WorldWideScience

Sample records for headspace gas sampling

  1. GNS Castor V/21 Headspace Gas Sampling 2014

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-01-01

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

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

    International Nuclear Information System (INIS)

    Huckaby, J.L.

    1994-01-01

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

  3. Quantitative Analysis of Bioactive Compounds from Aromatic Plants by Means of Dynamic Headspace Extraction and Multiple Headspace Extraction-Gas Chromatography-Mass Spectrometry

    NARCIS (Netherlands)

    Omar, Jone; Olivares, Maitane; Alonso, Ibone; Vallejo, Asier; Aizpurua-Olaizola, Oier; Etxebarria, Nestor

    2016-01-01

    Seven monoterpenes in 4 aromatic plants (sage, cardamom, lavender, and rosemary) were quantified in liquid extracts and directly in solid samples by means of dynamic headspace-gas chromatography-mass spectrometry (DHS-GC-MS) and multiple headspace extraction-gas chromatography-mass spectrometry

  4. Gas flow headspace liquid phase microextraction.

    Science.gov (United States)

    Yang, Cui; Qiu, Jinxue; Ren, Chunyan; Piao, Xiangfan; Li, Xifeng; Wu, Xue; Li, Donghao

    2009-11-06

    There is a trend towards the use of enrichment techniques such as microextraction in the analysis of trace chemicals. Based on the theory of ideal gases, theory of gas chromatography and the original headspace liquid phase microextraction (HS-LPME) technique, a simple gas flow headspace liquid phase microextraction (GF-HS-LPME) technique has been developed, where the extracting gas phase volume is increased using a gas flow. The system is an open system, where an inert gas containing the target compounds flows continuously through a special gas outlet channel (D=1.8mm), and the target compounds are trapped on a solvent microdrop (2.4 microL) hanging on the microsyringe tip, as a result, a high enrichment factor is obtained. The parameters affecting the enrichment factor, such as the gas flow rate, the position of the microdrop, the diameter of the gas outlet channel, the temperatures of the extracting solvent and of the sample, and the extraction time, were systematically optimized for four types of polycyclic aromatic hydrocarbons. The results were compared with results obtained from HS-LPME. Under the optimized conditions (where the extraction time and the volume of the extracting sample vial were fixed at 20min and 10mL, respectively), detection limits (S/N=3) were approximately a factor of 4 lower than those for the original HS-LPME technique. The method was validated by comparison of the GF-HS-LPME and HS-LPME techniques using data for PAHs from environmental sediment samples.

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

    International Nuclear Information System (INIS)

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

    1995-01-01

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

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

    International Nuclear Information System (INIS)

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

    1995-01-01

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

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

    International Nuclear Information System (INIS)

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

    1995-09-01

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

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

    International Nuclear Information System (INIS)

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

    1995-01-01

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

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

    International Nuclear Information System (INIS)

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

    1995-09-01

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

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

    International Nuclear Information System (INIS)

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

    1995-01-01

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

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

    International Nuclear Information System (INIS)

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

    1995-09-01

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

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

    International Nuclear Information System (INIS)

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

    1995-01-01

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

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

    International Nuclear Information System (INIS)

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

    1995-01-01

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

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

    International Nuclear Information System (INIS)

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

    1995-09-01

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

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

    International Nuclear Information System (INIS)

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

    1995-01-01

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

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

    International Nuclear Information System (INIS)

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

    1995-09-01

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

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

    International Nuclear Information System (INIS)

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

    1995-09-01

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

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

    International Nuclear Information System (INIS)

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

    1995-09-01

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

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

    International Nuclear Information System (INIS)

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

    1995-09-01

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

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

    International Nuclear Information System (INIS)

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

    1995-09-01

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

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

    International Nuclear Information System (INIS)

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

    1995-01-01

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

  2. Rapid determination of methanol in black liquors by full evaporation headspace gas chromatography.

    Science.gov (United States)

    Li, Hailong; Zhan, Huaiyu; Fu, Shiyu; Liu, Mengru; Chai, Xin-Sheng

    2007-12-14

    This paper reported a full evaporation headspace gas chromatographic (GC) technique for determination of methanol content in black liquors (pulping spent liquor). In this method, a very small volume (10-20 microL) of liquor sample is introduced into a headspace sample vial (20 mL) and heated up to a temperature of 105 degrees C. A near-complete mass transfer of methanol from the liquid phase to vapor phase (headspace), i.e., a full evaporation, can be achieved within 3 min. The methanol in the headspace of the vial is then measured by GC. The present method is simple, rapid and accurate.

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

    Science.gov (United States)

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

    2018-02-23

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

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

    Science.gov (United States)

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

    2016-09-01

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

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

    International Nuclear Information System (INIS)

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

    1995-09-01

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

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

    International Nuclear Information System (INIS)

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

    1995-09-01

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

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

    International Nuclear Information System (INIS)

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

    1995-09-01

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

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

    Science.gov (United States)

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

    2018-04-17

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

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

    International Nuclear Information System (INIS)

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

    1995-01-01

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

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

    International Nuclear Information System (INIS)

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

    1995-09-01

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

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

    International Nuclear Information System (INIS)

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

    1995-09-01

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

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

    International Nuclear Information System (INIS)

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

    1995-09-01

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

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

    International Nuclear Information System (INIS)

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

    1995-09-01

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

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

    International Nuclear Information System (INIS)

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

    1995-09-01

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

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

    International Nuclear Information System (INIS)

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

    1995-09-01

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

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

    International Nuclear Information System (INIS)

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

    1995-09-01

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

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

    International Nuclear Information System (INIS)

    Bratzel, D.R.

    1995-01-01

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

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

    International Nuclear Information System (INIS)

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

    1995-09-01

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

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

    International Nuclear Information System (INIS)

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

    1995-09-01

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

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

    International Nuclear Information System (INIS)

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

    1995-01-01

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

  1. Tank 241-U-104 headspace gas and vapor characterization results from samples collected on July 16, 1996

    International Nuclear Information System (INIS)

    Pool, K.H.; Evans, J.C.; Hayes, J.C.; Mitroshkov, A.V.; Edwards, J.A.; Julya, J.L.; Thornton, B.M.; Fruchter, J.S.; Silvers, K.L.

    1997-08-01

    This report presents the results from analyses of samples taken from the headspace of waste storage tank 241-U-104 (Tank U-104) at the Hanford Site in Washington State. Tank headspace samples collected by Westinghouse Hanford Company (WHC) were analyzed by Pacific Northwest National Laboratory (PNNL) to determine headspace concentrations of selected non-radioactive analytes. Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. Vapor concentrations from sorbent trap samples are based on measured sample volumes provided by WHC. No analytes were determined to be above the immediate notification limits specified by the sampling and analysis plan. None of the flammable constituents were present at concentrations above the analytical instrument detection limits. Total headspace flammability was estimated to be <0.108% of the lower flammability limit. Average measured concentrations of targeted gases, inorganic vapors, and selected organic vapors are provided in a table. A summary of experimental methods, including sampling methodology, analytical procedures, and quality assurance and control methods are presented in Section 2.0. Detailed descriptions of the analytical results are provided in Section 3.0

  2. Tank 241-BY-105 Headspace Gas and Vapor Characterization Results for Samples Collected in May 1994 and July 1994. Revision 2

    International Nuclear Information System (INIS)

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

    1995-09-01

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

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

    Science.gov (United States)

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

    2012-06-01

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

  4. Analysis of pollutants in air and water using gas chromatography and headspace gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Stenner, H.

    1980-01-01

    The combination 'personal sampling' with headspace gas chromatography to determine traces of formaldehyde, phenol and benzene in air is investigated in this work, with the aim of developing maximum workplace concentration values (MWL values). Further possible applications of gas chromatography in trace analysis in the environmentally protected area. The analysis of chromium in waste waters (Cr III as acetyl acetonate complex) is investigated as further possible application, whereby optimum conditions are obtained. A modified flame ionization detector was used to increase the detection sensitivity.

  5. Gram-negative and -positive bacteria differentiation in blood culture samples by headspace volatile compound analysis.

    Science.gov (United States)

    Dolch, Michael E; Janitza, Silke; Boulesteix, Anne-Laure; Graßmann-Lichtenauer, Carola; Praun, Siegfried; Denzer, Wolfgang; Schelling, Gustav; Schubert, Sören

    2016-12-01

    Identification of microorganisms in positive blood cultures still relies on standard techniques such as Gram staining followed by culturing with definite microorganism identification. Alternatively, matrix-assisted laser desorption/ionization time-of-flight mass spectrometry or the analysis of headspace volatile compound (VC) composition produced by cultures can help to differentiate between microorganisms under experimental conditions. This study assessed the efficacy of volatile compound based microorganism differentiation into Gram-negatives and -positives in unselected positive blood culture samples from patients. Headspace gas samples of positive blood culture samples were transferred to sterilized, sealed, and evacuated 20 ml glass vials and stored at -30 °C until batch analysis. Headspace gas VC content analysis was carried out via an auto sampler connected to an ion-molecule reaction mass spectrometer (IMR-MS). Measurements covered a mass range from 16 to 135 u including CO2, H2, N2, and O2. Prediction rules for microorganism identification based on VC composition were derived using a training data set and evaluated using a validation data set within a random split validation procedure. One-hundred-fifty-two aerobic samples growing 27 Gram-negatives, 106 Gram-positives, and 19 fungi and 130 anaerobic samples growing 37 Gram-negatives, 91 Gram-positives, and two fungi were analysed. In anaerobic samples, ten discriminators were identified by the random forest method allowing for bacteria differentiation into Gram-negative and -positive (error rate: 16.7 % in validation data set). For aerobic samples the error rate was not better than random. In anaerobic blood culture samples of patients IMR-MS based headspace VC composition analysis facilitates bacteria differentiation into Gram-negative and -positive.

  6. Performance evaluation of a thermal desorption/gas chromatographic/mass spectrometric method for the characterization of waste tank headspace samples

    International Nuclear Information System (INIS)

    Ma, C.Y.; Skeen, J.T.; Dindal, A.B.; Bayne, C.K.; Jenkins, R.A.

    1997-01-01

    A thermal desorption/gas chromatography/mass spectrometry (TD/GC/MS) method was validated for the determination of volatile organic compounds collected on carbonaceous triple sorbent traps and applied to characterize samples of headspace gases collected from underground nuclear waste storage tanks at the U.S. Department of Energy's Hanford site, in Richland, WA. Method validation used vapor-phase standards generated from 25 target analytes, including alkanes, alkyl alcohols, alkyl ketones, alkylated aromatics, and alkyl nitriles. The target analytes represent a group of compounds identified in one of the most problematic tanks. TD/GC/MS was carried out with modified injectors. Performance was characterized based on desorption efficiency, reproducibility, stability, and linearity of the calibration, method detection limits, preanalytical holding time, and quality control limits for surrogate standard recoveries. Desorption efficiencies were all greater than 82%, and the majority of the analytes (23 out of 25) had reproducibility values less than 24% near the method detection levels. The method was applied to the analysis of a total of 305 samples collected from the headspaces of 48 underground waste storge tanks. Quality control procedures were implemented to monitor sampling and TD/GC/MS method. 33 refs., 2 figs., 4 tabs

  7. Headspace profiling of cocaine samples for intelligence purposes.

    Science.gov (United States)

    Dujourdy, Laurence; Besacier, Fabrice

    2008-08-06

    A method for determination of residual solvents in illicit hydrochloride cocaine samples using static headspace-gas chromatography (HS-GC) associated with a storage computerized procedure is described for the profiling and comparison of seizures. The system involves a gas chromatographic separation of 18 occluded solvents followed by fully automatic data analysis and transfer to a PHP/MySQL database. First, a fractional factorial design was used to evaluate the main effects of some critical method parameters (salt choice, vial agitation intensity, oven temperature, pressurization and loop equilibration) on the results with a minimum of experiments. The method was then validated for tactical intelligence purposes (batch comparison) via several studies: selection of solvents and mathematical comparison tool, reproducibility and "cutting" influence studies. The decision threshold to determine the similarity of two samples was set and false positives and negatives evaluated. Finally, application of the method to distinguish geographical origins is discussed.

  8. Tank vapor characterization project - Tank 241-U-112 headspace gas and vapor characterization: Results for homogeneity samples collected on December 6, 1996

    Energy Technology Data Exchange (ETDEWEB)

    Sklarew, D.S.; Pool, K.H.; Evans, J.C.; Hayes, J.C. [and others

    1997-09-01

    This report presents the results of analyses of samples taken from the headspace of waste storage tank 241-U-112 (Tank U-112) at the Hanford Site in Washington State. Samples were collected to determine the homogeneity of selected inorganic and organic headspace constitutents. Two risers (Riser 3 and Riser 6) were sampled at three different elevations (Bottom, Middle, and Top) within the tank. Tank headspace samples were collected by SGN Eurisys Service Corporation (SESC) and were analyzed by Pacific Northwest National Laboratory (PNNL) to determine headspace concentrations of selected non-radioactive analytes. Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. Ammonia was determined to be above the immediate notification limit specified by the sampling and analysis plan.

