical data are used to calculate the calorific values and densities of the gases. The time requirements are very considerable and the laboratory has long been engaged in developing and introducing chromatographic procedures for the major constituents of coke-oven gas, rich gas and ethylene fraction. The procedure developed for the coke-oven and rich gases uses two parallel columns, one packed with molecular sieves and the other with grade KSM silica gel. Hydrogen was determined with argon as the carrier gas, and all other constituents with helium. The procedure was time-consuming and complicated. An attempt was made to separate the gases in an LKhM-7a chromatograph with a programme-controlled 50 to 250/sup 0/C heating cycle, but the procedure still had a number of serious defects and could not be recommended for regular quality control. The final variant involved two parallel columns and a procedure based on that in GOST 14920 (''Dry gas. Proximate analysis''). The chromatograph was a type KhL-69 with a 6-way cock in the gas line so that each of the columns could be brought on stream in succession. The analytical column packings were zeolite (in a 2 m column) and diatomaceous brick with 25% n-hexadecane (in a 6 m column).

  3. Development of a method based on on-line reversed phase liquid chromatography and gas chromatography coupled by means of an adsorption-desorption interface for the analysis of selected chiral volatile compounds in methyl jasmonate treated strawberries.

    Science.gov (United States)

    de la Peña Moreno, Fernando; Blanch, Gracia Patricia; Flores, Gema; Ruiz Del Castillo, Maria Luisa

    2010-02-12

    A method based on the use of the through oven transfer adsorption-desorption (TOTAD) interface in on-line coupling between reversed phase liquid chromatography and gas chromatography (RPLC-GC) for the determination of chiral volatile compounds was developed. In particular, the method was applied to the study of the influence of methyl jasmonate (MJ) treatment on the production and enantiomeric composition of selected aroma compounds in strawberry. The compounds studied were ethyl 2-methylbutanoate, linalool and 4-hydroxy-2,5-dimethyl-3(2H)-furanone (i.e. furaneol), which were examined on days 3, 6 and 9 after treatment. The method developed resulted in relative standard deviations (RSDs) of 21.6%, 8.1% and 9.8% and limits of detection (LD) of 0.04, 0.07 and 0.02mg/l for ethyl 2-methylbutanoate, linalool and furaneol, respectively. The application of the RPLC-TOTAD-GC method allowed higher levels of ethyl 2-methylbutanoate, linalool and furaneol to be detected, particularly after 9 days of treatment. Besides, MJ demonstrated to affect the enantiomeric distribution of ethyl 2-methylbutanoate. On the contrary, the enantiomeric composition of linalool and furaneol kept constant in both control and MJ-treated strawberries throughout the study. These results are discussed. Copyright 2009 Elsevier B.V. All rights reserved.

  4. Microwave assisted saponification (MAS) followed by on-line liquid chromatography (LC)-gas chromatography (GC) for high-throughput and high-sensitivity determination of mineral oil in different cereal-based foodstuffs.

    Science.gov (United States)

    Moret, Sabrina; Scolaro, Marianna; Barp, Laura; Purcaro, Giorgia; Conte, Lanfranco S

    2016-04-01

    A high throughput, high-sensitivity procedure, involving simultaneous microwave-assisted extraction (MAS) and unsaponifiable extraction, followed by on-line liquid chromatography (LC)-gas chromatography (GC), has been optimised for rapid and efficient extraction and analytical determination of mineral oil saturated hydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH) in cereal-based products of different composition. MAS has the advantage of eliminating fat before LC-GC analysis, allowing an increase in the amount of sample extract injected, and hence in sensitivity. The proposed method gave practically quantitative recoveries and good repeatability. Among the different cereal-based products analysed (dry semolina and egg pasta, bread, biscuits, and cakes), egg pasta packed in direct contact with recycled paperboard had on average the highest total MOSH level (15.9 mg kg(-1)), followed by cakes (10.4 mg kg(-1)) and bread (7.5 mg kg(-1)). About 50% of the pasta and bread samples and 20% of the biscuits and cake samples had detectable MOAH amounts. The highest concentrations were found in an egg pasta in direct contact with recycled paperboard (3.6 mg kg(-1)) and in a milk bread (3.6 mg kg(-1)). Copyright © 2015 Elsevier Ltd. All rights reserved.

  5. A study of the adsorption activities of silanol surface structures on a fused silica model substrate by combining 29Si CP MAS NMR and inverse gas chromatographic data

    NARCIS (Netherlands)

    Scholten, A.B.; Janssen, J.G.M.; Haan, de J.W.; Cramers, C.A.

    1994-01-01

    The possibilities of inverse gas-solid chromatog. (IGC) in obtaining chromatog. data on fumed silica were examd. Aerosil A-200, a fused silica model substrate in 29Si NMR anal., was trimethylsilylated to different degrees. IGC was used to vary reproducibly det. the free specific energies of

  6. Gas Chromatographic-Ion Trap Mass Spectrometric Analysis of Volatile Organic Compounds by Ion-Molecule Reactions Using the Electron-Deficient Reagent Ion CCl{3/+}

    Science.gov (United States)

    Wang, Cheng-Zhong; Su, Yue; Wang, Hao-Yang; Guo, Yin-Long

    2011-10-01

    When using tetrachloromethane as the reagent gas in gas chromatography-ion trap mass spectrometry equipped with hybrid ionization source, the cation CCl{3/+} was generated in high abundance and further gas-phase experiments showed that such an electron-deficient reagent ion CCl{3/+} could undergo interesting ion-molecule reactions with various volatile organic compounds, which not only present some informative gas-phase reactions, but also facilitate qualitative analysis of diverse volatile compounds by providing unique mass spectral data that are characteristic of particular chemical structures. The ion-molecule reactions of the reagent ion CCl{3/+} with different types of compounds were studied, and results showed that such reactions could give rise to structurally diagnostic ions, such as [M + CCl3 - HCl]+ for aromatic hydrocarbons, [M - OH]+ for saturated cyclic ether, ketone, and alcoholic compounds, [M - H]+ ion for monoterpenes, M·+ for sesquiterpenes, [M - CH3CO]+ for esters, as well as the further fragment ions. The mechanisms of ion-molecule reactions of aromatic hydrocarbons, aliphatic ketones and alcoholic compounds with the reagent ion CCl{3/+} were investigated and proposed according to the information provided by MS/MS experiments and theoretical calculations. Then, this method was applied to study volatile organic compounds in Dendranthema indicum var. aromaticum and 20 compounds, including monoterpenes and their oxygen-containing derivatives, aromatic hydrocarbon and sesquiterpenes were identified using such ion-molecule reactions. This study offers a perspective and an alternative tool for the analysis and identification of various volatile compounds.

  7. At-line gas chromatographic-mass spectrometric analysis of fatty acid profiles of green microalgae using a direct thermal desorption interface

    NARCIS (Netherlands)

    Blokker, P.; Pel, R.; Akoto, L.; Udo, A.; Brinkman, U.A.Th.; Vreuls, R.J.J.

    2002-01-01

    Thermally assisted hydrolysis and methylation¯gas chromatography (THM¯GC) is an important tool to analyse fatty acid in complex matrices. Since THM¯GC has major drawbacks such as isomerisation when applied to fatty acids in natural matrices, a direct thermal desorption (DTD) interface and an

  8. Analysis and chromatographic purification of eicosanoids multiply labeled by tritium

    International Nuclear Information System (INIS)

    Shevchenko, V.P.; Nagaev, I.Yu.; Myasoedov, N.F.

    1989-01-01

    We show the possibility of analysis and chromatographic purification of eicosanoids triply labeled by tritium. The described methods allow us to isolate chromatographically pure products obtained by selective hydrogenatin, chemical, and enzyme methods, with radiochemical purity at least 95-97%. The following methods are used to analyze the reaction mixtures and to isolate the tritium-labeled eicosanoids: gas-liquid chromatography, high-efficiency liquid chromatography, and thin-layer chromatography on supports impregnated with silver nitrate

  9. Volatilizable Biogenic Organic Compounds (VBOCs with two dimensional Gas Chromatography-Time of Flight Mass Spectrometry (GC × GC-TOFMS: sampling methods, VBOC complexity, and chromatographic retention data

    Directory of Open Access Journals (Sweden)

    C. Chen

    2012-02-01

    Full Text Available Two dimensional gas chromatography (GC × GC with detection by time-of-flight mass spectrometry (TOFMS was applied in the rapid analysis of air samples containing highly complex mixtures of volatilizable biogenic organic compounds (VBOCs. VBOC analytical methodologies are briefly reviewed, and optimal conditions are discussed for sampling with both adsorption/thermal desorption (ATD cartridges and solid-phase microextraction (SPME fibers. Air samples containing VBOC emissions from leaves of two tree species (Cedrus atlantica and Calycolpus moritzianus were obtained by both ATD and SPME. The optimized gas chromatographic conditions utilized a 45 m, 0.25 mm I.D. low-polarity primary column (DB-VRX, 1.4 μm film and a 1.5 m, 0.25 mm I.D. polar secondary column (StabilwaxTM, 0.25 μm film. Excellent separation was achieved in a 36 min temperature programmed GC × GC chromatogram. Thousands of VBOC peaks were present in the sample chromatograms; hundreds of tentative identifications by NIST mass spectral matching are provided. Very few of the tentatively identified compounds are currently available as authentic standards. Minimum detection limit values for a 5 l ATD sample were 3.5 pptv (10 ng m−3 for isoprene, methyl vinyl ketone, and methacrolein, and ~1.5 pptv (~10 ng m−3 for monoterpenes and sesquiterpenes. Kovats-type chromatographic retention index values on the primary column and relative retention time values on the secondary column are provided for 21 standard compounds and for 417 tentatively identified VBOCs. 19 of the 21 authentic standard compounds were found in one of the Cedrus atlantica SPME samples. In addition, easily quantifiable levels of at least 13 sesquiterpenes were found in an ATD sample obtained from a branch enclosure of Calycolpus moritzianus. Overall, the results obtained via GC × GC-TOFMS highlight an extreme, and largely uncharacterized diversity of VBOCs, consistent with the hypothesis that sesquiterpenes and

  10. Volatilizable Biogenic Organic Compounds (VBOCs) with two dimensional Gas Chromatography-Time of Flight Mass Spectrometry (GC × GC-TOFMS): sampling methods, VBOC complexity, and chromatographic retention data

    Science.gov (United States)

    Pankow, J. F.; Luo, W.; Melnychenko, A. N.; Barsanti, K. C.; Isabelle, L. M.; Chen, C.; Guenther, A. B.; Rosenstiel, T. N.

    2012-02-01

    Two dimensional gas chromatography (GC × GC) with detection by time-of-flight mass spectrometry (TOFMS) was applied in the rapid analysis of air samples containing highly complex mixtures of volatilizable biogenic organic compounds (VBOCs). VBOC analytical methodologies are briefly reviewed, and optimal conditions are discussed for sampling with both adsorption/thermal desorption (ATD) cartridges and solid-phase microextraction (SPME) fibers. Air samples containing VBOC emissions from leaves of two tree species (Cedrus atlantica and Calycolpus moritzianus) were obtained by both ATD and SPME. The optimized gas chromatographic conditions utilized a 45 m, 0.25 mm I.D. low-polarity primary column (DB-VRX, 1.4 μm film) and a 1.5 m, 0.25 mm I.D. polar secondary column (StabilwaxTM, 0.25 μm film). Excellent separation was achieved in a 36 min temperature programmed GC × GC chromatogram. Thousands of VBOC peaks were present in the sample chromatograms; hundreds of tentative identifications by NIST mass spectral matching are provided. Very few of the tentatively identified compounds are currently available as authentic standards. Minimum detection limit values for a 5 l ATD sample were 3.5 pptv (10 ng m-3) for isoprene, methyl vinyl ketone, and methacrolein, and ~1.5 pptv (~10 ng m-3) for monoterpenes and sesquiterpenes. Kovats-type chromatographic retention index values on the primary column and relative retention time values on the secondary column are provided for 21 standard compounds and for 417 tentatively identified VBOCs. 19 of the 21 authentic standard compounds were found in one of the Cedrus atlantica SPME samples. In addition, easily quantifiable levels of at least 13 sesquiterpenes were found in an ATD sample obtained from a branch enclosure of Calycolpus moritzianus. Overall, the results obtained via GC × GC-TOFMS highlight an extreme, and largely uncharacterized diversity of VBOCs, consistent with the hypothesis that sesquiterpenes and other compounds

  11. On line ion chromatography for the in situ characterization of the Callovo-Oxfordian pore water composition

    International Nuclear Information System (INIS)

    Lundy, M.; Vinsot, A.

    2010-01-01

    Document available in extended abstract form only. Since 1994, Andra has been studying the feasibility of a high-level long-lived radioactive waste disposal in the Callovo-Oxfordian formation. In order to improve the knowledge on the pore water composition, the PAC experiment has been conducted since 2005 in the Meuse/Haute-Marne Underground Research Laboratory. One of the experimental principles combined a gas equilibration test and the collection of water samples in the borehole named PAC1002. In October 2006, an ion chromatograph was installed to perform on line analysis of the sampled water. Six cations and seven anions were measured: lithium, sodium, potassium, magnesium, calcium, strontium, fluoride, chloride, bromide, iodide, sulfate, acetate and formate. This work presents the characteristics of the analytical equipment and the results obtained from the on line analysis of the sampled water. These results were compared with laboratory analyses which were performed by Hydroisotop GmbH. The experimental set up included a water sampling module which was connected to the borehole and to the ion chromatograph with inert PEEK lines. The water sampling module made it possible to collect the seepage water produced by the formation in 9-mL PEEK syringes without contact with the atmosphere. When a syringe was full, the collected water was immediately sent to a Metrohm 811 Online Ion Chromatograph and a programmed sample sequence was activated. The two-channel chromatograph allowed the simultaneous determination of cations (eluent: 4 mM HNO 3 , column: Metrosep C3) and anions (eluent: 3.6 mM Na 2 CO 3 , column: Metrosep A Supp 7). In addition, ten individual sample streams made it possible to execute inline calibrations and to analyse one or two certified control solutions. 200 workable analyses were obtained. The results showed a very good concordance of the on line and laboratory measurements for the following major and trace species: calcium, magnesium, sulfate

  12. Analysis of carbonyl compounds via headspace solid-phase microextraction with on-fiber derivatization and gas chromatographic-ion trap tandem mass spectrometric determination of their O-(2,3,4,5,6-pentafluorobenzyl)oxime derivatives

    Energy Technology Data Exchange (ETDEWEB)

    Schmarr, Hans-Georg [Dienstleistungszentrum Laendlicher Raum (DLR) Rheinpfalz, Breitenweg 71, D-67435 Neustadt an der Weinstrasse (Germany)], E-mail: hans-georg.schmarr@dlr.rlp.de; Potouridis, Theodoros; Ganss, Sebastian; Sang, Wei; Koepp, Benedikt; Bokuz, Ursula; Fischer, Ulrich [Dienstleistungszentrum Laendlicher Raum (DLR) Rheinpfalz, Breitenweg 71, D-67435 Neustadt an der Weinstrasse (Germany)

    2008-06-09

    An improved method for the analysis of carbonyls is described utilizing a headspace solid-phase microextraction (HS-SPME) step and on-fiber derivatization with O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine (PFBHA) hydrochloride. Thermal desorption of the oxime derivatives formed on the fiber is followed by gas chromatographic separation coupled to an ion trap tandem mass spectrometer (GC-ITMS). Selecting specific fragment ions within the electron ionization (EI{sup +}) mass spectra of these oxime derivatives as precursor ions for MS-MS fragmentation provides a suitable method for the target analysis of individual carbonyl classes, such as alkanals, (E)-2-alkenals, (E,E)-2,4-alkadienals, and others. Retention indices on polar as well as on apolar stationary phases along with EI{sup +} mass spectra patterns are presented for a large set of oxime derivatives, giving valuable information needed for unambiguous assignment of substances in complex sample matrices. The fast sample preparation and derivatization step via HS-SPME can be automated and is applicable to a variety of biological samples and foodstuffs, allowing rapid and sensitive screening analyses of important aldehydic biomarkers and aroma active compounds.

  13. Use of a hand-portable gas chromatograph-toroidal ion trap mass spectrometer for self-chemical ionization identification of degradation products related to O-ethyl S-(2-diisopropylaminoethyl) methyl phosphonothiolate (VX)

    Energy Technology Data Exchange (ETDEWEB)

    Smith, Philip A., E-mail: Smith.Philip.A@dol.gov [Uniformed Services University of the Health Sciences, Department of Preventive Medicine and Biometrics, 4301 Jones Bridge Road, Bethesda, MD, 20814 (United States); Lepage, Carmela R. Jackson [Defence R and D Canada - Suffield, Box 400, Station Main, Medicine Hat, Alberta, T1A 8K6 (Canada); Savage, Paul B. [Brigham Young University, Department of Chemistry and Biochemistry, Provo, UT, 84602 (United States); Bowerbank, Christopher R.; Lee, Edgar D. [Torion Technologies Inc., 796 East Utah Valley Drive, Suite 200, American Fork, UT, 84003 (United States); Lukacs, Michael J. [Defence R and D Canada - Suffield, Box 400, Station Main, Medicine Hat, Alberta, T1A 8K6 (Canada)

    2011-04-01

    The chemical warfare agent O-ethyl S-(2-diisopropylaminoethyl) methyl phosphonothiolate (VX) and many related degradation products produce poorly diagnostic electron ionization (EI) mass spectra by transmission quadrupole mass spectrometry. Thus, chemical ionization (CI) is often used for these analytes. In this work, pseudomolecular ([M+H]{sup +}) ion formation from self-chemical ionization (self-CI) was examined for four VX degradation products containing the diisopropylamine functional group. A person-portable toroidal ion trap mass spectrometer with a gas chromatographic inlet was used with EI, and both fixed-duration and feedback-controlled ionization time. With feedback-controlled ionization, ion cooling (reaction) times and ion formation target values were varied. Evidence for protonation of analytes was observed under all conditions, except for the largest analyte, bis(diisopropylaminoethyl)disulfide which yielded [M+H]{sup +} ions only with increased fixed ionization or ion cooling times. Analysis of triethylamine-d{sub 15} provided evidence that [M+H]{sup +} production was likely due to self-CI. Analysis of a degraded VX sample where lengthened ion storage and feedback-controlled ionization time were used resulted in detection of [M+H]{sup +} ions for VX and several relevant degradation products. Dimer ions were also observed for two phosphonate compounds detected in this sample.

  14. Use of a hand-portable gas chromatograph-toroidal ion trap mass spectrometer for self-chemical ionization identification of degradation products related to O-ethyl S-(2-diisopropylaminoethyl) methyl phosphonothiolate (VX)

    International Nuclear Information System (INIS)

    Smith, Philip A.; Lepage, Carmela R. Jackson; Savage, Paul B.; Bowerbank, Christopher R.; Lee, Edgar D.; Lukacs, Michael J.

    2011-01-01

    The chemical warfare agent O-ethyl S-(2-diisopropylaminoethyl) methyl phosphonothiolate (VX) and many related degradation products produce poorly diagnostic electron ionization (EI) mass spectra by transmission quadrupole mass spectrometry. Thus, chemical ionization (CI) is often used for these analytes. In this work, pseudomolecular ([M+H] + ) ion formation from self-chemical ionization (self-CI) was examined for four VX degradation products containing the diisopropylamine functional group. A person-portable toroidal ion trap mass spectrometer with a gas chromatographic inlet was used with EI, and both fixed-duration and feedback-controlled ionization time. With feedback-controlled ionization, ion cooling (reaction) times and ion formation target values were varied. Evidence for protonation of analytes was observed under all conditions, except for the largest analyte, bis(diisopropylaminoethyl)disulfide which yielded [M+H] + ions only with increased fixed ionization or ion cooling times. Analysis of triethylamine-d 15 provided evidence that [M+H] + production was likely due to self-CI. Analysis of a degraded VX sample where lengthened ion storage and feedback-controlled ionization time were used resulted in detection of [M+H] + ions for VX and several relevant degradation products. Dimer ions were also observed for two phosphonate compounds detected in this sample.

  15. Analytical Method Development and Validation for the Quantification of Acetone and Isopropyl Alcohol in the Tartaric Acid Base Pellets of Dipyridamole Modified Release Capsules by Using Headspace Gas Chromatographic Technique

    Directory of Open Access Journals (Sweden)

    Sriram Valavala

    2018-01-01

    Full Text Available A simple, sensitive, accurate, robust headspace gas chromatographic method was developed for the quantitative determination of acetone and isopropyl alcohol in tartaric acid-based pellets of dipyridamole modified release capsules. The residual solvents acetone and isopropyl alcohol were used in the manufacturing process of the tartaric acid-based pellets of dipyridamole modified release capsules by considering the solubility of the dipyridamole and excipients in the different manufacturing stages. The method was developed and optimized by using fused silica DB-624 (30 m × 0.32 mm × 1.8 µm column with the flame ionization detector. The method validation was carried out with regard to the guidelines for validation of analytical procedures Q2 demanded by the International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH. All the validation characteristics were meeting the acceptance criteria. Hence, the developed and validated method can be applied for the intended routine analysis.

  16. A Sensitive Method Approach for Chromatographic Analysis of Gas Streams in Separation Processes Based on Columns Packed with an Adsorbent Material

    Directory of Open Access Journals (Sweden)

    I. A. A. C. Esteves

    2016-01-01

    Full Text Available A sensitive method was developed and experimentally validated for the in-line analysis and quantification of gaseous feed and product streams of separation processes under research and development based on column chromatography. The analysis uses a specific mass spectrometry method coupled to engineering processes, such as Pressure Swing Adsorption (PSA and Simulated Moving Bed (SMB, which are examples of popular continuous separation technologies that can be used in applications such as natural gas and biogas purifications or carbon dioxide sequestration. These processes employ column adsorption equilibria on adsorbent materials, thus requiring real-time gas stream composition quantification. For this assay, an internal standard is assumed and a single-point calibration is used in a simple mixture-specific algorithm. The accuracy of the method was found to be between 0.01% and 0.25% (-mol for mixtures of CO2, CH4, and N2, tested as case-studies. This makes the method feasible for streams with quality control levels that can be used as a standard monitoring and analyzing procedure.

  17. Ionic liquid-based single-drop microextraction/gas chromatographic/mass spectrometric determination of benzene, toluene, ethylbenzene and xylene isomers in waters.

    Science.gov (United States)

    Aguilera-Herrador, Eva; Lucena, Rafael; Cárdenas, Soledad; Valcárcel, Miguel

    2008-08-01

    The direct coupling between ionic liquid-based single-drop microextraction and gas chromatography/mass spectrometry is proposed for the rapid and simple determination of benzene, toluene, ethylbenzene and xylenes isomers (BTEX) in water samples. The extraction procedure exploits not only the high affinity of the selected ionic liquid (1-methyl-3-octyl-imidazolium hexaflourophosphate) to these aromatic compounds but also its special properties like viscosity, low vapour pressure and immiscibility with water. All the variables involved in the extraction process have been studied in depth. The developed method allows the determination of these single-ring compounds in water under the reference concentration level fixed by the international legislation. In this case, limits of detection were in the range 20 ng L(-1) (obtained for benzene) and 91 ng L(-1) (for o-xylene). The repeatability of the proposed method, expressed as RSD (n=5), varied between 3.0% (o-xylene) and 5.2% (toluene).

  18. A novel multiple headspace extraction gas chromatographic method for measuring the diffusion coefficient of methanol in water and in olive oil.

    Science.gov (United States)

    Zhang, Chun-Yun; Chai, Xin-Sheng

    2015-03-13

    A novel method for the determination of the diffusion coefficient (D) of methanol in water and olive oil has been developed. Based on multiple headspace extraction gas chromatography (MHE-GC), the methanol released from the liquid sample of interest in a closed sample vial was determined in a stepwise fashion. A theoretical model was derived to establish the relationship between the diffusion coefficient and the GC signals from MHE-GC measurements. The results showed that the present method has an excellent precision (RSDwater and olive oil, when compared with data reported in the literature. The present method is simple and practical and can be a valuable tool for the determination of the diffusion coefficient of volatile analyte(s) into food simulants from food and beverage packaging material, both in research studies and in actual applications. Copyright © 2015 Elsevier B.V. All rights reserved.

  19. 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.

  20. Monolithic silica spin column extraction and simultaneous derivatization of amphetamines and 3,4-methylenedioxyamphetamines in human urine for gas chromatographic-mass spectrometric detection

    International Nuclear Information System (INIS)

    Nakamoto, Akihiro; Nishida, Manami; Saito, Takeshi; Kishiyama, Izumi; Miyazaki, Shota; Murakami, Katsunori; Nagao, Masataka; Namura, Akira

    2010-01-01

    A simple, sensitive, and specific method with gas chromatography-mass spectrometry was developed for simultaneous extraction and derivatization of amphetamines (APs) and 3,4-methylenedioxyamphetamines (MDAs) in human urine by using a monolithic silica spin column. All the procedures, such as sample loading, washing, and elution were performed by centrifugation. APs and MDAs in urine were adsorbed on the monolithic silica and derivatized with propyl chloroformate in the column. Methamphetamine-d 5 was used as an internal standard. The linear ranges were 0.01-5.0 μg mL -1 for methamphetamine (MA) and 3,4-methylenedioxymethamphetamine (MDMA) and 0.02-5.0 μg mL -1 for amphetamine (AP) and 3,4-methylenedioxyamphetamine (MDA) (coefficient of correlation ≥0.995). The recovery of APs and MDAs in urine was 84-94%, and the relative standard deviation of the intra- and interday reproducibility for urine samples containing 0.1, 1.0, and 4.0 μg mL -1 of APs and MDAs ranged from 1.4% to 13.6%. The lowest detection limit (signal-to-noise ratio ≥ 3) in urine was 5 ng mL -1 for MA and MDMA and 10 ng mL -1 for AP and MDA. The proposed method can be used to perform simultaneous extraction and derivatization on spin columns that have been loaded with a small quantity of solvent by using centrifugation.

