WorldWideScience

Sample records for gas chromatographic detection

  1. 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.

  2. Study on Detection and Identification of Gas Sensor Based on Chromatographic Separation

    Directory of Open Access Journals (Sweden)

    Xiao Wanfu

    2014-08-01

    Full Text Available This paper developed a chromatographic separation and sensor based on a combination of gas detector, the common precursor gases such as acetone, ether, chloroform and other gas detection. According to the obtained experimental data, proposed one kind based on the principal component analysis and support vector machine algorithm of gas chromatography identification sensor signal processing and recognition; the method used for detection and identification of the air in the precursor gases combine tester self-developed, obtained very good result. This paper designed and developed a chromatographic separation and sensor based on the combination of gas detection instruments, to multi gas detection instrument. On separation characteristics using chromatography, to solve the traditional single common precursor gas detection. The use of a pre processing based on domestication, principal component analysis for feature extraction method of all kinds of gas data. This effectively avoids the sensor substrate voltage fluctuation and gas concentration effects on body recognition, and reduces the gas sample feature vector dimension.

  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. 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.

  5. 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

  6. 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)

  7. 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).

  8. Selective gas-chromatographic detection using an ion-selective electrode-II Selective detection of fluorine compounds.

    Science.gov (United States)

    Kojima, T; Ichise, M; Seo, Y

    1972-04-01

    Components in samples are separated on a gas chromatography column using hydrogen as carrier gas. The individual components from the column are passed through a platinum tube heated at 1000 degrees , where they undergo hydrogenolysis, and fluorine compounds are converted into hydrogen fluoride. The hydrogen fluoride is dissolved in a slow stream of an absorption solution, and the fluoride ion concentration in the resulting solution is monitored in a flow-cell with a fluoride ion electrode. The potentiometric output of the cell is converted into a signal, which is proportional to the concentration of fluoride ion, by an antilogarithmic converter, and recorded. The response of the detector to fluorine compounds was about 10,000 times that to an equal quantity of other organic compounds, and 5 x 10(-11) mole of fluorobenzene could be detected.

  9. FTIR gas chromatographic analysis of perfumes

    Science.gov (United States)

    Diederich, H.; Stout, Phillip J.; Hill, Stephen L.; Krishnan, K.

    1992-03-01

    Perfumes, natural or synthetic, are complex mixtures consisting of numerous components. Gas chromatography (GC) and gas chromatography-mass spectrometry (GC-MS) techniques have been extensively utilized for the analysis of perfumes and essential oils. A limited number of perfume samples have also been analyzed by FT-IR gas chromatographic (GC-FTIR) techniques. Most of the latter studies have been performed using the conventional light pipe (LP) based GC-FTIR systems. In recent years, cold-trapping (in a matrix or neat) GC-FTIR systems have become available. The cold-trapping systems are capable of sub-nanogram sensitivities. In this paper, comparison data between the LP and the neat cold-trapping GC- FTIR systems is presented. The neat cold-trapping interface is known as Tracer. The results of GC-FTIR analysis of some commercial perfumes is also presented. For comparison of LP and Tracer GC-FTIR systems, a reference (synthetic) mixture containing 16 major and numerous minor constituents was used. The components of the mixture are the compounds commonly encountered in commercial perfumes. The GC-FTIR spectra of the reference mixture was obtained under identical chromatographic conditions from an LP and a Tracer system. A comparison of the two sets of data thus generated do indeed show the enhanced sensitivity level of the Tracer system. The comparison also shows that some of the major components detected by the Tracer system were absent from the LP data. Closer examination reveals that these compounds undergo thermal decomposition on contact with the hot gold surface that is part of the LP system. GC-FTIR data were obtained for three commercial perfume samples. The major components of these samples could easily be identified by spectra search against a digitized spectral library created using the Tracer data from the reference mixture.

  10. Portable gas chromatograph-mass spectrometer

    Science.gov (United States)

    Andresen, B.D.; Eckels, J.D.; Kimmons, J.F.; Myers, D.W.

    1996-06-11

    A gas chromatograph-mass spectrometer (GC-MS) is described for use as a field portable organic chemical analysis instrument. The GC-MS is designed to be contained in a standard size suitcase, weighs less than 70 pounds, and requires less than 600 watts of electrical power at peak power (all systems on). The GC-MS includes: a conduction heated, forced air cooled small bore capillary gas chromatograph, a small injector assembly, a self-contained ion/sorption pump vacuum system, a hydrogen supply, a dual computer system used to control the hardware and acquire spectrum data, and operational software used to control the pumping system and the gas chromatograph. This instrument incorporates a modified commercial quadrupole mass spectrometer to achieve the instrument sensitivity and mass resolution characteristic of laboratory bench top units. 4 figs.

  11. 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

  12. Capillary gas chromatographic detection of invert sugar in heated, adulterated, and adulterated and heated apple juice concentrates employing the equilibrium method.

    Science.gov (United States)

    Low, N H; McLaughlin, M; Hofsommer, H J; Hammond, D A

    1999-10-01

    The equilibrium method is introduced for the detection of invert sugar addition to apple juice. The method consists of a pre-equilibration of the sample with dry pyridine at 50 degrees C for 20 min followed by the addition of trimethylsilylimidazole and heating at 75 degrees C for 40 min. The resulting derivatized carbohydrates are then analyzed by capillary gas chromatography. This method was successfully used by independent laboratories to distinguish heated pure, intentionally adulterated (with invert sugar), and intentionally adulterated and then heated apple juice concentrates. The equilibrium method was shown to give significantly lower coefficients of variation for this sample set when compared to the original capillary gas chromatographic method. In addition, these results indicate that it may also be an effective method for the detection of medium invert sugar, depending on the level of the fingerprint oligosaccharides in this sweetener.

  13. 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 ...

  14. 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.

  15. Detection of clenbuterol at trace levels in doping analysis using different gas chromatographic-mass spectrometric techniques.

    Science.gov (United States)

    Yang, Sheng; Liu, Xin; Xing, Yanyi; Zhang, Dapeng; Wang, Shan; Wang, Xiaobing; Xu, Youxuan; Wu, Moutian; He, Zhenwen; Zhao, Jian

    2013-01-01

    This study demonstrates the development of a gas chromatography-triple quadrupole tandem mass spectrometry (GC-MS-MS) assay to detect clenbuterol in human urine and the comparison of this method with GC-MS techniques and gas chromatography-high resolution mass spectrometry (GC-HRMS) techniques. Urine samples were hydrolyzed with β-glucuronidase, extracted with methyl tert-butyl ether and dried under nitrogen. The derivative reagent was N-methyl-N-(trimethylsilyl)-trifluoroacetamide with NH4I and was analyzed by GC-MS, GC-MS-MS and GC-HRMS. A validation study was conducted by GC-MS-MS. The analyses of clenbuterol using different mass spectrometric techniques were compared. The limit of detection (LOD) for clenbuterol in human urine was 2 ng/mL by GC-MS (selected ion monitoring mode: SIM mode), 0.06 ng/mL by GC-HRMS and 0.03 ng/mL by GC-MS-MS, respectively, while the LOD by GC-HRMS was 0.06. With GC-MS-MS, the intra-assay and inter-assay precisions were less than 15%, the recoveries were 86 to 112% and the linear range was 0.06 to 8.0 ng/mL. The GC-MS under SIM mode can be used as a screening tool to detect clenbuterol at trace levels in human urine. The GC-MS-MS and GC-HRMS methods can confirm clenbuterol when its concentration is below 2 ng/mL. The results demonstrate that the GC-MS-MS method is quite sensitive, specific and reliable for the detection of clenbuterol in doping analysis.

  16. Fast gas chromatographic separation of biodiesel.

    Science.gov (United States)

    Pauls, R E

    2011-05-01

    A high-speed gas chromatographic method has been developed to determine the FAME distribution of B100 biodiesel. The capillary column used in this work has dimensions of 20 m × 0.100 mm and is coated with a polyethylene glycol film. Analysis times are typically on the order of 4-5 min depending upon the composition of the B100. The application of this method to a variety of vegetable and animal derived B100 is demonstrated. Quantitative results obtained with this method were in close agreement with those obtained by a more conventional approach on a 100 m column. The method, coupled with solid-phase extraction, was also found suitable to determine the B100 content of biodiesel-diesel blends.

  17. 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.

  18. Comparison of thin layer chromatographic and gas chromatographic determination of propoxur residues in a cocoa ecosystem

    International Nuclear Information System (INIS)

    Yeboah, P.O.; Lowor, S.; Akpabli, C.K.

    2005-01-01

    The fate of propoxur in a cocoa ecosystem has been studied using thin layer chromatographic (TLC) and gas chromatographic (GC) methods. Residues of propoxur as determined by both TLC and GC were not significantly different. TLC analysis of propoxur residues in soil, cocoa leaves and pods did not require any rigorous cleanup since residues measured from cleaned extracts and without cleanup were not significantly different. The residue levels of propoxur in the soil were found to decrease rapidly and, by the 21st day, none was detected in the topsoil (0-15 cm). Evidence of leaching of propoxur residues in the soil has also been demonstrated. The amount left in the top soil after the first seven days were 27%, 23% and 24% of the initial one as determined by the TLC without cleanup, TLC with cleanup and GLC, respectively. No propoxur residue was detected in topsoil 21 days after spraying. About 38% of pesticides detected on the cocoa pod on the day of treatment remained on the pod seven days after treatment. The residue detected on the leaves on the day of treatment was higher than that in or on the soil. This decreased rapidly to 1.7% in 21 days compared to 16% for the soil and 23% for the pod. (author)

  19. 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.

  20. 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.

  1. 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.

  2. 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.

  3. Chemical characterization of Brickellia cavanillesii (Asteraceae) using gas chromatographic methods

    OpenAIRE

    Eshiet, Etetor R; Zhu, Jinqiu; Anderson, Todd A; Smith, Ernest E

    2013-01-01

    A methanol extract of lyophilized Brickellia cavanillesii was quantitatively analyzed using gas chromatographic (GC) techniques. The chromatographic methods employed were (i) GC-flame ionization detector (GC-FID), (ii) GC-mass spectrometry (GC-MS), and (iii) purge and trap GC-MS (P&T GC-MS). Thirteen compounds were identified with a quality match of 90% and above using GC-MS. The compounds were (1) Cyclohexene, 6-ethenyl-6-methyl-1-(1-methylethyl)-3-(1-methylethylidene)-, (S)-; (2) Bicylo (2....

  4. Headspace solid-phase microextraction and gas chromatographic analysis of low-molecular-weight sulfur volatiles with pulsed flame photometric detection and quantification by a stable isotope dilution assay.

    Science.gov (United States)

    Ullrich, Sebastian; Neef, Sylvia K; Schmarr, Hans-Georg

    2018-02-01

    Low-molecular-weight volatile sulfur compounds such as thiols, sulfides, disulfides as well as thioacetates cause a sulfidic off-flavor in wines even at low concentration levels. The proposed analytical method for quantification of these compounds in wine is based on headspace solid-phase microextraction, followed by gas chromatographic analysis with sulfur-specific detection using a pulsed flame photometric detector. Robust quantification was achieved via a stable isotope dilution assay using commercial and synthesized deuterated isotopic standards. The necessary chromatographic separation of analytes and isotopic standards benefits from the inverse isotope effect realized on an apolar polydimethylsiloxane stationary phase of increased film thickness. Interferences with sulfur-specific detection in wine caused by sulfur dioxide were minimized by addition of propanal. The method provides adequate validation data, with good repeatability and limits of detection and quantification. It suits the requirements of wine quality management, allowing the control of oenological treatments to counteract an eventual formation of excessively high concentration of such malodorous compounds. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

    Indian Academy of Sciences (India)

    The lower detection limit was 10 ng/ml in 5 ml of urine. The conjugated steroids from urine were centrifuged to 2,430 for 10 min, the supernatant solution passed through Amberlite XAD-2 column and the steroids eluted fraction esterified by using MSTFA and TMSI. The rate of metabolism and urinary excretion seem to be ...

  6. 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.

  7. 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

  8. 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.

  9. 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.

  10. 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)

  11. 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

  12. A bubble-based microfluidic gas sensor for gas chromatographs.

    Science.gov (United States)

    Bulbul, Ashrafuzzaman; Kim, Hanseup

    2015-01-07

    We report a new proof-of-concept bubble-based gas sensor for a gas chromatography system, which utilizes the unique relationship between the diameters of the produced bubbles with the gas types and mixture ratios as a sensing element. The bubble-based gas sensor consists of gas and liquid channels as well as a nozzle to produce gas bubbles through a micro-structure. It utilizes custom-developed software and an optical camera to statistically analyze the diameters of the produced bubbles in flow. The fabricated gas sensor showed that five types of gases (CO2, He, H2, N2, and CH4) produced (1) unique volumes of 0.44, 0.74, 1.03, 1.28, and 1.42 nL (0%, 68%, 134%, 191%, and 223% higher than that of CO2) and (2) characteristic linear expansion coefficients (slope) of 1.38, 2.93, 3.45, 5.06, and 5.44 nL/(kPa (μL s(-1))(-1)). The gas sensor also demonstrated that (3) different gas mixture ratios of CO2 : N2 (100 : 0, 80 : 20, 50 : 50, 20 : 80 and 0 : 100) generated characteristic bubble diameters of 48.95, 77.99, 71.00, 78.53 and 99.50 μm, resulting in a linear coefficient of 10.26 μm (μL s(-1))(-1). It (4) successfully identified an injection (0.01 μL) of pentane (C5) into a continuous carrier gas stream of helium (He) by monitoring bubble diameters and creating a chromatogram and demonstrated (5) the output stability within only 5.60% variation in 67 tests over a month.

  13. 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%.

  14. 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

  15. Advanced ion chromatograph detects low MEA levels

    Energy Technology Data Exchange (ETDEWEB)

    Lindsay, S. (Texaco Refining and Marketing Inc., Anacortes, WA (US)); Palladino, D. (Beckmann Instruments Inc., Westbury, N.Y. (US))

    1990-01-22

    Texaco Refining and Marketing Inc. is using an advanced method of ion chromatography at its Puget Sound refinery in Anacortes, Wash., to detect and measure monoethanolamine (MEA) in process effluent water at low-ppm levels. The method reported in this article is electronically suppressed, single-column, ion chromatography (SCIC). The method was selected for use in this service subsequent to successful use to improve titrimetric analysis of wash water, where low-ppm ranges of chlorides needed to be measured. SCIC was also able to detect halides of other constituents, such as bromides and iodides. The advanced method can measure precisely very low levels of both monoethanolamine and ammonia, and it assists in locating the sources that allow the contaminants to escape into the wastewater stream. In these analyses, the SCIC unit operated in less than one third the time of automatic titrimetry and other wet chemistry methods available in the laboratory. It also proved to be more economical than conventional chemically suppressed ion chromatography (CSIC).

  16. A Simple and Rapid Extraction for Gas Chromatographic Determination of Thiabendazole and Imazalil Residues in Lemons

    Directory of Open Access Journals (Sweden)

    Navickiene Sandro

    2002-01-01

    Full Text Available A rapid and efficient method is described for the determination of thiabendazole and imazalil residues in lemons (peel and pulp. The procedure is based on the extraction with an hexane:ethyl acetate mixture (1:1, v/v and gas chromatographic analysis using thermionic specific detection (TSD. The possibility of matrix effect was also studied. Mean recoveries from 8 replicates of fortified samples ranged from 79% to 109%, with relative standard deviation values between 2.4% to 12.8%. The detection and quantification limits of the method were 0.2 mg kg-1 and 0.5 mg kg-1, respectively.

  17. 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...

  18. Gas chromatographic analysis of volatile hydrocarbons to detect irradiated chicken, pork and beef - an intercomparison study. A report in English and German

    International Nuclear Information System (INIS)

    Schreiber, G.A.; Schulzki, G.; Spiegelberg, A.; Helle, N.; Adam, S.T.; Ammon, J.; Baumann, P.; Brockmann, R.; Baenziger, U.; Delincee, H.; Droz, C.; Estendorfer, S.; Gemperle, C.; Grabowski, H.U. von; Kaenzig, A.; Kroells, W.; Matter, L.; Metschies, M.; Mildau, G.; Pfordt, J.; Plaga-Lodde, A.; Punkert, M.; Roennefahrt, B.; Ruge, W.; Stemmer, H.; Vater, N.; Wilmers, K.; Boegl, K.W.

    1993-01-01

    This report provides a detailed description of an inter-laboratory study to detect irradiation treatment of chicken carcasses, pork and beef using a method suitable for routine application. The 17 participating laboratories determined the quantity of four different radiation-induced hydrocarbons (1-tetradecene, pentadecane, 1,7-hexadecadiene, 8-heptadecene) in coded samples approx. 3 and 6 months after irradiation. The quantities detected were used to identify the samples as irradiated or non-irradiated. The samples of each type of meat to be examined had been supplied by two different producers. The dose range that was tested (approx. 0.6 to 7.5 kGy) included commercially used doses (approx. 1 to 5 kGy). The method employed enable 98.3% of a total of 864 samples to be correctly identified as irradiated or non-irradiated. This result is remarkable: Although the marker concentrations in the various samples showed a clear dose dependency, the variation was quite marked. The high rate of correct identifications could be achieved by defining a sample only as irradiated if certain quantities of at least 3 of the radiolytic products to be determined had been found. A similar identification rate was achieved if quantification of markers was omitted to identify a sample only as irradiated when all the expected radiolysis products could be clearly detected. For all three types of meat, no significant differences in marker yields could be shown for the products of the respective two producers. Also, in none of the types of meat, any significant difference could be revealed for the quantiatitive results achieved three and six months after irradiation. These results show that irradiation of chicken carcasses, pork and beef in the commerically used dose range can be clearly detected throughout the entire period in which products are normally stored and that the method described is suitable for routine analyses in food control laboratories. (orig.)

  19. 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.

  20. GAS-CHROMATOGRAPHIC DETERMINATION OF N-ACETYLISOPUTREANINE-GAMMA-LACTAM, A UNIQUE CATABOLITE OF N1-ACETYLSPERMIDINE

    NARCIS (Netherlands)

    HESSELS, J; KINGMA, AW; STURKENBOOM, MCJM; ELZINGA, H; VANDENBERG, GA; MUSKIET, FAJ

    1991-01-01

    A capillary gas chromatographic method with nitrogen-phosphorus detection for the determination of N-acetylisoputreanine-gamma-lactam (acisoga) in urine is described. The method was validated by comparing the results with those given by an isotope dilution mass fragmentographic method. Making use of

  1. [The gas chromatographic analysis of volatile compounds on the compact MKhP chromatograph].

    Science.gov (United States)

    Krasnova, R R; Ianovskiĭ, S M

    1998-01-01

    Methods of analysis of biological specimens, alcohol beverages, and technological liquids in columns with standard adsorbents carbopaque B and C with carbowax 20M, widely used abroad, are described and examples of analyses presented. A special portable chromatographer (MCP) with flame ionization detector has been designed. It is intended for analysis of volatile organic compounds (alcohols, carbohydrates, organochlorine compounds, glycols, esters, etc.) in columns of different polarity. The system of processing of chromatographic findings permits a quantitative analysis of complex chromatograms and automated identification of substances in biological samples by using the available database.

  2. Miniaturized MEMS-Based Gas Chromatograph for High Inertial Loads Associated with Planetary Missions, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — Thorleaf Research, Inc. proposes to develop a rugged, miniaturized, low power MEMS-based gas chromatograph (GC) capable of handling the high inertial loads...

  3. 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

  4. Design and Performance of a Gas Chromatograph for Automatic Monitoring of Pollutants in Ambient Air

    Science.gov (United States)

    Villalobos, R.; Stevens, D.; LeBlanc, R.; Braun, L.

    1971-01-01

    In recent years, interest in air pollution constituents has focused on carbon monoxide and hydrocarbons as prime components of polluted air. Instrumental methods have been developed, and commercial instruments for continuous monitoring of these components have been available for a number of years. For the measurement of carbon monoxide, non-dispersive infrared spectroscopy has been the accepted tool, in spite of its marginal sensitivity at low parts-per-million levels. For continuously monitoring total hydrocarbons, the hydrogen flame ionization analyzer has been widely accepted as the preferred method. The inadequacy of this latter method became evident when it was concluded that methane is non-reactive and cannot be considered a contaminant even though present at over 1 ppm in the earth's atmosphere. Hence, the need for measuring methane separately became apparent as a means of measuring the reactive and potentially harmful non-methane hydrocarbons fraction. A gas chromatographic method for the measurement of methane and total hydrocarbons which met these requirements has been developed. In this technique, methane was separated on conventional gas chromatographic columns and detected by a hydrogen flame ionization detector (FID) while the total hydrocarbons were obtained by introducing a second sample directly into the FID without separating the various components. The reactive, or non-methane hydrocarbons, were determined by difference. Carbon monoxide was also measured after converting to methane over a heated catalyst to render it detectable by the FID. The development of this method made it possible to perform these measurements with a sensitivity of as much as 1 ppm full scale and a minimum detectability of 20 ppb. Incorporating this technique, criteria were developed by APCO for a second generation continuous automatic instrument for atmospheric monitoring stations.

  5. New portable micro gas chromatograph for environmental analysis

    Energy Technology Data Exchange (ETDEWEB)

    Overton, E.B.; Carney, K.R.; Dharmasena, H.P.; Mainga, A.M.; Ehrmann, U. [Louisiana State Univ., Baton Rouge, LA (United States). Inst. for Environmental Studies

    1994-12-31

    Efforts directed at developing a truly portable method for the analysis of semivolatile compounds have led to the construction and testing of a new generation of micro-GC instrumentation. Building on the successful application of microbore GC columns for in-field analysis of volatile organic compounds, the instrument development group at the LSU-Institute for Environmental Studies has developed a hand portable GC capable of analyzing samples containing compounds with retention indices (100% dimethylpolysiloxane column) up to at least 2,000 in less than 4 minutes, using less than 50 watts (peak) of electrical power. In addition to the ability to analyze semivolatile compounds, the chromatograph is capable of analyzing volatile organics competitively with the most sophisticated of the current commercial portable GCs. The presentation will evaluate chromatographic performance of the instrument at its latest stage of development and demonstrate some applications to environmental analysis using the prototype instrument.

  6. An inverse gas chromatographic methodology for studying gas-liquid mass transfer.

    Science.gov (United States)

    Paloglou, A; Martakidis, K; Gavril, D

    2017-01-13

    A novel methodology of reversed flow inverse gas chromatography (RF-IGC) is presented. It permits the simultaneous determination of mass transfer coefficients across the gas liquid interface as well as the respective solubility parameters and thermodynamic functions of dissolution of gases into liquids. The standard deviation of the experimentally determined parameters is estimated for first time, which combined with the successful comparison of the values of the present parameters with other literature ones ascertain the reliability of the methodology. Another novelty of the present work is that the chromatographic sampling of the physicochemical phenomena is done without performing the usual flow reversals procedure. Vinyl chloride monomer's (VCM) interaction with various composition liquid foods: orange juice, milk and olive oil was used as model system. The present transfer rates are controlled by the gas film at lower temperatures, but at higher temperatures the resistances in both films tend to become equal. The found liquid diffusivity values express the total mass transfer from the gas phase into the liquid's bulk and they decrease with rising temperature, as the solubilities of gases in liquids do. Solubility, expressed by Henry's law constant and the mean values of interfacial thickness are of the same order of magnitude to literature ones. From the thermodynamic point of view, VCM dissolution in all liquids is accompanied by significant heat release and it is a slightly non-spontaneous process, near equilibrium, while the entropy change values are negative. Copyright © 2016 Elsevier B.V. All rights reserved.

  7. 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

  8. Gas chromatographic determination of pesticide residues in white mustard.

    Science.gov (United States)

    Słowik-Borowiec, Magdalena; Szpyrka, Ewa; Walorczyk, Stanisław

    2015-04-15

    A new analytical method employing gas chromatography coupled to electron capture and nitrogen phosphorus detection (GC-ECD/NPD) has been developed and validated for the screening and quantification of 51 pesticides in a matrix of high chlorophyll content - white mustard (Sinapis alba L.). For preparation of the sample extract, the citrate buffered QuEChERS procedure was followed. However certain changes were made to adapt the method to our needs and available laboratory resources. The sample size was reduced to 5 g, 10 mL water was added and exchange of solvent before GC analysis was done. The samples spiked with the target pesticides at the concentration level 0.01 mg/kg and a higher level (depending on the compound) yielded average recoveries in the range of 70-120% with relative standard deviations (RSDs) 0-19% except for HCB, S-metolachlor and teflubenzuron, and displayed very good linearity (R(2)>0.99) for nearly all the analytes. Limit of quantification was 0.01 mg/kg for the majority of the analytes. The expanded measurement uncertainties were estimated employing a "top-down" empirical model as being between 6% and 32% and yielding an average value of 18% (coverage factor k=2, confidence level 95%). Copyright © 2014 Elsevier Ltd. All rights reserved.

  9. 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.

  10. 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)

  11. 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, ...

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

    African Journals Online (AJOL)

    Yomi

    2010-08-27

    Aug 27, 2010 ... Key words: Acetone-butanol-ethanol fermentation, column temperature programme, gas chromatography, sweet sorghum juice. ..... dehydration of aqueous butanol solutions: a comparison of flux vs. permeance, separation factor vs. selectivity. J. Membrane Sci. 245: 199-210. Wang F, Kashket S, Kashket ...

  13. Sulphur hexafluoride gas detection

    CSIR Research Space (South Africa)

    Stolper, R

    2006-02-01

    Full Text Available .kashangroup.com ] Sulphur Hexafl uoride Gas Detection R Stolper CSIR Materials Science and Manufacturing, PO Box 395, Pretoria, 0001 rstolper@csir.co.za Imaging Michelson Interferometer Fabrey-Perot Etalon imaging solution Prism Spectrometer Grating...

  14. 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)

  15. 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...

  16. 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.

  17. Gas detection system

    International Nuclear Information System (INIS)

    Allan, C.J.; Bayly, J.G.

    1975-01-01

    The gas detection system provides for the effective detection of gas leaks over a large area. It includes a laser which has a laser line corresponding to an absorption line of the gas to be detected. A He-Xe laser scans a number of retroreflectors which are strategically located around a D 2 O plant to detect H 2 S leaks. The reflected beam is focused by a telescope, filtered, and passed into an infrared detector. The laser may be made to emit two frequencies, one of which corresponds with an H 2 S absorption line; or it may be modulated on and off the H 2 S absorption line. The relative amplitude of the absorbed light will be a measure of the H 2 S present

  18. 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

  19. 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.

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

    Science.gov (United States)

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

    2007-08-13

    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 degrees C for 60 min with 20% Na2SO4. The linear calibration curves were observed for the concentrations ranging from 1 to 300 microg L(-1) with the correlation coefficients (R2) being greater than 0.99. The method detection limits of most analytes were below 1 microg L(-1) except DCAA and MCAA that were 2 and 18 microg 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.

  1. 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

  2. Gas Chromatographic-Selected Ion Monitoring-Mass Spectrometric Determination of Cigarette Mainstream Smoke Components with Sensory Attributes

    Directory of Open Access Journals (Sweden)

    Coleman WM

    2014-12-01

    Full Text Available A new method has been developed that detects significant quantitative differences in the amounts of pyrazines, pyridines, furfurals, carboxylic acids, b-damascenone, sclareolide, and megastigmatrienones in the mainstream smoke of a series of five commercial cigarettes. This new quantitative method is based on the gas chromatographic-selected ion monitoring-mass spectrometric (GC-SIM-MS determination of the selected smoke constituents. The accuracy and precision of the approach were well within acceptable parameters with the majority of cases relative standard deviation (RSD values consistently around 5%. Sample preparation was simple requiring only the dissolution of the trapped particulate material in a known volume of methanol followed by injection of this clear dark colored solution into the gas chromatograph. This approach represents an advance in the technology in terms of higher sample throughput and less sample workup. Certain products demonstrated consistent trends in concentration of specific chemical classes. The mainstream smoke from a University of Kentucky reference cigarette, 2R4F, was included for reference purposes. These results are applicable in the overall evaluation of the components responsible for the taste associated with cigarette products.

  3. Ionic liquid functionalization of semi-packed columns for high-performance gas chromatographic separations.

    Science.gov (United States)

    Regmi, Bishnu P; Chan, Ryan; Agah, Masoud

    2017-08-11

    Gas chromatography columns fabricated using microelectromechanical system (MEMS) technology provide a number of clear advantages. However, successful deposition of stationary phases having a wide application range remains an important technical challenge. In this paper, we report, for the first time, on the deposition of room temperature ionic liquids (RTILs)-a versatile class of stationary phases-inside the channels of semi-packed columns (SPCs) for high-performance gas chromatographic separation of complex chemical mixtures. A 1m long, 240μm deep, 190μm wide column comprising an array circular micropillars of 20μm in diameter and 40μm post spacing was fabricated using MEMS processes. Two RTILs were immobilized inside these columns using a dynamic coating method, and the columns were tested for separation of three different mixtures: a 15-component mixture of hazardous chemical pollutants, an 8-component mixture of fatty acid methyl esters, and a sample of gasoline. These columns displayed sharp and symmetrical peaks, significant selectivity variation between the two columns, and rapid separation times. The columns yielded high separation efficiencies measured by approximately 2300 plates/m under isothermal conditions. This work highlights the potential of RTILs to be used as excellent stationary phases for SPCs, thereby dramatically expanding the range of complex mixtures that could be analyzed using a micro gas chromatograph. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. Gas chromatographic-mass spectrometric determination of levodropropizine plasma levels in healthy volunteers.

    Science.gov (United States)

    Zaratin, P; De Angelis, L; Cattabeni, F

    1988-08-01

    A gas chromatographic-mass spectrometric method for the qualitative and quantitative analysis of levodropropizine (S(-)-3-(4-phenyl-piperazin-1-yl)-propane-1,2-diol, DF 526) in plasma is described. The method proved to be highly selective and sensitive. Drug concentrations as low as 5 ng/ml could be measured. Levodropropizine plasma levels were measured in 6 healthy volunteers after administration of an acute 60 mg dose. Peak concentrations were reached between 40 and 60 min and measurable amounts of drug were present till 8 h after administration.

  5. 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

  6. Gas chromatograph analysis on closed air and nitrogen oxide storage atmospheres of recalcitrant seeds of Quercus Alba

    Science.gov (United States)

    Storage of recalcitrant seeds remains an unsolved problem. This study investigated the quantitative gas analysis of nitrous oxide (N2O) and air atmospheres on the recalcitrant seeds of Quercus alba by using gas chromatograph. Ten seeds were placed in each sealed atmospheric system of air and 98/2% N...

  7. 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.

  8. 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.

  9. 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...

  10. 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

  11. Gas Detection for Experiments

    CERN Document Server

    Hay, D

    2001-01-01

    Flammable gases are often used in detectors for physics experiments. The storage, distribution and manipulation of such flammable gases present several safety hazards. As most flammable gases cannot be detected by human senses, specific well-placed gas detection systems must be installed. Following a request from the user group and in collaboration with CERN safety officers, risk analyses are performed. An external contractor, who needs to receive detailed user requirements from CERN, performs the installations. The contract is passed on a guaranteed results basis. Co-ordination between all the CERN groups and verification of the technical installation is done by ST/AA/AS. This paper describes and focuses on the structured methodology applied to implement such installations based on goal directed project management techniques (GDPM). This useful supervision tool suited to small to medium sized projects facilitates the task of co-ordinating numerous activities to achieve a completely functional system.

  12. Comparison of two detection methods in thin layer chromatographic ...

    African Journals Online (AJOL)

    o-tolidine plus potassium iodide and photosynthesis inhibition detection methods were investigated for the analysis of three triazine herbicides (atrazine, ametryne, simazine) and two urea herbicides (diuron, metobromuron) in a coastal savanna soil using thin layer chromatography to compare the suitability of the two ...

  13. Liquid chromatographic determination of uranium in seawater with coulometric detection

    International Nuclear Information System (INIS)

    Maekoya, Chiaki; Takata, Yoshinori

    1980-01-01

    A method of the separation with anion-exchange chromatography and of the coulometric detection of uranium in seawater was investigated. The size of the separation column used was 9 mm in inside diameter and 100 mm in length, and strong basic anion-exchange resin (Hitachi No. 2632) of carbonate form was packed in the column. A concentrator with two mini-columns in which the same resin was packed was applied for the preconcentration of uranium in seawater containing 20 g of potassium thiocyanate and 10 ml of hydrochloric acid per liter. Good result was obtained when a mixed solution of sodium carbonate (0.12 mol/l), sodium bicarbonate (0.08 mol/l), sodium bisulfite (0.03 mol/l) and sodium chloride (0.5 mol/l) was used as an eluent for the separation of uranium from vanadium. Sodium bisulfite was of use for dropping the background current based on an electrochemical reduction of dissolved oxygen. Sodium bicarbonate acted as an eliminator of an unknown peak by its bufferise effect. The optimum working electrode potential for the detection was -1.45 V vs. ferri-ferrocyanide. The detection limit was 3.2 x 10 -10 mol (80 ngU). The coefficient of variation at 3.0 ppb was about 4% (n=5) for seawater analysis. And the analysis time was approximately 1.5 hours. (author)

  14. 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)

  15. 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.)

  16. 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.

  17. 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.

  18. 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)

  19. 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.

  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. New gas chromatographic instrumentation for studying the action of sulfur dioxide on marbles.

    Science.gov (United States)

    Bakaoukas, Nikolaos; Kapolos, John; Koliadima, Athanasia; Karaiskakis, George

    2005-09-16

    Reversed-flow gas chromatography, which is a sub-technique of inverse gas chromatography, is an experimental arrangement simulating a simple model for the action of air pollutants on buildings and monuments, in laboratory scale. By using a commercial gas chromatograph and an appropriate mathematical analysis, kinetic parameters such as rate constants for adsorption k1, adsorption/desorption kR and surface reaction k2, as well as surface diffusion coefficients Dgamma, deposition velocities Vd and reaction probabilities gamma of SO2 on marble surfaces at different temperatures (303.15-353.15 K) in the presence or in the absence of protective materials (an acrylic copolymer, Paraloid B-72 or a siloxane, CTS Silo 111) were calculated. From the above mentioned physicochemical quantities the ability of the examined materials to minimize the dry deposition of SO2 on marble is carrying out and a possible mechanism for the interaction between SO2 and Paraloid B-72 was suggested. Both materials (CTS SILO 111 and Paraloid B-72) are good enough for protecting marble against SO2 at low temperatures (303.15-323.15), while at high temperatures (333.15-353.15), siloxane seems to protect marble better than acrylic copolymer.

  2. 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...

  3. 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.

  4. Rapid gas chromatographic method for the determination of famoxadone, trifloxystrobin and fenhexamid residues in tomato, grape and wine samples.

    Science.gov (United States)

    Likas, D T; Tsiropoulos, N G; Miliadis, G E

    2007-05-25

    Trifloxystrobin, fenhexamid and famoxadone belong to the generation of fungicides acting against a broad spectrum of fungi and widely used in Integrated Pest Management strategies in different agricultural crops but mainly in viticulture. In the present work, a gas chromatographic (GC) method for their determination was developed and validated on tomato, grape and wine matrices. The method was based on a simple one step liquid-liquid microextraction with cyclohexane/dichloromethane (9+1, v/v) and determination of fungicides by gas chromatography with nitrogen phosphorous (NP-) and electron capture (EC-) detection, and ion trap mass spectrometry (ITMS) for confirmation. The method was validated by recovery experiments, assessment of matrix effect and calculation of the associated uncertainty. Recoveries for GC-NPD and GC-ECD were found in the range of 81-102% with RSD NPD, respectively, depending on the sensitivity of each compound with trifloxystrobin being the most sensitive. The expanded uncertainty, calculated for a sample concentration of 0.10 mg/kg, ranged from 4.8 to 13% for the GC-ECD and from 5.4 to 29% for the GC-NPD. The concentration levels for famoxadone residues found in tomato and grape samples from field experiments were clearly below the EU established MRL values, thus causing no problems in terms of food safety.

  5. On-line gas chromatographic analysis of higher alcohol synthesis products from syngas.

    Science.gov (United States)

    Andersson, Robert; Boutonnet, Magali; Järås, Sven

    2012-07-20

    An on-line gas chromatographic (GC) system has been developed for rapid and accurate product analysis in catalytic conversion of syngas (a mixture of H₂ and CO) to alcohols, so called "higher alcohol synthesis (HAS)". Conversion of syngas to higher alcohols is an interesting second step in the route of converting coal, natural gas and possibly biomass to liquid alcohol fuel and chemicals. The presented GC system and method are developed for analysis of the products formed from syngas using alkali promoted MoS₂ catalysts, however it is not limited to these types of catalysts. During higher alcohol synthesis not only the wanted short alcohols (∼C₂-C₅) are produced, but also a great number of other products in smaller or greater amounts, they are mainly short hydrocarbons (olefins, paraffins, branched, non-branched), aldehydes, esters and ketones as well as CO₂, H₂O. Trace amounts of sulfur-containing compounds can also be found in the product effluent when sulfur-containing catalysts are used and/or sulfur-containing syngas is feed. In the presented GC system, most of them can be separated and analyzed within 60 min without the use of cryogenic cooling. Previously, product analysis in "higher alcohol synthesis" has in most cases been carried out partly on-line and partly off-line, where the light gases (gases at room temp) are analyzed on-line and liquid products (liquid at room temp) are collected in a trap for later analysis off-line. This method suffers from many drawbacks compared to a complete on-line GC system. In this paper an on-line system using an Agilent 7890 gas chromatograph equipped with two flame ionization detectors (FID) and a thermal conductivity detector (TCD), together with an Agilent 6890 with sulfur chemiluminescence dual plasma detector (SCD) is presented. A two-dimensional GC system with Deans switch (heart-cut) and two capillary columns (HP-FFAP and HP-Al₂O₃) was used for analysis of the organic products on the FIDs. Light

  6. 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

  7. Gas Chromatographic Method: Tool for Rapid and Sensitive Analysis of Residual Solvents in Amoxicillin and Ampicillin Tablets

    Directory of Open Access Journals (Sweden)

    Sk Manirul Haque

    2015-12-01

    Full Text Available A simple and sensitive static head space gas chromatographic (SH-GC method equipped with FID has been developed and validated for simultaneous determination of residual solvents e.g.,  methanol, dichloromethane and toluene in two therapeutic drugs such as amoxicillin  and ampicillin. The separation was achieved with 30 m long Elite - 5 fused silica capillary column and 0.32 mm inner diameter. The developed SH-GC method offered symmetric peak shape, good resolution and reasonable retention time for all the solvents. Beer’s law was obeyed in the concentration ranges 100 – 1200, 50 – 1000 and 50 – 500 ppm for methanol, dichloromethane and toluene, respectively. The method was validated according to international conference on harmonization (ICH guidelines in terms of specificity, linearity, precision, accuracy, limit of detection, limit of quantitation, robustness and solution stability. The degrees of linearity of the calibration curves, the percent recoveries, relative standard deviation for the method were also determined. All the validation parameters were within the acceptable range. The developed SH-GC method could, therefore, be suitable for simple and rapid detection of trace levels residual solvents in other pharmaceutical products and thereby it could be used for routine analysis in any analytical laboratory.

  8. 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.

  9. 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.

  10. 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.

  11. 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.

  12. 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.

  13. Graphitic carbon nitride as high-resolution stationary phase for gas chromatographic separations.

    Science.gov (United States)

    Zheng, Yunzhong; Qi, Meiling; Fu, Ruonong

    2016-07-08

    This work presents the first example of utilization of graphitic carbon nitride (g-C3N4) as stationary phase for capillary gas chromatographic (GC) separations. The statically coated g-C3N4 column showed the column efficiencies of 3760 plates/m and weak polarity. Its resolving capability and retention behaviours were investigated by using the Grob test mixture, and mixtures of diverse types of analytes, and structural and positional isomers. The results showed superior separation performance of the g-C3N4 stationary phase for some critical analytes and preferential retention for aromatic analytes. Specifically, it exhibited high-resolution capability for aromatic and aliphatic isomers such as methylnaphthalenes and dimethylnaphthalenes, phenanthrene and anthracene and alkane isomers. In addition, g-C3N4 column showed excellent thermal stability up to 280°C and good repeatability with relative standard deviation (RSD) values less than 0.09% for intra-day, below 0.23% for inter-day and in the range of 1.9-8.4% for between-column, respectively. The advantageous separation performance shows the potential of g-C3N4 and related materials as stationary phase in GC and other separation technologies. Copyright © 2016 Elsevier B.V. All rights reserved.

  14. Graphitic carbon nitride nanofibers in seaweed-like architecture for gas chromatographic separations.

    Science.gov (United States)

    Zheng, Yunzhong; Han, Qing; Qi, Meiling; Qu, Liangti

    2017-05-05

    Seaweed-like graphitic carbon nitride (g-C 3 N 4 ) has a unique porous architecture composed of interlocking g-C 3 N 4 nanofibers (NF-C 3 N 4 ) with much higher surface area than bulk g-C 3 N 4 and shows good potential in separation science. This work investigated the separation performance of NF-C 3 N 4 as stationary phase for capillary gas chromatographic (GC) separations. The NF-C 3 N 4 column exhibits weak polarity and high column efficiency of 4728 plates/m for n-dodecane. Importantly, it displays good separation performance for a wide range of analytes and shows different retention behaviors from the bulk g-C 3 N 4 column and commercial HP-5MS column with 5% phenylpolysiloxane. Particularly, it shows high resolving capability for both aliphatic and aromatic isomers. In addition, NF-C 3 N 4 column has high thermal stability up to 280°C and good separation repeatability with relative standard deviation (RSD) values in the range of 0.29-0.61% for intra-day, 0.56-1.1% for inter-day and 2.0-4.9% for between-column, respectively. Moreover, it was applied for the determination of isomer impurities in real samples, showing good potential in GC applications. Copyright © 2017 Elsevier B.V. All rights reserved.

  15. Gas chromatographic-thermal energy analysis method for N-nitrosodibutylamine in latex infant pacifiers: collaborative study

    Energy Technology Data Exchange (ETDEWEB)

    Each of 5 collaborating laboratories determined volatile N-nitrosamines in 3 blind quadruplicate sets of latex rubber infant pacifier samples, using a gas chromatographic-thermal energy analysis (GC-TEA) method. Volatile N-nitrosamines are extracted from cut-up pacifier nipples with CH/sub 2/Cl/sub 2/. The extract is concentrated and subjected to high temperature purge and trap, and the nitrosamines are eluted from the trap and determined by GC-TEA. N-Nitrosodibutylamine (NDBA) was the only nitrosamine found in sufficient concentration to allow analysis. NDBA concentrations of the 3 sets of samples were 82.6, 21.0, and 7.12 ng/g rubber. The repeatability relative standard deviations ranged from 7.46 to 24.0% and the reproducibility relative standard deviations from 7.46 to 29.2%. The minimum detectable level of NDBA by this method is 3.6 ng/g rubber. The method has been adopted official first action.

  16. 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.

  17. Validated gas chromatographic-negative ion chemical ionization mass spectrometric method for delta(9)-tetrahydrocannabinol in sweat patches.

    Science.gov (United States)

    Saito, Takeshi; Wtsadik, Abraham; Scheidweiler, Karl B; Fortner, Neil; Takeichi, Sanae; Huestis, Marilyn A

    2004-11-01

    A sensitive gas chromatography-negative ion chemical ionization mass spectrometry (GC/MS-NICI) method was developed and validated for the measurement of Delta(9)-tetrahydrocannabinol (THC) in human sweat patches. THC-d(0) and THC-d(3) were added to worn blank sweat patches (PharmChek; PharmChem Incorporated) and extracted with 3 mL of methanol-0.2 mol/L sodium acetate buffer (pH 5.0, 3:1 by volume) on a reciprocating shaker at ambient temperature for 30 min. Extracted solution (2 mL) was diluted with 8 mL of 0.1 mol/L sodium acetate buffer (pH 4.5) and extracted by use of solid-phase extraction columns (CleanScreen; United Chemical Technologies). Dried extracts were derivatized with trifluoroacetic acid and analyzed with an Agilent 6890 gas chromatograph interfaced with an Agilent 5973 mass selective detector operated in NICI-selected ion-monitoring mode. The lower limits of detection and quantification for THC in human sweat were 0.2 and 0.4 ng/patch, respectively. The calibration curve was linear from 0.4 to 10 ng/patch (R(2) >0.995). Overall recovery of THC from blank worn patches to which 0.6, 4.0, and 8.0 ng of THC had been added was 44-46%. Assay imprecision, expressed as CV, was THC quantification. This GC/MS-NICI assay for THC in human sweat provides adequate sensitivity and performance characteristics for analyzing THC in sweat patches and meets the requirements of the proposed Substance Abuse and Mental Health Administration's guidelines for sweat testing.

  18. Miniature, Low Power Gas Chromatograph with Sample Pre-Processing Capability and Enhanced G-Force Survivability for Planetary Missions, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — Thorleaf Research, Inc. proposes to develop a miniaturized, low power gas chromatograph (GC) with sample pre-processing capability and enhanced capability for...

  19. Liquid chromatographic determination of zearalenone and zearalenol in animal feeds and grains, using fluorescence detection.

    Science.gov (United States)

    Bagneris, R W; Gaul, J A; Ware, G M

    1986-01-01

    A liquid chromatographic (LC) method was developed for the determination of zearalenone and zearalenol in grains and mixed animal feeds. Samples are extracted with chloroform and purified by a base-acid liquid-liquid partition. Zearalenone and zearalenol are separated by reverse phase LC and determined by fluorescence detection, excitation wavelength 236 nm with a 418 nm cutoff filter. The method was applied to the determination of zearalenone and zearalenol in 395 survey samples of corn, oats, barley, sorghum, silage, and finished feeds. The limit of detection is 10 ng/g for both toxins. The range of naturally occurring toxins found was 10-4,000 ng/g. Average recoveries were 84% for zearlenone and 69% for zearalenol. Coefficients of variation were 24.6% for zearalenone and 30.8% for zearalenol for crop year 1980, and 28.3% for zearalenone and 22.0% for zearalenol for crop year 1981.

  20. Relating gas chromatographic profiles to sensory measurements describing the end products of the Maillard reaction.

    Science.gov (United States)

    Stanimirova, I; Boucon, C; Walczak, B

    2011-01-30

    Often in analytical practice, a set of samples is described by different types of measurements in the hope that a comprehensive characterisation of samples will provide a more complete picture and will help in determining the similarities among samples. The main focus is then on how to combine the information described by different measurement variables and how to analyse it simultaneously. In other words, the main goal is to find a common representation of samples that emphasises the individual and common properties of the different blocks of variables. Several methods can be adopted for the simultaneous analysis of multiblock data with a common object mode. These are: consensus principal component analysis (CPCA), SUM-PCA, multiple factor analysis (MFA) and structuration des tableaux à trois indices de la statistique (STATIS).In this article we present a comparison of the performances of these methods for data describing the chemistry and sensory profiles of the Maillard reaction products. The aroma compounds formed during the reaction of thermal heating between one or two selected amino acids and one or two reducing sugars have been analysed by head space gas chromatography and the intensity and nature of the odour of the resulting products has been evaluated according to selected descriptors by a panel of sensory experts.The results showed that using the information of the chromatographic and sensory data in conjunction enhanced the interpretability of the data. SUM-PCA and more specifically multiple factor analysis, MFA, allowed for a detailed study of the similarities of mixtures in terms of reaction products and sensory profiles. Copyright © 2010 Elsevier B.V. All rights reserved.

  1. Comprehensive two-dimensional gas chromatographic separations with a microfabricated thermal modulator.

    Science.gov (United States)

    Serrano, Gustavo; Paul, Dibyadeep; Kim, Sung-Jin; Kurabayashi, Katsuo; Zellers, Edward T

    2012-08-21

    Rapid, comprehensive two-dimensional gas chromatographic (GC × GC) separations by use of a microfabricated midpoint thermal modulator (μTM) are demonstrated, and the effects of various μTM design and operating parameters on performance are characterized. The two-stage μTM chip consists of two interconnected spiral etched-Si microchannels (4.2 and 2.8 cm long) with a cross section of 250 × 140 μm(2), an anodically bonded Pyrex cap, and a cross-linked wall coating of poly(dimethylsiloxane) (PDMS). Integrated heaters provide rapid, sequential heating of each μTM stage, while a proximate, underlying thermoelectric cooler provides continual cooling. The first-dimension column used for GC × GC separations was a 6 m long, 250 μm i.d. capillary with a PDMS stationary phase, and the second-dimension column was a 0.5 m long, 100 μm i.d. capillary with a poly(ethylene glycol) phase. Using sets of five to seven volatile test compounds (boiling point ≤174 °C), the effects of the minimum (T(min)) and maximum (T(max)) modulation temperature, stage heating lag/offset (O(s)), modulation period (P(M)), and volumetric flow rate (F) on the quality of the separations were evaluated with respect to several performance metrics. Best results were obtained with a T(min) = -20 °C, T(max) = 210 °C, O(s) = 600 ms, P(M) = 6 s, and F = 0.9 mL/min. Replicate modulated peak areas and retention times were reproducible to <5%. A structured nine-component GC × GC chromatogram was produced, and a 21 component separation was achieved in <3 min. The potential for creating portable μGC × μGC systems is discussed.

  2. Statistical modelling of measurement errors in gas chromatographic analyses of blood alcohol content.

    Science.gov (United States)

    Moroni, Rossana; Blomstedt, Paul; Wilhelm, Lars; Reinikainen, Tapani; Sippola, Erkki; Corander, Jukka

    2010-10-10

    Headspace gas chromatographic measurements of ethanol content in blood specimens from suspect drunk drivers are routinely carried out in forensic laboratories. In the widely established standard statistical framework, measurement errors in such data are represented by Gaussian distributions for the population of blood specimens at any given level of ethanol content. It is known that the variance of measurement errors increases as a function of the level of ethanol content and the standard statistical approach addresses this issue by replacing the unknown population variances by estimates derived from large sample using a linear regression model. Appropriate statistical analysis of the systematic and random components in the measurement errors is necessary in order to guarantee legally sound security corrections reported to the police authority. Here we address this issue by developing a novel statistical approach that takes into account any potential non-linearity in the relationship between the level of ethanol content and the variability of measurement errors. Our method is based on standard non-parametric kernel techniques for density estimation using a large database of laboratory measurements for blood specimens. Furthermore, we address also the issue of systematic errors in the measurement process by a statistical model that incorporates the sign of the error term in the security correction calculations. Analysis of a set of certified reference materials (CRMs) blood samples demonstrates the importance of explicitly handling the direction of the systematic errors in establishing the statistical uncertainty about the true level of ethanol content. Use of our statistical framework to aid quality control in the laboratory is also discussed. Copyright © 2010 Elsevier Ireland Ltd. All rights reserved.

  3. 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

  4. Fuzzy C-means clustering for chromatographic fingerprints analysis: A gas chromatography-mass spectrometry case study.

    Science.gov (United States)

    Parastar, Hadi; Bazrafshan, Alisina

    2016-03-18

    Fuzzy C-means clustering (FCM) is proposed as a promising method for the clustering of chromatographic fingerprints of complex samples, such as essential oils. As an example, secondary metabolites of 14 citrus leaves samples are extracted and analyzed by gas chromatography-mass spectrometry (GC-MS). The obtained chromatographic fingerprints are divided to desired number of chromatographic regions. Owing to the fact that chromatographic problems, such as elution time shift and peak overlap can significantly affect the clustering results, therefore, each chromatographic region is analyzed using multivariate curve resolution-alternating least squares (MCR-ALS) to address these problems. Then, the resolved elution profiles are used to make a new data matrix based on peak areas of pure components to cluster by FCM. The FCM clustering parameters (i.e., fuzziness coefficient and number of cluster) are optimized by two different methods of partial least squares (PLS) as a conventional method and minimization of FCM objective function as our new idea. The results showed that minimization of FCM objective function is an easier and better way to optimize FCM clustering parameters. Then, the optimized FCM clustering algorithm is used to cluster samples and variables to figure out the similarities and dissimilarities among samples and to find discriminant secondary metabolites in each cluster (chemotype). Finally, the FCM clustering results are compared with those of principal component analysis (PCA), hierarchical cluster analysis (HCA) and Kohonon maps. The results confirmed the outperformance of FCM over the frequently used clustering algorithms. Copyright © 2016 Elsevier B.V. All rights reserved.

  5. High-performance liquid chromatographic determination of levodropropizine in human plasma with fluorometric detection.

    Science.gov (United States)

    Tagliaro, F; Moffa, M; De Battisti, Z; Smith, F P; Gentile, M

    1996-10-11

    The present paper describes a new high-performance liquid chromatographic method with fluorescence detection for the analysis of levodropropizine [S-(-)-3-(4-phenylpiperazin-1-yl)-propane-1,2-diol] (Levotuss), an anti-tussive drug, in human serum and plasma. A reversed-phase separation of levodropropizine was coupled with detection of the native fluorescence of the molecule, using excitation and emission wavelengths of 240 nm and 350 nm respectively. The analytical column was packed with spherical 5 microns poly(styrene-divinylbenzene) particles and the mobile phase was 0.1 M NaH2PO4 pH 3-methanol (70:30, v/v), containing 0.5% (v/v) tetrahydrofuran. For quantitation, p-methoxylevodropropizine was used as the internal standard. Samples of 200 microliters of either serum or plasma were mixed with 200 microliters of 0.1 M Na2HPO4 pH 8.9 and extracted with 5 ml of chloroform-2-propanol (9:1, v/v). The dried residue from the organic extract was redissolved with distilled water and directly injected into the chromatograph. The limit of detection for levodropropizine, in biological matrix, was about 1-2 ng/ml, at a signal-to-noise ratio of 3. The linearity was satisfactory over a range of concentrations from 3 to 1000 ng/ml (r2 = 0.99910); within-day precision tested in the range 5-100 ng/ml as well as day-to-day reproducibility proved acceptable, with relative standard deviations better than 1% in most cases. Interferences from as many as 91 therapeutic or illicit drugs were excluded.