  9. Determination of methanol in pulp washing filtrates by desiccated full evaporation headspace gas chromatography.

    Science.gov (United States)

    Hu, Hui-Chao; Chai, Xin-Sheng

    2012-01-27

    This paper reports on a desiccated full evaporation headspace gas chromatographic (FE HS-GC) technique for determination of the methanol content in dilute mill effluents. Anhydrous K(2)CO(3) was selected as the preferred salt for eliminating the water in the sample in the headspace sample vial. The results showed that the addition of 12 g K(2)CO(3) made it possible to introduce a larger sample size (up to 1 mL) into the FE HS-GC measurement, thereby increasing the sensitivity of the technique. At the given equilibration temperature (105°C), a near-complete mass transfer of methanol from the liquid phase to vapor phase (headspace) was achieved within 10 min. Replicate samples showed that the relative standard deviation of the method was less than 1.5%. Further, the limit of quantification (LOQ) was 0.12 μg and the recovery ranged from 95 to 104%. The present method greatly improves the methanol detection sensitivity in the FE HS-GC method and has the added advantage of being simple, rapid and accurate. Copyright © 2011 Elsevier B.V. All rights reserved.

  10. Effects of gas composition in headspace and bicarbonate concentrations in media on gas and methane production, degradability, and rumen fermentation using in vitro gas production techniques.

    Science.gov (United States)

    Patra, Amlan Kumar; Yu, Zhongtang

    2013-07-01

    Headspace gas composition and bicarbonate concentrations in media can affect methane production and other characteristics of rumen fermentation in in vitro gas production systems, but these 2 important factors have not been evaluated systematically. In this study, these 2 factors were investigated with respect to gas and methane production, in vitro digestibility of feed substrate, and volatile fatty acid (VFA) profile using in vitro gas production techniques. Three headspace gas compositions (N2+ CO2+ H2 in the ratio of 90:5:5, CO2, and N2) with 2 substrate types (alfalfa hay only, and alfalfa hay and a concentrate mixture in a 50:50 ratio) in a 3×2 factorial design (experiment 1) and 3 headspace compositions (N2, N2 + CO2 in a 50:50 ratio, and CO2) with 3 bicarbonate concentrations (80, 100, and 120 mM) in a 3×3 factorial design (experiment 2) were evaluated. In experiment 1, total gas production (TGP) and net gas production (NGP) was the lowest for CO2, followed by N2, and then the gas mixture. Methane concentration in headspace gas after fermentation was greater for CO2 than for N2 and the gas mixture, whereas total methane production (TMP) and net methane production (NMP) were the greatest for CO2, followed by the gas mixture, and then N2. Headspace composition did not affect in vitro digestibility or the VFA profile, except molar percentages of propionate, which were greater for CO2 and N2 than for the gas mixture. Methane concentration in headspace gas, TGP, and NGP were affected by the interaction of headspace gas composition and substrate type. In experiment 2, increasing concentrations of CO2 in the headspace decreased TGP and NGP quadratically, but increased the concentrations of methane, NMP, and in vitro fiber digestibility linearly, and TMP quadratically. Fiber digestibility, TGP, and NGP increased linearly with increasing bicarbonate concentrations in the medium. Concentrations of methane and NMP were unaffected by bicarbonate concentration, but

  11. Determination of sulfur dioxide in wine using headspace gas chromatography and electron capture detection.

    Science.gov (United States)

    Aberl, A; Coelhan, M

    2013-01-01

    Sulfites are routinely added as preservatives and antioxidants in wine production. By law, the total sulfur dioxide content in wine is restricted and therefore must be monitored. Currently, the method of choice for determining the total content of sulfur dioxide in wine is the optimised Monier-Williams method, which is time consuming and laborious. The headspace gas chromatographic method described in this study offers a fast and reliable alternative method for the detection and quantification of the sulfur dioxide content in wine. The analysis was performed using an automatic headspace injection sampler, coupled with a gas chromatograph and an electron capture detector. The method is based on the formation of gaseous sulfur dioxide subsequent to acidification and heating of the sample. In addition to free sulfur dioxide, reversibly bound sulfur dioxide in carbonyl compounds, such as acetaldehyde, was also measured with this method. A total of 20 wine samples produced using diverse grape varieties and vintages of varied provenance were analysed using the new method. For reference and comparison purposes, 10 of the results obtained by the proposed method were compared with those acquired by the optimised Monier-Williams method. Overall, the results from the headspace analysis showed good correlation (R = 0.9985) when compared with the conventional method. This new method requires minimal sample preparation and is simple to perform, and the analysis can also be completed within a short period of time.

  12. [Determination of olive oil content in olive blend oil by headspace gas chromatography-mass spectrometry].

    Science.gov (United States)

    Jiang, Wanfeng; Zhang, Ning; Zhang, Fengyan; Yang, Zhao

    2017-07-08

    A method for the determination of the content of olive oil in olive blend oil by headspace gas chromatography-mass spectrometry (SH-GC/MS) was established. The amount of the sample, the heating temperature, the heating time, the amount of injection, the injection mode and the chromatographic column were optimized. The characteristic compounds of olive oil were found by chemometric method. A sample of 1.0 g was placed in a 20 mL headspace flask, and heated at 180℃ for 2700 s. Then, 1.0 mL headspace gas was taken into the instrument. An HP-88 chromatographic column was used for the separation and the analysis was performed by GC/MS. The results showed that the linear range was 0-100%(olive oil content). The linear correlation coefficient ( r 2 ) was more than 0.995, and the limits of detection were 1.26%-2.13%. The deviations of olive oil contents in the olive blend oil were from -0.65% to 1.02%, with the relative deviations from -1.3% to 6.8% and the relative standard deviations from 1.18% to 4.26% ( n =6). The method is simple, rapid, environment friendly, sensitive and accurate. It is suitable for the determination of the content of olive oil in olive blend oil.

  13. Optimizing headspace sampling temperature and time for analysis of volatile oxidation products in fish oil

    DEFF Research Database (Denmark)

    Rørbæk, Karen; Jensen, Benny

    1997-01-01

    Headspace-gas chromatography (HS-GC), based on adsorption to Tenax GR(R), thermal desorption and GC, has been used for analysis of volatiles in fish oil. To optimize sam sampling conditions, the effect of heating the fish oil at various temperatures and times was evaluated from anisidine values (AV...

  14. Determination of binding-dioxygen in dioxygen complexes by headspace gas chromatography.

    Science.gov (United States)

    Wang, Wei; Feng, Shun; Li, Ya-ni; Wu, Meiying; Wang, Jide

    2008-06-06

    Dioxygen complexes play important roles in organisms' bodies, so the determination of binding-dioxygen has practical significance. A simple and robust method based on headspace gas chromatography was proposed to determine the binding-dioxygen in dioxygen complexes. By measuring the content change of nitrogen gas in a vial, the amount of oxygen released from dixoygen complexes can be determined. The method was validated using potassium chlorate as model sample, and the results exhibited good recoveries (90-99%) with the relative standard deviation less than 8%. It was also used to analyze dioxygen complex of cobalt bis(salicylaldehyde) ethylenediimine and polyamine cobalt complexes prepared by solid-phase reaction.

  15. A novel method for the determination of adsorption partition coefficients of minor gases in a shale sample by headspace gas chromatography.

    Science.gov (United States)

    Zhang, Chun-Yun; Hu, Hui-Chao; Chai, Xin-Sheng; Pan, Lei; Xiao, Xian-Ming

    2013-10-04

    A novel method has been developed for the determination of adsorption partition coefficient (Kd) of minor gases in shale. The method uses samples of two different sizes (masses) of the same material, from which the partition coefficient of the gas can be determined from two independent headspace gas chromatographic (HS-GC) measurements. The equilibrium for the model gas (ethane) was achieved in 5h at 120°C. The method also involves establishing an equation based on the Kd at higher equilibrium temperature, from which the Kd at lower temperature can be calculated. Although the HS-GC method requires some time and effort, it is simpler and quicker than the isothermal adsorption method that is in widespread use today. As a result, the method is simple and practical and can be a valuable tool for shale gas-related research and applications. Copyright © 2013 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

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

    2015-01-01

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

  17. Performance Demonstration Program Plan for Analysis of Simulated Headspace Gases

    International Nuclear Information System (INIS)

    2007-01-01

    The Performance Demonstration Program (PDP) for headspace gases distributes blind audit samples in a gas matrix for analysis of volatile organic compounds (VOCs). Participating measurement facilities (i.e., fixed laboratories, mobile analysis systems, and on-line analytical systems) are located across the United States. Each sample distribution is termed a PDP cycle. These evaluation cycles provide an objective measure of the reliability of measurements performed for transuranic (TRU) waste characterization. The primary documents governing the conduct of the PDP are the Quality Assurance Program Document (QAPD) (DOE/CBFO-94-1012) and the Waste Isolation Pilot Plant (WIPP) Waste Analysis Plan (WAP) contained in the Hazardous Waste Facility Permit (NM4890139088-TSDF) issued by the New Mexico Environment Department (NMED). The WAP requires participation in the PDP; the PDP must comply with the QAPD and the WAP. This plan implements the general requirements of the QAPD and the applicable requirements of the WAP for the Headspace Gas (HSG) PDP. Participating measurement facilities analyze blind audit samples of simulated TRU waste package headspace gases according to the criteria set by this PDP Plan. Blind audit samples (hereafter referred to as PDP samples) are used as an independent means to assess each measurement facility's compliance with the WAP quality assurance objectives (QAOs). To the extent possible, the concentrations of VOC analytes in the PDP samples encompass the range of concentrations anticipated in actual TRU waste package headspace gas samples. Analyses of headspace gases are required by the WIPP to demonstrate compliance with regulatory requirements. These analyses must be performed by measurement facilities that have demonstrated acceptable performance in this PDP. These analyses are referred to as WIPP analyses and the TRU waste package headspace gas samples on which they are performed are referred to as WIPP samples in this document

  18. Determination of 3-chloro-1,2-propanediol in polyamideamine epichlorohydrin resin solution by reaction-based headspace gas chromatography.

    Science.gov (United States)

    Yan, Ning; Wan, Xiao-Fang; Chai, Xin-Sheng; Chen, Run-Quan

    2018-04-01

    We report on a headspace gas chromatographic method for determining the content of 3-chloro-1,2-propanediol in polyamideamine epichlorohydrin resin solution. It was based on quantitatively converting 3-chloro-1,2-propanediol to formaldehyde by periodate oxidation in a closed headspace sample vial at a room temperature for 10 min, and then to methanol by borohydride reduction at 90°C for 40 min followed by the headspace gas chromatographic measurement. The results showed that the present method has an excellent measurement precision (relative standard deviation < 2.60%) and accuracy (recoveries from 96.4-102%) in 3-chloro-1,2-propanediol analysis. The limit of quantitation was 0.031 mg/mL. It is simple and suitable for determining the 3-chloro-1,2-propanediol content in polyamideamine epichlorohydrin resin solution. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. 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.

  20. Test plan for headspace gas concentration measurement and headspace ventilation rate measurement for DCRTs 241-A-244, 241-BX-244, 241-S-244, 241-TX-244

    International Nuclear Information System (INIS)

    Bauer, R.E.

    1998-01-01

    This test plan provides the directions to characterize the headspace gas concentrations and the headspace ventilation rate for double contained receiver tanks 241-A-244, 241-BX-244, 241-S-244, and 241-TX-244

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

    International Nuclear Information System (INIS)

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

    2013-01-01

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

  2. Performance Demonstration Program Plan for Analysis of Simulated Headspace Gases

    International Nuclear Information System (INIS)

    2006-01-01

    The Performance Demonstration Program (PDP) for headspace gases distributes sample gases of volatile organic compounds (VOCs) for analysis. Participating measurement facilities (i.e., fixed laboratories, mobile analysis systems, and on-line analytical systems) are located across the United States. Each sample distribution is termed a PDP cycle. These evaluation cycles provide an objective measure of the reliability of measurements performed for transuranic (TRU) waste characterization. The primary documents governing the conduct of the PDP are the Quality Assurance Program Document (QAPD) (DOE/CBFO-94-1012) and the Waste Isolation Pilot Plant (WIPP) Waste Analysis Plan (WAP) contained in the Hazardous Waste Facility Permit (NM4890139088-TSDF) issued by the New Mexico Environment Department (NMED). The WAP requires participation in the PDP; the PDP must comply with the QAPD and the WAP. This plan implements the general requirements of the QAPD and the applicable requirements of the WAP for the Headspace Gas (HSG) PDP. Participating measurement facilities analyze blind audit samples of simulated TRU waste package headspace gases according to the criteria set by this PDP Plan. Blind audit samples (hereafter referred to as PDP samples) are used as an independent means to assess each measurement facility's compliance with the WAP quality assurance objectives (QAOs). To the extent possible, the concentrations of VOC analytes in the PDP samples encompass the range of concentrations anticipated in actual TRU waste package headspace gas samples. Analyses of headspace gases are required by the WIPP to demonstrate compliance with regulatory requirements. These analyses must be performed by measurement facilities that have demonstrated acceptable performance in this PDP. These analyses are referred to as WIPP analyses and the TRU waste package headspace gas samples on which they are performed are referred to as WIPP samples in this document. Participating measurement

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2013-06-19

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

  4. Efficient quantification of water content in edible oils by headspace gas chromatography with vapour phase calibration.