  1. 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

  2. Monolithic silica spin column extraction and simultaneous derivatization of amphetamines and 3,4-methylenedioxyamphetamines in human urine for gas chromatographic-mass spectrometric detection

    Energy Technology Data Exchange (ETDEWEB)

    Nakamoto, Akihiro [Scientific Investigation Laboratory, Hiroshima Prefectural Police Headquarters, Kohnan 2-26-3, Naka-ku, Hiroshima 730-0825 (Japan); Nishida, Manami [Hiroshima University Technical Center, Kasumi 1-2-3, Minami-ku, Hiroshima 734-8551 (Japan); Saito, Takeshi [Department of Emergency and Critical Care Medicine, Tokai University School of Medicine, Shimokasuya 143, Isehara, Kanagawa 259-1143 (Japan); Kishiyama, Izumi; Miyazaki, Shota [GL Sciences Inc., Sayamagahara 237-2, Iruma, Saitama 358-0032 (Japan); Murakami, Katsunori [Scientific Investigation Laboratory, Hiroshima Prefectural Police Headquarters, Kohnan 2-26-3, Naka-ku, Hiroshima 730-0825 (Japan); Nagao, Masataka [Department of Forensic Medicine, Graduate School of Biomedical Sciences, Hiroshima University, Kasumi 1-2-3, Minami-ku, Hiroshima 734-8551 (Japan); Namura, Akira, E-mail: namera@hiroshima-u.ac.jp [Department of Forensic Medicine, Graduate School of Biomedical Sciences, Hiroshima University, Kasumi 1-2-3, Minami-ku, Hiroshima 734-8551 (Japan)

    2010-02-19

    A simple, sensitive, and specific method with gas chromatography-mass spectrometry was developed for simultaneous extraction and derivatization of amphetamines (APs) and 3,4-methylenedioxyamphetamines (MDAs) in human urine by using a monolithic silica spin column. All the procedures, such as sample loading, washing, and elution were performed by centrifugation. APs and MDAs in urine were adsorbed on the monolithic silica and derivatized with propyl chloroformate in the column. Methamphetamine-d{sub 5} was used as an internal standard. The linear ranges were 0.01-5.0 {mu}g mL{sup -1} for methamphetamine (MA) and 3,4-methylenedioxymethamphetamine (MDMA) and 0.02-5.0 {mu}g mL{sup -1} for amphetamine (AP) and 3,4-methylenedioxyamphetamine (MDA) (coefficient of correlation {>=}0.995). The recovery of APs and MDAs in urine was 84-94%, and the relative standard deviation of the intra- and interday reproducibility for urine samples containing 0.1, 1.0, and 4.0 {mu}g mL{sup -1} of APs and MDAs ranged from 1.4% to 13.6%. The lowest detection limit (signal-to-noise ratio {>=} 3) in urine was 5 ng mL{sup -1} for MA and MDMA and 10 ng mL{sup -1} for AP and MDA. The proposed method can be used to perform simultaneous extraction and derivatization on spin columns that have been loaded with a small quantity of solvent by using centrifugation.

  3. Gas chromatographic-mass spectrometric investigation of n-alkanes and carboxylic acids in bottom sediments of the northern Caspian Sea

    Science.gov (United States)

    Kenzhegaliev, Akimgali; Zhumagaliev, Sagat; Kenzhegalieva, Dina; Orazbayev, Batyr

    2018-03-01

    Prior to the start of experimental oil production in the Kashagan field (northern part of the Caspian Sea), n-alkanes and carboxylic acids contained in samples obtained from bottom sediments in the area of artificial island "D" were investigated by gas chromatography-mass spectrometry. Concentrations of 10 n-alkanes (composed of C10-C13, C15-C20) and 11 carboxylic acids (composed of C6-C12, C14-C16) were identified and measured. Concentrations of individual alkanes and carboxylic acids in bottom sediments of the various samples varied between 0.001 ÷ 0.88 μg/g and 0.001 ÷ 1.94 μg/g, respectively. Mass spectra, in particular the M+ molecular ion peak and the most intense peaks of fragment ions, are given. The present study illustrates the stability of molecular ions to electronic ionisation and the main fragment ions to the total ion current and shows that the initial fragmentation of alkanes implies radical cleavage of C2H5 rather than CH3. All aliphatic monocarboxylic acids studied were characterised by McLafferty rearrangement leading to the formation of F4 cation-radical with m/z 60 and F3 cation-radical with m/z 88 in the case of ethylhexanoic acid. The formation of oxonium ions presents another important aspect of acid fragmentation. Using mass numbers of oxonium ions and rearrangement ions allows determination of the substitution character in α- and β- C atoms. The essence of our approach is to estimate the infiltration of hydrocarbon fluids from the enclosing formation into sea water, comprising an analysis of derivatives of organic compounds in bottom sediments. Thus, concentrations of derived organic molecules can serve as a basis for estimates of the depth at which hydrocarbon fluids leak, i.e., to serve as an auxiliary technique in the search for hydrocarbon deposits and to repair well leaks.

  4. 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.

  5. Monolithic silica spin column extraction and simultaneous derivatization of amphetamines and 3,4-methylenedioxyamphetamines in human urine for gas chromatographic-mass spectrometric detection.

    Science.gov (United States)

    Nakamoto, Akihiro; Nishida, Manami; Saito, Takeshi; Kishiyama, Izumi; Miyazaki, Shota; Murakami, Katsunori; Nagao, Masataka; Namura, Akira

    2010-02-19

    A simple, sensitive, and specific method with gas chromatography-mass spectrometry was developed for simultaneous extraction and derivatization of amphetamines (APs) and 3,4-methylenedioxyamphetamines (MDAs) in human urine by using a monolithic silica spin column. All the procedures, such as sample loading, washing, and elution were performed by centrifugation. APs and MDAs in urine were adsorbed on the monolithic silica and derivatized with propyl chloroformate in the column. Methamphetamine-d(5) was used as an internal standard. The linear ranges were 0.01-5.0 microg mL(-1) for methamphetamine (MA) and 3,4-methylenedioxymethamphetamine (MDMA) and 0.02-5.0 microg mL(-1) for amphetamine (AP) and 3,4-methylenedioxyamphetamine (MDA) (coefficient of correlation > or = 0.995). The recovery of APs and MDAs in urine was 84-94%, and the relative standard deviation of the intra- and interday reproducibility for urine samples containing 0.1, 1.0, and 4.0 microg mL(-1) of APs and MDAs ranged from 1.4% to 13.6%. The lowest detection limit (signal-to-noise ratio > or = 3) in urine was 5 ng mL(-1) for MA and MDMA and 10 ng mL(-1) for AP and MDA. The proposed method can be used to perform simultaneous extraction and derivatization on spin columns that have been loaded with a small quantity of solvent by using centrifugation. Copyright 2009 Elsevier B.V. All rights reserved.

  6. Headspace solid-phase microextraction-gas chromatographic-time-of-flight mass spectrometric methodology for geographical origin verification of coffee

    International Nuclear Information System (INIS)

    Risticevic, Sanja; Carasek, Eduardo; Pawliszyn, Janusz

    2008-01-01

    Increasing consumer awareness of food safety issues requires the development of highly sophisticated techniques for the authentication of food commodities. The food products targeted for falsification are either products of high commercial value or those produced in large quantities. For this reason, the present investigation is directed towards the characterization of coffee samples according to the geographical origin. The conducted research involves the development of a rapid headspace solid-phase microextraction (HS-SPME)-gas chromatography-time-of-flight mass spectrometry (GC-TOFMS) method that is utilized for the verification of geographical origin traceability of coffee samples. As opposed to the utilization of traditional univariate optimization methods, the current study employs the application of multivariate experimental designs to the optimization of extraction-influencing parameters. Hence, the two-level full factorial first-order design aided in the identification of two influential variables: extraction time and sample temperature. The optimum set of conditions for the two variables was 12 min and 55 deg. C, respectively, as directed by utilization of Doehlert matrix and response surface methodology. The high-throughput automated SPME procedure was completed by implementing a single divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) 50/30 μm metal fiber with excellent durability properties ensuring the completion of overall sequence of coffee samples. The utilization of high-speed TOFMS instrument ensured the completion of one GC-MS run of a complex coffee sample in 7.9 min and the complete list of benefits provided by ChromaTOF software including fully automated background subtraction, baseline correction, peak find and mass spectral deconvolution algorithms was exploited during the data evaluation procedure. The combination of the retention index (RI) system using C 8 -C 40 alkanes and the mass spectral library search was utilized for the

  7. Headspace solid-phase microextraction-gas chromatographic-time-of-flight mass spectrometric methodology for geographical origin verification of coffee

    Energy Technology Data Exchange (ETDEWEB)

    Risticevic, Sanja [Department of Chemistry, University of Waterloo, 200 University Avenue West, Waterloo, Ontario, N2L 3G1 (Canada); Carasek, Eduardo [Department of Chemistry, Federal University of Santa Catarina, Trindade, Florianopolis, 88040-900, Santa Catarina (Brazil); Pawliszyn, Janusz [Department of Chemistry, University of Waterloo, 200 University Avenue West, Waterloo, Ontario, N2L 3G1 (Canada)], E-mail: janusz@uwaterloo.ca

    2008-06-09

    Increasing consumer awareness of food safety issues requires the development of highly sophisticated techniques for the authentication of food commodities. The food products targeted for falsification are either products of high commercial value or those produced in large quantities. For this reason, the present investigation is directed towards the characterization of coffee samples according to the geographical origin. The conducted research involves the development of a rapid headspace solid-phase microextraction (HS-SPME)-gas chromatography-time-of-flight mass spectrometry (GC-TOFMS) method that is utilized for the verification of geographical origin traceability of coffee samples. As opposed to the utilization of traditional univariate optimization methods, the current study employs the application of multivariate experimental designs to the optimization of extraction-influencing parameters. Hence, the two-level full factorial first-order design aided in the identification of two influential variables: extraction time and sample temperature. The optimum set of conditions for the two variables was 12 min and 55 deg. C, respectively, as directed by utilization of Doehlert matrix and response surface methodology. The high-throughput automated SPME procedure was completed by implementing a single divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) 50/30 {mu}m metal fiber with excellent durability properties ensuring the completion of overall sequence of coffee samples. The utilization of high-speed TOFMS instrument ensured the completion of one GC-MS run of a complex coffee sample in 7.9 min and the complete list of benefits provided by ChromaTOF software including fully automated background subtraction, baseline correction, peak find and mass spectral deconvolution algorithms was exploited during the data evaluation procedure. The combination of the retention index (RI) system using C{sub 8}-C{sub 40} alkanes and the mass spectral library search was

  8. CERN Video News on line

    CERN Multimedia

    2003-01-01

    The latest CERN video news is on line. In this issue : an interview with the Director General and reports on the new home for the DELPHI barrel and the CERN firemen's spectacular training programme. There's also a vintage video news clip from 1954. See: www.cern.ch/video or Bulletin web page

  9. On-line moisture analysis

    CERN Document Server

    Cutmore, N G

    2002-01-01

    Measurement of the moisture content of iron ore has become a key issue for controlling moisture additions for dust suppression. In most cases moisture content is still determined by manual or automatic sampling of the ore stream, followed by conventional laboratory analysis by oven drying. Although this procedure enables the moisture content to be routinely monitored, it is too slow for control purposes. This has generated renewed interest in on-line techniques for the accurate and rapid measurement of moisture in iron ore on conveyors. Microwave transmission techniques have emerged over the past 40 years as the dominant technology for on-line measurement of moisture in bulk materials, including iron ores. Alternative technologies have their limitations. Infra-red analysers are used in a variety of process industries, but rely on the measurement of absorption by moisture in a very thin surface layer. Consequently such probes may be compromised by particle size effects and biased presentation of the bulk mater...

  10. Gas chromatographic analysis of plant sterols

    Science.gov (United States)

    Phytosterols are well-known for their ability to lower blood cholesterol by competing with absorption of cholesterol from the diet and reabsorption of bile cholesterol. Phytosterols as food ingredients are “Generally Recognized As Safe” (GRAS) by the FDA, and they are increasingly incorporated into ...

  11. Gas chromatographic and mass spectrometric analysis of ...

    Indian Academy of Sciences (India)

    Unknown

    Following oral administration three major metabolites of ... It is well established that the stimulating anabolic effect of ... oral application of a single dose of clostebol (dose,. 20 mg) ..... 17â and testosterone production by ovarian follicles of the.

  12. Radioimmunoassay of methaqualone in human urine compared with chromatographic methods

    International Nuclear Information System (INIS)

    Mule, S.J.; Kogan, M.; Jukofsky, D.

    1978-01-01

    The 125 I-radioimmunoassay for methaqualone in human urine was evaluated by a comparison with newly modified gas-liquid chromatographic and thin-layer chromatographic methods. The statistically significant sensitivity value for the radioimmunoassay was at 2 μg of methaqualone per liter of urine. The coefficient of variation was 2.88 -+ 0.16% intraassay. There was cross-reactivity only with metabolites of methaqualone, 4'-hydroxymethaqualone being twice as sensitively measured as methaqualone. There was complete agreement between results by radioimmunoassay and by gas-liquid chromatography in 96.7% of the samples analyzed. Only 1.2% of the radioimmunoassay values were false positives, and 2.1% false negatives (phi = 0.8917, P < 0.001). Comparisons between the thin-layer chromatographic data and the gas--liquid chromatographic or radioimmunoassay data showed less agreement because of the 50- to 200-fold higher sensitivity of the latter techniques. Gas--liquid chromatography therefore appears to represent the best reference method for the evaluation of the radioimmunoassay, which appears to be a very sensitive and reliable technique for detecting methaqualone and its metabolites in human urine

  13. Determination of solute descriptors by chromatographic methods

    International Nuclear Information System (INIS)

    Poole, Colin F.; Atapattu, Sanka N.; Poole, Salwa K.; Bell, Andrea K.

    2009-01-01

    The solvation parameter model is now well established as a useful tool for obtaining quantitative structure-property relationships for chemical, biomedical and environmental processes. The model correlates a free-energy related property of a system to six free-energy derived descriptors describing molecular properties. These molecular descriptors are defined as L (gas-liquid partition coefficient on hexadecane at 298 K), V (McGowan's characteristic volume), E (excess molar refraction), S (dipolarity/polarizability), A (hydrogen-bond acidity), and B (hydrogen-bond basicity). McGowan's characteristic volume is trivially calculated from structure and the excess molar refraction can be calculated for liquids from their refractive index and easily estimated for solids. The remaining four descriptors are derived by experiment using (largely) two-phase partitioning, chromatography, and solubility measurements. In this article, the use of gas chromatography, reversed-phase liquid chromatography, micellar electrokinetic chromatography, and two-phase partitioning for determining solute descriptors is described. A large database of experimental retention factors and partition coefficients is constructed after first applying selection tools to remove unreliable experimental values and an optimized collection of varied compounds with descriptor values suitable for calibrating chromatographic systems is presented. These optimized descriptors are demonstrated to be robust and more suitable than other groups of descriptors characterizing the separation properties of chromatographic systems.

  14. Determination of solute descriptors by chromatographic methods.

    Science.gov (United States)

    Poole, Colin F; Atapattu, Sanka N; Poole, Salwa K; Bell, Andrea K

    2009-10-12

    The solvation parameter model is now well established as a useful tool for obtaining quantitative structure-property relationships for chemical, biomedical and environmental processes. The model correlates a free-energy related property of a system to six free-energy derived descriptors describing molecular properties. These molecular descriptors are defined as L (gas-liquid partition coefficient on hexadecane at 298K), V (McGowan's characteristic volume), E (excess molar refraction), S (dipolarity/polarizability), A (hydrogen-bond acidity), and B (hydrogen-bond basicity). McGowan's characteristic volume is trivially calculated from structure and the excess molar refraction can be calculated for liquids from their refractive index and easily estimated for solids. The remaining four descriptors are derived by experiment using (largely) two-phase partitioning, chromatography, and solubility measurements. In this article, the use of gas chromatography, reversed-phase liquid chromatography, micellar electrokinetic chromatography, and two-phase partitioning for determining solute descriptors is described. A large database of experimental retention factors and partition coefficients is constructed after first applying selection tools to remove unreliable experimental values and an optimized collection of varied compounds with descriptor values suitable for calibrating chromatographic systems is presented. These optimized descriptors are demonstrated to be robust and more suitable than other groups of descriptors characterizing the separation properties of chromatographic systems.

  15. The rationalization of desulfurization by on-line analysis

    Energy Technology Data Exchange (ETDEWEB)

    Murakami, Y; Kohmura, S; Taketomi, H; Matsumura, S; Sasaki, Y

    1986-01-01

    Nippon Kokan uses the Takahax and Sulfiban processes for the desulfurization of coke oven gas. The authors outline the Sulfiban Process and describe a recently developed system for the on-line determination of H/sub 2/S in coke oven gas, and of CO/sub 2/ and monoethanolamine (MEA) in the wash oil. This new on-line analysis system has proved effective in rationalizing the Sulfiban Process via lower MEA production costs and decreased power consumption. The introduction of a computerized control system is now being studied. 7 figs., 4 tabs.

  16. On line ultrasonic integrated backscatter

    International Nuclear Information System (INIS)

    Landini, L.; Picano, E.; Mazzarisi, A.; Santarelli, F.; Benassi, A.; De Pieri, G.

    1988-01-01

    A new equipment for on-line evaluation of index based on two-dimensional integrated backscatter from ultrasonic images is described. The new equipment is fully integrated into a B-mode ultrasonic apparatus which provides a simultaneous display of conventional information together with parameters of tissue characterization. The system has been tested with a backscattering model of microbubbles in polysaccharide solution, characterized by a physiological exponential time decay. An exponential fitting to the experimental data was performed which yielded r=0.95

  17. On-line nuclear orientation

    International Nuclear Information System (INIS)

    Krane, K.S.

    1990-01-01

    This grant has as its overall goal the pursuit of on-line nuclear orientation experiments for the purpose of eliciting details of nuclear structure from the decays of neutron-deficient nuclei, such as those produced by the Holifield Heavy-Ion Research Facility at Oak Ridge and extracted by the UNISOR Isotope Separator. This paper discusses: refrigerator development; the decay of 184 Au; the decay of 191 Hg to 191 Au; the decay of 189 Pt to 189 Ir; the decays of 109,111 Pd; the decay of 172 Er; and solid angle corrections

  18. Derivatization reactions in the gas—liquid chromatographic analysis of drugs in biological fluids

    NARCIS (Netherlands)

    Hulshoff, A.; Lingeman, H.

    1984-01-01

    Alkylation, acylation, silylation and other derivatization reactions applied to the gas chromatographic analysis of drugs in biological matrices are reviewed. Reaction conditions are discussed in relation to reaction mechanisms. Detector-oriented labelling of drugs, and derivatization with chiral

  19. Chromatographic decontamination of medium-activity waste concentrates

    International Nuclear Information System (INIS)

    Faubel, W.; Menzler, P.M.; Sameh, A.A.

    1988-01-01

    The chromatographic decontamination of a MAW concentrate was carried out in a laboratory plant in 1-l-batches in the following way: In order to purify the nitric MAW concentrate from its solid and organic contamination products, it is passed through a filter and an absorber (SM7) for organic species. Subsequently the purified solution runs on-line through all following columns. First the main activity carrier cesium ( 137 Cs, 134 Cs) is transferred to ammonium molybdate phosphate (AMP-1) by means of a newly developed fluidized bed process. In the further course, 125 Sb is separated on metal oxides (Sb 2 O 5 , MnO 2 ) and the three-valued actinides/lanthanides on an extraction-chromatographic CMPO column. Finally the remaining 106 Ru and 60 Co activities are separated on dimethylglyoximes (DMG) coated on active carbon. (orig./RB) [de

  20. On-line moisture analysis

    International Nuclear Information System (INIS)

    Cutmore, N.G.; Mijak, D.G

    2002-01-01

    Measurement of the moisture content of iron ore has become a key issue for controlling moisture additions for dust suppression. In most cases moisture content is still determined by manual or automatic sampling of the ore stream, followed by conventional laboratory analysis by oven drying. Although this procedure enables the moisture content to be routinely monitored, it is too slow for control purposes. This has generated renewed interest in on-line techniques for the accurate and rapid measurement of moisture in iron ore on conveyors. Microwave transmission techniques have emerged over the past 40 years as the dominant technology for on-line measurement of moisture in bulk materials, including iron ores. Alternative technologies have their limitations. Infra-red analysers are used in a variety of process industries, but rely on the measurement of absorption by moisture in a very thin surface layer. Consequently such probes may be compromised by particle size effects and biased presentation of the bulk material. Nuclear-based analysers measure the total hydrogen content in the sample and do not differentiate between free and combined moisture. Such analysers may also be sensitive to material presentation and elemental composition. Very low frequency electromagnetic probes, such as capacitance or conductance probes, operate in the frequency region where the DC conductivity dominates much of the response, which is a function not only of moisture content but also of ionic composition and chemistry. These problems are overcome using microwave transmission techniques, which also have the following advantages, as a true bulk moisture analysis is obtained, because a high percentage of the bulk material is analysed; the moisture estimate is mostly insensitive to any biased presentation of moisture, for example due to stratification of bulk material with different moisture content and because no physical contact is made between the sensor and the bulk material. This is

  1. Quantitative on-line analysis of sulfur compounds in complex hydrocarbon matrices.

    Science.gov (United States)

    Djokic, Marko R; Ristic, Nenad D; Olahova, Natalia; Marin, Guy B; Van Geem, Kevin M

    2017-08-04

    An improved method for on-line measurement of sulfur containing compounds in complex matrices is presented. The on-line system consists of a specifically designed sampling system connected to a comprehensive two-dimensional gas chromatograph (GC×GC) equipped with two capillary columns (Rtx ® -1 PONA×SGE BPX50), a flame ionization detector (FID) and a sulfur chemiluminescence detector (SCD). The result is an unprecedented sensitivity down to ppm level (1 ppm-w) for various sulfur containing compounds in very complex hydrocarbon matrices. In addition to the GC×GC-SCD, the low molecular weight sulfur containing compounds such as hydrogen sulfide (H 2 S) and carbonyl sulfide (COS) can be analyzed using a thermal conductivity detector of a so-called refinery gas analyzer (RGA). The methodology was extensively tested on a continuous flow pilot plant for steam cracking, in which quantification of sulfur containing compounds in the reactor effluent was carried out using 3-chlorothiophene as internal standard. The GC×GC-FID/-SCD settings were optimized for ppm analysis of sulfur compounds in olefin-rich (ethylene- and propylene-rich) hydrocarbon matrices produced by steam cracking of petroleum feedstocks. Besides that is primarily used for analysis of the hydrocarbon matrix, FID of the GC×GC-FID/-SCD set-up serves to double check the amount of added sulfur internal standard which is crucial for a proper quantification of sulfur compounds. When vacuum gas oil containing 780 ppm-w of elemental sulfur in the form of benzothiophenes and dibenzothiophenes is subjected to steam cracking, the sulfur balance was closed, with 75% of the sulfur contained in the feed is converted to hydrogen sulfide, 13% to alkyl homologues of thiophene while the remaining 12% is present in the form of alkyl homologues of benzothiophenes. The methodology can be applied for many other conversion processes which use sulfur containing feeds such as hydrocracking, catalytic cracking, kerogen

  2. On-line data display

    Science.gov (United States)

    Lang, Sherman Y. T.; Brooks, Martin; Gauthier, Marc; Wein, Marceli

    1993-05-01

    A data display system for embedded realtime systems has been developed for use as an operator's user interface and debugging tool. The motivation for development of the On-Line Data Display (ODD) have come from several sources. In particular the design reflects the needs of researchers developing an experimental mobile robot within our laboratory. A proliferation of specialized user interfaces revealed a need for a flexible communications and graphical data display system. At the same time the system had to be readily extensible for arbitrary graphical display formats which would be required for data visualization needs of the researchers. The system defines a communication protocol transmitting 'datagrams' between tasks executing on the realtime system and virtual devices displaying the data in a meaningful way on a graphical workstation. The communication protocol multiplexes logical channels on a single data stream. The current implementation consists of a server for the Harmony realtime operating system and an application written for the Macintosh computer. Flexibility requirements resulted in a highly modular server design, and a layered modular object- oriented design for the Macintosh part of the system. Users assign data types to specific channels at run time. Then devices are instantiated by the user and connected to channels to receive datagrams. The current suite of device types do not provide enough functionality for most users' specialized needs. Instead the system design allows the creation of new device types with modest programming effort. The protocol, design and use of the system are discussed.

  3. Development and validation of a highly sensitive gas chromatographic-mass spectrometric screening method for the simultaneous determination of nanogram levels of fentanyl, sufentanil and alfentanil in air and surface contamination wipes.