  6. 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.

  7. 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

  8. Gas chromatographic determination of N-nitrosamines in beverages following automatic solid-phase extraction.

    Science.gov (United States)

    Jurado-Sánchez, Beatriz; Ballesteros, Evaristo; Gallego, Mercedes

    2007-11-28

    A semiautomatic method for the determination of seven N-nitrosamines in beverages by gas chromatography with nitrogen-phosphorus detection is proposed. Beverage samples are aspirated into a solid-phase extraction module for preconcentration and cleanup. The influence of the experimental conditions was examined by using various sorbents among which LiChrolut EN was found to provide quantitative elution and the highest preconcentration factors of all. The proposed method is sensitive, with limits of detection between 7 and 33 ng/kg, and precise, with relative standard deviations from 4.3% to 6.0%. The recoveries of N-nitrosamines from beverage samples spiked with 0.5 or 1 microg/kg concentrations of these compounds ranged from 95% to 102%. The method was successfully applied to the determination of residues of the studied N-nitrosamines in beverages including beer, wine, liquor, whisky, cognac, rum, vodka, grape juice, cider, tonic water, and soft drinks. The analytes were only detected in beer samples, positives being confirmed by gas chromatography coupled with impact ionization mass spectrometry.

  9. 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

  10. Development and single-laboratory validation of a new gas chromatographic multi-pesticide method of analysis of commercial emulsifiable concentrate formulations containing alachlor, chlorpyrifos methyl, fenthion and trifluralin as active ingredients.

    Science.gov (United States)

    Karasali, Helen; Balayannis, George; Hourdakis, Adamantia; Ambrus, Arpad

    2006-10-06

    A multi-pesticide (MP) method was developed and single-laboratory validated for the quality control of commercial pesticide products containing alachlor, chlorpyrifos methyl, fenthion and trifluralin as active ingredients (a.i.). A capillary gas chromatographic system with flame ionization detection (FID) and a programmable temperature vaporising split injector was used. The performance characteristics (specificity, linearity, precision and repeatability) of the method satisfied international acceptability criteria.

  11. 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

  12. Forced-flow chromatographic determination of calcium and magnesium with continuous spectrophotometric detection

    Energy Technology Data Exchange (ETDEWEB)

    Arguello, M.D.

    1977-12-01

    Modifications to the forced-flow chromatograph include a flow-through pH monitor to continuously monitor the pH of the final effluent and an active low-pass filter to eliminate noise in the spectrophotometric detector. All separations are performed using partially sulfonated XAD-2 as the ion exchanger. Elution of calcium and magnesium is accomplished using ammonium chloride and ethylenediammonium chloride solutions. Calcium and magnesium are detected by means of Arsenazo I and PAR-ZnEDTA color-forming reagents. Other metal ions are detected by means of PAR and Chromazurol S color-forming reagents. Calcium and magnesium distribution coefficients on partially sulfonated XAD-2 as functions of ammonium chloride and ethylenediammonium chloride concentration are given together with distribution coefficients of other metal ions. Methods for the selective elution of interfering metal ions prior to the elution of calcium and magnesium are described. Beryllium and aluminum are selectively eluted with sulfosalicylic acid. Those elements forming anionic chloride complexes are selectively eluted with HCl-acetone. Nickel is selectively eluted with HCl-acetone-dimethylglyoxime. Synthetic samples containing calcium and magnesium, both alone and in combination with alkali metals, strontium, barium, beryllium, aluminum, transition metals, and rare earths, are analyzed. Hard water samples are analyzed for calcium and magnesium and the results compared to those obtained by EDTA titration, atomic absorption spectroscopy, and plasma emission spectroscopy. Several clinical serum samples are analyzed for calcium and magnesium and the results compared to those obtained by atomic absorption spectroscopy.

  13. 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

  14. POTENTIAL AND PITFALLS OF CHROMATOGRAPHIC TECHNIQUES AND DETECTION MODES IN SUBSTANCE IDENTIFICATION FOR SYSTEMATIC TOXICOLOGICAL ANALYSIS

    NARCIS (Netherlands)

    DEZEEUW, RA; HARTSTRA, J; FRANKE, JP

    1994-01-01

    The potential and the constraints of thin-layer chromatography (TLC), gas chromatography (GC) and high-performance liquid chromatography (HPLC) towards substance identification, together with their detection modes, are considered. The latter include colour reactions on the plate, molecular masses

  15. Gas tightness detecting method for overpack

    International Nuclear Information System (INIS)

    Harashima, Takeo; Hasegawa, Yasuyuki

    1999-01-01

    High level radioactive wastes and timing gas generation means for jetting out an inert gas after a predetermined period of time are contained together in a steel overpack. A steel lid is welded to the opening of the overpack so as to seal the high level radioactive wastes and the timing gas generation means. Then, the inert gas is jetted out from the timing gas generating device, and the gas tightness is detected by detecting the inert gas at the circumference of the overpack. Alternatively, a corrosion resistant coating layer having a gas generation means for jetting out an inert gas is coated at the circumference of a steel overpack containing high level radioactive wastes, and the overpack is sealed. The inert gas is generated from the gas generating means in the coating layer, and the inert gas at the periphery of the coating layer is detected to determine gas tightness. (N.H.)

  16. 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)

  17. 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)

  18. Thermal desorption-Gas chromatographic methodology for the determination of residual solvents in mesoporous silica.

    Science.gov (United States)

    Asfaw, Adissu Alemayehu; Wolfs, Kris; Schepdael, Ann Van; Adams, Erwin

    2017-06-02

    In this work, thermal desorption-gas chromatography-flame ionization detection (TD-GC-FID) was adapted to enable the determination of residual solvents (RS) in mesoporous silica (MPSi). MPSi is often utilized in various pharmaceutical formulations or drug delivery systems and the accurate determination of RS is an important part of pharmaceutical quality control. Seven commonly used solvents (methanol, ethanol, acetone, isopropanol, dichloromethane, tetrahydrofuran and hexafluoroisopropanol) were evaluated in combination with 3 types of MPSi having pore sizes of 2-3, 15 and 25nm. Validation results showed general recovery values >98% and good linearity over the concentration ranges studied. The limits of detection (LOD) and limits of quantification (LOQ) for the different solvents ranged from 0.03 to 0.08μg and from 0.1 to 0.2μg per tube, respectively. Verification of the accuracy of the TD method was investigated by using an alternative method based on complete dissolution of MPSi in hydrofluoric acid (HF) followed by full evaporation headspace-GC (HS-GC). The results obtained from both procedures were not statistically different (p>0.05) when applied to actual experimental drug samples consisting of itraconazole loaded on MPSi. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. 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

  20. Comparison of ultraviolet detection and charged aerosol detection methods for liquid-chromatographic determination of protoescigenin.

    Science.gov (United States)

    Filip, Katarzyna; Grynkiewicz, Grzegorz; Gruza, Mariusz; Jatczak, Kamil; Zagrodzki, Bogdan

    2014-01-01

    Escin, a complex mixture of pentacyclic triterpene saponins obtained from horse chestnut seeds extract (HCSE; Aesculus hippocastanum L.), constitutes a traditional herbal active substance of preparations (drugs) used for a treatment of chronic venous insufficiency and capillary blood vessel leakage. A new approach to exploitation of pharmacological potential of this saponin complex has been recently proposed, in which the β-escin mixture is perceived as a source of a hitherto unavailable raw material, pentacyclic triterpene aglycone-protoescigenin. Although many liquid chromatography methods are described in the literature for saponins determination, analysis of protoescigenin is barely mentioned. In this work, a new ultra-high performance liquid chromatography (UHPLC) method developed for protoescigenin quantification has been described. CAD (charged aerosol detection), as a relatively new detection method based on aerosol charging, has been applied in this method as an alternative to ultraviolet (UV) detection. The influence of individual parameters on CAD response and sensitivity was studied. The detection was performed using CAD and UV (200 nm) simultaneously and the results were compared with reference to linearity, accuracy, precision and limit of detection.

  1. Flow system for optical activity detection of vegetable extracts employing molecular exclusion continuous chromatographic detection

    Science.gov (United States)

    Fajer, V.; Rodríguez, C.; Naranjo, S.; Mesa, G.; Mora, W.; Arista, E.; Cepero, T.; Fernández, H.

    2006-02-01

    The combination of molecular exclusion chromatography and laser polarimetric detection has turned into a carbohydrate separation and quantification system for plant fluids of industrial value, making it possible the evaluation of the quality of sugarcane juices, agave juices and many other plant extracts. Some previous papers described a system where liquid chromatography separation and polarimetric detection using a LASERPOL 101M polarimeter with He-Ne light source allowed the collection and quantification of discrete samples for analytical purposes. In this paper, the authors are introducing a new improved system which accomplishes polarimetric measurements in a continuous flux. Chromatograms of several carbohydrates standard solutions were obtained as useful references to study juice quality of several sugarcane varieties under different physiological conditions. Results by either discrete or continuous flux systems were compared in order to test the validation of the new system. An application of the system to the diagnostics of scalded foliar is described. A computer program allowing the output of the chromatograms to a display on line and the possibility of digital storing, maxima detections, zone integration, and some other possibilities make this system very competitive and self-convincing.

  2. Chemometrics-enhanced one-dimensional/comprehensive two-dimensional gas chromatographic analysis for bioactive terpenoids and phthalides in Chaihu Shugan San essential oils.

    Science.gov (United States)

    He, Min; Yang, Zhi-Yu; Yang, Tian-Biao; Ye, Ying; Nie, Juan; Hu, Yong; Yan, Pan

    2017-05-01

    Chemometrics-enhanced one-dimensional/comprehensive two-dimensional gas chromatographic (GC/GC×GC) technologies, were used to explore the compositions of Chaihu Shugan San essential oils, that were extracted from the herbal formulae by different schemes. We have shown that chemometric resolution using gas chromatographic- mass spectrometry (GC-MS) could be used for the qualitative and quantitative analysis of the majority of Terpenoids or Phthalides from herb formulae and single herbs. A GC×GC system was further optimized to achieve the increased peak capacity and the enhanced signal of the hydro-distillation sample (CSSh). When hardware bottleneck resulted from very complex sample, chemometric tools were once again applied to recover the stained information in the second dimension ( 2 D) matrix data. Heuristic evolving latent projections (HELP) could be used for two dimensional (2D) sub-matrixes Xi at n spectral detection channels, after three dimensional (3D) data splitting. For a real 3D data matrix, alternating trilinear decomposition (ATLD) algorithm could conduct regularization for an iterative trilinear decomposition procedure, by Moore-Penrose pseudoinverse computations based on singular value decomposition. After retention indices (RI) confirmation, 216 target analytes (terpenoids or phthalides) could be elucidated both in CSSh and in supercritical fluid extract (CSSs). Based on the obtained data, some potential quality markers (Q-markers) were identified which may affect the quality of the products. Finally, a "connectivity map" was plotted to describe the unique mechanisms of tradition Chinese medicine (TCM). Copyright © 2017 Elsevier B.V. All rights reserved.

  3. Gas chromatographic-mass spectrometric urinary metabolome analysis to study mutations of inborn errors of metabolism.

    Science.gov (United States)

    Kuhara, Tomiko

    2005-01-01

    Urine contains numerous metabolites, and can provide evidence for the screening or molecular diagnosis of many inborn errors of metabolism (IEMs). The metabolomic analysis of urine by the combined use of urease pretreatment, stable-isotope dilution, and capillary gas chromatography/mass spectrometry offers reliable and quantitative data for the simultaneous screening or molecular diagnosis of more than 130 IEMs. Those IEMs include hyperammonemias and lactic acidemias, and the IEMs of amino acids, pyrimidines, purines, carbohydrates, and others including primary hyperoxalurias, hereditary fructose intolerance, propionic acidemia, and methylmalonic acidemia. Metabolite analysis is comprehensive for mutant genotypes. Enzyme dysfunction-either by the abnormal structure of an enzyme/apoenzyme, the reduced quantity of a normal enzyme/apoenzyme, or the lack of a coenzyme-is involved. Enzyme dysfunction-either by an abnormal regulatory gene, abnormal sub-cellular localization, or by abnormal post-transcriptional or post-translational modification-is included. Mutations-either known or unknown, common or uncommon-are involved. If the urine metabolome approach can accurately observe quantitative abnormality for hundreds of metabolites, reflecting 100 different disease-causing reactions in a body, then it is possible to simultaneously detect different mutant genotypes of far more than tens of thousands. (c) 2004 Wiley Periodicals, Inc., Mass Spec Rev 24:814-827, 2005.

  4. Nonlinear preprocessing method for detecting peaks from gas chromatograms

    Directory of Open Access Journals (Sweden)

    Min Hyeyoung

    2009-11-01

    Full Text Available Abstract Background The problem of locating valid peaks from data corrupted by noise frequently arises while analyzing experimental data. In various biological and chemical data analysis tasks, peak detection thus constitutes a critical preprocessing step that greatly affects downstream analysis and eventual quality of experiments. Many existing techniques require the users to adjust parameters by trial and error, which is error-prone, time-consuming and often leads to incorrect analysis results. Worse, conventional approaches tend to report an excessive number of false alarms by finding fictitious peaks generated by mere noise. Results We have designed a novel peak detection method that can significantly reduce parameter sensitivity, yet providing excellent peak detection performance and negligible false alarm rates from gas chromatographic data. The key feature of our new algorithm is the successive use of peak enhancement algorithms that are deliberately designed for a gradual improvement of peak detection quality. We tested our approach with real gas chromatograms as well as intentionally contaminated spectra that contain Gaussian or speckle-type noise. Conclusion Our results demonstrate that the proposed method can achieve near perfect peak detection performance while maintaining very small false alarm probabilities in case of gas chromatograms. Given the fact that biological signals appear in the form of peaks in various experimental data and that the propose method can easily be extended to such data, our approach will be a useful and robust tool that can help researchers highlight valid signals in their noisy measurements.

  5. Structure elucidation and chromatographic identification of anthraquinone components of cochineal (Dactylopius coccus) detected in historical objects.

    Science.gov (United States)

    Stathopoulou, Konstantina; Valianou, Lemonia; Skaltsounis, Alexios-Leandros; Karapanagiotis, Ioannis; Magiatis, Prokopios

    2013-12-04

    Cochineal is one of the most well known organic red dyes. Dactylopius coccus Costa (Dactylopiidae) is a scale insect that is used as the source of the dye known as Mexican cochineal. Although cochineal is today a natural food colorant (E120) and although it has been used in art objects (textiles and paintings) for centuries, its exact chemical consistency is not well clarified except for carminic acid which is the major component and kermesic and flavokermesic acids. Several minor components (typically less than 5% of the colouring material) remained unknown or partially studied, although their presence has been reported in numerous analytical works related to art objects. Chemical investigation of the methanol extract of the dried insects, after subsequent HPLC chromatographic separations, led to the isolation and structure elucidation of six new anthraquinones, along with the known compounds carminic acid, kermesic acid and flavokermesic acid. The new compounds formerly described as DCII and DCIII, were found to be the 2-C-glucoside of flavokermesic acid and 4-aminocarminic acid, respectively, while DCIV and DCVII were found to be the α/β C-glucofuranosides of kermesic acid, and were studied as a mixture due to equilibrium. In addition, 3-O-glucoside of flavokermesic acid (DCOFK), and 3,4-dideoxycarminic acid (DDCA) were identified. The structures of the new compounds were elucidated on the basis of their NMR and MS data. Finally, the new compounds were detected in silk dyed with cochineal, lake pigment and, furthermore, in historical objects of the cultural heritage (icon and textile) using LC-DAD and LC-MS. Copyright © 2013 Elsevier B.V. All rights reserved.

  6. 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.

  7. 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)

  8. 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

  9. 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

  10. Aging and analytical performances evolution of a gas chromatographic system at Mars

    OpenAIRE

    Bonnet, Jean-Yves; Szopa, Cyril; Millan, Maeva; Coscia, David; Cabane, Michel; Belmahdi, I.; Buch, A.; Dequaire, T.; Coll, Patrice; Teinturier, S.; Mahaffy, P.

    2015-01-01

    International audience; Health data from the gas chromatography (GC) module onboard the SAM instrument [1] will be presented to assess the analytical performances evolution of a GC device in Martian environment through 3 years.

  11. 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)

  12. Development and validation of a stability-indicating gas chromatographic method for quality control of residual solvents in blonanserin: a novel atypical antipsychotic agent.

    Science.gov (United States)

    Peng, Ming; Liu, Jin; Lu, Dan; Yang, Yong-Jian

    2012-09-01

    Blonanserin is a novel atypical antipsychotic agent for the treatment of schizophrenia. Ethyl alcohol, isopropyl alcohol and toluene are utilized in the synthesis route of this bulk drug. A new validated gas chromatographic (GC) method for the simultaneous determination of residual solvents in blonanserin is described in this paper. Blonanserin was dissolved in N, N-dimethylformamide to make a sample solution that was directly injected into a DB-624 column. A postrun oven temperature at 240°C for approximately 2 h after the analysis cycle was performed to wash out blonanserin residue in the GC column. Quantitation was performed by external standard analyses and the validation was carried out according to International Conference on Harmonization validation guidelines Q2A and Q2B. The method was shown to be specific (no interference in the blank solution), linear (correlation coefficients ≥0.99998, n = 10), accurate (average recoveries between 94.1 and 101.7%), precise (intra-day and inter-day precision ≤2.6%), sensitive (limit of detection ≤0.2 ng, and limit of quantitation ≤0.7 ng), robust (small variations of carrier gas flow, initial oven temperature, temperature ramping rate, injector and detector temperatures did not significantly affect the system suitability test parameters and peak areas) and stable (reference standard and sample solutions were stable over 48 h). This extensively validated method is ready to be used for the quality control of blonanserin.

  13. Quantification of Biogenic and Anthropogenic Hydrocarbons using a Commercial Gas Chromatograph - Ion Trap Mass Spectrometer at a Ground Site near Fort McKay, AB

    Science.gov (United States)

    Tokarek, T. W.; Osthoff, H. D.

    2014-12-01

    The extraction of fossil fuels from the Alberta oil sands has been the focus of considerable attention due to its association with sizeable emissions of a variety of atmospheric pollutants, the magnitude and impacts of which are currently poorly constrained by observations. In order to more reliably estimate the magnitude and impact of these emissions, an intensive air quality measurement campaign, called "Fort McMurray Oil Sands Strategic Investigation of Local Sources" (FOSSILS), was conducted in the summer of 2013 as part of the Alberta-Canada joint oil sands monitoring program (JOSM) to identify and quantify emissions and their transformations from the Alberta oil sands. The challenge is that the region is surrounded by boreal forest, which provides a substantial background of biogenic hydrocarbons during summer. In this presentation, measurements of volatile organic compounds (VOCs) at the AMS13 ground site near Fort McKay, Alberta, from Aug 17 to Sept 6, 2013 using a commercial Griffin 450 gas chromatograph equipped with ion trap mass spectrometric detection and Tenax preconcentration are described. The combination of retention information and electron impact mass spectral data allowed unambiguous identification and quantification of the major biogenic monoterpenes, e.g., α and β-pinene, limonene, camphene, and 3Δ-carene, and of many anthropogenically derived hydrocarbons. Mixing ratios of biogenic hydrocarbons varied with time of day, temperature, and solar radiation, with maxima typically occurring at night, rationalized by nocturnal mixing heights and low mixing ratios of the nocturnal oxidants ozone (O3) and the nitrate radical (NO3). In contrast, mixing ratios of anthropogenic VOCs, e.g., benzene, toluene, ethyl benzene, and o-, p-, and m-xylene (BTEX), strongly depended on meteorological conditions, i.e., local wind direction. During episodes with high BTEX abundance, many additional high molecular weight hydrocarbons were observed which were not

  14. 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.

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

    Science.gov (United States)

    Araújo, Henrique Peres; Félix, Juliana Silva; Manzoli, José Eduardo; Padula, Marisa; Monteiro, Magali

    2008-07-01

    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.

  16. 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.

  17. 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.

  18. Gas Chromatographic Verification of a Mathematical Model: Product Distribution Following Methanolysis Reactions.

    Science.gov (United States)

    Lam, R. B.; And Others

    1983-01-01

    Investigated application of binomial statistics to equilibrium distribution of ester systems by employing gas chromatography to verify the mathematical model used. Discusses model development and experimental techniques, indicating the model enables a straightforward extension to symmetrical polyfunctional esters and presents a mathematical basis…

  19. 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

  20. 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

  1. A reliable gas capillary chromatographic determination of lactulose in dairy samples

    OpenAIRE

    Montilla, Antonia; Moreno, F. Javier; Olano, Agustín

    2005-01-01

    A gas capillary chromatography of silylated carbohydrates on SPB-17 phase (50% diphenyl/50% dimethylsiloxane) method for the determination of lactulose has been developed. The method has been evaluated for precision and accuracy using phenyl-β-D-glucoside as internal standard with satisfactory results and, then, applied to 27 commercial milk samples (pasteurized, UHT, sterilized, powder, condensed and chocolate-based milks). Results showed that it was suitable for the determination of lactulo...

  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. Gas chromatographic-mass spectrometric analysis of creosotes extracted from wooden sleepers installed in playgrounds

    Energy Technology Data Exchange (ETDEWEB)

    Rotard, W.; Mailahn, W.

    1987-01-01

    In order to evaluate their hygienic risk, wood samples from sleepers (railroad cross ties) impregnated with coal tar creosote were taken from playgrounds and investigated for hazardous compounds. The samples were extracted with ether, and acid-base-neutral separations were made on the creosote extracts. Water-soluble compounds were also isolated. All the fractions were investigated by capillary gas chromatography-mass spectrometry. Besides phenols in the acidic fractions and N-heterocyclic polynuclear aromatic hydrocarbons (PAH) in the basic fractions, high amounts of neutral PAH and also, in several samples high levels of carcinogenic and cocarcinogenic PAH were determined.

  4. 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

  5. Performance characteristics of methods of analysis used for regulatory purposes. I. Drug dosage forms. B. Gas chromatographic methods.

    Science.gov (United States)

    Horwitz, W; Albert, R

    1984-01-01

    Gas chromatographic methods for the analysis of drug dosage forms consist of a simple extraction, dilution with an internal standard solution, and injection, or, even simpler, dilution with the internal standard solution and injection. These methods were used in 7 collaborative studies of the determination of 12 pharmaceuticals, published in the Journal of the AOAC during 1973-1983. A total of 43 individual materials consisting of various dosage forms were each analyzed, usually in duplicate, by an average of 8 laboratories, with a total of 582 reported determinations. The average within-laboratory coefficient of variation (CVo) was 1.25% and the average among-laboratories coefficient of variation (CVx) was 2.41%, for a CVo/CVx ratio of 0.52, at an average outlier rate of 1.4% of the reported values. The line of best fit for CVx plotted against concentration increases with decreasing concentration, extending from a CVx of approximately 1.8% at 100% concentration to a CVx of approximately 3.2% at 1% concentration. The change in CVx for a 10-fold decrease in concentration is approximately 0.7% CVx, independent of analyte and matrix.

  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. Fast gas chromatographic residue analysis in animal feed using split injection and atmospheric pressure chemical ionisation tandem mass spectrometry.

    Science.gov (United States)

    Tienstra, M; Portolés, T; Hernández, F; Mol, J G J

    2015-11-27

    Significant speed improvement for instrumental runtime would make GC–MS much more attractive for determination of pesticides and contaminants and as complementary technique to LC–MS. This was the trigger to develop a fast method (time between injections less than 10 min) for the determination of pesticides and PCBs that are not (or less) amenable to LC–MS. A key factor in achieving shorter analysis time was the use of split injection (1:10) which allowed the use of a much higher initial GC oven temperature. A shorter column (15 m), higher temperature ramp, and higher carrier gas flow rate (6 mL/min) further contributed to analysis-time reduction. Chromatographic resolution was slightly compromised but still well fit-for-purpose. Due to the high sensitivity of the technique used (GC–APCI-triple quadrupole MS/MS), quantification and identification were still possible down to the 10 μg/kg level, which was demonstrated by successful validation of the method for complex feed matrices according to EU guidelines. Other advantages of the method included a better compatibility of acetonitrile extracts (e.g. QuEChERS) with GC, and a reduced transfer of co-extractants into the GC column and mass spectrometer.

  8. Integration and Ruggedization of a Commercially Available Gas Chromatograph and Mass Spectrometer (GCMS) for the Resource Prospector Mission (RPM)

    Science.gov (United States)

    Loftin, Kathleen; Griffin, Timothy; Captain, Janine

    2013-01-01

    The Resource Prospector is a mission to prospect for lunar volatiles (primarily water) at one of the two lunar poles, as well as demonstrate In-Situ Resource Utilization (ISRU) on the Moon. The Resource Prospector consists of a lander, a rover, and a rover-borne scientific payload. The Regolith and Environment Science and Oxygen & Lunar Volatile Extraction (RESOLVE) payload, will be able to (1) locate near subsurface volatiles, (2) excavate and analyze samples of the volatile-bearing regolith, and (3) demonstrate the form, extractability and usefulness of the materials. The gas chromatograph mass spectrometer (GCMS) is the primary instrument in the RESOLVE instrumentation suite responsible for identification and quantification of the volatiles evolved from the lunar regolith. Specifically, this instrument must have: a low mass, a low power consumption, be able to perform fast analyses of samples ranging from less than one to greater than ninety nine percent water by mass, be autonomously controlled by the payload's software and avionics platform, and be able to operate in the harsh lunar environment. The RPM's short mission duration is the primary driver of the requirement for a very fast analysis time currently base lined at less than 2 minutes per sample. This presentation will discuss the requirements levied upon the GCMS design, lessons learned from a preliminary field demonstration deployment, the current design, and the path forward.

  9. Capillary gas chromatographic analysis of nerve agents using large volume injections

    NARCIS (Netherlands)

    Degenhardt, C.E.A.M.; Kientz, C.E.

    1996-01-01

    The use of large volume injections has been studied for the verification of intact organophosphorus chemical warfare agents in water samples. As the use of ethyl acetate caused severe detection problems new potential solvents were evaluated. With the developed procedure, the nerve agents sarin,

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

    Science.gov (United States)

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

    2009-05-30

    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.

  11. 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.

  12. Gas chromatographic study of the volatile products from co-pyrolysis of coal and polyethylene wastes.

    Science.gov (United States)

    Domínguez, A; Blanco, C G; Barriocanal, C; Alvarez, R; Díez, M A

    2001-05-18

    The aim of this study was to determine the volatile products distribution of co-processing of coal with two plastic wastes, low-density polyethylene from agriculture greenhouses and high-density polyethylene from domestic uses, in order to explain the observed decrease in coal fluidity caused by polyethylene waste addition. Polymeric materials, although they are not volatile themselves, may be analysed by gas chromatography through the use of pyrolysis experiments. In this way, a series of pyrolysis tests were performed at 400 and 500 degrees C in a Gray-King oven with each of the two plastic wastes, one high-volatile bituminous coal and blends made up of coal and plastic waste (9:1, w/w, ratio). The pyrolysis temperatures, 400 and 500 degrees C, were selected on the basis of the beginning and the end of the coal plastic stage. The organic products evolved from the oven were collected, dissolved in pyridine and analysed by capillary gas chromatography using a flame ionization detector. The analysis of the primary tars indicated that the amount of n-alkanes is always higher than that of n-alkenes and the formation of the alkenes is favoured by increasing the pyrolysis temperature. However, this effect may be influenced by the size of the hydrocarbon. Thus, the fraction C17-C31 showed a higher increase of n-alkenes/n-alkanes ratio than other fractions. On the other hand, the difference between the experimental and estimated values from tars produced from single components was positive for n-alkanes and n-alkenes, indicating that co-pyrolysis of the two materials enhanced the chemical reactivity during pyrolysis and produced a higher conversion than that from individual components.

  13. Chromatographic fingerprint analysis of secondary metabolites in citrus fruits peels using gas chromatography-mass spectrometry combined with advanced chemometric methods.

    Science.gov (United States)

    Parastar, Hadi; Jalali-Heravi, Mehdi; Sereshti, Hassan; Mani-Varnosfaderani, Ahmad

    2012-08-17

    Multivariate curve resolution (MCR) and multivariate clustering methods along with other chemometric methods are proposed to improve the analysis of gas chromatography-mass spectrometry (GC-MS) fingerprints of secondary metabolites in citrus fruits peels. In this way, chromatographic problems such as baseline/background contribution, low S/N peaks, asymmetric peaks, retention time shifts, and co-elution (overlapped and embedded peaks) occurred during GC-MS analysis of chromatographic fingerprints are solved using the proposed strategy. In this study, first, informative GC-MS fingerprints of citrus secondary metabolites are generated and then, whole data sets are segmented to some chromatographic regions. Each chromatographic segment for eighteen samples is column-wise augmented with m/z values as common mode to preserve bilinear model assumption needed for MCR analysis. Extended multivariate curve resolution alternating least squares (MCR-ALS) is used to obtain pure elution and mass spectral profiles for the components present in each chromatographic segment as well as their relative concentrations. After finding the best MCR-ALS model, the relative concentrations for resolved components are examined using principal component analysis (PCA) and k-nearest neighbor (KNN) clustering methods to explore similarities and dissimilarities among different citrus samples according to their secondary metabolites. In general, four clear-cut clusters are determined and the chemical markers (chemotypes) responsible to this differentiation are characterized by subsequent discriminate analysis using counter-propagation artificial neural network (CPANN) method. It is concluded that the use of proposed strategy is a more reliable and faster way for the analysis of large data sets like chromatographic fingerprints of natural products compared to conventional methods. Copyright © 2012 Elsevier B.V. All rights reserved.

  14. System and method for detecting gas

    Science.gov (United States)

    Chow, Oscar Ken; Moulthrop, Lawrence Clinton; Dreier, Ken Wayne; Miller, Jacob Andrew

    2010-03-16

    A system to detect a presence of a specific gas in a mixture of gaseous byproducts comprising moisture vapor is disclosed. The system includes an electrochemical cell, a transport to deliver the mixture of gaseous byproducts from the electrochemical cell, a gas sensor in fluid communication with the transport, the sensor responsive to a presence of the specific gas to generate a signal corresponding to a concentration of the specific gas, and a membrane to prevent transmission of liquid moisture, the membrane disposed between the transport and the gas sensor.

  15. Gas chromatographic and electron spin resonance investigations of gamma-irradiated frog legs

    International Nuclear Information System (INIS)

    Morehouse, K.M.; Ku, Yuoh; Albrecht, H.L.; Yang, G.C.

    1991-01-01

    Several very sensitive techniques to measure radiation-induced products in frog legs were investigated. Presented here are results from the use of electron spin resonance (ESR) spectroscopy and capillary gas chromatography (GC) to measure radiolysis products in γ-irradiated frog legs. When bone is irradiated, a characteristic ESR signal develops and is easily measured. The intensity of the ESR signal is dose-dependent and stable for several months at room temperature. When triglycerides or fatty acids are irradiated, some of the major stable products formed are hydrocarbons with one less carbon than the precursor fatty acids. These hydrocarbons are formed as the result of the loss of CO 2 during various free radical reactions. A capillary GC procedure was developed to monitor the formation of these hydrocarbons in γ-irradiated frog legs. Since frog legs contain large amounts of palmitic, stearic, oleic, and linoleic acids, the formation of the hydrocarbons (pentadecane, heptadecane, 8-heptadecene, and 6,9-heptadecadiene, respectively) from the decarboxylation of these fatty acids was monitored. The yields of these hydrocarbons were found to be linear with applied dose. A sample from a lot of imported frog legs that were believed to have been treated with ionizing radiation was also analyzed. The ESR technique, in conjunction with the GC data on the hydrocarbons, appears to be a useful approach for identifying and monitoring frog legs that have been treated with ionizing radiation. (author)

  16. A gas chromatographic method for the identification of gamma-irradiated frog legs

    International Nuclear Information System (INIS)

    Morehouse, K.M.; Yuoh Ku

    1990-01-01

    When triglycerides or fatty acids are irradiated, some of the major stable products formed are hydrocarbons with one less carbon than the parent fatty acids. These hydrocarbons are formed as the result of the loss of CO 2 via various free radical reactions. A procedure has been developed utilizing capillary gas chromatography (GC) to monitor the formation of these hydrocarbons in gamma-irradiated frog legs. Since frog legs contain large amounts of palmitic, stearic, oleic, and linoleic acids, the formation of the hydrocarbons (pentadecane, heptadecane, 8-heptadecene, and 6,9-heptadecadiene, respectively) from the decarboxylation of these fatty acids was monitored. The yield of these hydrocarbons was found to be linear with applied dose. A sample from a lot of imported frog legs that were believed to have been irradiated was also analyzed. The results obtained from the GC determination of the hydrocarbons compared favorably with those obtained by using electron spin resonance to monitor the free radicals trapped in the frog leg bone after irradiation. (author)

  17. Evaluation of gas chromatographic methods for the determination of trans fat.

    Science.gov (United States)

    Delmonte, Pierluigi; Rader, Jeanne I

    2007-09-01

    Consumption of trans fat has been associated with increased risk of coronary heart disease. For nutrition labeling purposes, the US Food and Drug Administration (FDA) defines trans fat as the sum of all the fatty acids with at least one nonconjugated double bond in the trans configuration. The FDA regulation states that label declarations of trans fat are not required for products that contain less than 0.5 g of trans fat per serving if no claims are made about fat, fatty acids or cholesterol. While attenuated total reflection Fourier-transformed infrared spectroscopy (ATR-FT-IR) provides reproducible measurements for samples containing more than 5% trans fat, methods based on gas chromatography (GC) are needed to measure lower trans fat levels. Trans fat quantitation by GC has recently been updated by considering more fatty acids, focusing more attention on fatty acids present in low amounts, and by using 100-m high-polarity capillary columns for optimal separation. The consistently high interlaboratory relative standard deviations (RSD, e.g., 21% at 1% trans fatty acids (TFA), 60% at 0.17% TFA), and intralaboratory RSD values (e.g., 10% at 1% TFA, 16% at 0.17% TFA) for trans fat at 1% or less of total fat reported in the collaborative study data for American Oil Chemists Society Official Method Ce 1h-05 suggest the need to carefully define the parameters associated with GC analysis of fatty acids.

  18. 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.

  19. 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

  20. Cross-column prediction of gas-chromatographic retention of polybrominated diphenyl ethers.

    Science.gov (United States)

    D'Archivio, Angelo Antonio; Giannitto, Andrea; Maggi, Maria Anna

    2013-07-12

    In this paper, we predict the retention of polybrominated diphenyl ethers (PBDEs) in capillary gas-chromatography (GC) within a useful range of separation conditions. In a first stage of this study, quantitative structure-retention relationships (QSRRs) of PBDEs in six stationary phases with different polarity are established. The single-column QSRR models are generated using the retention data of 126 PBDE congeners by multilinear regression (MLR) coupled to genetic algorithm variable selection applied to a large set of theoretical molecular descriptors of different classes. A quite accurate fitting of experimental retentions is obtained for each of the six GC columns adopting five molecular descriptors. In a further step of this work six molecular descriptors were extracted within the set of molecular descriptors (17 variables) involved in the various single-column QSRRs. The selected molecular descriptors are combined with observed retentions of ten representative PBDEs, adopted as descriptors of the GC system. These quantities are considered as the independent variables of a multiple-column retention model able to simultaneously relate GC retention to PBDE molecular structure and kind of column. The quantitative structure/column-retention relationship is established using a multi-layer artificial neural network (ANN) as regression tool. To optimise the ANN model, a validation set is generated by selecting two out of the six calibration columns. Splitting of columns between training and validation sets, as well as selection of PBDE congeners to be used as column descriptors, is performed with the help of a principal component analysis on the retention data. Cross-column predictive performance of the final model is tested on a large external set consisting of retention data of 180 PBDEs collected in four separation conditions different from those considered in model calibration (different columns and/or temperature program). Copyright © 2013 Elsevier B.V. All

  1. Characterization of low-temperature cofired ceramic tiles as platforms for gas chromatographic separations.

    Science.gov (United States)

    Darko, Ernest; Thurbide, Kevin B; Gerhardt, Geoff C; Michienzi, Joseph

    2013-06-04

    A gas chromatography (GC) column is fabricated within a low-temperature cofired ceramic (LTCC) tile, and its analytical properties are characterized. By using a dual-spiral design, a 100 μm wide square channel up to 15 m in length is produced within an 11 cm × 5.5 cm LTCC tile. The channel is dynamically coated with an OV-101 stationary phase that is cross-linked with dicumyl peroxide. While the uncoated LTCC tiles were able to separate a mixture of n-alkanes, the peak shapes were broad (base width of ~2 min) and tailing. In contrast to this, the coated LTCC tiles produced sharp (base width of ~8-10 s), symmetrical, well-resolved peaks for the same analytes. By using a 7.5 m long channel, about 15,000 plates were obtained for a dodecane test analyte. Further, the coated LTCC tiles were found to produce plate heights that were about 3-fold smaller than those obtained from a conventional capillary GC column of similar length, dimension, and coating operated under the same conditions. As a result, test analyte separations were slightly improved in the LTCC tiles, and their overall performance fared well. In terms of temperature programming, it was found that a series of n-alkanes separated on the LTCC tile provided a cumulative peak capacity of around 54 peaks when using C₈ to C₁₃ as analyte markers. Results indicate that LTCC tiles provide a viable and useful alternative platform for performing good quality GC separations.

  2. A fully automated chromatographic peak detection and treatment software for multi-user multi-task computers.

    Science.gov (United States)

    Cardot, P J; Trolliard, P; Tembely, S

    1990-01-01

    A fully automated method is presented for the detection and integration of chromatographic peak software in which the only parameter to define is the data acquisition frequency; this has to be chosen high enough to minimize some Nyquist frequency problems. Programmed in C language, the software is used on a Unix like system (Xenix) to emphasize its automaticity. The performance of the system in liquid chromatography has been studied in respect of noise frequency and intensity. It is shown that the classical signal-to-noise ratio is obsolete for definition of the detection limit since frequency analysis allows some signal filtration; these limitations are described. An example is given of simulation with Gaussian peaks convoluted with noise characterized by its intensity and frequency distribution. The validity of the software is demonstrated for some HPLC separations.

  3. Gas chromatographic--mass spectrometric quantitation of 16, 16-dimethyl-trans-delta 2-PGE1

    Energy Technology Data Exchange (ETDEWEB)

    Dimov, V.; Green, K.; Bygdeman, M.; Konishi, Y.; Imaki, K.; Hayashi, M.

    1983-02-01

    Di-deuterated and di-tritiated 16,16-dimethyl-trans-delta 2-PGE1 has been synthesized and used for development of a GC-MS method for quantitation of corresponding unlabelled drug in patient plasma. Although these carrier/internal standard molecules only contain 2 deuterium atoms the lower limit of detection at each injection is as low as about 40 pg. The maximum plasma levels of this drug following administration of vaginal suppositories used in clinical studies (1 mg 16,16-dimethyl-trans-delta 2-PGE1 methyl ester in 0.8 g Witepsol S-52) were 100-350 pg/ml i.e. in the same order of magnitude as earlier seen for 16,16-dimethyl-PGE2.

  4. Gas chromatographic--mass spectrometric quantitation of 16, 16-dimethyl-trans-delta 2-PGE1

    International Nuclear Information System (INIS)

    Dimov, V.; Green, K.; Bygdeman, M.; Konishi, Y.; Imaki, K.; Hayashi, M.

    1983-01-01

    Di-deuterated and di-tritiated 16,16-dimethyl-trans-delta 2-PGE1 has been synthesized and used for development of a GC-MS method for quantitation of corresponding unlabelled drug in patient plasma. Although these carrier/internal standard molecules only contain 2 deuterium atoms the lower limit of detection at each injection is as low as about 40 pg. The maximum plasma levels of this drug following administration of vaginal suppositories used in clinical studies (1 mg 16,16-dimethyl-trans-delta 2-PGE1 methyl ester in 0.8 g Witepsol S-52) were 100-350 pg/ml i.e. in the same order of magnitude as earlier seen for 16,16-dimethyl-PGE2

  5. [Residues of organochlorine compounds in plant drugs. 1. Gas chromatographic determination of residues of organochlorine insecticides].

    Science.gov (United States)

    Benecke, R; Thieme, H; Brotka, J

    1986-02-01

    A method for the identification and determination of HCH-and DDT-isomers and their respective metabolites in vegetable drugs is presented. The plant material is extracted with hexane in a Soxhlet apparatus in the presence of silicagel and sodium sulfate. For removing interfering endogenous plant constituents a Celite oleum column cleanup and usually and acetonitrile partitioning to follow are necessary. A mixed stationary phase OV-17/QF-1 has proved effective for the gc separation on packed columns. 3H-ECD is used for detection. For the quantitative determination by using an external standard the peak height measurement is recommended. Recoveries of all insecticides were in the order of 70-105% with coefficients of variation between 6 and 20%. To ensure the results the alkaline treatment and oxidation of extracts are proposed.

  6. Validation of a gas chromatographic method to quantify sesquiterpenes in copaiba oils.

    Science.gov (United States)

    Sousa, João Paulo B; Brancalion, Ana P S; Souza, Ariana B; Turatti, Izabel C C; Ambrósio, Sérgio R; Furtado, Niege A J C; Lopes, Norberto P; Bastos, Jairo K

    2011-03-25

    Copaifera species (Leguminoseae) are popularly known as "copaiba" or "copaíva". The oleoresins obtained from the trunk of these species have been extensively used in folk medicine and are commercialized in Brazil as crude oil and in several pharmaceutical and cosmetic products. This work reports a complete validated method for the quantification of β-caryophyllene, α-copaene, and α-humulene in distinct copaiba oleoresins available commercially. Thus, essential oil samples (100μL) were dissolved in 20mL of hexanes containing internal standard (1,2,4,5-tetramethylbenzene, 3.0mM) in a 25mL glass flask. A 1μL aliquot was injected into the GC-FID system. A fused-silica capillary column HP-5, coated with 5% phenyl-methylsiloxane was used for this study. The developed method gave a good detection response with linearity in the range of 0.10-18.74mM. Limits of detection and quantitation variety ranged between 0.003 and 0.091mM. β-Caryophyllene, α-copaene, and α-humulene were recovered in a range from 74.71% to 88.31%, displaying RSD lower than 10% and relative errors between -11.69% and -25.30%. Therefore, this method could be considered as an analytical tool for the quality control of different Copaifera oil samples and its products in both cosmetic and pharmaceutical companies. Copyright © 2010 Elsevier B.V. All rights reserved.

  7. Gas theft: Prevention and detection

    International Nuclear Information System (INIS)

    Johnson, G.

    1992-01-01

    The problem of gas theft is discussed. Roughly 2% of gas and power customers in the United States either steal or attempt to steal service. Most diversion programs focus on theft from a revenue protection viewpoint, however there is often insufficient money recovered to justify an anti-theft program. Successful action often involves focusing on large volume users. Safety should be a prime consideration in searching out gas theft, as many people have been killed or injured as a result of careless theft. A brief review is presented of anti-theft devices such as locks and seals; automated meter reading can also help reduce theft. The best defence against theft is a highly trained and motivated field staff, especially meter readers, and a computer billing program that monitors changes in gas usage. Fixed bypasses may be unlocked and used at will; fraud is also common. Investigation and prosecution should be carried out by trained personnel following a carefully developed procedure. Safety issues should be stressed, and every effort should be made to avoid the appearance that the justice system is being used as a bill collector. 3 refs

  8. Remote flammable gas detection/measuring device.

    CSIR Research Space (South Africa)

    Kononov, VA

    1999-11-01

    Full Text Available This research report presents the results of an evaluation of the existing open path remote flammable gas detection/monitoring technology and provides recommendations on possible limited implementation of this technology and future development...

  9. Italian and Argentine olive oils: a NMR and gas chromatographic study

    Directory of Open Access Journals (Sweden)

    Segre, Annalaura

    2001-12-01

    Full Text Available High-field Nuclear Magnetic Resonance (NMR spectroscopy and Gas Chromatography (GC were used to analyze 16 monovarietal olive oils obtained from few matched Mediterranean cultivars grown in experimental fields located in Italy and in the Catamarca region of Argentina. The Catamarca region is characterized by extreme pedoclimatic conditions and by a wild spontaneous vegetation. The proposed sampling allows to study the effect of different pedoclimatic conditions on olive oil composition. GC gives the fatty acid profile of olive oil samples. 1H and 13C NMR techniques provide different information: the 1H NMR spectrum allows the measurement of minor components of olive oils such as b-sytosterol, hexanal, trans-2-hexenal, formaldehyde, squalene, cycloartenol and linolenic acid; the 1C NMR spectrum allows to obtain information about glycerol tri-esters of olive oils, i.e., about their acyl composition and positional distribution on glycerol moiety. All the NMR and GC results have been submitted to Linear Discriminant Analysis (LDA and Tree Cluster Analysis (TCA. A careful analysis of the statistical results allows to select the Mediterranean cultivars less affected by the climatic conditions present in the Catamarca region. The selected cultivars produce olive oils which keep their Mediterranean characteristics and which can be proposed as colonizing plants in this wild Argentine region.La espectroscopía de Resonancia Magnética Nuclear de alta resolución (RMN y Cromatografía Gaseosa (CG fueron utilizadas para analizar 16 monovariedades de aceites de oliva, obtenidas de algunos olivares Mediterráneos cultivados contemporáneamente en campos experimentales localizados en Italia y en la región de Catamarca en Argentina. Estas muestras permiten estudiar diferentes condiciones pedoclimáticas en la composición de los aceite de oliva. La CG proporciona el perfil en ácidos grasos de los aceites de oliva y las técnicas RMN 1H y RMN 13C suministran

  10. Gas chromatographic determination of amino acid enantiomers in bottled and aged wines.

    Science.gov (United States)

    Ali, Hatem Salama Mohammed; Pätzold, Ralf; Brückner, Hans

    2010-03-01

    Free L- and D-amino acids were determined by chiral GC-MS in 26 wines, comprising white wines, red wines, ice wines and sparkling wines. The aim of the work was to investigate whether quantities and pattern of D-amino acids, in particular D-proline, correlate with the storage time of bottled wines. The relative quantities with respect to the corresponding L-enantiomer ranged in white wines from 0.4 to 3.9% D-Ala, 0.9-8.3% D-Asx, and 0.5-8.9% D-Glx, in red wines from 2.9 to 10.6% D-Ala, 2.2-10.9% D-Asx, and 3.9-7.4% D-Glx, and in sparkling wines from 2.2 to 9.8% D-Ala, 2.1-4.4% D-Asx and 1.3-6.1% D-Glx. Low relative quantities of 0.3-0.7% D-Pro were detected in three white wines stored for more than 20 years and did not exceed 0.2% D-Pro in two red wines stored for 10 and 20 years, respectively. An ice wine stored for 24 years contained 0.9% D-Pro, 6.4% D-Glx, 3.0% D-Asp and 1.5% D-Ala. The data confirm the presence of D-amino acids in wines. They do not provide evidence for a correlation between the storage time of bottled wines and quantities of D-amino acids.

  11. 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)

  12. Microstructure fibers for gas detection

    Czech Academy of Sciences Publication Activity Database

    Matějec, Vlastimil; Mrázek, Jan; Hayer, Miloš; Peterka, Pavel; Kaňka, Jiří; Honzátko, Pavel; Berková, Daniela

    2006-01-01

    Roč. 26, 2/3 (2006), s. 317-321 ISSN 0928-4931. [MADICA 2004. Tunis, 29.11.2004-01.12.2004] R&D Projects: GA ČR(CZ) GA102/02/0779 Institutional research plan: CEZ:AV0Z2067918 Keywords : photonic crystals * crystal microstructure * optical fibres * fibre optic sensors * gas Subject RIV: JB - Sensors, Measurment, Regulation Impact factor: 1.325, year: 2006

  13. Sonographic detection of portal venous gas

    International Nuclear Information System (INIS)

    Lee, Wang Yul; Lee, S. K.; Cho, O. K.

    1989-01-01

    Portal venous gas suggests underlying bowel disease such as strangulating intestinal obstruction and its demonstration carries with it an important implications with respect to patient management. Radiography has been the gold standard for the detection of portal venous gas. We have experienced two cases of portal venous gas diagnosed by ultrasound. Sonographic findings were floating echoes in the main portal vein and highly echogenic linear or patchy echoes within the hepatic parenchyma. Simple abdominal films of those cases failed to demonstrate gas in the portal venous system

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

    OpenAIRE

    E.O. Odebunmi; E.A. Ogunsakin; P.E.P. Ilukhor

    2002-01-01

    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 r...

  15. Rapid Analysis Procedures for Triglycerides and Fatty Acids as Pentyl and Phenethyl Esters for the Detection of Butter Adulteration Using Chromatographic Techniques

    Directory of Open Access Journals (Sweden)

    Daniele Naviglio

    2017-01-01

    Full Text Available This paper presents the development of three methods for quality control, fraud detection, and authentication of butter fat and other oils/fats using chromatographic techniques, with one method for triglycerides and two methods for fatty acids (FAs. The procedure for the analysis of triglycerides requires only dissolution of the sample in n-hexane and gas chromatography (GC analysis using a capillary column. The second method is based on the transesterification of triglycerides as pentyl esters in a single-step reaction using sodium pentanoate in pentanol. The reaction proceeds at room temperature and is similar to the potassium hydroxide-catalysed transesterification of triglycerides with methanol and even more similar to the sodium methoxide method and sodium butanoate method. The advantage of using pentyl esters includes reducing the volatility of short-chain FAs, and substantial recoveries were obtained compared with methyl ester analysis. The third method involves the transesterification of triglycerides in fat through reaction with 2-phenylethanol in a single step; 2-phenylethanol possesses a chromophore, and the phenethyl esters formed are analysed by high-performance liquid chromatography (HPLC with UV detection.

  16. Mass spectral identification and gas-liquid chromatographic determination of methyl 4-chloroindolyl-3-acetate in canned and frozen peas.

    Science.gov (United States)

    Heikes, D L

    1980-11-01

    Methyl 4-chloroindolyl-3-acetate (MCIA), a naturally occurring auxin, has been identified in canned and frozen peas by gas-liquid chromatography (GLC)/mass spectrometry. Eight samples were analyzed for MCIA using slightly modified official AOAC multiple pesticide residue procedures employing GLC with microcoulometric detection. Levels of MCIA averaged 0.20 ppm for canned peas and 0.16 ppm for frozen peas. Recovery of MCIA from a fortified sample was 40%.

  17. Permanent gas analysis using gas chromatography with vacuum ultraviolet detection.

    Science.gov (United States)

    Bai, Ling; Smuts, Jonathan; Walsh, Phillip; Fan, Hui; Hildenbrand, Zacariah; Wong, Derek; Wetz, David; Schug, Kevin A

    2015-04-03

    The analysis of complex mixtures of permanent gases consisting of low molecular weight hydrocarbons, inert gases, and toxic species plays an increasingly important role in today's economy. A new gas chromatography detector based on vacuum ultraviolet (VUV) spectroscopy (GC-VUV), which simultaneously collects full scan (115-240 nm) VUV and UV absorption of eluting analytes, was applied to analyze mixtures of permanent gases. Sample mixtures ranged from off-gassing of decomposing Li-ion and Li-metal batteries to natural gas samples and water samples taken from private wells in close proximity to unconventional natural gas extraction. Gas chromatography separations were performed with a porous layer open tubular column. Components such as C1-C5 linear and branched hydrocarbons, water, oxygen, and nitrogen were separated and detected in natural gas and the headspace of natural gas-contaminated water samples. Of interest for the transport of lithium batteries were the detection of flammable and toxic gases, such as methane, ethylene, chloromethane, dimethyl ether, 1,3-butadiene, CS2, and methylproprionate, among others. Featured is the capability for deconvolution of co-eluting signals from different analytes. Copyright © 2015 Elsevier B.V. All rights reserved.

  18. Gas sensitive materials for gas detection and method of making

    Science.gov (United States)

    Trakhtenberg, Leonid Israilevich; Gerasimov, Genrikh Nikolaevich; Gromov, Vladimir Fedorovich; Rozenberg, Valeriya Isaakovna

    2012-12-25

    A gas sensitive material comprising SnO2 nanocrystals doped with In2O3 and an oxide of a platinum group metal, and a method of making the same. The platinum group metal is preferably Pd, but also may include Pt, Ru, Ir, and combinations thereof. The SnO2 nanocrystals have a specific surface of 7 or greater, preferably about 20 m2/g, and a mean particle size of between about 10 nm and about 100 nm, preferably about 40 nm. A gas detection device made from the gas sensitive material deposited on a substrate, the gas sensitive material configured as a part of a current measuring circuit in communication with a heat source.

  19. Gas sensitive materials for gas detection and methods of making

    Science.gov (United States)

    Trakhtenberg, Leonid Israilevich; Gerasimov, Genrikh Nikolaevich; Gromov, Vladimir Fedorovich; Rozenberg, Valeriya Isaakovna

    2014-07-15

    A gas sensitive material comprising SnO.sub.2 nanocrystals doped with In.sub.2O.sub.3 and an oxide of a platinum group metal, and a method of making the same. The platinum group metal is preferably Pd, but also may include Pt, Ru, Ir, and combinations thereof. The SnO.sub.2 nanocrystals have a specific surface of 7 or greater, preferably about 20 m2/g, and a mean particle size of between about 10 nm and about 100 nm, preferably about 40 nm. A gas detection device made from the gas sensitive material deposited on a substrate, the gas sensitive material configured as a part of a current measuring circuit in communication with a heat source.