    Science.gov (United States)

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

    2018-06-01

    An automated and accurate headspace gas chromatographic (HS-GC) technique was investigated for rapidly quantifying water content in edible oils. In this method, multiple headspace extraction (MHE) procedures were used to analyse the integrated water content from the edible oil sample. A simple vapour phase calibration technique with an external vapour standard was used to calibrate both the water content in the gas phase and the total weight of water in edible oil sample. After that the water in edible oils can be quantified. The data showed that the relative standard deviation of the present HS-GC method in the precision test was less than 1.13%, the relative differences between the new method and a reference method (i.e. the oven-drying method) were no more than 1.62%. The present HS-GC method is automated, accurate, efficient, and can be a reliable tool for quantifying water content in edible oil related products and research. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

  5. Analysis of Furaneol in tomato using dynamic headspace sampling with sodium sulfate.

    Science.gov (United States)

    Buttery, R G; Takeoka, G R; Naim, M; Rabinowitch, H; Nam, Y

    2001-09-01

    High-flow dynamic headspace sampling with excess anhydrous sodium sulfate was found to be an effective method of isolating Furaneol from fresh tomatoes. Quantitative analysis was carried out by gas chromatography using maltol as internal standard. Furaneol was found in the highest concentrations (660-1100 ppb) in the summer crop of home-grown tomatoes and in some of the greenhouse hydroponically grown tomatoes, which are ripened on the plant before being transported to the supermarkets. Furaneol was found in the lowest concentrations (38-180 ppb) in the common ethylene-ripened, field-grown, supermarket tomatoes.

  6. Analysis of volatile headspace gases sampled by cryogenic traps from Westinghouse Hanford Company Tank 242-C-112 March 1992

    International Nuclear Information System (INIS)

    Lucke, R.B.; Clauss, S.A.

    1993-10-01

    Results are given from gas chromatography/mass spectrometry (GC/MS) analyses of the headspace samples obtained by using cryogenic traps from Westinghouse Hanford Company (WHC) Tank 112-C during the month of March, 1992. Samples were analyzed as received with no sample preparation. Analyses included direct GC/MS for volatile/semivolatile components, and direct GC/MS for ammonia. Purge and trap GC/MS analysis was not done. In addition, aliquots were sent to Karl Pool, Pacific Northwest Laboratory, for hydrogen cyanide analysis by ion chromatography, the results are reported here. All concentrations are reported for the methanol extract solutions. To calculate concentrations in the headspace, the cryo-sampling air volume and the methanol rinse volume must be obtained from cryo-sampling personnel at WHC. Triplicate analyses were done on all samples, and average concentrations and standard deviations are reported. One significant result was that no ammonia was detected

  7. Magnetic headspace adsorptive extraction of chlorobenzenes prior to thermal desorption gas chromatography-mass spectrometry

    International Nuclear Information System (INIS)

    Vidal, Lorena; Ahmadi, Mazaher; Fernández, Elena; Madrakian, Tayyebeh; Canals, Antonio

    2017-01-01

    This study presents a new, user-friendly, cost-effective and portable headspace solid-phase extraction technique based on graphene oxide decorated with iron oxide magnetic nanoparticles as sorbent, located on one end of a small neodymium magnet. Hence, the new headspace solid-phase extraction technique has been called Magnetic Headspace Adsorptive Extraction (Mag-HSAE). In order to assess Mag-HSAE technique applicability to model analytes, some chlorobenzenes were extracted from water samples prior to gas chromatography-mass spectrometry determination. A multivariate approach was employed to optimize the experimental parameters affecting Mag-HSAE. The method was evaluated under optimized extraction conditions (i.e., sample volume, 20 mL; extraction time, 30 min; sorbent amount, 10 mg; stirring speed, 1500 rpm, and ionic strength, non-significant), obtaining a linear response from 0.5 to 100 ng L −1 for 1,3-DCB, 1,4-DCB, 1,2-DCB, 1,3,5-TCB, 1,2,4-TCB and 1,2,3-TCB; from 0.5 to 75 ng L −1 for 1,2,4,5-TeCB, and PeCB; and from 1 to 75 ng L −1 for 1,2,3,4-TeCB. The repeatability of the proposed method was evaluated at 10 ng L −1 and 50 ng L −1 spiking levels, and coefficients of variation ranged between 1.5 and 9.5% (n = 5). Limits of detection values were found between 93 and 301 pg L −1 . Finally, tap, mineral and effluent water were selected as real water samples to assess method applicability. Relative recoveries varied between 86 and 110% showing negligible matrix effects. - Highlights: • A new extraction technique named Magnetic Headspace Adsorptive Extraction is presented. • Graphene oxide/iron oxide composite deposited on a neodymiun magnet as sorbent. • Sorbent of low cost, rapid and simple synthesis, easy manipulation and portability options. • Fast and efficient extraction and sensitive determination of chlorobenzenes in water samples.

  8. Analysis of residual toluene in food packaging via headspace extraction method using gas chromatography

    International Nuclear Information System (INIS)

    Lim, Ying Chin; Mohd Marsin Sanagi

    2008-01-01

    Polymeric materials are used in many food contact applications as packaging material. The presence of residual toluene in this food packaging material can migrate into food and thus affect the quality of food. In this study, a manual headspace analysis was successfully designed and developed. The determination of residual toluene was carried out with standard addition method and multiple headspace extraction, MHE) method using gas chromatography-flame ionization detector, GC-FID). Identification of toluene was performed by comparison of its retention time with standard toluene and GC-MS. It was found that the suitable heating temperature was 180 degree Celsius with an optimum heating time of 10 minutes. The study also found that the concentration of residual toluene in multicolored sample was higher compared to mono colored sample whereas residual toluene in sample analyzed using standard addition method was higher compared to MHE method. However, comparison with the results obtained from De Paris laboratory, France found that MHE method gave higher accuracy for sample with low analyte concentration. On the other hand, lower accuracy was obtained for sample with high concentration of residual toluene due to systematic errors. Comparison between determination methods showed that MHE method is more precise compared to standard addition method. (author)

  9. Use of a holder-vacuum tube device to save on-site hands in preparing urine samples for head-space gas-chromatography, and its application to determine the time allowance for sample sealing.

    Science.gov (United States)

    Kawai, Toshio; Sumino, Kimiaki; Ohashi, Fumiko; Ikeda, Masayuki

    2011-01-01

    To facilitate urine sample preparation prior to head-space gas-chromatographic (HS-GC) analysis. Urine samples containing one of the five solvents (acetone, methanol, methyl ethyl ketone, methyl isobutyl ketone and toluene) at the levels of biological exposure limits were aspirated into a vacuum tube via holder, a device commercially available for venous blood collection (the vacuum tube method). The urine sample, 5 ml, was quantitatively transferred to a 20-ml head-space vial prior to HS-GC analysis. The loaded tubes were stored at +4 ℃ in dark for up to 3 d. The vacuum tube method facilitated on-site procedures of urine sample preparation for HS-GC with no significant loss of solvents in the sample and no need of skilled hands, whereas on-site sample preparation time was significantly reduced. Furthermore, no loss of solvents was detected during the 3-d storage, irrespective of hydrophilic (acetone) or lipophilic solvent (toluene). In a pilot application, high performance of the vacuum tube method in sealing a sample in an air-tight space succeeded to confirm that no solvent will be lost when sealing is completed within 5 min after urine voiding, and that the allowance time is as long as 30 min in case of toluene in urine. The use of the holder-vacuum tube device not only saves hands for transfer of the sample to air-tight space, but facilitates sample storage prior to HS-GC analysis.

  10. The application of headspace gas chromatography coupled to tandem quadrupole mass spectrometry for the analysis of furan in baby food samples.

    Science.gov (United States)

    Pugajeva, Iveta; Rozentale, Irina; Viksna, Arturs; Bartkiene, Elena; Bartkevics, Vadims

    2016-12-01

    Selective methodology employing a tandem quadrupole mass spectrometer coupled to a gas chromatograph with headspace autosampler (HS-GC-MS/MS) was elaborated in this study. Application of the elaborated procedure resulted in a limit of detection of 0.021μgkg(-1) and a limit of quantification of 0.071μgkg(-1). The mean recoveries during in-house validation ranged from 89% to 109%, and coefficients of variation for repeatability ranged from 4% to 11%. The proposed analytical method was applied for monitoring the furan content of 30 commercial baby food samples available on the Latvian retail market. The level of furan found in these samples varied from 0.45 to 81.9μgkg(-1), indicating that infants whose sole diet comprises baby food sold in jars and cans are exposed constantly to furan. Samples containing vegetables and meat had higher levels of furan than those containing only fruits. Copyright © 2016 Elsevier Ltd. All rights reserved.

  11. A Headspace Solid Phase Microextraction (HS-SPME method for the chromatographic determination of alkylpyrazines in cocoa samples

    Directory of Open Access Journals (Sweden)

    Pini Gláucia F.

    2004-01-01

    Full Text Available A Headspace Solid Phase Microextraction (HS-SPME procedure for isolation and determination of alkylpyrazines in cocoa liquor, using Gas Chromatography with Flame Ionization Detection (GC-FID for the separation and detection of the analytes, is presented here. The HS-SPME operational conditions were optimized using extractions of samples spiked with known amounts of alkylpyrazines typically found on cocoa products. The maximum extraction efficiency was obtained using SPME fibers coated with 65 µm Carbowax/divinylbenzene. Additionally, the best results were achieved with extraction temperature of 60 ºC, 15 min of sample/headspace equilibration time and 45 min extraction time. It was also observed that suspending the samples in saturated aqueous NaCl solution during extractions resulted in a significant increment on the peak areas. This procedure was found to be effective to determine the so-called pyrazinic ratios (quotient between peak areas of alkylpyrazines, which are useful as quality parameters for cocoa liquor.

  12. Automated headspace solid-phase dynamic extraction to analyse the volatile fraction of food matrices.

    Science.gov (United States)

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

    2004-01-23

    High concentration capacity headspace techniques (headspace solid-phase microextraction (HS-SPME) and headspace sorptive extraction (HSSE)) are a bridge between static and dynamic headspace, since they give high concentration factors as does dynamic headspace (D-HS), and are as easy to apply and as reproducible as static headspace (S-HS). In 2000, Chromtech (Idstein, Germany) introduced an inside-needle technique for vapour and liquid sampling, solid-phase dynamic extraction (SPDE), also known as "the magic needle". In SPDE, analytes are concentrated on a 50 microm film of polydimethylsiloxane (PDMS) and activated carbon (10%) coated onto the inside wall of the stainless steel needle (5 cm) of a 2.5 ml gas tight syringe. When SPDE is used for headspace sampling (HS-SPDE), a fixed volume of the headspace of the sample under investigation is sucked up an appropriate number of times with the gas tight syringe and an analyte amount suitable for a reliable GC or GC-MS analysis accumulates in the polymer coating the needle wall. This article describes the preliminary results of both a study on the optimisation of sampling parameters conditioning HS-SPDE recovery, through the analysis of a standard mixture of highly volatile compounds (beta-pinene, isoamyl acetate and linalool) and of the HS-SPDE-GC-MS analyses of aromatic plants and food matrices. This study shows that HS-SPDE is a successful technique for HS-sampling with high concentration capability, good repeatability and intermediate precision, also when it is compared to HS-SPME.

  13. Dynamic Headspace Sampling as an Initial Step for Sample Preparation in Chromatographic Analysis.

    Science.gov (United States)

    Wojnowski, Wojciech; Majchrzak, Tomasz; Dymerski, Tomasz; Gębicki, Jacek; Namieśnik, Jacek

    2017-11-01

    This work represents a brief summary of the use of dynamic headspace (DHS) as a technique for sample preparation in chromatographic analysis. Despite numerous developments in the area of analyte isolation and enrichment, DHS remains one of the fundamental methods used with GC. In our opinion, interest in this technique will not diminish significantly because it conforms to stipulations of green analytical chemistry. Moreover, DHS fulfills the need for methods that facilitate detection and determination of analytes present at ultratrace levels in complex matrixes. The main focus of this work was placed on the theoretical fundamentals of this method. Also described herein were DHS development, the advantages and disadvantages of this technique compared with other headspace sampling techniques, and selected examples of its applications in food and environmental analyses.