    Science.gov (United States)

    Van Nimmen, Nadine F J; Veulemans, Hendrik A F

    2004-05-07

    A highly sensitive gas chromatographic-mass spectrometric (GC-MS) analytical method for the determination of the opioid narcotics fentanyl, alfentanil, and sufentanil in industrial hygiene personal air samples and surface contamination wipes was developed and comprehensively validated. Sample preparation involved a single step extraction of the samples with methanol, fortified with a fixed amount of the penta-deuterated analogues of the opioid narcotics as internal standard. The GC-MS analytical procedure using selected ion monitoring (SIM) was shown to be highly selective. Linearity was shown for levels of extracted wipe and air samples corresponding to at least 0.1-2 times their surface contamination limit (SCL) and accordingly to 0.1-2 times their time weighted average occupational exposure limit (OEL-TWA) based on a full shift 9601 air sample. Extraction recoveries were determined for spiked air samples and surface wipes and were found to be quantitative for both sampling media in the entire range studied. The air sampling method's limit of detection (LOD) was determined to be 0.4 ng per sample for fentanyl and sufentanil and 1.6 ng per sample for alfentanil, corresponding to less than 1% of their individual OEL for a full shift air sample (9601). The limit of quantification (LOQ) was found to be 1.4, 1.2, and 5.0 ng per filter for fentanyl, sufentanil, and alfentanil, respectively. The wipe sampling method had LODs of 4 ng per wipe for fentanyl and sufentanil and 16 ng per wipe for alfentanil and LOQs of respectively, 14, 12, and 50 ng per wipe. The analytical intra-assay precision of the air sampling and wipe sampling method, defined as the coefficient of variation on the analytical result of six replicate spiked media was below 10 and 5%, respectively, for all opioids at all spike levels. Accuracy expressed as relative error was determined to be below 10%, except for alfentanil at the lowest spike level (-13.1%). The stability of the opioids during simulated

  4. Reversed-phase liquid chromatography coupled on-line with capillary gas chromatography use of an anion-exchange membrane to remove an ion-pair reagent from the eluent.

    NARCIS (Netherlands)

    Brinkman, U.A.T.; Goosens, E.C.; de Jong, D.; de Jong, G.J.; Beerthuizen, I.M.

    1995-01-01

    In order to enable the coupling of reversed-phase liquid chromatography (RPLC) with capillary gas chromatography (GC), the performance of an anion-exchange micromembrane device has been studied to remove the ion-pair reagent methanesulphonic acid from an acetonitrile/water LC eluent. The regenerant

  5. Chromatographic and electrophoretic approaches in ink analysis.

    Science.gov (United States)

    Zlotnick, J A; Smith, F P

    1999-10-15

    Inks are manufactured from a wide variety of substances that exhibit very different chemical behaviors. Inks designed for use in different writing instruments or printing methods have quite dissimilar components. Since the 1950s chromatographic and electrophoretic methods have played important roles in the analysis of inks, where compositional information may have bearing on the investigation of counterfeiting, fraud, forgery, and other crimes. Techniques such as paper chromatography and electrophoresis, thin-layer chromatography, high-performance liquid chromatography, gas chromatography, gel electrophoresis, and the relatively new technique of capillary electrophoresis have all been explored as possible avenues for the separation of components of inks. This paper reviews the components of different types of inks and applications of the above separation methods are reviewed.

  6. Micro-column plasma emission liquid chromatograph. [Patent application

    Science.gov (United States)

    Gay, D.D.

    1982-08-12

    In a direct current plasma emission spectrometer for use in combination with a microcolumn liquid chromatograph, an improved plasma source unit is claimed. The plasma source unit includes a quartz capillary tube having an inlet means, outlet off gas means and a pair of spaced electrodes defining a plasma region in the tube. The inlet means is connected to and adapted to receive eluant of the liquid chromatograph along with a stream of plasma-forming gas. There is an opening through the wall of the capillary tube penetrating into the plasma region. A soft glass capillary light pipe is disposed at the opening, is connected to the spectrometer, and is adapted to transmit light passing from the plasma region to the spectrometer. There is also a source of electromotive force connected to the electrodes sufficient to initiate and sustain a plasma in the plasma region of the tube.

  7. Approaches for on-line coupling of extraction and chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Hyoetylaeinen, Tuulia; Riekkola, Marja-Liisa [Laboratory of Analytical Chemistry, Department of Chemistry, University of Helsinki, P.O. Box 55, 00014, Helsinki (Finland)

    2004-04-01

    This review provides an overview of the approaches available in order to perform on-line coupling of various extraction techniques with liquid and gas chromatography, for the analysis of semivolatile and nonvolatile analytes in liquid and solid samples. The main focus is on the instrumental set-up of these techniques. Selected real applications are described by way of illustration. The extraction methods suitable for on-line coupling covered in this review are: liquid-liquid extraction, solid-phase extraction, membrane-based techniques, pressurised liquid extraction, supercritical fluid extraction, and microwave- and sonication-assisted extractions. The following systems are not covered in this review: on-line coupled solid-phase extraction-liquid chromatography, purge-and-trap-GC, and membrane extraction with a sorbent interface-GC. (orig.)

  8. Assays for chloramphenicol compared: radioenzymatic, gas chromatographic with electron capture, and gas chromatographic-mass specteometric

    International Nuclear Information System (INIS)

    Pickering, L.K.; Hoecker, J.L.; Kramer, W.G.; Liehr, J.G.; Caprioli, R.M.

    1979-01-01

    We compared these three techniques for measuring chloramphenicol in serum or urine. Although each has its particular advantages, any of them is shown to be satisfactory and may appropriately be used by clinical laboratories, according to the facilities available

  9. Simple setup for gas-phase h/d exchange mass spectrometry coupled to electron transfer dissociation and ion mobility for analysis of polypeptide structure on a liquid chromatographic time scale

    DEFF Research Database (Denmark)

    Mistarz, Ulrik Hvid; Brown, Jeffery M; Haselmann, Kim F

    2014-01-01

    gas immediately upstream or downstream of the primary skimmer cone. The approach was implemented on three commercially available mass spectrometers and required no or minor fully reversible reconfiguration of gas-inlets of the ion source. Results from gas-phase HDX-MS of peptides using the aqueous ND3....../D2O as HDX reagent indicate that labeling is facilitated exclusively through gaseous ND3, yielding similar results to the infusion of purified ND3-gas, while circumventing the complications associated with the use of hazardous purified gases. Comparison of the solution-phase- and gas-phase deuterium...

  10. Vibrational Spectroscopy of Chromatographic Interfaces

    Energy Technology Data Exchange (ETDEWEB)

    Jeanne E. Pemberton

    2011-03-10

    Chromatographic separations play a central role in DOE-supported fundamental research related to energy, biological systems, the environment, and nuclear science. The overall portfolio of research activities in the Separations and Analysis Program within the DOE Office of Basic Energy Sciences includes support for activities designed to develop a molecular-level understanding of the chemical processes that underlie separations for both large-scale and analytical-scale purposes. The research effort funded by this grant award was a continuation of DOE-supported research to develop vibrational spectroscopic methods to characterize the interfacial details of separations processes at a molecular level.

  11. Towards optical spectroscopy of the element nobelium (Z = 102) in a buffer gas cell. First on-line experiments on {sup 155}Yb at the velocity filter SHIP with a novel ion collection and atom re-evaporation method of high efficiency

    Energy Technology Data Exchange (ETDEWEB)

    Backe, H.; Kunz, P.; Lauth, W.; Dretzke, A.; Horn, R.; Kolb, T. [Mainz Univ., Institut fur Kernphysik (Germany); Laatiaoui, M.; Sewtz, M. [Munchen Ludwig-Maximilians-Univ., Dept. fur Physik, Garching (Germany); Ackermann, D.; Block, M.; Herfurth, F.; Hebberger, F.P.; Hofmann, S.; Mann, R. [Gesellschaft fur Schwerionenforschung, Darmstadt (Germany)

    2007-10-15

    For the investigation of the atomic level structure of heavy elements which can only be produced at on-line facilities such as GSI (Darmstadt, Germany), a novel experimental procedure has been developed. It is based on Radiation Detected Resonance Ionization Spectroscopy (RADRIS) and can be applied to elements like nobelium produced at rates of a few ions per second. Fusion reaction products are separated from the primary beam by the velocity filter SHIP at GSI, stopped in a buffer gas cell, collected on a tantalum filament and then re-evaporated as atoms. The ions produced by resonance ionization with tunable laser beams are detected via their characteristic alpha decay. First on-line experiments on alpha-active {sup 155}Yb, which is supposed to have an atomic level structure similar to nobelium, were performed. These test experiments focused on the optimization of the collection and re-evaporation process of the radioactive ions, the laser ionization efficiency and the detection via alpha decay. An overall efficiency for RADRIS of 0.8% with respect to the target production rate was measured. While further improvements of this efficiency are in progress it should already be sufficient for the search for atomic levels in nobelium. (authors)

  12. Towards optical spectroscopy of the element nobelium (Z = 102) in a buffer gas cell. First on-line experiments on 155Yb at the velocity filter SHIP with a novel ion collection and atom re-evaporation method of high efficiency

    International Nuclear Information System (INIS)

    Backe, H.; Kunz, P.; Lauth, W.; Dretzke, A.; Horn, R.; Kolb, T.; Laatiaoui, M.; Sewtz, M.; Ackermann, D.; Block, M.; Herfurth, F.; Hebberger, F.P.; Hofmann, S.; Mann, R.

    2007-01-01

    For the investigation of the atomic level structure of heavy elements which can only be produced at on-line facilities such as GSI (Darmstadt, Germany), a novel experimental procedure has been developed. It is based on Radiation Detected Resonance Ionization Spectroscopy (RADRIS) and can be applied to elements like nobelium produced at rates of a few ions per second. Fusion reaction products are separated from the primary beam by the velocity filter SHIP at GSI, stopped in a buffer gas cell, collected on a tantalum filament and then re-evaporated as atoms. The ions produced by resonance ionization with tunable laser beams are detected via their characteristic alpha decay. First on-line experiments on alpha-active 155 Yb, which is supposed to have an atomic level structure similar to nobelium, were performed. These test experiments focused on the optimization of the collection and re-evaporation process of the radioactive ions, the laser ionization efficiency and the detection via alpha decay. An overall efficiency for RADRIS of 0.8% with respect to the target production rate was measured. While further improvements of this efficiency are in progress it should already be sufficient for the search for atomic levels in nobelium. (authors)

  13. Chiral ionic liquids in chromatographic and electrophoretic separations.

    Science.gov (United States)

    Kapnissi-Christodoulou, Constantina P; Stavrou, Ioannis J; Mavroudi, Maria C

    2014-10-10

    This report provides an overview of the application of chiral ionic liquids (CILs) in separation technology, and particularly in capillary electrophoresis and both gas and liquid chromatography. There is a large number of CILs that have been synthesized and designed as chiral agents. However, only a few have successfully been applied in separation technology. Even though this application of CILs is still in its early stages, the scientific interest is increasing dramatically. This article is focused on the use of CILs as chiral selectors, background electrolyte additives, chiral ligands and chiral stationary phases in electrophoretic and chromatographic techniques. Different examples of CILs, which contain either a chiral cation, a chiral anion or both, are presented in this review article, and their major advantages along with their potential applications in chiral electrophoretic and chromatographic recognition are discussed. Copyright © 2014 Elsevier B.V. All rights reserved.

  14. Project development and commercialization of on-line analysis systems

    International Nuclear Information System (INIS)

    Watt, J.S.

    1997-01-01

    A project team first in the Australian Atomic Energy Commission (AAEC) and since 1982 in CSIRO has developed many on-line analysis systems for the mineral and energy industries. The development of these projects has followed a common pattern of laboratory R and D, field trials, commercialisation and technology transfer. This successful pattern is illustrated using examples of the development of systems for the on-line analysis of mineral slurries, for determination of the ash content of coal on conveyors, and for determination of the flow rates of oil, water and gas in pipelines. The first two systems are licensed to Australian companies, Amdel Ltd and Mineral Control Instrumentation Ltd. Both systems are used by industry worldwide, and are the market leaders for radioisotope gauges in their application field. The third system, the multiphase flow meter, was licensed in 1997 to Kvaerner FSSL Ltd of Aberdeen. This meter has even greater potential than the other two systems for economic benefit from its used and for numbers of installations. The on-line analysis systems have been developed to increase the productivity of the Australian mineral and energy industries, and to provide economic benefit to Australia. The economic benefit sought is predominantly improved process control based on use of the instrument, rather than from its sale. Sales of instruments are significant, however, with about A$80 million from the analysis systems and their derivatives since the 1970s. Some of the issues associated with the development of the on-line analysis system are outlined

  15. Shawnee Mission's On-Line Cataloging System

    Directory of Open Access Journals (Sweden)

    Ellen Wasby Miller

    1971-03-01

    Full Text Available An on-line cataloging pilot project for two elementary schools is discussed. The system components are 2740 terminals, upper-lower-case input, IBM's FASTER generalized software package, and usual cards/labels output. Reasons for choosing FASTER, software and hardware features, operating procedures, system performance and costs are detailed. Future expansion to cataloging 100,000 annual K-12 acquisitions, on-line circulation, retrospective conversion, and union book catalogs is set forth.

  16. INIS retrieval service, towards on-line

    International Nuclear Information System (INIS)

    Ebinuma, Yukio; Komatsubara, Yasutoshi

    1983-01-01

    Japan Atomic Energy Research Institute executes the retrieval service of INIS atomic energy information by batch system in cooperation with Genshiryoku Kozaikai. This service is very popular to the users in whole Japan, but the demand of on-line service has increased recently. Therefore, it was decided to begin the INIS on-line service from January, 1984, through the on-line information retrieval system of the Japan Information Center of Science and Technology. It is expected that when the operation will be started, the utilization of INIS atomic energy information in Japan will drastically increase. Also Japan Atomic Energy Research Institute has carried out the retrieval service by on-line system for those in the institute besides the batch system, accordingly, at this opportunity, the state of utilization of both systems and their distinction to use effectively, and the operation and the method of utilization of the on-line information retrieval system of JICST are explained. In the on-line system, the users are accessible to the data base themselves, and immediate information retrieval is possible, while in the batch system, the related information can be retrieved without fail, and the troublesome operation of equipment is not necessary. (Kako, I.)

  17. Chromatographic Techniques for Rare Earth Elements Analysis

    Science.gov (United States)

    Chen, Beibei; He, Man; Zhang, Huashan; Jiang, Zucheng; Hu, Bin

    2017-04-01

    The present capability of rare earth element (REE) analysis has been achieved by the development of two instrumental techniques. The efficiency of spectroscopic methods was extraordinarily improved for the detection and determination of REE traces in various materials. On the other hand, the determination of REEs very often depends on the preconcentration and separation of REEs, and chromatographic techniques are very powerful tools for the separation of REEs. By coupling with sensitive detectors, many ambitious analytical tasks can be fulfilled. Liquid chromatography is the most widely used technique. Different combinations of stationary phases and mobile phases could be used in ion exchange chromatography, ion chromatography, ion-pair reverse-phase chromatography and some other techniques. The application of gas chromatography is limited because only volatile compounds of REEs can be separated. Thin-layer and paper chromatography are techniques that cannot be directly coupled with suitable detectors, which limit their applications. For special demands, separations can be performed by capillary electrophoresis, which has very high separation efficiency.

  18. Chromatographic Separation of Vitamin E Enantiomers

    Directory of Open Access Journals (Sweden)

    Ju-Yen Fu

    2017-02-01

    Full Text Available Vitamin E is recognized as an essential vitamin since its discovery in 1922. Most vegetable oils contain a mixture of tocopherols and tocotrienols in the vitamin E composition. Structurally, tocopherols and tocotrienols share a similar chromanol ring and a side chain at the C-2 position. Owing to the three chiral centers in tocopherols, they can appear as eight different stereoisomers. Plant sources of tocopherol are naturally occurring in the form of RRR while synthetic tocopherols are usually in the form of all-racemic mixture. Similarly, with only one chiral center, natural tocotrienols occur as the R-isoform. In this review, we aim to discuss a few chromatographic methods that had been used to separate the stereoisomers of tocopherols and tocotrienols. These methods include high performance liquid chromatography, gas chromatography and combination of both. The review will focus on method development including selection of chiral columns, detection method and choice of elution solvent in the context of separation efficiency, resolution and chiral purity. The applications for separation of enantiomers in vitamin E will also be discussed especially in terms of the distinctive biological potency among the stereoisoforms.

  19. 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)

  20. On-line application of the PANTHER advanced nodal code

    International Nuclear Information System (INIS)

    Hutt, P.K.; Knight, M.P.

    1992-01-01

    Over the last few years, Nuclear Electric has developed an integrated core performance code package for both light water reactors (LWRs) and advanced gas-cooled reactors (AGRs) that can perform a comprehensive range of calculations for fuel cycle design, safety analysis, and on-line operational support for such plants. The package consists of the following codes: WIMS for lattice physics, PANTHER whole reactor nodal flux and AGR thermal hydraulics, VIPRE for LWR thermal hydraulics, and ENIGMA for fuel performance. These codes are integrated within a UNIX-based interactive system called the Reactor Physics Workbench (RPW), which provides an interactive graphic user interface and quality assurance records/data management. The RPW can also control calculational sequences and data flows. The package has been designed to run both off-line and on-line accessing plant data through the RPW

  1. On-line meters monitor gas concentrations in transformers

    Energy Technology Data Exchange (ETDEWEB)

    Pirhonen, R.; Lustre, L. [ed.

    1997-11-01

    Power transformers are by far the most expensive single components of 400 kV transmission grid substations. The acquisition price of a transformer is about FIM 15 to 20 million. A good way to extend the service life of a transformer considerably is to conduct a general overhaul. The cornerstone of cost-efficient maintenance is the correct timing of the general overhaul, which usually costs a couple million Finnish marks

  2. Modeling Aquatic Toxicity through Chromatographic Systems.

    Science.gov (United States)

    Fernández-Pumarega, Alejandro; Amézqueta, Susana; Farré, Sandra; Muñoz-Pascual, Laura; Abraham, Michael H; Fuguet, Elisabet; Rosés, Martí

    2017-08-01

    Environmental risk assessment requires information about the toxicity of the growing number of chemical products coming from different origins that can contaminate water and become toxicants to aquatic species or other living beings via the trophic chain. Direct toxicity measurements using sensitive aquatic species can be carried out but they may become expensive and ethically questionable. Literature refers to the use of chromatographic measurements that correlate to the toxic effect of a compound over a specific aquatic species as an alternative to get toxicity information. In this work, we have studied the similarity in the response of the toxicity to different species and we have selected eight representative aquatic species (including tadpoles, fish, water fleas, protozoan, and bacteria) with known nonspecific toxicity to chemical substances. Next, we have selected four chromatographic systems offering good perspectives for surrogation of the eight selected aquatic systems, and thus prediction of toxicity from the chromatographic measurement. Then toxicity has been correlated to the chromatographic retention factor. Satisfactory correlation results have been obtained to emulate toxicity in five of the selected aquatic species through some of the chromatographic systems. Other aquatic species with similar characteristics to these five representative ones could also be emulated by using the same chromatographic systems. The final aim of this study is to model chemical products toxicity to aquatic species by means of chromatographic systems to reduce in vivo testing.

  3. Determination of thromboxanes, leukotrienes and lipoxins using high-temperature capillary liquid chromatography-tandem mass spectrometry and on-line sample preparation

    DEFF Research Database (Denmark)

    Dahl, Sandra Rinne; Kleiveland, Charlotte Ramstad; Kassem, Moustapha

    2009-01-01

    An on-line strong cation-exchange (SCX)-reversed-phase (RP) capillary liquid chromatographic (cLC) method with ion-trap tandem mass spectrometric (IT-MS/MS) detection for the simultaneous determination of thromboxane (TX) B(2), TXB(3), leukotriene (LT) B(4), LTD(4) and lipoxin (LX) A(4) in cell...

  4. Automated chromatographic laccase-mediator-system activity assay.

    Science.gov (United States)

    Anders, Nico; Schelden, Maximilian; Roth, Simon; Spiess, Antje C

    2017-08-01

    To study the interaction of laccases, mediators, and substrates in laccase-mediator systems (LMS), an on-line measurement was developed using high performance anion exchange chromatography equipped with a CarboPac™ PA 100 column coupled to pulsed amperometric detection (HPAEC-PAD). The developed method was optimized for overall chromatographic run time (45 to 120 min) and automated sample drawing. As an example, the Trametes versicolor laccase induced oxidation of 1-(3,4-dimethoxyphenyl)-2-(2-methoxyphenoxy)-1,3-dihydroxypropane (adlerol) using 1-hydroxybenzotriazole (HBT) as mediator was measured and analyzed on-line. Since the Au electrode of the PAD detects only hydroxyl group containing substances with a limit of detection being in the milligram/liter range, not all products are measureable. Therefore, this method was applied for the quantification of adlerol, and-based on adlerol conversion-for the quantification of the LMS activity at a specific T. versicolor laccase/HBT ratio. The automated chromatographic activity assay allowed for a defined reaction start of all laccase-mediator-system reactions mixtures, and the LMS reaction progress was automatically monitored for 48 h. The automatization enabled an integrated monitoring overnight and over-weekend and minimized all manual errors such as pipetting of solutions accordingly. The activity of the LMS based on adlerol consumption was determined to 0.47 U/mg protein for a laccase/mediator ratio of 1.75 U laccase/g HBT. In the future, the automated method will allow for a fast screening of combinations of laccases, mediators, and substrates which are efficient for lignin modification. In particular, it allows for a fast and easy quantification of the oxidizing activity of an LMS on a lignin-related substrate which is not covered by typical colorimetric laccase assays. ᅟ.

  5. Chromatographic analysis and purification of multiply tritium-labelled eicosanoids

    International Nuclear Information System (INIS)

    Shevchenko, V.P.; Nagaev, I.Yu.; Myasoedov, N.F.

    1988-01-01

    A comparative study of different chromatographic techniques (gas-liquid (GLC), thin-layer (TLC), liquid (LC), high-pressure liquid (HPLC) chromatography) is presented. They were applied to the analysis and preparative purification of tritium-labelled eicosanoids with a molar radioactivity of 1.8-8.8 TBq/mmol, obtained by selective hydrogenation and by chemical or enzymic methods. The possibility of analyzing reaction mixtures and isolating individual multiply labelled eicosanoids with a chemical and radiochemical purity of 95-98% was demonstrated. Special features of HPLC for high molar radioactivity eicosanoids are considered. (author) 9 refs.; 6 tabs

  6. Identification of radiation-induced hydrocarbons in halibut, cod and prawns by on-line coupled LC-GC/MS technique

    International Nuclear Information System (INIS)

    Spiegelberg, A.; Schulzki, G.; Boegl, K.W.; Schreiber, G.A.

    1997-01-01

    Radiation-induced hydrocarbons were analysed in a fatty (halibut) and a lean fish (cod) as well as in a prawn species by on-line coupled liquid chromatography (LC) - gas chromatography (GC) combined with mass spectrometrical detection. In irradiated halibut which contains mainly saturated and monounsaturated fatty acids all expected radiolytic alkanes, alkenes and alkadienes could be detected. The yields of the C n-1 and C n-2:1 hydrocarbons were comparable with those found in irradiated lipids of land animals and plants. However, in cod and the prawn species which contain high levels of polyunsaturated fatty acids (PUFA), the C n-1 hydrocarbons were found in concentrations up to tenfold higher whereas the C n-2:1 products were again comparable to those of land animals and plants. The identification of radiation-induced hydrocarbons in fish lipids was achieved by transfer of the hydrocarbons from the LC column to the gas chromatographic column in fractions differing in the degree of unsaturation. For the first time radiation induced hydrocarbons with more than four double bonds generated from polyunsaturated fatty acids (20:4ω6 and 20:5ω3) could be identified. (orig.) [de

  7. On-line monitoring for calibration reduction

    International Nuclear Information System (INIS)

    Hoffmann, M.

    2005-09-01

    On-Line Monitoring evaluates instrument channel performance by assessing its consistency with other plant indications. Elimination or reduction of unnecessary field calibrations can reduce associated labour costs, reduce personnel radiation exposure, and reduce the potential for calibration errors. On-line calibration monitoring is an important technique to implement a state-based maintenance approach and reduce unnecessary field calibrations. In this report we will look at how the concept is currently applied in the industry and what the arising needs are as it becomes more commonplace. We will also look at the PEANO System, a tool developed by the Halden Project to perform signal validation and on-line calibration monitoring. Some issues will be identified that are being addressed in the further development of these tools to better serve the future needs of the industry in this area. An outline for how to improve these points and which aspects should be taken into account is described in detail. (Author)

  8. On-line signal trend identification

    International Nuclear Information System (INIS)

    Tambouratzis, T.; Antonopoulos-Domis, M.

    2004-01-01

    An artificial neural network, based on the self-organizing map, is proposed for on-line signal trend identification. Trends are categorized at each incoming signal as steady-state, increasing and decreasing, while they are further classified according to characteristics such signal shape and rate of change. Tests with model-generated signals illustrate the ability of the self-organizing map to accurately and reliably perform on-line trend identification in terms of both detection and classification. The proposed methodology has been found robust to the presence of white noise

  9. On line routing per mobile phone

    DEFF Research Database (Denmark)

    Bieding, Thomas; Görtz, Simon; Klose, Andreas

    2009-01-01

    On-line routing is concerned with building vehicle routes in an ongoing fashion in such a way that customer requests arriving dynamically in time are efficiently and effectively served. An indispensable prerequisite for applying on-line routing methods is mobile communication technology....... Additionally it is of utmost importance that the employed communication system is suitable integrated with the firm’s enterprise application system and business processes. On basis of a case study, we describe in this paper a system that is cheap and easy to implement due to the use of simple mobile phones...

  10. On-line atomic data access

    Energy Technology Data Exchange (ETDEWEB)

    Schultz, D.R. [Oak Ridge National Lab., TN (United States); Nash, J.K. [Lawrence Livermore National Lab., CA (United States)

    1996-04-01

    The need for atomic data is one which continues to expand in a wide variety of applications including fusion energy, astrophysics, laser- produced plasma research, and plasma processing. Modern computer database and communications technology nables this data to be placed on-line and obtained by users of the Internet. Presented here is a summary of the observations and conclusions regarding such on-line atomic data access derived from a forum held at the Tenth APS Topical Conference on Atomic Processes in Plasmas.