  20. Interlaboratory study of a multiresidue gas chromatographic method for determination of organochlorine and pyrethroid pesticides and polychlorobiphenyls in milk, fish, eggs, and beef fat.

    Science.gov (United States)

    Bordet, François; Inthavong, Dary; Fremy, Jean-Marc

    2002-01-01

    An interlaboratory study was conducted to validate a gas chromatographic (GC) method for determination of 21 organochlorine pesticides, 6 pyrethroid pesticides, and 7 polychlorobiphenyl (PCB) congeners in milk, beef fat, fish, and eggs. The method was performed at low contamination levels, which represent relevant contents in food, and is an extension of the European standard (method NF-EN-1528, Parts 1-4). It enlarges the applicable scope of the reference EN method to pyrethroid pesticides and proposes the use of solid-phase extraction (SPE) as a cleanup procedure. Cryogenic extraction was made, and SPE cleanup was performed with 2 successive SPE cartridges: C18 and Florisil. After injection of the purified extract onto a GC column, residues were measured by electron capture detection. Food samples (liquid milk, beef fat, mixed fish, and mixed eggs) were prepared, tested for homogeneity, and sent to 17 laboratories in France. Test portions were spiked with 27 pesticides and 7 PCBs at levels from 26 to 45, 4 to 27, 31 to 67, and 19 to 127 ng/g into milk, eggs, fish, and fat, respectively. Based on results for spiked samples, the relative standard deviation for repeatability ranged from 1.5 to 6.8% in milk, 3 to 39% in eggs, 4.5 to 12.2% in fish, and 7 to 13% in fat. The relative standard deviation for reproducibility ranged from 33 to 50% in milk, 29 to 59% in eggs, 31 to 57% in fish, and 30 to 62% in fat. This method showed acceptable intra- and interlaboratory precision data, as corroborated by HORRAT values at low levels of pesticide and PCB contamination. The statistical evaluation of the results was performed according to the International Organization for Standardization (ISO; ISO 3534 standard) and 5725-2 Guideline.

  1. On greenhouse gas signal detection strategies

    International Nuclear Information System (INIS)

    Barnett, T.P.; Schlesinger, M.E.; Xingjian Jiang

    1990-01-01

    Important elements of a greenhouse gas signal detection strategy are discussed and demonstrated with both model and observed data. The analysis also demonstrates the high level of unexplained interdecadal variability that occurs naturally in the climate system and how this noise will greatly complicate any detection strategy. The indisputable detection of a greenhouse gas signal in the global climate system will be a true decision point for mankind. Yet, at this stage of knowledge, the details of an appropriate detection strategy are only beginning to be developed. Two key elements in the eventual strategy are the subject of this report: (1) what variables should be monitored in a detection program, and (2) the comparison of the equilibrium versus transient climate system response. Subsequent sections consider these items in turn, while a final section summarizes the main conclusion of the study

  2. Parabens determination in cosmetic and personal care products exploiting a multi-syringe chromatographic (MSC) system and chemiluminescent detection.

    Science.gov (United States)

    Rodas, Melisa; Portugal, Lindomar A; Avivar, Jessica; Estela, José Manuel; Cerdà, Víctor

    2015-10-01

    Parabens are widely used in dairy products, such as in cosmetics and personal care products. Thus, in this work a multi-syringe chromatographic (MSC) system is proposed for the first time for the determination of four parabens: methylparaben (MP), ethylparaben (EP), propylparaben (PP) and butylparaben (BP) in cosmetics and personal care products, as a simpler, practical, and low cost alternative to HPLC methods. Separation was achieved using a 5mm-long precolumn of reversed phase C18 and multi-isocratic separation, i.e. using two consecutive mobile phases, 12:88 acetonitrile:water and 28:72 acetonitrile:water. The use of a multi-syringe buret allowed the easy implementation of chemiluminescent (CL) detection after separation. The chemiluminescent detection is based on the reduction of Ce(IV) by p-hydroxybenzoic acid, product of the acid hydrolysis of parabens, to excite rhodamine 6G (Rho 6G) and measure the resulting light emission. Multivariate designs combined with the concepts of multiple response treatments and desirability functions have been employed to simultaneously optimize and evaluate the responses. The optimized method has proved to be sensitive and precise, obtaining limits of detection between 20 and 40 µg L(-1) and RSD <4.9% in all cases. The method was satisfactorily applied to cosmetics and personal care products, obtaining no significant differences at a confidence level of 95% comparing with the HPLC reference method. Copyright © 2015 Elsevier B.V. All rights reserved.

  3. Gas chromatographic-mass spectroscopic determination of benzene in indoor air during the use of biomass fuels in cooking time.

    Science.gov (United States)

    Sinha, Sukesh Narayan; Kulkarni, P K; Desai, N M; Shah, S H; Patel, G M; Mansuri, M M; Parikh, D J; Saiyed, H N

    2005-02-18

    A gas chromatography-mass spectroscopic method in electron ionization (EI) mode with MS/MS ion preparation using helium at flow rate 1 ml min(-1) as carrier gas on DB-5 capillary column (30 m x 0.25 mm i.d. film thickness 0.25 microm) has been developed for the determination of benzene in indoor air. The detection limit for benzene was 0.002 microg ml(-1) with S/N: 4 (S: 66, N: 14). The benzene concentration for cooks during cooking time in indoor kitchen using dung fuel was 114.1 microg m(-3) while it was 6.6 microg m(-3) for open type kitchen. The benzene concentration was significantly higher (p analytical chemist dealing with GC-MS in confirmation and quantification of benzene in environmental samples with health risk exposure assessment.

  4. Comparison of two detection methods in thin layer chromatographic analysis of herbicides in a coastal savannah soil

    International Nuclear Information System (INIS)

    Afful, S.; Yeboah, P.O.; Dogbe, S.A.; Akpabli, C.K.

    2004-01-01

    o-tolidine + potassium iodide and photosynthesis inhibition detection methods, were investigated for the analysis of three triazine herbicides (atrazine, ametryne, simazine), and two urea herbicides (diuron, metobromuron) in a coastal savannah soil using thin layer chromatographic methodology to compare the suitability of the two methods for the study of the herbicides. This was done by spiking 5 g of the soil sample with specific amount of the herbicides standard to generate herbicide-soil concentration of 40.23, 40.28, 41.46, 39.90 and 40.64 μ g/g for atrazine, ametryne, simazine, diuron and metobromuron respectively. Extraction was performed with acetone/hexane mixture (4:1) and the detection limit of each herbicide was then determined. In all, the photosynthesis inhibition method performed better for both the triazine and the urea herbicides, while the o-tolidine + potassium iodide method was suitable for only the triazine herbicides. With the photosynthesis inhibition method, detectability in the range of 0.004 - 0.008±0.02 μ g/g was attained for the herbicides using the unclean extracts. In the case of o-tolidine ± potassium iodide method, detectability of 0.008 - 0.40 0.02 ± g/g was obtained. With the clean up extracts, detectability in the range of 0.025 - 0.162±0.004 μ g/g was obtained using the photosynthesis inhibition method, however, metobromuron was not detected with the clean up extracts with the o-tolidine + KI method. (au)

  5. Exploring reverse shape selectivity and molecular sieving effect of metal-organic framework UIO-66 coated capillary column for gas chromatographic separation.

    Science.gov (United States)

    Chang, Na; Yan, Xiu-Ping

    2012-09-28

    Metal-organic frameworks (MOFs) which offer a variety of topologies, porous networks and high surface areas are promising and have potential for the applications of specific adsorption, isomerization, catalysis and separation. UIO-66 is the first MOF that has been observed to have reverse shape selectivity. However, such reverse shape selectivity of MOFs has never been explored for capillary gas chromatographic separation. Here we report the fabrication of MOF UIO-66 coated capillary column and exploration of the reverse shape selectivity and molecular sieving effect of such column for capillary gas chromatographic separation of alkane isomers and benzene homologues with excellent selectivity and precision. The adsorption enthalpies and entropies on the interaction between hydrocarbons and UIO-66 were measured to illustrate the energy effect on the separation of alkane isomers and benzene homologues on the UIO-66 coated capillary column. UIO-66 coated capillary column gave preferential retention of branched alkane isomers over their linear isomer, showing reverse shape selectivity, making UIO-66 coated capillary column attractive for capillary gas chromatographic separation of alkane isomers. iso-Propylbenzene (branched) eluted after n-propylbenzene on the UIO-66 coated capillary column again shows reverse shape selectivity. However, much bulkier 1,3,5-trimethylbenzene eluted earlier than n-propylbenzene and iso-propylbenzene on the UIO-66 coated capillary column, exhibiting molecular sieving effect. The combination of reverse shape selectivity with molecular sieving effect makes the UIO-66 coated capillary column promising for the separation of structural isomers. Copyright © 2012 Elsevier B.V. All rights reserved.

  6. Determination of triazine and chloroacetanilide herbicides in soils by microwave-assisted extraction (MAE) coupled to gas chromatographic analysis with either GC-NPD or GC-MS.

    Science.gov (United States)

    Vryzas, Zisis; Papadopoulou-Mourkidou, Euphemia

    2002-08-28

    A simple and rapid method based on microwave-assisted extraction (MAE) coupled to gas chromatographic analysis was developed for the analysis of triazine (atrazine, cyanazine, metribuzine, simazine and deethylatrazine, and deisopropylatrazine) and chloroacetanilide (acetochlor, alachlor, and metolachlor) herbicide residues in soils. Soil samples are processed by MAE for 5 min at 80 degrees C in the presence of acetonitrile (20 mL/sample). Mean recovery values of most solutes are >80% in the 10 to 500 microg/kg fortification range with respective RSDs (relative standard deviations) NPD) or a mass spectrometric detector (GC-MS).

  7. Automated chromatographic system with polarimetric detection laser applied in the control of fermentation processes and seaweed extracts characterization

    International Nuclear Information System (INIS)

    Fajer, V.; Naranjo, S.; Mora, W.; Patinno, R.; Coba, E.; Michelena, G.

    2012-01-01

    There are presented applications and innovations of chromatographic and polarimetric systems in which develop methodologies for measuring the input molasses and the resulting product of a fermentation process of alcohol from a rich honey and evaluation of the fermentation process honey servery in obtaining a drink native to the Yucatan region. Composition was assessed optically active substances in seaweed, of interest to the pharmaceutical industry. The findings provide measurements alternative raw materials and products of the sugar industry, beekeeping and pharmaceutical liquid chromatography with automated polarimetric detection reduces measurement times up to 15 min, making it comparable to the times of high chromatography resolution, significantly reducing operating costs. By chromatography system with polarimetric detection (SCDP) is new columns have included standard size designed by the authors, which allow process samples with volumes up to 1 ml and reduce measurement time to 15 min, decreasing to 5 times the volume sample and halving the time of measurement. Was evaluated determining the concentration of substances using the peaks of the chromatograms obtained for the different columns and calculate the uncertainty of measurements. The results relating to the improvement of a data acquisition program (ADQUIPOL v.2.0) and new programs for the preparation of chromatograms (CROMAPOL CROMAPOL V.1.0 and V.1.2) provide important benefits, which allow a considerable saving of time the processing of the results and can be applied in other chromatography systems with the appropriate adjustments. (Author)

  8. Immuno-chromatographic wicking assay for the rapid detection of dengue viral antigens in mosquitoes (Diptera: Culicidae).

    Science.gov (United States)

    Wanja, Elizabeth; Parker, Zahra F; Odusami, Oluwakemi; Rowland, Tobin; Davé, Kirti; Davé, Sonia; Turell, Michael J

    2014-01-01

    There is a threat for dengue virus (DENV) reemergence in many regions of the world, particularly in areas where the DENV vectors, Aedes aegypti (L.) and Aedes albopictus (Skuse), are readily available. However, there are currently no accurate and reliable diagnostic methods to provide critical, real-time information for early detection of DENV within the vector populations to implement appropriate vector control and personal protective measures. In this article, we report the ability of an immuno-chromatographic assay developed by VecTOR Test Systems Inc. to detect DENV in a pool of female Aedes mosquitoes infected with any of the four viral serotypes. The DENV dipstick assay was simple to use, did not require a cold chain, and provided clear results within 30 min. It was highly specific and did not cross-react with samples spiked with West Nile, yellow fever, Japanese encephalitis, Rift Valley fever, chikungunya, Venezuelan equine encephalomyelitis, Ross River, LaCrosse, or Caraparu viruses. The DENV assay can provide real-time critical information on the presence of DENV in mosquitoes to public health personnel. Results from this assay will allow a rapid threat assessment and the focusing of vector control measures in high-risk areas.

  9. Detection of arecoline by simple high-performance thin-layer chromatographic method in Indian nontobacco pan masala

    Directory of Open Access Journals (Sweden)

    Anjan Adhikari

    2015-01-01

    Full Text Available Chewing the habit of blended pan masala containing areca nut with or without tobacco is a common practice in the Indian subcontinent. Arecoline, a pyridine alkaloid presence in areca nut alarmed for oral carcinogenesis and strictly prohibited in the western world. However, in India using blended pan masala is very popular among young and old individuals. In this context, we aimed to detect arecoline in Indian blended nontobacco pan masala sold in Kolkata using a simple densitometric high-performance thin-layer chromatographic (HPTLC method and for alarming their use in common people. Eleven popularly Indian blended nontobacco pan masala were collected from the territory of Kolkata and isolated arecoline, following solvent extraction method derived for pyridine alkaloid. The quantitative analysis of arecoline was measured using automated software-based HPTLC instruments and validated the method according to International Conference on Harmonization guidelines. Arecoline was detected in all 11 blended nontobacco pan masala samples in a range of minimum 130 to maximum 415 μg/g dry samples. Arecoline is hazardous carcinogenic compound, so the use of Indian blended nontobacco pan masala should be restricted. Further, the method was found suitable for routine quantitative analysis of arecoline in areca nut containing substances.

  10. Detection of gas atoms with carbon nanotubes

    Science.gov (United States)

    Arash, B.; Wang, Q.

    2013-05-01

    Owning to their unparalleled sensitivity resolution, nanomechanical resonators have excellent capabilities in design of nano-sensors for gas detection. The current challenge is to develop new designs of the resonators for differentiating distinct gas atoms with a recognizably high sensitivity. In this work, the characteristics of impulse wave propagation in carbon nanotube-based sensors are investigated using molecular dynamics simulations to provide a new method for detection of noble gases. A sensitivity index based on wave velocity shifts in a single-walled carbon nanotube, induced by surrounding gas atoms, is defined to explore the efficiency of the nano-sensor. The simulation results indicate that the nano-sensor is able to differentiate distinct noble gases at the same environmental temperature and pressure. The inertia and the strengthening effects by the gases on wave characteristics of carbon nanotubes are particularly discussed, and a continuum mechanics shell model is developed to interpret the effects.

  11. Detection of gas atoms with carbon nanotubes

    Science.gov (United States)

    Arash, B.; Wang, Q.

    2013-01-01

    Owning to their unparalleled sensitivity resolution, nanomechanical resonators have excellent capabilities in design of nano-sensors for gas detection. The current challenge is to develop new designs of the resonators for differentiating distinct gas atoms with a recognizably high sensitivity. In this work, the characteristics of impulse wave propagation in carbon nanotube-based sensors are investigated using molecular dynamics simulations to provide a new method for detection of noble gases. A sensitivity index based on wave velocity shifts in a single-walled carbon nanotube, induced by surrounding gas atoms, is defined to explore the efficiency of the nano-sensor. The simulation results indicate that the nano-sensor is able to differentiate distinct noble gases at the same environmental temperature and pressure. The inertia and the strengthening effects by the gases on wave characteristics of carbon nanotubes are particularly discussed, and a continuum mechanics shell model is developed to interpret the effects.

  12. Active mems microbeam device for gas detection

    KAUST Repository

    Bouchaala, Adam M.

    2017-10-05

    Sensors and active switches for applications in gas detection and other fields are described. The devices are based on the softening and hardening nonlinear response behaviors of microelectromechanical systems (MEMS) clamped-clamped microbeams. In that context, embodiments of gas-triggered MEMS microbeam sensors and switches are described. The microbeam devices can be coated with a Metal-Organic Framework to achieve high sensitivity. For gas sensing, an amplitude-based tracking algorithm can be used to quantify an amount of gas captured by the devices according to frequency shift. Noise analysis is also conducted according to the embodiments, which shows that the microbeam devices have high stability against thermal noise. The microbeam devices are also suitable for the generation of binary sensing information for alarming, for example.

  13. Automated Hydrogen Gas Leak Detection System

    Science.gov (United States)

    1995-01-01

    The Gencorp Aerojet Automated Hydrogen Gas Leak Detection System was developed through the cooperation of industry, academia, and the Government. Although the original purpose of the system was to detect leaks in the main engine of the space shuttle while on the launch pad, it also has significant commercial potential in applications for which there are no existing commercial systems. With high sensitivity, the system can detect hydrogen leaks at low concentrations in inert environments. The sensors are integrated with hardware and software to form a complete system. Several of these systems have already been purchased for use on the Ford Motor Company assembly line for natural gas vehicles. This system to detect trace hydrogen gas leaks from pressurized systems consists of a microprocessor-based control unit that operates a network of sensors. The sensors can be deployed around pipes, connectors, flanges, and tanks of pressurized systems where leaks may occur. The control unit monitors the sensors and provides the operator with a visual representation of the magnitude and locations of the leak as a function of time. The system can be customized to fit the user's needs; for example, it can monitor and display the condition of the flanges and fittings associated with the tank of a natural gas vehicle.

  14. Enhancement of concentration range of chromatographically detectable components with array detector mass spectrometry

    Science.gov (United States)

    Enke, Christie

    2013-02-19

    Methods and instruments for high dynamic range analysis of sample components are described. A sample is subjected to time-dependent separation, ionized, and the ions dispersed with a constant integration time across an array of detectors according to the ions m/z values. Each of the detectors in the array has a dynamically adjustable gain or a logarithmic response function, producing an instrument capable of detecting a ratio of responses or 4 or more orders of magnitude.

  15. Liquid chromatographic separation and indirect detection of non-absorbing aliphatic compounds using m-nitrophenol as a detection agent

    International Nuclear Information System (INIS)

    Lee, Seung Seok; Kang, Sam Woo; Moon, Young Ja

    1991-01-01

    m-Nitrophenol(m-NP) was a detection agent for the use of the detection and separation of non-absorbing compounds such as aliphatic acids, alcohols, amines and tetraalkylammonium salts by indirect photometric detection in reversed-phase liquid chromatography. Response of samples was investigated to the several factors such as pH, temperature, and concentration of MeOH as well as concentration of detection reagent in mobile phase. The separation of several mixtures were attempted under optimum condition. (Author)

  16. Determination of fluoxetine and norfluoxetine in plasma by gas chromatography with electron-capture detection

    Energy Technology Data Exchange (ETDEWEB)

    Nash, J.F.; Bopp, R.J.; Carmichael, R.H.; Farid, K.Z.; Lemberger, L.

    1982-10-01

    This gas-chromatographic method for assay of fluoxetine and norfluoxetine in human plasma involves extraction of the drugs and use of a /sup 63/Ni electron-capture detector. The linear range of detection is 25 to 800 micrograms/L for each drug. Overall precision (CV) in the concentration range of 10 to 100 micrograms/L for both drugs was approximately 10%. Accuracy (relative error) in the same concentration range was approximately +10%. None of the commonly prescribed antidepressants or tranquilizers that we tested interfere with the assay.

  17. Hyphenation of a near-infrared Echelle spectrometer to a microplasma for element-selective detection in gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Cziesla, K.; Otto, M. [Inst. of Analytical Chemistry, Freiberg University of Mining and Technology (Germany); Platzer, B. [Graz Univ. of Technology, Dept. of Analytical Chemistry (Austria); Okruss, M. [Gesellschaft zur Foerderung angewandter Optik, Optoelektronik, Quantenelektronik und Spektroskopie (GOS) e.V., Berlin (Germany); Florek, S. [Inst. of Spectrochemistry and Applied Spectroscopy, Institutsteil Berlin (Germany)

    2001-12-01

    The coupling of a near-infrared Echelle spectrometer (NIRES) with a gas chromatograph for element-selective detection is introduced. The miniaturized capacitive plasma device is operated at a frequency of 40.68 MHz and is mounted directly on an Hewlett-Packard HP6890 GC. First results with a mixture of halogenated standard compounds are presented and discussed in terms of the advantages and problems with this system. (orig.)

  18. Quantification of five plasticizers used in PVC tubing through high performance liquid chromatographic-UV detection.

    Science.gov (United States)

    Radaniel, Tsanta; Genay, Stéphanie; Simon, Nicolas; Feutry, Frédéric; Quagliozzi, Francesca; Barthélémy, Christine; Lecoeur, Marie; Sautou, Valérie; Décaudin, Bertrand; Odou, Pascal

    2014-08-15

    Searching for alternatives to di-(2-ethylhexyl)-phthalate, a plasticizer that has been widely used in the manufacturing of PVC medical devices, has become a major challenge since a European regulation underlined some clinical risks. The aim of this study is to develop an HPLC-UV method to quantify the currently used alternative plasticizers to DEHP. Five plasticizers, acetyl tributyl citrate, di-(2-ethylhexyl)-phthalate, di-(ethylhexyl)-terephthalate, di-isononyl-1,2-cyclohexane-dicarboxylate, and trioctyl trimellitate, were separated on a C8 stationary phase (2.6 μm, 100 mm × 4.6mm) under gradient elution in 13 min. They were detected at 221 nm leading to a quantification threshold from 0.3 to 750 μg/mL as a function of the plasticizer. Within-day and between-day precisions were inferior to 0.9% and 18%, respectively. The assays were validated according to the accuracy profile method. Plasticizers were extracted from PVC-tubing by dissolving PVC in THF then precipitating it in methanol with a yield of over 90% for each plasticizer. This assay could feasibly be used to quantify plasticizers in PVC medical devices. Copyright © 2014 Elsevier B.V. All rights reserved.

  19. High gas temperature furnace for species determination of organometallic compounds with a high pressure liquid chromatograph and a Zeeman atomic absorption spectrometer

    Energy Technology Data Exchange (ETDEWEB)

    Koizumi, H.; McLaughlin, R.D.; Hadeishi, T.

    1979-03-01

    A new furnace has been constructed that allows atomic absorption detection of volatile organometallic compounds. The operation of this furnace is demonstrated by analyzing the eluent of a high pressure liquid chromatograph utilizing Zeeman atomic absorption spectrometry. The content of tetraethyllead in National Bureau of Standards gasoline standards was determined. Data are presented on the ability of this furnace to suppress interference with cadmium and lead determinations by MgCl/sub 2/, CuCl/sub 2/, and CaCl/sub 2/. It was found that two orders of magnitude more interferent can be tolerated. The determination of lead in automotive exhaust is also described. 7 figures, 4 tables.

  20. 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.

  1. Novel gas-based detection techniques

    International Nuclear Information System (INIS)

    Graaf, Harry van der

    2009-01-01

    This year we celebrate the 100th birthday of gaseous detectors: Hans Geiger operated the first gas-filled counter in Manchester in 1908. The thin wires, essential for obtaining gas amplification, have been replaced by Micro Pattern Gas Detectors (MPGDs): Micromegas (1995) and GEM (1996). In the GridPix detector, each of the grid holes of a MPGD is equipped with its own electronic readout channel in the form of an active pixel in suitable pixel CMOS chips. By means of MEMS technology, the grid has been integrated with the chip, forming a monolithic readout device for gas volumes. By applying a protection layer made of hydrogenated amorphous silicon, the chips can be made spark proof. New protection layers have been made of silicon nitride. The use of gas as detection material for trackers is compared to Si, and the issue of chamber aging is addressed. New developments are set out: the development of Micro Channel Plates, integrated on pixel chips, the development of electron emission foil, and the realization of TimePix-2: a general-purpose pixel chip with time and amplitude measurement, per pixel, of charge signals.

  2. Gas analysis of irradiated frozen meat and poultry for irradiation detection

    International Nuclear Information System (INIS)

    Furuta, Masakazu; Dohmaru, Takaaki; Katayama, Tadashi; Toratani, Hirokazu

    1991-01-01

    A novel method to detect irradiated frozen meat and poultry has been developed based on the fact that CO are formed in foodstuffs irradiated with an ionizing radiation. Gamma-irradiated frozen beef, pork or chicken was put in a glass screw vial with a rubber spetum, together with a given amount of water, and then quickly thawed out by microwave heating. Gas-chromatographic analyses of the headspace gases showed that much of the radiolytically formed CO remained long in the irradiated samples (Fig. 1), suggesting that, by measuring the level of CO, irradiation detection would by possible for more than 1 year even at a dose below 3 kGy. This method has advantages of general applicability including boneless products and accessibility to gas chromatography. (author)

  3. Air Monitoring for Hazardous Gas Detection

    Science.gov (United States)

    Arkin, C. Richard; Naylor, Guy; Haskell, William; Floyd, David; Curley, Charles; Griffin, Timothy P.; Adams, Frederick; Follistein, Duke

    2003-01-01

    The Hazardous Gas Detection Lab is involved in the design and development of instrumentation that can detect and quantify various hazardous gases. Traditionally these systems are designed for leak detection of the cryogenic gases used for the propulsion of the Shuttle and other vehicles. Mass spectrometers are the basis of these systems, which provide excellent quantitation, sensitivity, selectivity, response and limits of detection. Unfortunately, these systems are large, heavy and expensive. This feature limits the ability to perform gas analysis in certain applications. Smaller and lighter mass spectrometer systems could be used in many more applications primarily due to the portability of the system. Such applications would include air analysis in confined spaces, in-situ environmental analysis and emergency response. In general, system cost is lowered as size is reduced. With a low cost air analysis system, several systems could be utilized for monitoring large areas. These networked systems could be deployed at job-sites for worker safety, throughout a community for pollution warnings, or dispersed in a battlefield for early warning of chemical or biological threats. Presented will be information on the first prototype of this type of system. Included will be field trial data, with this prototype performing air analysis autonomously from an aircraft.

  4. 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.

  5. 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.

  6. 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.

  7. 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.

  8. Distributed gas detection system and method

    Science.gov (United States)

    Challener, William Albert; Palit, Sabarni; Karp, Jason Harris; Kasten, Ansas Matthias; Choudhury, Niloy

    2017-11-21

    A distributed gas detection system includes one or more hollow core fibers disposed in different locations, one or more solid core fibers optically coupled with the one or more hollow core fibers and configured to receive light of one or more wavelengths from a light source, and an interrogator device configured to receive at least some of the light propagating through the one or more solid core fibers and the one or more hollow core fibers. The interrogator device is configured to identify a location of a presence of a gas-of-interest by examining absorption of at least one of the wavelengths of the light at least one of the hollow core fibers.

  9. Characteristic chromatographic fingerprint study of short-chain fatty acids in human milk, infant formula, pure milk and fermented milk by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Jiang, Zhenzuo; Liu, Yanan; Zhu, Yan; Yang, Jing; Sun, Lili; Chai, Xin; Wang, Yuefei

    2016-09-01

    Human milk, infant formula, pure milk and fermented milk as food products or dietary supplements provide a range of nutrients required to both infants and adults. Recently, a growing body of evidence has revealed the beneficial roles of short-chain fatty acids (SCFAs), a subset of fatty acids produced from the fermentation of dietary fibers by gut microbiota. The objective of this study was to establish a chromatographic fingerprint technique to investigate SCFAs in human milk and dairy products by gas chromatography coupled with mass spectrometry. The multivariate method for principal component analysis assessed differences between milk types. Human milk, infant formula, pure milk and fermented milk were grouped independently, mainly because of differences in formic acid, acetic acid, propionic acid and hexanoic acid levels. This method will be important for the assessment of SCFAs in human milk and various dairy products.

  10. Gas chromatographic determination of pesticides in vegetable samples by sequential positive and negative chemical ionization and tandem mass spectrometric fragmentation using an ion trap analyser.

    Science.gov (United States)

    Hernando, M D; Agüera, A; Fernández-Alba, A R; Piedra, L; Contreras, M

    2001-01-01

    A selective and sensitive chromatographic method is described for the determination of nine organochlorine and organophosphorus pesticides in vegetable samples by gas chromatography-mass spectrometry. The proposed method combines the use of positive and negative chemical ionisation and tandem mass spectrometric fragmentation, resulting in a significant increase in selectivity and allowing the simultaneous confirmation and quantification of trace levels of pesticides in complex vegetable matrices. Parameters relative to ionisation and fragmentation processes were optimised to obtain maximum sensitivity. Repeatability and reproducibility studies yielded relative standard deviations lower than 25% in all cases. Identification criteria, such as retention time and relative abundance of characteristic product ions, were also evaluated in order to guarantee the correct identification of the target compounds. The method was applied to real vegetable samples to demonstrate its use in routine analysis.

  11. 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

  12. A Method for the Analysis of Tabun in Multisol Using Gas Chromatographic Flame Photometric Detection

    Science.gov (United States)

    2006-05-01

    methanephosphonate (DIMP) was obtained from Lancaster Synthesis , Pelham, NH. NMR measurements were made on GA in modified Multisol (48.5% D2O, 40...ethoxy-phosphoryl cyanide (Tabun), Acta Chim.Scand. 1953; 7: 306-314. 12. Holmstedt B. Synthesis and pharmacology of dimethylamido-ethoxy-phosphoryl...Anticonvulsant treatment of nerve agent seizures: anticholinergics vs diazepam in soman- intoxicated guinea pigs. Epilepsy Research 2000; 38: 1-14. 19

  13. Gas chromatographical detection of oxygenated compounds in gasoline with a switching capillary column system

    Energy Technology Data Exchange (ETDEWEB)

    Winskowski, J.

    1988-01-01

    In this paper the separation and identification of oxygenated compounds in gasoline is described. Using a two-dimensional column system swtiching from a high polar TCEP-capillary column (1,2,3-Tris(cyanoethoxy)propan) to a non-polar column with a greater filmthickness of DMS (dimethylpolysiloxane) acetone and alcohols as well as further ketones and esters were separated from the hydrocarbon matrix without any difficulties. The analysis of the ethers is more difficult, especially in presence of olefinic compounds, mainly occuring in crack and pyrolysis gasoline, and can only be carried out if highly efficient capillary columns are applied. A test mixture is proposed which can be used to find out whether column systems are suitable for this purpose. The total amount of oxygen can be calculated from the single components after identification. (orig.)

  14. A Method for the Analysis of Tabun in Multisol Using Gas Chromatographic Flame Photometric Detection

    National Research Council Canada - National Science Library

    Logan, Thomas P; Allen, Edward D; Way, Mark R; Swift, Austin T; Soni, Sunil-Datta; Koplovitz, Irwin

    2006-01-01

    ...; however, GA is very unstable in saline solutions. In the past we have found GA in saline at 2 micrograms/mL to be stable for a month or less at -70 degrees C, whereas saline solutions of sarin (GB), soman (GD), and cyclosarin (GF...

  15. On-site monitoring of biogenic emissions from Eucalyptus dunnii leaves using membrane extraction with sorbent interface combined with a portable gas chromatograph system.

    Science.gov (United States)

    Liu, Xinyu; Pawliszyn, Richard; Wang, Limei; Pawliszyn, Janusz

    2004-01-01

    Membrane extraction with sorbent interface, combined with a portable gas chromatograph system (MESI-Portable GC) for continuous on-line monitoring of biogenic volatile organic compounds (BVOCs) emissions (from leaves of Eucalytus dunnii in a greenhouse), is presented herein. A sampling chamber was designed to facilitate the extraction and identification of the BVOCs emitted by the Eucalytus dunnii leaves. Preliminary experiments, including; enrichment times, microtrap temperatures, stripping gas flow rates, and desorption temperatures were investigated to optimize experimental parameters. The main components of BVOCs released by the Eucalytus dunnii leaves were identified by comparing the retention times of peaks with those of authentic standard solutions. They were then confirmed with solid phase microextraction coupled with gas chromatography and mass spectrometry (SPME-GC-MS). BVOC emission profiles of [small alpha]-pinene, eucalyptol, and [gamma]-terpinene emitted by intact and damaged Eucalytus dunnii leaves were obtained. The findings suggest that the MESI-Portable GC system is a simple and useful tool for field monitoring changes in plant emissions as a function of time.

  16. Chemometrics-assisted high performance liquid chromatography-diode array detection strategy to solve varying interfering patterns from different chromatographic columns and sample matrices for beverage analysis.

    Science.gov (United States)

    Yin, Xiao-Li; Wu, Hai-Long; Gu, Hui-Wen; Hu, Yong; Wang, Li; Xia, Hui; Xiang, Shou-Xia; Yu, Ru-Qin

    2016-02-26

    This work reports a chemometrics-assisted high performance liquid chromatography-diode array detection (HPLC-DAD) strategy to solve varying interfering patterns from different chromatographic columns and sample matrices for the rapid simultaneous determination of six synthetic colorants in five kinds of beverages with little sample pretreatment. The investigation was performed using two types of LC columns under the same elution conditions. Although analytes using different columns have different co-elution patterns that appear more seriously in complex backgrounds, all colorants were properly resolved by alternating trilinear decomposition (ATLD) method and accurate chromatographic elution profiles, spectral profiles as well as relative concentrations were obtained. The results were confirmed by those obtained from traditional HPLC-UV method at a particular wavelength and the results of both methods were consistent with each other. All results demonstrated that the proposed chemometrics-assisted HPLC-DAD method is accurate, economical and universal, and can be promisingly applied to solve varying interfering patterns from different chromatographic columns and sample matrices for the analysis of complex food samples. Copyright © 2016 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

    Pacáková, V; Leclercq, P A

    1991-08-30

    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 products.

  18. Analysis of cave atmospheres by comprehensive two-dimensional gas chromatography (GC×GC with flame ionization detection (FID

    Directory of Open Access Journals (Sweden)

    Ryan C. Blase

    2015-03-01

    Full Text Available In this paper, we describe a simple method for sampling, pre-concentrating, and separating volatile and semi-volatile components from two different cave atmospheres. Sampling is performed by capturing a volume of cave atmosphere in a Tedlar bag or Suma canister for sample storage and transport back to the laboratory. Loading a portion of the sample on a multi-bed sorption trap allows for sample pre-concentration prior to separation and detection of components on a comprehensive two-dimensional gas chromatograph (GC×GC. Comparison of two Texas caves reveals the power of comprehensive two-dimensional gas chromatography (GC×GC for volatile separation and detection, and to our knowledge marks the first use of GC×GC for the analysis of cave atmospheres. Analysis of the results revealed 138 and 146 chromatographic signals over an S/N threshold of 500 and direct comparison of the two samples revealed 50 identical chromatographic signals. This study is a first step toward demonstrating the ability of GC×GC to separate the complex volatiles and semi-volatiles in the cave atmosphere as a fingerprinting tool.

  19. Time reversal technique for gas leakage detection.

    Science.gov (United States)

    Maksimov, A O; Polovinka, Yu A

    2015-04-01

    The acoustic remote sensing of subsea gas leakage traditionally uses sonars as active acoustic sensors and hydrophones picking up the sound generated by a leak as passive sensors. When gas leaks occur underwater, bubbles are produced and emit sound at frequencies intimately related to their sizes. The experimental implementation of an acoustic time-reversal mirror (TRM) is now well established in underwater acoustics. In the basic TRM experiment, a probe source emits a pulse that is received on an array of sensors, time reversed, and re-emitted. After time reversal, the resulting field focuses back at the probe position. In this study, a method for enhancing operation of the passive receiving system has been proposed by using it in the regime of TRM. Two factors, the local character of the acoustic emission signal caused by the leakage and a resonant nature of the bubble radiation at their birth, make particularly effective scattering with the conjugate wave (CW). Analytical calculations are performed for the scattering of CW wave on a single bubble when CW is formed by bubble birthing wail received on an array, time reversed, and re-emitted. The quality of leakage detection depends on the spatio-temporal distribution of ambient noise.

  20. High performance liquid chromatographic separations of gas oil samples and their hydrotreated products using commercial normal phases.

    Science.gov (United States)

    Oro, Nicole E; Lucy, Charles A

    2011-10-28

    Three commercially available high performance liquid chromatography columns are used in normal phase or quasi-normal phase mode for the separation of gas oil samples. The columns are tested with 20 analytical standards to determine their suitability for separations of petroleum samples and their ability to separate the nitrogen group-types (pyrrole and pyridine) found in petroleum. The columns studied are polymeric hypercrosslinked polystyrene (HGN), a biphenyl phase, and a Chromegabond "DNAP" column from ES Industries. The HGN column separates gas oils based on both ring structure and heteroatom, while the biphenyl phase has low retention of most compounds studied in quasi-normal phase mode. The "DNAP" column is selective for nitrogen-containing compounds, separating them from PAHs as well as oxygen and sulphur compounds. Retention data of standards on all three columns is shown, along with chromatograms of gas oil samples on the HGN and "DNAP" columns. Copyright © 2011 Elsevier B.V. All rights reserved.

  1. 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

  2. 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

  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. Fully automated system for the gas chromatographic characterization of polar biopolymers based on thermally assisted hydrolysis and methylation

    NARCIS (Netherlands)

    Kaal, E.; de Koning, S.; Brudin, S.; Janssen, H.-G.

    2008-01-01

    Pyrolysis-gas chromatography (Py-GC) is a powerful tool for the detailed compositional analysis of polymers. A major problem of Py-GC is that polar (bio)polymers yield polar pyrolyzates which are not easily accessible to further GC characterization. In the present work, a newly developed fully

  5. 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.

  6. 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)

  7. 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.

  8. Contamination of the operating room by anesthetic gases and vapors. II. Gas chromatographic analysis of nitrous oxide

    Energy Technology Data Exchange (ETDEWEB)

    Cattaneo, A.D.; Ferraiolo, G.; Rovatti, M.; Zattoni, J.; Donato, A.

    1981-12-01

    The contamination by nitrous oxide of an operating room atmosphere was studied in a number of experiments, in the absence of personnel and using a gaschromatographic method. The evacuating device of the anesthesia machine proved to be ineffective to overcome the hazard of leaks in the breathing system, whereas the air conditioning flow rates (12 outside air changes per hour) minimized waste anesthetic gas concentrations.

  9. 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.

  10. Flammable Gas Detection for the D-Zero Gas System

    Energy Technology Data Exchange (ETDEWEB)

    Spires, L.D.; Foglesong, J.; /Fermilab

    1991-02-11

    The use of flammable gas and high voltage in detector systems is common in many experiments at Fermilab. To mitigate the hazards associated with these systems, Fermilab Engineering Standard SD-45B (Ref. 1) was adopted. Since this note is meant to be a guide and not a mandatory standard, each experiment is reviewed for compliance with SD-45B by the flammable gas safety subcommittee. Currently, there are only two types of flammable gas in use, ethane (Appendix A) and methane (Appendix B). The worst flammable-gas case is C2H6 (ethane), which has an estimated flow rate that is 73% of the CH4 (methane) flow but a heat of combustion (in kcal/g-mole) that is 173% of that of methane. In the worst case, if ethane were to spew through its restricting orifice into its gas line at 0 psig and then through a catastrophic leak into Room 215 (TRD) or Room 511 (CDC/FDCNTX), the time that would be required to build up a greater than Class 1 inventory (0.4kg H2 equivalent) would be 5.2 hours (Ref. 2). Therefore a worst-case flammable gas leak would have to go undetected for over 5 hours in order to transform a either mixing room to an environment with a Risk Class greater than Class 1. The mixing systems, gas lines, and detectors themselves will be thoroughly leak checked prior to active service. All vessels that are part of the mixing systems will be protected from overpressure by safety valves vented outside the building. Both the input and output of all detector volumes are protected from overpressure in the same way. The volume immediately outside the central tracking detectors is continuously purged by nitrogen from boiloff from the main nitrogen dewar at the site. However, if flammable gas were to build up in the mixing rooms or particular detector areas, no matter how unlikely, flammable gas detectors that are part of the interlock chain of each gas mixing system will shut down the appropriate system. This includes shutting off the output of flammable gas manifolds within the

  11. Detection device for off-gas system accidents

    International Nuclear Information System (INIS)

    Kubota, Ryuji; Tsuruoka, Ryozo; Yamanari, Shozo.

    1984-01-01

    Purpose: To rapidly isolate the off-gas system by detecting the off-gas system failure accident in a short time. Constitution: Radiation monitors are disposed to ducts connecting an exhaust gas area and an air conditioning system as a portion of a turbine building. The ducts are disposed independently such that they ventilate only the atmosphere in the exhaust gas area and do not mix the atmosphere in the turbine building. Since radioactivity issued upon off-gas accidents to the exhaust gas area is sucked to the duct, it can be detected by radiation detection monitors in a short time after the accident. Further, since the operator judges it as the off-gas system accident, the off-gas system can be isolated in a short time after the accident. (Moriyama, K.)

  12. Gas chromatographic-mass spectrometric determination of aromatic hydrocarbon metabolites from livers of fish exposed to fuel oil.

    Science.gov (United States)

    Krahn, M M; Malins, D C

    1982-10-15

    Metabolites of several two- and three-ring aromatic hydrocarbons (AHs) have been found in livers of English sole exposed to No. 2 fuel oil. Four metabolites of the C2H5-naphthalenes, six of the C3H7-naphthalenes and one each of fluorene, phenanthrene and anthracene have been partially characterized and their concentrations, which ranged from 50 to 1100 ng/g, were determined. Metabolites were separated from the liver matrix using an automated extractor/concentrator. The resulting extract was then purified by high-performance liquid chromatography, and the metabolites were characterized and quantitated by gas chromatography-mass spectrometry.

  13. Detection and identification of radiation induced hydrocarbons in meets with the use of gas chromatography as one of methods for the detection of irradiated food

    International Nuclear Information System (INIS)

    Lehner, K.; Stachowicz, W.

    2000-01-01

    Results of the determination of the content of radiation induced hydrocarbons in meat samples (chicken, pork, beef) as well as proportion between the concentration of individual hydrocarbons in relation to the content of fatty acids in a given product are presented. The measurements have been done with the use of a Perkin Elmer model 8700 gas chromatograph equipped with a FID detector. The present study is a preliminary work on the implementation of a routine method for the detection of irradiation in foods that contain fats. (author)

  14. 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.

  15. Gas chromatographic determination of electron capture sensitive volatile industrial chemical residues in foods, using AOAC pesticide multiresidue extraction and cleanup procedures.

    Science.gov (United States)

    Yurawecz, M P; Puma, B J

    1986-01-01

    Electron capture (EC) gas chromatographic (GC) parameters have been developed for determining some of the more volatile industrial chemicals that can be determined by the AOAC multiresidue method for organochlorine and organophosphorus pesticides with modified GC operating conditions. Retention times relative to pentachlorobenzene are reported for 143 industrial chemicals, pesticides, and related compounds on OV-101 GC columns at 130 degrees C. Also reported for most of the compounds are recoveries from fortified samples carried through the AOAC extraction and cleanup procedures for fatty and/or nonfatty foods, Florisil elution characteristics, and GC relative retention times on mixed OV-101 + OV-210 columns at 130 degrees C. Our laboratory has used the modified EC/GC parameters with the AOAC multiresidue extraction/cleanup procedures to determine many volatile halogenated industrial chemical contaminants in foods, chiefly in samples of fresh-water fish. Other modifications of the AOAC method are described to improve the tentative identification and quantitative measurement of these volatile residues.

  16. Radiolytic degradation of TBP-HNO3 system: gas chromatographic determination of radiation chemical yields of n-butanol and nitrobutane

    International Nuclear Information System (INIS)

    Krishnamurthy, M.V.; Sipahimalani, A.T.

    1995-01-01

    Radiolytic degradation of the TBP-HNO 3 system has been studied for the radiation dose range of 19.8 to 262 kGy by the gas chromatographic method. n-Butanol and nitrobutane formed due to irradiation have been identified and estimated in pure TBP, TBP-3M HNO 3 extract and TBP-5M HNO 3 extract. The G-values (radiation chemical yields) of n-butanol are determined to be 0.28, 0.77 and 0.47 for a pure TBP, TBP-3M HNO 3 extract and TBP-5M HNO 3 extract, respectively. The G-values of nitrobutane (1-nitrobutane) are 0.55 and 1.09 for TBP-3M HNO 3 extract and TBP-5M HNO 3 extract. It is found that G(n-butanol) is less for TBP-5M HNO 3 extract than for TBP-3M HNO 3 extract, while G(nitrobutane) is grater for TBP-5M HNO 3 extract than for TBP-3M HNO 3 extract. This is explained on the basis of the formation of TBP.HNO 3 species and the role played by nitric acid in the TBP phase. (author) 12 refs.; 2 figs

  17. Multiplex real-time quantitative PCR, microscopy and rapid diagnostic immuno-chromatographic tests for the detection of Plasmodium spp: performance, limit of detection analysis and quality assurance.

    Science.gov (United States)

    Khairnar, Krishna; Martin, Donald; Lau, Rachel; Ralevski, Filip; Pillai, Dylan R

    2009-12-09

    Accurate laboratory diagnosis of malaria species in returning travelers is paramount in the treatment of this potentially fatal infectious disease. A total of 466 blood specimens from returning travelers to Africa, Asia, and South/Central America with suspected malaria infection were collected between 2007 and 2009 at the reference public health laboratory. These specimens were assessed by reference microscopy, multipex real-time quantitative polymerase chain reaction (QPCR), and two rapid diagnostic immuno-chromatographic tests (ICT) in a blinded manner. Key clinical laboratory parameters such as limit of detection (LOD) analysis on clinical specimens by parasite stage, inter-reader variability of ICTs, staffing implications, quality assurance and cost analysis were evaluated. QPCR is the most analytically sensitive method (sensitivity 99.41%), followed by CARESTART (sensitivity 88.24%), and BINAXNOW (sensitivity 86.47%) for the diagnosis of malaria in returning travelers when compared to reference microscopy. However, microscopy was unable to specifically identify Plasmodia spp. in 18 out of 170 positive samples by QPCR. Moreover, the 17 samples that were negative by microscopy and positive by QPCR were also positive by ICTs. Quality assurance was achieved for QPCR by exchanging a blinded proficiency panel with another reference laboratory. The Kappa value of inter-reader variability among three readers for BINAXNOW and CARESTART was calculated to be 0.872 and 0.898 respectively. Serial dilution studies demonstrated that the QPCR cycle threshold correlates linearly with parasitemia (R(2) = 0.9746) in a clinically relevant dynamic range and retains a LOD of 11 rDNA copies/microl for P. falciparum, which was several log lower than reference microscopy and ICTs. LOD for QPCR is affected not only by parasitemia but the parasite stage distribution of each clinical specimen. QPCR was approximately 6-fold more costly than reference microscopy. These data suggest that

  18. Multiplex real-time quantitative PCR, microscopy and rapid diagnostic immuno-chromatographic tests for the detection of Plasmodium spp: performance, limit of detection analysis and quality assurance

    Directory of Open Access Journals (Sweden)

    Ralevski Filip

    2009-12-01

    Full Text Available Abstract Background Accurate laboratory diagnosis of malaria species in returning travelers is paramount in the treatment of this potentially fatal infectious disease. Materials and methods A total of 466 blood specimens from returning travelers to Africa, Asia, and South/Central America with suspected malaria infection were collected between 2007 and 2009 at the reference public health laboratory. These specimens were assessed by reference microscopy, multipex real-time quantitative polymerase chain reaction (QPCR, and two rapid diagnostic immuno-chromatographic tests (ICT in a blinded manner. Key clinical laboratory parameters such as limit of detection (LOD analysis on clinical specimens by parasite stage, inter-reader variability of ICTs, staffing implications, quality assurance and cost analysis were evaluated. Results QPCR is the most analytically sensitive method (sensitivity 99.41%, followed by CARESTART (sensitivity 88.24%, and BINAXNOW (sensitivity 86.47% for the diagnosis of malaria in returning travelers when compared to reference microscopy. However, microscopy was unable to specifically identify Plasmodia spp. in 18 out of 170 positive samples by QPCR. Moreover, the 17 samples that were negative by microscopy and positive by QPCR were also positive by ICTs. Quality assurance was achieved for QPCR by exchanging a blinded proficiency panel with another reference laboratory. The Kappa value of inter-reader variability among three readers for BINAXNOW and CARESTART was calculated to be 0.872 and 0.898 respectively. Serial dilution studies demonstrated that the QPCR cycle threshold correlates linearly with parasitemia (R2 = 0.9746 in a clinically relevant dynamic range and retains a LOD of 11 rDNA copies/μl for P. falciparum, which was several log lower than reference microscopy and ICTs. LOD for QPCR is affected not only by parasitemia but the parasite stage distribution of each clinical specimen. QPCR was approximately 6-fold more

  19. 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.

  20. Rapid and sensitive assay for fluconazole which uses gas chromatography with electron capture detection.

    Science.gov (United States)

    Rege, A B; Walker-Cador, J Y; Clark, R A; Lertora, J J; Hyslop, N E; George, W J

    1992-03-01

    Fluconazole, an orally active antifungal agent, has been shown to be clinically beneficial for maintenance therapy of cryptococcal meningitis. A sensitive gas-liquid chromatographic assay with electron capture detection, which required only a single extraction step and precluded any pretreatment of the chromatographic column, was developed for fluconazole. The assay was linear from 0.1 to 20 micrograms/ml, with a correlation coefficient of 0.999. The intraassay and interassay coefficients of variation were less than 9%. The measured values on average were within 8% of the target values. The extraction recoveries ranged from 87 to 106%. Steady-state plasma fluconazole levels (mean +/- standard deviation) in three AIDS patients with cryptococcal meningitis receiving 200 mg of fluconazole per day ranged from 8.95 +/- 1.32 to 11.41 +/- 0.63 micrograms/ml and were within the expected range for this dosing rate, on the basis of previous studies. The ratio of fluconazole concentration in cerebrospinal fluid to fluconazole concentration in plasma in one patient receiving 400 mg/day was 0.73 at steady state and was consistent with published reports.

  1. Comparison of a jet separator and an open splitter as an interface between a multi-capillary gas chromatographic column and a time-of-flight mass spectrometer

    Science.gov (United States)

    Pongpun; Mlynski; Crisp; Guilhaus

    2000-09-01

    A gas chromatographic/time-of-flight mass spectrometric (GC/TOFMS) interface is being developed for fast on-line analysis utilizing multi-capillary column technology. A variable gap-distance jet separator has been constructed and its performance compared with that of a commercially supplied post-column open splitter recommended for use between the multi-capillary column and a mass spectrometer. Both interfaces were found to be compatible with the GC/TOFMS system at high carrier gas flow-rates, facilitating high-speed and high-resolution separations. The systems were investigated and tested with a mixture of volatile organic compounds (VOCs) with molecular masses from 85 to 166: dichloromethane, toluene, m-dichlorobenzene, o-dichlorobenzene and tetrachloroethylene. The optimum tip-to-tip gap distance corresponding to the highest efficiency of the jet separator was found to be 0.030 mm for each compound at carrier gas flow-rates of 20, 40 and 60 ml min(-1) giving, in the ion source housing, ion gauge pressure readings of 1.6 x 10(-6), 5.0 x 10(-6) and 5.8 x 10(-6) mbar, respectively. The efficiency of the jet separator (10-30% yields) was significantly higher than that of the open splitter (6-9% yields). The observation that the open splitter did not provide a constant flow-rate to the ion source was not in agreement with the manufacturer's specifications. A method for measuring the gas flow-rates in all parts of the equipment is described. The correlation between yield in the jet separator and molecular mass for the heterogeneous set of compounds studied was found to be less linear than usually reported for homologous series of compounds in jet separator studies. The result suggests that the pressure conditions in the jet may be sufficient for the separation process to be partly controlled by diffusion rather than predominately by effusion. Copyright 2000 John Wiley & Sons, Ltd.

  2. Antioxidant Activity and Gas Chromatographic-Mass Spectrometric Analysis of Extracts of the Marine Algae, Caulerpa peltata and Padina Gymnospora.

    Science.gov (United States)

    Murugan, Kavitha; Iyer, Vidhya V

    2014-01-01

    The results of our previous investigations on extracts of selected marine algae showed that Caulerpa peltata and Padina gymnospora had more promising antiproliferative and antioxidant activities than Gelidiella acerosa and Sargassum wightii. Based on these results, the more active chloroform extract of C. peltata and ethyl acetate extract of P. gymnospora were further analyzed for their constituents by using gas chromatography in tandem with mass spectrometry. The GC-MS analysis (GC % peak area given in parentheses) showed that fucosterol (12.45%) and L-(+)-ascorbic acid 2, 6-dihexadecanoate (8.13%) were the major compounds present in P. gymnospora ethyl acetate extract. On the other hand, C. peltata chloroform extract had 1-heptacosanol (10.52%), hexacosanol acetate (9.28%), tetradecyl ester of chloroacetic acid (7.22%), Z,Z-6, 28-heptatriactontadien-2-one (6.77%) and 10, 13-dimethyl-methyl ester of tetradecanoic acid (5.34%) as major compounds. Also described in the report are the beta-carotene bleaching inhibitory and total reducing activities of the chloroform and ethyl acetate extracts of C. peltata and P. gymnospora, respectively, relative to the other three extracts (aqueous, methanol, chloroform or ethyl acetate) of the two algae.

  3. Characterization of odorous contaminants in post-consumer plastic packaging waste using multidimensional gas chromatographic separation coupled with olfactometric resolution.