  14. A headspace solid-phase microextraction procedure coupled with gas chromatography-mass spectrometry for the analysis of volatile polycyclic aromatic hydrocarbons in milk samples

    Energy Technology Data Exchange (ETDEWEB)

    Aguinaga, N.; Campillo, N.; Vinas, P.; Hernandez-Cordoba, M. [University of Murcia, Department of Analytical Chemistry, Faculty of Chemistry, Murcia (Spain)

    2008-06-15

    A sensitive and solvent-free method for the determination of ten polycyclic aromatic hydrocarbons, namely, naphthalene, acenaphthylene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benzo[a]anthracene and chrysene, with up to four aromatic rings, in milk samples using headspace solid-phase microextraction and gas chromatography-mass spectrometry detection has been developed. A polydimethylsiloxane-divinylbenzene fiber was chosen and used at 75 C for 60 min. Detection limits ranging from 0.2 to 5 ng L{sup -1} were attained at a signal-to-noise ratio of 3, depending on the compound and the milk sample under analysis. The proposed method was applied to ten different milk samples and the presence of six of the analytes studied in a skimmed milk with vegetal fiber sample was confirmed. The reliability of the procedure was verified by analyzing two different certified reference materials and by recovery studies. (orig.)

  15. A rapid method for simultaneously determining ethanol and methanol content in wines by full evaporation headspace gas chromatography.

    Science.gov (United States)

    Zhang, Chun-Yun; Lin, Neng-Biao; Chai, Xin-Sheng; Zhong-Li; Barnes, Donald G

    2015-09-15

    This work reports on a full evaporation headspace gas chromatographic (FE HS-GC) method for simultaneously determining the ethanol (EtOH) and methanol (MeOH) content in wines. A small sample (10μL) was placed in a headspace sample vial, and a near-complete mass transfer of ethanol and methanol from the liquid sample to the vapor phase was obtained within three minutes at a temperature of 105°C, which allowed the measurement of the EtOH and MeOH content in the sample by GC. The results showed excellent precision and accuracy, as shown by the reproducibilities of 1.02% and 2.11% for EtOH and MeOH, respectively, and recoveries that ranged from 96.1% to 104% for both alcohols. The method is efficient, accurate and suitable for the determination of EtOH and MeOH in wine production and quality control. Copyright © 2015 Elsevier Ltd. All rights reserved.

  16. Analysis of hydrogen and methane in seawater by "Headspace" method: Determination at trace level with an automatic headspace sampler.

    Science.gov (United States)

    Donval, J P; Guyader, V

    2017-01-01

    "Headspace" technique is one of the methods for the onboard measurement of hydrogen (H 2 ) and methane (CH 4 ) in deep seawater. Based on the principle of an automatic headspace commercial sampler, a specific device has been developed to automatically inject gas samples from 300ml syringes (gas phase in equilibrium with seawater). As valves, micro pump, oven and detector are independent, a gas chromatograph is not necessary allowing a reduction of the weight and dimensions of the analytical system. The different steps from seawater sampling to gas injection are described. Accuracy of the method is checked by a comparison with the "purge and trap" technique. The detection limit is estimated to 0.3nM for hydrogen and 0.1nM for methane which is close to the background value in deep seawater. It is also shown that this system can be used to analyze other gases such as Nitrogen (N 2 ), carbon monoxide (CO), carbon dioxide (CO 2 ) and light hydrocarbons. Copyright © 2016 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

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

    2012-05-18

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

  18. Measurement of activity coefficients of mixtures by head-space gas chromatography: general procedure.

    Science.gov (United States)

    Luis, Patricia; Wouters, Christine; Van der Bruggen, Bart; Sandler, Stanley I

    2013-08-09

    Head-space gas chromatography (HS-GC) is an applicable method to perform vapor-liquid equilibrium measurements and determine activity coefficients. However, the reproducibility of the data may be conditioned by the experimental procedure concerning to the automated pressure-balanced system. The study developed in this work shows that a minimum volume of liquid in the vial is necessary to ensure the reliability of the activity coefficients since it may become a parameter that influences the magnitude of the peak areas: the helium introduced during the pressurization step may produce significant variations of the results when too small volume of liquid is selected. The minimum volume required should thus be evaluated prior to obtain experimentally the concentration in the vapor phase and the activity coefficients. In this work, the mixture acetonitrile-toluene is taken as example, requiring a sample volume of more than 5mL (about more than 25% of the vial volume). The vapor-liquid equilibrium and activity coefficients of mixtures at different concentrations (0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9 molar fraction) and four temperatures (35, 45, 55 and 70°C) have been determined. Relative standard deviations (RSD) lower than 5% have been obtained, indicating the good reproducibility of the method when a sample volume larger than 5mL is used. Finally, a general procedure to measure activity coefficients by means of pressure-balanced head-space gas chromatography is proposed. Copyright © 2013 Elsevier B.V. All rights reserved.

  19. Magnetic headspace adsorptive extraction of chlorobenzenes prior to thermal desorption gas chromatography-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Vidal, Lorena, E-mail: lorena.vidal@ua.es [Department of Analytical Chemistry, Nutrition and Food Sciences and University Institute of Materials, University of Alicante, P.O. Box 99, E-03080, Alicante (Spain); Ahmadi, Mazaher [Faculty of Chemistry, Bu-Ali Sina University, Hamedan (Iran, Islamic Republic of); Fernández, Elena [Department of Analytical Chemistry, Nutrition and Food Sciences and University Institute of Materials, University of Alicante, P.O. Box 99, E-03080, Alicante (Spain); Madrakian, Tayyebeh [Faculty of Chemistry, Bu-Ali Sina University, Hamedan (Iran, Islamic Republic of); Canals, Antonio, E-mail: a.canals@ua.es [Department of Analytical Chemistry, Nutrition and Food Sciences and University Institute of Materials, University of Alicante, P.O. Box 99, E-03080, Alicante (Spain)

    2017-06-08

    This study presents a new, user-friendly, cost-effective and portable headspace solid-phase extraction technique based on graphene oxide decorated with iron oxide magnetic nanoparticles as sorbent, located on one end of a small neodymium magnet. Hence, the new headspace solid-phase extraction technique has been called Magnetic Headspace Adsorptive Extraction (Mag-HSAE). In order to assess Mag-HSAE technique applicability to model analytes, some chlorobenzenes were extracted from water samples prior to gas chromatography-mass spectrometry determination. A multivariate approach was employed to optimize the experimental parameters affecting Mag-HSAE. The method was evaluated under optimized extraction conditions (i.e., sample volume, 20 mL; extraction time, 30 min; sorbent amount, 10 mg; stirring speed, 1500 rpm, and ionic strength, non-significant), obtaining a linear response from 0.5 to 100 ng L{sup −1} for 1,3-DCB, 1,4-DCB, 1,2-DCB, 1,3,5-TCB, 1,2,4-TCB and 1,2,3-TCB; from 0.5 to 75 ng L{sup −1} for 1,2,4,5-TeCB, and PeCB; and from 1 to 75 ng L{sup −1} for 1,2,3,4-TeCB. The repeatability of the proposed method was evaluated at 10 ng L{sup −1} and 50 ng L{sup −1} spiking levels, and coefficients of variation ranged between 1.5 and 9.5% (n = 5). Limits of detection values were found between 93 and 301 pg L{sup −1}. Finally, tap, mineral and effluent water were selected as real water samples to assess method applicability. Relative recoveries varied between 86 and 110% showing negligible matrix effects. - Highlights: • A new extraction technique named Magnetic Headspace Adsorptive Extraction is presented. • Graphene oxide/iron oxide composite deposited on a neodymiun magnet as sorbent. • Sorbent of low cost, rapid and simple synthesis, easy manipulation and portability options. • Fast and efficient extraction and sensitive determination of chlorobenzenes in water samples.

  20. Possibilities and limitations of dynamic headspace sampling as a pre-concentration technique for trace analysis of organics by capillary gas chromatography

    NARCIS (Netherlands)

    Curvers, J.M.P.M.; Noij, T.H.M.; Cramers, C.A.M.G.; Rijks, J.A.

    1984-01-01

    The possibilities, the limitations and the quantitative performance of dynamic headspace sampling, in particular closed-loop stripping, were investigated for various classes of organic substances in aqueous samples with concentrations down to the parts per 1012 (ppt) level. The effects of variations

  1. Determination of microstickies in recycled whitewater by headspace gas chromatography.

    Science.gov (United States)

    Chai, X-S; Samp, J C; Yang, Q F; Song, H N; Zhang, D C; Zhu, J Y

    2006-03-03

    This study proposed a novel headspace gas chromatographic (HS-GC) method for determination of adhesive contaminants (microstickies) in recycled whitewater, a fiber containing process stream, in the paper mill. It is based on the adsorption behavior of toluene (as a tracer) on the hydrophobic surface of microstickies, which affects the apparent vapor-liquid equilibration partitioning of toluene. It was found that the equilibrium concentration of toluene in the vapor phase is inversely proportional to the apparent effective surface area of microstickies that remain in the corresponding solution. Thus, the amount of microsticky materials in the recycled whitewater can be quantified by HS-GC via indirect measurement of the toluene content in the vapor phase of the sample without any pretreatment. The presented method is simple, rapid and automated.

  2. Headspace gas and vapor characterization summary for the 43 vapor program suspect tanks

    International Nuclear Information System (INIS)

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

    1995-01-01

    During the time period between February 1994 and September 1995, Westinghouse Hanford Company (WHC) sampled the waste tank headspace of 43 single-shell tanks for a variety of gaseous and/or volatile and semi-volatile compounds. This report summarizes the results of analyses of those sampling activities with respect to both the Priority 1 Safety Issues and relative to the detection in the headspace of significant concentrations of target analytes relating to worker breathing space consideration as recommended by the Pacific Northwest Laboratory (PNL) Toxicology Review Panel. The information contained in the data tables was abstracted from the vapor sampling and analysis tank characterization reports. Selected results are tabulated and summarized. Sampling equipment and methods, as well as sample analyses, are briefly described. Vapor sampling of passively ventilated single-shell tanks (tanks C-105, C-106, and SX-106 were sampled and are actively ventilated) has served to highlight or confirm tank headspace conditions associated with both priority 1 safety issues and supports source term analysis associated with protecting worker health and safety from noxious vapors

  3. Determination of the Three Main Components of the Grapevine Moth Pest Pheromone in Grape-Related Samples by Headspace-Gas Chromatography-Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    María del Carmen Alcudia-León

    2017-10-01

    Full Text Available The grapevine moth (Lobesia botrana is the most significant pest of viticulture. This article reports the development of an analytical method that allows the instrumental determination of the three main pheromone components of the pest ((E,Z-7,9-dodecadien-1-yl acetate, (E,Z-7,9-dodecadien-1-ol and (Z-9-dodecen-1-yl acetate in grape-related samples (must, table grape and wine grape. The combination of headspace, gas chromatography and mass spectrometry provides limits of detection in the range of 60–420 ng/Kg and precision, expressed as a relative standard deviation, better than 8.5%. This analytical approach is rapid and simple and opens a door to the study of the pest incidence on the final products.

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

    Directory of Open Access Journals (Sweden)

    Kyriaki Machera

    2008-05-01

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

  5. Determination of carboxyl groups in wood fibers by headspace gas chromatography

    Science.gov (United States)

    X.-S. Chai; Q.X. Hou; J.Y. Zhu; S.-L. Chen; S.F. Wang; L. Lucia

    2003-01-01

    The phase reaction conversion (PRC) headspace gas chromatographic (HSGC) technique was employed to develop a method for the determination of the content of carboxyl groups in wood fibers. Acid treatment of the wood fibers using hydrochloric was applied to convert carboxyl groups to carboxyl acids. Bicarbonate solution is then used to react with carboxyl acids on the...

  6. Development of headspace solid-phase microextraction method for ...

    African Journals Online (AJOL)

    A headspace solid-phase microextraction (HS-SPME) method was developed as a preliminary investigation using univariate approach for the analysis of 14 multiclass pesticide residues in fruits and vegetable samples. The gas chromatography mass spectrometry parameters (desorption temperature and time, column flow ...