  11. High-resolution gas chromatographic analysis of polycyclic aromatic hydrocarbons and aliphatic hydrocarbons; Separacion por cromatografia de gases de alta eficiencia de hidrocarburos aromaticos policiclicos, (PAH) y alifaticos (AH) ambientales, empleado como fases estacionarias OV-1 y SE-54

    Energy Technology Data Exchange (ETDEWEB)

    Perez, M.; Gonzalez, D.

    1988-07-01

    A study of the analysis by gas chromatography of aromatic polycyclic hydrocarbons and aliphatic hydrocarbons is presented. The separation has been carried out by glass and fused silica capillary column in two different polar stationary phases OV-1 and SE-54. The limitation and the advantages of the procedure are discussed in terms of separation, sensitivity and precision. (Author) 20 refs.

  12. Reactor cover gas monitoring at the Fast Flux Test Facility

    Energy Technology Data Exchange (ETDEWEB)

    Bechtold, R A; Holt, F E; Meadows, G E; Schenter, R E [Westinghouse Hanford Company, Richland, WA (United States)

    1987-07-01

    The Fast Flux Test Facility (FFTF) is a 400 megawatt (thermal) sodium cooled reactor designed for irradiation testing of fuels, materials and components for LMRs. It is operated by the Westinghouse Hanford Company for the U. S. Department of Energy on the government-owned Hanford reservation near Richland, Washington. The first 100 day operating cycle began in April 1982 and the eighth operating cycle was completed In July 1986. Argon is used as the cover gas for all sodium systems at the plant. A program for cover gas monitoring has been in effect since the start of sodium fill in 1978. The argon is supplied to the FFTF by a liquid argon Dewar System and used without further purification. A liquid argon Dewar system provides the large volume of inert gas required for operation of the FFTF. The gas is used as received and is not recycled. Low concentrations of krypton and xenon in the argon supply are essential to preclude interference with the gas tag system. Gas chromatography has been valuable for detection of inadvertent air in leakage during refueling operations. A temporary system is installed over the reactor during outages to prevent oxide formation in the sodium vapor traps upstream from the on line gas chromatograph. On line gas monitoring by gamma spectrometry and grab sampling with GTSTs has been successful for the identification of numerous radioactive gas releases from creep capsule experiments as well as 9 fuel pin ruptures. A redundant fission gas monitoring system has been installed to insure constant surveillance of the reactor cover gas.

  13. On-line monitoring for calibration reduction

    International Nuclear Information System (INIS)

    Hoffmann, Mario; Gran, Frauke Schmitt; Thunem, Harald P-J.

    2004-04-01

    On-Line Monitoring (OLM) of a channel's calibration state evaluates instrument channel performance by assessing its consistency with other plant indications. Industry and experience at several plants has shown this overall approach to be very effective in identifying instrument channels that are exhibiting degrading or inconsistent performance characteristics. The Halden Reactor Project has developed the signal validation system PEANO, which can be used to assist with the tasks of OLM. To further enhance the PEANO System for use as a calibration reduction tool, the following two additional modules have been developed; HRP Prox, which performs pre-processing and statistical analysis of signal data, Batch Monitoring Module (BMM), which is an off-line batch monitoring and reporting suite. The purpose and functionality of the HRP Prox and BMM modules are discussed in this report, as well as the improvements made to the PEANO Server to support these new modules. The Halden Reactor Project has established a Halden On-Line Monitoring User Group (HOLMUG), devoted to the discussion and implementation of on-line monitoring techniques in power plants. It is formed by utilities, vendors, regulatory bodies and research institutes that meet regularly to discuss implementation aspects of on-line monitoring, technical specification changes, cost-benefit analysis and regulatory issues. (Author)

  14. SPIRES I: on-line search guide

    International Nuclear Information System (INIS)

    Addis, L.

    1975-06-01

    SPIRES I is the first generation of the on-line Stanford Public Information Retrieval System. Designed as a prototype system, SPIRES I was later moved to the SLAC computing facility where it has been routinely available to SLAC users in the field of high-energy physics. The scope and use of the SPIRES I system are described in this manual

  15. HOPI: on-line injection optimization program

    International Nuclear Information System (INIS)

    LeMaire, J.L.

    1977-01-01

    A method of matching the beam from the 200 MeV linac to the AGS without the necessity of making emittance measurements is presented. An on-line computer program written on the PDP10 computer performs the matching by modifying independently the horizontal and vertical emittance. Experimental results show success with this method, which can be applied to any matching section

  16. 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

  17. Chromatographic retention and structure roofing tile effect of isomers and its fine structure

    NARCIS (Netherlands)

    Walraven, J.J.; Ladon, A.W.; Keulemans, A.I.M.

    1968-01-01

    Logarithmic plots of gas chromatographic retention data for different classes of compds. on different pairs of stationary phases were constructed. A remarkable effect was found. Isomers are spread along parallel lines in a repeated pattern, forming a \\"roofing-tile\\" series. The scattering of points

  18. Development of analytical methods for the gas chromatographic determination of 1,2-epoxy-3-butene, 1,2:3,4-diepoxybutane, 3-butene-1,2-diol, 3,4-epoxybutane-1,2-diol and crotonaldehyde from perfusate samples of 1,3-butadiene exposed isolated mouse and rat livers

    Energy Technology Data Exchange (ETDEWEB)

    Bhowmik, S.; Schuster, A.; Filser, J.G.

    2003-07-01

    Mutagenicity and carcinogenicity of 1,3-butadiene (BD) highly probably results from epoxide metabolites as 1,2-epoxy-3-butene (EB), 1,2:3,4-diepoxybutane (DEB) and 3,4-epoxybutane-1,2-diol (EBD). A further metabolite crotonaldehyde (CA) has also been discussed to be relevant. So far, in BD exposed rodents only EB and DEB concentrations had been quantified. However, the methods used were either not very sensitive or instrumentally expensive. Therefore, the goal of the present work was to establish simple analytical methods selective and sensitive enough to determine all of these compounds and a further secondary BD intermediate, 3-butene-1,2-diol (B-diol), in BD exposed rodent livers. The once-through perfused liver system was chosen for testing the applicability of the methods to be developed, since it enables BD exposures of this quantitatively most relevant metabolising organ near to the in-vivo situation. All the metabolites were extracted from the aqueous perfusion medium and analysed using a gas chromatograph equipped with a mass selective detector (GC/MS) in the PCI mode. (orig.)

  19. Educational On-Line Gaming Propensity

    DEFF Research Database (Denmark)

    Sudzina, Frantisek; Razmerita, Liana; Kirchner, Kathrin

    2014-01-01

    Educational on-line games are promising for new generations of students who are grown up digital. Th e new generations of students are technology savvy and spend lots of time on the web and on social networks. Based on an exploratory study, this article investigates the factors that infl uence...... students’ willingness to participate in serious games for teaching/learning. Th is study investigates the relationship between students’ behavior on Facebook, Facebook games, and their attitude toward educational on-line games. Th e results of the study reveal that the early adopters of educational games...... are likely to be students, who are young, have only a few Facebook connections, who currently play Facebook game(s). Furthermore, the study emphasizes that there may be differences between students coming from various countries....

  20. Trends in on-line data processing

    International Nuclear Information System (INIS)

    Masetti, M.

    1981-01-01

    The developement of integrated circuits has been characterized by an exponential growth of gates on a single chip that will still continue in the coming years. In parallel the price per bit is dropping down with more or less the same law. As a consequence of this a few statements can be made: The present 16-bit minicomputer in a small configuration is going to be substituted by a 16-bit microcomputer, and the 16-bit microcomputer in a powerful configuration by a 32-bit midi having also a virtual memory facility. Fully programmable or microcoded powerful devices like the LASS hardware processor or MICE, will allow an efficient on-line filter. Higher computing speed can be achieved by a multiprocessor configuration which can be insensitive to hardware failures. Therefore we are moving towards an integrated on-line computing system with much higher computing power than now and the present distinction between on-line and off-line will no longer be so sharp. As more processing can be performed on-line, fast high quality feed-back can be provided for the experiment. In the years to come the trend towards more processing power, at a lower price, and assembled in the same hardware volume will continue for at least five years; at the same time the future large high-energy physics experiments at LEP will be carried out within a wide international collaboration. In this environment methods must be found for a large fraction of the work to be distributed amongst the collaborators. To accomplish this aim it is necessary to introduce common standard practices concerning both hardware and software, in such a way that the seperate parts, developed by the collaborators, will be plug-compatible. (orig.)

  1. New Trends in on-line Marketing

    OpenAIRE

    Palkovič, Lukáš

    2011-01-01

    This bachelor thesis deals with new trend of internet marketing, it focuses especially on viral marketing. The theoretical part charasterizes the process of viral campaigns, furthermore deals with the components and aspects of on-line environment. Another separated chapter presents social networks, their place in viral marketing and at last but not least the viral video making process. The practical part contains different analyses of specific viral campaigns. The next and equally the last pa...

  2. On-Line Maintenance Methodology Development

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Hyo Won; Kim, Jae Ho; Jae, Moo Sung [Hanyang University, Seoul (Korea, Republic of)

    2012-05-15

    Most of domestic maintenance activities for nuclear power plants are performed while overhaul. Therefore, On-Line Maintenance (OLM) is one of the proper risks informed application techniques for diffusing maintenance burden during overhaul with safety of the plant is secured. The NUMARC 93-01 (Rev.3) presents the OLM state of the art and it provides methodology. This study adopts NUMARC 93-01 (Rev.3) and present OLM. The reference component is Emergency Diesel Generator (EDG) of Ulchin 3, 4

  3. Rapid differentiation of rocky mountain spotted fever from chickenpox, measles, and enterovirus infections and bacterial meningitis by frequency-pulsed electron capture gas-liquid chromatographic analysis of sera.

    Science.gov (United States)

    Brooks, J B; McDade, J E; Alley, C C

    1981-01-01

    Normal sera and sera from patients with Rocky Mountain spotted fever, chickenpox, enterovirus infections, measles, and Neisseria meningitidis infections were extracted with organic solvents under acidic and basic conditions and then derivatized with trichloroethanol or heptafluorobutyric anhydride-ethanol to form electron-capturing derivatives of organic acids, alcohols, and amines. The derivatives were analyzed by frequency-pulsed electron capture gas-liquid chromatography (FPEC-GLC). There were unique differences in the FPEC-GLC profiles of sera obtained from patients with these respective diseases. With Rocky Mountain spotted fever patients, typical profiles were detected as early as 1 day after onset of disease and before antibody could be detected in the serum. Rapid diagnosis of Rocky Mountain spotted fever by FPEC-GLC could permit early and effective therapy, thus preventing many deaths from this disease. PMID:7276147

  4. Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of semivolatile organic compounds in bottom sediment by solvent extraction, gel permeation chromatographic fractionation, and capillary-column gas chromatography/mass spectrometry

    Science.gov (United States)

    Furlong, E.T.; Vaught, D.G.; Merten, L.M.; Foreman, W.T.; Gates, Paul M.

    1996-01-01

    A method for the determination of 79 semivolatile organic compounds (SOCs) and 4 surrogate compounds in soils and bottom sediment is described. The SOCs are extracted from bottom sediment by solvent extraction, followed by partial isolation using high-performance gel permeation chromatography (GPC). The SOCs then are qualitatively identified and quantitative concentrations determined by capillary-column gas chromatography/mass spectrometry (GC/MS). This method also is designed for an optional simultaneous isolation of polychlorinated biphenyls (PCBs) and organochlorine (OC) insecticides, including toxaphene. When OCs and PCBs are determined, an additional alumina- over-silica column chromatography step follows GPC cleanup, and quantitation is by dual capillary- column gas chromatography with electron-capture detection (GC/ECD). Bottom-sediment samples are centrifuged to remove excess water and extracted overnight with dichloromethane. The extract is concentrated, centrifuged, and then filtered through a 0.2-micrometer polytetrafluoro-ethylene syringe filter. Two aliquots of the sample extract then are quantitatively injected onto two polystyrene- divinylbenzene GPC columns connected in series. The SOCs are eluted with dichloromethane, a fraction containing the SOCs is collected, and some coextracted interferences, including elemental sulfur, are separated and discarded. The SOC-containing GPC fraction then is analyzed by GC/MS. When desired, a second aliquot from GPC is further processed for OCs and PCBs by combined alumina-over-silica column chromatography. The two fractions produced in this cleanup then are analyzed by GC/ECD. This report fully describes and is limited to the determination of SOCs by GC/MS.

  5. On-line chemical sensors for applications in fast reactors

    International Nuclear Information System (INIS)

    Jayaraman, V.

    2015-01-01

    Hydrogen sensors are essential components of fast reactor sodium circuits. These sensors are needed in fast reactors for the immediate detection of any steam leak into sodium during reactor operation which can lead to failure of steam generator. Depending on the operating power of the reactor, sodium-water reaction results in either an increase in dissolved hydrogen level in sodium or an increase in hydrogen content of argon cover gas used above sodium coolant. Hence, on-line monitoring of hydrogen continuously in sodium and cover circuits helps in detection of any steam leak. In the event of accidental leak of high temperature sodium, it reacts with oxygen and moisture in air leading to sodium fires. These fires produce sodium aerosol containing oxides of sodium (Na 2 O and Na 2 O 2 ) and NaOH. For early detection of sodium fires, sensor systems based on sodium ionization detector, pH measurement and modulation of conductivity of graphite films are known in the literature. This presentation deals with the development of on-line sensors for these two applications. A diffusion based sensor using a thin walled nickel coil at 773 K and a sensitive thermal conductivity detector (TCD) has been developed for monitoring hydrogen levels in argon cover gas. This sensor has a lower detection limit of 30 ppm of hydrogen in argon. To extend the detection limit of the sensor, a surface conductivity based sensor has been developed which makes use of a thin film of semi-conducting tin oxide. Integration of this sensor with the TCD, can extend the lower detection limit to 2 ppm of hydrogen in cover gas. Electrochemical sensor based on sodium-beta-alumina has been designed, fabricated and its performance in laboratory and industrial environment was evaluated. This paper presents the logical development of these sensors highlighting their merits and limitations

  6. More than 170 polyunsaturated tocopherol-related compounds in a vitamin E capsule: Countercurrent chromatographic enrichment, gas chromatography/mass spectrometry analysis and preliminary identification of the potential artefacts.

    Science.gov (United States)

    Hammann, Simon; Kröpfl, Alexander; Vetter, Walter

    2016-12-09

    Tocopherols and tocotrienols (usually summed up as vitamin E) are a class of structurally related natural antioxidants. Commonly, only some of the eight classic representatives (four tocopherols and four tocotrienols) are found with varied composition in food. In this study we fractionated 230mg oil from commercial vitamin E supplement capsules by countercurrent chromatography (CCC) and subsequent analysis by gas chromatography with mass spectrometry (GC/MS) of silylated CCC fractions showed that these eight isomers represented only about 70% of total tocopherol compounds. Detailed analysis enabled the detection of 161T 3 isomers (α-, γ- and δ-T 3 ) along with 18 tetra- and several penta-unsaturated isomers (tocools), two tocomonoenol isomers, and several degradation products with shorter isoprenoid side chain (apo-tocools). Altogether, over 170 tocool compounds, most likely artefacts which originated from an inappropriate oil refining process were described in this study. Silver ion high performance liquid chromatography (Ag + -HPLC) was used to separate one fraction rich in γ-T 3 into four peaks each consisting of at least five peaks according to GC/MS. About ten γ-T 3 isomers were also detected in rice bran oils from one producer bought retail in Germany. Copyright © 2016 Elsevier B.V. All rights reserved.

  7. Liquid-liquid extraction/headspace/gas chromatographic/mass spectrometric determination of benzene, toluene, ethylbenzene, (o-, m- and p-)xylene and styrene in olive oil using surfactant-coated carbon nanotubes as extractant.

    Science.gov (United States)

    Carrillo-Carrión, Carolina; Lucena, Rafael; Cárdenas, Soledad; Valcárcel, Miguel

    2007-11-09

    BTEX-S compounds are widely distributed in the environment and can be present in different foodstuffs, including olive oil. Taking into account the risks of the exposure to these compounds, analytical methods for their determination in different matrices are mandatory. In this paper, the use of surfactant-coated multiwalled carbon nanotubes as additive in liquid-liquid extraction is applied for the determination of single-ring aromatic compounds in olive oil samples. After sample treatment, the aqueous extracts are subsequently analyzed by headspace/gas chromatography/mass spectrometry allowing the determination of BTEX-S within ca. 15 min. Each stage of the proposed LLE/HS/GC/MS configuration involves a selectivity enhancement avoiding the interference of other compounds of the sample matrix. Limits of detection were in the range 0.25 ng mL(-1) (obtained for ethylbenzene) and 0.43 ng mL(-1) (for benzene). The repeatability of the proposed method expressed as RSD varied between 1.9% (styrene) and 3.3% (benzene) (n=11).

  8. A novel analytical method of 1-(3-trifluoromethylphenyl piperazine and 1-(3-chlorophenyl piperazine in fluids of drug addicts using liquid-liquid extraction-gas chromatographic/nitrogen-phosphorous detection

    Directory of Open Access Journals (Sweden)

    Jing Chang

    2017-01-01

    Full Text Available In accordance with the research specifications and guidelines in China, we developed a novel experimental method to detect new piperazine-type drugs, such as 1-(3-trifluoromethylphenyl piperazine and 1-(3-chlorophenyl piperazine. In this study, a new pretreatment method and gas chromatography (GC/nitrogen-phosphorus detector detection technique were used to characterize these two kinds of drugs in urine and blood samples. For the purpose of isolation of these trace drugs from the samples, liquid-liquid extraction/solid-phase extraction was modified and validated for this specific study. The pretreatment method presented in this paper has many advantages, such as high recovery rate, high extraction efficiency, high detection sensitivity, low limit of detection, and simple operation. The GC/NPD instrument is popular in most laboratories because it can meet the routine requirements of forensic science. All these aspects make this combination of sample pretreatment and GC/NPD technique the most suitable choice for drug detection in biological samples.

  9. Comparison of a disposable sorptive sampler with thermal desorption in a gas chromatographic inlet, or in a dedicated thermal desorber, to conventional stir bar sorptive extraction-thermal desorption for the determination of micropollutants in water.

    Science.gov (United States)

    Wooding, Madelien; Rohwer, Egmont R; Naudé, Yvette

    2017-09-01

    The presence of micropollutants in the aquatic environment is a worldwide environmental concern. The diversity of micropollutants and the low concentration levels at which they may occur in the aquatic environment have greatly complicated the analysis and detection of these chemicals. Two sorptive extraction samplers and two thermal desorption methods for the detection of micropollutants in water were compared. A low-cost, disposable, in-house made sorptive extraction sampler was compared to SBSE using a commercial Twister sorptive sampler. Both samplers consisted of polydimethylsiloxane (PDMS) as a sorptive medium to concentrate micropollutants. Direct thermal desorption of the disposable samplers in the inlet of a GC was compared to conventional thermal desorption using a commercial thermal desorber system (TDS). Comprehensive gas chromatography coupled to time-of-flight mass spectrometry (GC × GC-TOFMS) was used for compound separation and identification. Ten micropollutants, representing a range of heterogeneous compounds, were selected to evaluate the performance of the methods. The in-house constructed sampler, with its associated benefits of low-cost and disposability, gave results comparable to commercial SBSE. Direct thermal desorption of the disposable sampler in the inlet of a GC eliminated the need for expensive consumable cryogenics and total analysis time was greatly reduced as a lengthy desorption temperature programme was not required. Limits of detection for the methods ranged from 0.0010 ng L -1 to 0.19 ng L -1 . For most compounds, the mean (n = 3) recoveries ranged from 85% to 129% and the % relative standard deviation (% RSD) ranged from 1% to 58% with the majority of the analytes having a %RSD of less than 30%. Copyright © 2017 Elsevier B.V. All rights reserved.

  10. Development of a fast and simple gas chromatographic protocol based on the combined use of alkyl chloroformate and solid phase microextraction for the assay of polyamines in human urine.

    Science.gov (United States)

    Naccarato, Attilio; Elliani, Rosangela; Cavaliere, Brunella; Sindona, Giovanni; Tagarelli, Antonio

    2018-05-11

    Polyamines are aliphatic amines with low molecular weight that are widely recognized as one of the most important cancer biomarkers for early diagnosis and treatment. The goal of the work herein presented is the development of a rapid and simple method for the quantification of free polyamines (i.e., putrescine, cadaverine, spermidine, spermine) and N-monoacetylated polyamines (i.e., N 1 -Acetylspermidine, N 8 -Acetylspermidine, and N 1 -Acetylspermine) in human urine. A preliminary derivatization with propyl chloroformate combined with the use of solid phase microextraction (SPME) allowed for an easy and automatable protocol involving minimal sample handling and no consumption of organic solvents. The affinity of the analytes toward five commercial SPME coatings was evaluated in univariate mode, and the best result in terms of analyte extraction was achieved using the divinylbenzene/carboxen/polydimethylsiloxane fiber. The variables affecting the performance of SPME analysis were optimized by the multivariate approach of experimental design and, in particular, using a central composite design (CCD). The optimal working conditions in terms of response values are the following: extraction temperature 40 °C, extraction time of 15 min and no addition of NaCl. Analyses were carried out by gas chromatography-triple quadrupole mass spectrometry (GC-QqQ-MS) in selected reaction monitoring (SRM) acquisition mode. The developed method was validated according to the guidelines issued by the Food and Drug Administration (FDA). The satisfactory performances reached in terms of linearity, sensitivity (LOQs between 0.01 and 0.1 μg/mL), matrix effect (68-121%), accuracy, and precision (inter-day values between -24% and +16% and in the range 3.3-28.4%, respectively) make the proposed protocol suitable to be adopted for quantification of these important biomarkers in urine samples. Copyright © 2018 Elsevier B.V. All rights reserved.

  11. Chromatographic properties PLOT multicapillary columns.

    Science.gov (United States)

    Nikolaeva, O A; Patrushev, Y V; Sidelnikov, V N

    2017-03-10

    Multicapillary columns (MCCs) for gas chromatography make it possible to perform high-speed analysis of the mixtures of gaseous and volatile substances at a relatively large amount of the loaded sample. The study was performed using PLOT MCCs for gas-solid chromatography (GSC) with different stationary phases (SP) based on alumina, silica and poly-(1-trimethylsilyl-1-propyne) (PTMSP) polymer as well as porous polymers divinylbenzene-styrene (DVB-St), divinylbenzene-vinylimidazole (DVB-VIm) and divinylbenzene-ethylene glycol dimethacrylate (DVB-EGD). These MCCs have the efficiency of 4000-10000 theoretical plates per meter (TP/m) and at a column length of 25-30cm can separate within 10-20s multicomponent mixtures of substances belonging to different classes of chemical compounds. The sample amount not overloading the column is 0.03-1μg and depends on the features of a porous layer. Examples of separations on some of the studied columns are considered. Copyright © 2017 Elsevier B.V. All rights reserved.

  12. Project development and commercialisation of on-line analysis systems

    International Nuclear Information System (INIS)

    Watt, J.S.

    2000-01-01

    A project team first in the Australian Atomic Energy Commission (AAEC) and since 1982 in CSIRO has developed many on-line analysis systems for the mineral and energy industries. The development of these projects, usually lasting 7-10 years, has followed a common pattern of laboratory R and D, field trials, commercialisation and technology transfer. This successful pattern is illustrated using examples of the development of systems for the on-line analysis of mineral slurries, for determination of the ash content of coal on conveyors, and for determination of the flow rates of oil, water and gas in pipelines. The first two systems, licensed to Australian companies, are used world-wide. They are now the market leaders for radioisotope gauges in their application field. The third, the multiphase flow meter, was licensed in 1997 to an international company. This meter has even greater potential than the other two systems for economic benefit from its use and for numbers of installations. (author)

  13. On-line neutron activation analyzers

    International Nuclear Information System (INIS)

    Flahaut, V.; Colmon, A.

    1999-01-01

    A neutronic analyser has been designed to determine the composition of the flow of raw materials entering a cement factory on the conveyor belt. This new system gives a reliable analysis of the whole cargo that outdates the sampling or the usual surface analysis based on fluorescence spectrometry. The accuracy is about 1%.The neutrons interact with the materials on an average depth of 25 cm and are absorbed by nuclei, these nuclei produce photons whose energy is characteristic of the chemical element itself. The composition can be deduced by measuring the number of photons emitted and their energy. The analysis is made on-line and can concern the search for about 10 compounds. In the case of cement the list of compounds is: SiO 2 , CaO, Al 2 O 3 , Fe 2 O 3 , MgO, Na 2 O, TiO 2 , S, Mn 2 O 3 , K 2 O, and H 2 O. The neutron generator involves a deuterium ion source whose deuterium ions are accelerated by means of an electrical field and impinge on a tritiated target, the nuclear reactions between deuterium and tritium produce 14 MeV neutrons. This neutron analysing technique can be adapted to any need of on-line composition determination. (A.C.)