    Science.gov (United States)

    Strangl, Miriam; Fell, Tanja; Schlummer, Martin; Maeurer, Andreas; Buettner, Andrea

    2017-04-01

    The increasing world population with their growing consumption of goods escalates the issue of sustainability concepts with increasing demands in recycling technologies. Recovery of post-consumer packaging waste is a major topic in this respect. However, contamination with odorous constituents currently curtails the production of recycling products that meet the high expectations of both consumers and industry. To guarantee odor-free recyclates, the main prerequisite is to characterize the molecular composition of the causative odorants in post-consumer plastic packaging waste. However, targeted characterization of odorous trace contaminants among an abundance of volatiles is a major challenge and requires specialized and high-resolution analytical approaches. For this aim, post-consumer packaging waste was characterized by sensory analysis and two-dimensional high resolution gas chromatography coupled with mass spectrometry and olfactometry. The 33 identified odorants represent various structural classes as well as a great diversity of smell impressions with some of the compounds being identified in plastics for the first time. Substances unraveled within this study provide insights into sources of odorous contamination that will require specific attention in the future in terms of screening and prevention in recycling products. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Comprehensive two-dimensional gas chromatographic profiling and chemometric interpretation of the volatile profiles of sweat in knit fabrics.

    Science.gov (United States)

    de la Mata, A Paulina; McQueen, Rachel H; Nam, Seo Lin; Harynuk, James J

    2017-03-01

    Human axillary sweat is a poorly explored biofluid within the context of metabolomics when compared to other fluids such as blood and urine. In this paper, we explore the volatile organic compounds emitted from two different types of fabric samples (cotton and polyester) which had been worn repeatedly during exercise by participants. Headspace solid-phase microextraction (SPME) and comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC×GC-TOFMS) were employed to profile the (semi)volatile compounds on the fabric. Principal component analysis models were applied to the data to aid in visualizing differences between types of fabrics, wash treatment, and the gender of the subject who had worn the fabric. Statistical tools included with commercial chromatography software (ChromaTOF) and a simple Fisher ratio threshold-based feature selection for model optimization are compared with a custom-written algorithm that uses cluster resolution as an objective function to maximize in a hybrid backward-elimination forward-selection approach for optimizing the chemometric models in an effort to identify some compounds that correlate to differences between fabric types. The custom algorithm is shown to generate better models than the simple Fisher ratio approach. Graphical Abstract A route from samples and questions to data and then answers.

  5. Gas chromatographic/mass spectrometric identification of chlorinated and oxygenated cyclohexene artifacts formed during the analysis of chlorinated water samples.

    Science.gov (United States)

    Dietrich, A M; Christman, R F; Durell, G S

    1988-04-15

    Chlorinated and oxygenated cyclohexene derivatives detected in methylene chloride extracts of chlorinated drinking water were demonstrated to be artifacts produced during sample preparation. Commercial methylene chloride contains cyclohexene as a preservative, and this reacted during the extraction/concentration process to produce microgram amounts of chlorocyclohexene, 2-chlorocyclohexanol, trans-1,2-dichlorocyclohexane, cyclohexenone and cyclohexenol. Quantitative analysis indicated that over 90% of the initial cyclohexene was consumed during the process. Dechlorination of drinking water with sodium arsenite significantly reduced but did not eliminate cyclohexene artifact formation.

  6. Gas chromatographic determination of organic acids from fruit juices by combined resin mediated methylation and extraction in supercritical carbon dioxide.

    Science.gov (United States)

    Barden, T J; Croft, M Y; Murby, E J; Wells, R J

    1997-10-17

    A procedure in which anionic analytes, trapped on ion exchange resin, are simultaneously methylated and released using methyl iodide in either supercritical carbon dioxide or acetonitrile has been extended to polyfunctional organic acids. The combined SFE methylation of fruit juice acids trapped onto ion exchange resin proceeds in good yield producing the methyl esters of fumaric, succinic, malic, tartaric, isocitric and citric acids which are readily separated by GC. Using this procedure low concentrations of one acid can be detected and quantitated in the presence of very high concentrations of another. This new method detects tartaric acid at levels of 10 ppm in juices containing 10,000 ppm citric acid. Quantitation was performed either by using GC-FID with triethyl citrate or diethyl tartrate as internal standards or with the element specific calibration capability of the GC-AED. A simple new technique for the determination of citric/isocitric acid ratio is now available. Also, in contrast to HPLC methods, the identity of an analyte is readily confirmed by GC-MS.

  7. Chromatographic separation and detection of contaminants from whole milk powder using a chitosan-modified silver nanoparticles surface-enhanced Raman scattering device.

    Science.gov (United States)

    Li, Dan; Lv, Di Y; Zhu, Qing X; Li, Hao; Chen, Hui; Wu, Mian M; Chai, Yi F; Lu, Feng

    2017-06-01

    Methods for the on-site analysis of food contaminants are in high demand. Although portable Raman spectroscopy is commonly used to test food on-site, it can be challenge to achieve this goal with rapid detection and inexpensive substrate. In this study, we detected trace food contaminants in samples of whole milk powder using the methods that combined chromatography with surface-enhanced Raman scattering detection (SERS). We developed a simple and efficient technique to fabricate the paper with chitosan-modified silver nanoparticles as a SERS-active substrate. The soaking time of paper and the concentration of chitosan solution were optimized for chromatographic separation and SERS detection. We then studied the separation properties for real applications including complex sample matrices, and detected melamine at 1mg/L, dicyandiamide at 100mg/L and sodium sulfocyanate at 10mg/L in whole milk powder. As such, our methods have great potential for field-based detection of milk contaminants. Copyright © 2016 Elsevier Ltd. All rights reserved.

  8. Green Ocean Amazon (GoAmazon) 2014/15. Semi-Volatile Thermal Desorption Aerosol Gas Chromatograph (SVTAG) Field Campaign Report

    Energy Technology Data Exchange (ETDEWEB)

    Goldstein, A. H. [Univ. of California, Berkeley, CA (United States); Yee, L. D. [Univ. of California, Berkeley, CA (United States); Issacman-VanWertz, G. [Univ. of California, Berkeley, CA (United States); Wernis, R. A. [Univ. of California, Berkeley, CA (United States)

    2016-03-01

    In areas where biogenic emissions are oxidized in the presence of anthropogenic pollutants such as SO2, NOx, and black carbon, it has become increasingly apparent that secondary organic aerosol (SOA) formation from biogenic volatile organic compounds (VOCs) is substantially enhanced. Research is urgently needed to elucidate fundamental processes of natural and anthropogenically influenced VOC oxidation and the contribution of these processes to SOA formation. GoAmazon 2014/15 afforded study of the chemical transformations in the region downwind of Manaus, Brazil, where local biogenic VOC emissions are high, and their chemical oxidation can be studied both inside and outside of the urban plume to differentiate the role of anthropogenic influence on secondary aerosol formation during oxidation of these natural VOC emissions. To understand the connection between primary biogenic VOC emissions and their secondary products that form aerosols, we made time-resolved molecular level measurements by deploying a Semi-Volatile Thermal Desorption Aerosol Gas Chromatograph (SV-TAG) and a sequential filter sampler during two intensive operational periods (IOPs) of the GoAmazon 2014/15 field campaign. The SV-TAG measured semi-volatile organic compounds in both the gas and particle phases and the sequential filter sampler collected aerosols on quartz fiber filters in four-hour increments used for offline analysis. SV-TAG employed novel online derivatization that provided chemical speciation of highly oxygenated or functionalized compounds that comprise a substantial fraction of secondary organic aerosols, yet are poorly characterized. It also provided partitioning of these compounds between the vapor and particle phases at sufficient time resolution to define the importance of competing atmospheric processes. These measurements were supported by offline analysis of the filters using two-dimensional gas chromatography (GC x GC) with high-resolution time-of-flight mass spectrometry

  9. Determinação espectrofotométrica e cromatográfica em fase gasosa de ácido tricloracético em urina Spectrophotometric and gas chromatographic determination of trichloroacetic acid in urine

    Directory of Open Access Journals (Sweden)

    Maria de Fatima M. Pedrozo

    1996-06-01

    Full Text Available Solventes halogenados -- 1,1,1-tricloretano, tricloretileno, percloretileno -- apresentam o ácido tricloracético (TCA como produto de biotransformação comum, o qual pode ser utilizado como indicador biológico de dose interna na exposição a estes compostos. Foi realizado estudo de métodos espectrofotométrico e cromatográfico em fase gasosa para a determinação do TCA, bem como da aplicação destes métodos à sua determinação em urina de indivíduos expostos ao 1,1,1-tricloretano. Os resultados mostram a boa precisão à determinação do TCA em urina de indivíduos expostos ao 1,1,1-tricloretano e nenhuma diferença significativa foi observada entre os métodos, ainda que o cromatográfico em fase gasosa apresentasse menor limite de detecção.Some chlorinated hydrocarbon solvents -- 1,1,1-trichloroethane, tricloroethylene and perchloroethylene -- have a common biotransformation product, trichloroacetic acid, which can be used as their biological exposure index. The spectrophotometric and gas chromatographic methods for the determination of trichloroacetic acid were studied and used as well as in its determination in the urine of workers exposed to 1,1,1-trichloroethane . Both methods showed good precision and no statistically significant difference was found although the gas cromatographic method presented a lower detection limit.

  10. Microwave-accelerated derivatization for the simultaneous gas chromatographic-mass spectrometric analysis of natural and synthetic estrogenic steroids.

    Science.gov (United States)

    Zuo, Yuegang; Zhang, Kai; Lin, Yuejuan

    2007-05-04

    A rapid microwave-accelerated derivatization process for the GC-MS analysis of steroid estrogens, estrone (E1), 17beta-estradiol (E2), estriol (E3), 17alpha-ethynylestradiol (EE2) and mestranol (MeEE2), was developed. Under microwave irradiation, the five estrogenic hormones studied were simultaneously derivatized with N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA)+trimethylchlorosilane (TMCS) in pyridine solution. Effects of irradiation time (15-120 s) and power level (240-800 W) on the yield of the derivatization were investigated. The derivatization under the irradiation of 800 W microwave for 60s produced comparable results when compared with the conventional heating process in a sand bath for 30 min at 80 degrees C in terms of derivatization yield, linearity and precision for all steroid hormones tested. The calibration curves are linear between 3.00 and 3.00 x 10(2) microg mL(-1). The square of the regression coefficients (R(2)) range from 0.979 to 1.000. The applicability of the method was evaluated on spiked river and distilled water samples at two concentrations, 25.0 and 2.00 x 10(2) ng mL(-1). The recoveries obtained by using microwave heating (60s, 800 W) were similar to those by conventional heating. When combined solid-phase extraction (SPE) with the application of the microwave-accelerated derivatization proposed here, the detection limits of 0.02-0.1 ng L(-1) for the steroid hormones have been achieved. The results demonstrated that microwave-accelerated derivatization is an efficient and suitable sample preparation method for the GC-MS analysis of estrogenic steroids.

  11. Determination of pyrethroid pesticide residues in processed fruits and vegetables by gas chromatography with electron capture and mass spectrometric detection.

    Science.gov (United States)

    Sannino, Anna; Bandini, Mirella; Bolzoni, Luciana

    2003-01-01

    A gas chromatographic method was developed for the simultaneous determination of 12 pyrethroids (tefluthrin, bifenthrin, fenpropathrin, cyhalothrin, permethrin, cyfluthrin, cypermethrin, alpha-cypermethrin, flucythrinate, fenvalerate, fluvalinate, and deltamethrin) in tomato puree, peach nectar, orange juice, and canned peas. A miniaturized extraction-partition procedure requiring small amounts of nonchlorinated solvents is used. Samples are extracted with acetone, partitioned with ethyl acetate-cyclohexane (50 + 50, v/v), and cleaned up on a Florisil cartridge. The final extract is analyzed by gas chromatography with both electron capture and mass spectrometric detection modes. Studies at fortification levels of 0.010-0.100 mg/kg gave mean recoveries ranging from 70.2 to 96.0% and coefficients of variation between 4.0 and 13.9% for all compounds. Quantitation limits were < 0.010 mg/kg for electron capture detection.

  12. On camera-based smoke and gas leakage detection

    Energy Technology Data Exchange (ETDEWEB)

    Nyboe, Hans Olav

    1999-07-01

    Gas detectors are found in almost every part of industry and in many homes as well. An offshore oil or gas platform may host several hundred gas detectors. The ability of the common point and open path gas detectors to detect leakages depends on their location relative to the location of a gas cloud. This thesis describes the development of a passive volume gas detector, that is, one than will detect a leakage anywhere in the area monitored. After the consideration of several detection techniques it was decided to use an ordinary monochrome camera as sensor. Because a gas leakage may perturb the index of refraction, parts of the background appear to be displaced from their true positions, and it is necessary to develop algorithms that can deal with small differences between images. The thesis develops two such algorithms. Many image regions can be defined and several feature values can be computed for each region. The value of the features depends on the pattern in the image regions. The classes studied in this work are: reference, gas, smoke and human activity. Test show that observation belonging to these classes can be classified fairly high accuracy. The features in the feature set were chosen and developed for this particular application. Basically, the features measure the magnitude of pixel differences, size of detected phenomena and image distortion. Interesting results from many experiments are presented. Most important, the experiments show that apparent motion caused by a gas leakage or heat convection can be detected by means of a monochrome camera. Small leakages of methane can be detected at a range of about four metres. Other gases, such as butane, where the densities differ more from the density of air than the density of methane does, can be detected further from the camera. Gas leakages large enough to cause condensation have been detected at a camera distance of 20 metres. 59 refs., 42 figs., 13 tabs.

  13. Determination of Odor Release in Hydrocolloid Model Systems Containing Original or Carboxylated Cellulose at Different pH Values Using Static Headspace Gas Chromatographic (SHS-GC Analysis

    Directory of Open Access Journals (Sweden)

    Pahn-Shick Chang

    2013-02-01

    Full Text Available Static headspace gas chromatographic (SHS-GC analysis was performed to determine the release of 13 odorants in hydrocolloid model systems containing original or regio-selectively carboxylated cellulose at different pH values. The release of most odor compounds was decreased in the hydrocolloid solutions compared to control, with the amounts of 2-propanol, 3-methyl-1-butanol, and 2,3-butanedione released into the headspace being less than those of any other odor compound in the hydrocolloid model systems. However, there was no considerable difference between original cellulose-containing and carboxylated-cellulose containing systems in the release of most compounds, except for relatively long-chain esters such as ethyl caprylate and ethyl nonanoate. The release from the original and carboxylated cellulose solutions controlled to pH 10 was significantly higher than that from solutions adjusted to pH 4 and 7 in the case of some esters (ethyl acetate, methyl propionate, ethyl propionate, ethyl butyrate, butyl propionate, ethyl caproate and alcohols (2-propanol, 3-methyl-1-butanol, in particular, ethyl butyrate and 3-methyl-1-butanol. In contrast, the release of 2,3-butanedione from both the original and carboxylated cellulose solutions was increased at pH 4 and 7 compared to that at pH 10 by about 70% and 130%, respectively. Our study demonstrated that the release of some odorants could be changed significantly by addition of both original and carboxylated cellulose in hydrocolloid model systems, but only minor effect was observed in pH of the solution.

  14. The gas chromatographic determination of volatile fatty acids in wastewater samples: evaluation of experimental biases in direct injection method against thermal desorption method.

    Science.gov (United States)

    Ullah, Md Ahsan; Kim, Ki-Hyun; Szulejko, Jan E; Cho, Jinwoo

    2014-04-11

    The production of short-chained volatile fatty acids (VFAs) by the anaerobic bacterial digestion of sewage (wastewater) affords an excellent opportunity to alternative greener viable bio-energy fuels (i.e., microbial fuel cell). VFAs in wastewater (sewage) samples are commonly quantified through direct injection (DI) into a gas chromatograph with a flame ionization detector (GC-FID). In this study, the reliability of VFA analysis by the DI-GC method has been examined against a thermal desorption (TD-GC) method. The results indicate that the VFA concentrations determined from an aliquot from each wastewater sample by the DI-GC method were generally underestimated, e.g., reductions of 7% (acetic acid) to 93.4% (hexanoic acid) relative to the TD-GC method. The observed differences between the two methods suggest the possibly important role of the matrix effect to give rise to the negative biases in DI-GC analysis. To further explore this possibility, an ancillary experiment was performed to examine bias patterns of three DI-GC approaches. For instance, the results of the standard addition (SA) method confirm the definite role of matrix effect when analyzing wastewater samples by DI-GC. More importantly, their biases tend to increase systematically with increasing molecular weight and decreasing VFA concentrations. As such, the use of DI-GC method, if applied for the analysis of samples with a complicated matrix, needs a thorough validation to improve the reliability in data acquisition. Copyright © 2014 Elsevier B.V. All rights reserved.

  15. Naturally fractured tight gas reservoir detection optimization

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1999-06-01

    Building upon the partitioning of the Greater Green River Basin (GGRB) that was conducted last quarter, the goal of the work this quarter has been to conclude evaluation of the Stratos well and the prototypical Green River Deep partition, and perform the fill resource evaluation of the Upper Cretaceous tight gas play, with the goal of defining target areas of enhanced natural fracturing. The work plan for the quarter of November 1-December 31, 1998 comprised four tasks: (1) Evaluation of the Green River Deep partition and the Stratos well and examination of potential opportunity for expanding the use of E and P technology to low permeability, naturally fractured gas reservoirs, (2) Gas field studies, and (3) Resource analysis of the balance of the partitions.

  16. Comparison of three chromatographic techniques for the detection of mitragynine and other indole and oxindole alkaloids in Mitragyna speciosa (kratom) plants.

    Science.gov (United States)

    Wang, Mei; Carrell, Emily J; Ali, Zulfiqar; Avula, Bharathi; Avonto, Cristina; Parcher, Jon F; Khan, Ikhlas A

    2014-06-01

    Leaves of the Southeast Asian plant Mitragyna speciosa are used to suppress pain and mitigate opioid withdrawal syndromes. The potential threat of abuse and ready availability of this uncontrolled psychoactive plant have led to the need for improved analytical techniques for the detection of the major active components, mitragynine and 7-hydroxymitragynine. Three independent chromatographic methods coupled to two detection systems, GC with MS, supercritical fluid chromatography with diode array detection, and HPLC with MS and diode array detection, were compared for the analysis of mitragynine and other indole and oxindole alkaloids in M. speciosa plants. The indole alkaloids included two sets of diastereoisomers: (i) paynantheine and 3-isopaynantheine and (ii) mitragynine, speciogynine, and speciociliatine. Two oxindole alkaloid diastereoisomers, corynoxine and corynoxine B, were also studied. The HPLC and supercritical fluid chromatography methods successfully resolved the major components with slightly different elution orders. The GC method was less satisfactory because it was unable to resolve mitragynine and speciociliatine. This separation was difficult by GC with a liquid stationary phase because these diastereoisomers differ only in the orientation of an interior hydrogen atom. The observed lack of resolution of the indole alkaloid diastereoisomers coupled with the likeness of the mass and tandem mass spectra, calls into question proposed GC methods for the analysis of mitragynine based on solely GC with MS separation and identification. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. 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.

  18. Detection of gas entrainment into liquid metals

    Energy Technology Data Exchange (ETDEWEB)

    Vogt, T., E-mail: t.vogt@hzdr.de [Helmholtz-Zentrum Dresden-Rossendorf (HZDR), Institute of Fluid Dynamics, 01328 Dresden (Germany); Boden, S. [Helmholtz-Zentrum Dresden-Rossendorf (HZDR), Institute of Fluid Dynamics, 01328 Dresden (Germany); Andruszkiewicz, A. [Faculty of Mechanical and Power Engineering, Wroclaw University of Technology (Poland); Eckert, K. [Technische Universität Dresden, Institute of Fluid Mechanics, 01062 Dresden (Germany); Eckert, S.; Gerbeth, G. [Helmholtz-Zentrum Dresden-Rossendorf (HZDR), Institute of Fluid Dynamics, 01328 Dresden (Germany)

    2015-12-01

    Highlights: • We present liquid metal experiments dedicated to gas entrainment on the free surface. • Ultrasonic and X-ray attenuation techniques have been used to study the mechanisms of gas entrainment. • A comparison between bubbly flow in water and GaInSn showed substantial differences. • Our results emphasize the importance of liquid metal experiments which are able to provide a suitable data base for numerical code validation. - Abstract: Entrainment of cover gas into the liquid metal coolant is one of the principal safety issues in the design of innovative liquid metal-cooled fast reactors. We present generic experimental studies of this phenomenon in low-melting metals. Ultrasonic and X-ray diagnostic tools were considered for a visualization of gas entrainment at the free surface of the melt. Laboratory experiments were conducted using the eutectic alloy GaInSn, which is liquid at room temperature. Vortex-activated entrainment of air at the free surface of a rotating flow was revealed by ultrasonic techniques. X-ray radioscopy was used to visualize the behavior of argon bubbles inside a slit geometry. The measurements reveal distinct differences between water and GaInSn, especially with respect to the process of bubble formation and the coalescence and breakup of bubbles. Our results emphasize the importance of liquid metal experiments which are able to provide a suitable data base for numerical code validation.

  19. Detecting gas leaks by ultrasonic emission

    DEFF Research Database (Denmark)

    Rasmussen, Karsten Bo; Henriksen, Eigil

    1997-01-01

    The emission of noise in the frequency range 10 kHz to 25.6 kHz from an experimental gas leak in a flanged joint has been experimentally investigated. The overall conclusion is that the emitted noise is almost frequency independent in level within the considered frequency range.A small PC program...

  20. 46 CFR 154.1350 - Flammable gas detection system.

    Science.gov (United States)

    2010-10-01

    ... between the doors of an air lock under § 154.345. (b) The sampling points under paragraph (a) of this... automatic valve that prevents cross-communication between sampling points. (p) Each flammable gas detection...

  1. Mobile Passive Optical Imager for Remote Gas Detection, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — Tunable filters based on electro-optic effect have shown great potential in detecting gas concentration through obtaining its absorption spectrum. In filter-based...

  2. Detection of Greenhouse-Gas-Induced Climatic Change

    Energy Technology Data Exchange (ETDEWEB)

    Jones, P.D.; Wigley, T.M.L.

    1998-05-26

    The objective of this report is to assemble and analyze instrumental climate data and to develop and apply climate models as a basis for (1) detecting greenhouse-gas-induced climatic change, and (2) validation of General Circulation Models.

  3. Derivative Quotient Spectrophotometry and an Eco-Friendly Micellar Chromatographic Approach with Time-Programmed UV-Detection for the Separation of Two Fluoroquinolones and Phenazopyridine

    Science.gov (United States)

    Tolba, Manar M.; Salim, Mohamed M.

    2016-01-01

    In this study, two analytical approaches were exploited for the resolution of binary mixtures of ciprofloxacin HCl (CIP) or norfloxacin (NOR) and phenazopyridine HCl (PHZ). In the first approach, the amplitudes of the first derivative of the ratio spectra were measured at 267 or 287 nm for CIP and at 268 or 291 nm for NOR. PHZ could be directly determined in the presence of CIP or NOR at 405 nm. The calibration graphs were rectilinear over the ranges of 1.0–16.0 µg/mL for CIP or NOR and 1.0–10.0 µg/mL for PHZ. In the second approach, an accurate, reliable and environmentally nontoxic micellar liquid chromatographic (MLC) method was developed. A good chromatographic separation was achieved using a 150 mm × 4.6 mm i.d., 5 µm particle size Spherisorb ODS-2 column. Eco-friendly mobile phase containing 0.12 M sodium dodecyl sulphate, 0.3% triethylamine and 6% n-butanol in 0.02 M orthophosphoric acid of pH 3.0 was pumped at a flow rate of 1 mL/min. Time programmed UV-detection was applied to allow sensitive determination of the studied drugs. The analytes were eluted without interferences in <10 min. Methocarbamol was used as an internal standard. The MLC method was found to be rectilinear over the concentration range of 0.5–20.0 μg/mL for CIP, NOR or PHZ. These optimized and validated methods were successfully applied for the simultaneous analysis of the studied drugs in their synthetic mixtures and co-formulated tablets. Moreover, the second method was further extended to the determination of these drugs in human urine with direct injection and without any pretreatment. PMID:26867555

  4. Collection and determination of volatile organic mercury compounds in the atmosphere by gas chromatography with microwave plasma detection

    Energy Technology Data Exchange (ETDEWEB)

    Ballantine, D.S. Jr.; Zoller, W.H.

    1984-07-01

    A method for the collection of two volatile organic mercury compounds in the atmosphere is described, using Chromosorb 101 as a collection substrate. The analytical method involves direct elution of the organic mercury compounds from the collection substrate onto a gas chromatographic column prior to detection with a microwave plasma detector. Methylmercury chloride (MMC) is collected at ambient temperatures, and dimethylmercury (DMM) is collected by use of a cryogenic trap at -80/sup 0/C. Collection efficiencies for MMC and DMM are 95 +/- 3% and 96 +/- 2%, respectively. The absolute detection limit of the system is 0.05 ng, with a detection limit for real atmospheric samples of 0.1 ng/m/sup 3/. Positive identification of collected compounds is achieved by comparison of sample elution volumes with standards. 14 references, 5 figures, 3 tables.

  5. Microstructuring of piezoresistive cantilevers for gas detection and analysis

    International Nuclear Information System (INIS)

    Sarov, Y.; Sarova, V.; Bitterlich, Ch.; Richter, O.; Guliyev, E.; Zoellner, J.-P.; Rangelow, I. W.; Andok, R.; Bencurova, A.

    2011-01-01

    In this work we report on a design and fabrication of cantilevers for gas detection and analysis. The cantilevers have expanded area of interaction with the gas, while the signal transduction is realized by an integrated piezoresistive deflection sensor, placed at the narrowed cantilever base with highest stress along the cantilever. Moreover, the cantilevers have integrated bimorph micro-actuator detection in a static and dynamic mode. The cantilevers are feasible as pressure, temperature and flow sensors and under chemical functionalization - for gas recognition, tracing and composition analysis. (authors)

  6. 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

  7. 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

  8. Detection of Griseofulvin and Dechlorogriseofulvin by Thin-Layer Chromatography and Gas-Liquid Chromatography

    Science.gov (United States)

    Cole, R. J.; Kirksey, J. W.; Holaday, C. E.

    1970-01-01

    A rapid and accurate method is described for the determination of griseofulvin and dechlorogriseofulvin extracted from Penicillium urticae with chloroform. Thinlayer chromatography was used to tentatively identify griseofulvin or dechlorogriseofulvin, or both. Two gas-liquid chromatographic systems provided additional qualitative information and simultaneous quantitation of the individual compounds. PMID:5415206

  9. Rapid high-performance thin-layer chromatographic method for detection of 5% adulteration of black cohosh with Cimicifuga foetida, C. heracleifolia, C. dahurica, or C. americana.

    Science.gov (United States)

    Ankli, Anita; Reich, Eike; Steiner, Mario

    2008-01-01

    Black cohosh (Cimicifuga racemosa) is used to treat discomfort during menopause and as a substitute for synthetic drugs in hormone replacement therapy. The mostly wildcrafted plant is ranked among the top-selling herbs in the United States. There is a risk for adulteration with the similar-looking C. americana, which grows in the same habitats of the eastern United States. Other adulterants found in today's global marketplace are the 3 Asian Cimicifuga species C. foetida, C. heracleifolia, and C. dahurica. A very practical, rapid, and reliable high-performance thin-layer chromatographic (HPTLC) method was developed for identification of C. racemosa and detection of its most common adulterants by fingerprint profiles. With specific derivatization reagents, mixtures of C. racemosa with a minimum of 5% of one of the adulterants can be detected. The proposed method was validated with respect to specificity, stability, precision, and robustness. It can be used for quality control of black cohosh raw material in a current Good Manufacturing Practices environment.

  10. Comparison of two detection methods in thin layer chromatographic analysis of some herbicides in a coastal savannah soil in Ghana

    International Nuclear Information System (INIS)

    Afful, S.; Yeboah, P.O.; Dogbe, S.A.; Akpabli, C.K.

    2008-01-01

    o-tolidine plus potassium iodide and photosynthesis inhibition detection methods were investigated for the analysis of three triazine herbicides (atrazine, ametryne, simazine) and two urea herbicides (diuron, metbromuron) in a coastal savannah soil using thin layer chromatography to compare the suitability of the two methods for the study of the herbicides. This was done by spiking 5 g of the soil sample with specific amount of the herbicide standards to generate herbicide-soil concentration of 40.24, 41.46, 40.28, 39.90 and 40.64 μg/g for atrazine, ametryne, simazine, diuron and metbromuron, respectively. Extraction was performed with acetone/hexane mixture (4:1) and the detection limit of each herbicide was then determined. In all, the photosynthesis inhibition method performed better for both the triazine and the urea herbicides, while the o-tolidine plus potassium iodide method was suitable for only the triazine herbicides. With the photosynthesis inhibition method, detectability in the range of 0.004-0.008 ± 0.002 μg/g was attained for the herbicides using the unclean extracts. In the case of o-tolidine plus potassium iodide method, detectability of 0.008-0.406 ± 0.02 μg/g was obtained. With the clean up extracts detectability in the range of 0.025-0.162 ± 0.004 μg/g was obtained using the photosynthesis inhibition method. However, metbromuron was not detected in the cleaned up extracts when o-tolidine plus potassium iodide detection method was used. For the methods described, clean up with SPE cartridge, equipped with C-18, is not critical to obtain the desired results. (au)

  11. Gas Environment Recoverable Detection (GERD) HMI

    CERN Document Server

    Sillat, Mari Liis

    2016-01-01

    Report on the work done during the summer student project. The goal was to produce HMI panels for the GERD smoke detection system. The required platform was WinCC OA and the running sensor data needed to be displayed, pump controls were needed and an alarm was required to be set for the smoke sensors upper limit range.

  12. Naturally fractured tight gas reservoir detection optimization

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1998-11-30

    The work plan for October 1, 1997 to September 30, 1998 consisted of investigation of a number of topical areas. These topical areas were reported in four quarterly status reports, which were submitted to DOE earlier. These topical areas are reviewed in this volume. The topical areas covered during the year were: (1) Development of preliminary tests of a production method for determining areas of natural fracturing. Advanced Resources has demonstrated that such a relationship exists in the southern Piceance basin tight gas play. Natural fracture clusters are genetically related to stress concentrations (also called stress perturbations) associated with local deformation such a faulting. The mechanical explanation of this phenomenon is that deformation generally initiates at regions where the local stress field is elevated beyond the regional. (2) Regional structural and geologic analysis of the Greater Green River Basin (GGRB). Application of techniques developed and demonstrated during earlier phases of the project for sweet-spot delineation were demonstrated in a relatively new and underexplored play: tight gas from continuous-typeUpper Cretaceous reservoirs of the Greater Green River Basin (GGRB). The effort included data acquisition/processing, base map generation, geophysical and remote sensing analysis and the integration of these data and analyses. (3) Examination of the Table Rock field area in the northern Washakie Basin of the Greater Green River Basin. This effort was performed in support of Union Pacific Resources- and DOE-planned horizontal drilling efforts. The effort comprised acquisition of necessary seismic data and depth-conversion, mapping of major fault geometry, and analysis of displacement vectors, and the development of the natural fracture prediction. (4) Greater Green River Basin Partitioning. Building on fundamental fracture characterization work and prior work performed under this contract, namely structural analysis using satellite and

  13. Early detection of LPG gas leakage based Wireless Sensor Networking

    Directory of Open Access Journals (Sweden)

    Kusriyanto Medilla

    2018-01-01

    Full Text Available LPG gas is the main fuel used in households. These days LPG gas leak triggered an accident that resulted in huge losses, especially if the accident occurred within the dense housing. LPG gas leakage monitoring and early detection of a gas leak and a leak warning is needed to prevent more fatal accident. Wireless sensor networking is a technology that can be used to build a centralized monitoring system by using a microcontroller as the interface and control system. This research developed system device monitoring and early detection of gas leaks by utilizing gas sensors MQ-4 and AVR microcontroller family as control devices. The system is also equipped with XBee PRO S2B nirkable devices as the interface to the wireless networking system that is used to transmit sensor data from the detection point to the monitoring center equipped with a PC and software integrated Visual Basic. Gas leak alert is sent with the message formats through social networking Gtalk.

  14. Novel preconcentration technique for on-line coupling to high-speed narrow-bore capillary gas chromatography: sample enrichment by equilibrium (ab)sorption. II. Coupling to a portable micro gas chromatograph.

    Science.gov (United States)

    Tuan, H P; Janssen, H G; Cramers, C A; Mussche, P; Lips, J; Wilson, N; Handley, A

    1997-12-12

    The technique of equilibrium (ab)sorption has been proven to be a powerful method for preconcentration of gaseous samples for high-speed narrow-bore capillary gas chromatography (GC) in general and field-portable GC instruments, often referred as micro GCs, in particular. Using a simple experimental set-up equipped with an open-tubular enrichment column it is possible to produce a homogeneously enriched sample plug, allowing reproducible injections of an enriched sample into the micro GC. Using a non-polar trapping column enrichment factors found for n-alkanes in the range of C7 to C10 ranged from 15 to 150 and agree well with calculated values. Using a highly retentive Thermocap column, the enrichment factor observed for heptane was above 500. As the use of this new preconcentration method requires only minimum modification of the micro GC, the chromatographic performance of the instrument was not compromised by direct coupling to the preconcentration device. Examples of on-line enrichment with portable micro GC analysis of VOCs from air are shown. These examples clearly demonstrate the potentials of the new method in field analysis.

  15. Temperature detection in a gas turbine

    Science.gov (United States)

    Lacy, Benjamin; Kraemer, Gilbert; Stevenson, Christian

    2012-12-18

    A temperature detector includes a first metal and a second metal different from the first metal. The first metal includes a plurality of wires and the second metal includes a wire. The plurality of wires of the first metal are connected to the wire of the second metal in parallel junctions. Another temperature detector includes a plurality of resistance temperature detectors. The plurality of resistance temperature detectors are connected at a plurality of junctions. A method of detecting a temperature change of a component of a turbine includes providing a temperature detector include ing a first metal and a second metal different from the first metal connected to each other at a plurality of junctions in contact with the component; and detecting any voltage change at any junction.

  16. Simultaneous determination of methanol, acetaldehyde, acetone, and ethanol in human blood by gas chromatography with flame ionization detection.

    Science.gov (United States)

    Schlatter, J; Chiadmi, F; Gandon, V; Chariot, P

    2014-01-01

    Methanol, acetaldehyde, acetone, and ethanol, which are commonly used as biomarkers of several diseases, in acute intoxications, and forensic settings, can be detected and quantified in biological fluids. Gas chromatography (GC)-mass spectrometry techniques are complex, require highly trained personnel and expensive materials. Gas chromatographic determinations of ethanol, methanol, and acetone have been reported in one study with suboptimal accuracy. Our objective was to improve the assessment of these compounds in human blood using GC with flame ionization detection. An amount of 50 µl of blood was diluted with 300 µl of sterile water, 40 µl of 10% sodium tungstate, and 20 µl of 1% sulphuric acid. After centrifugation, 1 µl of the supernatant was injected into the gas chromatograph. We used a dimethylpolysiloxane capillary column of 30 m × 0.25 mm × 0.25 µm. We observed linear correlations from 7.5 to 240 mg/l for methanol, acetaldehyde, and acetone and from 75 to 2400 mg/l for ethanol. Precision at concentrations 15, 60, and 120 mg/l for methanol, acetaldehyde, and acetone and 150, 600, and 1200 mg/ml for ethanol were 0.8-6.9%. Ranges of accuracy were 94.7-98.9% for methanol, 91.2-97.4% for acetaldehyde, 96.1-98.7% for acetone, and 105.5-111.6% for ethanol. Limits of detection were 0.80 mg/l for methanol, 0.61 mg/l for acetaldehyde, 0.58 mg/l for acetone, and 0.53 mg/l for ethanol. This method is suitable for routine clinical and forensic practices.

  17. Development of a chromatographic low pressure flow injection system using amperometric detection: Application to the analysis of niacin in coffee.

    Science.gov (United States)

    Santos, João Rodrigo; Rangel, António O S S

    2015-11-15

    In this work, an analytical flow system able to perform low pressure chromatography with amperometric detection is presented. As case study, the determination of niacin (vitamin B3) in coffee brewed samples was selected. The manifold comprised a 1.0 cm length monolithic column coated with didecyldimethylammonium bromide, a laboratory-made boron doped diamond electrode, and featured in-line ionic strength adjustment of the mobile phase. The figures of merit concerning the selected case study namely, detection limit, 7.90 × 10(-7) M, determination rate, ca. 10 samplesh(-1), mobile phase and ISA solution consumption, ca. 2.6 mL per analysis, and CV, below 5% for retention time and peak height, showed the competitiveness of this analytical strategy comparing to the described HPLC methods for niacin determination. The strategy displays a simple configuration, low cost, fast and easy assembling, foreseeing its use to general purpose applications. Copyright © 2015 Elsevier Ltd. All rights reserved.

  18. New approach for sensitive photothermal detection of C60 and C70 fullerenes on micro-thin-layer chromatographic plates.

    Science.gov (United States)

    Suszyński, Zbigniew; Zarzycki, Paweł K

    2015-03-10

    In this paper the pulse thermovision (photothermal) detection and quantification methods of C60 and C70 fullerenes are presented. Quantification results are compared with optical and fluorescence measurements. Target components were separated under isothermal conditions (30 °C) on micro-TLC plates (RP18WF254S) using n-hexane as the mobile phase. The principle of described analytical protocol is based on sensitive measurement of the temperature contrast generated within TLC stationary phase and fullerenes spots after white light pulse excitation. It has been demonstrated that observed temperature contrast is mainly driven by the optical properties of fullerenes (UV-vis absorption spectra). Contrary to the commonly applied optical reflection or transmission techniques the proposed thermovision method involves dissipated light. The results of presented experimental work have revealed that both types of quantitative measurements provide similar outcome despite the key differences in the signal origin. However, it has been found that thermovision method was characterized by smaller value of LOD, particularly for C60 molecule. We demonstrated that application of correlation technique to post-acquisition analysis of the sequence of temperature contrast images significantly increase detection limits of fullerenes, even in comparison to fluorescence quenching detection mode. Moreover, the thermal contrast images and particularly, computed correlation image, allow detection of stationary phase layer nonuniformities, including changes in the adsorbent thickness and thermal conductivity. Therefore, invented pulsed thermovision methodology can be additionally used for fast quality screening of home made and commercially available TLC plates. Copyright © 2014 Elsevier B.V. All rights reserved.

  19. Kinetic studies of gas mixtures and their application to gas lasers and pollutant detection

    International Nuclear Information System (INIS)

    Chen, C.H.; Judish, J.P.; Payne, M.G.

    1978-01-01

    A 2-MeV proton beam with a 10-ns pulse width was used to excite various gas mixtures. The emitted vacuum ultraviolet (500 A to 2000 A) and ultraviolet visible (2000 A to 8000 A) photons passing through separate monochromators were detected by using single photon counting techniques. Time-resolved and time-integrated fluorescent spectroscopy was used to study the detailed mechanism of excitation energy transfer, Penning ionization, charge transfer, and ion-ion recombination processes. The energy precursors of various excited species in a number of gas mixtures were identified, and the quenching rates of excited atoms and ions by numerous small molecules were measured. Relative fluorescence efficiencies and energy pathways of proton-excited gas mixtures were used to study the kinetics of high power gas lasers. An ultrasensitive method for the detection of certain pollutants utilizing energy or charge transfer processes in proton-excited gas mixtures has been developed

  20. Phenomena and Detection of Gas Accumulation in Piping Systems

    International Nuclear Information System (INIS)

    Lee, D. Y.; Jeon, S. S.; Hong, S. J.; Song, Y. J.

    2011-01-01

    U.S. Nuclear Regulatory Commission (NRC) issued Generic Letter (GL) 2008-01 which provides recommendation and guidance to nuclear power plants for managing gas intrusion and accumulation in safety systems such as Emergency Core Cooling (ECC), Decay Heat Removal (DHR) and Containment Spray (CS) systems. Following the GL2008-01, Nuclear Energy Institute (NEI) reported NEI 09-10 that gives industry guidance for effective prevention and management of system gas accumulation. All of U.S. utilities responded to the GL2008-01 with evaluation results for gas accumulation in safety systems mentioned above. This paper summarizes key phenomena to be evaluated against gas accumulation in safety systems and detection methods for gas accumulation in subjected systems

  1. Gas Leak Detection by Dilution of Atmospheric Oxygen.

    Science.gov (United States)

    Lambrecht, Armin; Maier, Eric; Pernau, Hans-Fridtjof; Strahl, Thomas; Herbst, Johannes

    2017-12-05

    Gas leak detection is an important issue in infrastructure monitoring and industrial production. In this context, infrared (IR) absorption spectroscopy is a major measurement method. It can be applied in an extractive or remote detection scheme. Tunable laser spectroscopy (TLS) instruments are able to detect CH₄ leaks with column densities below 10 ppm·m from a distance of 30 m in less than a second. However, leak detection of non-IR absorbing gases such as N₂ is not possible in this manner. Due to the fact that any leaking gas displaces or dilutes the surrounding background gas, an indirect detection is still possible. It is shown by sensitive TLS measurements of the ambient background concentration of O₂ that N₂ leaks can be localized with extractive and standoff methods for distances below 1 m. Minimum leak rates of 0.1 mbar·L/s were determined. Flow simulations confirm that the leakage gas typically effuses in a narrow jet. The sensitivity is mainly determined by ambient flow conditions. Compared to TLS detection of CH₄ at 1651 nm, the indirect method using O₂ at 761 nm is experimentally found to be less sensitive by a factor of 100. However, the well-established TLS of O₂ may become a universal tool for rapid leakage screening of vessels that contain unknown or inexpensive gases, such as N₂.

  2. Are Optical Gas Imaging Technologies Effective For Methane Leak Detection?

    Science.gov (United States)

    Ravikumar, Arvind P; Wang, Jingfan; Brandt, Adam R

    2017-01-03

    Concerns over mitigating methane leakage from the natural gas system have become ever more prominent in recent years. Recently, the U.S. Environmental Protection Agency proposed regulations requiring use of optical gas imaging (OGI) technologies to identify and repair leaks. In this work, we develop an open-source predictive model to accurately simulate the most common OGI technology, passive infrared (IR) imaging. The model accurately reproduces IR images of controlled methane release field experiments as well as reported minimum detection limits. We show that imaging distance is the most important parameter affecting IR detection effectiveness. In a simulated well-site, over 80% of emissions can be detected from an imaging distance of 10 m. Also, the presence of "superemitters" greatly enhance the effectiveness of IR leak detection. The minimum detectable limits of this technology can be used to selectively target "superemitters", thereby providing a method for approximate leak-rate quantification. In addition, model results show that imaging backdrop controls IR imaging effectiveness: land-based detection against sky or low-emissivity backgrounds have higher detection efficiency compared to aerial measurements. Finally, we show that minimum IR detection thresholds can be significantly lower for gas compositions that include a significant fraction nonmethane hydrocarbons.

  3. Methods for gas detection using stationary hyperspectral imaging sensors

    Science.gov (United States)

    Conger, James L [San Ramon, CA; Henderson, John R [Castro Valley, CA

    2012-04-24

    According to one embodiment, a method comprises producing a first hyperspectral imaging (HSI) data cube of a location at a first time using data from a HSI sensor; producing a second HSI data cube of the same location at a second time using data from the HSI sensor; subtracting on a pixel-by-pixel basis the second HSI data cube from the first HSI data cube to produce a raw difference cube; calibrating the raw difference cube to produce a calibrated raw difference cube; selecting at least one desired spectral band based on a gas of interest; producing a detection image based on the at least one selected spectral band and the calibrated raw difference cube; examining the detection image to determine presence of the gas of interest; and outputting a result of the examination. Other methods, systems, and computer program products for detecting the presence of a gas are also described.

  4. [A mobile sensor for remote detection of natural gas leakage].

    Science.gov (United States)

    Zhang, Shuai; Liu, Wen-qing; Zhang, Yu-jun; Kan, Rui-feng; Ruan, Jun; Wang, Li-ming; Yu, Dian-qiang; Dong, Jin-ting; Han, Xiao-lei; Cui, Yi-ben; Liu, Jian-guo

    2012-02-01

    The detection of natural gas pipeline leak becomes a significant issue for body security, environmental protection and security of state property. However, the leak detection is difficult, because of the pipeline's covering many areas, operating conditions and complicated environment. A mobile sensor for remote detection of natural gas leakage based on scanning wavelength differential absorption spectroscopy (SWDAS) is introduced. The improved soft threshold wavelet denoising was proposed by analyzing the characteristics of reflection spectrum. And the results showed that the signal to noise ratio (SNR) was increased three times. When light intensity is 530 nA, the minimum remote sensitivity will be 80 ppm x m. A widely used SWDAS can make quantitative remote sensing of natural gas leak and locate the leak source precisely in a faster, safer and more intelligent way.

  5. Modelling and interpretation of gas detection using remote laser pointers.

    Science.gov (United States)

    Hodgkinson, J; van Well, B; Padgett, M; Pride, R D

    2006-04-01

    We have developed a quantitative model of the performance of laser pointer style gas leak detectors, which are based on remote detection of backscattered radiation. The model incorporates instrumental noise limits, the reflectivity of the target background surface and a mathematical description of gas leak dispersion in constant wind speed and turbulence conditions. We have investigated optimum instrument performance and limits of detection in simulated leak detection situations. We predict that the optimum height for instruments is at eye level or above, giving an operating range of 10 m or more for most background surfaces, in wind speeds of up to 2.5 ms(-1). For ground based leak sources, we find laser pointer measurements are dominated by gas concentrations over a short distance close to the target surface, making their readings intuitive to end users in most cases. This finding is consistent with the results of field trials.

  6. Residual detection of buparvaquone, nystatin, and etomidate in animal-derived food products in a single chromatographic run using liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Zhang, Dan; Park, Jin-A; Abd El-Aty, A M; Kim, Seong-Kwan; Cho, Sang-Hyun; Wang, Yanmei; Shim, Jae-Han; Jeong, Ji Hoon; Shin, Sung Chul; Kim, Jin-Suk; Chang, Byung-Joon; Shin, Ho-Chul

    2017-12-15

    A reliable and highly sensitive screening method based on liquid chromatography coupled withtriple-quadrupoleelectrospray tandemmass spectrometry (LC-MS/MS) analysis has been developed for the detection and quantification of three veterinary drugs, including buparvaquone, nystatin, and etomidate impurity B CRS. The tested drugs were extracted from samples of porcine muscle, pasteurized whole milk, and eggs using 10mM ammonium formate in acetonitrile followed by liquid-liquid purification with n-hexane. Chromatographic separation was achieved on a Phenomenex Luna C18 analytical column using 0.1% formic acid in ultrapure water (A) and acetonitrile (B) as mobile phases. All the matrix-matched calibration curves were linear (R 2 ≥0.9756) over the concentration levels of the drugs tested. Recovery at two spiking levels (equivalent to the limit of quantification (LOQ)=5ng/g and 2×LOQ) ranged from 72.88% to 92.59% with intra- and inter-day precisions animal-derived food products meant for human consumption. Copyright © 2017 Elsevier Ltd. All rights reserved.

  7. ACOUSTIC DETECTING AND LOCATING GAS PIPE LINE INFRINGEMENT

    Energy Technology Data Exchange (ETDEWEB)

    John L. Loth; Gary J. Morris; George M. Palmer; Richard Guiler; Patrick Browning

    2004-12-01

    The extensive network of high-pressure natural gas transmission pipelines covering the United States provides an important infrastructure for our energy independence. Early detection of pipeline leaks and infringements by construction equipment, resulting in corrosion fractures, presents an important aspect of our national security policy. The National Energy Technology Laboratory Strategic Center for Natural Gas (SCVG) is and has been funding research on various applicable techniques. The WVU research team has focused on monitoring pipeline background acoustic signals generated and transmitted by gas flowing through the gas inside the pipeline. In case of a pipeline infringement, any mechanical impact on the pipe wall, or escape of high-pressure gas, generates acoustic signals traveling both up and down stream through the gas. Sudden changes in flow noise are detectable with a Portable Acoustic Monitoring Package (PAMP), developed under this contract. It incorporates a pressure compensating microphone and a signal- recording device. Direct access to the gas inside the line is obtained by mounting such a PAMP, with a 1/2 inch NPT connection, to a pipeline pressure port found near most shut-off valves. An FFT of the recorded signal subtracted by that of the background noise recorded one-second earlier appears to sufficiently isolate the infringement signal to allow source interpretation. Using cell phones for data downloading might allow a network of such 1000-psi rated PAMP's to acoustically monitor a pipeline system and be trained by neural network software to positively identify and locate any pipeline infringement.

  8. ACOUSTIC DETECTING AND LOCATING GAS PIPE LINE INFRINGEMENT

    Energy Technology Data Exchange (ETDEWEB)

    John L. Loth; Gary J. Morris; George M. Palmer; Richard Guiler; Patrick Browning

    2004-10-31

    The extensive network of high-pressure natural gas transmission pipelines covering the United States provides an important infrastructure for our energy independence. Early detection of pipeline leaks and infringements by construction equipment, resulting in corrosion fractures, presents an important aspect of our national security policy. The National Energy Technology Laboratory Strategic Center for Natural Gas (SCVG) is and has been funding research on various applicable techniques. The WVU research team has focused on monitoring pipeline background acoustic signals generated and transmitted by gas flowing through the gas inside the pipeline. In case of a pipeline infringement, any mechanical impact on the pipe wall, or escape of high-pressure gas, generates acoustic signals traveling both up and down stream through the gas. Sudden changes in flow noise are detectable with a Portable Acoustic Monitoring Package (PAMP), developed under this contract. It incorporates a pressure compensating microphone and a signal- recording device. Direct access to the gas inside the line is obtained by mounting such a PAMP, with a 1/2 inch NPT connection, to a pipeline pressure port found near most shut-off valves. An FFT of the recorded signal subtracted by that of the background noise recorded one-second earlier appears to sufficiently isolate the infringement signal to allow source interpretation. Using cell phones for data downloading might allow a network of such 1000-psi rated PAMP's to acoustically monitor a pipeline system and be trained by neural network software to positively identify and locate any pipeline infringement.

  9. High-performance liquid chromatographic assay of parabens in wash-off cosmetic products and foods using chemiluminescence detection

    International Nuclear Information System (INIS)

    Zhang Qunlin; Lian Mei; Liu Lijuan; Cui Hua

    2005-01-01

    A new method for the simultaneous determination of parabens including methylparaben, ethylparaben, propylparaben, and butylparaben by high-performance liquid chromatography (HPLC) coupled with chemiluminescence detection was developed. The procedure was based on the chemiluminescent enhancement by parabens of the cerium(IV)-rhodamine 6G system in the strong sulfuric acid medium. The good separation of parabens was carried out with an isocratic elution using a mixture of methanol and water (60:40, v/v) within 8.5 min. Under the optimized conditions, a linear working range extends three orders of magnitude with the relative standard deviations of intra- and inter-day precision below 4.5%, and the detection limits were 1.9 x 10 -9 , 2.7 x 10 -9 , 3.9 x 10 -9 , and 5.3 x 10 -9 g ml -1 for methylparaben, ethylparaben, propylparaben, and butylparaben, respectively. The chemiluminescence reaction was well compatible with the mobile phase of high-performance liquid chromatography. The proposed method has been successfully applied to the assay of parabens in wash-off cosmetic products and foods with the minimal sample preparation

  10. High-performance liquid chromatographic assay of parabens in wash-off cosmetic products and foods using chemiluminescence detection

    Energy Technology Data Exchange (ETDEWEB)

    Zhang Qunlin [Department of Chemistry, University of Science and Technology of China, Jinzai Road 96, Hefei, Anhui 230026 (China); Lian Mei [Department of Chemistry, University of Science and Technology of China, Jinzai Road 96, Hefei, Anhui 230026 (China); Liu Lijuan [Department of Chemistry, University of Science and Technology of China, Jinzai Road 96, Hefei, Anhui 230026 (China); Cui Hua [Department of Chemistry, University of Science and Technology of China, Jinzai Road 96, Hefei, Anhui 230026 (China)]. E-mail: hcui@ustc.edu.cn

    2005-04-29

    A new method for the simultaneous determination of parabens including methylparaben, ethylparaben, propylparaben, and butylparaben by high-performance liquid chromatography (HPLC) coupled with chemiluminescence detection was developed. The procedure was based on the chemiluminescent enhancement by parabens of the cerium(IV)-rhodamine 6G system in the strong sulfuric acid medium. The good separation of parabens was carried out with an isocratic elution using a mixture of methanol and water (60:40, v/v) within 8.5 min. Under the optimized conditions, a linear working range extends three orders of magnitude with the relative standard deviations of intra- and inter-day precision below 4.5%, and the detection limits were 1.9 x 10{sup -9}, 2.7 x 10{sup -9}, 3.9 x 10{sup -9}, and 5.3 x 10{sup -9} g ml{sup -1} for methylparaben, ethylparaben, propylparaben, and butylparaben, respectively. The chemiluminescence reaction was well compatible with the mobile phase of high-performance liquid chromatography. The proposed method has been successfully applied to the assay of parabens in wash-off cosmetic products and foods with the minimal sample preparation.

  11. Gas chromatographic quantification of aliphatic aldehydes in freshly distilled Calvados and Cognac using 3-methylbenzothiazolin-2-one hydrazone as derivative agent.