  7. Microwave-assisted headspace single-drop microextration of chlorobenzenes from water samples

    Energy Technology Data Exchange (ETDEWEB)

    Vidal, Lorena [Departamento de Quimica Analitica, Nutricion y Bromatologia, Universidad de Alicante, P.O. Box 99, E-03080 Alicante (Spain); Domini, Claudia E. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Universidad de Alicante, P.O. Box 99, E-03080 Alicante (Spain); Grane, Nuria [Departamento de Quimica Analitica, Nutricion y Bromatologia, Universidad de Alicante, P.O. Box 99, E-03080 Alicante (Spain); Psillakis, Elefteria [Department of Environmental Engineering, Technical University of Crete, Polytechneioupolis, GR-73100 Chania, Crete (Greece); Canals, Antonio [Departamento de Quimica Analitica, Nutricion y Bromatologia, Universidad de Alicante, P.O. Box 99, E-03080 Alicante (Spain)]. E-mail: a.canals@ua.es

    2007-05-29

    A one-step and in-situ sample preparation method used for quantifying chlorobenzene compounds in water samples has been developed, coupling microwave and headspace single-drop microextraction (MW-HS-SDME). The chlorobenzenes in water samples were extracted directly onto an ionic liquid single-drop in headspace mode under the aid of microwave radiation. For optimization, a Plackett-Burman screening design was initially used, followed by a mixed-level factorial design. The factors considered were: drop volume, aqueous sample volume, stirring speed, ionic strength, extraction time, ionic liquid type, microwave power and length of the Y-shaped glass-tube. The optimum experimental conditions found from this statistical evaluation were: a 5 {mu}L microdrop of 1-hexyl-3-methylimidazolium hexafluorophosphate exposed for 20 min to the headspace of a 30 mL aqueous sample, irradiated by microwaves at 200 W and placed in a 50 mL spherical flask connected to a 25 cm Y-shaped glass-tube. Under the optimised experimental conditions, the response of a high performance liquid chromatographic system was found to be linear over the range studied and with correlation coefficients ranging between 0.9995 and 0.9999. The method showed a good level of repeatability, with relative standard deviations varying between 2.3 and 8.3% (n = 5). Detection limits were found in the low {mu}g L{sup -1} range varying between 0.016 and 0.039 {mu}g L{sup -1}. Overall, the performance of the proposed method demonstrated the favourable effect of microwave sample irradiation upon HS-SDME. Finally, recovery studies from different types of environmental water samples revealed that matrix had little effect upon extraction.

  8. Microwave-assisted headspace single-drop microextration of chlorobenzenes from water samples

    International Nuclear Information System (INIS)

    Vidal, Lorena; Domini, Claudia E.; Grane, Nuria; Psillakis, Elefteria; Canals, Antonio

    2007-01-01

    A one-step and in-situ sample preparation method used for quantifying chlorobenzene compounds in water samples has been developed, coupling microwave and headspace single-drop microextraction (MW-HS-SDME). The chlorobenzenes in water samples were extracted directly onto an ionic liquid single-drop in headspace mode under the aid of microwave radiation. For optimization, a Plackett-Burman screening design was initially used, followed by a mixed-level factorial design. The factors considered were: drop volume, aqueous sample volume, stirring speed, ionic strength, extraction time, ionic liquid type, microwave power and length of the Y-shaped glass-tube. The optimum experimental conditions found from this statistical evaluation were: a 5 μL microdrop of 1-hexyl-3-methylimidazolium hexafluorophosphate exposed for 20 min to the headspace of a 30 mL aqueous sample, irradiated by microwaves at 200 W and placed in a 50 mL spherical flask connected to a 25 cm Y-shaped glass-tube. Under the optimised experimental conditions, the response of a high performance liquid chromatographic system was found to be linear over the range studied and with correlation coefficients ranging between 0.9995 and 0.9999. The method showed a good level of repeatability, with relative standard deviations varying between 2.3 and 8.3% (n = 5). Detection limits were found in the low μg L -1 range varying between 0.016 and 0.039 μg L -1 . Overall, the performance of the proposed method demonstrated the favourable effect of microwave sample irradiation upon HS-SDME. Finally, recovery studies from different types of environmental water samples revealed that matrix had little effect upon extraction

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

    Science.gov (United States)

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

    2014-04-18

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

  10. Determination of the content of alkyl ketene dimer in its latex by an ionic-liquid assisted headspace gas chromatography.

    Science.gov (United States)

    Yan, Ning; Wan, Xiao-Fang; Chai, Xin-Sheng; Chen, Run-Quan; Chen, Chun-Xia

    2017-12-29

    This paper reports on an ionic-liquid assisted headspace gas chromatographic (HS-GC) for the determination of the content of alkyl ketene dimer (AKD) in its latex samples, in which the GC system was equipped with a thermal conductivity detector (TCD). The method was based on the AKD hydrolysis conducted in 1-butyl-3-methylimidazolium chloride (ionic-liquid) added medium at 100°C for 10min in a closed headspace sample vial, and the measured CO 2 (the resulting product of the hydrolysis) by HS-GC. The results showed that the present method has a good measurement precision (RSD <2.3%) and accuracy (recoveries from 96 - 105%), and the limit of quantitation (LOQ) is 0.9%. The present method is very suitable to be used for the routine check of AKD content in its latex sample in mill applications. The study also showed that the content of AKD in the tested commercial latex samples were in the range of 3.5-12%. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Monitoring gas-phase CO2 in the headspace of champagne glasses through combined diode laser spectrometry and micro-gas chromatography analysis.

    Science.gov (United States)

    Moriaux, Anne-Laure; Vallon, Raphaël; Parvitte, Bertrand; Zeninari, Virginie; Liger-Belair, Gérard; Cilindre, Clara

    2018-10-30

    During Champagne or sparkling wine tasting, gas-phase CO 2 and volatile organic compounds invade the headspace above glasses, thus progressively modifying the chemical space perceived by the consumer. Gas-phase CO 2 in excess can even cause a very unpleasant tingling sensation perturbing both ortho- and retronasal olfactory perception. Monitoring as accurately as possible the level of gas-phase CO 2 above glasses is therefore a challenge of importance aimed at better understanding the close relationship between the release of CO 2 and a collection of various tasting parameters. Here, the concentration of CO 2 found in the headspace of champagne glasses served under multivariate conditions was accurately monitored, all along the 10 min following pouring, through a new combined approach by a CO 2 -Diode Laser Sensor and micro-gas chromatography. Our results show the strong impact of various tasting conditions (volume dispensed, intensity of effervescence, and glass shape) on the release of gas-phase CO 2 above the champagne surface. Copyright © 2018 Elsevier Ltd. All rights reserved.

  12. Solid phase microextraction headspace sampling of chemical warfare agent contaminated samples : method development for GC-MS analysis

    Energy Technology Data Exchange (ETDEWEB)

    Jackson Lepage, C.R.; Hancock, J.R. [Defence Research and Development Canada, Medicine Hat, AB (Canada); Wyatt, H.D.M. [Regina Univ., SK (Canada)

    2004-07-01

    Defence R and D Canada-Suffield (DRDC-Suffield) is responsible for analyzing samples that are suspected to contain chemical warfare agents, either collected by the Canadian Forces or by first-responders in the event of a terrorist attack in Canada. The analytical techniques used to identify the composition of the samples include gas chromatography-mass spectrometry (GC-MS), liquid chromatography-mass spectrometry (LC-MS), Fourier-transform infrared spectroscopy (FT-IR) and nuclear magnetic resonance spectroscopy. GC-MS and LC-MS generally require solvent extraction and reconcentration, thereby increasing sample handling. The authors examined analytical techniques which reduce or eliminate sample manipulation. In particular, this paper presented a screening method based on solid phase microextraction (SPME) headspace sampling and GC-MS analysis for chemical warfare agents such as mustard, sarin, soman, and cyclohexyl methylphosphonofluoridate in contaminated soil samples. SPME is a method which uses small adsorbent polymer coated silica fibers that trap vaporous or liquid analytes for GC or LC analysis. Collection efficiency can be increased by adjusting sampling time and temperature. This method was tested on two real-world samples, one from excavated chemical munitions and the second from a caustic decontamination mixture. 7 refs., 2 tabs., 3 figs.

  13. Rapid identification of pork for halal authentication using the electronic nose and gas chromatography mass spectrometer with headspace analyzer.

    Science.gov (United States)

    Nurjuliana, M; Che Man, Y B; Mat Hashim, D; Mohamed, A K S

    2011-08-01

    The volatile compounds of pork, other meats and meat products were studied using an electronic nose and gas chromatography mass spectrometer with headspace analyzer (GCMS-HS) for halal verification. The zNose™ was successfully employed for identification and differentiation of pork and pork sausages from beef, mutton and chicken meats and sausages which were achieved using a visual odor pattern called VaporPrint™, derived from the frequency of the surface acoustic wave (SAW) detector of the electronic nose. GCMS-HS was employed to separate and analyze the headspace gasses from samples into peaks corresponding to individual compounds for the purpose of identification. Principal component analysis (PCA) was applied for data interpretation. Analysis by PCA was able to cluster and discriminate pork from other types of meats and sausages. It was shown that PCA could provide a good separation of the samples with 67% of the total variance accounted by PC1. Copyright © 2011 Elsevier Ltd. All rights reserved.

  14. Performance demonstration program plan for analysis of simulated headspace gases

    International Nuclear Information System (INIS)

    1995-06-01

    The Performance Demonstration Program (PDP) for analysis of headspace gases will consist of regular distribution and analyses of test standards to evaluate the capability for analyzing VOCs, hydrogen, and methane in the headspace of transuranic (TRU) waste throughout the Department of Energy (DOE) complex. Each distribution is termed a PDP cycle. These evaluation cycles will provide an objective measure of the reliability of measurements performed for TRU waste characterization. Laboratory performance will be demonstrated by the successful analysis of blind audit samples of simulated TRU waste drum headspace gases according to the criteria set within the text of this Program Plan. Blind audit samples (hereinafter referred to as PDP samples) will be used as an independent means to assess laboratory performance regarding compliance with the QAPP QAOs. The concentration of analytes in the PDP samples will encompass the range of concentrations anticipated in actual waste characterization gas samples. Analyses which are required by the WIPP to demonstrate compliance with various regulatory requirements and which are included in the PDP must be performed by laboratories which have demonstrated acceptable performance in the PDP

  15. Determination of Porosity in Shale by Double Headspace Extraction GC Analysis.

    Science.gov (United States)

    Zhang, Chun-Yun; Li, Teng-Fei; Chai, Xin-Sheng; Xiao, Xian-Ming; Barnes, Donald

    2015-11-03

    This paper reports on a novel method for the rapid determination of the shale porosity by double headspace extraction gas chromatography (DHE-GC). Ground core samples of shale were placed into headspace vials and DHE-GC measurements of released methane gas were performed at a given time interval. A linear correlation between shale porosity and the ratio of consecutive GC signals was established both theoretically and experimentally by comparing with the results from the standard helium pycnometry method. The results showed that (a) the porosity of ground core samples of shale can be measured within 30 min; (b) the new method is not significantly affected by particle size of the sample; (c) the uncertainties of measured porosities of nine shale samples by the present method range from 0.31 to 0.46 p.u.; and (d) the results obtained by the DHE-GC method are in a good agreement with those from the standard helium pycnometry method. In short, the new DHE-GC method is simple, rapid, and accurate, making it a valuable tool for shale gas-related research and applications.

  16. Lab-In-Syringe automation of stirring-assisted room-temperature headspace extraction coupled online to gas chromatography with flame ionization detection for determination of benzene, toluene, ethylbenzene, and xylenes in surface waters.

    Science.gov (United States)

    Horstkotte, Burkhard; Lopez de Los Mozos Atochero, Natalia; Solich, Petr

    2018-06-22

    Online coupling of Lab-In-Syringe automated headspace extraction to gas chromatography has been studied. The developed methodology was successfully applied to surface water analysis using benzene, toluene, ethylbenzene, and xylenes as model analytes. The extraction system consisted of an automatic syringe pump with a 5 mL syringe into which all solutions and air for headspace formation were aspirated. The syringe piston featured a longitudinal channel, which allowed connecting the syringe void directly to a gas chromatograph with flame ionization detector via a transfer capillary. Gas injection was achieved via opening a computer-controlled pinch valve and compressing the headspace, upon which separation was initialized. Extractions were performed at room temperature; yet sensitivity comparable to previous work was obtained by high headspace to sample ratio V HS /V Sample of 1.6:1 and injection of about 77% of the headspace. Assistance by in-syringe magnetic stirring yielded an about threefold increase in extraction efficiency. Interferences were compensated by using chlorobenzene as an internal standard. Syringe cleaning and extraction lasting over 10 min was carried out in parallel to the chromatographic run enabling a time of analysis of <19 min. Excellent peak area repeatabilities with RSD of <4% when omitting and <2% RSD when using internal standard corrections on 100 μg L -1 level were achieved. An average recovery of 97.7% and limit of detection of 1-2 μg L -1 were obtained in analyses of surface water. Copyright © 2018 Elsevier B.V. All rights reserved.

  17. Determination of suspected allergens in cosmetic products by headspace-programmed temperature vaporization-fast gas chromatography-quadrupole mass spectrometry.