  14. Determinação de efedrinas em urina por cromatografia em fase gasosa (CG/DNP para o controle da dopagem no esporte Gas chromatographic method for the determination of ephedrines in urine for doping control purposes

    Directory of Open Access Journals (Sweden)

    Paula Rodrigues Garcia

    2005-09-01

    included in the prohibited list of substances by the International Olympic Committee (IOC. Urinary threshold concentrations were established (ephedrine and methylephedrine >10 µg/mL. The aim of this work was to develop and validate a method for the simultaneous determination of ephedrines present in urine samples for doping purposes by gas chromatography with nitrogenous-phosphorous detector (GC/NPD. The method was based on a liquid-liquid extraction of alkalinized urine and further derivatization with trifluoroacetic anhydride (TFA. The validated method showed to be simple, practical and linear at the studied concentrations range. Urine samples collected from volunteers, who reported the use of ephedrines, were submitted to the proposed method.

  15. Chromatographic, Spectroscopic and Mass Spectrometric Approaches for Exploring the Habitability of Mars in 2012 and Beyond with the Curiosity Rover

    Science.gov (United States)

    Mahaffy, Paul

    2012-01-01

    The Sample Analysis at Mars (SAM) suite of instruments on the Curiosity Rover of Mars Science Laboratory Mission is designed to provide chemical and isotopic analysis of organic and inorganic volatiles for both atmospheric and solid samples. The goals of the science investigation enabled by the gas chromatograph mass spectrometer and tunable laser spectrometer instruments of SAM are to work together with the other MSL investigations is to quantitatively assess habitability through a series of chemical and geological measurements. We describe the multi-column gas chromatograph system employed on SAM and the approach to extraction and analysis of organic compounds that might be preserved in ancient martian rocks.

  16. Liquid chromatographic-mass spectrometric method for ...

    African Journals Online (AJOL)

    Tropical Journal of Pharmaceutical Research ... Purpose: To develop and validate a simple, efficient and reliable Liquid chromatographic-mass spectrometric (LC-MS/MS) method for the quantitative determination of two dermatological drugs, ... By Country · List All Titles · Free To Read Titles This Journal is Open Access.

  17. Liquid chromatographic analysis of phenobarbitone, ethosuximide ...

    African Journals Online (AJOL)

    A liquid chromatographic method for the simultaneous assay of four anticonvulsant drugs, phenobarbitone, ethosuximide, phenytoin and carbamazepine on a polystyrene-divinyl benzene column is described. The method was developed by the systematic study of different types of co-polymer materials, type and ...

  18. Validated high performance liquid chromatographic (HPLC) method ...

    African Journals Online (AJOL)

    STORAGESEVER

    2010-02-22

    Feb 22, 2010 ... specific and accurate high performance liquid chromatographic method for determination of ZER in micro-volumes ... tional medicine as a cure for swelling, sores, loss of appetite and ... Receptor Activator for Nuclear Factor κ B Ligand .... The effect of ... be suitable for preclinical pharmacokinetic studies. The.

  19. Chromatographic characterisation, in vitro antioxidant and free ...

    African Journals Online (AJOL)

    Chromatographic fractionation and spectroscopic analysis of the ME4 fraction revealed the presence of four compounds namely garcinia biflavonoids GB1 and GB2, garcinal and garcinoic acid. These findings show that these four compounds are partly responsible for the great antioxidant potential of G. kola seeds.

  20. Identificação de compostos orgânicos e farmacêuticos em esgoto hospitalar utilizando cromatografia gasosa acoplada a espectrometria de massa Identification of organic and pharmaceutical compositions in hospital wastewater using a gas chromatograph coupled to mass spectrometry

    Directory of Open Access Journals (Sweden)

    Francisco Vieira Paiva

    2011-03-01

    Full Text Available Os resíduos líquidos provenientes dos estabelecimentos assistenciais de saúde são mais complexos do que os esgotos domésticos. Sua composição contém inúmeros compostos farmacêuticos, saneantes, elementos radiativos e de laboratórios. O conhecimento desses compostos pode auxiliar na escolha do tratamento adequado para esses esgotos e diminuir os impactos ambientais nos corpos receptores. A pesquisa foi realizada utilizando um sistema combinado (UASB e lodos ativados para tratar a água residuária de um hospital. Neste trabalho, foram realizadas análises físico-químicas para caracterização do esgoto e cromatografia gasosa acoplada à espectrometria de massa para identificação de compostos químicos farmacêuticos, podendo-se constatar a presença de inúmeros elementos residuais dos fármacos usados no hospital.Liquid waste residues from health care establishments are more complex than those from residential sewage. Their composition contains several pharmaceutical chemical composites, sanitizers, radioactive, and laboratorial elements. Knowing about these composites may aid in choosing the proper treatment for these sewages, and diminish the environmental impact in receptors. The study was carried out in a combined system (UASB and activated sludge to treat a hospital wastewater. In this experiment, material and chemical analyses were employed to trace sewage characteristics and gas chromatography associated with mass spectrometry to identify pharmacologic chemical composites, where innumerous residual elements were found in chromatographs.

  1. On line nuclear orientation: opportunity and challenge

    International Nuclear Information System (INIS)

    Stone, N.J.

    1985-01-01

    The development of the on-line nuclear orientation (OLNO) technique is reviewed. The present potential of the technique is discussed in the light of the attainable temperatures, the use of ion implantation and the required isotope flux. Limitations associated with spin-lattice relaxation are considered in some detail and a survey of accessible nuclei is presented. An outline comparison is given between OLNO and other methods for producing orientation of nuclei, for measuring nuclear spins and static moments and for the study of level structure and transition probabilities. The conclusion is drawn that the method in its present form has extensive potential over a wide range of nuclei. Future prospects for in-beam polarisation giving access to nuclei of shorter half lives are referred to briefly. (Auth.)

  2. An on-line diagnostic expert system

    International Nuclear Information System (INIS)

    Felkel, L.

    1987-01-01

    As experience with on-line information systems, experts systems and artificial intelligence tools grows, the authors retreat from the first euphoria that AI could help them solve the problem they were unable to solve with conventional programming. The major effort of the development time goes into building the knowledge-base. There is no such thing as a generic knowledge-base for nuclear power plants as there is, for example, for the diagnosis of a Boeing 747 aircraft. AI-methods, tools and hardware are still in a state which does not optimally lend itself to real-time application. The ability of developing prototype systems to investigate variants otherwise too costly to justify is one advantage that the authors gladly accept. Last, but no least the tools provide a flexible and adaptable user interface (desktop window systems) etc. The development of such tools in a project would be prohibitive and room for experimentation would be limited

  3. On-Line Algorithms and Reverse Mathematics

    Science.gov (United States)

    Harris, Seth

    In this thesis, we classify the reverse-mathematical strength of sequential problems. If we are given a problem P of the form ∀X(alpha(X) → ∃Zbeta(X,Z)) then the corresponding sequential problem, SeqP, asserts the existence of infinitely many solutions to P: ∀X(∀nalpha(Xn) → ∃Z∀nbeta(X n,Zn)). P is typically provable in RCA0 if all objects involved are finite. SeqP, however, is only guaranteed to be provable in ACA0. In this thesis we exactly characterize which sequential problems are equivalent to RCA0, WKL0, or ACA0.. We say that a problem P is solvable by an on-line algorithm if P can be solved according to a two-player game, played by Alice and Bob, in which Bob has a winning strategy. Bob wins the game if Alice's sequence of plays 〈a0, ..., ak〉 and Bob's sequence of responses 〈 b0, ..., bk〉 constitute a solution to P. Formally, an on-line algorithm A is a function that inputs an admissible sequence of plays 〈a 0, b0, ..., aj〉 and outputs a new play bj for Bob. (This differs from the typical definition of "algorithm", though quite often a concrete set of instructions can be easily deduced from A.). We show that SeqP is provable in RCA0 precisely when P is solvable by an on-line algorithm. Schmerl proved this result specifically for the graph coloring problem; we generalize Schmerl's result to any problem that is on-line solvable. To prove our separation, we introduce a principle called Predictk(r) that is equivalent to -WKL0 for standard k, r.. We show that WKL0 is sufficient to prove SeqP precisely when P has a solvable closed kernel. This means that a solution exists, and each initial segment of this solution is a solution to the corresponding initial segment of the problem. (Certain bounding conditions are necessary as well.) If no such solution exists, then SeqP is equivalent to ACA0 over RCA 0 + ISigma02; RCA0 alone suffices if only sequences of standard length are considered. We use different techniques from Schmerl to prove

  4. Software for on-line experiments

    International Nuclear Information System (INIS)

    Ivanchenko, I.M.

    1981-01-01

    A review of nowadays development state of software of on-line electron experiments is presented. The principles of organization of real time systems on second generation computer base are considered. The following methods for projections search are considered: combinator methods, global methods, methods of tracking, methods of a supporting band. The following methods for determining parameter estimates based on the Lorentz equation are analysed: analytical simulation of trajectories, determination of parameters by the iterative method using the technique of calculation of recycled integrals, multidimensional statistical analysis. For the purpose of successful usage and development of software the technique of selfdocumented programs is created and the computer is applied for preparing, revising and circulation of external descriptions which as program complexes are constructed according to the hierarchical principle [ru

  5. On line protection systems for induction motors

    International Nuclear Information System (INIS)

    Colak, I.; Celik, H.; Sefa, I.; Demirbas, S.

    2005-01-01

    Protection of induction motors is very important since they are widely used in industry for many applications due to their high robustness, reliability, low cost and maintenance, high efficiency and long service life. So, protecting these motors is crucial for operations. This paper presents a combined protection approach for induction motors. To achieve this, the electrical values of the induction motor were measured with sensitivity ±1% through a data acquisition card and processed with software developed in Visual C++. An on line protection system for induction motors was achieved easily and effectively. The experimental results have shown that the induction motor was protected against the possible problems faced during the operation. The software developed for this protection provides flexible and reliable media for operators and their motors. It is expected that the motor protection achieved in this study might be faster than the classical techniques and also may be applied to larger motors easily after small modifications of the software

  6. Aprender a innovar: una experiencia on line

    Directory of Open Access Journals (Sweden)

    Joaquín MORENO MARCHAL

    2014-11-01

    Full Text Available La creatividad y la innovación se han convertido en recursos clave en la denominada sociedad del conocimiento, que bien podría ser también llamada sociedad de la innovación. Pero innovar es una actividad compleja, que integra la aplicación de múltiples capacidades, el pensamiento divergente y convergente, la gestión de equipos humanos, la comunicación. Ahora bien, a innovar se puede, y se debe, aprender. Aprender a innovar es un reto y también una obligación para el conjunto del sistema educativo en todos sus niveles. Partiendo de estas consideraciones este trabajo expone una experiencia de aprendizaje de la creatividad y de la innovación a través de un curso totalmente on line basado en la plataforma MOODLE, en el marco del Programa de Formación Permanente de la Universidad de Cádiz. Se presenta un modelo del proceso de innovación, denominado CREALAB, de elaboración propia. Este modelo se ha utilizado como base del proceso de aprendizaje de la creatividad y de la innovación y en el diseño del curso, está organizado en torno a actividades y tiene un carácter iterativo y realimentado. Se presentan además el conjunto del diseño metodológico y los resultados obtenidos en las dos ediciones celebradas hasta el momento. El diseño del curso totalmente on line y los resultados alcanzados permiten estimar un alto potencial de aplicación, tanto a nivel personal como a nivel organizacional.

  7. Effects of chromatographic fractions of Euphorbia hirta on the rat ...

    African Journals Online (AJOL)

    The effects of the chromatographic fractions of Euphorbia hirta Linn on the serum biochemical parameters in rats were investigated. The ethanolic extract of this plant was subjected to chromatographic separation using the vacuum liquid chromatographic technique, a modified form of classical column chromatography.

  8. Chromatographic assay of degradation products of tributyl phosphate

    International Nuclear Information System (INIS)

    Tripathi, S.C.; Ramanujam, A.; Nadkarni, M.N.; Rao, K.A.; Bandyopadhyay, C.

    1985-01-01

    Gas-liquid chromatography (GLC) and thin-layer chromatographic (TLC) procedures have been developed for the estimation of monobutyl phosphoric acid (H 2 MBP) and dibutyl phosphoric acid (HDBP) present in tributyl phosphate (TBP). Less than one microgram of H 2 MBP and HDBP is visually detected on TLC plate made of silicagel-cellulose (1:1). HDBP as separated by TLC has been quantitatively estimated in the range of 40-260 μg using an indirect spectrophotometric method. GLC method using 10 percent (W/W) XE-60 column can be effectively used for the simultaneous determination of 0.25 percent W/V H 2 MBP and HDBP present in 30 percent TBP-n-dodecane. The sensitivity may be enhanced 100 fold by careful column conditioning and judicious control of operational parameters. (author)

  9. Chromatographic separation of radioactive noble gases from xenon

    Science.gov (United States)

    Akerib, D. S.; Araújo, H. M.; Bai, X.; Bailey, A. J.; Balajthy, J.; Beltrame, P.; Bernard, E. P.; Bernstein, A.; Biesiadzinski, T. P.; Boulton, E. M.; Bramante, R.; Cahn, S. B.; Carmona-Benitez, M. C.; Chan, C.; Chiller, A. A.; Chiller, C.; Coffey, T.; Currie, A.; Cutter, J. E.; Davison, T. J. R.; Dobi, A.; Dobson, J. E. Y.; Druszkiewicz, E.; Edwards, B. N.; Faham, C. H.; Fiorucci, S.; Gaitskell, R. J.; Gehman, V. M.; Ghag, C.; Gibson, K. R.; Gilchriese, M. G. D.; Hall, C. R.; Hanhardt, M.; Haselschwardt, S. J.; Hertel, S. A.; Hogan, D. P.; Horn, M.; Huang, D. Q.; Ignarra, C. M.; Ihm, M.; Jacobsen, R. G.; Ji, W.; Kamdin, K.; Kazkaz, K.; Khaitan, D.; Knoche, R.; Larsen, N. A.; Lee, C.; Lenardo, B. G.; Lesko, K. T.; Lindote, A.; Lopes, M. I.; Manalaysay, A.; Mannino, R. L.; Marzioni, M. F.; McKinsey, D. N.; Mei, D.-M.; Mock, J.; Moongweluwan, M.; Morad, J. A.; Murphy, A. St. J.; Nehrkorn, C.; Nelson, H. N.; Neves, F.; O'Sullivan, K.; Oliver-Mallory, K. C.; Palladino, K. J.; Pease, E. K.; Pech, K.; Phelps, P.; Reichhart, L.; Rhyne, C.; Shaw, S.; Shutt, T. A.; Silva, C.; Solovov, V. N.; Sorensen, P.; Stephenson, S.; Sumner, T. J.; Szydagis, M.; Taylor, D. J.; Taylor, W.; Tennyson, B. P.; Terman, P. A.; Tiedt, D. R.; To, W. H.; Tripathi, M.; Tvrznikova, L.; Uvarov, S.; Verbus, J. R.; Webb, R. C.; White, J. T.; Whitis, T. J.; Witherell, M. S.; Wolfs, F. L. H.; Yazdani, K.; Young, S. K.; Zhang, C.

    2018-01-01

    The Large Underground Xenon (LUX) experiment operates at the Sanford Underground Research Facility to detect nuclear recoils from the hypothetical Weakly Interacting Massive Particles (WIMPs) on a liquid xenon target. Liquid xenon typically contains trace amounts of the noble radioactive isotopes 85Kr and 39Ar that are not removed by the in situ gas purification system. The decays of these isotopes at concentrations typical of research-grade xenon would be a dominant background for a WIMP search experiment. To remove these impurities from the liquid xenon, a chromatographic separation system based on adsorption on activated charcoal was built. 400 kg of xenon was processed, reducing the average concentration of krypton from 130 ppb to 3.5 ppt as measured by a cold-trap assisted mass spectroscopy system. A 50 kg batch spiked to 0.001 g/g of krypton was processed twice and reduced to an upper limit of 0.2 ppt.

  10. Time-resolved chromatographic analysis and mechanisms in adsorption and catalysis.

    Science.gov (United States)

    Roubani-Kalantzopoulou, Fani

    2009-03-06

    The main object of this review is the study of fundamentals of adsorption and heterogeneous catalysis, a benefit for the understanding of adsorptive and catalytic properties. This work aims to define and record, with the utmost accuracy, the phenomena and the possible reactions. A new methodology for the study of the adsorption is presented, which is a version of the well-known inverse gas chromatography. This reversed-flow inverse gas chromatography (RF-IGC) is technically very simple, and it is combined with a mathematical analysis that gives the possibility for the estimation of various physicochemical parameters related to adsorbent or catalyst characterization, under conditions compatible with the operation of real adsorbents and catalysts. On this base, this methodology has been successfully applied to the study of the impact of air pollutants, volatile organic and/or inorganic, on many solids such as marbles, ceramics, oxide-pigments of works of art, building materials, authentic statues of the Greek Archaeological Museums. Moreover, this methodology proved to be a powerful tool for studying the topography of active sites of heterogeneous surfaces in the nano-scale domain. Thus, some very important local quantities for the surface chemistry have been determined experimentally for many solids including thin films. These physicochemical local quantities (among which adsorption energy and entropy, surface diffusion coefficient, probability density function) have been determined from the experimental pairs of height of extra chromatographic peaks and time by a nonlinear least-squares method, through personal computer programs written in GW BASIC and lately in FORTRAN. Through the time-resolved analysis the surface characterization of the examined materials took place. In addition, the kinetic constants responsible for adsorption/desorption and surface chemical reactions have also been calculated. Thus, important answers have been provided to the following

  11. On-line fuel and control rod integrity management in BWRs

    International Nuclear Information System (INIS)

    Larsson, Irina; Sihver, Lembit

    2011-01-01

    Surveillance of fuel and control rod integrity in a BWR core is essential to maintain a safe and reliable operation of a nuclear power plant. An accurate and prompt way to monitor fuel integrity in a reactor core during reactor operation is by using on-line measurements of the gamma emitting noble gas activities in the off-gas system. The integrity of control rods can be efficiently followed by on-line measurements of the helium (He) concentration in the off-gases. This method also gives information about fuel rod failures since He is used as a fill gas in the fuel rods. To survey fuel and control rod integrity during reactor operation, a system consisting of combined gamma and He on-line measurements in the off-gases should be used. Such a system can detect and follow the behavior of fuel and control rod failures. In addition, it can separate fuel failures from control rod failures since fuel rods contain both He and gamma emitting noble gases, while control rods only contain He. Moreover, the system is able to distinguish primary fuel failures from degradation of already existing ones. In this paper we present a combined system for on-line measurements of He and gamma emitting noble gases in the reactor off-gas system and measuring experiences from different BWRs. (author)

  12. On-line supercritical fluid extraction-supercritical fluid chromatography-mass spectrometry of polycyclic aromatic hydrocarbons in soil.

    Science.gov (United States)

    Wicker, A Paige; Carlton, Doug D; Tanaka, Kenichiro; Nishimura, Masayuki; Chen, Vivian; Ogura, Tairo; Hedgepeth, William; Schug, Kevin A

    2018-06-01

    On-line supercritical fluid extraction - supercritical fluid chromatography - mass spectrometry (SFE-SFC-MS) has been applied for the determination of polycyclic aromatic hydrocarbons (PAHs) in soil. The purpose of this study was to develop and validate the first on-line SFE-SFC-MS method for the quantification of PAHs in various types of soil. By coupling the sample extraction on-line with chromatography and detection, sample preparation is minimized, diminishing sample loss and contamination, and significantly decreasing the required extraction time. Parameters for on-line extraction coupled to chromatographic analysis were optimized. The method was validated for concentrations of 10-1500 ng of PAHs per gram of soil in Certified Reference Material (CRM) sediment, clay, and sand with R 2  ≥ 0.99. Limits of detection (LOD) were found in the range of 0.001-5 ng/g, and limits of quantification (LOQ) in the range of 5-15 ng/g. The method developed in this study can be effectively applied to the study of PAHs in the environment, and may lay the foundation for further applications of on-line SFE-SFC-MS. Copyright © 2018 Elsevier B.V. All rights reserved.

  13. Development of an On-Line Uranium Enrichment Monitor

    International Nuclear Information System (INIS)

    Xuesheng, L.; Guorong, L.; Yonggang, Z.; Xueyuan, H. X.-Y.

    2015-01-01

    An on-line enrichment monitor was developed to measure the enrichment of UF6 flowing through the processing pipes in centrifuge uranium enrichment plant. A NaI(Tl) detector was used to measure the count rates of the 186 keV gamma ray emitted from 235U, and the total quantity of uranium was determined from thermodynamic characteristics of gaseous uranium hexafluoride. The results show that the maximum relative standard deviation is less than 1% when the measurement time is 120 s or more and the pressure is more than 2 kPa in the measurement chamber. There are two working models for the monitor. The monitor works normally in the continuous model, When the gas's pressure in the pipe fluctuates greatly, it can work in the intermittent model, and the measurement result is very well. The background of the monitor can be measured automatically periodically. It can control automatically electromagnetic valves open and close, so as to change the gas's quantity in the chamber. It is a kind of unattended and remote monitor, all of data can be transfer to central control room. It should be effective for nuclear materials accountability verifications and materials balance verification at uranium enrichment plant by using the monitor to monitor Uranium enrichment of gaseous uranium hexafluoride in the output end of cascade continuously. (author)

  14. Principles of qualitative analysis in the chromatographic context.

    Science.gov (United States)

    Valcárcel, M; Cárdenas, S; Simonet, B M; Carrillo-Carrión, C

    2007-07-27

    This article presents the state of the art of qualitative analysis in the framework of the chromatographic analysis. After establishing the differences between two main classes of qualitative analysis (analyte identification and sample classification/qualification) the particularities of instrumental qualitative analysis are commented on. Qualitative chromatographic analysis for sample classification/qualification through the so-called chromatographic fingerprint (for complex samples) or the volatiles profile (through the direct coupling headspace-mass spectrometry using the chromatograph as interface) is discussed. Next, more technical exposition of the qualitative chromatographic information is presented supported by a variety of representative examples.

  15. Comparison of chromatographic methods for the determination of bound glycerol in biodiesel

    Energy Technology Data Exchange (ETDEWEB)

    Foglia, T.A.; Jones, K.C.; Nunez, A.; Phillips, J.G. [U.S. Dept. of Agriculture, Agricultural Research Service, Eastern Regional Research Center, Wyndmoor, PA (United States); Mittelbach, M. [Inst. for Chemistry, Univ. of Graz, Graz (Austria)

    2004-09-01

    An important fuel criterion for biodiesel is bound glycerol, which is a function of the residual amount of triglycerides and partial glycerides in the biodiesel. Either high-temperature gas chromatography or high performance liquid chromatography can be used for determining these minor but important components in biodiesel. In this paper we have conducted a statistical study on the accuracy of the two methods for ascertaining the bound glycerol in biodiesel fuels obtained from different feedstocks. Analysis of variance showed that with one exception, namely diacylglycerols in some soy oil based biodiesel, there was no statistical difference in bound glycerol for the biodiesel samples analyzed or a difference between methods. Operationally, the high performance liquid chromatographic method is superior to the high temperature gas chromatographic method in that it requires no sample derivatization, has shorter analysis times, and is directly applicable to most biodiesel fuels. (orig.)

  16. On-line maintenance at Cofrentes NPP

    International Nuclear Information System (INIS)

    Roldan Vilches, J.; Moreno Matarranz, M. A.; Hermana Mendioroz, I.

    1998-01-01

    Cofrentes NPP has begun in 1997 activities related to At Power Preventive Maintenance over trains or systems which lead to a voluntary entry in a Limitative Condition of Operation (LCO) of the Technical Specifications. From others benefits, this program ha improved the risk management and the staff's knowledge over the functions and safety implications of the different systems, the better exploit of the resources, the co-ordination of the different organisations involved (Maintenance an Operation) and the reductions of works during shutdowns. Previous to each work, a feasibility study analyzes qualitative and quantitative (PSA), using the Risk Monitor, the implications on safety of all the tasks, assuring that the global safety of the Plant is always maintained. Tech. Spec. are analyzed in detail and also are analyzed situations of simultaneous unavailabilities of systems which could lead to a high risk situation. Two different risk controls are defined (punctual and accumulated) to assure that high risk situations will not be given. Finally, historical risk profile is analyzed to assure that the accumulated risk increase is not significant. Risk Monitor helps staff in the schedule and follow-up of the activities of On-Line Maintenance. Each one of the tasks are deeply planned and harshly analyzed and are carried out by high qualified workers. By the moment, this program is running with fully satisfaction on the Plant. (Author)

  17. SOL: INNOVACIÓN ON-LINE

    Directory of Open Access Journals (Sweden)

    Rubén Faúndez

    2007-11-01

    Full Text Available Las aplicaciones de simulación tienden a ser cada vez más cercanas a usuarios e industrias. Sin embargo, muchas de ellas no poseen ni la capacidad ni el conocimiento como para desarrollar internamente sus modelos de simulación. Por este motivo, y como una forma de apoyar la toma de decisiones basándose en modelos de simulación, se presenta la plataforma SOL (Simulación On Line. La metodología completa de trabajo, así como la interacción entre SOL, Empresa y Asesor, son presentadas. Su base de datos, los niveles de usuarios, sus funcionalidades, y la creación automatizada de información grafica y visual, también son explicadas. En el caso de aplicación, el uso de SOL para apoyar la toma de decisiones en una operación de movimiento de material, permite a los tomadores de decisión acceder a análisis robustos basados en información extraída de los modelos de simulación. SOL, al almacenar información, funcionar vía web, generar análisis automatizados y crear visualizaciones, permite cumplir con las expectativas de los usuarios respecto a una solución integral en simulación.