    Science.gov (United States)

    Ledauphin, Jérôme; Barillier, Daniel; Beljean-Leymarie, Martine

    2006-05-19

    A new precise and sensitive method was used for the quantification of aliphatic aldehydes from C5 to C11 in highly ethanolic beverages such as freshly distilled spirits. Carbonyl compounds were derivatized using 3-methylbenzothiazolin-2-one hydrazone (MBTH) and then separated and detected by gas chromatography-mass spectrometry (GC-MS). Selective mass spectrometric detection of molecular ions of derivatives was performed to obtain a good sensibility (0.2-1.2 microg l(-1)) and a good selectivity. For a concentration of 20 microg l(-1), relative standard deviations were lower than 10% except for heaviest compounds (decanal and undecanal) where RSD were between 11 and 13%. The concentrations of aliphatic aldehydes were determined in nine samples of freshly distilled Calvados and two samples of freshly distilled Cognac with highest concentrations reported for 3-methylbutanal (from 170 to 1220 microg l(-1) in Calvados and from 1540 to 5500 microg l(-1) in Cognac). 3-Methylbutanal and hexanal, due to their low detection thresholds, could be important olfactive markers of these two products. Less than 1h30 is required to quantify the nine studied aliphatic aldehydes in freshly distilled spirits.

  12. Gas chromatographic determination of N-nitrosamines, aromatic amines, and melamine in milk and dairy products using an automatic solid-phase extraction system.

    Science.gov (United States)

    Jurado-Sanchez, Beatriz; Ballesteros, Evaristo; Gallego, Mercedes

    2011-07-13

    A reliable analytical method was presented for the simultaneous determination of six N-nitrosamines, nine aromatic amines, and melamine in milk and dairy products using gas chromatography coupled with mass spectrometry. The sample treatment includes the precipitation of proteins with acetonitrile, centrifugation, solvent changeover by evaporation, and continuous solid-phase extraction for cleanup and preconcentration purposes. Samples (5 g) containing 0.15-500 ng of each amine were analyzed, and low detection limits (15-130 ng/kg) were achieved. Recoveries for milk and dairy products samples spiked with 1, 10, and 50 μg/kg ranged from 92% to 101%, with intraday and interday relative standard deviation values below 7.5%. The method was successfully applied to determine amine residues in several milk types (human breast, cow, and goat) and dairy products.

  13. Determination of uranium and thorium in complex samples using chromatographic separation, ICP-MS and spectrophotometric detection.

    Science.gov (United States)

    Rozmarić, Martina; Ivsić, Astrid Gojmerac; Grahek, Zeljko

    2009-11-15

    The paper describes a research of possible application of UTEVA and TRU resins and anion exchanger AMBERLITE CG-400 in nitrate form for the isolation of uranium and thorium from natural samples. The results of determination of distribution coefficient have shown that uranium and thorium bind on TRU and UTEVA resins from the solutions of nitric and hydrochloric acids, and binding strength increases proportionally to increase the concentration of acids. Uranium and thorium bind rather strongly to TRU resin from the nitric acid in concentration ranging from 0.5 to 5 mol L(-1), while large quantities of other ions present in the sample do not influence on the binding strength. Due to the difference in binding strength in HCl and HNO(3) respectively, uranium and thorium can be easily separated from each other on the columns filled with TRU resin. Furthermore, thorium binds to anion exchanger in nitrate form from alcohol solutions of nitric acid very strongly, while uranium does not, so they can be easily separated. Based on these results, we have created the procedures of preconcentration and separation of uranium and thorium from the soil, drinking water and seawater samples by using TRU and UTEVA resins and strong base anion exchangers in nitrate form. In one of the procedures, uranium and thorium bind directly from the samples of drinking water and seawater on the column filled with TRU resin from 0.5 mol L(-1) HNO(3) in a water sample. After binding, thorium is separated from uranium with 0.5 mol L(-1) HCl, and uranium is eluted with deionised water. By applying the described procedure, it is possible to achieve the concentration factor of over 1000 for the column filled with 1g of resin and splashed with 2L of the sample. Spectrophotometric determination with Arsenazo III, with this concentration factor results in detection limits below 1 microg L(-1) for uranium and thorium. In the second procedure, uranium and thorium are isolated from the soil samples with TRU

  14. Detection of greenhouse-gas-induced climatic change

    International Nuclear Information System (INIS)

    Wigley, T.M.L.; Jones, P.D.

    1992-01-01

    The aims of the US Department of Energy's Carbon Dioxide Research Program are to improve assessments of greenhouse-gas-induced climatic change and to define and reduce uncertainties through selected research. This project will address: The regional and seasonal details of the expected climatic changes; how rapidly will these changes occur; how and when will the climatic effects of CO 2 and other greenhouse gases be first detected; and the relationships between greenhouse-gas-induced climatic change and changes caused by other external and internal factors. The present project addresses all of these questions. Many of the diverse facets of greenhouse-gas-related climate research can be grouped under three interlinked subject areas: modeling, first detection and supporting data. This project will include the analysis of climate forcing factors, the development and refinement of transient response climate models, and the use of instrumental data in validating General Circulation Models (GCMs)

  15. Fabrication of a P3HT-ZnO Nanowires Gas Sensor Detecting Ammonia Gas

    Directory of Open Access Journals (Sweden)

    Chin-Guo Kuo

    2017-12-01

    Full Text Available In this study, an organic-inorganic semiconductor gas sensor was fabricated to detect ammonia gas. An inorganic semiconductor was a zinc oxide (ZnO nanowire array produced by atomic layer deposition (ALD while an organic material was a p-type semiconductor, poly(3-hexylthiophene (P3HT. P3HT was suitable for the gas sensing application due to its high hole mobility, good stability, and good electrical conductivity. In this work, P3HT was coated on the zinc oxide nanowires by the spin coating to form an organic-inorganic heterogeneous interface of the gas sensor for detecting ammonia gas. The thicknesses of the P3HT were around 462 nm, 397 nm, and 277 nm when the speeds of the spin coating were 4000 rpm, 5000 rpm, and 6000 rpm, respectively. The electrical properties and sensing characteristics of the gas sensing device at room temperature were evaluated by Hall effect measurement and the sensitivity of detecting ammonia gas. The results of Hall effect measurement for the P3HT-ZnO nanowires semiconductor with 462 nm P3HT film showed that the carrier concentration and the mobility were 2.7 × 1019 cm−3 and 24.7 cm2∙V−1∙s−1 respectively. The gas sensing device prepared by the P3HT-ZnO nanowires semiconductor had better sensitivity than the device composed of the ZnO film and P3HT film. Additionally, this gas sensing device could reach a maximum sensitivity around 11.58 per ppm.

  16. Fabrication of a P3HT-ZnO Nanowires Gas Sensor Detecting Ammonia Gas.

    Science.gov (United States)

    Kuo, Chin-Guo; Chen, Jung-Hsuan; Chao, Yi-Chieh; Chen, Po-Lin

    2017-12-25

    In this study, an organic-inorganic semiconductor gas sensor was fabricated to detect ammonia gas. An inorganic semiconductor was a zinc oxide (ZnO) nanowire array produced by atomic layer deposition (ALD) while an organic material was a p-type semiconductor, poly(3-hexylthiophene) (P3HT). P3HT was suitable for the gas sensing application due to its high hole mobility, good stability, and good electrical conductivity. In this work, P3HT was coated on the zinc oxide nanowires by the spin coating to form an organic-inorganic heterogeneous interface of the gas sensor for detecting ammonia gas. The thicknesses of the P3HT were around 462 nm, 397 nm, and 277 nm when the speeds of the spin coating were 4000 rpm, 5000 rpm, and 6000 rpm, respectively. The electrical properties and sensing characteristics of the gas sensing device at room temperature were evaluated by Hall effect measurement and the sensitivity of detecting ammonia gas. The results of Hall effect measurement for the P3HT-ZnO nanowires semiconductor with 462 nm P3HT film showed that the carrier concentration and the mobility were 2.7 × 10 19 cm -3 and 24.7 cm²∙V -1 ∙s -1 respectively. The gas sensing device prepared by the P3HT-ZnO nanowires semiconductor had better sensitivity than the device composed of the ZnO film and P3HT film. Additionally, this gas sensing device could reach a maximum sensitivity around 11.58 per ppm.

  17. Low-Cost Resonant Cavity Raman Gas Probe for Multi-Gas Detection

    Science.gov (United States)

    Thorstensen, J.; Haugholt, K. H.; Ferber, A.; Bakke, K. A. H.; Tschudi, J.

    2014-12-01

    Raman based gas sensing can be attractive in several industrial applications, due to its multi-gas sensing capabilities and its ability to detect O_2 and N_2. In this article, we have built a Raman gas probe, based on low-cost components, which has shown an estimated detection limit of 0.5 % for 30 second measurements of N_2 and O_2. While this detection limit is higher than that of commercially available equipment, our estimated component cost is approximately one tenth of the price of commercially available equipment. The use of a resonant Fabry-Pérot cavity increases the scattered signal, and hence the sensitivity, by a factor of 50. The cavity is kept in resonance using a piezo-actuated mirror and a photodiode in a feedback loop. The system described in this article was made with minimum-cost components to demonstrate the low-cost principle. However, it is possible to decrease the detection limit using a higher-powered (but still low-cost) laser and improving the collection optics. By applying these improvements, the detection limit and estimated measurement precision will be sufficient for e.g. the monitoring of input gases in combustion processes, such as e.g. (bio-)gas power plants. In these processes, knowledge about gas compositions with 0.1 % (absolute) precision can help regulate and optimize process conditions. The system has the potential to provide a low-cost, industrial Raman sensor that is optimized for specific gas-detection applications.

  18. [Determination of pesticide residues in fugu, eel and prawn using gas chromatography-mass spectrometry with gel permeation chromatographic clean-up].

    Science.gov (United States)

    Zheng, Feng; Pang, Guofang; Li, Yan; Wang, Minglin; Fan, Chunlin

    2009-09-01

    A multiresidue analytical method was developed for the determination of 191 pesticides in fugu, eel and prawn using gas chromatography-mass spectrometry (GC-MS). The samples were extracted with ethyl acetate and cyclohexane (1:1, v/v), and cleaned-up by gel permeation chromatography (GPC). The GPC eluant collected from 26 min to 44 min was concentrated to 1 mL, then analyzed using GC-MS. A DB-1701 column was used for the separation. The MS detection was performed in selected ion monitoring mode. The recoveries were determined at the two spiked levels of I LOQ and 4 LOQ (LOQ: limit of quantification). The overall recoveries were from 50.2% to 120%, and in which the recoveries of 89.5% pesticides were from 70% to 120%. The relative standard deviations (RSDs) of the recoveries were from 0.6% to 21.6%. The calibration curves of all pesticides showed good linearities in the respective ranges with the correlation coefficient above 0.97. The limits of detection and the limits of quantification were 0.002-0.3 mg/kg and 0.007-1.2 mg/kg, respectively. The sensitivity and accuracy of the method met the requirements of the multiple pesticide residues. This method was applicable to determine 191 multiple pesticide residues in fugu, eel, prawn and other fishes.

  19. Liquid chromatographic extraction medium

    Science.gov (United States)

    Horwitz, E. Philip; Dietz, Mark L.

    1994-01-01

    A method and apparatus for extracting strontium and technetium values from biological, industrial and environmental sample solutions using a chromatographic column is described. An extractant medium for the column is prepared by generating a solution of a diluent containing a Crown ether and dispersing the solution on a resin substrate material. The sample solution is highly acidic and is introduced directed to the chromatographic column and strontium or technetium is eluted using deionized water.

  20. Establishment of analysis method for methane detection by gas chromatography

    Science.gov (United States)

    Liu, Xinyuan; Yang, Jie; Ye, Tianyi; Han, Zeyu

    2018-02-01

    The study focused on the establishment of analysis method for methane determination by gas chromatography. Methane was detected by hydrogen flame ionization detector, and the quantitative relationship was determined by working curve of y=2041.2x+2187 with correlation coefficient of 0.9979. The relative standard deviation of 2.60-6.33% and the recovery rate of 96.36%∼105.89% were obtained during the parallel determination of standard gas. This method was not quite suitable for biogas content analysis because methane content in biogas would be over the measurement range in this method.

  1. Neutron detection by scintillation of noble-gas excimers

    Science.gov (United States)

    McComb, Jacob Collin

    Neutron detection is a technique essential to homeland security, nuclear reactor instrumentation, neutron diffraction science, oil-well logging, particle physics and radiation safety. The current shortage of helium-3, the neutron absorber used in most gas-filled proportional counters, has created a strong incentive to develop alternate methods of neutron detection. Excimer-based neutron detection (END) provides an alternative with many attractive properties. Like proportional counters, END relies on the conversion of a neutron into energetic charged particles, through an exothermic capture reaction with a neutron absorbing nucleus (10B, 6Li, 3He). As charged particles from these reactions lose energy in a surrounding gas, they cause electron excitation and ionization. Whereas most gas-filled detectors collect ionized charge to form a signal, END depends on the formation of diatomic noble-gas excimers (Ar*2, Kr*2,Xe* 2) . Upon decaying, excimers emit far-ultraviolet (FUV) photons, which may be collected by a photomultiplier tube or other photon detector. This phenomenon provides a means of neutron detection with a number of advantages over traditional methods. This thesis investigates excimer scintillation yield from the heavy noble gases following the boron-neutron capture reaction in 10B thin-film targets. Additionally, the thesis examines noble-gas excimer lifetimes with relationship to gas type and gas pressure. Experimental data were collected both at the National Institute of Standards and Technology (NIST) Center for Neutron Research, and on a newly developed neutron beamline at the Maryland University Training Reactor. The components of the experiment were calibrated at NIST and the University of Maryland, using FUV synchrotron radiation, neutron imaging, and foil activation techniques, among others. Computer modeling was employed to simulate charged-particle transport and excimer photon emission within the experimental apparatus. The observed excimer

  2. Fuel leak detection apparatus for gas cooled nuclear reactors

    Science.gov (United States)

    Burnette, Richard D.

    1977-01-01

    Apparatus is disclosed for detecting nuclear fuel leaks within nuclear power system reactors, such as high temperature gas cooled reactors. The apparatus includes a probe assembly that is inserted into the high temperature reactor coolant gaseous stream. The probe has an aperture adapted to communicate gaseous fluid between its inside and outside surfaces and also contains an inner tube for sampling gaseous fluid present near the aperture. A high pressure supply of noncontaminated gas is provided to selectively balance the pressure of the stream being sampled to prevent gas from entering the probe through the aperture. The apparatus includes valves that are operable to cause various directional flows and pressures, which valves are located outside of the reactor walls to permit maintenance work and the like to be performed without shutting down the reactor.

  3. Combination of electromembrane extraction with dispersive liquid-liquid microextraction followed by gas chromatographic analysis as a fast and sensitive technique for determination of tricyclic antidepressants.

    Science.gov (United States)

    Seidi, Shahram; Yamini, Yadollah; Rezazadeh, Maryam

    2013-01-15

    For the first time, combination of electromembrane extraction (EME) and dispersive liquid-liquid microextraction (DLLME) followed by gas chromatography-flame ionization detection (GC/FID) was developed for determination of tricyclic antidepressants (TCAs) in untreated human plasma and urine samples. Response surface methodology (RSM) was used for optimization of experimental parameters, so that extraction time of 14min, voltage of 240V, donor phase of 64mM HCl and acceptor phase of 100mM HCl were obtained as optimal extraction conditions. Matrix effect and carry-over were investigated in this work. The results indicated matrix effect for urine and plasma samples in comparison with neat solutions, so match matrix method was used for drawing working calibration curves. However, no carry-over was appeared at the retention time of investigated TCAs (S/N86.5%. The results showed that EME-DLLME-GC/FID is a promising combination for analysis of TCAs present at low concentrations in biological matrices. Copyright © 2012 Elsevier B.V. All rights reserved.

  4. Development of the infrared instrument for gas detection

    Science.gov (United States)

    Chen, Ching-Wei; Chen, Chia-Ray

    2017-08-01

    MWIR (Mid-Wave Infrared) spectroscopy shows a large potential in the current IR devices market, due to its multiple applications, such as gas detection, chemical analysis, industrial monitoring, combustion and flame characterization. It opens this technique to the fields of application, such as industrial monitoring and control, agriculture and environmental monitoring. However, a major barrier, which is the lack of affordable specific key elements such a MWIR light sources and low cost uncooled detectors, have held it back from its widespread use. In this paper an uncooled MWIR detector combined with image enhancement technique is reported. This investigation shows good results in gas leakage detection test. It also verify the functions of self-developed MWIR lens and optics. A good agreement in theoretical design and experiment give us the lessons learned for the potential application in infrared satellite technology. A brief discussions will also be presented in this paper.

  5. Gas leak detection in infrared video with background modeling

    Science.gov (United States)

    Zeng, Xiaoxia; Huang, Likun

    2018-03-01

    Background modeling plays an important role in the task of gas detection based on infrared video. VIBE algorithm is a widely used background modeling algorithm in recent years. However, the processing speed of the VIBE algorithm sometimes cannot meet the requirements of some real time detection applications. Therefore, based on the traditional VIBE algorithm, we propose a fast prospect model and optimize the results by combining the connected domain algorithm and the nine-spaces algorithm in the following processing steps. Experiments show the effectiveness of the proposed method.

  6. Capacitive micromachined ultrasonic resonator for ultra sensitive trace gas detection

    Science.gov (United States)

    Ge, Li-Feng

    2013-01-01

    The ultra-sensitive trace gas detection has become increasingly important due to the demand for environment and sci-tech progress. In recent years a capacitive micromachined ultrasonic transducer (CMUT) with circular diaphragms used for imaging has been successfully used to detect chemical gases, and shows promising results. However, its behavior is the same as that of CMUTs for ranging, imaging and therapy applications, where the acoustic radiation with a certain power, produced by the vibration of circular diaphragms operating at the first bending mode, is required but is undesirable for gas sensing since it disturbs inevitably the environment to be measured. This paper, therefore, presents to optimize its behavior after an ideal capacitive micromachined ultrasonic resonator (CMUR) and then to utilize second-order and high-order bending modes of the circular diaphragm to minimize its acoustic radiation and obtain higher resonance frequency also. Since the resonance frequencies of high-order modes much higher than the fundamental frequency, an ultra-high operating frequency of GHz can be reached so that raising greatly the sensitivity of the CMUR and being able to realize the ultra-sensitive trace gas detections.

  7. Quantitative Analysis of Humectants in Tobacco Products Using Gas Chromatography (GC with Simultaneous Mass Spectrometry (MSD and Flame Ionization Detection (FID

    Directory of Open Access Journals (Sweden)

    Rainey CL

    2014-12-01

    Full Text Available This paper describes the modification of an existing gas chromatographic (GC method to incorporate simultaneous mass spectrometric (MSD and flame ionization detection (FID into the analysis of tobacco humectants. Glycerol, propylene glycol, and triethylene glycol were analyzed in tobacco labeled as roll-your-own (RYO, cigar, cigarette, moist snuff, and hookah tobacco. Tobacco was extracted in methanol containing 1,3-butanediol (internal standard, filtered, and separated on a 15 m megabore DB-Wax column. Post-column flow was distributed using a microfluidic splitter between the MSD and FID for simultaneous detection. The limits of detection for the FID detector were 0.5 μg/mL (propylene glycol and triethylene glycol and 0.25 μg/mL (glycerol with a linear range of 2-2000 μg/mL (propylene glycol and triethylene glycol and 1-4000 μg/mL (glycerol. The limits of detection for the MSD detector were 2 μg/mL (propylene glycol and triethylene glycol and 4 μg/mL (glycerol with a linear range of 20-2000 μg/mL (propylene glycol and triethylene glycol and 40-4000 μg/mL (glycerol. Significant improvement in the sensitivity of the MSD can be achieved by employing selective ion monitoring (SIM detection mode. Although a high degree of correlation was observed between the results from FID and MSD analyses, marginal chromatographic resolution between glycerol and triethylene glycol limits the applicability of FID to samples containing low levels of both of these humectants. Utilizing MSD greatly improves the reliability of quantitative results because compensation for inadequate chromatographic resolution can be accomplished with mass selectivity in detection.

  8. Gas detection by means of surface plasmon resonance enhanced ellipsometry

    Energy Technology Data Exchange (ETDEWEB)

    Nooke, Alida

    2012-11-01

    This thesis investigated gas sensing by means of surface plasmon resonance enhanced ellipsometry. Surface plasmons were excited in a 40 - 50 nm gold layer by a He-Ne-laser using the Kretschmann configuration, which was arranged on a self-made copper measuring cell. A fixed angle of incidence and the ellipsometric parameter {Delta} as the measured value were used to monitor changes in the gas phase. Different types of gases were investigated: flammable (hydrocarbons and hydrogen), oxidising (oxygen and ozone), toxic (carbon monoxide) and inert (helium and nitrogen). The gas types can be distinguished by their refractive indices, whereas the sensor responds instantly relative to the reference gas with an increase or a decrease in {Delta}. Diluting the analyte gas with a reference gas (nitrogen or air) allowed the detection limits to be determined, these lay in the low % range. The sensor stability was also enhanced as well as the sensitivity by modifying the gold layers with a 3-10 nm additional layer. These additional layers consisted of the inorganic materials TiO{sub 2}, ZrO{sub 2}, MgF{sub 2} and Fe: SnO{sub 2} which were deposited by different coating processes. Surface investigations were made of every utilised layer: scanning electron microscope and atomic force microscope measurements for surface topology and spectroscopic ellipsometry mapping to determine the optical constants and the layer thicknesses. All applied materials protected the gold layer from contaminations and thus prolonged the life span of the sensor. Furthermore, the detection limits were reduced significantly, to the low ppm range. The material Fe: SnO{sub 2} demonstrates a special behaviour in reaction with the toxic gas carbon monoxide: Due to the iron doping, the response to carbon monoxide is extraordinary and concentrations below 1 ppm were detected. In order to approach a future application in industry, the sensor system was adapted to a stainless steel tube. With this measuring

  9. An investigation of the matrix sensitivity of refinery gas analysis using gas chromatography with flame ionisation detection.

    Science.gov (United States)

    Ferracci, Valerio; Brown, Andrew S; Harris, Peter M; Brown, Richard J C

    2015-02-27

    The response of a flame ionisation detector (FID) on a gas chromatograph to methane, ethane, propane, i-butane and n-butane in a series of multi-component refinery gas standards was investigated to assess the matrix sensitivity of the instrument. High-accuracy synthetic gas standards, traceable to the International System of Units, were used to minimise uncertainties. The instrument response exhibited a small dependence on the component amount fraction: this behaviour, consistent with that of another FID, was thoroughly characterised over a wide range of component amount fractions and was shown to introduce a negligible bias in the analysis of refinery gas samples, provided a suitable reference standard is employed. No significant effects of the molar volume, density and viscosity of the gas mixtures on the instrument response were observed, indicating that the FID is suitable for the analysis of refinery gas mixtures over a wide range of component amount fractions provided that appropriate drift-correction procedures are employed. Copyright © 2015 Elsevier B.V. All rights reserved.

  10. 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

  11. Chromatographic hydrogen isotope separation

    Science.gov (United States)

    Aldridge, F.T.

    Intermetallic compounds with the CaCu/sub 5/ type of crystal structure, particularly LaNiCo/sub 4/ and CaNi/sub 5/, exhibit high separation factors and fast equilibrium times and therefore are useful for packing a chromatographic hydrogen isotope separation column. The addition of an inert metal to dilute the hydride improves performance of the column. A large scale multi-stage chromatographic separation process run as a secondary process off a hydrogen feedstream from an industrial plant which uses large volumes of hydrogen cn produce large quantities of heavy water at an effective cost for use in heavy water reactors.

  12. Gas chromatographic determination and mechanism of formation of D-amino acids occurring in fermented and roasted cocoa beans, cocoa powder, chocolate and cocoa shell.

    Science.gov (United States)

    Pätzold, R; Brückner, H

    2006-07-01

    Fermented cocoa beans of various countries of origin (Ivory Coast, Ghana, Sulawesi), cocoa beans roasted under defined conditions (100-150 degrees C; 30-120 min), low and high fat cocoa powder, various brands of chocolate, and cocoa shells were analyzed for their contents of free L-and D-amino acids. Amino acids were isolated from defatted products using a cation exchanger and converted into volatile N(O)-pentafluoropropionyl amino acid 2-propyl esters which were analyzed by enantioselective gas chromatography mass spectrometry on a Chirasil-L-Val capillary column. Besides common protein L-amino acids low amounts of D-amino acids were detected in fermented cocoa beans. Quantities of D-amino acids increased on heating. On roasting cocoa beans of the Forastero type from the Ivory Coast at 150 degrees C for 2 h, relative quantities of D-amino acids approached 17.0% D-Ala, 11.7% D-Ile, 11.1% D-Asx (Asp + Asn), 7.9% D-Tyr, 5.8% D-Ser, 4.8% D-Leu, 4.3% D-Phe, 37.0% D-Pro, and 1.2% D-Val. In cocoa powder and chocolate relative quantities amounted to 14.5% D-Ala, 10.6% D-Tyr, 9.8% D-Phe, 8.1% L-Asx, and 7.2% D-Ile. Lower quantities of other D-amino acids were also detected. In order to corroborate our hypothesis that D-amino acids are generated from Amadori compounds (fructose amino acids) formed in the course of the Maillard reaction, fructose-L-phenylalanine and fructose-D-phenylalanine were synthesized and heated at 200 degrees C for 5-60 min. Already after 5 min release of 11.7% D-Phe and 11.8% L-Phe in the free form could be analyzed. Based on the data a racemization mechanism is presented founded on the intermediate and reversible formation of an amino acid carbanion in the Amadori compounds.

  13. Liquid metal-to-gas leak-detection instruments

    International Nuclear Information System (INIS)

    Matlin, E.; Witherspoon, J.E.; Johnson, J.L.

    1982-01-01

    It is desirable for liquid-metal-cooled reactors that small liquid metal-to-gas leaks be reliably detected. Testing has been performed on a number of detection systems to evaluate their sensitivity, response time, and performance characteristics. This testing has been scheduled in three phases. The first phase was aimed at screening out the least suitable detectors and optimizing the performance of the most promising. In the second phase, candidates were tested in a 1500 ft 3 walk-in type enclosure in which leaks were simulated on 24-in. and 3-in. piping. In the third phase of testing, selected type detectors were tested in the 1500-ft 3 enclosure with Clinch River Breeder Reactor Plant (CRBRP) pipe insulation configurations and detector tubing configuration with cell gas recirculation simulated. Endurance testing of detection equipment was also performed as part of this effort. Test results have been shown that aerosol-type detectors will reliably detect leaks as small as a few grams per hour when sampling pipe insulation annuli

  14. Development of a transportable gas analyzer: thermal desorber / micro gas chromatograph / mass spectrometer coupling (m-TD / m-GC / MS). Application to on-line analysis of volatile organic compounds at traces level; Developpement d'un analyseur de gaz transportable: couplage thermodesorbeur / micro-chromatographe / spectrometre de masse (m-TD / m-CG / SM). Application a l'analyse en ligne des composes organiques volatils a l'etat de traces

    Energy Technology Data Exchange (ETDEWEB)

    Cozic, R.

    2004-06-01

    Volatile organic compounds (VOC) play a central part in the photochemical pollution of the atmosphere. Monitoring of these products in air became a need, because of their toxicity. Currently, traditional analytical methods of air have drawbacks. Instruments are too specific or the technique consists in trapping pollutants and then to turn over the sample to the laboratory for analysis. The subject of the thesis is the development of an on-site analytical technique, offering new prospects for air analysis. The developed transportable analyzer results from the coupling of a thermal desorber (m-TD), a micro gas chromatograph (m-GC) and a mass spectrometer (MS). The instrument makes it possible, in a few minutes, to perform qualitative and quantitative analysis of a very broad range of VOC at traces level. An example of on-site application of the analyzer relates to the monitoring of working atmospheres. (author)

  15. 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.)

  16. Carbon nanotubes for gas detection: materials preparation and device assembly

    International Nuclear Information System (INIS)

    Terranova, M L; Lucci, M; Orlanducci, S; Tamburri, E; Sessa, V; Reale, A; Carlo, A Di

    2007-01-01

    An efficient sensing device for NH 3 and NO x detection has been realized using ordered arrays of single-walled C nanotubes deposited onto an interdigitated electrode platform operating at room temperature. The sensing material has been prepared using several chemical-physical techniques for purification and positioning of the nanotubes inside the electrode gaps. In particular, both DC and AC fields have been applied in order to move and to align the nanostructures by electrophoresis and dielectrophoresis processes. We investigated the effects of different voltages applied to a gate contact on the back side of the substrate on the performances of the device and found that for different gas species (NH 3 , NO x ) a constant gate bias increases the sensitivity for gas detection. Moreover, in this paper we demonstrate that a pulsed bias applied to the gate contact facilitates the gas interaction with the nanotubes, either reducing the absorption times or accelerating the desorption times, thus providing a fast acceleration and a dramatic improvement of the time dependent behaviour of the device

  17. MICROSCOPIC, PHYSICOCHEMICAL AND CHROMATOGRAPHIC ...

    African Journals Online (AJOL)

    Peters

    MICROSCOPIC, PHYSICOCHEMICAL AND CHROMATOGRAPHIC. FINGERPRINTS OF LEAVES OF NIGERIAN CASSIA TORA LINN. Fatokun Omolola T1*., EsievoKevwe B2., Ugbabe Grace E3. and Kunle Oluyemisi F4. Department of Medicinal Plant Research and Traditional Medicine, National Institute for.

  18. CHROMATOGRAPHIC SEPARATION AND SPECTRO ...

    African Journals Online (AJOL)

    The spectro-analytical techniques used for characterization included energy dispersive X-ray fluorescence (EDXRF), X-ray diffractometry (XRD), Optical microscopy, infrared (IR) and UV-VIS spectroscopy. Four different fractions having colours yellow, grey, orange and purple were obtained from the chromatographic ...

  19. Detection of individual gas molecules adsorbed on graphene.

    Science.gov (United States)

    Schedin, F; Geim, A K; Morozov, S V; Hill, E W; Blake, P; Katsnelson, M I; Novoselov, K S

    2007-09-01

    The ultimate aim of any detection method is to achieve such a level of sensitivity that individual quanta of a measured entity can be resolved. In the case of chemical sensors, the quantum is one atom or molecule. Such resolution has so far been beyond the reach of any detection technique, including solid-state gas sensors hailed for their exceptional sensitivity. The fundamental reason limiting the resolution of such sensors is fluctuations due to thermal motion of charges and defects, which lead to intrinsic noise exceeding the sought-after signal from individual molecules, usually by many orders of magnitude. Here, we show that micrometre-size sensors made from graphene are capable of detecting individual events when a gas molecule attaches to or detaches from graphene's surface. The adsorbed molecules change the local carrier concentration in graphene one by one electron, which leads to step-like changes in resistance. The achieved sensitivity is due to the fact that graphene is an exceptionally low-noise material electronically, which makes it a promising candidate not only for chemical detectors but also for other applications where local probes sensitive to external charge, magnetic field or mechanical strain are required.

  20. Naturally fractured tight gas reservoir detection optimization. Final report

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1997-11-19

    This DOE-funded research into seismic detection of natural fractures is one of six projects within the DOE`s Detection and Analysis of Naturally Fractured Gas Reservoirs Program, a multidisciplinary research initiative to develop technology for prediction, detection, and mapping of naturally fractured gas reservoirs. The demonstration of successful seismic techniques to locate subsurface zones of high fracture density and to guide drilling orientation for enhanced fracture permeability will enable better returns on investments in the development of the vast gas reserves held in tight formations beneath the Rocky Mountains. The seismic techniques used in this project were designed to capture the azimuthal anisotropy within the seismic response. This seismic anisotropy is the result of the symmetry in the rock fabric created by aligned fractures and/or unequal horizontal stresses. These results may be compared and related to other lines of evidence to provide cross-validation. The authors undertook investigations along the following lines: Characterization of the seismic anisotropy in three-dimensional, P-wave seismic data; Characterization of the seismic anisotropy in a nine-component (P- and S-sources, three-component receivers) vertical seismic profile; Characterization of the seismic anisotropy in three-dimensional, P-to-S converted wave seismic data (P-wave source, three-component receivers); and Description of geological and reservoir-engineering data that corroborate the anisotropy: natural fractures observed at the target level and at the surface, estimation of the maximum horizontal stress in situ, and examination of the flow characteristics of the reservoir.

  1. Dual-gas tracers for subsurface characterization and NAPL detection

    International Nuclear Information System (INIS)

    Gauglitz, P.A.; Peurrung, L.M.; Mendoza, D.P.; Pillay, G.

    1994-11-01

    Effective design of in situ remediation technologies often requires an understanding of the mass transfer limitations that control the removal of contaminants from the soil. In addition, the presence of nonaqueous phase liquids (NAPLs) in soils will affect the ultimate success or failure of remediation processes. Knowing the location of NAPLs within the subsurface is critical to designing the most effective remediation approach. This work focuses on demonstrating that gas tracers can detect the location of the NAPLs in the subsurface and elucidating the mass transfer limitations associated with the removal of contaminants from soils

  2. Wireless gas detection with a smartphone via rf communication.

    Science.gov (United States)

    Azzarelli, Joseph M; Mirica, Katherine A; Ravnsbæk, Jens B; Swager, Timothy M

    2014-12-23

    Chemical sensing is of critical importance to human health, safety, and security, yet it is not broadly implemented because existing sensors often require trained personnel, expensive and bulky equipment, and have large power requirements. This study reports the development of a smartphone-based sensing strategy that employs chemiresponsive nanomaterials integrated into the circuitry of commercial near-field communication tags to achieve non-line-of-sight, portable, and inexpensive detection and discrimination of gas-phase chemicals (e.g., ammonia, hydrogen peroxide, cyclohexanone, and water) at part-per-thousand and part-per-million concentrations.

  3. High performance liquid chromatographic determination of ...

    African Journals Online (AJOL)

    STORAGESEVER

    2010-02-08

    Feb 8, 2010 ... liquid chromatographic with UV/Fluorescence detection is described. Proguanil was derivatised to its corresponding ... proguanil in combination with other antimalarial drugs has also been reported to posses synergic toxicity ..... Chlorophenyl Biguanide in Biological Fluids. Afr. J. Biotechnol. 4(8):. 856-861.

  4. 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.

  5. Comparing Natural Gas Leakage Detection Technologies Using an Open-Source "Virtual Gas Field" Simulator.

    Science.gov (United States)

    Kemp, Chandler E; Ravikumar, Arvind P; Brandt, Adam R

    2016-04-19

    We present a tool for modeling the performance of methane leak detection and repair programs that can be used to evaluate the effectiveness of detection technologies and proposed mitigation policies. The tool uses a two-state Markov model to simulate the evolution of methane leakage from an artificial natural gas field. Leaks are created stochastically, drawing from the current understanding of the frequency and size distributions at production facilities. Various leak detection and repair programs can be simulated to determine the rate at which each would identify and repair leaks. Integrating the methane leakage over time enables a meaningful comparison between technologies, using both economic and environmental metrics. We simulate four existing or proposed detection technologies: flame ionization detection, manual infrared camera, automated infrared drone, and distributed detectors. Comparing these four technologies, we found that over 80% of simulated leakage could be mitigated with a positive net present value, although the maximum benefit is realized by selectively targeting larger leaks. Our results show that low-cost leak detection programs can rely on high-cost technology, as long as it is applied in a way that allows for rapid detection of large leaks. Any strategy to reduce leakage should require a careful consideration of the differences between low-cost technologies and low-cost programs.

  6. Resonant optical transducers for in-situ gas detection

    Science.gov (United States)

    Bond, Tiziana C; Cole, Garrett; Goddard, Lynford

    2016-06-28

    Configurations for in-situ gas detection are provided, and include miniaturized photonic devices, low-optical-loss, guided-wave structures and state-selective adsorption coatings. High quality factor semiconductor resonators have been demonstrated in different configurations, such as micro-disks, micro-rings, micro-toroids, and photonic crystals with the properties of very narrow NIR transmission bands and sensitivity up to 10.sup.-9 (change in complex refractive index). The devices are therefore highly sensitive to changes in optical properties to the device parameters and can be tunable to the absorption of the chemical species of interest. Appropriate coatings applied to the device enhance state-specific molecular detection.

  7. Resonant optical transducers for in-situ gas detection

    Energy Technology Data Exchange (ETDEWEB)

    Bond, Tiziana C.; Cole, Garrett; Goddard, Lynford

    2018-01-30

    Configurations for in-situ gas detection are provided, and include miniaturized photonic devices, low-optical-loss, guided-wave structures and state-selective adsorption coatings. High quality factor semiconductor resonators have been demonstrated in different configurations, such as micro-disks, micro-rings, micro-toroids, and photonic crystals with the properties of very narrow NIR transmission bands and sensitivity up to 10.sup.-9 (change in complex refractive index). The devices are therefore highly sensitive to changes in optical properties to the device parameters and can be tunable to the absorption of the chemical species of interest. Appropriate coatings applied to the device enhance state-specific molecular detection.

  8. Development of failure detection system for gas-cooled reactor

    International Nuclear Information System (INIS)

    Feirreira, M.P.

    1990-01-01

    This work presents several kinds of Failure Detection Systems for Fuel Elements, stressing their functional principles and major applications. A comparative study indicates that the method of electrostatic precipitation of the fission gases Kr and Xe is the most efficient for fuel failure detection in gas-cooled reactors. A detailed study of the physical phenomena involved in electrostatic precipitation led to the derivation of an equation for the measured counting rate. The emission of fission products from the fuel and the ion recombination inside the chamber are evaluated. A computer program, developed to simulate the complete operation of the system, relates the counting rate to the concentration of Kr and Xe isotopes. The project of a mock-up is then presented. Finally, the program calculations are compared to experimental data, available from the literature, yielding a close agreement. (author)

  9. Trans fat labeling and levels in U.S. foods: assessment of gas chromatographic and infrared spectroscopic techniques for regulatory compliance.

    Science.gov (United States)

    Mossoba, Magdi M; Moss, Julie; Kramer, John K G

    2009-01-01

    Trans fatty acids are found in a variety of foods like dairy and meat products, but the major dietary sources are products that contain commercially hydrogenated fats. There has been a renewed need for accurate analytical methods for the quantitation of total trans fat since mandatory requirements to declare the amount of trans fat present in food products and dietary supplements were issued in many countries. Official capillary GC and IR methodologies are the two most common validated methods used to identify and quantify trans fatty acids for regulatory compliance. The present article provides a comprehensive discussion of the GC and IR techniques, including the latest attenuated total reflection (ATR)-FTIR methodology called the negative second derivative ATR-FTIR procedure, which is currently being validated in an international collaborative study. The identification and quantitation of trans fatty acid isomers by GC is reviewed and an alternative GC method is proposed using two temperature programs and combining their results; this proposed method deals more effectively with the resolution of large numbers of geometric and positional monoene, diene, and triene fatty acid isomers present in ruminant fats. In addition, the different methylation procedures that affect quantitative conversion to fatty acid methyl esters are reviewed. There is also a lack of commercial chromatographic standards for many trans fatty acid isomers. This review points to potential sources of interferences in the FTIR determination that may lead to inaccurate results, particularly at low trans levels. The presence of high levels of saturated fats may lead to interferences in the FTIR spectra observed for trans triacylglycerols (TAGs). TAGs require no derivatization, but have to be melted prior to IR measurement. While GC is currently the method of choice, ATR-FTIR spectroscopy is a viable, rapid alternative, and a complementary method to GC for a more rapid determination of total trans

  10. Enhancement of drug detection and identification by use of various derivatizing reagents on GC-FTIR analysis.

    Science.gov (United States)

    1992-07-01

    Phenylpropanolamine (PPA) is a relatively common non-prescription sympathomimetic amine. As such, it is frequently detected during forensic analysis. The presence of phenylpropanolamine can be confirmed by using Gas Chromatograph-Fourier Transform In...

  11. High Altitude Aerial Natural Gas Leak Detection System

    Energy Technology Data Exchange (ETDEWEB)

    Richard T. Wainner; Mickey B. Frish; B. David Green; Matthew C. Laderer; Mark G. Allen; Joseph R. Morency

    2006-12-31

    The objective of this program was to develop and demonstrate a cost-effective and power-efficient advanced standoff sensing technology able to detect and quantify, from a high-altitude (> 10,000 ft) aircraft, natural gas leaking from a high-pressure pipeline. The advanced technology is based on an enhanced version of the Remote Methane Leak Detector (RMLD) platform developed previously by Physical Sciences Inc. (PSI). The RMLD combines a telecommunications-style diode laser, fiber-optic components, and low-cost DSP electronics with the well-understood principles of Wavelength Modulation Spectroscopy (WMS), to indicate the presence of natural gas located between the operator and a topographic target. The transceiver transmits a laser beam onto a topographic target and receives some of the laser light reflected by the target. The controller processes the received light signal to deduce the amount of methane in the laser's path. For use in the airborne platform, we modified three aspects of the RMLD, by: (1) inserting an Erbium-doped optical fiber laser amplifier to increase the transmitted laser power from 10 mW to 5W; (2) increasing the optical receiver diameter from 10 cm to 25 cm; and (3) altering the laser wavelength from 1653 nm to 1618 nm. The modified RMLD system provides a path-integrated methane concentration sensitivity {approx}5000 ppm-m, sufficient to detect the presence of a leak from a high capacity transmission line while discriminating against attenuation by ambient methane. In ground-based simulations of the aerial leak detection scenario, we demonstrated the ability to measure methane leaks within the laser beam path when it illuminates a topographic target 2000 m away. We also demonstrated simulated leak detection from ranges of 200 m using the 25 cm optical receiver without the fiber amplifier.

  12. 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.

  13. 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.

  14. Determination of Low Concentrations of Acetochlor in Water by Automated Solid-Phase Extraction and Gas Chromatography with Mass-Selective Detection

    Science.gov (United States)

    Lindley, C.E.; Stewart, J.T.; Sandstrom, M.W.

    1996-01-01

    A sensitive and reliable gas chromatographic/mass spectrometric (GC/MS) method for determining acetochlor in environmental water samples was developed. The method involves automated extraction of the herbicide from a filtered 1 L water sample through a C18 solid-phase extraction column, elution from the column with hexane-isopropyl alcohol (3 + 1), and concentration of the extract with nitrogen gas. The herbicide is quantitated by capillary/column GC/MS with selected-ion monitoring of 3 characteristic ions. The single-operator method detection limit for reagent water samples is 0.0015 ??g/L. Mean recoveries ranged from about 92 to 115% for 3 water matrixes fortified at 0.05 and 0.5 ??g/L. Average single-operator precision, over the course of 1 week, was better than 5%.

  15. Smooth esterification of Di-and Tricarboxylic acids with methyl and ethyl chloroformates in gas chromatographic profiling of urinary acidic metabolites

    Czech Academy of Sciences Publication Activity Database

    Hušek, Petr; Šimek, Petr; Matucha, P.

    2003-01-01

    Roč. 58, - (2003), s. 623-630 ISSN 0009-5893 R&D Projects: GA AV ČR IPP1050128; GA ČR GA203/01/1586 Institutional research plan: CEZ:AV0Z5007907 Keywords : gas chromatography * esterification with chloroformates Subject RIV: CC - Organic Chemistry Impact factor: 1.145, year: 2003

  16. 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

  17. Evaluation of liquid chromatographic behavior of lumazinic derivatives, from α-dicarbonyl compounds, in different C18 columns: application to wine samples using a fused-core column and fluorescence detection.

    Science.gov (United States)

    Hurtado-Sánchez, María del Carmen; Espinosa-Mansilla, Anunciación; Rodríguez-Cáceres, María Isabel; Durán-Merás, Isabel

    2014-01-08

    Several C18 columns, packed with totally porous particles of different sizes and shell thicknesses, have been compared for simultaneous determination of α-dicarbonyl compounds, previous derivatization to lumazinic derivatives. Chromatographic conditions for the separation have been optimized for each column, and chromatographic parameters have been calculated and exhaustively compared. A core-shell C18 column provided the best results, and a HPLC method with fluorimetric detection has been proposed. The developed method has been validated in terms of linearity, precision, and sensitivity. Detection and quantification limits obtained were comprised between 0.02 and 0.30 and 0.07 and 1.0 ng mL(-1), respectively, while RSD values obtained were lower than 6% and 5% in intraday and interday repeatability studies, respectively. The method has been applied to analysis of the α-dicarbonyl compounds in different types of wines. The higher levels of the total α-dicarbonyl compounds were found in sweet wines and the lower levels in white wines.

  18. First detection of hydrogen in the β Pictoris gas disk

    Science.gov (United States)

    Wilson, P. A.; Lecavelier des Etangs, A.; Vidal-Madjar, A.; Bourrier, V.; Hébrard, G.; Kiefer, F.; Beust, H.; Ferlet, R.; Lagrange, A.-M.

    2017-03-01

    The young and nearby star β Pictoris (β Pic) is surrounded by a debris disk composed of dust and gas known to host a myriad evaporating exocomets, planetesimals and at least one planet. At an edge-on inclination, as seen from Earth, this system is ideal for debris disk studies providing an excellent opportunity to use absorption spectroscopy to study the planet forming environment. Using the Cosmic Origins Spectrograph (COS) instrument on the Hubble Space Telescope (HST) we observe the most abundant element in the disk, hydrogen, through the H I Lyman α (Ly-α) line. We present a new technique to decrease the contamination of the Ly-α line by geocoronal airglow in COS spectra. This Airglow Virtual Motion (AVM) technique allows us to shift the Ly-α line of the astrophysical target away from the contaminating airglow emission revealing more of the astrophysical line profile. This new AVM technique, together with subtraction of an airglow emission map, allows us to analyse the shape of the β Pic Ly-α emission line profile and from it, calculate the column density of neutral hydrogen surrounding β Pic. The column density of hydrogen in the β Pic stable gas disk at the stellar radial velocity is measured to be log (NH/ 1 cm2) ≪ 18.5. The Ly-α emission line profile is found to be asymmetric and we propose that this is caused by H I falling in towards the star with a bulk radial velocity of 41 ± 6 km s-1 relative to β Pic and a column density of log (NH/ 1 cm2) = 18.6 ± 0.1. The high column density of hydrogen relative to the hydrogen content of CI chondrite meteorites indicates that the bulk of the hydrogen gas does not come from the dust in the disk. This column density reveals a hydrogen abundance much lower than solar, which excludes the possibility that the detected hydrogen could be a remnant of the protoplanetary disk or gas expelled by the star. We hypothesise that the hydrogen gas observed falling towards the star arises from the dissociation of

  19. Quantum-cascade laser photoacoustic detection of methane emitted from natural gas powered engines

    Science.gov (United States)

    Rocha, M. V.; Sthel, M. S.; Silva, M. G.; Paiva, L. B.; Pinheiro, F. W.; Miklòs, A.; Vargas, H.

    2012-03-01

    In this work we present a laser photoacoustic arrangement for the detection of the important greenhouse gas methane. A quantum-cascade laser and a differential photoacoustic cell were employed. A detection limit of 45 ppbv in nitrogen was achieved as well as a great selectivity. The same methodology was also tested in the detection of methane issued from natural gas powered vehicles (VNG) in Brazil, which demonstrates the excellent potential of this arrangement for greenhouse gas detection emitted from real sources.

  20. Development of bremsstrahlung detection type tritium gas monitoring system, (1)

    International Nuclear Information System (INIS)

    Bingo, Kazuyoshi; Yoshida, Makoto; Chida, Tohru; Kawasaki, Katsuya

    1982-11-01

    A tritium monitoring system by means of bremsstrahlung detecting was developed. A prototype system consisted of a sampling cylinder, a gas circulating apparatus, an NaI(T1) detector, an amplifier and a multichannel analyzer. The sizes of sampling cylinders used 208 mm phi x 290; 170; 70 mmH, 133 mm phi x 292; 172; 72 mmH and 55 mm phi x 294; 174; 74 mmH, respectively. The sensitivity of prototype system was from 12 to 57 cps/μCi.cm - 3 , depending on the size of sampling cylinder and an efficiency of NaI(T1) detector. When pulses due to breamsstrahlungs with energy from 4 to 17 keV were counted, the minimum detectable concentration of the prototype tritium monitoring system was obtained to be 5.2 x 10 - 3 μCi/cm 3 . It was evaluated that the detectable range of concentration was from 1 x 10 - 2 to 1 x 10 3 μCi/cm 3 . (author)

  1. 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

  2. Miniaturized Hollow-Waveguide Gas Correlation Radiometer (GCR) for Trace Gas Detection in the Martian Atmosphere

    Science.gov (United States)

    Wilson, Emily L.; Georgieva, E. M.; Melroy, H. R.

    2012-01-01

    Gas correlation radiometry (GCR) has been shown to be a sensitive and versatile method for detecting trace gases in Earth's atmosphere. Here, we present a miniaturized and simplified version of this instrument capable of mapping multiple trace gases and identifying active regions on the Mars surface. Reduction of the size and mass of the GCR instrument has been achieved by implementing a lightweight, 1 mm inner diameter hollow-core optical fiber (hollow waveguide) for the gas correlation cell. Based on a comparison with an Earth orbiting CO2 gas correlation instrument, replacement of the 10 meter mUltipass cell with hollow waveguide of equivalent pathlength reduces the cell mass from approx 150 kg to approx 0.5 kg, and reduces the volume from 1.9 m x 1.3 m x 0.86 m to a small bundle of fiber coils approximately I meter in diameter by 0.05 m in height (mass and volume reductions of >99%). This modular instrument technique can be expanded to include measurements of additional species of interest including nitrous oxide (N2O), hydrogen sulfide (H2S), methanol (CH3OH), and sulfur dioxide (SO2), as well as carbon dioxide (CO2) for a simultaneous measure of mass balance.

  3. Microfabricated planar glass gas chromatography with photoionization detection.

    Science.gov (United States)

    Lewis, Alastair C; Hamilton, Jacqueline F; Rhodes, Christopher N; Halliday, Jaydene; Bartle, Keith D; Homewood, Philip; Grenfell, Robin J P; Goody, Brian; Harling, Alice M; Brewer, Paul; Vargha, Gergely; Milton, Martin J T

    2010-01-29

    We report the development of a microfabricated gas chromatography system suitable for the separation of volatile organic compounds (VOCs) and compatible with use as a portable measurement device. Hydrofluoric acid etching of 95x95mm Schott B270 wafers has been used to give symmetrical hemi-spherical channels within a glass substrate. Two matching glass plates were subsequently cold bonded with the channels aligned; the flatness of the glass surfaces resulted in strong bonding through van der Waals forces. The device comprised gas fluidic interconnections, injection zone and 7.5 and 1.4m long, 320microm internal diameter capillaries. Optical microscopy confirmed the capillaries to have fully circular channel profiles. Direct column heating and cooling could be achieved using a combination of resistive heaters and Peltier devices. The low thermal conductivity of glass allowed for multiple uniform temperature zones to be achieved within a single glass chip. Temperature control over the range 10-200 degrees C was achieved with peak power demand of approximately 25W. The 7.5m capillary column was static coated with a 2microm film of non-polar dimethylpolysiloxane stationary phase. A standard FID and a modified lightweight 100mW photoionization detector (PID) were coupled to the column and performance tested with gas mixtures of monoaromatic and monoterpene species at the parts per million concentration level. The low power GC-PID device showed good performance for a small set of VOCs and sub ng detection sensitivity to monoaromatics. Copyright (c) 2009 Elsevier B.V. All rights reserved.

  4. Trace analysis of residual methyl methanesulfonate, ethyl methanesulfonate and isopropyl methanesulfonate in pharmaceuticals by capillary gas chromatography with flame ionization detection.

    Science.gov (United States)

    Li, Weiyong

    2004-08-13

    A capillary gas chromatographic method using flame ionization detection was developed and validated for the trace analysis (ppm level) of methyl methanesulfonate, ethyl methanesulfonate, and isopropyl methanesulfonate in pharmaceutical drug substance. The method utilizes a megabore capillary column with bonded and crosslinked polyethylene glycol stationary phase. A dissolve-and-injection approach was adopted for sample introduction in a splitless mode. The investigated sample solvents include acetonitrile, ethyl acetate, methylene chloride, 1,2-dichloromethane, and toluene. Aqueous mixtures of acetonitrile and water can also be used as sample solvent. A limit of detection of about 1 microg/g (1 ppm) and limit of quantitation of 5 microg/g (5 ppm) were achieved for the mesylate esters in drug substance samples. The method optimization and validation are also discussed in this paper.

  5. Parallel-plate wet denuder coupled ion chromatograph for near-real-time detection of trace acidic gases in clean room air.

    Science.gov (United States)

    Takeuchi, Masaki; Tsunoda, Hiromichi; Tanaka, Hideji; Shiramizu, Yoshimi

    2011-01-01

    This paper describes the performance of our automated acidic (CH(3)COOH, HCOOH, HCl, HNO(2), SO(2), and HNO(3)) gases monitor utilizing a parallel-plate wet denuder (PPWD). The PPWD quantitatively collects gaseous contaminants at a high sample flow rate (∼8 dm(3) min(-1)) compared to the conventional methods used in a clean room. Rapid response to any variability in the sample concentration enables near-real-time monitoring. In the developed monitor, the analyte collected with the PPWD is pumped into one of two preconcentration columns for 15 min, and determined by means of ion chromatography. While one preconcentration column is used for chromatographic separation, the other is used for loading the sample solution. The system allows continuous monitoring of the common acidic gases in an advanced semiconductor manufacturing clean room. 2011 © The Japan Society for Analytical Chemistry

  6. Infrared video based gas leak detection method using modified FAST features

    Science.gov (United States)

    Wang, Min; Hong, Hanyu; Huang, Likun

    2018-03-01

    In order to detect the invisible leaking gas that is usually dangerous and easily leads to fire or explosion in time, many new technologies have arisen in the recent years, among which the infrared video based gas leak detection is widely recognized as a viable tool. However, all the moving regions of a video frame can be detected as leaking gas regions by the existing infrared video based gas leak detection methods, without discriminating the property of each detected region, e.g., a walking person in a video frame may be also detected as gas by the current gas leak detection methods.To solve this problem, we propose a novel infrared video based gas leak detection method in this paper, which is able to effectively suppress strong motion disturbances.Firstly, the Gaussian mixture model(GMM) is used to establish the background model.Then due to the observation that the shapes of gas regions are different from most rigid moving objects, we modify the Features From Accelerated Segment Test (FAST) algorithm and use the modified FAST (mFAST) features to describe each connected component. In view of the fact that the statistical property of the mFAST features extracted from gas regions is different from that of other motion regions, we propose the Pixel-Per-Points (PPP) condition to further select candidate connected components.Experimental results show that the algorithm is able to effectively suppress most strong motion disturbances and achieve real-time leaking gas detection.