    Science.gov (United States)

    del Nogal Sánchez, Miguel; Pérez-Pavón, José Luis; Moreno Cordero, Bernardo

    2010-07-01

    In the present work, a strategy for the qualitative and quantitative analysis of 24 volatile compounds listed as suspected allergens in cosmetics by the European Union is reported. The list includes benzyl alcohol, limonene, linalool, methyl 2-octynoate, beta-citronellol, geraniol, citral (two isomers), 7-hydroxycitronellal, anisyl alcohol, cinnamal, cinnamyl alcohol, eugenol, isoeugenol (two isomers), coumarin, alpha-isomethyl ionone, lilial, alpha-amylcinnamal, lyral, alpha-amylcinnamyl alcohol, farnesol (three isomers), alpha-hexyl cinnamal, benzyl cinnamate, benzyl benzoate, and benzyl salicylate. The applicability of a headspace (HS) autosampler in combination with a gas chromatograph (GC) equipped with a programmable temperature vaporizer (PTV) and a quadrupole mass spectrometry (qMS) detector is explored. By using a headspace sampler, sample preparation is reduced to introducing the sample into the vial. This reduces the analysis time and the experimental errors associated with this step of the analytical process. Two different injection techniques were used: solvent-vent injection and hot-split injection. The first offers a way to improve sensitivity at the same time maintaining the simple headspace instrumentation and it is recommended for compounds at trace levels. The use of a liner packed with Tenax-TA allowed the compounds of interest to be retained during the venting process. The signals obtained when hot-split injection was used allowed quantification of all the compounds according to the thresholds of the European Cosmetics Directive. Monodimensional gas chromatography coupled to a conventional quadrupole mass spectrometry detector was used and the 24 analytes were separated appropriately along a run time of about 12 min. Use of the standard addition procedure as a quantification technique overcame the matrix effect. It should be emphasized that the method showed good precision and accuracy. Furthermore, it is rapid, simple, and--in view of the

  18. Zero-Headspace Coal-Core Gas Desorption Canister, Revised Desorption Data Analysis Spreadsheets and a Dry Canister Heating System

    Science.gov (United States)

    Barker, Charles E.; Dallegge, Todd A.

    2005-01-01

    Coal desorption techniques typically use the U.S. Bureau of Mines (USBM) canister-desorption method as described by Diamond and Levine (1981), Close and Erwin (1989), Ryan and Dawson (1993), McLennan and others (1994), Mavor and Nelson (1997) and Diamond and Schatzel (1998). However, the coal desorption canister designs historically used with this method have an inherent flaw that allows a significant gas-filled headspace bubble to remain in the canister that later has to be compensated for by correcting the measured desorbed gas volume with a mathematical headspace volume correction (McLennan and others, 1994; Mavor and Nelson, 1997).

  19. Headspace Solid Phase Microextraction in Pesticide Residues Analysis: 2. Apple Samples

    Directory of Open Access Journals (Sweden)

    Jelena Milinović

    2007-01-01

    Full Text Available Headspace solid phase microextraction method (HS/SPME, optimised previously for pesticide water solutions, was applied to trace residues of the pesticides chlorpyrifos, fenthion and bifenthrin in apple samples. One-hour extraction procedure was performed at 60oC extraction temperature. Nonpolar polydimethyl siloxane (PDMS fiber was used. Detection and quantification were carried out by gas chromatography/mass spectrometry (GC/MS. A non-pesticide treated apple sample was fortified with the pesticides over a 0.025-1.25 mg/kg concentration range in order to determine analytical parameters of the method applied. Linearity with regression coefficient (R values higher than 0.99 were obtained over the whole concentration range investigated for chlorpyrifos and fenthion, while linear dependence was observed in the 0.1-1.25 mg/kg range for bifenthrin. Relative recovery values for samples fortified at different levels were in the 56.68-82.91% range. Limit of detection (LOD values were determined as follows: 0.014 mg/kg for chlorpyrifos, 0.021 mg/kg for fenthion and 0.053 mg/kg for bifenthrin. Relative standard deviation (RSD values obtained for multiple analysis of the sample fortified at 0.6 mg/kg level were not higher than 20%.

  20. Full evaporation headspace gas chromatography for sensitive determination of high boiling point volatile organic compounds in low boiling matrices.

    Science.gov (United States)

    Mana Kialengila, Didi; Wolfs, Kris; Bugalama, John; Van Schepdael, Ann; Adams, Erwin

    2013-11-08

    Determination of volatile organic components (VOC's) is often done by static headspace gas chromatography as this technique is very robust and combines easy sample preparation with good selectivity and low detection limits. This technique is used nowadays in different applications which have in common that they have a dirty matrix which would be problematic in direct injection approaches. Headspace by nature favors the most volatile compounds, avoiding the less volatile to reach the injector and column. As a consequence, determination of a high boiling solvent in a lower boiling matrix becomes challenging. Determination of VOCs like: xylenes, cumene, N,N-dimethylformamide (DMF), dimethyl sulfoxide (DMSO), N,N-dimethylacetamide (DMA), N-methyl-2-pyrrolidone (NMP), 1,3-dimethyl-2-imidazolidinone (DMI), benzyl alcohol (BA) and anisole in water or water soluble products are an interesting example of the arising problems. In this work, a headspace variant called full evaporation technique is worked out and validated for the mentioned solvents. Detection limits below 0.1 μg/vial are reached with RSD values below 10%. Mean recovery values ranged from 92.5 to 110%. The optimized method was applied to determine residual DMSO in a water based cell culture and DMSO and DMA in tetracycline hydrochloride (a water soluble sample). Copyright © 2013 Elsevier B.V. All rights reserved.

  1. Olive Oil Headspace Characterization by a Gas Sensor Array

    International Nuclear Information System (INIS)

    Santonico, Marco; Capuano, Rosamaria; Catini, Alexandro; Dini, Francesca; Martinelli, Eugenio; Gianni, Giacomo; Migliorini, Marzia; Paolesse, Roberto; D'Amico, Arnaldo; Di Natale, Corrado

    2011-01-01

    Olive oil quality is strictly correlated to the volatile compounds profile. Both quality and defects can be connected to the presence of specific volatile compounds in the oil headspace. In this paper, olive oil samples have been artificially modified by adding a number of compounds known to be typical of the more frequent defects: fusty, musty, muddy and rancid. Results demonstrate the sensitivity of the electronic nose to the compounds characterizing the defects and then the capability of the instrument to identify the defects in real samples.

  2. 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.

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

    Science.gov (United States)

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

    2001-01-01

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

  4. Quantitative analysis of total starch content in wheat flour by reaction headspace gas chromatography.

    Science.gov (United States)

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

    2017-09-01

    This paper proposed a new reaction headspace gas chromatographic (HS-GC) method for efficiently quantifying the total starch content in wheat flours. A certain weight of wheat flour was oxidized by potassium dichromate in an acidic condition in a sealed headspace vial. The results show that the starch in wheat flour can be completely transferred to carbon dioxide at the given conditions (at 100 °C for 40 min) and the total starch content in wheat flour sample can be indirectly quantified by detecting the CO 2 formed from the oxidation reaction. The data showed that the relative standard deviation of the reaction HS-GC method in the precision test was less than 3.06%, and the relative differences between the new method and the reference method (titration method) were no more than 8.90%. The new reaction HS-GC method is automated, accurate, and can be a reliable tool for determining the total starch content in wheat flours in both laboratory and industrial applications. Graphical abstract The total starch content in wheat flour can be indirectly quantified by the GC detection of the CO 2 formed from the oxidation reaction between wheat flour and potassium dichromate in an acidic condition.

  5. Analysis of benzene, toluene, ethylbenzene and xylenes in soils by headspace and gas chromatography/flame ionization detector

    Directory of Open Access Journals (Sweden)

    Jurandir Pereira Pinto

    2006-02-01

    Full Text Available The constituents of gasoline: benzene, toluene, ethylbenzene and xylenes (BTEX are frequently found in soils due to leaks in fuel storage tanks and they present chronic toxicity. In this work it was developed and validated a methodology of BTEX analysis in soil by gas chromatography/ flame ionization detector and static headspace. The recovery of BTEX in soil samples was evaluated using soils with different textures (sandy and loamy. The analysis method showed good resolution, in a low time of analysis (less than 30 minutes. Limits of quantification of 0.05 mg Kg¯¹ soil for benzene, toluene, ethylbenzene and xylenes are below the guiding values that range from 0.15 to 95 mg Kg¯¹ soil, established to determine soil quality. It was verified that the methodology enables the use of this method for BTEX analysis of soil samples for passive environmental identification of gas stations.

  6. Isolation and quantification of volatiles in fish by dynamic headspace sampling and mass spectrometry

    DEFF Research Database (Denmark)

    Refsgaard, Hanne; Haahr, Anne-Mette; Jensen, Benny

    1999-01-01

    A dynamic headspace sampling method for isolation of volatiles in fish has been developed. The sample preparation involved freezing of fish tissue in liquid nitrogen, pulverizing the tissue, and sampling of volatiles from an aqueous slurry of the fish powder. Similar volatile patterns were...

  7. [Determination of flavor compounds in foxtail millet wine by gas chromatography-mass spectrometry coupled with headspace solid phase microextraction].

    Science.gov (United States)

    Liu, Jingke; Zhang, Aixia; Li, Shaohui; Zhao, Wei; Zhang, Yuzong; Xing, Guosheng

    2017-11-08

    To comprehensively understand flavor compounds and aroma characteristics of foxtail millet wine, extraction conditions were optimized with 85 μm polyacrylate (PA), 100 μm polydimethylsiloxane (PDMS), 75 μm carboxen (CAR)/PDMS and 50/30 μm divinylbenzene (DVB)/CAR/PDMS fibers. The flavor compounds in foxtail millet wine were investigated by gas chromatography-mass spectrometry (GC-MS) coupled with headspace solid phase microextraction (HS-SPME), and the odor characteristics and intensity were analyzed by odor active values (OAVs). The samples of 8 mL were placed in headspace vials with 1.5 g NaCl, then the headspace vials were heated at 60℃ for 40 min. Using HS-SPME with different fibers, a total of 55 flavor compounds were identified from the samples, including alcohols, esters, benzene derivatives, hydrocarbons, acids, aldehydes, ketones, terpenes, phenols and heterocycle compounds. The main flavor compounds were alcohols compounds. According to their OAVs, phenylethyl alcohol, styrene, 1-methyl-naphthalene, 2-methyl-naphthalene, benzaldehyde, benzeneacetaldehyde and 2-methoxy-phenol were established to be odor-active compounds. Phenylethyl alcohol and benzeneacetaldehyde were the most prominent odor-active compounds. PA and PDMS fibers had good extraction effect for polar and nonpolar compounds, respectively. CAR/PDMS and DVB/CAR/PDMS provided a similar compounds profile for moderate polar compounds. This research comprehensively determined flavor compounds of foxtail millet wine, and provided theoretical basis for product development and quality control.

  8. Determination of ketone bodies in blood by headspace gas chromatography-mass spectrometry

    DEFF Research Database (Denmark)

    Holm, Karen Marie Dollerup; Linnet, Kristian; Rasmussen, Brian Schou

    2010-01-01

    A gas chromatography-mass spectrometry (GC-MS) method for determination of ketone bodies (ß-hydroxybutyrate, acetone, and acetoacetate) in blood is presented. The method is based on enzymatic oxidation of D-ß-hydroxybutyrate to acetoacetate, followed by decarboxylation to acetone, which...... was quantified by the use of headspace GC-MS using acetone-(13)C(3) as an internal standard. The developed method was found to have intra- and total interday relative standard deviations

  9. Determination of volatile organic compounds in eucalyptus fast pyrolysis bio-oil by full evaporation headspace gas chromatography.

    Science.gov (United States)

    Kosinski Lima, Nathalya; Romualdo Lopes, André; Gimenes Guerrero, Palimecio; Itsuo Yamamoto, Carlos; Augusto Hansel, Fabricio

    2018-01-01

    This paper reports a full evaporation (FE) headspace gas chromatographic (HS-GC) method for the determination of the volatile organic compounds (VOCs) in bio-oil (i.e. methanol, ethanol, acetone, acetic acid and furfural). The method uses a 4μL sample of bio-oil in a headspace vial (ca. 20mL). Complete evaporation of the compounds was achieved after seven minutes at 90°C. The method showed good precision and accuracy for methanol, ethanol, acetone and acetic acid. The recovery of furfural was low (74.3%). The results showed that the protocol can be applied for the determination of methanol, ethanol, acetone and acetic acid in bio-oil. Detection limits ranged from 0.13 to 0.16μg. Acetic acid was the dominant analyte in the heavy bio-oil and light bio-oil analysis (113. 3 and 85.1µgmg -1 , respectively), followed by methanol, ethanol, and acetone. The polymerisation of furfural was suspected as the cause of its poor quantification. Copyright © 2017 Elsevier B.V. All rights reserved.