  18. Simplified automatic on-line document searching

    International Nuclear Information System (INIS)

    Ebinuma, Yukio

    1983-01-01

    The author proposed searching method for users who need not-comprehensive retrieval. That is to provide flexible number of related documents for the users automatically. A group of technical terms are used as search terms to express an inquiry. Logical sums of the terms in the ascending order of frequency of the usage are prepared sequentially and automatically, and then the search formulas, qsub(m) and qsub(m-1) which meet certain threshold values are selected automatically also. Users justify precision of the search output up to 20 items retrieved by the formula qsub(m). If a user wishes more than 30% of recall ratio, the serach result should be output by qsub(m), and if he wishes less than 30% of it, it should be output by qsub(m-1). The search by this method using one year volume of INIS Database (76,600 items) and five inquiries resulted in 32% of recall ratio and 36% of precision ratio on the average in the case of qsub(m). The connecting time of a terminal was within 15 minutes per an inquiry. It showed more efficiency than that of an inexperienced searcher. The method can be applied to on-line searching system for database in which natural language only or natural language and controlled vocabulary are used. (author)

  19. On-Line Impact Load Identification

    Directory of Open Access Journals (Sweden)

    Krzysztof Sekuła

    2013-01-01

    Full Text Available The so-called Adaptive Impact Absorption (AIA is a research area of safety engineering devoted to problems of shock absorption in various unpredictable scenarios of collisions. It makes use of smart technologies (systems equipped with sensors, controllable dissipaters and specialised tools for signal processing. Examples of engineering applications for AIA systems are protective road barriers, automotive bumpers or adaptive landing gears. One of the most challenging problems for AIA systems is on-line identification of impact loads, which is crucial for introducing the optimum real-time strategy of adaptive impact absorption. This paper presents the concept of an impactometer and develops the methodology able to perform real-time impact load identification. Considered dynamic excitation is generated by a mass M1 impacting with initial velocity V0. An analytical formulation of the problem, supported with numerical simulations and experimental verifications is presented. Two identification algorithms based on measured response of the impacted structure are proposed and discussed. Finally, a concept of the AIA device utilizing the idea of impactometer is briefly presented.

  20. Application of on-line analytical processing technique in accelerator

    International Nuclear Information System (INIS)

    Xie Dong; Li Weimin; He Duohui; Liu Gongfa; Xuan Ke

    2005-01-01

    A method of application of the on-line analytical processing technique in accelerator is described, which includes data pre-processing, the process of constructing of data warehouse and on-line analytical processing. (authors)

  1. Simultaneous Determination of Palladium and Platinum by On-line ...

    African Journals Online (AJOL)

    NJD

    using high performance liquid chromatography equipped with an on-line enrichment technique. Prior to ... The on-line enrichment system (Waters Corporation, USA) that was ... Using an appropriate volume (industrial plant effluents 20 mL,.

  2. Gas Chromatographic-Mass Spectrometric Analysis of Essential Oil ...

    African Journals Online (AJOL)

    hepatitis, dysmenorrhea, stomatitis, duodenitis and depression in south China [1]. There are few reports about its chemical constituents and pharmacological properties, such as the hydroalcoholic extract from the buds of. Jasminum grandiflorum showing preferable antiviral efficacy against HBV replication in. HepG2 2.2.15 ...

  3. Gas Chromatographic Analysis of Sulfur Mustard in Diethyl Phthalate

    National Research Council Canada - National Science Library

    Lancaster, Paul

    1998-01-01

    ...) that had been trapped in the solvent, diethyl phthalate (DEP) is described. The method utilises the improved sensitivity and selectivity offered by the new Pulsed Flame Photometric Detector to detect routinely samples containing...

  4. Gas chromatographic measurement of the radiolytic products of irradiated pork

    International Nuclear Information System (INIS)

    Zhou Yingcai; Wang Xiuying; Xu Peishu; Yuan Bihuai

    1988-01-01

    The radiolytic products of irradiated pork were isolated, analyzed and identified by the techniques of vacuum distillation, GC-MS. The higher boiling point compounds in fat were collected by cold-finger and its lower boiling point compounds were recovered on a short precolumn packed with alumina, and the volatiles of lean pork were collected on a short column packed with TCEP/Chromosovb. Some experimental conditions were studied. 49 compounds were identified. These compounds include hydrocarbons and sulphides etc. (author)

  5. Fluoroalkyl chloroformates in treating amino acids for gas chromatographic analysis

    Czech Academy of Sciences Publication Activity Database

    Hušek, Petr; Šimek, Petr; Hartvich, Petr; Zahradníčková, Helena

    2008-01-01

    Roč. 1186, 1/2 (2008), s. 391-400 ISSN 0021-9673 R&D Projects: GA ČR GA203/04/0192; GA ČR GA303/06/1674 Institutional research plan: CEZ:AV0Z50070508 Keywords : amino acids * derivatization * pentafluoropropyl- and heptafluorobutyl chloroformates Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.756, year: 2008

  6. Improvement of gas chromatographic analysis for organic acids and ...

    African Journals Online (AJOL)

    Yomi

    2010-08-27

    Aug 27, 2010 ... and ethanol fermentation by using the anaerobic bacterium. Clostridium ... GC analysis. Standard solution for GC analysis consisted of acetic acid (Sigma-. Aldrich ... Microorganism and inoculum preparation. C. beijerinckii ...

  7. Influence of visualization on consumption during on-line shopping

    OpenAIRE

    Hictaler, Urška

    2013-01-01

    This diploma work studies the influence of visualization on consumption during on-line shopping. The first part of the thesis starts with key areas of visualization, consumption and on-line shopping. Visualization, areas of use, human perception and ways of product presentation in on-line shops are defined discussed first. Next, consumption, consumers and factors that influence their decisions and satisfaction are defined. The last topic in the first part of the thesis discusses on-line shopp...

  8. Amalgam-chromatographic separation of magnesium isotopes

    International Nuclear Information System (INIS)

    Klinskij, G.D.; Levkin, A.V.; Ivanov, S.A.

    1990-01-01

    Separation of magnesium isotopes within Mg(Hg)-MgI 2 system (in dimethylformamide) is conducted under amalgam-chromatographic conditions. Separation maximal degree, that is (1.09), for 24 Mg and 26 Mg and separation coefficient (α = 1.0089±0.006) are determined. Light isotopes are found to concentrate in the amalgam. Technique of thermal conversion of flows within amalgam-dimethylformamide system is suggested on the basis of reversible reaction of Ca-Mg element exchange

  9. Validation for chromatographic and electrophoretic methods

    OpenAIRE

    Ribani, Marcelo; Bottoli, Carla Beatriz Grespan; Collins, Carol H.; Jardim, Isabel Cristina Sales Fontes; Melo, Lúcio Flávio Costa

    2004-01-01

    The validation of an analytical method is fundamental to implementing a quality control system in any analytical laboratory. As the separation techniques, GC, HPLC and CE, are often the principal tools used in such determinations, procedure validation is a necessity. The objective of this review is to describe the main aspects of validation in chromatographic and electrophoretic analysis, showing, in a general way, the similarities and differences between the guidelines established by the dif...

  10. Development of an on-line size exclusion chromatographic - reversed-phase liquid chromatographic two-dimensional system for the quantitative determination of peptides with concentration prior to reversed-phase liquid chromatographic separation

    NARCIS (Netherlands)

    Stroink, T.; Wiese, G.; Lingeman, H.; Bult, A.; Underberg, W.J.M.

    2001-01-01

    Complex samples, containing endogenous peptides require analytical methods with high sensitivity and selectivity to enable reliable analysis of these compounds in biological samples. In a number of cases, the selectivity of mono-dimensional separation systems is not sufficient. In order to improve

  11. A Distributed System for Learning Programming On-Line

    Science.gov (United States)

    Verdu, Elena; Regueras, Luisa M.; Verdu, Maria J.; Leal, Jose P.; de Castro, Juan P.; Queiros, Ricardo

    2012-01-01

    Several Web-based on-line judges or on-line programming trainers have been developed in order to allow students to train their programming skills. However, their pedagogical functionalities in the learning of programming have not been clearly defined. EduJudge is a project which aims to integrate the "UVA On-line Judge", an existing…

  12. Progress and performance of on-line analyzers of coal

    International Nuclear Information System (INIS)

    Spencer, C.M.; Brown, D.R.; Gozani, T.; Bozorgmanesh, H.; Bernatowicz, H.; Tassicker, O.J.; Karlson, F.

    1982-01-01

    This paper describes the past year's progress in the laboratory testing of the most comprehensive Nucoalyzer, the CONAC, and the performance of a Nucoalyzer-Sulfurmeter in special field tests. Previous papers and presentations provide more detailed background information. The near real-time analysis provided by a Nucoalyzer can be used in a variety of strategies to optimize efficiency of coal use. Nucoalyzers can be used to monitor coal deliveries and achieve uniformity in coal storage and recovery. In a coal cleaning plant, on-line analysis with a Nucoalyzer can lead to optimum Btu recovery while meeting specifications for the washed coal. A Nucoalyzer can monitor the blending of different coals to maintain a key cosntituent such as sulfur below a specified level, or can predict sulfur dioxide emissions, allowing feed-forward control to gas scrubbers and precipitators. Variability in coal feed to the boiler can lead to gross changes in thermodynamic efficiency in combustion. In addition, fouling and slagging incidents due to poor coal quality cause costly boiler shutdowns and maintenance. Nucoalyzer monitoring of key constituents and Btu in the coal feed allows operators to adjust boiler parameters for increased efficiency. To summarize, the primary advantages of Nucoalyzers relate to their ability to quickly identify changes in coal composition so that adjustments can be made in a timely manner to accommodate these changes in the process being monitored. Nucoalyzers are the only instruments available that can monitor the coal (for ash, Btu, sulfur, etc.) on-line and provide real-time continuous results. One Nucoalyzer is already working in the field, and by the time of the next Symposium we will have had performance reports on two more

  13. Analyzing chromatographic data using multilevel modeling.

    Science.gov (United States)

    Wiczling, Paweł

    2018-06-01

    It is relatively easy to collect chromatographic measurements for a large number of analytes, especially with gradient chromatographic methods coupled with mass spectrometry detection. Such data often have a hierarchical or clustered structure. For example, analytes with similar hydrophobicity and dissociation constant tend to be more alike in their retention than a randomly chosen set of analytes. Multilevel models recognize the existence of such data structures by assigning a model for each parameter, with its parameters also estimated from data. In this work, a multilevel model is proposed to describe retention time data obtained from a series of wide linear organic modifier gradients of different gradient duration and different mobile phase pH for a large set of acids and bases. The multilevel model consists of (1) the same deterministic equation describing the relationship between retention time and analyte-specific and instrument-specific parameters, (2) covariance relationships relating various physicochemical properties of the analyte to chromatographically specific parameters through quantitative structure-retention relationship based equations, and (3) stochastic components of intra-analyte and interanalyte variability. The model was implemented in Stan, which provides full Bayesian inference for continuous-variable models through Markov chain Monte Carlo methods. Graphical abstract Relationships between log k and MeOH content for acidic, basic, and neutral compounds with different log P. CI credible interval, PSA polar surface area.

  14. High performance liquid chromatographic determination of ...

    African Journals Online (AJOL)

    STORAGESEVER

    2010-02-08

    ) high performance liquid chromatography (HPLC) grade .... applications. These are important requirements if the reagent is to be applicable to on-line pre or post column derivatisation in a possible automation of the analytical.

  15. MHTGR steam generator on-line heat balance, instrumentation and function

    International Nuclear Information System (INIS)

    Klapka, R.E.; Howard, W.W.; Etzel, K.T.; Basol, M.; Karim, N.U.

    1991-09-01

    Instrumentation is used to measure the Modular High Temperature Gas-Cooled Reactor (MHTGR) steam generator dissimilar metal weld temperature during start-up testing. Additional instrumentation is used to determine an on-line heat balance which is maintained during the 40 year module life. In the process of calibrating the on-line heat balance, the helium flow is adjusted to yield the optimum boiling level in the steam generator relative to the dissimilar metal weld. After calibration is complete the weld temperature measurement is non longer required. The reduced boiling level range results in less restrictive steam generator design constraints

  16. On-Line Coolant Chemistry Analysis

    International Nuclear Information System (INIS)

    LM Bachman

    2006-01-01

    Impurities in the gas coolant of the space nuclear power plant (SNPP) can provide valuable indications of problems in the reactor and an overall view of system health. By monitoring the types and amounts of these impurities, much can be implied regarding the status of the reactor plant. However, a preliminary understanding of the expected impurities is important before evaluating prospective detection and monitoring systems. Currently, a spectroscopy system is judged to hold the greatest promise for monitoring the impurities of interest in the coolant because it minimizes the number of entry and exit points to the plant and provides the ability to detect impurities down to the 1 ppm level

  17. Performance and optimization of a combustion interface for isotope ratio monitoring gas chromatography/mass spectrometry

    Science.gov (United States)

    Merritt, D. A.; Freeman, K. H.; Ricci, M. P.; Studley, S. A.; Hayes, J. M.

    1995-01-01

    Conditions and systems for on-line combustion of effluents from capillary gas chromatographic columns and for removal of water vapor from product streams were tested. Organic carbon in gas chromatographic peaks 15 s wide and containing up to 30 nanomoles of carbon was quantitatively converted to CO2 by tubular combustion reactors, 200 x 0.5 mm, packed with CuO or NiO. No auxiliary source of O2 was required because oxygen was supplied by metal oxides. Spontaneous degradation of CuO limited the life of CuO reactors at T > 850 degrees C. Since NiO does not spontaneously degrade, its use might be favored, but Ni-bound carbon phases form and lead to inaccurate isotopic results at T Water must be removed from the gas stream transmitted to the mass spectrometer or else protonation of CO2 will lead to inaccuracy in isotopic analyses. Although thresholds for this effect vary between mass spectrometers, differential permeation of H2O through Nafion tubing was effective in both cases tested, but the required length of the Nafion membrane was 4 times greater for the more sensitive mass spectrometer.

  18. Determination of drugs in biological fluids by direct injection of samples for liquid-chromatographic analysis.

    Science.gov (United States)

    Mullett, Wayne M

    2007-03-10

    The analysis of drugs in various biological fluids is an important criterion for the determination of the physiological performance of a drug. After sampling of the biological fluid, the next step in the analytical process is sample preparation. The complexity of biological fluids adds to the challenge of direct determination of the drug by chromatographic analysis, therefore demanding a sample preparation step that is often time-consuming, tedious, and frequently overlooked. However, direct on-line injection methods offer the advantage of reducing sample preparation steps and enabling effective pre-concentration and clean-up of biological fluids. These procedures can be automated and therefore reduce the requirements for handling potentially infectious biomaterial, improve reproducibility, and minimize sample manipulations and potential contamination. The objective of this review is to present an overview of the existing literature with emphasis on advances in automated sample preparation methods for liquid-chromatographic methods. More specifically, this review concentrates on the use of direct injection techniques, such as restricted-access materials, turbulent-flow chromatography and other automated on-line solid-phase extraction (SPE) procedures. It also includes short overviews of emerging automated extraction-phase technologies, such as molecularly imprinted polymers, in-tube solid-phase micro-extraction, and micro-extraction in a packed syringe for a more selective extraction of analytes from complex samples, providing further improvements in the analysis of biological materials. Lastly, the outlook for these methods and potential new applications for these technologies are briefly discussed.

  19. On-line alkali monitoring - Part 1

    International Nuclear Information System (INIS)

    Andersson, Christer; Ljung, P.; Woxlin, H.

    1997-02-01

    As a consequence of the increased knowledge of the environmental impact of combustion based heat and power generation, the use of renewable biofuels will be increased. An obstacle associated to biofuel combustion compared to other fuels is the large release of alkali. Alkali compounds in flue gases are known to cause severe operational problems. Three of the major problems are; fouling of superheating tubes (causing reduced heat transfer and possibly corrosion), agglomeration of the bed material in fluidized beds, and poisoning of SCR catalysts. Yet another alkali related problem arises when, in order to increase the electric efficiency of combustion power plants, combined-cycle technology is used. Alkali vapour present in the fuel gas for the gas turbine is condensed to particles which increase corrosion and erosion of the turbine blades. The research on ash related operational problems has to be extended in order to ensure future use of biofuels in heat and power generation. In all successful research, adequate tools are necessary. To investigate ash related problems the key issue is to be able to perform continuous alkali measurements. This pilot study has investigated the need of continuous alkali measurements, which alkali species are harmful in the different applications and also available instrumentation capable of measuring the specific alkali species. The report gives a short summary presenting alkali related operational problems. In addition a schematic overview is given, showing the alkali species that possibly can exist in various parts of the power plant. 48 refs, 13 figs, 4 tabs

  20. On line system monitoring and analysis for efficient maintenance management [Paper No.: I-10

    International Nuclear Information System (INIS)

    Verma, R.M.P.

    1981-01-01

    Continuously operating chemical plants and nuclear reactors with huge investments cannot afford unscheduled shut down, costly down time, undesired exposure of people to radiation and high cost of inventory. To obtain cost effectiveness in terms of increased plant availability with increased quality, safety and reliability of plant operations a good maintenance system is required. A preventive maintenance programme, though successful to a greater extent, has got the limitations of being based upon elapsed time, subjective approach or statistical data. Hence, maintenance action is mistimed. Preventive maintenance can become very effective if rational and scientific data on equipment under working conditions are available. It can be achieved through on-line predictive instruments like sound level and vibration analyzers, probologs, corrosmeters, strain gages, thermographic infrared sensors, on-line ferrographs, chromatographs, acoustic emission, eddy current ultrasonic and wireless sensors etc. Instruments help maintenance engineer to diagnose, inspect, monitor, and help in forecasting failures and scheduling the frequencies optimally for overhauls, replacements, lubrication etc. They are also helpful in establishing work load, manpower, resource planning and inventory control. This paper discusses real time computer based system as well as conventional instruments and techniques. (author)

  1. The use of on-line ion chromatography for high temperature and high pressure reaction studies

    International Nuclear Information System (INIS)

    Lynch, G.J.

    1993-10-01

    This paper describes the use of on-line ion chromatography as a tool for chemistry reaction studies in small volume systems. The technique was used to study chemistry behavior in a high temperature and high pressure autoclave system. A dual analyzer, multi-channel on-line ion chromatograph (IC) was configured to automate the sampling and analysis. Analytical channels were set up for analysis of inorganic anions, monovalent cations, conductivity, and pH. Conductivity and pH were measured using the IC as a flow injection analyzer. Use of the IC system provides significant advantages over conventional sampling and analysis techniques: Reduction in sample volume, a closed sampling system that protects air or light sensitive analytes from breakdown, around-the-clock test performance combined with automatic calibration and quality control checking, and detection and tracking of reaction products or unexpected contaminants. Methods used to correct measured concentrations for the effects of sampling and for calculation of control chemical loss half-lives are presented. A limited evaluation of the flow injection analysis methods for conductivity and pH is provided

  2. Robust on-line monitoring of biogas processes; Robusta maettekniker on-line foer optimerad biogasproduktion

    Energy Technology Data Exchange (ETDEWEB)

    Nordberg, Aake; Hansson, Mikael; Kanerot, Mija; Krozer, Anatol; Loefving, Bjoern; Sahlin, Eskil

    2010-03-15

    Although demand for biomethane in Sweden is higher than ever, many Swedish codigestion plants are presently operated below their designed capacity. Efforts must be taken to increase the loading rate and guarantee stable operation and high availability of the plants. There are currently no commercial systems for on-line monitoring, and due to the characteristics of the material, including corrosion and tearing, robust applications have to be developed. The objective of this project was to identify and study different monitoring technologies with potential for on-line monitoring of both substrate mixtures and anaerobic digester content. Based on the prerequisites and demands at Boraas Energi och Miljoe AB's (BEMAB, the municipal energy and waste utility in the city of Boraas, Sweden) biogas plant, the extent of the problems, measurement variables and possible ways of managing these issues have been identified and prioritized. The substrate mixtures in question have a high viscosity and are inhomogeneous with variation in composition, which calls for further homogenization, dilution and filtration to achieve high precision in the necessary analyses. Studies of using different mixers and mills showed that the particle size (800 mum) needed for on-line COD measurement could not be achieved. The problem of homogenization can be avoided if indirect measurement methods are used. Laboratory tests with NIR (near-infra red spectroscopy) showed that VS can be predicted (R2=0,78) in the interval of 2-9% VS. Furthermore, impedance can give a measurement of soluble components. However, impedance is not sensitive enough to give a good measurement of total TS. Microwave technology was installed at the production plant and showed a faster response to changes in TS than the existing TS-sensor. However, due to technical problems, the evaluation only could be done during a limited period of ten days. BEMAB will continue the measurements and evaluation of the instrument. The

  3. On-line monitoring of methane in sewer air.

    Science.gov (United States)

    Liu, Yiwen; Sharma, Keshab R; Murthy, Sudhir; Johnson, Ian; Evans, Ted; Yuan, Zhiguo

    2014-10-16

    Methane is a highly potent greenhouse gas and contributes significantly to climate change. Recent studies have shown significant methane production in sewers. The studies conducted so far have relied on manual sampling followed by off-line laboratory-based chromatography analysis. These methods are labor-intensive when measuring methane emissions from a large number of sewers, and do not capture the dynamic variations in methane production. In this study, we investigated the suitability of infrared spectroscopy-based on-line methane sensors for measuring methane in humid and condensing sewer air. Two such sensors were comprehensively tested in the laboratory. Both sensors displayed high linearity (R(2) > 0.999), with a detection limit of 0.023% and 0.110% by volume, respectively. Both sensors were robust against ambient temperature variations in the range of 5 to 35°C. While one sensor was robust against humidity variations, the other was found to be significantly affected by humidity. However, the problem was solved by equipping the sensor with a heating unit to increase the sensor surface temperature to 35°C. Field studies at three sites confirmed the performance and accuracy of the sensors when applied to actual sewer conditions, and revealed substantial and highly dynamic methane concentrations in sewer air.

  4. Isotope Ratio Monitoring Gas Chromatography Mass Spectrometry (IRM-GCMS)

    International Nuclear Information System (INIS)

    Freeman, K.H.; Ricci, S.A.; Studley, A.; Hayes, J.M.

    1989-01-01

    On Earth, the C-13 content of organic compounds is depleted by roughly 13 to 23 permil from atmospheric carbon dioxide. This difference is largely due to isotope effects associated with the fixation of inorganic carbon by photosynthetic organisms. If life once existed on Mars, then it is reasonable to expect to observe a similar fractionation. Although the strongly oxidizing conditions on the surface of Mars make preservation of ancient organic material unlikely, carbon-isotope evidence for the existence of life on Mars may still be preserved. Carbon depleted in C-13 could be preserved either in organic compounds within buried sediments, or in carbonate minerals produced by the oxidation of organic material. A technique is introduced for rapid and precise measurement of the C-13 contents of individual organic compounds. A gas chromatograph is coupled to an isotope-ratio mass spectrometer through a combustion interface, enabling on-line isotopic analysis of isolated compounds. The isotope ratios are determined by integration of ion currents over the course of each chromatographic peak. Software incorporates automatic peak determination, corrections for background, and deconvolution of overlapped peaks. Overall performance of the instrument was evaluated by the analysis of a mixture of high purity n-alkanes of know isotopic composition. Isotopic values measured via IRM-GCMS averaged withing 0.55 permil of their conventionally measured values

  5. Ethanol production from lignocellulosic materials. Fermentation and on-line analysis

    Energy Technology Data Exchange (ETDEWEB)

    Olsson, L.

    1994-04-01

    The fermentation performance of bacteria, yeast and fungi was investigated in lignocellulosic hydrolysates with the aim of finding microorganisms which both withstand the inhibitors and that have the ability to ferment pentoses. Firstly, the performance of Saccharomyces cidri, Saccharomyces cerevisiae, Lactobacillus brevis, Lactococcus lactis ssp lactis, Escherichia coli and Zymomonas mobilis was investigated in spent sulphite liquor and enzymatic hydrolysate of steam-pretreated willow. Secondly, the performance of natural and recombinant E. coli, Pichia stipitis, recombinant S. cerevisiae, S. cerevisiae in combination with xylose isomerase and Fusarium oxysporum was investigated in a xylose-rich acid hydrolysate of corn cob. Recombinant E. coli was the best alternative for fermentation of lignocellulosic hydrolysates, giving both high yields and productivities. The main drawback was that detoxification was necessary. The kinetics of the fermentation with recombinant E. coli KO11 was investigated in the condensate of steam-pretreated willow. A cost analysis of the ethanol production from willow was made, which predicted an ethanol production cost of 3.9 SEK/l for the pentose fermentation. The detoxification cost constituted 22% of this cost. The monitoring of three monosaccharides and ethanol in lignocellulosic hydro lysates is described. The monosaccharides were determined using immobilized pyranose oxidase in an on-line amperometric analyser. Immobilization and characterization of pyranose oxidase from Phanerochaete chrysosporium is also described. The ethanol was monitored on-line using a micro dialysis probe as an in situ sampling device. The dialysate components were then separated in a column liquid chromatographic system and the ethanol was selectively detected by an amperometric alcohol bio sensor. The determinations with on-line analysis methods agreed well with off-line methods. 248 refs, 4 figs, 12 tabs

  6. DOE-EPRI On-Line Monitoring Implementation Guidelines

    International Nuclear Information System (INIS)

    E. Davis, R. Bickford

    2003-01-01

    Industry and EPRI experience at several plants has shown on-line monitoring to be very effective in identifying out-of-calibration instrument channels or indications of equipment-degradation problems. The EPRI implementation project for on-line monitoring has demonstrated the feasibility of on-line monitoring at several participating nuclear plants. The results have been very encouraging, and substantial progress is anticipated in the coming years

  7. The Separation of Hydrogen Tritium and Tritium Hydride by Gas Chromatography; Separation de l'hydrogene, du tritium et de l'hydrure de tritium par chromatographic en phase gazeuse; Razdelenie vodoroda, tritiya i gidrida tritiya posredstvom gazovoj khromatografii; Separacion del hidrogeno, tritio e hidruro de tritio por cromatografia de gases

    Energy Technology Data Exchange (ETDEWEB)

    Smith, H A; Carter, Jr, E H [University of Tennessee, Knoxville, TN (United States)

    1962-01-15

    Now that successful separation of hydrogen, deuterium and hydrogen deuteride has been achieved by gas chromatography, similar studies are being made dealing with mixtures of hydrogen, tritium and tritium hydride. Since tritium is used in tracer quantities the usual katharometer cannot be employed for its detection. This difficulty has been overcome by providing immediately following the katharometer a vibrating reed electrometer equipped with a high resistance leak which allows continuous monitoring of the activity of any tritium or tritium hydride emerging from the column by means of synchronized recorders. Separation of such mixtures has been tested with columns packed with palladium on silica, silica, alumina, and alumina coated with chromium oxide or ferric oxide. No effective separation was obtained with the palladium on silica column. Good separation was achieved with the plain silica column where hydrogen was employed as the carrier gas, but helium failed to elute the isotopes. Satisfactory results were obtained with the coated, partially deactivated alumina packing when helium or neon was the carrier gas, but the best separation was found with a column packing of uncoated activated alumina. Calibration with helium-tritium mixtures of known activity plus equilibrated hydrogen-tritium mixtures also of known activity allows quantitative estimation of tritium and tritium hydride. (author) [French] La separation de l'hydrogene, du deuterium et du deuterure d'hydrogene par chromatographic en phase gazeuse ayant ete realisee, on procede maintenant a des etudes semblables sur des melanges d'hydrogene de tritium et d'hydrure de tritium. Comme le tritium n'est present qu'en quantites infimes, on ne peut utiliser le catharometre ordinaire pour le detecter. On a surmonte cette difficulte en faisant suivre le catharometre d'un electrometre a lame vibrante, muni d'une fuite haute resistance, qui permet de mesurer, a l'aide d'enregistreurs synchronises, l'activite de

  8. Recent advances in metal-organic frameworks and covalent organic frameworks for sample preparation and chromatographic analysis.