  7. Determination of physiological levels of volatile organic compounds in blood using static headspace capillary gas chromatography with serial triple detection.

    Science.gov (United States)

    Schroers, H J; Jermann, E; Begerow, J; Hajimiragha, H; Chiarotti-Omar, A M; Dunemann, L

    1998-04-01

    A static capillary gas chromatographic method using three different detectors [photoionization detector (PID), electron capture detector (ECD) and flame ionization detector (FID)] switched in series is presented for the determination of volatile organic compounds (VOCs) in sub microgram l-1 levels. The method was applied for the analysis of selected environmentally and occupationally relevant non-halogenated and chlorinated aromatic hydrocarbons (e.g., benzene, toluene, xylenes, dichlorobenzenes) as well as chlorinated aliphatic hydrocarbons (e.g., trichloroethene, tetrachloroethene) in blood samples. Detailed investigations, in respect to the figures of merit were carried out. For most of the selected VOCs detection limits (calculated as the three-fold standard deviation of low level calibration standards) in the range from 26 (benzene) to 67 ng l-1 (m/p-xylene) were achieved which are comparable with those reported for dynamic headspace techniques in combination with mass spectrometric detection. For the individual VOCs the within-series precision varied from 4 to 19% and the day-to-day precision from 11 to 28%. Regarding PID as well as FID the calibration graphs for all substances were linear up to at least 10 micrograms l-1 while the ECD response was linear up to concentrations of about 0.6 microgram l-1 for the halogenated compounds. Our method is applicable for the quantitative determination of VOCs in blood in the occupationally as well as in the physiologically relevant (normal) concentration range.

  8. 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)

  9. Trace Detection of Pentaerythritol Tetranitrate Using Electrochemical Gas Sensors

    Directory of Open Access Journals (Sweden)

    Praveen K. Sekhar

    2014-01-01

    Full Text Available Selective and sensitive detection of trace amounts of pentaerythritol tetranitrate (PETN is demonstrated. The screening system is based on a sampling/concentrator front end and electrochemical potentiometric gas sensor as the detector. A single sensor is operated in the dominant hydrocarbon (HC and nitrogen oxides (NOx mode by varying the sensor operating condition. The potentiometric sensor with integrated heaters was used to capture the signature of PETN. Quantitative measurements based on hydrocarbon and nitrogen oxide sensor responses indicated that the detector sensitivity scaled proportionally with the mass of the explosives (10 μg down to 200 ng. The ratio of the HC integrated peak area to the NOx integrated peak area is identified as an indicator of selectivity. The HC/NOx ratio is unique for PETN and has a range from 1.7 to 2.7. This detection technique has the potential to become an orthogonal technique to the existing explosive screening technologies for reducing the number of false positives/false negatives in a cost-effective manner.

  10. A new headspace gas chromatographic method for the determination of methanol content in paper materials used for food and drink packaging.

    Science.gov (United States)

    Hu, Hui-Chao; Tian, Ying-Xin; Jin, Hui-Jun; Chai, Xin-Sheng; Barnes, Donald G

    2013-10-02

    This study reports on a method for determination of methanol in paper products by headspace gas chromatography (HS-GC). The method is based on the hydrolysis of the pulp or paper matrix, using a phosphoric acid solution (42.5%) as the medium at 120 °C in 5 h (excluding air contact) in order to release matrix-entrapped methanol, which is then determined by HS-GC. Data show that, under the given conditions of hydrolysis, no methanol was formed from the methoxyl groups in the material. Reproducibility tests of the method generated a relative standard deviation of methanol content in paper-related materials. The method can play an important role in addressing food safety concerns that may be raised regarding the use of paper materials in food and beverage packaging.

  11. Joint approximate diagonalization of eigenmatrices as a high-throughput approach for analysis of hyphenated and comprehensive two-dimensional gas chromatographic data.

    Science.gov (United States)

    Zarghani, Maryam; Parastar, Hadi

    2017-11-17

    The objective of the present work is development of joint approximate diagonalization of eigenmatrices (JADE) as a member of independent component analysis (ICA) family, for the analysis of gas chromatography-mass spectrometry (GC-MS) and comprehensive two-dimensional gas chromatography-mass spectrometry (GC×GC-MS) data to address incomplete separation problem occurred during the analysis of complex sample matrices. In this regard, simulated GC-MS and GC×GC-MS data sets with different number of components, different degree of overlap and noise were evaluated. In the case of simultaneous analysis of multiple samples, column-wise augmentation for GC-MS and column-wise super-augmentation for GC×GC-MS was used before JADE analysis. The performance of JADE was evaluated in terms of statistical parameters of lack of fit (LOF), mutual information (MI) and Amari index as well as analytical figures of merit (AFOMs) obtained from calibration curves. In addition, the area of feasible solutions (AFSs) was calculated by two different approaches of MCR-BANDs and polygon inflation algorithm (FACPACK). Furthermore, JADE performance was compared with multivariate curve resolution-alternating least squares (MCR-ALS) and other ICA algorithms of mean-field ICA (MFICA) and mutual information least dependent component analysis (MILCA). In all cases, JADE could successfully resolve the elution and spectral profiles in GC-MS and GC×GC-MS data with acceptable statistical and calibration parameters and their solutions were in AFSs. To check the applicability of JADE in real cases, JADE was used for resolution and quantification of phenanthrene and anthracene in aromatic fraction of heavy fuel oil (HFO) analyzed by GC×GC-MS. Surprisingly, pure elution and spectral profiles of target compounds were properly resolved in the presence of baseline and interferences using JADE. Once more, the performance of JADE was compared with MCR-ALS in real case. On this matter, the mutual information

  12. Naturally fractured tight gas: Gas reservoir detection optimization. Quarterly report, January 1--March 31, 1997

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1997-12-31

    Economically viable natural gas production from the low permeability Mesaverde Formation in the Piceance Basin, Colorado requires the presence of an intense set of open natural fractures. Establishing the regional presence and specific location of such natural fractures is the highest priority exploration goal in the Piceance and other western US tight, gas-centered basins. Recently, Advanced Resources International, Inc. (ARI) completed a field program at Rulison Field, Piceance Basin, to test and demonstrate the use of advanced seismic methods to locate and characterize natural fractures. This project began with a comprehensive review of the tectonic history, state of stress and fracture genesis of the basin. A high resolution aeromagnetic survey, interpreted satellite and SLAR imagery, and 400 line miles of 2-D seismic provided the foundation for the structural interpretation. The central feature of the program was the 4.5 square mile multi-azimuth 3-D seismic P-wave survey to locate natural fracture anomalies. The interpreted seismic attributes are being tested against a control data set of 27 wells. Additional wells are currently being drilled at Rulison, on close 40 acre spacings, to establish the productivity from the seismically observed fracture anomalies. A similar regional prospecting and seismic program is being considered for another part of the basin. The preliminary results indicate that detailed mapping of fault geometries and use of azimuthally defined seismic attributes exhibit close correlation with high productivity gas wells. The performance of the ten new wells, being drilled in the seismic grid in late 1996 and early 1997, will help demonstrate the reliability of this natural fracture detection and mapping technology.

  13. Quantification of Delta9-tetrahydrocannabinol and its major metabolites in meconium by gas chromatographic-mass spectrometric assay: assay validation and preliminary results of the "meconium project".

    Science.gov (United States)

    Marchei, Emilia; Pellegrini, Manuela; Pacifici, Roberta; Palmi, Ilaria; Lozano, Jaime; García-Algar, Oscar; Pichini, Simona

    2006-10-01

    A rapid and simple procedure based on gas chromatography-mass spectrometry (GC-MS) is described for determination of Delta-tetrahydrocannabinol (THC), 11-hydroxy-Delta-tetrahydrocannabinol (THC-OH) and 11-nor-Delta-tetrahydrocannabinol-9-carboxylic acid (THC-COOH) in meconium using Delta-tetrahydrocannabinol (Delta-THC) and deuterated THC-COOH as internal standards. The biological matrix was subjected to liquid-liquid extraction after enzyme hydrolysis for conjugated analytes.Chromatography was performed on a fused silica capillary column and analytes were determined in the selected-ion-monitoring (SIM) mode. The method was validated in the range 20 to 500 microg/g using 1g of meconium per assay. The method was applied to the analysis of meconium in a cohort of newborns to assess eventual fetal exposure to cannabis. Within positive samples, THC-COOH and THC-OH (range: 33.7 to 182.1 and 20.7 to 493.3 microg/g, respectively) were both present in the majority of cases with only 1 specimen with THC-OH as the most abundant metabolite and 2 with THC only.

  14. 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.

  15. Derivatizations for improved detection of alcohols by gas chromatography and photoionization detection (GC-PID)

    International Nuclear Information System (INIS)

    Krull, I.S.; Swartz, M.; Driscoll, J.N.

    1984-01-01

    Pentafluorophenyldimethylsilyl chloride (flophemesyl chloride, Fl) is a well known derivatization reagent for improved electron capture detection (ECD) in gas chromatography (GC)(GC-ECD), but it has never been utilized for improved detectability and sensitivity in GC-photoionization detection (GC-PID). A wide variety of flophemesyl alcohol derivatives have been used in order to show a new approach for realizing greatly reduced minimum detection limits (MDL) of virtually all alcohol derivatives in GC-PID analysis. This particular derivatization approach is inexpensive and easy to apply, leading to quantitative or near 100% conversion of the starting alcohols to the expected flophemesyl ethers (silyl ethers). Detection limits can be lowered by 2-3 orders of magnitude for such derivatives when compared with the starting alcohols, along with calibration plots that are linear over 5-7 orders of magnitude. Specific GC conditions have been developed for many flophemesyl derivatives, in all cases using packed columns. Both ECD and PID relative response factors (RRFs) and normalized RRFs have been determined, and such ratios can now be used for improved analytic identification from complex sample matrices, where appropriate. 28 references, 2 figures, 5 tables

  16. 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

  17. Laser Doppler detection systems for gas velocity measurement.

    Science.gov (United States)

    Huffaker, R M

    1970-05-01

    The velocity of gas flow has been remotely measured using a technique which involves the coherent detection of scattered laser radiation from small particles suspended in the fluid utilizing the doppler effect. Suitable instrumentation for the study of wind tunnel type and atmospheric flows are described. Mainly for reasons of spatial resolution, a function of the laser wavelength, the wind tunnel system utilizes an argon laser operating at 0.5 micro. The relaxed spatial resolution requirement of atmospheric applications allows the use of a carbon dioxide laser, which has superior performance at a wavelength of 10.6 micro, a deduction made from signal-to-noise ratio considerations. Theoretical design considerations are given which consider Mie scattering predictions, two-phase flow effects, photomixing fundamentals, laser selection, spatial resolution, and spectral broadening effects. Preliminary experimental investigations using the instrumentation are detailed. The velocity profile of the flow field generated by a 1.27-cm diam subsonic jet was investigated, and the result compared favorably with a hot wire investigation conducted in the same jet. Measurements of wind velocity at a range of 50 m have also shown the considerable promise of the atmospheric system.

  18. Validation of a gas chromatography/thermal conductivity detection method for the determination of the water content of oxygenated solvents.

    Science.gov (United States)

    O'Keefe, W K; Ng, F T T; Rempel, G L

    2008-02-22

    A gas chromatographic (GC) method for the determination of the water content of acetone solutions containing methyl isobutyl ketone (MIBK) and other by-products of MIBK synthesis was developed and validated. Linearity is demonstrated (R2=0.9999) over a broad range of water concentrations in acetone ranging from 0.04 to 15.2% (w/w). The quantitation limit (QL) of this technique was found to be 0.346% (w/w) and the detection limit (DL) was estimated to be 13ppm. Validation of this analytical method's accuracy against a coulometric Karl Fischer titration (KFT) method showed excellent agreement between these two techniques. The GC/TCD method is accurate to within a relative error of 3.49% with respect to the KFT method for water concentration above the QL. However, the analysis of six samples below the QL showed an average relative error of 10.96%. Consequently, the KFT method is recommended for the moisture analysis of samples for water concentrations below 0.35% (w/w). Excellent precision is realized for water concentration above the QL (RSD<0.8%). Good precision (RSD=1.1%) was obtained for the sample with the lowest water concentration investigated (0.04%, w/w). Repeatability, robustness and excellent specificity of this technique are demonstrated.

  19. Thermally modulated nano-trampoline material as smart skin for gas molecular mass detection

    Science.gov (United States)

    Xia, Hua

    2012-06-01

    Conventional multi-component gas analysis is based either on laser spectroscopy, laser and photoacoustic absorption at specific wavelengths, or on gas chromatography by separating the components of a gas mixture primarily due to boiling point (or vapor pressure) differences. This paper will present a new gas molecular mass detection method based on thermally modulated nano-trampoline material as smart skin for gas molecular mass detection by fiber Bragg grating-based gas sensors. Such a nanomaterial and fiber Bragg grating integrated sensing device has been designed to be operated either at high-energy level (highly thermal strained status) or at low-energy level (low thermal strained status). Thermal energy absorption of gas molecular trigs the sensing device transition from high-thermal-energy status to low-thermal- energy status. Experiment has shown that thermal energy variation due to gas molecular thermal energy absorption is dependent upon the gas molecular mass, and can be detected by fiber Bragg resonant wavelength shift with a linear function from 17 kg/kmol to 32 kg/kmol and a sensitivity of 0.025 kg/kmol for a 5 micron-thick nano-trampoline structure and fiber Bragg grating integrated gas sensing device. The laboratory and field validation data have further demonstrated its fast response characteristics and reliability to be online gas analysis instrument for measuring effective gas molecular mass from single-component gas, binary-component gas mixture, and multi-gas mixture. The potential industrial applications include fouling and surge control for gas charge centrifugal compressor ethylene production, gas purity for hydrogen-cooled generator, gasification for syngas production, gasoline/diesel and natural gas fuel quality monitoring for consumer market.

  20. MRGC performance evaluation model of gas leak infrared imaging detection system.

    Science.gov (United States)

    Li, Jiakun; Jin, Weiqi; Wang, Xia; Zhang, Xu

    2014-12-15

    Gas leak infrared imaging detection technology has become one of the most effective means to detect gas leaks. We propose a novel MRGC (minimum resolvable gas concentration) model that is suitable for evaluating the performance of passive GLIIDSs (gas leak infrared imaging detection systems). An MRGC equivalent calculation method and a direct MRGC measurement method based on the MRTD (minimum resolvable temperature difference) model are also proposed. The MRGC measurement system is designed and built. The measured and calculated results are in good agreement, which verifies the MRGC model's correctness and demonstrates the effectiveness of the MRGC performance evaluation method.

  1. Detection of Hot Gas in Galaxy Groups via the Sunyaev-Zel'dovich Effect

    OpenAIRE

    Moodley, K.; Warne, R.; Goheer, N.; Trac, H.

    2008-01-01

    Motivated by the observed shortfall of baryons in the local universe, we investigate the ability of high resolution cosmic microwave background (CMB) experiments to detect hot gas in the outer regions of nearby group halos. We construct hot gas models with the gas in hydrostatic equilibrium with the dark matter and described by a polytropic equation of state. We also consider models that add entropy to the gas in line with constraints from X-ray observations. We calculate the thermal Sunyaev-...

  2. Measurement of H2S in Crude Oil and Crude Oil Headspace Using Multidimensional Gas Chromatography, Deans Switching and Sulfur-selective Detection.

    Science.gov (United States)

    Heshka, Nicole E; Hager, Darcy B

    2015-12-10

    A method for the analysis of dissolved hydrogen sulfide in crude oil samples is demonstrated using gas chromatography. In order to effectively eliminate interferences, a two dimensional column configuration is used, with a Deans switch employed to transfer hydrogen sulfide from the first to the second column (heart-cutting). Liquid crude samples are first separated on a dimethylpolysiloxane column, and light gases are heart-cut and further separated on a bonded porous layer open tubular (PLOT) column that is able to separate hydrogen sulfide from other light sulfur species. Hydrogen sulfide is then detected with a sulfur chemiluminescence detector, adding an additional layer of selectivity. Following separation and detection of hydrogen sulfide, the system is backflushed to remove the high-boiling hydrocarbons present in the crude samples and to preserve chromatographic integrity. Dissolved hydrogen sulfide has been quantified in liquid samples from 1.1 to 500 ppm, demonstrating wide applicability to a range of samples. The method has also been successfully applied for the analysis of gas samples from crude oil headspace and process gas bags, with measurement from 0.7 to 9,700 ppm hydrogen sulfide.

  3. Detecting surface oil slick related to gas hydrate/petroleum on the ocean bed of South China Sea by ENVI/ASAR radar data

    Science.gov (United States)

    Wang, Yunpeng; Chen, Duofu; Song, Zhiguang

    2013-03-01

    For exploring the distribution of oil slick related to gas hydrate or petroleum in the northern part of South China Sea and evaluating the potential of ENVI/ASAR radar data for detecting oil slick, this paper tries to detect the oil slick on ocean surface of some potential areas in South China Sea and map oil slick from anomaly area in radar image. Seven surface oil slicks in Qiongdongnan Basin and four potential targets of oil slicks in Taixi-Dongsha Basin were detected and extracted by using ENIV/ASAR data. The anomalies of the radar image representing oil slick are validated by in-site sampling and laboratory analyzing. The Gas Chromatograph (GC) results of the extracted oil from the water samples gathered from the sites of detected oil slick demonstrate a typical composition of oil rather than that of ocean microbial origins, and Total Organic Carbon (TOC) concentrations in two designed vertical profiles keep steady in different depths, showing that the organic contents in water column are steady from the deep area to ocean surface. These results suggest the detected oil slick is a thin floating oil rather than a thick spill. Influencing factors to the results of oil slick detection including wind speed, current, small islands and capes as well as deep-sea petroleum reservoirs are discussed. The results in this study exhibit that extracting the anomaly signals related to oil slick related to oil/gas seeps using image processing techniques from ENVI/ASAR data is helpful to predict anomaly areas as potential targets for further exploration in this area.

  4. [A review of mixed gas detection system based on infrared spectroscopic technique].

    Science.gov (United States)

    Dang, Jing-Min; Fu, Li; Yan, Zi-Hui; Zheng, Chuan-Tao; Chang, Yu-Chun; Chen, Chen; Wang, Yi-Din

    2014-10-01

    In order to provide the experiences and references to the researchers who are working on infrared (IR) mixed gas detection field. The proposed manuscript reviews two sections of the aforementioned field, including optical multiplexing structure and detection method. At present, the coherent light sources whose representative are quantum cascade laser (QCL) and inter-band cascade laser(ICL) become the mainstream light source in IR mixed gas detection, which replace the traditional non-coherent light source, such as IR radiation source and IR light emitting diode. In addition, the photon detector which has a super high detectivity and very short response time is gradually beyond thermal infrared detector, dominant in the field of infrared detector. The optical multiplexing structure is the key factor of IR mixed gas detection system, which consists of single light source multi-plexing detection structure and multi light source multiplexing detection structure. Particularly, single light source multiplexing detection structure is advantages of small volume and high integration, which make it a plausible candidate for the portable mixed gas detection system; Meanwhile, multi light source multiplexing detection structure is embodiment of time division multiplex, frequency division multiplexing and wavelength division multiplexing, and become the leading structure of the mixed gas detection system because of its wider spectral range, higher spectral resolution, etc. The detection method applied to IR mixed gas detection includes non-dispersive infrared (NDIR) spectroscopy, wavelength and frequency-modulation spectroscopy, cavity-enhanced spectroscopy and photoacoustic spectroscopy, etc. The IR mixed gas detection system designed by researchers after recognizing the whole sections of the proposed system, which play a significant role in industrial and agricultural production, environmental monitoring, and life science, etc.

  5. 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 ...

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

    Indian Academy of Sciences (India)

    Unknown

    prevent this abuse and the side effects of these drugs in various countries, the urine and fluids are analysed ... samples in fishes and animals (Wright and Hunt 1982;. Young et al 1983; Kagawa et al 1984; McFarilane ... and metabolism of anabolic steroids in man or animal, although a knowledge of metabolism is necessary ...

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

    Indian Academy of Sciences (India)

    Unknown

    over sodium sulphate, evaporated at room temperature under nitrogen and the residues dissolved in 30–50 µl of methanol and injected. 2.4 Urine collection ... with potassium bicarbonate and extracted with 5 ml of diethylether. The residue, after evaporation of the diethyl- ether, was derivatized with 50 µl of a solution of.

  8. Chromatographic analysis of tryptophan metabolites.

    Science.gov (United States)

    Sadok, Ilona; Gamian, Andrzej; Staniszewska, Magdalena Maria

    2017-08-01

    The kynurenine pathway generates multiple tryptophan metabolites called collectively kynurenines and leads to formation of the enzyme cofactor nicotinamide adenine dinucleotide. The first step in this pathway is tryptophan degradation, initiated by the rate-limiting enzymes indoleamine 2,3-dioxygenase, or tryptophan 2,3-dioxygenase, depending on the tissue. The balanced kynurenine metabolism, which has been a subject of multiple studies in last decades, plays an important role in several physiological and pathological conditions such as infections, autoimmunity, neurological disorders, cancer, cataracts, as well as pregnancy. Understanding the regulation of tryptophan depletion provide novel diagnostic and treatment opportunities, however it requires reliable methods for quantification of kynurenines in biological samples with complex composition (body fluids, tissues, or cells). Trace concentrations, interference of sample components, and instability of some tryptophan metabolites need to be addressed using analytical methods. The novel separation approaches and optimized extraction protocols help to overcome difficulties in analyzing kynurenines within the complex tissue material. Recent developments in chromatography coupled with mass spectrometry provide new opportunity for quantification of tryptophan and its degradation products in various biological samples. In this review, we present current accomplishments in the chromatographic methodologies proposed for detection of tryptophan metabolites and provide a guide for choosing the optimal approach. © 2017 The Authors. Journal of Separation Science published by Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Flow injection gas chromatography with sulfur chemiluminescence detection for the analysis of total sulfur in complex hydrocarbon matrixes.

    Science.gov (United States)

    Hua, Yujuan; Hawryluk, Myron; Gras, Ronda; Shearer, Randall; Luong, Jim

    2018-01-01

    A fast and reliable analytical technique for the determination of total sulfur levels in complex hydrocarbon matrices is introduced. The method employed flow injection technique using a gas chromatograph as a sample introduction device and a gas phase dual-plasma sulfur chemiluminescence detector for sulfur quantification. Using the technique described, total sulfur measurement in challenging hydrocarbon matrices can be achieved in less than 10 s with sample-to-sample time ideal for fast analysis or trace sulfur analysis. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Ultrasound detection in the Gulf menhaden requires gas-filled bullae and an intact lateral line

    DEFF Research Database (Denmark)

    Wilson, Maria; Montie, Eric W.; Mann, Kenneth A.

    2009-01-01

    recess are involved in ultrasound detection in Gulf menhaden. Removal of a small portion of the lateral line overlying the lateral recess membrane eliminates the ability of Gulf menhaden to detect ultrasound. We further show that the gas-filled bullae vibrates in response to ultrasound, that the gas......-filled bullae are necessary for detecting ultrasound, and that the bullae connections to the lateral line via the lateral recess membrane play an important role in ultrasound detection. These results add a new dimension to the role of the lateral line and bullae as part of the ultrasonic detection system...

  11. 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.

  12. 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.

  13. Chromatographic screening techniques in systematic toxicological analysis.

    Science.gov (United States)

    Drummer, O H

    1999-10-15

    A review of techniques used to screen biological specimens for the presence of drugs was conducted with particular reference to systematic toxicological analysis. Extraction systems of both the liquid-liquid and solid-phase type show little apparent difference in their relative ability to extract a range of drugs according to their physio-chemical properties, although mixed-phase SPE extraction is a preferred technique for GC-based applications, and liquid-liquid were preferred for HPLC-based applications. No one chromatographic system has been shown to be capable of detecting a full range of common drugs of abuse, and common ethical drugs, hence two or more assays are required for laboratories wishing to cover a reasonably comprehensive range of drugs of toxicological significance. While immunoassays are invariably used to screen for drugs of abuse, chromatographic systems relying on derivatization and capable of extracting both acidic and basic drugs would be capable of screening a limited range of targeted drugs. Drugs most difficult to detect in systematic toxicological analysis include LSD, psilocin, THC and its metabolites, fentanyl and its designer derivatives, some potent opiates, potent benzodiazepines and some potent neuroleptics, many of the newer anti-convulsants, alkaloids colchicine, amantins, aflatoxins, antineoplastics, coumarin-based anti-coagulants, and a number of cardiovascular drugs. The widespread use of LC-MS and LC-MS-MS for specific drug detection and the emergence of capillary electrophoresis linked to MS and MS-MS provide an exciting possibility for the future to increase the range of drugs detected in any one chromatographic screening system.

  14. Development of conjugate methods with gas chromatography for inorganic compounds analysis

    International Nuclear Information System (INIS)

    Baccan, N.

    1975-01-01

    The application of gas chromatography combined with mass spectrometry or with nuclear methods for the analysis of inorganic compounds is studied. The advantages of the use of a gas chromatograph coupled with a quadrupole mass spectrometer or with a high resolution radiation detector, are discussed. We also studied the formation and solvent extraction of metal chelates; an aliquot of the organic phase was directly injected into the gas chromatograph and the eluted compounds were detected by mass spectrometry or, when radioactive, by nuclear methods. (author)

  15. Comprehensive two-dimensional gas chromatography combined to multivariate data analysis for detection of disease-resistant clones of Eucalyptus.

    Science.gov (United States)

    Hantao, Leandro Wang; Toledo, Bruna Regina; Ribeiro, Fabiana Alves de Lima; Pizetta, Marilia; Pierozzi, Caroline Geraldi; Furtado, Edson Luiz; Augusto, Fabio

    2013-11-15

    In this paper it is reported the use of the chromatographic profiles from volatile fractions of plant clones - in this case, hybrids of Eucalyptus grandis×Eucalyptus urophylla - to determine specimens susceptible to rust disease. The analytes were isolated by headspace solid phase microextraction (HS-SPME) and analyzed by comprehensive two-dimensional gas chromatography combined to fast quadrupole mass spectrometry (GC×GC-qMS). Parallel Factor Analysis (PARAFAC) was employed for estimate the correlation between the chromatographic profiles and resistance against Eucalyptus rust, after preliminary variable selection performed by Fisher ratio analysis. The proposed method allowed the differentiation between susceptible and non-susceptible clones and determination of three resistance biomarkers. This approach can be a valuable alternative for the otherwise time-consuming and labor-intensive methods commonly used. © 2013 Elsevier B.V. All rights reserved.

  16. Noble Gas Migration Experiment to Support the Detection of Underground Nuclear Explosions

    Energy Technology Data Exchange (ETDEWEB)

    Olsen, Khris B.; Kirkham, Randy R.; Woods, Vincent T.; Haas, Derek A.; Hayes, James C.; Bowyer, Ted W.; Mendoza, Donaldo P.; Lowrey, Justin D.; Lukins, Craig D.; Suarez, Reynold; Humble, Paul H.; Ellefson, Mark D.; Ripplinger, Mike D.; Zhong, Lirong; Mitroshkov, Alexandre V.; Aalseth, Craig E.; Prinke, Amanda M.; Mace, Emily K.; McIntyre, Justin I.; Stewart, Timothy L.; Mackley, Rob D.; Milbrath, Brian D.; Emer, Dudley; Biegalski, S.

    2016-03-01

    A Noble Gas Migration Experiment (NGME) funded by the National Center for Nuclear Security and conducted at the Nevada National Security Site (NNSS) in collaboration with Lawrence Livermore national Laboratory and National Security Technology provided critical on-site inspection (OSI) information related to the detection of an underground nuclear explosion (UNE) event using noble gas signatures.

  17. 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

  18. A gas chromatography-thermal conductivity detection method for helium detection in postmortem blood and tissue specimens.

    Science.gov (United States)

    Schaff, Jason E; Karas, Roman P; Marinetti, Laureen

    2012-03-01

    In cases of death by inert gas asphyxiation, it can be difficult to obtain toxicological evidence supporting assignment of a cause of death. Because of its low mass and high diffusivity, and its common use as a carrier gas, helium presents a particular challenge in this respect. We describe a rapid and simple gas chromatography-thermal conductivity detection method to qualitatively screen a variety of postmortem biological specimens for the presence of helium. Application of this method is demonstrated with three case examples, encompassing an array of different biological matrices.

  19. An approach to on-line electrospray mass spectrometric detection of polypeptide antibiotics of enramycin for high-speed counter-current chromatographic separation.

    Science.gov (United States)

    Inoue, Koichi; Hattori, Yasuko; Hino, Tomoaki; Oka, Hisao

    2010-04-06

    In the field of pharmaceutical and biomedical analysis of peptides, a rapid on-line detection and identification for a methodology have been required for the discovery of new biological active products. In this study, a high-speed counter-current chromatography with electrospray mass spectrometry (HSCCC/ESI-MS) was developed for the on-line detection and purification of polypeptide antibiotics of enramycin-A and -B. The analytes were purified on HSCCC model CCC-1000 (multi-layer coil planet centrifuge) with a volatile solvent of two-phase system composed of n-butanol/hexane/0.05% aqueous trifluoroacetic acid solution (43/7/50, V/V/V), and detected on an LCMS-2010EV quadrupole mass spectrometer fitted with an ESI source system in positive ionization following scan mode (m/z 100-2000). The HSCCC/ESI-MS peaks indicated that enramycin-A (major m/z 786 [M+3H](3+) and minor m/z 1179 [M+2H](2+)) and enramycin-B (major m/z 791 [M+3H](3+) and minor m/z 1185 [M+2H](2+)) have the peak resolution value of 2.9 from 15mg of loaded enramycin powder. The HSCCC collected amounts of the peak fractions were additionally 4.3mg (enramycin-A), and 5.9mg (enramycin-B), respectively. These purified substances were analyzed by LC/ESI-MS with scan positive mode. Based on the LC/ESI-MS chromatograms and spectra of the fractions, enramycin-A and -B were estimated to be over 95% purity. The overall results indicate that this approach of HSCCC/ESI-MS is a powerful technique for the purification and identification of bioactive peptides. Copyright 2009 Elsevier B.V. All rights reserved.

  20. Speciation of eight arsenic compounds in human urine by high performance liquid chromatography with inductively coupled plasma mass spectrometric detection using antimonate for internal chromatographic standardization

    DEFF Research Database (Denmark)

    Larsen, Erik Huusfeldt; Pritzl, G.; Hansen, S. H.

    1993-01-01

    to arsenate in urine but was stable after at least 4-fold dilution of the urine with water. Arsenite was unstable in both urine samples and standard mixtures when diluted with the basic (pH 10.3) mobile phase used for anion chromatography. This could not be prevented by adding ascorbic acid as antioxidant......Four anionic and four cationic arsenic compounds in urine were separated by anion- and cation-exchange high-performance liquid chromatography and detected by inductively coupled plasma mass spectrometry (ICP-MS) at m/z 75. The species were the anions arsenite, arsenate, monomethylarsonate...

  1. Chemoresistive Gas Sensors for the Detection of Colorectal Cancer Biomarkers

    OpenAIRE

    Malagù, Cesare; Fabbri, Barbara; Gherardi, Sandro; Giberti, Alessio; Guidi, Vincenzo; Landini, Nicolò; Zonta, Giulia

    2014-01-01

    Numerous medical studies show that tumor growth is accompanied by protein changes that may lead to the peroxidation of the cell membrane with consequent emission of volatile organic compounds (VOCs) by breath or intestinal gases that should be seen as biomarkers for colorectal cancer (CRC). The analysis of VOCs represents a non-invasive and potentially inexpensive preliminary screening technique. An array of chemoresistive gas sensors based on screen-printed metal oxide semiconducting films h...

  2. First Detection of Hydrogen in the \\beta\\ Pictoris Gas Disk

    OpenAIRE

    Wilson, P. A.; Etangs, A. Lecavelier des; Vidal-Madjar, A.; Bourrier, V.; Hébrard, G.; Kiefer, F.; Beust, H.; Ferlet, R.; Lagrange, A. -M.

    2016-01-01

    The young and nearby star \\beta\\ Pictoris (\\beta\\ Pic) is surrounded by a debris disk composed of dust and gas known to host a myriad evaporating exocomets, planetesimals and at least one planet. At an edge-on inclination, as seen from Earth, this system is ideal for debris disk studies providing an excellent opportunity to use absorption spectroscopy to study the planet forming environment. Using the Cosmic Origins Spectrograph (COS) instrument on the Hubble Space Telescope (HST) we observe ...

  3. Detecting gas hydrate behavior in crude oil using NMR.

    Science.gov (United States)

    Gao, Shuqiang; House, Waylon; Chapman, Walter G

    2006-04-06

    Because of the associated experimental difficulties, natural gas hydrate behavior in black oil is poorly understood despite its grave importance in deep-water flow assurance. Since the hydrate cannot be visually observed in black oil, traditional methods often rely on gas pressure changes to monitor hydrate formation and dissociation. Because gases have to diffuse through the liquid phase for hydrate behavior to create pressure responses, the complication of gas mass transfer is involved and hydrate behavior is only indirectly observed. This pressure monitoring technique encounters difficulties when the oil phase is too viscous, the amount of water is too small, or the gas phase is absent. In this work we employ proton nuclear magnetic resonance (NMR) spectroscopy to observe directly the liquid-to-solid conversion of the water component in black oil emulsions. The technique relies on two facts. The first, well-known, is that water becomes essentially invisible to liquid state NMR as it becomes immobile, as in hydrate or ice formation. The second, our recent finding, is that in high magnetic fields of sufficient homogeneity, it is possible to distinguish water from black oil spectrally by their chemical shifts. By following changes in the area of the water peak, the process of hydrate conversion can be measured, and, at lower temperatures, the formation of ice. Taking only seconds to accomplish, this measurement is nearly direct in contrast to conventional techniques that measure the pressure changes of the whole system and assume these changes represent formation or dissociation of hydrates - rather than simply changes in solubility. This new technique clearly can provide accurate hydrate thermodynamic data in black oils. Because the technique measures the total mobile water with rapidity, extensions should prove valuable in studying the dynamics of phase transitions in emulsions.

  4. Fiber-Optic Based Compact Gas Leak Detection System

    Science.gov (United States)

    deGroot, Wim A.

    1995-01-01

    A propellant leak detection system based on Raman scattering principles is introduced. The proposed system is flexible and versatile as the result of the use of optical fibers. It is shown that multiple species can be monitored simultaneously. In this paper oxygen, nitrogen, carbon monoxide, and hydrogen are detected and monitored. The current detection sensitivity for both hydrogen and carbon monoxide is 1% partial pressure at ambient conditions. The sensitivity for oxygen and nitrogen is 0.5% partial pressure. The response time to changes in species concentration is three minutes. This system can be used to monitor multiple species at several locations.

  5. Ion chromatographic analysis of high specific activity 18FDG preparations and detection of the chemical impurity 2-deoxy-2-chloro-D-glucose

    International Nuclear Information System (INIS)

    Alexoff, D.L.; Casati, R.; Fowler, J.S.; Wolf, A.P.; Shea, C.; Schlyer, D.J.; Chyng-Yann Shiue

    1992-01-01

    Because of the widespread use of 2-deoxy-2-[ 18 F]fluoro-D-glucose(FDG) prepared by the ''Julich'' method or its variants it was decided necessary to determine the major chemical impurities present in the final product. An analytical system for quantifying FDG was developed using pulsed amperometry after separation by high-performance anion exchange chromotography. With this system a heretofore unidentified impurity, 2-deoxy-2-chloro-D-glucose(C1DG) was found in our preparation and in those from other laboratories using the ''Julich'' method. C1DG arises from C1 - ion displacement during the labeling procedure where C1 - ion comes from several sources, and C1 - ion displacement from the HC1 used in the hydrolysis step. FDG mass was present in the same preparations at a level of ca 1-40 μg. Other major chemical constituents were glucose (ca 1-6 mg) and mannose (ca 10-18 μg). Glycerol, arising from sterilizing filters, was also detected in most preparations. Although C1DG is a chemical impurity which has not been detected previously in nca FDG preparations, its biochemical and pharmacological properties are similar to FDG and 2-deoxy-D-glucose. Thus it is unlikely that the presence of small quantities of C1DG found in typical FDG preparations (ca 100 μg) would have adverse pharmacological or toxicological consequences that would limit continued application of this radiopharmaceutical in basic and clinical studies. (Author)

  6. Cross validation of gas chromatography-flame photometric detection and gas chromatography-mass spectrometry methods for measuring dialkylphosphate metabolites of organophosphate pesticides in human urine.

    Science.gov (United States)

    Prapamontol, Tippawan; Sutan, Kunrunya; Laoyang, Sompong; Hongsibsong, Surat; Lee, Grace; Yano, Yukiko; Hunter, Ronald Elton; Ryan, P Barry; Barr, Dana Boyd; Panuwet, Parinya

    2014-01-01

    We report two analytical methods for the measurement of dialkylphosphate (DAP) metabolites of organophosphate pesticides in human urine. These methods were independently developed/modified and implemented in two separate laboratories and cross validated. The aim was to develop simple, cost effective, and reliable methods that could use available resources and sample matrices in Thailand and the United States. While several methods already exist, we found that direct application of these methods required modification of sample preparation and chromatographic conditions to render accurate, reliable data. The problems encountered with existing methods were attributable to urinary matrix interferences, and differences in the pH of urine samples and reagents used during the extraction and derivatization processes. Thus, we provide information on key parameters that require attention during method modification and execution that affect the ruggedness of the methods. The methods presented here employ gas chromatography (GC) coupled with either flame photometric detection (FPD) or electron impact ionization-mass spectrometry (EI-MS) with isotopic dilution quantification. The limits of detection were reported from 0.10ng/mL urine to 2.5ng/mL urine (for GC-FPD), while the limits of quantification were reported from 0.25ng/mL urine to 2.5ng/mL urine (for GC-MS), for all six common DAP metabolites (i.e., dimethylphosphate, dimethylthiophosphate, dimethyldithiophosphate, diethylphosphate, diethylthiophosphate, and diethyldithiophosphate). Each method showed a relative recovery range of 94-119% (for GC-FPD) and 92-103% (for GC-MS), and relative standard deviations (RSD) of less than 20%. Cross-validation was performed on the same set of urine samples (n=46) collected from pregnant women residing in the agricultural areas of northern Thailand. The results from split sample analysis from both laboratories agreed well for each metabolite, suggesting that each method can produce

  7. Instrumental Analysis in Environmental Chemistry - Gas Phase Detection Systems

    Science.gov (United States)

    Stedman, Donald H.; Meyers, Philip A.

    1974-01-01

    Discusses advances made in chemical analysis instrumentation used in environmental monitoring. This first of two articles is concerned with analytical instrumentation in which detection and dispersion depend ultimately on the properties of gaseous molecules. (JR)

  8. [Gas pipeline leak detection based on tunable diode laser absorption spectroscopy].

    Science.gov (United States)

    Zhang, Qi-Xing; Wang, Jin-Jun; Liu, Bing-Hai; Cai, Ting-Li; Qiao, Li-Feng; Zhang, Yong-Ming

    2009-08-01

    The principle of tunable diode laser absorption spectroscopy and harmonic detection technique was introduced. An experimental device was developed by point sampling through small multi-reflection gas cell. A specific line near 1 653. 7 nm was targeted for methane measurement using a distributed feedback diode laser as tunable light source. The linearity between the intensity of second harmonic signal and the concentration of methane was determined. The background content of methane in air was measured. The results show that gas sensors using tunable diode lasers provide a high sensitivity and high selectivity method for city gas pipeline leak detection.

  9. Remote detection of gas markers of artificial explosives

    Science.gov (United States)

    Ageev, B. G.; Klimkin, A. V.; Kuryak, A. N.; Osipov, K. Yu.; Ponomarev, Yu. N.

    2015-11-01

    At the recent years, the increasing interest to laser methods of detection of harmful and dangerous admixtures in the open atmosphere is observed. In this work, experimental results are given of remote detection of acetone vapors, which is the marker of triacetone triperoxide (TATP), with the use of the frequency-pulse 13C16O2 laser with generation line at 11.2 μm.

  10. The application of inductively coupled plasma dynamic reaction cell mass spectrometry for measurement of selenium isotopes, isotope ratios and chromatographic detection of selenoamino acids

    DEFF Research Database (Denmark)

    Sloth, Jens Jørgen; Larsen, Erik Huusfeldt

    2000-01-01

    . A linear relationship (r mass from the Se-80 reference isotope. This indicated that the error was caused by mass bias. The slope of the curve at -3.0% error per mass unit can be used for correction of the measured......Inductively coupled plasma dynamic reaction cell mass spectrometry (ICP-DRC-MS) was characterised for the detection of the six naturally occurring selenium isotopes. The potentially interfering argon dimers at the selenium masses m/z 74, 76, 78 and 80 were reduced in intensity by approximately five...... ratios was close to the theoretical values for selenium concentrations at 1 and 10 ng ml(-1). The accuracy of the isotope ratios, however, was improved by correcting the count rate of all selenium isotopes equivalent to the formation of SeH at 9.6 +/- 0.5% one mass unit above the selenium isotopes...

  11. A new 3D printed radial flow-cell for chemiluminescence detection: Application in ion chromatographic determination of hydrogen peroxide in urine and coffee extracts.

    Science.gov (United States)

    Gupta, Vipul; Mahbub, Parvez; Nesterenko, Pavel N; Paull, Brett

    2018-04-16

    A new polymer flow-cell for chemiluminescence detection (CLD) has been designed and developed by diverging multiple linear channels from a common centre port in a radial arrangement. The fabrication of radial flow-cell by 3D PolyJet printing and fused deposition modeling (FDM) has been evaluated, and compared with a similarly prepared spiral flow-cell design commonly used in chemiluminescence detectors. The radial flow-cell required only 10 h of post-PolyJet print processing time as compared to ca. 360 h long post-PolyJet print processing time required for the spiral flow-cell. Using flow injection analysis, the PolyJet 3D printed radial flow-cell provided an increase in both the signal magnitude and duration, with an average increase in the peak height of 63% and 58%, peak area of 89% and 90%, and peak base width of 41% and 42%, as compared to a coiled-tubing spiral flow-cell and the PolyJet 3D printed spiral flow-cell, respectively. Computational fluid dynamic (CFD) simulations were applied to understand the origin of the higher CLD signal obtained with the radial flow-cell design, indicating higher spatial coverage near the inlet and lower linear velocities in the radial flow-cell. The developed PolyJet 3D printed radial flow-cell was applied in a new ion chromatography chemiluminescence based assay for the detection of H 2 O 2 in urine and coffee extracts. Copyright © 2018 Elsevier B.V. All rights reserved.

  12. Detection of Volatile Organic Compound Gas Using Localized Surface Plasmon Resonance of Gold Nanoparticles

    International Nuclear Information System (INIS)

    Sri Nengsih; Akrajas Ali Umar; Muhamad Mat Salleh; Muhammad Yahaya

    2011-01-01

    This paper reports on the detection of several organic vapors using the unique characteristic of localized surface plasmon resonance (LSPR) gold nanoparticles. Gold nanoparticles on quartz substrate were prepared using seed mediated growth method. In a typical process, gold nanoparticles with average size ca. 36 nm were obtained to densely grown on the substrate. Detection of gas was based on the change in the LSPR of the gold nanoparticles film upon the exposure to the gas sample. It was found that gold nanoparticles were sensitive to the presence of volatile organic compound (VOC) gas from the change in the surface plasmon resonance (SPR) intensity. The mechanism for the detection of VOCs gas will be discussed. (author)

  13. Detection of atypical bile acids in disease states and their identification by gas chromatography-mass spectrometry-computer techniques

    Energy Technology Data Exchange (ETDEWEB)

    Szczepanik-Van Leeuwen, P. A.; Stellaard, F.

    1978-01-01

    The study of the bile acid constituents of serum, bile, urine, and stool of patients exhibiting liver disease has increased in importance with the availability of newer methods for their detection and identification. A cogent question for study has been whether specific bile acids are toxic and thus are the cause of liver disease, or whether they accumulate as a result of disease-induced alteration in metabolism. Examining a wide variety of clinical samples, we have observed that many patients with diagnosed cholestasis show the presence of atypical bile acids due to metabolic aberrations in either the side chain or in the steroid ring. Because cholestasis represents a spectrum of diseases with differing metabolic and/or anatomic defects and because our studies cover a variety of cholestatic states, we have sought to establish a correlation between the presence of these atypical bile acids and the disease state. The complexity of the bile acid mixtures to be examined requires that gas chromatographic-mass spectrometric-computer techniques be used to provide a reliable analysis. It is believed that atypical bile acids can be readily identified by GC/CI mass spectrometry with great sensitivity. It is also believed that such bile acid analysis may prove useful to the study and diagnosis of liver disease. Present data suggest that the identification of atypical bile acids in biological samples may enable differentiation between different types of intrahepatic cholestasis. Such analyses may prove useful to distinguish specific diseases, such as Byler's disease (and Byler's-like cholestasis) from other types of cholestasis and may distinguish diseases involving mitochondrial defects. Finally, the presence of atypical bile acids may indicate, by the particular compounds formed, where and what kind of damage occurs in a disease and may ultimately establish if these atypical bile acids are a cause or effect of the liver damage.

  14. CHROMATOGRAPHIC SEPARATION AND SPECTRO ...

    African Journals Online (AJOL)

    contain aromatic nucleus based on IR and UV-VIS spectroscopic data. Other functional groups detected ... Qualitative analysis of dye using thin layer chromatography studies of some novel analogous of phthalein dyes have been .... facility runs on PC with Maestro software for spectra acquisition. Sensitivity calibration using.

  15. Anomaly Detection in Gas Turbine Fuel Systems Using a Sequential Symbolic Method

    Directory of Open Access Journals (Sweden)

    Fei Li

    2017-05-01

    Full Text Available Anomaly detection plays a significant role in helping gas turbines run reliably and economically. Considering the collective anomalous data and both sensitivity and robustness of the anomaly detection model, a sequential symbolic anomaly detection method is proposed and applied to the gas turbine fuel system. A structural Finite State Machine is used to evaluate posterior probabilities of observing symbolic sequences and the most probable state sequences they may locate. Hence an estimation-based model and a decoding-based model are used to identify anomalies in two different ways. Experimental results indicate that both models have both ideal performance overall, but the estimation-based model has a strong robustness ability, whereas the decoding-based model has a strong accuracy ability, particularly in a certain range of sequence lengths. Therefore, the proposed method can facilitate well existing symbolic dynamic analysis- based anomaly detection methods, especially in the gas turbine domain.

  16. Nuclear reactor neutron flux detection by gas optical detectors

    International Nuclear Information System (INIS)

    Dmitriev, A.B.; Il'yashenko, V.S.; Mis'kevich, A.I.; Salamakha, B.S.; Sarylov, V.N.

    1983-01-01

    A gas scintillation detector consisting of a neutron-sensitive volume with 10 B-coated walls connected with a photomultiplier through a hollow-type polished light guide 7m long and 12 mm in dia. is described. The results of measuring its sensitivity, linearity, temperature- and time-dependent stability are given. The detector was tested in the IRT-2000 reactor vertical channel. In the 4X10 7 -10 10 neutr./(cm 2 x s) flux density range the nonlinearity of the measured characteristic does not exceed 5% The detector sensitivity is 4.6x10S -5 pulse/neutr. x cm -2 . Variations in the detector readings during 420 h of reactor operation at nominal power do not exceed +-3.5%, which indicates a high detector stability. The conclusion is drawn that detectors filled with thw He+0.1% N 2 mixture possess the highest sensitivity

  17. Chemoresistive Gas Sensors for the Detection of Colorectal Cancer Biomarkers

    Directory of Open Access Journals (Sweden)

    Cesare Malagù

    2014-10-01

    Full Text Available Numerous medical studies show that tumor growth is accompanied by protein changes that may lead to the peroxidation of the cell membrane with consequent emission of volatile organic compounds (VOCs by breath or intestinal gases that should be seen as biomarkers for colorectal cancer (CRC. The analysis of VOCs represents a non-invasive and potentially inexpensive preliminary screening technique. An array of chemoresistive gas sensors based on screen-printed metal oxide semiconducting films has been selected to discriminate gases of oncological interest, e.g., 1-iodononane and benzene, widely assumed to be biomarkers of colorectal cancer, from those of interference in the gut, such as methane and nitric oxide.

  18. [A Detection Technique for Gas Concentration Based on the Spectral Line Shape Function].

    Science.gov (United States)

    Zhou, Mo; Yang, Bing-chu; Tao, Shao-hua

    2015-04-01

    The methods that can rapidly and precisely measure concentrations of various gases have extensive applications in the fields such as air quality analysis, environmental pollution detection, and so on. The gas detection method based on the tunable laser absorption spectroscopy is considered a promising technique. For the infrared spectrum detection techniques, the line shape function of an absorption spectrum of a gas is an important parameter in qualitative and quantitative analysis of a gas. Specifically, how to obtain the line shape function of an absorption spectrum of a gas quickly and accurately is a key problem in the gas detection fields. In this paper we analyzed several existing line shape functions and proposed a method to calculate precisely the line shape function of a gas, and investigated the relation between the gas concentration and the peak value of a line shape function. Then we experimentally measured the absorption spectra of an acetylene gas in the wavelength range of 1,515-1,545 nm with a tunable laser source and a built-in spectrometer. With Lambert-Beer law we calculated the peak values of the line shape function of the gas at the given frequencies, and obtained a fitting curve for the line shape function in the whole waveband by using a computer program. Comparing the measured results with the calculated results of the Voigt function, we found that there was a deviation-between the experimental results and the calculated results. And we found that the measured concentration of the acetylene gas by using the fitting curve of the line shape function was more accurate and compatible with the actual situation. Hence, the empirical formula for the line shape function obtained from the experimental results would be more suitable for the concentration measurement of a gas. As the fitting curve for the line shape function of the acetylene gas has been deduced from the experiment, the corresponding peak values of the spectral lines can be

  19. Specific high-performance liquid chromatographic assay with ultraviolet detection for the determination of 1-(2-chloroethyl)-3-sarcosinamide-1-nitrosourea in plasma.

    Science.gov (United States)

    Supko, J G; Phillips, L R; Malspeis, L

    1996-03-03

    .1 micrograms/ml, exhibited R.S.D. values ranging from 1.3 to 4.7%. Thermospray-ionization MS detection was used to definitively establish the specificity of the method. The sensitivity of the assay was shown by application to be more than adequate for characterizing the plasma pharmacokinetics of SarCNU in mice.

  20. Ionization spectrometer to detect dangerous gas; Le spectrometre a ionisation surveille les gaz dangereux

    Energy Technology Data Exchange (ETDEWEB)

    Vivarat-Perrin, M.P

    2004-03-01

    Draeger-Industry proposes a portable (7 Kg) gas analyzer able to detect about 100 dangerous substances. This device is based on ionization spectrometry, it uses a radioactive source that ionizes molecules, the electrical current generated by the motion of the ions is measured, its intensity is proportional to the concentration of the substance. About 16 substances can be detected simultaneously, the threshold of detection is as low as about 1 ppb (10{sup -9}). (A.C.)

  1. High performance liquid chromatographic determination of ...

    African Journals Online (AJOL)

    STORAGESEVER

    2010-02-08

    sulphonate (synthesized). Instrumentation. The chromatographic apparatus consisted of a Cecil 1200 series. 1000 high performance liquid chromatograph. The analytical column was ODS hypersil C18,5 µm particle size in 250 mm ...

  2. Continuum removed band depth analysis for detecting the effects of natural gas, methane and ethane on maize reflectance

    NARCIS (Netherlands)

    Noomen, M.F.; Skidmore, A.K.; Meer, van der F.D.; Prins, H.H.T.

    2006-01-01

    It is known that natural gas in the soil affects vegetation health, which may be detected through analysis of reflectance spectra. Since natural gas is invisible, changes in the vegetation could potentially indicate gas leakage. Although it is known that gas in soil affects plant reflectance, the

  3. A design of toxic gas detecting security robot car based on wireless path-patrol

    Directory of Open Access Journals (Sweden)

    Cheng Ho-Chih

    2017-01-01

    Full Text Available Because a toxic gas detecting/monitoring system in a chemical plant is not movable, a gas detecting/monitoring system will be passive and the detecting range will also be constrained. This invention is an active multi-functional wireless patrol car that can substitute for humans that inspect a plant's security. In addition, to widen the monitoring vision within the environment, two motors used to rotate a wireless IPCAM with two axes are presented. Also, to control the robot car's movement, two axis motors used to drive the wheel of the robot car are also installed. Additionally, a toxic gas detector is linked to the microcontroller of the patrol car. The detected concentration of the gas will be fed back to the server pc. To enhance the robot car's patrolling duration, a movable electrical power unit in conjunction with a wireless module is also used. Consequently, this paper introduces a wireless path-patrol and toxic gas detecting security robot car that can assure a plant's security and protect workers when toxic gases are emitted.