  10. Analysis of acrylonitrile, 1,3-butadiene, and related compounds in acrylonitrile-butadiene-styrene copolymers for kitchen utensils and children's toys by headspace gas chromatography/mass spectrometry.

    Science.gov (United States)

    Ohno, Hiroyuki; Kawamura, Yoko

    2010-01-01

    A headspace gas chromatography/mass spectrometry method was developed for the simultaneous determination of the residual levels of acrylonitrile (AN), 1,3-butadiene (1,3-BD), and their related compounds containing propionitrile (PN) and 4-vinyl-1-cyclohexene (4-VC) in acrylonitrile-butadiene-styrene (ABS) copolymers for kitchen utensils and children's toys. A sample was cut into small pieces, then N,N-dimethylacetamide and an internal standard were added in a sealed headspace vial. The vial was incubated for 1 h at 90 degrees C and the headspace gas was analyzed by gas chromatography/mass spectrometry. The recovery rates of the analytes were 93.3-101.8% and the coefficients of variation were 0.3-6.5%. In ABS copolymers, the levels were 0.3-50.4 microg/g for AN, ND-4.5 microg/g for PN, 0.06-1.58 microg/g for 1,3-BD, and 1.1-295 microg/g for 4-VC. The highest level was found for 4-VC, which is a dimer of 1,3-BD, and the next highest was for AN, which is one of the monomers of the ABS copolymer. Furthermore, the method was also applied to acrylonitrile-styrene (AS) copolymers and polystyrenes (PS) for kitchen utensils, and nitrile-butadiene rubber (NBR) gloves. In AS copolymers, AN and PN were detected at 16.8-54.5 and 0.8-6.9 microg/g, respectively. On the other hand, the levels in PS and NBR samples were all low.

  11. Headspace needle-trap analysis of priority volatile organic compounds from aqueous samples: application to the analysis of natural and waste waters.

    Science.gov (United States)

    Alonso, Monica; Cerdan, Laura; Godayol, Anna; Anticó, Enriqueta; Sanchez, Juan M

    2011-11-11

    Combining headspace (HS) sampling with a needle-trap device (NTD) to determine priority volatile organic compounds (VOCs) in water samples results in improved sensitivity and efficiency when compared to conventional static HS sampling. A 22 gauge stainless steel, 51-mm needle packed with Tenax TA and Carboxen 1000 particles is used as the NTD. Three different HS-NTD sampling methodologies are evaluated and all give limits of detection for the target VOCs in the ng L⁻¹ range. Active (purge-and-trap) HS-NTD sampling is found to give the best sensitivity but requires exhaustive control of the sampling conditions. The use of the NTD to collect the headspace gas sample results in a combined adsorption/desorption mechanism. The testing of different temperatures for the HS thermostating reveals a greater desorption effect when the sample is allowed to diffuse, whether passively or actively, through the sorbent particles. The limits of detection obtained in the simplest sampling methodology, static HS-NTD (5 mL aqueous sample in 20 mL HS vials, thermostating at 50 °C for 30 min with agitation), are sufficiently low as to permit its application to the analysis of 18 priority VOCs in natural and waste waters. In all cases compounds were detected below regulated levels. Copyright © 2011 Elsevier B.V. All rights reserved.

  12. [Analysis of the components of floral scent in Glochidion puberum using gas chromatography-mass spectrometry with dynamic headspace adsorption].

    Science.gov (United States)

    Huang, Daihong; Zhang, Zhenguo; Chen, Guoping; Li, Houhun; Shi, Fuchen

    2015-03-01

    The floral scent plays the important key role in maintaining the obligate pollination mutualism between Glochidion plants and Epicephala moths. In the study, the dynamic headspace adsorption technique was employed to collect the floral scent emitted by Glochidion puberum, gas chromatography coupled with mass spectrometry (GC-MS) was used for the detection and identification of volatile chemical components in headspace samples of flowers from G. puberum. The peak area normalization was used to determine the relative contents of each odour component. The results showed that 45 compounds mainly consisting of monoterpenes and sesquiterpenes were isolated from the floral scent produced by G. puberum. Especially, both linalool (38.06%) and β-elemene (23.84%) were considered as the major scent components of G. puberum. It was speculated that linalool and β-elemene may be the two potential compounds attracting female Epicephala moths. The study provided the basic data for further electroantennographic detection and bioassays to identify the compounds having the actual physiological activity to female Epicephala moths.

  13. Headspace analysis of foams and fixatives

    Energy Technology Data Exchange (ETDEWEB)

    Harper, Kyle [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Truong, Thanh-Tam [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Magwood, Leroy [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Peters, Brent [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Nicholson, James [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Washington, II, Aaron L. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

    2017-07-27

    In the process of decontaminating and decommissioning (D&D) older nuclear facilities, special precautions must be taken with removable or airborne contamination. One possible strategy utilizes foams and fixatives to affix these loose contaminants. Many foams and fixatives are already commercially available, either generically or sold specifically for D&D. However, due to a lack of revelant testing in a radioactive environment, additional verification is needed to confirm that these products not only affix contamination to their surfaces, but also will function in a D&D environment. Several significant safety factors, including flammability and worker safety, can be analyzed through the process of headspace analysis, a technique that analyzes the off gas formed before or during the curing process of the foam/fixative, usually using gas chromatography-mass spectrometry (GC-MS). This process focuses on the volatile components of a chemical, which move freely between the solid/liquid form within the sample and the gaseous form in the area above the sample (the headspace). Between possibly hot conditions in a D&D situation and heat created in a foaming reaction, the volatility of many chemicals can change, and thus different gasses can be released at different times throughout the reaction. This project focused on analysis of volatile chemicals involved in the process of using foams and fixatives to identify any potential hazardous or flammable compounds.

  14. Multiple responses optimization in the development of a headspace gas chromatography method for the determination of residual solvents in pharmaceuticals

    Directory of Open Access Journals (Sweden)

    Carla M. Teglia

    2015-10-01

    Full Text Available An efficient generic static headspace gas chromatography (HSGC method was developed, optimized and validated for the routine determination of several residual solvents (RS in drug substance, using a strategy with two sets of calibration. Dimethylsulfoxide (DMSO was selected as the sample diluent and internal standards were used to minimize signal variations due to the preparative step. A gas chromatograph from Agilent Model 6890 equipped with flame ionization detector (FID and a DB-624 (30 m×0.53 mm i.d., 3.00 µm film thickness column was used. The inlet split ratio was 5:1. The influencing factors in the chromatographic separation of the analytes were determined through a fractional factorial experimental design. Significant variables: the initial temperature (IT, the final temperature (FT of the oven and the carrier gas flow rate (F were optimized using a central composite design. Response transformation and desirability function were applied to find out the optimal combination of the chromatographic variables to achieve an adequate resolution of the analytes and short analysis time. These conditions were 30 °C for IT, 158 °C for FT and 1.90 mL/min for F. The method was proven to be accurate, linear in a wide range and very sensitive for the analyzed solvents through a comprehensive validation according to the ICH guidelines. Keywords: Headspace gas chromatography, Residual solvents, Pharmaceuticals, Surface response methodology, Desirability function

  15. Headspace vapor characterization of Hanford Waste Tank 241-U-112: Results from samples collected on 7/09/96

    International Nuclear Information System (INIS)

    Evans, J.C.; Pool, K.H.; Thomas, B.L.; Olsen, K.B.; Fruchter, J.S.; Silvers, K.L.

    1997-01-01

    This report describes the analytical results of vapor samples taken from the headspace of the waste storage tank 241-U-112 at the Hanford Site in Washington State. The results described in this report were obtained to characterize the vapors present in the tank headspace and to support safety evaluations and tank farm operations. The results include air concentrations of selected inorganic and organic analytes and grouped compounds from samples obtained by Westinghouse Hanford Company

  16. Analysis of volatile organic compounds in pleural effusions by headspace solid-phase microextraction coupled with cryotrap gas chromatography and mass spectrometry.

    Science.gov (United States)

    Huang, Zhongping; Zhang, Jie; Zhang, Peipei; Wang, Hong; Pan, Zaifa; Wang, Lili

    2016-07-01

    Headspace solid-phase microextraction coupled with cryotrap gas chromatography and mass spectrometry was applied to the analysis of volatile organic compounds in pleural effusions. The highly volatile organic compounds were separated successfully with high sensitivity by the employment of a cryotrap device, with the construction of a cold column head by freezing a segment of metal capillary with liquid nitrogen. A total of 76 volatile organic compounds were identified in 50 pleural effusion samples (20 malignant effusions and 30 benign effusions). Among them, 34 more volatile organic compounds were detected with the retention time less than 8 min, by comparing with the normal headspace solid-phase microextraction coupled with gas chromatography and mass spectrometry method. Furthermore, 24 volatile organic compounds with high occurrence frequency in pleural effusion samples, 18 of which with the retention time less than 8 min, were selected for the comparative analysis. The results of average peak area comparison and box-plot analysis showed that except for cyclohexanone, 2-ethyl-1-hexanol, and tetramethylbenzene, which have been reported as potential cancer biomarkers, cyclohexanol, dichloromethane, ethyl acetate, n-heptane, ethylbenzene, and xylene also had differential expression between malignant and benign effusions. Therefore, the proposed approach was valuable for the comprehensive characterization of volatile organic compounds in pleural effusions. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Multivariate analysis of the volatile components in tobacco based on infrared-assisted extraction coupled to headspace solid-phase microextraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Yang, Yanqin; Pan, Yuanjiang; Zhou, Guojun; Chu, Guohai; Jiang, Jian; Yuan, Kailong; Xia, Qian; Cheng, Changhe

    2016-11-01

    A novel infrared-assisted extraction coupled to headspace solid-phase microextraction followed by gas chromatography with mass spectrometry method has been developed for the rapid determination of the volatile components in tobacco. The optimal extraction conditions for maximizing the extraction efficiency were as follows: 65 μm polydimethylsiloxane-divinylbenzene fiber, extraction time of 20 min, infrared power of 175 W, and distance between the infrared lamp and the headspace vial of 2 cm. Under the optimum conditions, 50 components were found to exist in all ten tobacco samples from different geographical origins. Compared with conventional water-bath heating and nonheating extraction methods, the extraction efficiency of infrared-assisted extraction was greatly improved. Furthermore, multivariate analysis including principal component analysis, hierarchical cluster analysis, and similarity analysis were performed to evaluate the chemical information of these samples and divided them into three classifications, including rich, moderate, and fresh flavors. The above-mentioned classification results were consistent with the sensory evaluation, which was pivotal and meaningful for tobacco discrimination. As a simple, fast, cost-effective, and highly efficient method, the infrared-assisted extraction coupled to headspace solid-phase microextraction technique is powerful and promising for distinguishing the geographical origins of the tobacco samples coupled to suitable chemometrics. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Identification of volatile organic compounds (VOCs) in different colour carrot (Daucus carota L.) cultivars using static headspace/gas chromatography/mass spectrometry

    OpenAIRE

    Zehra Güler; Fatih Karaca; Halit Yetisir

    2015-01-01

    Volatile organic compounds (VOCs) as well as sugar and acid contents affect carrot flavour. This study compared VOCs in 11 carrot cultivars. Gas chromatography/mass spectrometry using static headspace technique was applied to analyse the VOCs. The number of VOCs per sample ranged from 17 to 31. The primarily VOCs identified in raw carrots with the exception of “Yellow Stone” were terpenes, ranging from 65 to 95%. The monoterpenes with values ranging from 31 to 89% were higher than those (from...

  19. Organic analysis of the headspace of Hanford waste Tank 241-C-103

    International Nuclear Information System (INIS)

    Goheen, S.C.; McVeety, B.D.; Clauss, T.W.; Lucke, R.B.; Ligotke, M.W.; Edwards, J.A.; Fruchter, J.S.

    1996-01-01

    Organic species from the headspace of one Hanford radioactive waste tank are described. Samples were collected either using a sorbent trap or a SUMMA TM canister and were analyzed by gas chromatography and mass spectrometry. The headspace contained several organic components, including alkanes, alkanes, ketones, aldehydes, organic nitriles, and chlorinated hydrocarbons. Sorbent trap samples were designed to collect only normal paraffin hydrocarbons (NPHs). A comparison of NPH data from sorbent traps and SUMMA TM cans revealed results of 693 and 1320 mg/m 3 , NPH respectively. Significant differences were observed in NPH values when samples were collected at different times, or at different locations in the tank. These data suggest either the time of collection, or the position of the sampling device are important variables in the analysis of organic species from Hanford tanks. (author). 16 refs., 3 figs., 2 tabs

  20. A simple headspace equilibration method for measuring dissolved methane

    Science.gov (United States)

    Magen, C; Lapham, L.L.; Pohlman, John W.; Marshall, Kristin N.; Bosman, S.; Casso, Michael; Chanton, J.P.