    Science.gov (United States)

    Wang, Xuan; Ye, Nengsheng

    2017-12-01

    In the field of analytical chemistry, sample preparation and chromatographic separation are two core procedures. The means by which to improve the sensitivity, selectivity and detection limit of a method have become a topic of great interest. Recently, porous organic frameworks, such as metal-organic frameworks (MOFs) and covalent organic frameworks (COFs), have been widely used in this research area because of their special features, and different methods have been developed. This review summarizes the applications of MOFs and COFs in sample preparation and chromatographic stationary phases. The MOF- or COF-based solid-phase extraction (SPE), solid-phase microextraction (SPME), gas chromatography (GC), high-performance liquid chromatography (HPLC) and capillary electrochromatography (CEC) methods are described. The excellent properties of MOFs and COFs have resulted in intense interest in exploring their performance and mechanisms for sample preparation and chromatographic separation. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Supercritical Fluid Chromatographic Separation of Dimethylpolysiloxane Polymer

    Energy Technology Data Exchange (ETDEWEB)

    Pyo, Dong Jin; Lim, Chang Hyun [Kangwon National University, Chuncheon (Korea, Republic of)

    2005-02-15

    Water was used as a polar modifier and a μ-porasil column as a saturator column. The μ-porasil column was inserted between the pump outlet and the injection valve. During the passage of the supercritical fluid mobile phase through the silica column, a polar modifier (water) can be dissolved in the pressurized supercritical fluid. Dimethylpolysiloxane polymer has been known as more polar polymer than polystyrene polymer. Dimethylpolysiloxane polymer has never been separated using water modified mobile phase. In this paper, using a μ-porasil column as a saturator column, excellent supercritical fluid chromatograms of dimethylpolysiloxane oligomers were obtained. The use of compressed (dense) gases and supercritical fluids as chromatographic mobile phases in conjunction with liquid chromatographic (LC)-type packed columns was first reported by Klesper et al. in 1962. During its relatively short history, supercritical fluid chromatography (SFC) has become an attractive alternative to GC and LC in certain industrially important applications. SFC gives the advantage of high efficiency and allows the analysis of nonvolatile or thermally labile mixtures.

  10. Supercritical Fluid Chromatographic Separation of Dimethylpolysiloxane Polymer

    International Nuclear Information System (INIS)

    Pyo, Dong Jin; Lim, Chang Hyun

    2005-01-01

    Water was used as a polar modifier and a μ-porasil column as a saturator column. The μ-porasil column was inserted between the pump outlet and the injection valve. During the passage of the supercritical fluid mobile phase through the silica column, a polar modifier (water) can be dissolved in the pressurized supercritical fluid. Dimethylpolysiloxane polymer has been known as more polar polymer than polystyrene polymer. Dimethylpolysiloxane polymer has never been separated using water modified mobile phase. In this paper, using a μ-porasil column as a saturator column, excellent supercritical fluid chromatograms of dimethylpolysiloxane oligomers were obtained. The use of compressed (dense) gases and supercritical fluids as chromatographic mobile phases in conjunction with liquid chromatographic (LC)-type packed columns was first reported by Klesper et al. in 1962. During its relatively short history, supercritical fluid chromatography (SFC) has become an attractive alternative to GC and LC in certain industrially important applications. SFC gives the advantage of high efficiency and allows the analysis of nonvolatile or thermally labile mixtures

  11. Inexpensive on-line alcohol sensor for fermentation monitoring and control

    Energy Technology Data Exchange (ETDEWEB)

    Birch, S W; Turner, A P.F.; Ashby, R E

    1987-01-01

    An inorganic electrochemical fuel cell sensor was interfaced to a microcomputer and used to measure on-line the alcohol concentration in the off-gas of a fermentor. A calibration curve was obtained for methanol (linear range 0-9 g/l) and ethanol (linear range 0-6 g/l) to relate the alcohol concentration in the fermentor liquid with that in the off-gas. The consumption of methanol in a batch fermentation of the methylotroph Ps.BB1 was monitored (sampling frequency of 5 minutes) and compared with samples taken for off-line analysis by GLC. On-line control of the methanol concentration in a fed-batch fermentation was achieved by proportional and integral control. 24 references.

  12. Ion chromatographic determination of Di-n-butyl phosphate in degraded organic solvent

    International Nuclear Information System (INIS)

    Velavendan, P.; Pandey, N.K.; Kamachi Mudali, U.; Natarajan, R.

    2011-01-01

    In the present work a method for the determination of Di-n-butyl phosphate in organic streams using Ion Chromatography technique is developed and described here. The method involves the separation of Di-n-butyl phosphate (DBP) from 30% TBP-NPH (Tri-n-butylphosphate diluted in Normal Paraffin Hydrocarbon) and uranium/nitric acid matrix by an extraction of DBP in alkaline medium and subsequent ion-exchange separation in ion chromatography column followed by suppressed conductivity detection. Direct determination of DBP in lean/loaded organic solvent will lead to in accurate determination of DBP due to organic interference. DBP is quantified to lower limit of 1 ppm with 3% RSD. The results obtained with ion chromatographic technique are compared with those obtained by standard gas chromatographic technique. The developed method is much faster and total analysis can be completed within two hours. (author)

  13. Chromatographic Determination of Toluene and its Metabolites in Urine for Toluene Exposure - A Review

    International Nuclear Information System (INIS)

    Mohamad Raizul Zinalibdin; Abdul Rahim Yacob; Mohd Marsin Sanagi

    2016-01-01

    The determinations of toluene and their metabolites in biological samples such as urine and blood allow the estimation of the degree of exposure to this chemical. Chromatographic methods and preliminary methods are now universally employed for this purpose. Preliminary color test methods are well established for qualitative determination of toluene and its metabolites. Mobile test kits using color test methods are a vast tool for screening urine samples but chromatographic methods are still needed for confirmation and quantitative analysis. Gas chromatography (GC) methods are well-adapted for the determination of toluene metabolite in urine, but these methods often require several pretreatment steps. Meanwhile, high performance liquid chromatography (HPLC) is becoming a powerful tool for the accurate and easy determination of toluene metabolites considering its decisive advantages for routine monitoring. Furthermore, recent development in HPLC could widen the usefulness of this method to solve the most complex analytical problems that could be encountered during the measurement. (author)

  14. Radio Column Chromatographic Assay of H3-Labelled Substances

    International Nuclear Information System (INIS)

    Scharpenseel, H.W.; Menke, K.H.

    1962-01-01

    Combined radio-chromatographic investigations of H 3 -labelled substances are an integral part of the majority of biochemical experiments with H 3 -labelled compounds. H 3 -radio paper chromatography yields, in a scanner with a windowless flow counter, a counting efficiency of 0,5 -1,5%, depending largely on the thickness of the paper and the self-absorption of the labelled compound. The radio gas chromatography of tritiated compounds presents no major problem. Successful use is being made of a combination of a gas chromatograph with a flow ionization chamber and vibrating reed electrometer, a system originated by K. E. Wilzbach and P. Riessz, and improved by H. Dutton, L. Mason and L. Blair. Through the use of ''Teflon'' and silicone-rubber for the insulating parts of the flow ion chamber, it can be operated at close to 300 o C. Radio column chromatography with tritium holds little promise, when the column effluent is spread out as a shallow layer and slowly passes under a windowless flow counter or a scintillation counter, as was successfully tried with C 14 . Liquid scintillation spectrometry is likely to be the chosen method. Essentially, there are two different approaches feasible. These have been compared: 1. The column effluent is passed through a coil of plastic scintillator tubing, which is wound around a ''Plexiglas'' cylinder and placed in a bath of silicone oil in a light pipe with TiO 2 -reflector. Similarly, the HP-containing effluent can be directed through a test vial, filled - very much as in Steinberg's method - with plastic scintillator beads. These two approaches, that operate highly satisfactorily in the case of C 14 , offer low counting efficiencies of less than 1% for H 3 due to the unfavourable surface to volume ratio. 2. The column effluent is combined 1:30 with a mixture of 3:2 toluene/ethanol by the action of a magnet-vibrator before being assayed while passing through a K 40 -free glass - coiled between the analyser- and monitor

  15. Anionchromatografische analyse met een on-line eluens generator

    NARCIS (Netherlands)

    Neele J; Cleven RFMJ; LAC

    1999-01-01

    An automated sensitive and selective ion chromatographic method was developed and described for the simultaneous determinations of minor and major analytes in water. The study resulted in a method for the simultaneous determinations of fluoride, chloride, nitrite, nitrate, sulphate, bromide and

  16. Determination of insecticides malathion and lambda-cyhalothrin residues in zucchini by gas chromatography

    OpenAIRE

    Lofty, Hayam M.; Abd El-Aleem, Abd El-Aziz A.; Monir, Hany H.

    2013-01-01

    A sensitive gas chromatographic method has been developed for the determination of malathion and lambda-cyhalothrin (λ-cyhalothrin) insecticide residues in zucchini. The developed method consists of extraction with acetone, purification and partitioning with methylene chloride, column chromatographic clean-up, and finally capillary gas chromatographic determination of the insecticides. The recoveries of method were greater than 90% and limit of determination was 0.001 ppm for both insecticide...

  17. Gas analysis during the chemical vapor deposition of carbon

    International Nuclear Information System (INIS)

    Lieberman, M.L.; Noles, G.T.

    1973-01-01

    Gas chromatographic analyses were performed during the chemical vapor deposition of carbon in both isothermal and thermal gradient systems. Such data offer insight into the gas phase processes which occur during deposition and the interrelations which exist between gas composition, deposition rate, and resultant structure of the deposit. The results support a carbon CVD model presented previously. The application of chromatographic analysis to research, development, and full-scale facilities is shown. (U.S.)

  18. Algorithms for the on-line travelling salesman

    NARCIS (Netherlands)

    Ausiello, G.; Feuerstein, E.; Leonardi, S.; Stougie, L.; Talamo, M.

    1999-01-01

    In this paper the problem of efficiently serving a sequence of requests presented in an on-line fashion located at points of a metric space is considered. We call this problem the On-Line Travelling Salesman Problem (OLTSP). It has a variety of relevant applications in logistics and robotics. We

  19. An algorithm for on-line price discrimination

    NARCIS (Netherlands)

    D.D.B. van Bragt; D.J.A. Somefun (Koye); E. Kutschinski; J.A. La Poutré (Han)

    2002-01-01

    textabstractThe combination of on-line dynamic pricing with price discrimination can be very beneficial for firms operating on the Internet. We therefore develop an on-line dynamic pricing algorithm that can adjust the price schedule for a good or service on behalf of a firm. This algorithm (a

  20. On-Line Voltage Stability Assessment based on PMU Measurements

    DEFF Research Database (Denmark)

    Garcia-Valle, Rodrigo; P. Da Silva, Luiz C.; Nielsen, Arne Hejde

    2009-01-01

    This paper presents a method for on-line monitoring of risk voltage collapse based on synchronised phasor measurement. As there is no room for intensive computation and analysis in real-time, the method is based on the combination of off-line computation and on-line monitoring, which are correlat...

  1. From Off-line to On-line Handwriting Recognition

    NARCIS (Netherlands)

    Lallican, P.; Viard-Gaudin, C.; Knerr, S.

    2004-01-01

    On-line handwriting includes more information on time order of the writing signal and on the dynamics of the writing process than off-line handwriting. Therefore, on-line recognition systems achieve higher recognition rates. This can be concluded from results reported in the literature, and has been

  2. On-line Learning of Prototypes and Principal Components

    NARCIS (Netherlands)

    Biehl, M.; Freking, A.; Hölzer, M.; Reents, G.; Schlösser, E.; Saad, David

    1998-01-01

    We review our recent investigation of on-line unsupervised learning from high-dimensional structured data. First, on-line competitive learning is studied as a method for the identification of prototype vectors from overlapping clusters of examples. Specifically, we analyse the dynamics of the

  3. (E-2-Nonenal determination in brazilian beers using headspace solid-phase microextraction and gas chromatographic coupled mass spectrometry (HS-SPME-GC-MS Determinação de (E-2-nonenal em cervejas brasileiras utilizando microextração em fase sólida do headspace e cromatografia gasosa acoplada a espectrometria de massas

    Directory of Open Access Journals (Sweden)

    Rodrigo Scherer

    2010-05-01

    Full Text Available (E-2-nonenal is considered an important off-flavor of beer, related to the flavor of beer staling. In this study, a new method for determination of (E-2-nonenal in beer using headspace solid-phase microextraction and gas chromatographic coupled mass spectrometry (HS-SPME-GC-MS was developed and applied in Brazilian beer samples. The extractions were carried out in CAR-PDMS (carboxen-polydimethylsiloxane fiber and the best results were found with 15 minutes of equilibrium and 90 minutes of extraction at 50 °C. The method was linear in the range from 0.02 to 4.0 μg.L-1 with correlation coefficient of 0.9994. The limits of detection and quantification were 0.01 and 0.02 μg.L-1, respectively. 96.5% of recovery and 4% precision (RSD were obtained in the fortification of beer samples with 2.0 μg.L-1 of (E-2-nonenal. The developed method proved to be simple, efficient and highly sensitive to the determination of this analyte being easily applied in the quality control of the brewery. (E-2-nonenal was found in all beer samples analyzed with levels between 0.17 and 0.42 μg.L-1.O (E-2-nonenal é considerado um importante off-flavor da cerveja, sendo relacionado ao sabor de cerveja envelhecida. Neste estudo, um novo método para determinação de (E-2-nonenal em cerveja usando microextração em fase sólida do headspace e cromatografia a gás acoplada à espectrometria de massa (HS-SPME-GC-MS foi desenvolvido e aplicado em amostras de cerveja brasileira. As extrações foram realizadas utilizando a fibra CAR/PDMS (carboxen/polidimetilsiloxano, com 15 minutos de tempo de equilíbrio e 90 minutos de exposição da fibra a 50 °C. O método foi linear na faixa de 0,02 e 4,0 μg.L-1, com coeficiente de correlação de 0,9994. Os limites de detecção e quantificação foram 0,01 e 0,02 μg.L-1, respectivamente. Foram obtidos 96,5% de recuperação e 4% de variação entre replicatas de amostras de cerveja fortificadas com 2,0 μg.L-1 de (E-2-nonenal. O m

  4. Probabilistic peak detection for first-order chromatographic data

    NARCIS (Netherlands)

    Lopatka, M.; Vivó-Truyols, G.; Sjerps, M.J.

    2014-01-01

    We present a novel algorithm for probabilistic peak detection in first-order chromatographic data. Unlike conventional methods that deliver a binary answer pertaining to the expected presence or absence of a chromatographic peak, our method calculates the probability of a point being affected by

  5. On-line and bulk analysis for the resource industries

    International Nuclear Information System (INIS)

    Lim, C.S.; Sowerby, B.D.; Tickner, J.R.; Madsen, I.C.

    2001-01-01

    Nuclear techniques are the basis of many CSIRO on-line and bulk analysis systems that are now widely used in the mineral and energy industries. The continuous analysis and rapid response of these systems have led to improved control of mining, processing and blending operations. This paper reviews recent developments in neutron, gamma-ray and X-ray techniques for on-line and bulk analysis by CSIRO Minerals including neutron techniques for the on-conveyor belt determination of the composition of cement raw meal, the on-line analysis of composition in pyrometallurgical applications, the on-conveyor belt determination of ash in coal, and the rapid and accurate determination of gold in bulk laboratory samples. The paper also discusses a new gamma-ray technique for the on-line determination of ash in coal and the application of X-ray diffraction techniques for the on-line determination of mineralogy in the cement industry

  6. New extraction chromatographic material for rhenium separation

    International Nuclear Information System (INIS)

    Lucanikova, M.; Czech Technical University, Prague; Kucera, J.; Czech Technical University, Prague; Sebesta, F.

    2008-01-01

    Three types of the extraction chromatographic materials, composed from Aliquat R 336 deposited in the polyacrylonitrile (PAN) beads and prepared by different procedures, were compared for extraction of rhenium. The best properties were exhibited when the solid extractant was prepared by impregnation of the ready-made PAN beads. Solid extractant prepared by direct coagulation of the beads from the suspension of Aliquat R 336 in solution of PAN in nitric acid differs only by lower capacity in dynamic conditions. Material prepared from the PAN solution in dimethylsulfoxide was the worst because Aliquat R 336 was washed out from the beads during coagulation of the polymer and the extraction capacity was low. As it is shown, the first two solid extractants are fully comparable with the commercial TEVA Resin. (author)

  7. Aligning of single and multiple wavelength chromatographic

    DEFF Research Database (Denmark)

    Nielsen, Niels-Peter Vest; Carstensen, Jens Michael; Smedsgaard, Jørn

    1998-01-01

    optimised warping (COW) using two input parameters which can be estimated from the observed peak width. COW is demonstrated on constructed single trace chromatograms and on single and multiple wavelength chromatograms obtained from HPLC diode detection analyses of fungal extractsA copy of the C program......The use of chemometric data processing is becoming an important part of modern chromatography. Most chemometric analyses are performed on reduced data sets using areas of selected peaks detected in the chromatograms, which means a loss of data and introduces the problem of extracting peak data from...... to utilise the entire data matrix or rely on peak detection, thus having the same limitations as the commonly used chemometric procedures. The method presented uses the entire chromatographic data matrices and does not require any preprocessing e.g., peak detection. It relies on piecewise linear correlation...

  8. Brazilian organic sugarcane spirits: Physicochemical and chromatographic profile

    Directory of Open Access Journals (Sweden)

    Felipe Cimino Duarte

    Full Text Available ABSTRACT There has been a growing demand for products from organic agriculture for the food market. Brazil leads the production of sugarcane spirits and produces about 1.6 billion liters/year. New technologies have been sought throughout the supply chain to improve production, and organic raw material has been used in the production of sugar cane for the production of beverages. This study aimed to define the physicochemical and chromatographic profiles of eleven organic sugarcane spirits samples from various Brazilian states. The secondary components and contaminants were identified and quantified through physicochemical analyses, HPLC and gas chromatography (GC. A significant percentage of the organic sugarcane spirits samples contained concentrations of components that were above the limits required by the Ministry of Agriculture, Livestock and Provisioning (MAPA, specifically the esters (18.20%, copper and dry extract (9.10%. This contamination is caused by bad conditions employed during the production process, which are not in compliance with the good manufacturing practices determined and legislated by Brazilian law.

  9. Understanding on-line community: the affordances of virtual space

    Directory of Open Access Journals (Sweden)

    Karen Ruhleder

    2002-01-01

    Full Text Available Increasing numbers of on-line venues for learning are emerging as virtual communities become more accessible and commonplace. This paper looks at one particular virtual community, an on-line degree programme at the University of Illinois, Urbana-Champaign, which offers an M.S. in Library and Information Science (called LEEP. It draws on a framework presented by Mynatt, et al. (1998, which provides a lens for talking about on-line community as a set of affordances. This framework is applied to illustrate the interactions, artefacts, and expectations that shape this community.

  10. An Approach to On-line Risk Assessment in NPP

    International Nuclear Information System (INIS)

    Simic, Z.; Mikulicic, V.; O'Brien, J.

    1996-01-01

    Probabilistic Risk Assessment (PRA) can provide safety status information for a plant during different configurations; additional effort is needed to do this in real time for on-line operation. This paper describes an approach to use PRA to achieve these goals. A Risk Assessment On-Line (RAOL) application was developed to monitor maintenance (on-line and planned) activities. RAOL is based on the results from a full-scope PRA, engineering/operational judgment and incorporates a user friendly program interface approach. Results from RAOL can be used by planners or operations to effectively manage the level of risk by controlling the actual plant configuration. (author)

  11. On-line spectroscopy with thermal atomic beams

    International Nuclear Information System (INIS)

    Thibault, C.; Guimbal, P.; Klapisch, R.; Saint Simon, M. de; Serre, J.M.; Touchard, F.; Duong, H.T.; Jacquinot, P.; Juncar, P.

    1981-01-01

    On-line high resolution laser spectroscopy experiments have been performed in which the light from a cw tunable dye laser interacts at right angles with a thermal atomic beam. sup(76-98)Rb, sup(118-145)Cs and sup(208-213)Fr have been studied using the ionic beam delivered by the ISOLDE on-line mass separator at CERN while sup(20-31)Na and sup(38-47)K have been studied by setting the apparaturs directly on-line with the PS 20 GeV proton beam. The principle of the method is briefly explained and some results concerning nuclear structure are given. (orig.)

  12. Comparison of On-Line Maintenance Support Tools

    International Nuclear Information System (INIS)

    Simic, Z.; Follen, S. M.; Mikulicic, V.

    1998-01-01

    Modeling approach to on-line risk monitoring is today in a rapid developing phase. For that reason number of different solutions are available. This paper will attempt to present existing approaches to address on-line risk modeling problem Starting with description of on-line risk monitoring issues in general, then following by presentation of existing software tools (EPRI's Safety Monitor, Equipment Out of Service Monitor, and ORAM-SENTINEL) the current state of the art in this area will be demonstrated. Finally, conclusions and ideas will be outlined. (author)

  13. Gas chromatography at the Tritium Laboratory Karlsruhe

    International Nuclear Information System (INIS)

    Laesser, R.; Gruenhagen, S.

    2003-08-01

    Among the analytical techniques (mass spectrometry, laser Raman spectroscopy, gas chromatography, use of ionisation chambers) employed at the Tritium Laboratory Karlsruhe (TLK), gas chromatography plays a prominent role. The main reasons for that are the simplicity of the gas chromatographic separation process, the small space required for the equipment, the low investment costs in comparison to other methods, the robustness of the equipment, the simple and straightforward analysis and the fact that all gas species of interest (with the exception of water) can easily be detected by gas chromatographic means. The conventional gas chromatographs GC1 and GC2 used in the Tritium Measurement Techniques (TMT) System of the TLK and the gas chromatograph GC3 of the experiment CAPER are presented in detail, by discussing their flow diagrams, their major components, the chromatograms measured by means of various detectors, shortcomings and possible improvements. One of the main disadvantages of the conventional gas chromatography is the long retention times required for the analysis of hydrogen gas mixtures. To overcome this disadvantage, micro gas chromatography for hydrogen analysis was developed. Reduction of the retention times by one order of magnitude was achieved. (orig.)

  14. Nuclear techniques for on-line analysis in the mineral and energy industries

    International Nuclear Information System (INIS)

    Sowerby, B.D.; Watt, J.S.

    1994-01-01

    Nuclear techniques are the basis of many on-line analysis systems which are now widely used in the mineral and energy industries. Some of the systems developed by the CSIRO depend entirely on nuclear techniques; others use a combination of nuclear techniques and microwave, capacitance, or ultrasonic techniques. The continuous analysis and rapid response of these CSIRO systems has led to improved control of mining, processing and blending operations, with increased productivity valued at A$50 million per year to Australia, and $90 million per year world wide. This paper reviews developments in nuclear on-line analysis systems by the On-Line Analysis Group in CSIRO at Lucas Heights. Commercialised systems based on this work analyse mineral and coal slurries and determine the ash and moisture contents of coal and coke on conveyors. This paper also reviews two on-line nuclear analysis systems recently developed and licensed to industry, firstly for the determination of the mass flow rates of oil/water/gas mixtures in pipelines, and secondly for determination of the moisture, specific energy, ash and fouling index in low rank coals. 8 refs., 3 tabs., 4 figs

  15. Risk-based equipment removal guide for on-line maintenance at PSE ampersand G

    International Nuclear Information System (INIS)

    Knoll, A.; Smith, C.; Pollock, J.