  4. Detection of gas molecules on single Mn adatom adsorbed graphyne: a DFT-D study

    Science.gov (United States)

    Lu, Zhansheng; Lv, Peng; Ma, Dongwei; Yang, Xinwei; Li, Shuo; Yang, Zongxian

    2018-02-01

    As one of the prominent applications in intelligent systems, gas sensing technology has attracted great interest in both industry and academia. In the current study, the pristine graphyne (GY) without and with a single Mn atom is investigated to detect the gas molecules (CO, CH4, CO2, NH3, NO and O2). The pristine GY is promising to detect O2 molecules because of its chemical adsorption on GY with large electron transfer. The great stability of the Mn/GY is found, and the Mn atom prefers to anchor at the alkyne ring as a single atom. Upon single Mn atom anchoring, the sensitivity and selectivity of GY based gas sensors is significantly improved for various molecules, except CH4. The recovery time of the Mn/GY after detecting the gas molecules may help to appraise the detection efficiency for the Mn/GY. The current study will help to understand the mechanism of detecting the gas molecules, and extend the potentially fascinating applications of GY-based materials.

  5. Estimation of the limit of detection in semiconductor gas sensors through linearized calibration models.

    Science.gov (United States)

    Burgués, Javier; Jiménez-Soto, Juan Manuel; Marco, Santiago

    2018-07-12

    The limit of detection (LOD) is a key figure of merit in chemical sensing. However, the estimation of this figure of merit is hindered by the non-linear calibration curve characteristic of semiconductor gas sensor technologies such as, metal oxide (MOX), gasFETs or thermoelectric sensors. Additionally, chemical sensors suffer from cross-sensitivities and temporal stability problems. The application of the International Union of Pure and Applied Chemistry (IUPAC) recommendations for univariate LOD estimation in non-linear semiconductor gas sensors is not straightforward due to the strong statistical requirements of the IUPAC methodology (linearity, homoscedasticity, normality). Here, we propose a methodological approach to LOD estimation through linearized calibration models. As an example, the methodology is applied to the detection of low concentrations of carbon monoxide using MOX gas sensors in a scenario where the main source of error is the presence of uncontrolled levels of humidity. Copyright © 2018 Elsevier B.V. All rights reserved.

  6. Methods and systems for detecting gas flow by photoacoustic signal generation

    Energy Technology Data Exchange (ETDEWEB)

    Choudhury, Niloy; Challener, William Albert

    2018-03-06

    A method for the detection of a gas flowing from a location in a structure is described. A hollow-core optical fiber is placed in a position adjacent the structure. The fiber includes a sound-conductive cladding layer; and further includes at least one aperture extending into its cross-sectional diameter. A beam of pulsed, optical is transmitted into the fiber with a tunable laser. The optical energy is characterized by a wavelength that can be absorbed by the gas that flows into the fiber through the aperture. This causes a temperature fluctuation in the region of gas absorption, which in turn generates an acoustic wave in the absorption region. The acoustic wave travels through the cladding layer, and can be detected with a microphone, so as to provide the location of gas flow, based on the recorded position and movement of the acoustic wave. A related system is also described.

  7. Gas chromatographic-tandem mass spectrometric analysis of β-lyase metabolites of sulfur mustard adducts with glutathione in urine and its use in a rabbit cutaneous exposure model.

    Science.gov (United States)

    Lin, Ying; Dong, Yuan; Chen, Jia; Li, Chun-Zheng; Nie, Zhi-Yong; Guo, Lei; Liu, Qin; Xie, Jian-Wei

    2014-01-15

    A method for quantitation of β-lyase metabolites of sulfur mustard (SM) adducts with glutathione has been developed and validated using gas chromatography-tandem mass spectrometry (GC-MS/MS). The linear range of quantitation was 0.1-1000ng/mL in urine with a method detection limit of 0.02ng/mL. The method was applied in a rabbit exposure model. Domestic rabbits were cutaneously exposed to neat liquid SM in three dosage levels, and the β-lyase metabolites in urine were determined as 1,1'-sulfonylbis[2-(methylthio)ethane] (SBMTE). The study showed that even though more than 99% of the total amount of β-lyase metabolites was excreted in the first week after exposure, the β-lyase metabolites of SM adducts with glutathione could be detected in urine from rabbits for up to 3 or 4 weeks after the SM cutaneous exposure. For high dosage group (15mg/kg, 0.15 LD50), the mean concentration of SBMTE detected was 0.32ng/mL on day 28. For middle (5mg/kg, 0.05 LD50) and low (2mg/kg, 0.02 LD50) dosage groups, the mean concentrations of SBMTE were 0.07ng/mL and 0.02ng/mL on day 21, respectively. The data from this study indicate that the method is sensitive and provides a relatively long time frame for the retrospective detection of SM exposure. Copyright © 2013 Elsevier B.V. All rights reserved.

  8. Naturally fractured tight gas reservoir detection optimization. Quarterly report, January 1, 1997--March 31, 1997

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1998-04-01

    This document contains the quarterly report dated January 1-March 31, 1997 for the Naturally Fractured Tight Gas Reservoir Detection Optimization project. Topics covered in this report include AVOA modeling using paraxial ray tracing, AVOA modeling for gas- and water-filled fractures, 3-D and 3-C processing, and technology transfer material. Several presentations from a Geophysical Applications Workshop workbook, workshop schedule, and list of workshop attendees are also included.

  9. Tunable nanostructured columnar growth of SnO2 for efficient detection of CO gas

    Science.gov (United States)

    Singh, Avneet; Sharma, Anjali; Tomar, Monika; Gupta, Vinay

    2018-02-01

    The present work is focused on the growth and modification of the columnar nanostructures of SnO2 using a glancing angle deposition (GLAD) assisted rf sputtering technique for low temperature detection of carbon monoxide (CO) gas. The GLAD angle and deposition pressure are optimized to tailor the grow of columnar nanostructures of SnO2, which exhibit an enhanced gas sensing response of 1.50 × 102 towards 500 ppm of CO gas at a comparatively lower operating temperature of 110 °C. The enhanced sensing response at low operating temperature is related to the growth of nanoporous columnar structures of SnO2 thin film under the GLAD configuration, which results in an enhanced interaction of target CO gas molecules with the large surface area of sensing SnO2 thin film. The origin of the sensing mechanism supporting the observed response characteristics towards CO gas is identified and discussed in detail.

  10. Study of gas ionization in a glow discharge and development of a micro gas ionizer for gas detection and analysis

    OpenAIRE

    Longwitz, Ralf G.

    2004-01-01

    In the pursuit of a portable gas detector/analyser we studied the components of an ion mobility spectrometer (IMS), which is a device that lends itself well to miniaturisation. The component we focused on was the ionizer. We fabricated a series of micro ionizers with micro electromechanical systems (MEMS) technology, which had a gap spacing between 1 and 50 μm and a thickness from 0.3 to 50 μm. They were used to examine micro discharges as such and as a means of ionization. In our measurement...

  11. Study of gas ionization in a glow discharge and development of a micro gas ionizer for gas detection and analysis

    OpenAIRE

    Longwitz, Ralf G.; Renaud, Philippe

    2005-01-01

    In the pursuit of a portable gas detector/analyser we studied the components of an ion mobility spectrometer (IMS), which is a device that lends itself well to miniaturisation. The component we focused on was the ionizer. We fabricated a series of micro ionizers with micro electromechanical systems (MEMS) technology, which had a gap spacing between 1 and 50 μm and a thickness from 0.3 to 50 μm. They were used to examine micro discharges as such and as a means of ionization. In our measurement...

  12. Combined raman and IR fiber-based sensor for gas detection

    Science.gov (United States)

    Carter, Jerry C; Chan, James W; Trebes, James E; Angel, Stanley M; Mizaikoff, Boris

    2014-06-24

    A double-pass fiber-optic based spectroscopic gas sensor delivers Raman excitation light and infrared light to a hollow structure, such as a hollow fiber waveguide, that contains a gas sample of interest. A retro-reflector is placed at the end of this hollow structure to send the light back through the waveguide where the light is detected at the same end as the light source. This double pass retro reflector design increases the interaction path length of the light and the gas sample, and also reduces the form factor of the hollow structure.

  13. Signal-based Gas Leakage Detection for Fluid Power Accumulators in Wind Turbines

    DEFF Research Database (Denmark)

    Liniger, Jesper; Sepehri, Nariman; N. Soltani, Mohsen

    2017-01-01

    This paper describes the development and application of a signal-based fault detection method for identifying gas leakage in hydraulic accumulators used in wind turbines. The method uses Multiresolution Signal Decomposition (MSD) based on wavelets for feature extraction from a~single fluid pressure...... measurement located close to the accumulator. Gas leakage is shown to create increased variations in this pressure signal. The Root Mean Square (RMS) of the detail coefficient Level 9 from the MSD is found as the most sensitive and robust fault indicator of gas leakage. The method is verified...

  14. ZnO:Al Thin Film Gas Sensor for Detection of Ethanol Vapor

    Directory of Open Access Journals (Sweden)

    Min Hsiung Hon

    2006-10-01

    Full Text Available The ZnO:Al thin films were prepared by RF magnetron sputtering on Si substrateusing Pt as interdigitated electrodes. The structure was characterized by XRD and SEManalyses, and the ethanol vapor gas sensing as well as electrical properties have beeninvestigated and discussed. The gas sensing results show that the sensitivity for detecting400 ppm ethanol vapor was ~20 at an operating temperature of 250°C. The high sensitivity,fast recovery, and reliability suggest that ZnO:Al thin film prepared by RF magnetronsputtering can be used for ethanol vapor gas sensing.

  15. Fault detection, isolation, and diagnosis of status self-validating gas sensor arrays.

    Science.gov (United States)

    Chen, Yin-Sheng; Xu, Yong-Hui; Yang, Jing-Li; Shi, Zhen; Jiang, Shou-da; Wang, Qi

    2016-04-01

    The traditional gas sensor array has been viewed as a simple apparatus for information acquisition in chemosensory systems. Gas sensor arrays frequently undergo impairments in the form of sensor failures that cause significant deterioration of the performance of previously trained pattern recognition models. Reliability monitoring of gas sensor arrays is a challenging and critical issue in the chemosensory system. Because of its importance, we design and implement a status self-validating gas sensor array prototype to enhance the reliability of its measurements. A novel fault detection, isolation, and diagnosis (FDID) strategy is presented in this paper. The principal component analysis-based multivariate statistical process monitoring model can effectively perform fault detection by using the squared prediction error statistic and can locate the faulty sensor in the gas sensor array by using the variables contribution plot. The signal features of gas sensor arrays for different fault modes are extracted by using ensemble empirical mode decomposition (EEMD) coupled with sample entropy (SampEn). The EEMD is applied to adaptively decompose the original gas sensor signals into a finite number of intrinsic mode functions (IMFs) and a residual. The SampEn values of each IMF and the residual are calculated to reveal the multi-scale intrinsic characteristics of the faulty sensor signals. Sparse representation-based classification is introduced to identify the sensor fault type for the purpose of diagnosing deterioration in the gas sensor array. The performance of the proposed strategy is compared with other different diagnostic approaches, and it is fully evaluated in a real status self-validating gas sensor array experimental system. The experimental results demonstrate that the proposed strategy provides an excellent solution to the FDID of status self-validating gas sensor arrays.

  16. CO and CO2 dual-gas detection based on mid-infrared wideband absorption spectroscopy

    Science.gov (United States)

    Dong, Ming; Zhong, Guo-qiang; Miao, Shu-zhuo; Zheng, Chuan-tao; Wang, Yi-ding

    2018-03-01

    A dual-gas sensor system is developed for CO and CO2 detection using a single broadband light source, pyroelectric detectors and time-division multiplexing (TDM) technique. A stepper motor based rotating system and a single-reflection spherical optical mirror are designed and adopted for realizing and enhancing dual-gas detection. Detailed measurements under static detection mode (without rotation) and dynamic mode (with rotation) are performed to study the performance of the sensor system for the two gas samples. The detection period is 7.9 s in one round of detection by scanning the two detectors. Based on an Allan deviation analysis, the 1σ detection limits under static operation are 3.0 parts per million (ppm) in volume and 2.6 ppm for CO and CO2, respectively, and those under dynamic operation are 9.4 ppm and 10.8 ppm for CO and CO2, respectively. The reported sensor has potential applications in various fields requiring CO and CO2 detection such as in the coal mine.

  17. A Gas Cell Based on Hollow-Core Photonic Crystal Fiber (PCF and Its Application for the Detection of Greenhouse Gas (GHG: Nitrous Oxide (N2O

    Directory of Open Access Journals (Sweden)

    Jonas K. Valiunas

    2016-01-01

    Full Text Available The authors report the detection of nitrous oxide gas using intracavity fiber laser absorption spectroscopy. A gas cell based on a hollow-core photonic crystal fiber was constructed and used inside a fiber ring laser cavity as an intracavity gas cell. The fiber laser in the 1.55 μm band was developed using a polarization-maintaining erbium-doped fiber as the gain medium. The wavelength of the laser was selected by a fiber Bragg grating (FBG, and it matches one of the absorption lines of the gas under investigation. The laser wavelength contained multilongitudinal modes, which increases the sensitivity of the detection system. N2O gas has overtones of the fundamental absorption bands and rovibrational transitions in the 1.55 μm band. The system was operated at room temperature and was capable of detecting nitrous oxide gas at sub-ppmv concentration level.

  18. Fault Detection of Inline Reciprocating Diesel Engine: A Mass and Gas-Torque Approach

    Directory of Open Access Journals (Sweden)

    S. H. Gawande

    2012-01-01

    Full Text Available Early fault detection and diagnosis for medium-speed diesel engines are important to ensure reliable operation throughout the course of their service. This work presents an investigation of the diesel engine combustion-related fault detection capability of crankshaft torsional vibrations. Proposed methodology state the way of early fault detection in the operating six-cylinder diesel engine. The model of six cylinders DI Diesel engine is developed appropriately. As per the earlier work by the same author the torsional vibration amplitudes are used to superimpose the mass and gas torque. Further mass and gas torque analysis is used to detect fault in the operating engine. The DFT of the measured crankshaft’s speed, under steady-state operating conditions at constant load shows significant variation of the amplitude of the lowest major harmonic order. This is valid both for uniform operating and faulty conditions and the lowest harmonic orders may be used to correlate its amplitude to the gas pressure torque and mass torque for a given engine. The amplitudes of the lowest harmonic orders (0.5, 1, and 1.5 of the gas pressure torque and mass torque are used to map the fault. A method capable to detect faulty cylinder of operating Kirloskar diesel engine of SL90 Engine-SL8800TA type is developed, based on the phases of the lowest three harmonic orders.

  19. [Carbon monoxide gas detection system based on mid-infrared spectral absorption technique].

    Science.gov (United States)

    Li, Guo-Lin; Dong, Ming; Song, Nan; Song, Fang; Zheng, Chuan-Tao; Wang, Yi-Ding

    2014-10-01

    Based on infrared spectral absorption technique, a carbon monoxide (CO) detection system was developed using the fundamental absorption band at the wavelength of 4.6 μm of CO molecule and adopting pulse-modulated wideband incandescence and dual-channel detector. The detection system consists of pulse-modulated wideband incandescence, open ellipsoid light-collec- tor gas-cell, dual-channel detector, main-control and signal-processing module. By optimizing open ellipsoid light-collector gas- cell, the optical path of the gas absorption reaches 40 cm, and the amplitude of the electrical signal from the detector is 2 to 3 times larger than the original signal. Therefore, by using the ellipsoidal condenser, the signal-to-noise ratio of the system will be to some extent increased to improve performance of the system. With the prepared standard CO gas sample, sensing characteris- tics on CO gas were investigated. Experimental results reveal that, the limit of detection (LOD) is about 10 ppm; the relative er- ror at the LOD point is less than 14%, and that is less than 7. 8% within the low concentration range of 20~180 ppm; the maxi- mum absolute error of 50 min long-term measurement concentration on the 0 ppm gas sample is about 3 ppm, and the standard deviation is as small as 0. 18 ppm. Compared with the CO detection systems utilizing quantum cascaded lasers (QCLs) and dis- tributed feedback lasers (DFBLs), the proposed sensor shows potential applications in CO detection under the circumstances of coal-mine and environmental protection, by virtue of high performance-cost ratio, simple optical-path structure, etc.

  20. 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.

  1. Phytotoxic volatiles in the roots and shoots of Artemisia tridentata as detected by headspace solid-phase microextraction and gas chromatographic-mass spectrometry analysis.

    Science.gov (United States)

    Jassbi, Amir Reza; Zamanizadehnajari, Simin; Baldwin, Ian Thomas

    2010-12-01

    In the vicinity of big sagebrush (Artemisia tridentata), the growth of Nicotiana attenuata is negatively affected, in part due to the alleopathic effect of methyl jasmonate (MeJA) which is produced in large quantities by the aerial parts of sagebrush. Preliminary experiments suggested that growth-inhibiting substances were being emitted from the sagebrush roots. To identify the allelochemical secondary metabolites, we tested different root extracts in seedling growth bioassays with the naturally co-occurring native tobacco, Nicotiana attenuata, in a two-chamber Petri dish assay, optimized for tests of volatiles. Fractions rich in volatile compounds were particularly phytotoxic. We analyzed the volatiles emitted from the roots of intact Artemisia tridentata plants grown in soil, sand, and hydroponic cultures by using dynamic headspace extraction, headspace solvent-microextraction (HSME) and headspace solid-phase microextraction (HSPME), and GC-MS. Camphor, 1,8-cineol, nerol, and neryl isovalerate were phytotoxic and released as the major constituents. In addition to the phytotoxic monoterpenes, himachalenes, longifolene, caryophyllene, and acetylenic spiroethers, were found as characteristic components in the root's volatiles. The allelopathic potential of these root volatiles was compared with that of methyl jasmonate (MeJA), one of the most active compounds emitted from above-ground parts of the plant.

  2. Gas detection in sands of high silt-clay content in the Cook Inlet area

    International Nuclear Information System (INIS)

    Bettis, F.

    1976-01-01

    When a sand contains a large amount of silt and clay it is often difficult to detect zones that contain gas using only the Archie Saturation Relationship. However, gas may be detected in these shaly formations using certain quick-look techniques. Log examples of these are presented in this paper. The first quick-look technique is an overlay of the neutron log on a density log. The neutron log is shifted relative to the density log to make the two porosity curves track in shaly water sands. Gas-bearing intervals become readily apparent from separations of the two curves where the density porosity is reading higher than the shifted neutron porosity. The second is an overlay of a neutron log on the sonic interval-transit-time log. The sonic log is shifted so as to match the neutron log in average tight sands in the section. This method has proved to be more optimistic than the density-neutron overlay above. It will find the gas-bearing zones, but may result in testing a zone or two which is nonproductive. The third method, used when no neutron log has been run, is a crossplot of the difference, sonic porosity minus density porosity, versus gamma ray API units. This is the most unreliable of the three methods because of the difficulty of determining the end points and the slope of the line on the plot which separates the gas zones from the non-gas zones

  3. Toward Adequate Operation of Amorphous Oxide Thin-Film Transistors for Low-Concentration Gas Detection.

    Science.gov (United States)

    Kim, Kyung Su; Ahn, Cheol Hyoun; Jung, Sung Hyeon; Cho, Sung Woon; Cho, Hyung Koun

    2018-03-28

    We suggest the use of a thin-film transistor (TFT) composed of amorphous InGaZnO (a-IGZO) as a channel and a sensing layer for low-concentration NO 2 gas detection. Although amorphous oxide layers have a restricted surface area when reacting with NO 2 gas, such TFT sensors have incomparable advantages in the aspects of electrical stability, large-scale uniformity, and the possibility of miniaturization. The a-IGZO thin films do not possess typical reactive sites and grain boundaries, so that the variation in drain current of the TFTs strictly originates from oxidation reaction between channel surface and NO 2 gas. Especially, the sensing data obtained from the variation rate of drain current makes it possible to monitor efficiently and quickly the variation of the NO 2 concentration. Interestingly, we found that enhancement-mode TFT (EM-TFT) allows discrimination of the drain current variation rate at NO 2 concentrations ≤10 ppm, whereas a depletion-mode TFT is adequate for discriminating NO 2 concentrations ≥10 ppm. This discrepancy is attributed to the ratio of charge carriers contributing to gas capture with respect to total carriers. This capacity for the excellent detection of low-concentration NO 2 gas can be realized through (i) three-terminal TFT gas sensors using amorphous oxide, (ii) measurement of the drain current variation rate for high selectivity, and (iii) an EM mode driven by tuning the electrical conductivity of channel layers.

  4. An attempt to detect the greenhouse-gas signal in a transient GCM simulation

    International Nuclear Information System (INIS)

    Barnett, T.P.

    1990-01-01

    Results from the GISS model forced by transient greenhouse-gas (GHG) increases are used to demonstrate methods of detecting the theoretically predicted GHG signal. The signal predicted to occur in the surface temperature of the world's ocean since 1958 is not found in the observations but this is not surprising since the signal was small in the first place. The main result of the study is to demonstrate many of the key issues/difficulties that attend the detection problem

  5. EXTENDED PERFORMANCE HANDHELD AND MOBILE SENSORS FOR REMOTE DETECTION OF NATURAL GAS LEAKS

    Energy Technology Data Exchange (ETDEWEB)

    Michael B. Frish; B. David Green; Richard T. Wainner; Francesca Scire-Scappuzzo; Paul Cataldi; Matthew C. Laderer

    2005-05-01

    This report summarizes work performed by Physical Sciences Inc. (PSI) to advance the state-of-the-art of surveying for leaks of natural gas from transmission and distribution pipelines. The principal project goal was to develop means of deploying on an automotive platform an improved version of the handheld laser-based standoff natural gas leak detector previously developed by PSI and known as the Remote Methane Leak Detector or RMLD. A laser beam which interrogates the air for methane is projected from a spinning turret mounted upon a van. As the van travels forward, the laser beam scans an arc to the front and sides of the van so as to survey across streets and to building walls from a moving vehicle. When excess methane is detected within the arc, an alarm is activated. In this project, we built and tested a prototype Mobile RMLD (MRMLD) intended to provide lateral coverage of 10 m and one lateral scan for every meter of forward motion at forward speeds up to 10 m/s. Using advanced detection algorithms developed as part of this project, the early prototype MRMLD, installed on the back of a truck, readily detected simulated gas leaks of 50 liters per hour. As a supplement to the originally planned project, PSI also participated in a DoE demonstration of several gas leak detection systems at the Rocky Mountain Oilfield Testing Center (RMOTC) during September 2004. Using a handheld RMLD upgraded with the advanced detection algorithms developed in this project, from within a moving vehicle we readily detected leaks created along the 7.4 mile route of a virtual gas transmission pipeline.

  6. Fault Detection Using the Clustering-kNN Rule for Gas Sensor Arrays

    Directory of Open Access Journals (Sweden)

    Jingli Yang

    2016-12-01

    Full Text Available The k-nearest neighbour (kNN rule, which naturally handles the possible non-linearity of data, is introduced to solve the fault detection problem of gas sensor arrays. In traditional fault detection methods based on the kNN rule, the detection process of each new test sample involves all samples in the entire training sample set. Therefore, these methods can be computation intensive in monitoring processes with a large volume of variables and training samples and may be impossible for real-time monitoring. To address this problem, a novel clustering-kNN rule is presented. The landmark-based spectral clustering (LSC algorithm, which has low computational complexity, is employed to divide the entire training sample set into several clusters. Further, the kNN rule is only conducted in the cluster that is nearest to the test sample; thus, the efficiency of the fault detection methods can be enhanced by reducing the number of training samples involved in the detection process of each test sample. The performance of the proposed clustering-kNN rule is fully verified in numerical simulations with both linear and non-linear models and a real gas sensor array experimental system with different kinds of faults. The results of simulations and experiments demonstrate that the clustering-kNN rule can greatly enhance both the accuracy and efficiency of fault detection methods and provide an excellent solution to reliable and real-time monitoring of gas sensor arrays.

  7. Fault Detection Using the Clustering-kNN Rule for Gas Sensor Arrays

    Science.gov (United States)

    Yang, Jingli; Sun, Zhen; Chen, Yinsheng

    2016-01-01

    The k-nearest neighbour (kNN) rule, which naturally handles the possible non-linearity of data, is introduced to solve the fault detection problem of gas sensor arrays. In traditional fault detection methods based on the kNN rule, the detection process of each new test sample involves all samples in the entire training sample set. Therefore, these methods can be computation intensive in monitoring processes with a large volume of variables and training samples and may be impossible for real-time monitoring. To address this problem, a novel clustering-kNN rule is presented. The landmark-based spectral clustering (LSC) algorithm, which has low computational complexity, is employed to divide the entire training sample set into several clusters. Further, the kNN rule is only conducted in the cluster that is nearest to the test sample; thus, the efficiency of the fault detection methods can be enhanced by reducing the number of training samples involved in the detection process of each test sample. The performance of the proposed clustering-kNN rule is fully verified in numerical simulations with both linear and non-linear models and a real gas sensor array experimental system with different kinds of faults. The results of simulations and experiments demonstrate that the clustering-kNN rule can greatly enhance both the accuracy and efficiency of fault detection methods and provide an excellent solution to reliable and real-time monitoring of gas sensor arrays. PMID:27929412

  8. Tunnel-field-effect-transistor based gas-sensor: Introducing gas detection with a quantum-mechanical transducer

    Science.gov (United States)

    Sarkar, Deblina; Gossner, Harald; Hansch, Walter; Banerjee, Kaustav

    2013-01-01

    A gas-sensor based on tunnel-field-effect-transistor (TFET) is proposed that leverages the unique current injection mechanism in the form of quantum-mechanical band-to-band tunneling to achieve substantially improved performance compared to conventional metal-oxide-semiconductor field-effect-transistors (MOSFETs) for detection of gas species under ambient conditions. While nonlocal phonon-assisted tunneling model is used for detailed device simulations, in order to provide better physical insights, analytical formula for sensitivity is derived for both metal as well as organic conducting polymer based sensing elements. Analytical derivations are also presented for capturing the effects of temperature on sensor performance. Combining the developed analytical and numerical models, intricate properties of the sensor such as gate bias dependence of sensitivity, relationship between the required work-function modulation and subthreshold swing, counter-intuitive increase in threshold voltage for MOSFETs and reduction in tunneling probability for TFETs with temperature are explained. It is shown that TFET gas-sensors can not only lead to more than 10 000× increase in sensitivity but also provide design flexibility and immunity against screening of work-function modulation through non-specific gases as well as ensure stable operation under temperature variations.

  9. Flight Testing of an Advanced Airborne Natural Gas Leak Detection System

    Energy Technology Data Exchange (ETDEWEB)

    Dawn Lenz; Raymond T. Lines; Darryl Murdock; Jeffrey Owen; Steven Stearns; Michael Stoogenke

    2005-10-01

    ITT Industries Space Systems Division (Space Systems) has developed an airborne natural gas leak detection system designed to detect, image, quantify, and precisely locate leaks from natural gas transmission pipelines. This system is called the Airborne Natural Gas Emission Lidar (ANGEL) system. The ANGEL system uses a highly sensitive differential absorption Lidar technology to remotely detect pipeline leaks. The ANGEL System is operated from a fixed wing aircraft and includes automatic scanning, pointing system, and pilot guidance systems. During a pipeline inspection, the ANGEL system aircraft flies at an elevation of 1000 feet above the ground at speeds of between 100 and 150 mph. Under this contract with DOE/NETL, Space Systems was funded to integrate the ANGEL sensor into a test aircraft and conduct a series of flight tests over a variety of test targets including simulated natural gas pipeline leaks. Following early tests in upstate New York in the summer of 2004, the ANGEL system was deployed to Casper, Wyoming to participate in a set of DOE-sponsored field tests at the Rocky Mountain Oilfield Testing Center (RMOTC). At RMOTC the Space Systems team completed integration of the system and flew an operational system for the first time. The ANGEL system flew 2 missions/day for the duration for the 5-day test. Over the course of the week the ANGEL System detected leaks ranging from 100 to 5,000 scfh.

  10. Determination of daminozide residues in apples using gas chromatography with nitrogen-phosphorus detection

    NARCIS (Netherlands)

    Brinkman, J.H.W.; Dijk, A.G. van; Wagenaar, R.; Quirijns, J.K.

    1996-01-01

    A method was developed for the determination of daminozide in apples using gas chromatography (GC) with nitrogen-phosphorus detection (NPD). Daminozide is hydrolysed to 1,1-dimethylhydrazine (UDMH) by alkaline digestion. The UDMH generated is distilled from the apple matrix, derivatized with

  11. Soil-gas helium and surface-waves detection of fault zones in ...

    Indian Academy of Sciences (India)

    Soil-gas helium emanometry has been utilized in Wailapally watershed, near Hyderabad in southern India, for the detection of fracture and fault zones in a granite basement terrain having a thin regolith. Based on satellite imagery and geologic mapping, three sites were selected for detailed investigation. High spatial ...

  12. 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-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...... 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...

  13. Combined cation-exchange and extraction chromatographic method of pre-concentration and concomitant separation of Cu(II) with high molecular mass liquid cation exchanger after its online detection.

    Science.gov (United States)

    Mandal, B; Roy, U S; Datta, D; Ghosh, N

    2011-08-19

    A selective method has been developed for the extraction chromatographic trace level separation of Cu(II) with Versatic 10 (liquid cation exchanger) coated on silanised silica gel (SSG-V10). Cu(II) has been extracted from 0.1M acetate buffer at the range of pH 4.0-5.5. The effects of foreign ions, pH, flow-rate, stripping agents on extraction and elution have been investigated. Exchange capacity of the prepared exchanger at different temperatures with respect to Cu(II) has been determined. The extraction equilibrium constant (K(ex)) and different standard thermodynamic parameters have also been calculated by temperature variation method. Positive value of ΔH (7.98 kJ mol⁻¹) and ΔS (0.1916 kJ mol⁻¹) and negative value of ΔG (-49.16 kJ mol⁻¹) indicated that the process was endothermic, entropy gaining and spontaneous. Preconcentration factor was optimized at 74.7 ± 0.2 and the desorption constants K(desorption)¹(1.4 × 10⁻²) and K(desorption)²(9.8 × 10⁻²) were determined. The effect of pH on R(f) values in ion exchange paper chromatography has been investigated. In order to investigate the sorption isotherm, two equilibrium models, the Freundlich and Langmuir isotherms, were analyzed. Cu(II) has been separated from synthetic binary and multi-component mixtures containing various metal ions associated with it in ores and alloy samples. The method effectively permits sequential separation of Cu(II) from synthetic quaternary mixture containing its congeners Bi(III), Sn(II), Hg(II) and Cu(II), Cd(II), Pb(II) of same analytical group. The method was found effective for the selective detection, removal and recovery of Cu(II) from industrial waste and standard alloy samples following its preconcentration on the column. A plausible mechanism for the extraction of Cu(II) has been suggested. Copyright © 2011 Elsevier B.V. All rights reserved.

  14. Network coverage of the IMS noble gas component to detect nuclear explosions

    Energy Technology Data Exchange (ETDEWEB)

    Schoeppner, Michael [Institut fuer Friedensforschung und Sicherheitspolitik an der Universitaet Hamburg, Beim Schlump 83, 20144 Hamburg (Germany)

    2014-07-01

    The noble gas component of the International Monitoring System (IMS) is supposed to detect radioxenon fission products from nuclear explosions and thereby deliver proof of the nuclear character of suspicious events. In this work an approach is presented to determine the network coverage of the IMS {sup 133}Xe component. Various parameters that influence the network coverage are identified and included. The global radioxenon background from legitimate facilities has been simulated and the resulting impact on the IMS noble gas component calculated. From this background a station-specific detection criterion has been deducted. Furthermore, emissions from underground as well as surface test explosions of 1kt devices have been simulated for each grid point and time step of one year. The percentage of detectable nuclear explosions has been calculated and analysed for geographical and temporal variances.

  15. AIRBORNE, OPTICAL REMOTE SENSNG OF METHANE AND ETHANE FOR NATURAL GAS PIPELINE LEAK DETECTION

    Energy Technology Data Exchange (ETDEWEB)

    Jerry Myers

    2005-04-15

    Ophir Corporation was awarded a contract by the U. S. Department of Energy, National Energy Technology Laboratory under the Project Title ''Airborne, Optical Remote Sensing of Methane and Ethane for Natural Gas Pipeline Leak Detection'' on October 14, 2002. The scope of the work involved designing and developing an airborne, optical remote sensor capable of sensing methane and, if possible, ethane for the detection of natural gas pipeline leaks. Flight testing using a custom dual wavelength, high power fiber amplifier was initiated in February 2005. Ophir successfully demonstrated the airborne system, showing that it was capable of discerning small amounts of methane from a simulated pipeline leak. Leak rates as low as 150 standard cubic feet per hour (scf/h) were detected by the airborne sensor.

  16. Acoustic detection of seabed gas leaks, with application to Carbon Capture and Storage (CCS), and leak prevention for the oil and gas industry

    OpenAIRE

    Berges, B.J.P.

    2015-01-01

    The acoustic remote sensing of subsea gas leakage, applied to the monitoring of underwater gas discharges from anthropogenic and natural sources, is becoming increasingly important. First, as the oil and gas industry is facing increasing regulation, there is a need to put more control in the industrial process and to assess the impact on the marine environment. The applications are diverse, including: early warnings of "blow-out" from offshore installations, detection of leaks from underwater...

  17. Use of nonlocal helium microplasma for gas impurities detection by the collisional electron spectroscopy method

    Energy Technology Data Exchange (ETDEWEB)

    Kudryavtsev, Anatoly A., E-mail: akud@ak2138.spb.edu [St. Petersburg State University, 7-9 Universitetskaya nab., 199034 St. Petersburg (Russian Federation); Stefanova, Margarita S.; Pramatarov, Petko M. [Institute of Solid State Physics, Bulgarian Academy of Sciences, 72 Tzarigradsko Chaussee blvd., 1784 Sofia (Bulgaria)

    2015-10-15

    The collisional electron spectroscopy (CES) method, which lays the ground for a new field for analytical detection of gas impurities at high pressures, has been verified. The CES method enables the identification of gas impurities in the collisional mode of electron movement, where the advantages of nonlocal formation of the electron energy distribution function (EEDF) are fulfilled. Important features of dc negative glow microplasma and probe method for plasma diagnostics are applied. A new microplasma gas analyzer design is proposed. Admixtures of 0.2% Ar, 0.6% Kr, 0.1% N{sub 2}, and 0.05% CO{sub 2} are used as examples of atomic and molecular impurities to prove the possibility for detecting and identifying their presence in high pressure He plasma (50–250 Torr). The identification of the particles under analysis is made from the measurements of the high energy part of the EEDF, where maxima appear, resulting from the characteristic electrons released in Penning reactions of He metastable atoms with impurity particles. Considerable progress in the development of a novel miniature gas analyzer for chemical sensing in gas phase environments has been made.

  18. Suitability of selected chromatographic columns for analysis of fatty acids in dialyzed patients.

    Science.gov (United States)

    Pazda, Magdalena; Stepnowski, Piotr; Sledzinski, Tomasz; Chmielewski, Michal; Mika, Adriana

    2017-11-01

    Gas chromatography-mass spectrometry is a preferred method for fatty acid (FA) analysis in biofluids from patients with metabolic diseases. Complex characteristics of FAs make their analysis particularly challenging. Selection of an appropriate chromatographic column is particularly important component of the process as it provides optimal separation and detection of possibly all FAs present in the sample. However, no accurate protocol for comparative evaluation of capillary columns for the analysis of whole serum FA profile in patients with chronic kidney disease (CKD) has been developed thus far. Therefore, in the present study four columns were examined to select the one providing optimal separation and determination of FA profiles in this group of patients. Moreover, serum FA profiles obtained with the selected column in CKD patients subjected to peritoneal dialysis and healthy controls were compared. Thirty-seven component FAME Mix and sera from CKD patients were used to optimize chromatographic conditions and to select the most appropriate column. The ZB-5 column turned out to be the most appropriate for the analysis of whole FA profile in CKD patients' sera. Then, this column was used to compare FA profiles in patients subjected to peritoneal dialysis and in healthy controls. The analysis demonstrated many abnormalities in the FA profile of CKD patients. Further studies involving larger groups of patients presenting with other stages of CKD are required to explain the impact of the disease progression on composition of serum FAs. Copyright © 2017 John Wiley & Sons, Ltd.

  19. 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.

  20. DETECTION OF MOLECULAR GAS IN VOID GALAXIES: IMPLICATIONS FOR STAR FORMATION IN ISOLATED ENVIRONMENTS

    Energy Technology Data Exchange (ETDEWEB)

    Das, M.; Honey, M. [Indian Institute of Astrophysics, Bangalore (India); Saito, T. [Department of Astronomy, Graduate school of Science, The University of Tokyo, 7-3-1 Hongo, Bunkyo-ku, Tokyo 133-0033 (Japan); Iono, D. [Chile Observatory, NAOJ (Japan); Ramya, S., E-mail: mousumi@iiap.res.in [Shanghai Astronomical Observatory, Shanghai (China)

    2015-12-10

    We present the detection of molecular gas from galaxies located in nearby voids using the CO(1–0) line emission as a tracer. The observations were performed using the 45 m single dish radio telescope of the Nobeyama Radio Observatory. Void galaxies lie in the most underdense parts of our universe and a significant fraction of them are gas rich, late-type spiral galaxies. Although isolated, they have ongoing star formation but appear to be slowly evolving compared to galaxies in denser environments. Not much is known about their star formation properties or cold gas content. In this study, we searched for molecular gas in five void galaxies. The galaxies were selected based on their relatively high IRAS fluxes or Hα line luminosities, both of which signify ongoing star formation. All five galaxies appear to be isolated and two lie within the Bootes void. We detected CO(1–0) emission from four of the five galaxies in our sample and their molecular gas masses lie between 10{sup 8} and 10{sup 9} M{sub ⊙}. We conducted follow-up Hα imaging observations of three detected galaxies using the Himalayan Chandra Telescope and determined their star formation rates (SFRs) from their Hα fluxes. The SFR varies from 0.2 to 1 M{sub ⊙} yr{sup −1}; which is similar to that observed in local galaxies. Our study indicates that although void galaxies reside in underdense regions, their disks contain molecular gas and have SFRs similar to galaxies in denser environments. We discuss the implications of our results.

  1. Multiple chromatographic fingerprinting and its application to the quality control of herbal medicines

    Energy Technology Data Exchange (ETDEWEB)

    Fan Xiaohui [Pharmaceutical Informatics Institute, College of Pharmaceutical Sciences, Zhejiang University, Hangzhou 310027 (China); Cheng Yiyu [Pharmaceutical Informatics Institute, College of Pharmaceutical Sciences, Zhejiang University, Hangzhou 310027 (China)]. E-mail: chengyy@zju.edu.cn; Ye Zhengliang [Pharmaceutical Informatics Institute, College of Pharmaceutical Sciences, Zhejiang University, Hangzhou 310027 (China); Lin Ruichao [National Institute for the Control of Pharmaceutical and Biological Products, Beijing 100050 (China); Qian Zhongzhi [Committee of Chinese Pharmacopoeia, Beijing 100061 (China)

    2006-01-12

    Recently, chromatographic fingerprinting has become one of the most powerful approaches to quality control of herbal medicines. However, the performance of reported chromatographic fingerprinting constructed by single chromatogram sometimes turns out to be inadequate for complex herbal medicines, such as multi-herb botanical drug products. In this study, multiple chromatographic fingerprinting, which consists of more than one chromatographic fingerprint and represents the whole characteristics of chemical constitutions of the complex medicine, is proposed as a potential strategy in this complicated case. As a typical example, a binary chromatographic fingerprinting of 'Danshen Dropping Pill' (DSDP), the best-sold traditional Chinese medicine in China, was developed. First, two HPLC fingerprints that, respectively, represent chemical characteristics of depsides and saponins of DSDP were developed, which were used to construct binary chromatographic fingerprints of DSDP. Moreover, the authentication and validation of the binary fingerprints were performed. Then, a data-level information fusion method was employed to capture the chemical information encoded in two chromatographic fingerprints. Based on the fusion results, the lot-to-lot consistency and frauds can be determined either using similarity measure or by chemometrics approach. The application of binary chromatographic fingerprinting to consistency assessment and frauds detection of DSDP clearly demonstrated that the proposed method was a powerful approach to quality control of complex herbal medicines.

  2. Multiple chromatographic fingerprinting and its application to the quality control of herbal medicines

    International Nuclear Information System (INIS)

    Fan Xiaohui; Cheng Yiyu; Ye Zhengliang; Lin Ruichao; Qian Zhongzhi

    2006-01-01

    Recently, chromatographic fingerprinting has become one of the most powerful approaches to quality control of herbal medicines. However, the performance of reported chromatographic fingerprinting constructed by single chromatogram sometimes turns out to be inadequate for complex herbal medicines, such as multi-herb botanical drug products. In this study, multiple chromatographic fingerprinting, which consists of more than one chromatographic fingerprint and represents the whole characteristics of chemical constitutions of the complex medicine, is proposed as a potential strategy in this complicated case. As a typical example, a binary chromatographic fingerprinting of 'Danshen Dropping Pill' (DSDP), the best-sold traditional Chinese medicine in China, was developed. First, two HPLC fingerprints that, respectively, represent chemical characteristics of depsides and saponins of DSDP were developed, which were used to construct binary chromatographic fingerprints of DSDP. Moreover, the authentication and validation of the binary fingerprints were performed. Then, a data-level information fusion method was employed to capture the chemical information encoded in two chromatographic fingerprints. Based on the fusion results, the lot-to-lot consistency and frauds can be determined either using similarity measure or by chemometrics approach. The application of binary chromatographic fingerprinting to consistency assessment and frauds detection of DSDP clearly demonstrated that the proposed method was a powerful approach to quality control of complex herbal medicines

  3. PDMS membranes as sensing element in optical sensors for gas detection in water

    Directory of Open Access Journals (Sweden)

    Stefania Torino

    2017-11-01

    Full Text Available Polydimethylsiloxane (PDMS has been introduced the first time about 20years ago. This polymer is worldwide used for the rapid prototyping of microfluidic device through a replica molding process. However, the great popularity of PDMS is not only related to its easy processability, but also to its chemical and physical properties. For its interesting properties, the polymer has been implied for several applications, including sensing. In this work, we investigated how to use functionalized PDMS membranes as sensing elements in optical sensors for gas detection in water samples. Keywords: Polydimethylsiloxane (PDMS, Surface Plasmon Resonance (SPR sensors, Gas sensor

  4. Sulfate reducing bacteria detection in gas pipelines; Deteccao de bacterias redutoras de sulfato em gasodutos

    Energy Technology Data Exchange (ETDEWEB)

    Lutterbach, Marcia Teresa S.; Oliveira, Ana Lucia C. de; Cavalcanti, Eduardo H. de S. [Instituto Nacional de Tecnologia (INT), Rio de Janeiro, RJ (Brazil). Div. de Corrosao e Degradacao]. E-mails: marciasl@int.gov.br; analucia@int.gov.br; eduardoh@int.gov.br

    2004-07-01

    Microbiology induced corrosion (MIC) process associated with sulfate reducing bacteria (BRS) are one of the most important matter of concern for the oil and gas industry as 77% of failures have been attributed this sort of degradation. Corrosion products found present in gas transportation pipelines, the so-called 'black-powder' problem, are also a nuisance and source of economic losses for the gas industry. According to the literature, the incidence of black-powder can be ascribed to the metabolism of BRS that can be found in the gas environment. Integrity monitoring programs of gas pipelines adopt pigging as an important tool for internal corrosion monitoring. Solid residue such as the black-powder, collected by pigging, as well as the condensed, can be seen as a very valuable samples for microbiological analyses that can be used to detect and quantify bacteria related to the incidence of MIC processes. In the present work results concerning samples collected by pigging and condensed are presented. Small populations of viable BRS have been found in the pipeline. It can be seen that the inclusion of microbiological analyses of solid and liquid residues as a complementary action in the integrity monitoring programs adopted by gas transportation industry can be very helpful on the decision making concerning preventive and corrective actions to be taken in order to maintain the CIM processes under control. (author)

  5. Optical partial discharge diagnostic in SF6gas insulated system via multi-spectral detection.

    Science.gov (United States)

    Ren, Ming; Song, Bo; Zhuang, Tianxin; Yang, Shujing

    2018-02-20

    Light emitted from partial discharges (PDs) in SF 6 gas is investigated in the view point of insulation status diagnostics. Light intensity and integral spectrum of PD are proved to have significant correlations with PD activities and the involved dielectric interfaces. Based on synchronous light pulse detections in ultraviolet (UV), visible (VIS) and near-infrared (NIR) regions, the multispectral stochastic PD diagnosis is realized with more information beyond the conventional PD detections. The optical PD detection is also compared with ultra-high frequency (UHF) PD detection and acoustic emission (AE) PD detection in term of linearity, sensitivity and statistical property. Beyond that, a clustering analysis is performed on the multispectral photon counts of different conditions by quantifying them in a ternary diagram where some distinguishable regions emerge for PD recognition. Copyright © 2018 ISA. Published by Elsevier Ltd. All rights reserved.

  6. THIN FILM-BASED SENSOR FOR MOTOR VEHICLE EXHAUST GAS, NH3, AND CO DETECTION

    Directory of Open Access Journals (Sweden)

    S. Sujarwata

    2016-10-01

    Full Text Available A copper phthalocyanine (CuPc thin film based gas sensor with FET structure and channel length 100 μm has been prepared by VE method and lithography technique to detect NH3, motor cycle exhaust gases and CO. CuPc material layer was deposited on SiO2 by the vacuum evaporator (VE method at room temperature and pressure of 8 x10-4 Pa. The stages of manufacturing gas sensor were Si/SiO2 substrate blenching with ethanol in an ultrasonic cleaner, source, and drain electrodes deposition on the substrate by using a vacuum evaporator, thin film deposition between the source/drain and gate deposition. The sensor response times to NH3, motorcycle exhaust gases and CO were 75 s, 135 s, and 150, respectively. The recovery times were 90 s, 150 s and 225, respectively. It is concluded that the CuPc thin film-based gas sensor with FET structure is the best sensor to detect the NH3 gas.Sensor gas berbasis film tipis copper phthalocyanine (CuPc berstruktur FET dengan panjang channel 100 μm telah dibuatdengan metode VE dan teknik lithography untuk mendeteksi NH3 gas buang kendaraan bermotor dan CO. Lapisan bahan CuPc dideposisikan pada permukaan silikon dioksida (SiO2 dengan metode vacuum evaporator (VE pada temperatur ruang dengan tekanan 8 x10-4 Pa. Tahapan pembuatan sensor gas adalah pencucian substrat Si/SiO2 dengan etanol dalam ultrasonic cleaner, deposisi elektroda source dan drain di atas substrat dengan metode vacuum evaporator, deposisi film tipis diantara source/drain dan deposisi gate. Waktu tanggap sensor terhadap NH3, gas buang kendaraan bermotor dan CO berturut-turut adalah 75 s, 135 s,dan 150 s. Waktu pemulihan berturut-turut adalah 90 s, 150 s,dan 225 s. Disimpulkan bahwa sensor gas berstruktur FET berbasis film tipis CuPc merupakan sensor paling baik untuk mendeteksi adanya gas NH3.

  7. Is Optical Gas Imaging Effective for Detecting Fugitive Methane Emissions? - A Technological and Policy Perspective

    Science.gov (United States)

    Ravikumar, A. P.; Wang, J.; Brandt, A. R.

    2016-12-01

    Mitigating fugitive methane emissions from the oil and gas industry has become an important concern for both businesses and regulators. While recent studies have improved our understanding of emissions from all sectors of the natural gas supply chain, cost-effectively identifying leaks over expansive natural gas infrastructure remains a significant challenge. Recently, the Environmental Protection Agency (EPA) has recommended the use of optical gas imaging (OGI) technologies to be used in industry-wide leak detection and repair (LDAR) programs. However, there has been little to no systematic study of the effectiveness of infrared-camera-based OGI technology for leak detection applications. Here, we develop a physics-based model that simulates a passive infrared camera imaging a methane leak against varying background and ambient conditions. We verify the simulation tool through a series of large-volume controlled release field experiments wherein known quantities of methane were released and imaged from a range of distances. After simulator verification, we analyze the effects of environmental conditions like temperature, wind, and imaging background on the amount of methane detected from a statistically representative survey program. We also examine the effects of LDAR design parameters like imaging distance, leak size distribution, and gas composition. We show that imaging distance strongly affects leak detection - EPA's expectation of a 60% reduction in fugitive emissions based on a semi-annual LDAR survey will be realized only if leaks are imaged at a distance less than 10 m from the source under ideal environmental conditions. Local wind speed is also shown to be important. We show that minimum detection limits are 3 to 4 times higher for wet-gas compositions that contain a significant fraction of ethane and propane, resulting a significantly large leakage rate. We also explore the importance of `super-emitters' on the performance of an OGI-based leak

  8. 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

  9. 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

  10. Interface engineering: broadband light and low temperature gas detection abilities using a nano-heterojunction device.

    Science.gov (United States)

    Chang, Chien-Min; Hsu, Ching-Han; Liu, Yi-Wei; Chien, Tzu-Chiao; Sung, Chun-Han; Yeh, Ping-Hung

    2015-12-21

    Herein, we have designed a nano-heterojunction device using interface defects and band bending effects, which can have broadband light detection (from 365-940 nm) and low operating temperature (50 °C) gas detection abilities. The broadband light detection mechanism occurs because of the defects and band bending between the heterojunction interface. We have demonstrated this mechanism using CoSi2/SnO2, CoSi2/TiO2, Ge/SnO2 and Ge/TiO2 nano-heterojunction devices, and all these devices show broadband light detection ability. Furthermore, the nano-heterojunction of the nano-device has a local Joule-heating effect. For gas detection, the results show that the nano-heterojunction device presents a high detection ability. The reset time and sensitivity of the nano-heterojunction device are an order faster and larger than Schottky-contacted devices (previous works), which is due to the local Joule-heating effect between the interface of the nano-heterojunction. Based on the abovementioned idea, we can design diverse nano-devices for widespread use.

  11. Evaluation of an Interferometric Sensor for In-Space Detection of Gas Leaks

    Science.gov (United States)

    Polzin, Kurt A.; Korman, Valentin; Sinko, John; Hendrickson, Adam

    2009-01-01

    Space mission planning often involves long-term storage of volatile liquids or high-pressure gases. These may include cryogenic fuels and oxidizers, high-pressure gases, and life-support-critical consumables. The risk associated with the storage of fluids and gases in space systems has long been an issue and the ability to retain these fluids is often tied to mission success. A leak in the storage or distribution system can cause many different problems, including a simple, but mission endangering, loss of inventory or, in severe cases, unbalanced thrust loads on a flight vehicle. Cryogenic propellants are especially difficult to store, especially over a long duration. The propellant can boil off and be lost through the insulating walls of the tank or simple thermal cycling of the fittings, valves, and propellant feed lines may unseat seals allowing the fluid to escape. Current NASA missions call for long-duration in-space storage of propellants, oxidizers, and life support supplies. Leaks of a scale detectable through a pressure drop in the storage tank are often catastrophic and have long been the focus of ground-based mitigation efforts where redundant systems are often employed. However, there is presently no technology available for detecting and monitoring low-level, but still mission-endangering, gas leaks in space. Standard in-space gas detection methods either have a very limited pressure range over which they operate effectively or are limited to certain gases. Mass spectrometer systems are able to perform the detection tasks, but their size, mass and use of high voltage, which could potentially lead to an arc that ignites a combustible propellent, severely limit their usefulness in a space system. In this paper, we present results from testing of the light-based interferometric gas monitoring and leak detection sensor shown in Fig. 1. The output of the sensor is an interference fringe pattern that is a function of the gas density, and commensurate index

  12. Determination of ethylenethiourea in food commodities by a two-step derivatization method and gas chromatography with electron-capture and nitrogen-phosphorus detection.

    Science.gov (United States)

    Dubey, J K; Heberer, T; Stan, H J

    1997-03-21

    Ethylenethiourea (ETU) is a decomposition product from ethylene-bis-dithiocarbamates (EBDCs), the most widely used class of fungicides in the world. ETU has been classified as a possible human carcinogen. The maximum permitted residue level (MRL) in the European Union was set at 0.05 ppm. Gas chromatographic determination of ETU can be achieved only after derivatization. ETU is extracted from food samples and cleaned up by a combination of two-step derivatization and liquid-liquid partitioning. In the first step, ETU is derivatized with benzyl chloride to form S-benzyl ETU, which is then trifluoroacetylated to form the final product, which is amenable to GC. The determination is carried out with capillary gas chromatography using electron-capture (ECD) and nitrogen-phosphorus detection (NPD) as selective detection methods in parallel. The responses of ECD and NPD were found to be of the same order of magnitude. Therefore, the parallel response was found to be a useful criterion for peak identification down to the limit of detection. Reproducibility of the two-step derivatization of ETU to form trifluoroacetylated S-benzyl ETU was found to be satisfactory. The recoveries from apple, pear, tomato and a common baby food, at various concentration levels, were found to be between 82-92%, with a limit of detection of less than 1 ppb. Commercial samples, submitted for routine monitoring of dithiocarbamates (DTC) were also monitored in our laboratory for the presence of ETU. Four of the twenty samples found positive for DTC were also found to be contaminated with ETU in the range of 0.01 to 0.37 ppm. Three of these food samples were found to contain ETU residues above the MRL of 0.05, while those food samples containing DTC residues between 0.2 and 0.8 ppm were all below the MRL of DTC. No relation exists between the DTC residues concentration and the level of ETU. The screening data were further confirmed by electron impact mass spectrometry in selected ion monitoring

  13. CANDU pressure tube leak detection by annulus gas dew point measurement. A critical review

    Energy Technology Data Exchange (ETDEWEB)

    Greening, F.R. [CTS-NA, Tiverton, ON (Canada)

    2017-03-15

    In the event of a pressure tube leak from a small through-wall crack during CANDU reactor operations, there is a regulatory requirement - referred to as Leak Before Break (LBB) - for the licensee to demonstrate that there will be sufficient time for the leak to be detected and the reactor shut down before the crack grows to the critical size for fast-uncontrolled rupture. In all currently operating CANDU reactors, worldwide, this LBB requirement is met via continuous dew point measurements of the CO{sub 2} gas circulating in the reactor's Annulus Gas System (AGS). In this paper the historical development and current status of this leak detection capability is reviewed and the use of moisture injection tests as a verification procedure is critiqued. It is concluded that these tests do not represent AGS conditions that are to be expected in the event of a real pressure tube leak.

  14. Method for analysis of heavy sulphur compounds using gas chromatography with flame photometric detection

    OpenAIRE

    Moreira, N.; Pinho, P. Guedes de; Vasconcelos, I.

    2004-01-01

    A method for analysis of heavy sulphur compounds in wines, based on gas chromatography (GC) with flame photometric detection, is reported. Wine samples preparation includes a dichloromethane liquid–liquid extraction followed by concentration under a nitrogen atmosphere. The extracted fraction was also analysed by GC–mass spectrometry. The method enables high recovery of sulphur compounds in wine and satisfies the requirements of repeatability and sensitivity. Applications of the meth...

  15. Wavelength modulation spectroscopy--digital detection of gas absorption harmonics based on Fourier analysis.

    Science.gov (United States)

    Mei, Liang; Svanberg, Sune

    2015-03-20

    This work presents a detailed study of the theoretical aspects of the Fourier analysis method, which has been utilized for gas absorption harmonic detection in wavelength modulation spectroscopy (WMS). The lock-in detection of the harmonic signal is accomplished by studying the phase term of the inverse Fourier transform of the Fourier spectrum that corresponds to the harmonic signal. The mathematics and the corresponding simulation results are given for each procedure when applying the Fourier analysis method. The present work provides a detailed view of the WMS technique when applying the Fourier analysis method.

  16. Rapid quantitative detection of glucose content in glucose injection by reaction headspace gas chromatography.

    Science.gov (United States)

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

    2017-10-20

    This work investigates an automated technique for rapid detecting the glucose content in glucose injection by reaction headspace gas chromatography (HS-GC). This method is based on the oxidation reaction of glucose in glucose injection with potassium dichromate. The carbon dioxide (CO 2 ) formed from the oxidation reaction can be quantitatively detected by GC. The results show that the relative standard deviation (RSD) of the present method was within 2.91%, and the measured glucose contents in glucose injection closely match those quantified by the reference method (relative differences glucose content in glucose injection related applications. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. Detection of outliers by neural network on the gas centrifuge experimental data of isotopic separation process

    International Nuclear Information System (INIS)

    Andrade, Monica de Carvalho Vasconcelos

    2004-01-01

    This work presents and discusses the neural network technique aiming at the detection of outliers on a set of gas centrifuge isotope separation experimental data. In order to evaluate the application of this new technique, the result obtained of the detection is compared to the result of the statistical analysis combined with the cluster analysis. This method for the detection of outliers presents a considerable potential in the field of data analysis and it is at the same time easier and faster to use and requests very less knowledge of the physics involved in the process. This work established a procedure for detecting experiments which are suspect to contain gross errors inside a data set where the usual techniques for identification of these errors cannot be applied or its use/demands an excessively long work. (author)

  18. Determination of acoustic speed for improving leak detection and location in gas pipelines.

    Science.gov (United States)

    Li, Shuaiyong; Wen, Yumei; Li, Ping; Yang, Jin; Yang, Lili

    2014-02-01

    The commonly used cross-correlation technique for leak location requires that the acoustic speed is known and invariable. In practice, the gas leakage-induced acoustic waves propagate along multiple paths including in-pipe gas and pipe wall, and the acoustic waves in different transmission paths exhibit different acoustic speeds and different dispersive behaviors, which bring a great challenge for leak detection and location in the gas pipelines. In this study, based on the vibration theory of cylindrical elastic thin shell, the wavenumber formulae in different transmission paths are derived to predict the acoustic speeds and the acoustical coupling between the in-pipe gas and the pipe wall is analyzed to determine the dominant transmission path. In addition, the velocity dispersions in the dominant transmission path are suppressed by selection of a characteristic frequency band of the gas leakage-induced acoustic waves. The theoretical predictions are verified in the experiment and the results show that the theoretical acoustic speed is slightly larger than the measured acoustic speed. Thus, the theoretical acoustic speed formula is modified considering the effect of the structural loss factor and consequently the location error using the modified acoustic speed is reduced by two times compared to that using the theoretical acoustic speed.

  19. Gas Hydrates Accumulations on the South Shetland Continental Margin: New Detection Possibilities

    Directory of Open Access Journals (Sweden)

    V. D. Solovyov

    2011-01-01

    Full Text Available The results of investigations in 2006–2010 for hydrocarbon and gas hydrates on the Antarctic Peninsula continental margin are given. In 2004 and 2006, the marine geoelectric researches by methods of forming a short-pulsed electromagnetic field (FSPEF and vertical electric-resonance sounding (VERS had been conducted in this region. The “deposit” type anomaly was mapped by FSPEF survey, and anomalous polarized layers of “hydrocarbon deposit” type were chosen by VERS sounding within this anomaly on Antarctic margin in the region of UAS “Academician Vernadsky.” Anomalous zones of “gas hydrate deposit” type were detected on the South Shetland margin due to the special technology of satellite data processing and interpretation using. These results confirm the high gas hydrates potential of the West Antarctica region. Some practical results of the experimental approbation of these original technologies for the “direct” prospecting and exploration of hydrocarbon (HC and gas hydrates accumulations in different oil-and-gas bearing basins of Russia and Gulf of Mexico are proposed. The integration of satellite data processing and materials of FSPEF-VERS methods enable improving their efficiency for different geological and geophysical problems solving.

  20. Quantitation of dissolved gas content in emulsions and in blood using mass spectrometric detection

    Science.gov (United States)

    Grimley, Everett; Turner, Nicole; Newell, Clayton; Simpkins, Cuthbert; Rodriguez, Juan

    2011-01-01

    Quantitation of dissolved gases in blood or in other biological media is essential for understanding the dynamics of metabolic processes. Current detection techniques, while enabling rapid and convenient assessment of dissolved gases, provide only direct information on the partial pressure of gases dissolved in the aqueous fraction of the fluid. The more relevant quantity known as gas content, which refers to the total amount of the gas in all fractions of the sample, can be inferred from those partial pressures, but only indirectly through mathematical modeling. Here we describe a simple mass spectrometric technique for rapid and direct quantitation of gas content for a wide range of gases. The technique is based on a mass spectrometer detector that continuously monitors gases that are rapidly extracted from samples injected into a purge vessel. The accuracy and sample processing speed of the system is demonstrated with experiments that reproduce within minutes literature values for the solubility of various gases in water. The capability of the technique is further demonstrated through accurate determination of O2 content in a lipid emulsion and in whole blood, using as little as 20 μL of sample. The approach to gas content quantitation described here should greatly expand the range of animals and conditions that may be used in studies of metabolic gas exchange, and facilitate the development of artificial oxygen carriers and resuscitation fluids. PMID:21497566

  1. Data-driven fault detection, isolation and estimation of aircraft gas turbine engine actuator and sensors

    Science.gov (United States)

    Naderi, E.; Khorasani, K.

    2018-02-01

    In this work, a data-driven fault detection, isolation, and estimation (FDI&E) methodology is proposed and developed specifically for monitoring the aircraft gas turbine engine actuator and sensors. The proposed FDI&E filters are directly constructed by using only the available system I/O data at each operating point of the engine. The healthy gas turbine engine is stimulated by a sinusoidal input containing a limited number of frequencies. First, the associated system Markov parameters are estimated by using the FFT of the input and output signals to obtain the frequency response of the gas turbine engine. These data are then used for direct design and realization of the fault detection, isolation and estimation filters. Our proposed scheme therefore does not require any a priori knowledge of the system linear model or its number of poles and zeros at each operating point. We have investigated the effects of the size of the frequency response data on the performance of our proposed schemes. We have shown through comprehensive case studies simulations that desirable fault detection, isolation and estimation performance metrics defined in terms of the confusion matrix criterion can be achieved by having access to only the frequency response of the system at only a limited number of frequencies.

  2. Research and Development of Non-Spectroscopic MEMS-Based Sensor Arrays for Targeted Gas Detection

    Energy Technology Data Exchange (ETDEWEB)

    Loui, A; McCall, S K

    2011-10-24

    The ability to monitor the integrity of gas volumes is of interest to the stockpile surveillance community. Specifically, the leak detection of noble gases, at relevant concentration ranges and distinguished from other chemical species that may be simultaneously present, is particularly challenging. Aside from the laboratory-based method of gas chromatography-mass spectrometry (GC-MS), where samples may be collected by solid-phase microextraction (SPME) or cryofocusing, the other major approaches for gas-phase detection employ lasers typically operating in the mid-infrared wavelength region. While mass spectrometry can readily detect noble gases - the helium leak detector is an obvious example - laser-based methods such as infrared (IR) or Raman spectroscopy are completely insensitive to them as their monatomic nature precludes a non-zero dipole moment or changes in polarizability upon excitation. Therefore, noble gases can only be detected by one of two methods: (1) atomic emission spectroscopies which require the generation of plasmas through laser-induced breakdown, electrical arcing, or similar means; (2) non-spectroscopic methods which measure one or more physical properties (e.g., mass, thermal conductivity, density). In this report, we present our progress during Fiscal Year 2011 (FY11) in the research and development of a non-spectroscopic method for noble gas detection. During Fiscal Year 2010 (FY10), we demonstrated via proof-of-concept experiments that the combination of thermal conductivity detection (TCD) and coating-free damped resonance detection (CFDRD) using micro-electromechanical systems (MEMS) could provide selective sensing of these inert species. Since the MEMS-based TCD technology was directly adapted from a brassboard prototype commissioned by a previous chemical sensing project, FY11 efforts focused on advancing the state of the newer CFDRD method. This work, guided by observations previously reported in the open literature, has not only

  3. Research on Ground-Based LWIR Hyperspectral Imaging Remote Gas Detection.

    Science.gov (United States)

    Zheng, Wei-jian; Lei, Zheng-gang; Yu, Chun-chao; Yang, Zhi-xiong; Wang, Hai-yangi; Fu, Yan-peng; Li, Xun-niu; Liao, Ning-fang; Su, Jun-hong

    2016-02-01

    The new progress of ground-based long-wave infrared remote sensing is presented, which describes the windowing spatial and temporal modulation Fourier spectroscopy imaging in details. The prototype forms the interference fringes based on the corner-cube of spatial modulation of Michelson interferometer, using cooled long-wave infrared photovoltaic staring FPA (focal plane array) detector. The LWIR hyperspectral imaging is achieved by the process of collection, reorganization, correction, apodization, FFT etc. from data cube. Noise equivalent spectral radiance (NESR), which is the sensitivity index of CHIPED-1 LWIR hyperspectral imaging prototype, can reach 5.6 x 10⁻⁸ W · (cm⁻¹ · sr · cm²)⁻¹ at single sampling. The data is the same as commercial temporal modulation hyperspectral imaging spectrometer. It can prove the advantage of this technique. This technique still has space to be improved. For instance, spectral response range of CHIPED-1 LWIR hyperspectral imaging prototype can reach 11. 5 µm by testing the transmission curve of polypropylene film. In this article, choosing the results of outdoor high-rise and diethyl ether gas experiment as an example, the authors research on the detecting method of 2D distribution chemical gas VOC by infrared hyperspectral imaging. There is no observed diethyl ether gas from the infrared spectral slice of the same wave number in complicated background and low concentration. By doing the difference spectrum, the authors can see the space distribution of diethyl ether gas clearly. Hyperspectral imaging is used in the field of organic gas VOC infrared detection. Relative to wide band infrared imaging, it has some advantages. Such as, it has high sensitivity, the strong anti-interference ability, identify the variety, and so on.

  4. Leak before break detection-annulus gas monitoring system evolution and operating experience at KGS

    International Nuclear Information System (INIS)

    Jain, D.D.; Sanathkumar, V.V.; Ramamurthy, K.; Nageswara Rao, G.

    2002-01-01

    Full text: Pressurised heavy water reactors (PHWR) at RAPS 1 and 2 and MAPS have provision for detection of pressure tube leak by indirect method. The reactor vessel (calandria) is housed in calandria vault (C/V) filled with air and C/V moisture element indicates the water leak from calandria tube or pressure tube. Further, detection of leak is a cumbersome process. From NAPS onwards, calandria is housed in C/V filled with water, annulus between calandria tube and pressure tube is filled with CO 2 and annulus gas monitoring system (AGMS) is provided by design for detection of any pressure tube leak. The design was improved and AGMS for Kaiga 1 and 2 and RAPS 3 and 4 is having re-circulation mode of operation. The design provides for monitoring dew point of annulus gas (CO 2 ) for indicating the leak and later to identify the pressure tube/calandria tube having leak. The paper deals with operating experience of AGMS at Kaiga generating station (KGS). During the commissioning and initial power operation at KGS, problems were encountered in re-circulation mode. These problems were high radiation field near AGMS piping, high temperature on blower body, blower bearing failure and system leaks. Design modifications were carried out for effective performance of the system for detecting leak before break

  5. Research on fiber-optic cantilever-enhanced photoacoustic spectroscopy for trace gas detection

    Science.gov (United States)

    Chen, Ke; Zhou, Xinlei; Gong, Zhenfeng; Yu, Shaochen; Qu, Chao; Guo, Min; Yu, Qingxu

    2018-01-01

    We demonstrate a new scheme of cantilever-enhanced photoacoustic spectroscopy, combining a sensitivity-improved fiber-optic cantilever acoustic sensor with a tunable high-power fiber laser, for trace gas detection. The Fabry-Perot interferometer based cantilever acoustic sensor has advantages such as high sensitivity, small size, easy to install and immune to electromagnetic. Tunable erbium-doped fiber ring laser with an erbium-doped fiber amplifier is used as the light source for acoustic excitation. In order to improve the sensitivity for photoacoustic signal detection, a first-order longitudinal resonant photoacoustic cell with the resonant frequency of 1624 Hz and a large size cantilever with the first resonant frequency of 1687 Hz are designed. The size of the cantilever is 2.1 mm×1 mm, and the thickness is 10 μm. With the wavelength modulation spectrum and second-harmonic detection methods, trace ammonia (NH3) has been measured. The gas detection limits (signal-to-noise ratio = 1) near the wavelength of 1522.5 nm is achieved to be 3 ppb.

  6. A Survey on Gas Sensing Technology

    Directory of Open Access Journals (Sweden)

    Huansheng Ning

    2012-07-01

    Full Text Available Sensing technology has been widely investigated and utilized for gas detection. Due to the different applicability and inherent limitations of different gas sensing technologies, researchers have been working on different scenarios with enhanced gas sensor calibration. This paper reviews the descriptions, evaluation, comparison and recent developments in existing gas sensing technologies. A classification of sensing technologies is given, based on the variation of electrical and other properties. Detailed introduction to sensing methods based on electrical variation is discussed through further classification according to sensing materials, including metal oxide semiconductors, polymers, carbon nanotubes, and moisture absorbing materials. Methods based on other kinds of variations such as optical, calorimetric, acoustic and gas-chromatographic, are presented in a general way. Several suggestions related to future development are also discussed. Furthermore, this paper focuses on sensitivity and selectivity for performance indicators to compare different sensing technologies, analyzes the factors that influence these two indicators, and lists several corresponding improved approaches.

  7. Selective detection of carbon-13, nitrogen-15, and deuterium labeled metabolites by capillary gas chromatography-chemical reaction interface/mass spectrometry

    International Nuclear Information System (INIS)

    Chace, D.H.; Abramson, F.P.

    1989-01-01

    We have applied a new chemical reaction interface/mass spectrometer technique (CRIMS) to the selective detection of 13C-, 15N-, and 2H-labeled phenytoin and its metabolites in urine following separation by capillary gas chromatography. The microwave-powered chemical reaction interface converts materials from their original forms into small molecules whose mass spectra serve to identify and quantify the nuclides that make up each analyte. The presence of each element is followed by monitoring the isotopic variants of CO2, NO, or H2 that are produced by the chemical reaction interface. Chromatograms showing only enriched 13C and 15N were produced by subtracting the abundance of naturally occurring isotopes from the observed M + 1 signal. A selective chromatogram of 2H (D) was obtained by measuring HD at m/z 3.0219 with a resolution of 2000. Metabolites representing less than 1.5% of the total labeled compounds could be identified in the chromatogram. Detection limits from urine of 380 pg/mL of a 15N-labeled metabolite, 7 ng/mL of a 13C-labeled metabolite, and 16 ng/mL of a deuterium labeled metabolite were determined at a signal to noise ratio of 2. Depending on the isotope examined, a linear dynamic range of 250-1000 was observed using CRIMS. To identify many of these labeled peaks (metabolites), the chromatographic analysis was repeated with the chemical reaction interface turned off and mass spectra obtained at the retention times found in the CRIMS experiment. CRIMS is a new analytical method that appears to be particularly useful for metabolism studies

  8. Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory : determination of organophosphate pesticides in bottom sediment by gas chromatography with flame photometric detection

    Science.gov (United States)

    Jha, Virendra Kumar; Wydoski, Duane S.

    2003-01-01

    A method for the isolation of 20 parent organophosphate pesticides and 5 pesticide degradates from bottom-sediment samples is described. The compound O-ethyl-O-methyl-S-proplyphosphorothioate is reported as an estimated concentration because of variable performance. In this method, the sediment samples are centrifuged to remove excess waster mixed with anhydrous sodium sulfate and Soxhlet extracted overnight with dichloromethane (93 percent) and methanol (7 percent). The extract is concentrated and then filtered through a 0.2-micrometer polytetrafluoroethylene membrane syringe filter. An aliquot of the sample extract is quantitatively injected onto two polystyrene-divinylbenzene gel-permeation chromatographic columns connected in series. The compounds are eluted with dichloromethane and a fraction is collected for analysis, with some coextracted interferences, including elemental sulfur, separated and discarded. The aliquot is concentrated and solvent exchanged to ethyl acetate. The extract is analyzed by dual capillary-column gas chromatography with flame photometric detection. Single-operator method detection limits in sodium sulfate matrix samples ranged from 0.81 to 2 micrograms per kilogram. Method performance was validated by spiking all compounds into three different solid matrices (sodium sulfate, bed sediment from Clear Creek, and bed sediment from Evergreen Lake) at three different concentrations. Eight replicates were analyzed at each concentration in each matrix. Mean recoveries of method compounds spiked in Clear Creek samples ranged from 43 to 110 percent, and those in Evergreen Lake samples ranged from 62 to 118 percent for all pesticides. Mean recoveries of method compounds spiked in reagent sodium sulfate samples ranged from 41 to 101 percent for all pesticides. The only exception was O-ethyl-O-methyl-S-propylphosphorothioate, which had an average recovery of 35 percent, and, thus, sample concentration is reported as estimated ('E' remark code).

  9. Method for detection of trace metal and metalloid contaminants in coal-generated fuel gas using gas chromatography/ion trap mass spectrometry.

    Science.gov (United States)

    Rupp, Erik C; Granite, Evan J; Stanko, Dennis C

    2010-07-15

    There exists an increasing need to develop a reliable method to detect trace contaminants in fuel gas derived from coal gasification. While Hg is subject to current and future regulations, As, Se, and P emissions may eventually be regulated. Sorbents are the most promising technology for the removal of contaminants from coal-derived fuel gas, and it will be important to develop a rapid analytical detection method to ensure complete removal and determine the ideal time for sorbent replacement/regeneration in order to reduce costs. This technical note explores the use of a commercial gas chromatography/ion trap mass spectrometry system for the detection of four gaseous trace contaminants in a simulated fuel gas. Quantitative, repeatable detection with limits at ppbv to ppmv levels were obtained for arsine (AsH(3)), phosphine (PH(3)), and hydrogen selenide (H(2)Se), while qualitative detection was observed for mercury. Decreased accuracy and response caused by the primary components of fuel gas were observed.

  10. Detecting naphthenic acids in waters by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Merlin, Mireya; Guigard, Selma E; Fedorak, Phillip M

    2007-01-26

    Naphthenic acids (general formula C(n)H(2n+Z)O(2)) are water-soluble, toxic compounds found in petroleum and bitumen. Some of the current methods for detecting these acids in waters depend on measuring the presence of the carboxylic acid functional group, and therefore many of these methods also detect naturally occurring carboxylic acids that are not naphthenic acids. We report a procedure that includes liquid-liquid extraction, cleanup, and derivatization to form t-butyldimethylsilyl esters prior to gas chromatography-mass spectrometry (GC-MS) analysis. Using low- and high-resolution MS to detect the ion C(15)H(27)O(2)Si(+) (nominal m/z=267) is an excellent indicator of the presence of naphthenic acids at concentrations > or =10microgL(-1).

  11. A Portable Array-Type Optical Fiber Sensing Instrument for Real-Time Gas Detection.

    Science.gov (United States)

    Hung, San-Shan; Chang, Hsing-Cheng; Chang, I-Nan

    2016-12-08

    A novel optical fiber array-type of sensing instrument with temperature compensation for real-time detection was developed to measure oxygen, carbon dioxide, and ammonia simultaneously. The proposed instrument is multi-sensing array integrated with real-time measurement module for portable applications. The sensing optical fibers were etched and polished before coating to increase sensitivities. The ammonia and temperature sensors were each composed of a dye-coated single-mode fiber with constructing a fiber Bragg grating and a long-period filter grating for detecting light intensity. Both carbon dioxide and oxygen sensing structures use multimode fibers where 1-hydroxy-3,6,8-pyrene trisulfonic acid trisodium salt is coated for carbon dioxide sensing and Tris(2,2'-bipyridyl) dichlororuthenium(II) hexahydrate and Tris(bipyridine)ruthenium(II) chloride are coated for oxygen sensing. Gas-induced fluorescent light intensity variation was applied to detect gas concentration. The portable gas sensing array was set up by integrating with photo-electronic measurement modules and a human-machine interface to detect gases in real time. The measured data have been processed using piecewise-linear method. The sensitivity of the oxygen sensor were 1.54%/V and 9.62%/V for concentrations less than 1.5% and for concentrations between 1.5% and 6%, respectively. The sensitivity of the carbon dioxide sensor were 8.33%/V and 9.62%/V for concentrations less than 2% and for concentrations between 2% and 5%, respectively. For the ammonia sensor, the sensitivity was 27.78%/V, while ammonia concentration was less than 2%.

  12. A Portable Array-Type Optical Fiber Sensing Instrument for Real-Time Gas Detection

    Directory of Open Access Journals (Sweden)

    San-Shan Hung

    2016-12-01

    Full Text Available A novel optical fiber array-type of sensing instrument with temperature compensation for real-time detection was developed to measure oxygen, carbon dioxide, and ammonia simultaneously. The proposed instrument is multi-sensing array integrated with real-time measurement module for portable applications. The sensing optical fibers were etched and polished before coating to increase sensitivities. The ammonia and temperature sensors were each composed of a dye-coated single-mode fiber with constructing a fiber Bragg grating and a long-period filter grating for detecting light intensity. Both carbon dioxide and oxygen sensing structures use multimode fibers where 1-hydroxy-3,6,8-pyrene trisulfonic acid trisodium salt is coated for carbon dioxide sensing and Tris(2,2′-bipyridyl dichlororuthenium(II hexahydrate and Tris(bipyridineruthenium(II chloride are coated for oxygen sensing. Gas-induced fluorescent light intensity variation was applied to detect gas concentration. The portable gas sensing array was set up by integrating with photo-electronic measurement modules and a human-machine interface to detect gases in real time. The measured data have been processed using piecewise-linear method. The sensitivity of the oxygen sensor were 1.54%/V and 9.62%/V for concentrations less than 1.5% and for concentrations between 1.5% and 6%, respectively. The sensitivity of the carbon dioxide sensor were 8.33%/V and 9.62%/V for concentrations less than 2% and for concentrations between 2% and 5%, respectively. For the ammonia sensor, the sensitivity was 27.78%/V, while ammonia concentration was less than 2%.

  13. Fingerprinting of the volatile fraction from selected thyme species by means of headspace gas chromatography with mass spectrometric detection.

    Science.gov (United States)

    Staszek, Dorota; Orłowska, Marta; Rzepa, Józef; Wróbel, Michał S; Kowalska, Teresa; Szymczak, Grażyna; Waksmundzka-Hajnos, Monika

    2014-01-01

    The Thymus genus has a firm position in Mediterranean folk medicine and culinary tradition, and yet certain confusion is observed in its botanical taxonomy. Therefore, chemical analysis of secondary metabolites and selection of reliable chemotaxonomic markers can prove helpful. In this study, the volatile fraction derived from 20 different thyme specimens was analyzed by means of headspace GC with MS detection. From the obtained chromatographic fingerprints, the diversity of the volatile fraction originating from the different thyme species clearly emerged. Identification of volatile components was based on a software library of mass spectra. There was only one common component derived from all 20 investigated thyme species, i.e., ß-linalool. For three different Thymus species, a comparison was made of the performance of the headspace extraction and hydrodistillation. Characteristic differences in composition of the volatile fraction obtained with use of these two techniques were discussed. Finally, the obtained chromatographic fingerprints of the volatile fraction were analyzed by means of a chemometric approach (principal component analysis), in order to trace similarities in their chemical composition.

  14. Detection of solvent losses (entrainment) in gas streams of process vessels using radioisotope tracing techniques

    International Nuclear Information System (INIS)

    Wan Zakaria Wan Muhamad Tahir; Juhari Mohd Yusof

    2002-01-01

    Liquid droplets (MDEA aqueous solution) entrained in the gas streams can cause severe problems on chemical plants. On-line detection of liquid entrainment (carry over) into gas streams from process vessel is investigated using radioisotope iodine ( 131 I). In order to obtain information on whether there is any carry-over of MDEA in the vapour space leaving from the process system, a number of test and calibration injections involving the released of certain amount of tracer activity (mCi) at the inlet and overhead lines of the process vessels were made using a special injection device. MDEA solvent- tagged tracer in the overhead line of the designated process vessels was monitored using radiation scintillation detectors mounted externally at specified locations of the vessels. Output pulses (response curves) with respect to time of measurements from all detectors were plotted and analysed for the finger prints of solvent losses leaving the vessels. From this study, no distinguishable peaks were detected at the outlet vessels of the overhead lines. Thus, no significant MDEA solvent losses in the form of vapour being discovered along the gas streams due to the process taking place in the system. (Author)

  15. A DETECTION OF MOLECULAR GAS EMISSION IN THE HOST GALAXY OF GRB 080517

    Energy Technology Data Exchange (ETDEWEB)

    Stanway, E. R.; Levan, A. J. [Department of Physics, University of Warwick, Gibbet Hill Road, Coventry, CV4 7AL (United Kingdom); Tanvir, N. R.; Wiersema, K. [Department of Physics and Astronomy, University of Leicester, University Road, Leicester LE1 7RH (United Kingdom); Van der Laan, T. P. R., E-mail: e.r.stanway@warwick.ac.uk [Institute de Radioastronomie Millimetrique (IRAM), 300 Rue de la Piscine, 38406 St. Martin d' Heres, Grenoble (France)

    2015-01-01

    We have observed the host galaxy of the low-redshift, low-luminosity Swift GRB 080517 at 105.8 GHz using the IRAM Plateau de Bure interferometer. We detect an emission line with integrated flux SΔν = 0.39 ± 0.05 Jy km s{sup –1}—consistent both spatially and in velocity with identification as the J = 1-0 rotational transition of carbon monoxide (CO) at the host galaxy redshift. This represents only the third long gamma-ray burst (GRB) host galaxy with molecular gas detected in emission. The inferred molecular gas mass, M{sub H{sub 2}}∼6.3×10{sup 8} M {sub ☉}, implies a gas consumption timescale of ∼40 Myr if star formation continues at its current rate. Similar short timescales appear characteristic of the long GRB population with CO observations to date, suggesting that the GRB in these sources occurs toward the end of their star formation episode.

  16. A Sensor for Gas Detection Fabricated by a Circular Single-wall Carbon Nanotube

    Directory of Open Access Journals (Sweden)

    Lun-Wei Chang

    2008-04-01

    Full Text Available This work endeavors to describe a circular shape of carbon nanotubes (CNT performed by ultrasonic agitation and assisted by a surfactant implemented for gas detection. In a well-dispersed CNT solution, we observed that the thinner thickness and the larger diameter CNT rings were formed than those of our previous study. This fact can be elucidated more fully that the depletion contact energy is modulated by theoretical estimation with the corresponding tendency in our samples. The separated CNT ring possessed with negative charges in sodium dodecyl sulfate (SDS surfactant solution can be easily absorbed on the sliced surface. Through the e-beam lithography and the lift-off process, a CNT ring was exploited as a gas sensor to detect an extremely low concentration of methane gas. The circular CNT sensor has a prominent conduction response embodied in the existence of more defects in the ring CNT sensor than those of the straight CNT sensor. Moreover, the much fast response time in the circular CNT illustrates the demand of the shorter length of CNTs. The CNT ring features with longer persistent to current conduction after long time measurements appraising to be a robust and durable material in the sensor applications.

  17. 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

  18. 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.

  19. 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.

  20. Waste heat recovery system including a mechanism for collection, detection and removal of non-condensable gas

    Science.gov (United States)

    Ernst, Timothy C.; Zigan, James A.

    2017-06-20

    The disclosure describes a non-condensable gas collection, detection, and removal system for a WHR system that helps to maintain cycle efficiency of the WHR system across the life of an engine system associated with the WHR system. A storage volume is configured to collect non-condensable gas received from the working fluid circuit, and a release valve is configured to selectively release non-condensable gas contained within the storage volume.

  1. Gas detection with microelectromechanical Fabry-Perot interferometer technology in cell phone

    Science.gov (United States)

    Mannila, Rami; Hyypiö, Risto; Korkalainen, Marko; Blomberg, Martti; Kattelus, Hannu; Rissanen, Anna

    2015-06-01

    VTT Technical Research Centre of Finland has developed a miniaturized optical sensor for gas detection in a cell phone. The sensor is based on a microelectromechanical (MEMS) Fabry-Perot interferometer, which is a structure with two highly reflective surfaces separated by a tunable air gap. The MEMS FPI is a monolithic device, i.e. it is made entirely on one substrate in a batch process, without assembling separate pieces together. The gap is adjusted by moving the upper mirror with electrostatic force, so there are no actual moving parts. VTT has designed and manufactured a MEMS FPI based carbon dioxide sensor demonstrator which is integrated to a cell phone shield cover. The demonstrator contains light source, gas cell, MEMS FPI, detector, control electronics and two coin cell batteries as a power source. It is connected to the cell phone by Bluetooth. By adjusting the wavelength range and customizing the MEMS FPI structure, it is possible to selectively sense multiple gases.

  2. The transition from silicon to gas detection media in nuclear physics

    International Nuclear Information System (INIS)

    Pollacco, Emanuel C.

    2016-01-01

    Emerging radioactive beams and multi petawatt laser facilities are sturdily transforming our base concepts in instruments in nuclear physics. The changes are fuelled by studies of nuclei close to the drip-line or exotic reactions. This physics demands high luminosity, wide phase space cover with good resolution in energy, time, position and sampled waveform. By judiciously modifying the micro-world of the particle or space physics instruments (Double Sided Strip Si Detectors, Micro-Pattern Gas Amplifiers, microelectronics), we are on the path to initiate dream experiments. In the following a brief status in the domain is reported for selected instruments that highlight the present trends with silicon and the growing shift towards gas media for charged particle detection.

  3. The transition from silicon to gas detection media in nuclear physics

    Science.gov (United States)

    Pollacco, Emanuel C.

    2016-06-01

    Emerging radioactive beams and multi petawatt laser facilities are sturdily transforming our base concepts in instruments in nuclear physics. The changes are fuelled by studies of nuclei close to the drip-line or exotic reactions. This physics demands high luminosity, wide phase space cover with good resolution in energy, time, position and sampled waveform. By judiciously modifying the micro-world of the particle or space physics instruments (Double Sided Strip Si Detectors, Micro-Pattern Gas Amplifiers, microelectronics), we are on the path to initiate dream experiments. In the following a brief status in the domain is reported for selected instruments that highlight the present trends with silicon and the growing shift towards gas media for charged particle detection.

  4. Development of a real-time absorption method for detecting the mercaptan odorizing mixture of natural gas

    NARCIS (Netherlands)

    Kireev, SV; Petrov, NG; Podolyako, EM; Shnyrev, SL

    The absorption of mercaptan mixtures used for odorizing natural gas and mixtures of natural gas is experimentally studied in the spectral range 2.5-20 mu m. An absorption method for the real-time detection of the odorant concentration is proposed. The method is based on intensity measurements of the

  5. A Cost Effective Multi-Spectral Scanner for Natural Gas Detection

    Energy Technology Data Exchange (ETDEWEB)

    Yudaya Sivathanu; Jongmook Lim; Vinoo Narayanan; Seonghyeon Park

    2005-12-07

    The objective of this project is to design, fabricate and demonstrate a cost effective, multi-spectral scanner for natural gas leak detection in transmission and distribution pipelines. During the first year of the project, a laboratory version of the multi-spectral scanner was designed, fabricated, and tested at EnUrga Inc. The multi-spectral scanner was also evaluated using a blind Department of Energy study at the Rocky Mountain Oilfield Testing Center. The performance of the scanner was inconsistent during the blind study. However, most of the leaks were outside the view of the multi-spectral scanner that was developed during the first year of the project. Therefore, a definite evaluation of the capability of the scanner was not obtained. Despite the results, sufficient number of plumes was detected fully confirming the feasibility of the multi-spectral scanner. During the second year, the optical design of the scanner was changed to improve the sensitivity of the system. Laboratory tests show that the system can reliably detect small leaks (20 SCFH) at 30 to 50 feet. A prototype scanner was built and evaluated during the second year of the project. Only laboratory evaluations were completed during the second year. The laboratory evaluations show the feasibility of using the scanner to determine natural gas pipeline leaks. Further field evaluations and optimization of the scanner are required before commercialization of the scanner can be initiated.

  6. Nanofiber-net-binary structured membranes for highly sensitive detection of trace HCl gas.

    Science.gov (United States)

    Wang, Xianfeng; Wang, Jialin; Si, Yang; Ding, Bin; Yu, Jianyong; Sun, Gang; Luo, Wenjing; Zheng, Gang

    2012-12-07

    This work describes the detection of trace hydrogen chloride (HCl) gas through analyses of the resonance frequency signal from quartz crystal microbalance (QCM) sensors coated with polyaniline (PANI) functionalized polyamide 6 (PA 6) (PANI-PA 6) nanofiber-net-binary (NNB) structured membranes. The PA 6 NNB substrate comprising nanofibers and spider-web-like nano-nets fabricated by a versatile electro-spinning/netting (ESN) process offered an ideal interface for the uniform PANI functionalization and enhanced sensing performance. Benefiting from the large specific surface area, high porosity, and strong adhesive force to the QCM electrode of the PANI-PA 6 NNB membranes, the developed HCl-selective sensors exhibited a rapid response, good reproducibility and stability, and low detection limit (7 ppb) at room temperature. Additionally, the PANI-PA 6 NNB sensing membranes presented visible color changes upon cycled exposure to HCl and ammonia, suggesting their potential application in the development of colorimetric sensors. The PANI-PA 6 NNB coated QCM sensors are considered to be a promising candidate for trace HCl gas detection in practical applications.

  7. Miniaturized Gas Correlation Radiometer for the Detection of Trace Gases in the Martian Atmosphere

    Science.gov (United States)

    Melroy, H.; Wilson, E. L.; Georgieva, E.

    2012-12-01

    We present a miniaturized and simplified version of a gas correlation radiometer (GCR) capable of simultaneously mapping multiple trace gases and identifying active regions on the Mars surface. Gas correlation radiometry (GCR) has been shown to be a sensitive and versatile method for detecting trace gases in Earth's atmosphere. Reduction of the size and mass of the GCR was achieved by implementing compact, light-weight 1 mm inner diameter hollow-core optical fibers (hollow waveguides) as the gas correlation cells. In a comparison with an Earth orbiting CO2 GCR instrument, exchanging the 10 m multipass cells with hollow waveguide gas correlation cells of equivalent pathlength reduces the mass from ~150 kg to ~0.5 kg, and reduces the volume from 1.9 m x 1.3 m x 0.86 m to a small bundle of fiber coils approximately 1 meter in diameter by 0.05 m in height (mass and volume reductions of >99%). A unique feature of this instrument is its stackable module design, with a single module for each trace gas. Each of the modules is self-contained, and fundamentally identical; differing by the bandpass filter wavelength range and gas mixtures inside the hollow-waveguide absorption cells. The current configuration contains four stacked modules for simultaneous measurements of methane (CH4), formaldehyde (H2CO), water vapor (H2O), and deuterated water vapor (HDO) but could easily be expanded to include measurements of additional species of interest including nitrous oxide (N2O), hydrogen sulfide (H2S), methanol (CH3OH), and sulfur dioxide (SO2), as well as carbon dioxide (CO2) for a simultaneous measure of mass balance. Preliminary results indicate that a 1 ppb detection limit is possible for both formaldehyde and methane with one second of averaging. Using non-optimized components, we have demonstrated an instrument sensitivity equivalent to ~30 ppb for formaldehyde, and ~500 ppb for methane. We expect custom bandpass filters and 6 m long waveguides to significantly improve these

  8. Nanomolecular gas sensor architectures based on functionalized carbon nanotubes for vapor detection

    Science.gov (United States)

    Hines, Deon; Zhang, Henan; Rümmeli, Mark H.; Adebimpe, David; Akins, Daniel L.

    2015-05-01

    There is enormous interest in detection of simple & complex odors by mean of electronic instrumentation. Specifically, our work focuses on creating derivatized-nanotube-based "electronic noses" for the detection and identification of gases, and other materials. We have grafted single-walled carbon nanotubes (SWNTs) with an array of electron-donating and electron withdrawing moieties and have characterized some of the physicochemical properties of the modified nanotubes. Gas sensing elements have been fabricated by spin coating the functionalized nanotubes onto interdigitated electrodes (IDE's), creating an array of sensors. Each element in the sensor array can contain a different functionalized matrix. This facilitates the construction of chemical sensor arrays with high selectivity and sensitivity; a methodology that mimics the mammalian olfactory system. Exposure of these coated IDEs to organic vapors and the successful classification of the data obtained under DC monitoring, indicate that the system can function as gas sensors of high repeatability and selectivity for a wide range of common analytes. Since the detection of explosive materials is also of concern in this research, our next phase focuses on explosives such as, TNT, RDX, and Triacetone Triperoxide (TATP). Sensor data from individual detection are assessed on their own individual merits, after which they are amalgamated and reclassified to present each vapor as unique data point on a 2-dimensional map and with minimum loss of information. This approach can assist the nation's need for a technology to defeat IEDs through the use of methods that detect unique chemical signatures associated with explosive molecules and byproducts.

  9. Tentative detection of warm intervening gas towards PKS 0548-322 with XMM-Newton

    Energy Technology Data Exchange (ETDEWEB)

    Barcons, X.

    2005-03-17

    We present the results of a long ({approx} 93 ksec) XMM-Newton observation of the bright BL-Lac object PKS 0548-322 (z = 0.069). Our Reflection Grating Spectrometer (RGS) spectrum shows a single absorption feature at an observed wavelength {lambda} = 23.33 {+-} 0.01 {angstrom} which we interpret as OVI K{alpha} absorption at z = 0.058, i.e., {approx} 3000 km s{sup -1} from the background object. The observed equivalent width of the absorption line {approx} 30m {angstrom}, coupled with the lack of the corresponding absorption edge in the EPIC pn data, implies a column density N{sub OVI} {approx} 2 x 10{sup 16} cm{sup -2} and turbulence with a Doppler velocity parameter b > 100 km s{sup -1}. Within the limitations of our RGS spectrum, no OVII or OV K{alpha} absorption are detected. Under the assumption of ionization equilibrium by both collisions and the extragalactic background, this is only marginally consistent if the gas temperature is {approx} 2.5 x 10{sup 5} K, with significantly lower or higher values being excluded by our limits on OV or OVII. If confirmed, this would be the first X-ray detection of a large amount of intervening warm absorbing gas through OVI absorption. The existence of such a high column density absorber, much stronger than any previously detected one in OVI, would place stringent constraints on the large-scale distribution of baryonic gas in the Universe.

  10. Investigation of Natural Gas Fugitive Leak Detection Using an Unmanned Aerial Vehicle

    Science.gov (United States)

    Yang, S.; Talbot, R. W.; Frish, M. B.; Golston, L.; Aubut, N. F.; Zondlo, M. A.

    2017-12-01

    The U.S is now the world's largest natural gas producer, of which methane (CH4) is the main component. About 2% of the CH4 is lost through fugitive leaks. This research is under the DOE Methane Observation Networks with Innovative Technology to Obtain Reductions (MONITOR) program of ARPA-E. Our sentry measurement system is composed of four state-of-the-art technologies centered around the RMLDTM (Remote Methane Leak Detector). An open path RMLDTM measures column-integrated CH4 concentration that incorporates fluctuations in the vertical CH4 distribution. Based on Backscatter Tunable Diode Laser Absorption Spectroscopy and Small Unmanned Aerial Vehicles, the sentry system can autonomously, consistently and cost-effectively monitor and quantify CH4 leakage from sites associated with natural gas production. This system provides an advanced capability in detecting leaks at hard-to-access sites (e.g., wellheads) compared to traditional manual methods. Automated leak detecting and reporting algorithms combined with wireless data link implement real-time leak information reporting. Early data were gathered to set up and test the prototype system, and to optimize the leak localization and calculation strategies. The flight pattern is based on a raster scan which can generate interpolated CH4 concentration maps. The localization and quantification algorithms can be derived from the plume images combined with wind vectors. Currently, the accuracy of localization algorithm can reach 2 m and the calculation algorithm has a factor of 2 accuracy. This study places particular emphasis on flux quantification. The data collected at Colorado and Houston test fields were processed, and the correlation between flux and other parameters analyzed. Higher wind speeds and lower wind variation are preferred to optimize flux estimation. Eventually, this system will supply an enhanced detection capability to significantly reduce fugitive CH4 emissions in the natural gas industry.

  11. Influence of tryptophan loading on urinary excretion of anthranilic acid and 3-hydroxyanthranilic acid by men and women as determined by alkali flame ionization gas chromatography

    NARCIS (Netherlands)

    Poll, J.M. van der; Vink, M.; Schrijver, J.; Odink, J.

    1986-01-01

    A gas chromatographic method with alkali flame ionization detection is described for the determination of urinary total (free and conjugated) anthranilic acid (AA) and 3-hydroxyanthranilic acid (HAA) as their pentafluorobenzyl esters. Prior to analysis, urine was hydrolysed using hydrochloric acid

  12. Gas chromatography interfaced with atmospheric pressure ionization-quadrupole time-of-flight-mass spectrometry by low-temperature plasma ionization

    DEFF Research Database (Denmark)

    Norgaard, Asger W.; Kofoed-Sorensen, Vivi; Svensmark, Bo

    2013-01-01

    A low temperature plasma (LTP) ionization interface between a gas chromatograph (GC) and an atmospheric pressure inlet mass spectrometer, was constructed. This enabled time-of-flight mass spectrometric detection of GC-eluting compounds. The performance of the setup was evaluated by injection...

  13. A hydroxyl radical detection system using gas expansion and fast gating laser-induced fluorescence techniques.

    Science.gov (United States)

    Chen, Hao; Hu, Renzhi; Xie, Pinhua; Xing, Xingbiao; Ling, Liuyi; Li, Zhiyan; Wang, Fengyang; Wang, Yihui; Liu, Jianguo; Liu, Wenqing

    2018-03-01

    An OH radical measurement instrument based on Fluorescence Assay by Gas Expansion (FAGE) has been developed in our laboratory. Ambient air is introduced into a low-pressure fluorescence cell through a pinhole aperture and irradiated by a dye laser at a high repetition rate of 8.5kHz. The OH radical is both excited and detected at 308nm using A-X(0,0) band. To satisfy the high efficiency needs of fluorescence collection and detection, a 4-lens optical system and a self-designed gated photomultiplier (PMT) is used, and gating is actualized by switching the voltage applied on the PMT dynodes. A micro channel photomultiplier (MCP) is also prepared for fluorescence detection. Then the weak signal is accumulated by a photon counter in a specific timing. The OH radical excitation spectrum range in the wavelength of 307.82-308.2nm is detected and the excited line for OH detection is determined to be Q 1 (2) line. The calibration of the FAGE system is researched by using simultaneous photolysis of H 2 O and O 2 . The minimum detection limit of the instrument using gated PMT is determined to be 9.4×10 5 molecules/cm 3 , and the sensitivity is 9.5×10 -7 cps/(OH·cm -3 ), with a signal-to-noise ratio of 2 and an integration time of 60sec, while OH detection limit and the detection sensitivity using MCP is calculated to be 1.6×10 5 molecules/cm 3 and 2.3×10 -6 cps/(OH·cm -3 ). The laboratory OH radical measurement is carried out and results show that the proposed system can be used for atmospheric OH radical measurement. Copyright © 2017. Published by Elsevier B.V.

  14. Review of Slug Detection, Modeling and Control Techniques for Offshore Oil & Gas Production Processes

    DEFF Research Database (Denmark)

    Pedersen, Simon; Løhndorf, Petar Durdevic; Yang, Zhenyu

    2015-01-01

    The current offshore oil & gas multi-phase production and transportation installations have big challenges related with the slugging flow: An unstable multi-phase flow regime where the flow rates, pressures and temperatures oscillate in the considered processes. Slug can be caused by different...... severe consequences to the production processes because of the slugging flow. This paper reviews some observed latest status and key challenges about slug detection, dynamical modeling and elimination of slugging flows. Mathematical modeling of slug has been used to investigate the slug mechanism...... decades, the cost-effective and optimal slug modeling and control are still open topics with many related challenges....

  15. Microsecond fiber laser pumped, single-frequency optical parametric oscillator for trace gas detection.

    Science.gov (United States)

    Barria, Jessica Barrientos; Roux, Sophie; Dherbecourt, Jean-Baptiste; Raybaut, Myriam; Melkonian, Jean-Michel; Godard, Antoine; Lefebvre, Michel

    2013-07-01

    We report on the first microsecond doubly resonant optical parametric oscillator (OPO). It is based on a nested cavity OPO architecture allowing single longitudinal mode operation and low oscillation threshold (few microjoule). The combination with a master oscillator-power amplifier fiber pump laser provides a versatile optical source widely tunable in the 3.3-3.5 μm range with an adjustable pulse repetition rate (from 40 to 100 kHz), high duty cycle (~10(-2)) and mean power (up to 25 mW in the idler beam). The potential for trace gas sensing applications is demonstrated through photoacoustic detection of atmospheric methane.

  16. Electrospun ZnO Nanowires as Gas Sensors for Ethanol Detection

    Directory of Open Access Journals (Sweden)

    Huang Po-Jung

    2009-01-01

    Full Text Available Abstract ZnO nanowires were produced using an electrospinning method and used in gas sensors for the detection of ethanol at 220 °C. This electrospinning technique allows the direct placement of ZnO nanowires during their synthesis to bridge the sensor electrodes. An excellent sensitivity of nearly 90% was obtained at a low ethanol concentration of 10 ppm, and the rest obtained at higher ethanol concentrations, up to 600 ppm, all equal to or greater than 90%.

  17. Potential application of microsensor technology in radioactive waste management with emphasis on headspace gas detection

    International Nuclear Information System (INIS)

    Davis, Chad Edward; Thomas, Michael Loren; Wright, Jerome L.; Pohl, Phillip Isabio; Hughes, Robert Clark; Wang, Yifeng; McGrath, Lucas K.; Ho, Clifford Kuofei; Gao, Huizhen

    2004-01-01

    Waste characterization is probably the most costly part of radioactive waste management. An important part of this characterization is the measurements of headspace gas in waste containers in order to demonstrate the compliance with Resource Conservation and Recovery Act (RCRA) or transportation requirements. The traditional chemical analysis methods, which include all steps of gas sampling, sample shipment and laboratory analysis, are expensive and time-consuming as well as increasing worker's exposure to hazardous environments. Therefore, an alternative technique that can provide quick, in-situ, and real-time detections of headspace gas compositions is highly desirable. This report summarizes the results obtained from a Laboratory Directed Research and Development (LDRD) project entitled 'Potential Application of Microsensor Technology in Radioactive Waste Management with Emphasis on Headspace Gas Detection'. The objective of this project is to bridge the technical gap between the current status of microsensor development and the intended applications of these sensors in nuclear waste management. The major results are summarized below: (sm b ullet) A literature review was conducted on the regulatory requirements for headspace gas sampling/analysis in waste characterization and monitoring. The most relevant gaseous species and the related physiochemical environments were identified. It was found that preconcentrators might be needed in order for chemiresistor sensors to meet desired detection (sm b ullet) A long-term stability test was conducted for a polymer-based chemresistor sensor array. Significant drifts were observed over the time duration of one month. Such drifts should be taken into account for long-term in-situ monitoring. (sm b ullet) Several techniques were explored to improve the performance of sensor polymers. It has been demonstrated that freeze deposition of black carbon (CB)-polymer composite can effectively eliminate the so-called 'coffee ring

  18. FTIR gas analysis with improved sensitivity and selectivity for CWA and TIC detection

    Science.gov (United States)

    Phillips, Charles M.; Tan, Huwei

    2010-04-01

    This presentation describes the use of an FTIR (Fourier Transform Infrared)-based spectrometer designed to continuously monitor ambient air for the presence of chemical warfare agents (CWAs) and toxic industrial chemicals (TICs). The necessity of a reliable system capable of quickly and accurately detecting very low levels of CWAs and TICs while simultaneously retaining a negligible false alarm rate will be explored. Technological advancements in FTIR sensing have reduced noise while increasing selectivity and speed of detection. These novel analyzer design characteristics are discussed in detail and descriptions are provided which show how optical throughput, gas cell form factor, and detector response are optimized. The hardware and algorithms described here will explain why this FTIR system is very effective for the simultaneous detection and speciation of a wide variety of toxic compounds at ppb concentrations. Analytical test data will be reviewed demonstrating the system's sensitivity to and selectivity for specific CWAs and TICs; this will include recent data acquired as part of the DHS ARFCAM (Autonomous Rapid Facility Chemical Agent Monitor) project. These results include analyses of the data from live agent testing for the determination of CWA detection limits, immunity to interferences, detection times, residual noise analysis and false alarm rates. Sensing systems such as this are critical for effective chemical hazard identification which is directly relevant to the CBRNE community.

  19. Fission signal detection using helium-4 gas fast neutron scintillation detectors

    Energy Technology Data Exchange (ETDEWEB)

    Lewis, J. M., E-mail: lewisj@ufl.edu; Kelley, R. P.; Jordan, K. A. [Nuclear Engineering Program, University of Florida, Gainesville, Florida 32611 (United States); Murer, D. [Arktis Radiation Detectors Ltd., 8045 Zurich (Switzerland)

    2014-07-07

    We demonstrate the unambiguous detection of the fission neutron signal produced in natural uranium during active neutron interrogation using a deuterium-deuterium fusion neutron generator and a high pressure {sup 4}He gas fast neutron scintillation detector. The energy deposition by individual neutrons is quantified, and energy discrimination is used to differentiate the induced fission neutrons from the mono-energetic interrogation neutrons. The detector can discriminate between different incident neutron energies using pulse height discrimination of the slow scintillation component of the elastic scattering interaction between a neutron and the {sup 4}He atom. Energy histograms resulting from this data show the buildup of a detected fission neutron signal at higher energies. The detector is shown here to detect a unique fission neutron signal from a natural uranium sample during active interrogation with a (d, d) neutron generator. This signal path has a direct application to the detection of shielded nuclear material in cargo and air containers. It allows for continuous interrogation and detection while greatly minimizing the potential for false alarms.

  20. Fission signal detection using helium-4 gas fast neutron scintillation detectors

    Science.gov (United States)

    Lewis, J. M.; Kelley, R. P.; Murer, D.; Jordan, K. A.

    2014-07-01

    We demonstrate the unambiguous detection of the fission neutron signal produced in natural uranium during active neutron interrogation using a deuterium-deuterium fusion neutron generator and a high pressure 4He gas fast neutron scintillation detector. The energy deposition by individual neutrons is quantified, and energy discrimination is used to differentiate the induced fission neutrons from the mono-energetic interrogation neutrons. The detector can discriminate between different incident neutron energies using pulse height discrimination of the slow scintillation component of the elastic scattering interaction between a neutron and the 4He atom. Energy histograms resulting from this data show the buildup of a detected fission neutron signal at higher energies. The detector is shown here to detect a unique fission neutron signal from a natural uranium sample during active interrogation with a (d, d) neutron generator. This signal path has a direct application to the detection of shielded nuclear material in cargo and air containers. It allows for continuous interrogation and detection while greatly minimizing the potential for false alarms.