    1995-01-01

    On-line maintenance plays an important role in achieving safe and reliable power generation in a nuclear power plant. However, maintenance, if not properly planned and performed, may also be an important contributor to plant risk. Therefore, plant-specific procedures are needed for equipment removal from service to enhance the benefits of on-line maintenance and minimize the risks involved. The problem is to identify and implement the most effective on-line maintenance policy in the form of a proceduralized guide to assure plant safety under various operation and maintenance constraints. This paper presents a methodology to develop plant-specific on-line maintenance strategies and acceptance criteria using a multivariate safety approach based on risk assessment. Based on plant-specific data as modeled in the individual plant evaluation (IPE) and the updated probabilistic safety assessment (PSA), the risk-based methodology is currently being applied to the development of proceduralized equipment removal guides at Hope Creek and Salem units 1 and 2 of Public Service Electric and Gas Company (PSE ampersand G)

  16. Liquid chromatographic determination with fluorescence detection of B6 vitamers and riboflavin in milk and pharmaceuticals

    International Nuclear Information System (INIS)

    Gatti, R.; Gioia, M.G.

    2005-01-01

    A simple, reliable and selective high performance liquid chromatographic method with fluorescence detection at different programmed wavelengths has been developed for the simultaneous analysis of B 6 vitamers (pyridoxal 5'-phosphate, 4-pyridoxic acid, pyridoxal, pyridoxine and pyridoxamine) and Vitamin B 2 in commercial vitaminized milk and in woman milk. The chromatographic separations were performed on a reversed phase octyl column by using a mobile phase consisting of sodium pentanesulfonate in 1% acetic acid-methanol-tetrahydrofuran under gradient elution conditions. The fluorescence intensity of pyridoxal 5'-phosphate was enhanced by post-column photochemical conversion, giving significantly different fluorescence spectra by a on-line photoreactor switched OFF and ON under irradiation at 254 nm. In addition, a simple and rapid method in isocratic conditions without the need of photochemical conversion was proposed for the analysis of Vitamin B 6 and Vitamin B 2 in pharmaceuticals. Linearity, precision, recovery, selectivity and sensitivity were found satisfactory for each analysed compound. Quantitation limits ranged from 26 to 240 fmol

  17. On-line methanol sensor system development for recombinant ...

    African Journals Online (AJOL)

    On-line methanol sensor system development for recombinant human serum ... of the methanol sensor system was done in a medium environment with yeast cells ... induction at a low temperature and a pH where protease does not function.

  18. On-line control systems in power plants

    International Nuclear Information System (INIS)

    Freymeyer, P.

    1981-01-01

    This report is a review of on-line control systems as a complex system connected with all problems like, development, planning, degree of automation, economics, service, quality and documentation. (orig.) [de

  19. Why do People Stop Playing On-Line Games?

    DEFF Research Database (Denmark)

    Sudzina, Frantisek; Razmerita, Liana

    2012-01-01

    The recent initial public offering of shares of Zynga, probably the most important on-line game provider, drew interest of potential investors but also of general public to their business model. What the most interested people learned so far is that if Zynga had not changed their accounting...... practice, they would be in red numbers for several months already. This is most likely caused by people stopping to play their games. This paper provides an estimate of what proportion of people, who played on-line games, already stopped playing them. Additionally, it analyzed the reasons why people...... stopped playing on-line games. It also compares Facebook and other on-line games....

  20. Chemometric approach for development, optimization, and validation of different chromatographic methods for separation of opium alkaloids.

    Science.gov (United States)

    Acevska, J; Stefkov, G; Petkovska, R; Kulevanova, S; Dimitrovska, A

    2012-05-01

    The excessive and continuously growing interest in the simultaneous determination of poppy alkaloids imposes the development and optimization of convenient high-throughput methods for the assessment of the qualitative and quantitative profile of alkaloids in poppy straw. Systematic optimization of two chromatographic methods (gas chromatography (GC)/flame ionization detector (FID)/mass spectrometry (MS) and reversed-phase (RP)-high-performance liquid chromatography (HPLC)/diode array detector (DAD)) for the separation of alkaloids from Papaver somniferum L. (Papaveraceae) was carried out. The effects of various conditions on the predefined chromatographic descriptors were investigated using chemometrics. A full factorial linear design of experiments for determining the relationship between chromatographic conditions and the retention behavior of the analytes was used. Central composite circumscribed design was utilized for the final method optimization. By conducting the optimization of the methods in very rational manner, a great deal of excessive and unproductive laboratory research work was avoided. The developed chromatographic methods were validated and compared in line with the resolving power, sensitivity, accuracy, speed, cost, ecological aspects, and compatibility with the poppy straw extraction procedure. The separation of the opium alkaloids using the GC/FID/MS method was achieved within 10 min, avoiding any derivatization step. This method has a stronger resolving power, shorter analysis time, better cost/effectiveness factor than the RP-HPLC/DAD method and is in line with the "green trend" of the analysis. The RP-HPLC/DAD method on the other hand displayed better sensitivity for all tested alkaloids. The proposed methods provide both fast screening and an accurate content assessment of the six alkaloids in the poppy samples obtained from the selection program of Papaver strains.

  1. The Daresbury On-Line Isotope Separator (DOLIS)

    International Nuclear Information System (INIS)

    Grant, I.S.; Eastham, D.A.; Groves, J.; Tolfree, D.W.L.; Walker, P.M.; Green, V.R.; Rikovska, J.; Stone, N.J.; Hamilton, W.D.

    1987-01-01

    The isotope separator DOLIS, which is on-line to the Daresbury Laboratory's 20-MV tandem accelerator, is used to measure nuclear moments and decay schemes. Separated beams may be collected on a tape and transported to a counting station, implanted directly into a host lattice at on-line temperatures down to less than 10 mK, or allowed to interact with a collinear laser beam. The present status of DOLIS and its ancillary equipment is described

  2. The Daresbury on-line isotope separator (DOLIS)

    International Nuclear Information System (INIS)

    Grant, I.S.; Eastham, D.A.; Groves, J.; Tolfree, D.W.L.; Walker, P.M.; Green, V.R.; Rikovska, J.; Stone, N.J.; Hamilton, W.D.

    1987-01-01

    The isotope separator DOLIS, which is on-line to the Daresbury Laboratory's 20-MV tandem accelerator, is used to measure nuclear moments and decay schemes. Separated beams may be collected on a tape and transported to a counting station, implanted directly into a host lattice at on-line temperatures down to less than 10 mK, or allowed to interact with a collinear laser beam. The present status of DOLIS and its ancillary equipment is described. (orig.)

  3. Considerations in applying on-line IC techniques to BWR's

    International Nuclear Information System (INIS)

    Kaleda, R.J.

    1992-01-01

    Ion-Chromatography (IC) has moved from its traditional role as a laboratory analytical tool to a real time, dynamic, on-line measurement device to follow ppb and sub-ppb concentrations of deleterious impurities in nuclear power plants. Electric Power Research Institute (EPRI), individual utilities, and industry all have played significant roles in effecting the transition. This paper highlights considerations and the evolution in current on-line Ion Chromatography systems. The first applications of on-line techniques were demonstrated by General Electric (GE) under EPRI sponsorship at Rancho Seco (1980), Calvert Cliffs, and McGuire nuclear units. The primary use was for diagnostic purposes. Today the on-line IC applications have been expanded to include process control and routine plant monitoring. Current on-line IC's are innovative in design, promote operational simplicity, are modular for simplified maintenance and repair, and use field-proven components which enhance reliability. Conductivity detection with electronic or chemical suppression and spectrometric detection techniques are intermixed in applications. Remote multi-point sample systems have addressed memory effects. Early applications measured ionic species in the part per billion range. Today reliable part per trillion measurements are common for on-line systems. Current systems are meeting the challenge of EPRI guideline requirements. Today's on-line IC's, with programmed sampling systems, monitor fluid streams throughout a power plant, supplying data that can be trended, stored and retrieved easily. The on-line IC has come of age. Many technical challenges were overcome to achieve today's IC

  4. On-line mixture-based alternative to logistic regression

    Czech Academy of Sciences Publication Activity Database

    Nagy, Ivan; Suzdaleva, Evgenia

    2016-01-01

    Roč. 26, č. 5 (2016), s. 417-437 ISSN 1210-0552 R&D Projects: GA ČR GA15-03564S Institutional support: RVO:67985556 Keywords : on-line modeling * on-line logistic regression * recursive mixture estimation * data dependent pointer Subject RIV: BB - Applied Statistics, Operational Research Impact factor: 0.394, year: 2016 http://library.utia.cas.cz/separaty/2016/ZS/suzdaleva-0464463.pdf

  5. Chromatographic Separations of Enantiomers and Underivatized Oligosaccharides

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Ying [Iowa State Univ., Ames, IA (United States)

    2004-01-01

    My graduate research has focused on separation science and bioanalytical analysis, which emphasized in method development. It includes three major areas: enantiomeric separations using high performance liquid chromatography (HPLC), Super/subcritical fluid chromatography (SFC), and capillary electrophoresis (CE); drug-protein binding behavior studies using CE; and carbohydrate analysis using liquid chromatograph-electrospray ionization mass spectrometry (LC-ESI-MS). Enantiomeric separations continue to be extremely important in the pharmaceutical industry. An in-depth evaluation of the enantiomeric separation capabilities of macrocyclic glycopeptides CSPs with SFC mobile phases was investigated using a set of over 100 chiral compounds. It was found that the macrocyclic based CSPs were able to separate enantiomers of various compounds with different polarities and functionalities. Seventy percent of all separations were achieved in less than 4 min due to the high flow rate (4.0 ml/min) that can be used in SFC. Drug-protein binding is an important process in determining the activity and fate of a drug once it enters the body. Two drug/protein systems have been studied using frontal analysis CE method. More sensitive fluorescence detection was introduced in this assay, which overcame the problem of low sensitivity that is common when using UV detection for drug-protein studies. In addition, the first usage of an argon ion laser with 257 nm beam coupled with CCD camera as a frontal analysis detection method enabled the simultaneous observation of drug fluorescence as well as the protein fluorescence. LC-ESI-MS was used for the separation and characterization of underivatized oligosaccharide mixtures. With the limits of detection as low as 50 picograms, all individual components of oligosaccharide mixtures (up to 11 glucose-units long) were baseline resolved on a Cyclobond I 2000 column and detected using ESI-MS. This system is characterized by high chromatographic

  6. Chromatographic Separations of Enantiomers and Underivatized Oligosaccharides

    International Nuclear Information System (INIS)

    Ying Liu

    2004-01-01

    My graduate research has focused on separation science and bioanalytical analysis, which emphasized in method development. It includes three major areas: enantiomeric separations using high performance liquid chromatography (HPLC), Super/subcritical fluid chromatography (SFC), and capillary electrophoresis (CE); drug-protein binding behavior studies using CE; and carbohydrate analysis using liquid chromatograph-electrospray ionization mass spectrometry (LC-ESI-MS). Enantiomeric separations continue to be extremely important in the pharmaceutical industry. An in-depth evaluation of the enantiomeric separation capabilities of macrocyclic glycopeptides CSPs with SFC mobile phases was investigated using a set of over 100 chiral compounds. It was found that the macrocyclic based CSPs were able to separate enantiomers of various compounds with different polarities and functionalities. Seventy percent of all separations were achieved in less than 4 min due to the high flow rate (4.0 ml/min) that can be used in SFC. Drug-protein binding is an important process in determining the activity and fate of a drug once it enters the body. Two drug/protein systems have been studied using frontal analysis CE method. More sensitive fluorescence detection was introduced in this assay, which overcame the problem of low sensitivity that is common when using UV detection for drug-protein studies. In addition, the first usage of an argon ion laser with 257 nm beam coupled with CCD camera as a frontal analysis detection method enabled the simultaneous observation of drug fluorescence as well as the protein fluorescence. LC-ESI-MS was used for the separation and characterization of underivatized oligosaccharide mixtures. With the limits of detection as low as 50 picograms, all individual components of oligosaccharide mixtures (up to 11 glucose-units long) were baseline resolved on a Cyclobond I 2000 column and detected using ESI-MS. This system is characterized by high chromatographic

  7. Chromatographic air analyser microsystem for the selective and sensitive detection of atmospheric pollutants

    International Nuclear Information System (INIS)

    Sanchez, Jean-Baptiste; Lahlou, Houda; Mohsen, Yehya; Berger, Franck; Vilanova, Xavier; Correig, Xavier

    2011-01-01

    The development of industry and automotive trafic produces Volatile Organic Compounds (VOCs) whose toxicity can affect seriously human health and environment. The level of those contaminants in air must be as low as possible. In this context, there is a need for in situ systems that could monitor selectively the concentration of these compounds. The aim of this study is to demonstrate the efficiency of a system build with a pre-concentrator, a chromatographic micro-column and a tin oxide-based gas sensor for the selective and sensitive detection of atmospheric pollutants. In particular, this study is focused on the selective detection of benzene and 1,3 butadiene.

  8. Chromatographic methods of the measurements of the chloride compounds in troposphere and stratosphere

    International Nuclear Information System (INIS)

    Lasa, J.; Rosiek, J.

    1992-01-01

    The paper contains a description of various chromatographic techniques used for the analysis of the tropospheric techniques used for the analysis of the tropospheric and stratospheric halogenated compounds. The types of the column packings used for separation of halogenated compounds are described. Model chromatograms illustrating the separation of halogenated compounds are presented. The methods of the air sampling and injection for the packed and capillary columns were described. The methods of the preparation of gas calibration mixtures are presented. Operational conditions for electron capture detector used by the authors of quoted paper are also given. (author). 66 refs, 29 figs, 13 tabs

  9. Volume overload cleanup: An approach for on-line SPE-GC, GPC-GC, and GPC-SPE-GC

    NARCIS (Netherlands)

    Kerkdijk, H.; Mol, H.G.J.; Nagel, B. van der

    2007-01-01

    A new concept for cleanup, based on volume overloading of the cleanup column, has been developed for on-line coupling of gel permeation chromatography (GPC), solid-phase extraction (SPE), or both, to gas chromatography (GC). The principle is outlined and the applicability demonstrated by the

  10. Chemical investigations of isotope separation on line target units for carbon and nitrogen beams

    CERN Document Server

    Franberg, H; Gäggeler, H W; Köster, U

    2006-01-01

    Radioactive ion beams (RIBs) are of significant interest in a number of applications. Isotope separation on line (ISOL) facilities provide RIB with high beam intensities and good beam quality. An atom that is produced within the ISOL target will first diffuse out from the target material. During the effusion towards the transfer line and into the ion source the many contacts with the surrounding surfaces may cause unacceptable delays in the transport and, hence, losses of the shorter-lived isotopes. We performed systematic chemical investigations of adsorption in a temperature and concentration regime relevant for ISOL targets and ion source units, with regard to CO/sub x/ and NOmaterials are potential construction materials for the above-mentioned areas. Off-line and on-line tests have been performed using a gas thermochromatography setup with radioactive tracers. The experiments were performed at the production of tracers for atmospheric chemistry (PROTRAC) facility at the Paul Schener Institute in Villigen...

  11. Automation and integration of multiplexed on-line sample preparation with capillary electrophoresis for DNA sequencing

    Energy Technology Data Exchange (ETDEWEB)

    Tan, H.

    1999-03-31

    The purpose of this research is to develop a multiplexed sample processing system in conjunction with multiplexed capillary electrophoresis for high-throughput DNA sequencing. The concept from DNA template to called bases was first demonstrated with a manually operated single capillary system. Later, an automated microfluidic system with 8 channels based on the same principle was successfully constructed. The instrument automatically processes 8 templates through reaction, purification, denaturation, pre-concentration, injection, separation and detection in a parallel fashion. A multiplexed freeze/thaw switching principle and a distribution network were implemented to manage flow direction and sample transportation. Dye-labeled terminator cycle-sequencing reactions are performed in an 8-capillary array in a hot air thermal cycler. Subsequently, the sequencing ladders are directly loaded into a corresponding size-exclusion chromatographic column operated at {approximately} 60 C for purification. On-line denaturation and stacking injection for capillary electrophoresis is simultaneously accomplished at a cross assembly set at {approximately} 70 C. Not only the separation capillary array but also the reaction capillary array and purification columns can be regenerated after every run. DNA sequencing data from this system allow base calling up to 460 bases with accuracy of 98%.

  12. Gas-phase chemistry of Mo, Ru, W, and Os metal carbonyl complexes

    International Nuclear Information System (INIS)

    Wang, Y.; Qin, Z.; Fan, F.L.

    2014-01-01

    Metal carbonyl complexes were used for studying the gas-phase chemical behavior of Mo, Ru, W and Os isotopes with an on-line low temperature isothermal gas chromatography apparatus. Short-lived Mo and Ru isotopes were produced by a 252 Cf spontaneous fission source. Short-lived nuclides of W and Os were produced using the heavy ion reactions 19 F + 159 Tb and 165 Ho, respectively. Short-lived products were thermalized in a recoil chamber filled with a gas mixture of helium and carbon monoxide. The carbonyls formed were then transported through capillaries to an isothermal chromatography column for study of the adsorption behavior as a function of temperature. On-line isothermal chromatography (IC) experiments on Teflon (PTFE) and quartz surfaces showed that short-lived isotopes of the listed elements can form carbonyl complexes which are very volatile and interact most likely in physical sorption processes. Deduced adsorption enthalpies of Mo and Ru carbonyls were -38 ± 2 kJ/mol and -36 ± 2 kJ/mol, respectively. These values are in good agreement with literature data, partly obtained with different chromatographic techniques. A validation of the applied Monte Carlo model to deduce adsorption enthalpies with Mo isotopes of different half-lives proved the validity of the underlying adsorption model. The investigations using a gas-jet system coupled to a heavy ion accelerator without any preseparator clearly showed the limitations of the approach. The He and CO gas mixture, which was directly added into the chamber, will result in decomposition of CO gas and produce some aerosol particles. After the experiment of 173 W and 179 Os in the heavy ion experiments, the Teflon column was covered by a yellowish deposit; the adsorption enthalpy of W and Os carbonyls could therefore not be properly deduced using Monte Carlo simulations. (orig.)

  13. Method for chromatographically recovering scandium and yttrium

    International Nuclear Information System (INIS)

    Snyder, T.S.; Stoltz, R.A.

    1991-01-01

    This paper describes a method for chromatographically recovering scandium and yttrium from the residue of a sand chlorinator. It comprises: providing a residue from a sand chlorinator, the residue containing scandium, yttrium, sodium, calcium and at least one radioactive metal of the group consisting of radium, thorium and uranium; digesting the residue with an acid to produce an aqueous liquid containing scandium, yttrium, sodium, calcium and at least one radioactive metal of the group consisting of radium, thorium and uranium; feeding the metal containing liquid through a cation exchanger; eluding the cation exchanger with an acid eluant to to produce: a first eluate containing at least half of the total weight of the calcium and sodium in the feed liquid; a second eluate containing at least half of the total weight of the one or more radioactive metals in the feed liquid; a third eluate containing at least half of the yttrium in the feed liquid, and a fourth eluate containing at least half of the weight of the scandium in the feed liquid

  14. On-line separation of Pu(III) and Am(III) using extraction and ion chromatography

    International Nuclear Information System (INIS)

    Jernstroem, J.; Lehto, J.; Betti, M.

    2007-01-01

    An on-line method developed for separating plutonium and americium was developed. The method is based on the use of HPLC pump with three analytical chromatographic columns. Plutonium is reduced throughout the procedure to trivalent oxidation state, and is recovered in the various separation steps together with americium. Light lanthanides and trivalent actinides are separated with TEVA resin in thiocyanate/formic acid media. Trivalent plutonium and americium are pre-concentrated in a TCC-II cation-exchange column, after which the separation is performed in CS5A ion chromatography column by using two different eluents. Pu(III) is eluted with a dipicolinic acid eluent, and Am(III) with oxalic acid eluent. Radiochemical and chemical purity of the eluted plutonium and americium fractions were ensured with alpha-spectrometry. (author)

  15. Quantitation of promethazine and metabolites in urine samples using on-line solid-phase extraction and column-switching

    Science.gov (United States)

    Song, Q.; Putcha, L.; Harm, D. L. (Principal Investigator)

    2001-01-01

    A chromatographic method for the quantitation of promethazine (PMZ) and its three metabolites in urine employing on-line solid-phase extraction and column-switching has been developed. The column-switching system described here uses an extraction column for the purification of PMZ and its metabolites from a urine matrix. The extraneous matrix interference was removed by flushing the extraction column with a gradient elution. The analytes of interest were then eluted onto an analytical column for further chromatographic separation using a mobile phase of greater solvent strength. This method is specific and sensitive with a range of 3.75-1400 ng/ml for PMZ and 2.5-1400 ng/ml for the metabolites promethazine sulfoxide, monodesmethyl promethazine sulfoxide and monodesmethyl promethazine. The lower limits of quantitation (LLOQ) were 3.75 ng/ml with less than 6.2% C.V. for PMZ and 2.50 ng/ml with less than 11.5% C.V. for metabolites based on a signal-to-noise ratio of 10:1 or greater. The accuracy and precision were within +/- 11.8% in bias and not greater than 5.5% C.V. in intra- and inter-assay precision for PMZ and metabolites. Method robustness was investigated using a Plackett-Burman experimental design. The applicability of the analytical method for pharmacokinetic studies in humans is illustrated.

  16. Chromatographic separation of low-temperature tar. Part II

    Energy Technology Data Exchange (ETDEWEB)

    Terres, E; Gebert, F; Huelsemann, H; Petereit, H; Toepsch, H; Ruppert, W

    1955-01-01

    Chromatographic methods and apparatus are discussed. The Folin-Denis reagent (Na tungstate molybdate in H/sub 3/PO/sub 4/) is used for developing paper chromatograms of phenol mixtures. Other reagents are given.

  17. Ion Chromatographic Analyses of Sea Waters, Brines and Related Samples

    OpenAIRE

    Nataša Gros

    2013-01-01

    This review focuses on the ion chromatographic methods for the analyses of natural waters with high ionic strength. At the beginning a natural diversity in ionic composition of waters is highlighted and terminology clarified. In continuation a brief overview of other review articles of potential interest is given. A review of ion chromatographic methods is organized in four sections. The first section comprises articles focused on the determination of ionic composition of water samples as com...

  18. On-line maintenance PSA support at NPP Krsko

    International Nuclear Information System (INIS)

    Prosen, R.; Vrbanic, I.; Kastelan, M.

    2000-01-01

    In 1997 Krsko NPP initiated the on-line maintenance (OLM) practice. On-line maintenance constitutes of corrective activities, preventive activities, surveillance activities, tests and inspections, as well as calibrations and modifications, taking place during the normal power operations. The on-line maintenance is a multidisciplinary process consisting of activity specification, planning, and preparation and performing of the OLM activity of interest. The primary role of the PSA group is to assess from the r isk perspective , using the plant-specific NEK PSA model, system unavailability and the impact to the plant operational risk. The intent is to support planning of the on-line maintenance activities from the risk perspective. The risk evaluation of the OLM activities is based on the probability of core damage evaluation for the defined discrete plant configuration states, determined by the OLM activities. Within this application, the optimized, plant-specific PSA model is used on Risk Spectrum platform. To perform the risk assessment of the on-line maintenance activities, first the systems to be affected are defined based on the planned OLM activities. The next important step is the assessment of the planned work schedule. To define the final schedule, the co-ordination and optimizing the planned OLM activities needs activation of all participating departments, supported also from PSA group. The P3 (i.e. Primavera) planning tool system windows are defined for different systems and groups of systems, and the activities are sorted in particular weeks according to these windows. (author)

  19. OLDASS: On-line data acquisition system at SF cyclotron

    International Nuclear Information System (INIS)

    Omata, Kazuo; Yasue, Masaharu; Hamagaki, Hideki

    1982-01-01

    The on-line data acquisition system in the Institute for Nuclear Study, the University of Tokyo, is composed of 2 systems of Fujitsu mini-computer PFU-400 for data processing at the high energy synchrotron and one system of that computer for low energy cyclotron as terminals, the host computer being M 180 II AD of the same company. This system has been developed to have the features of being the on-line system capable of following the improvement of host computer performance, being capable of developing the on-line programmes of other experimenting groups in parallel with batch jobs or the operation of the on-line system, and capable of developing programmes using FORTRAN. The result of about 220 KB/s was obtained for the data transfer rate between the programmes of the host computer and terminals, and this fulfilled the aimed performance. The terminal system on the low energy side is provided with an ADC interface and a display interface specified particularly in addition to the miniature computer PFU400 and standard I/O devices of the manufacture. The accumulating type graphic display of the I/O devices can be switched to be connected to the host computer, and immediately displays the results transferred to the host computer and analyzed. Hard copy is also available. The above hardware and software are explained. The on-line system insures 80 K bytes of the total memory of 224 K bytes for data area. (Wakatsuki, Y.)

  20. Sport Management Taught On-Line: A Discussion

    Directory of Open Access Journals (Sweden)

    William F. Stier Jr

    2009-01-01

    Full Text Available An introduction to the world of on-line courses (distance education/learning is presented. In addition, the world of on-line learning, as it pertains to sport management, is examined within the framework of (a pedagogy, (b finances,(c assessment, and (d choosing to transition from the traditional classroom to on-line learning. Pertinent points relative to each of the four categories are presented from the literature. In an effort to stimulate thought and discussion to the subject of on-line learning for sport management programs/courses the authors provide their reactions to the literature points by presenting their comments/reactions from a sport management perspective. Sport management professors and administrators are encouraged to critically examine the feasibility of such on-line courses (distance education/learning within their own curricula while maintaining an appropriate framework revolving around sound theoretical instructional strategies, methods as well as appropriate use of instructional tools, including but not limited to, computersand the WWW.