    2014-01-01

    Dissolved methane concentrations in the ocean are close to equilibrium with the atmosphere. Because methane is only sparingly soluble in seawater, measuring it without contamination is challenging for samples collected and processed in the presence of air. Several methods for analyzing dissolved methane are described in the literature, yet none has conducted a thorough assessment of the method yield, contamination issues during collection, transport and storage, and the effect of temperature changes and preservative. Previous extraction methods transfer methane from water to gas by either a "sparge and trap" or a "headspace equilibration" technique. The gas is then analyzed for methane by gas chromatography. Here, we revisit the headspace equilibration technique and describe a simple, inexpensive, and reliable method to measure methane in fresh and seawater, regardless of concentration. Within the range of concentrations typically found in surface seawaters (2-1000 nmol L-1), the yield of the method nears 100% of what is expected from solubility calculation following the addition of known amount of methane. In addition to being sensitive (detection limit of 0.1 ppmv, or 0.74 nmol L-1), this method requires less than 10 min per sample, and does not use highly toxic chemicals. It can be conducted with minimum materials and does not require the use of a gas chromatograph at the collection site. It can therefore be used in various remote working environments and conditions.

  1. Headspace solid-phase microextraction with 1-pyrenyldiazomethane on-fibre derivatisation for analysis of fluoroacetic acid in biological samples.

    Science.gov (United States)

    Sporkert, Frank; Pragst, Fritz; Hübner, Sandra; Mills, Graham

    2002-05-25

    A new and in part automated headspace solid-phase microextraction method for quantitative determination of the highly toxic rodenticide fluoroacetic acid (FAA) in serum and other biological samples has been developed. FAA and deuterated acetic acid (internal standard) were extracted from acidified samples by a StableFlex divinylbenzene-Carboxen on polydimethylsiloxane fibre. The acids were derivatised on the fibre in-situ with 1-pyrenyldiazomethane and detected using gas chromatography-mass spectrometry with electron impact ionisation and selected ion monitoring. The calibration curve for FAA in serum was linear over the range from 0.02 to 5 microg/ml, with limits of detection and quantification of 0.02 and 0.07 microg/ml, respectively. The method was also tested with spiked whole blood, urine, stomach contents and kidney samples. It was sufficiently reliable, reproducible and sensitive for use in routine forensic toxicology applications.

  2. Headspace vapor characterization of Hanford Waste Tank SX-102: Results from samples collected on July 19, 1995. Tank Vapor Characterization Project

    International Nuclear Information System (INIS)

    McVeety, B.D.; Evans, J.C.; Clauss, T.W.; Pool, K.H.

    1996-05-01

    This report describes the results of vapor samples taken from the headspace of waste storage tank 241-SX-102 (Tank SX-102) at the Hanford Site in Washington State. Pacific Northwest National Laboratory (PNNL) contracted with Westinghouse Hanford Company (WHC) to provide sampling devices and analyze samples for inorganic and organic analytes collected from the tank headspace and ambient air near the tank. The analytical work was performed under the PNNL Vapor Analytical Laboratory (VAL) by the Tank Vapor Characterization Project. Work performed was based on a sample and analysis plan (SAP) prepared by WHC. The SAP provided job-specific instructions for samples, analyses, and reporting. The SAP for this sample job was open-quotes Vapor Sampling and Analysis Planclose quotes, and the sample job was designated S5046. Samples were collected by WHC on July 19, 1995, using the vapor sampling system (VSS), a truck-based sampling method using a heated probe inserted into the tank headspace

  3. Headspace vapor characterization of Hanford Waste Tank AX-103: Results from samples collected on June 21, 1995. Tank Vapor Characterization Project

    International Nuclear Information System (INIS)

    Ligotke, M.W.; Pool, K.H.; Clauss, T.W.

    1996-05-01

    This report describes the results of vapor samples taken from the headspace of waste storage tank 241-AX-103 (Tank AX-103) at the Hanford Site in Washington State. Pacific Northwest National Laboratory (PNNL) contracted with Westinghouse Hanford Company (WHC) to provide sampling devices and analyze samples for inorganic and organic analytes collected from the tank headspace and ambient air near the tank. The analytical work was performed by the PNNL Vapor Analytical Laboratory (VAL) by the Tank Vapor Characterization Project. Work performed was based on a sample and analysis plan (SAP) prepared by WHC. The SAP provided job-specific instructions for samples, analyses, and reporting. The SAP for this sample job was open-quotes Vapor Sampling and Analysis Planclose quotes, and the sample job was designated S5029. Samples were collected by WHC on June 21, 1995, using the Vapor Sampling System (VSS), a truck-based sampling method using a heated probe inserted into the tank headspace

  4. Headspace vapor characterization of Hanford Waste Tank AX-101: Results from samples collected on June 15, 1995. Tank Vapor Characterization Project

    International Nuclear Information System (INIS)

    Pool, K.H.; Clauss, T.W.; Evans, J.C.; McVeety, B.D.

    1996-05-01

    This report describes the results of vapor samples taken from the headspace of waste storage tank 241-AX-101 (Tank AX-101) at the Hanford Site in Washington State. Pacific Northwest National Laboratory (PNNL) contracted with Westinghouse Hanford Company (WHC) to provide sampling devices and analyze samples for inorganic and organic analytes collected from the tank headspace and ambient air near the tank. The analytical work was performed by the PNNL Vapor Analytical Laboratory (VAL) under the Tank Vapor Characterization Project. Work performed was based on a sample and analysis plan (SAP) prepared by WHC. The SAP provided job-specific instructions for samples, analyses, and reporting. The SAP for this sample job was open-quotes Vapor Sampling and Analysis Planclose quotes, and the sample job was designated S5028. Samples were collected by WHC on June 15, 1995, using the Vapor Sampling System (VSS), a truck-based sampling method using a heated probe inserted into the tank headspace

  5. Determination of organotin compounds by headspace solid-phase microextraction-gas chromatography-pulsed flame-photometric detection (HS-SPME-GC-PFPD)

    Energy Technology Data Exchange (ETDEWEB)

    Bravo, Manuel [Universite de Pau et des Pays de L' Adour, Laboratoire de Chimie Analytique, LCABIE, UMR CNRS 5034, Pau (France); Pontificia Universidad Catolica de Valparaiso, Laboratorio de Quimica Analitica y Ambiental, Instituto de Quimica, Valparaiso (Chile); Lespes, Gaetane; Gautier, Martine Potin [Pontificia Universidad Catolica de Valparaiso, Laboratorio de Quimica Analitica y Ambiental, Instituto de Quimica, Valparaiso (Chile); Gregori, Ida de; Pinochet, Hugo [Universite de Pau et des Pays de L' Adour, Laboratoire de Chimie Analytique, LCABIE, UMR CNRS 5034, Pau (France)

    2005-12-01

    A method based on Headspace solid-phase microextraction (HS-SPME, with a 100 {mu}m PDMS-fiber) in combination with gas-chromatography and pulsed flame-photometric detection (GC-PFPD) has been investigated for simultaneous determination of eight organotin compounds. Monobutyltin (MBT), dibutyltin (DBT), tributyltin (TBT), monophenyltin (MPhT), and the semi-volatile diphenyltin (DPhT), triphenyltin (TPhT), monooctyltin (MOcT), and dioctyltin (DOcT) were determined after derivatization with sodium tetraethylborate. The conditions used for the extraction and preconcentration step were optimised by experimental design methodology. Tripropyltin (TPrT) and diheptyltin (DHepT) were used as internal standards for quantification of volatile and semi-volatile organotin compounds, respectively. The analytical precision (RSD) for ten successive injections of a standard mixture containing all the organic tin compounds ranged between 2 and 11%. The limits of detection for all the organotin compounds were sub ng (Sn) L{sup -1} in water and close to ng (Sn) kg{sup -1} in sediments. The accuracy of the method was evaluated by analysis of two certified reference material (CRM) sediment samples. The HS-SPME-GC-PFPD was then applied to the analysis of three harbour sediment samples. The results showed that headspace SPME is an attractive tool for analysis of organotin compounds in solid environmental matrices. (orig.)

  6. Quantification of 13 priority polycyclic aromatic hydrocarbons in human urine by headspace solid-phase microextraction gas chromatography-isotope dilution mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Campo, Laura [Department of Occupational and Environmental Health, University of Milan and Fondazione IRCCS Ospedale Maggiore Policlinico, Mangiagalli e Regina Elena, Milan (Italy)], E-mail: laura.campo@unimi.it; Mercadante, Rosa; Rossella, Federica; Fustinoni, Silvia [Department of Occupational and Environmental Health, University of Milan and Fondazione IRCCS Ospedale Maggiore Policlinico, Mangiagalli e Regina Elena, Milan (Italy)

    2009-01-12

    Polycyclic aromatic hydrocarbons (PAHs) are common environmental pollutants in both living and working environments. The aim of this study was the development of a headspace solid-phase microextraction gas chromatography-isotope dilution mass spectrometry (HS-SPME/GC-IDMS) method for the simultaneous quantification of 13 PAHs in urine samples. Different parameters affecting PAHs extraction by HS-SPME were considered and optimized: type/thickness of fiber coatings, extraction temperature/time, desorption temperature/time, ionic strength and sample agitation. The stability of spiked PAHs solutions and of real urine samples stored up to 90 days in containers of different materials was evaluated. In the optimized method, analytes were absorbed for 60 min at 80 deg. C in the sample headspace with a 100 {mu}m polydimethylsiloxane fiber. The method is very specific, with linear range from the limit of quantification to 8.67 x 10{sup 3} ng L{sup -1}, a within-run precision of <20% and a between-run precision of <20% for 2-, 3- and 4-ring compounds and of <30% for 5-ring compounds, trueness within 20% of the spiked concentration, and limit of quantification in the 2.28-2.28 x 10{sup 1} ng L{sup -1} range. An application of the proposed method using 15 urine samples from subjects exposed to PAHs at different environmental levels is shown.

  7. Investigations on the emission of fragrance allergens from scented toys by means of headspace solid-phase microextraction gas chromatography-mass spectrometry.

    Science.gov (United States)

    Masuck, Ines; Hutzler, Christoph; Luch, Andreas

    2010-04-30

    In the revised European toy safety directive 2009/48/EC the application of fragrance allergens in children's toys is restricted. The focus of the present work lies on the instrumental analytics of 13 banned fragrance allergens, as well as on 11 fragrance allergens that require declaration when concentrations surpass 100 microg per gram material. Applying a mixture of ethyl acetate and toluene solid/liquid extraction was performed prior to quantitative analysis of mass contents of fragrances in scented toys. In addition, an easy-to-perform method for the determination of emitted fragrances at 23 degrees C (handling conditions) or at 40 degrees C (worst case scenario) has been worked out to allow for the evaluation of potential risks originating from inhalation of these compounds during handling of or playing with toys. For this purpose a headspace solid-phase microextraction (HS-SPME) technique was developed and coupled to subsequent gas chromatography-mass spectrometry (GC-MS) analysis. Fragrance allergens were adsorbed (extracted) from the gas phase onto an 85 microm polyacrylate fiber while incubating pieces of the scented toys in sealed headspace vials at 23 degrees C and 40 degrees C. Quantification of compounds was performed via external calibration. The newly developed headspace method was subsequently applied to five perfumed toys. As expected, the emission of fragrance allergens from scented toys depends on the temperature and on the content of fragrance allergens present in those samples. In particular at conditions mimicking worst case (40 degrees C), fragrance allergens in toys may pose a risk to children since considerable amounts of compound might be absorbed by lung tissue via breathing of contaminated air. 2010 Elsevier B.V. All rights reserved.

  8. Headspace vapor characterization of Hanford waste tank 241-U-108: Results from samples collected on 8/29/95

    International Nuclear Information System (INIS)

    Thomas, B.L.; Clauss, T.W.; Evans, J.C.; McVeety, B.D.; Pool, K.H.; Olsten, K.B.; Fruchter, J.S.; Ligotke, M.W.

    1996-05-01

    This report describes the analytical results of vapor samples taken from the headspace of the waste storage tank 241-U-108 (Tank U-108) at the Hanford Site in Washington State. The results described in the report were obtained to characterize the vapors present in the tank headspace and to support safety evaluations and tank farm operations. The results include air concentrations of selected inorganic and organic analytes and grouped compounds from samples obtained by Westinghouse Hanford Company (WHC) and provided for analysis to Pacific Northwest National Laboratory (PNNL). Analyte concentrations were based on analytical results and, where appropriate, sample volumes provided by WHC

  9. Liquid paraffin as new dilution medium for the analysis of high boiling point residual solvents with static headspace-gas chromatography.

    Science.gov (United States)

    D'Autry, Ward; Zheng, Chao; Bugalama, John; Wolfs, Kris; Hoogmartens, Jos; Adams, Erwin; Wang, Bochu; Van Schepdael, Ann

    2011-07-15

    Residual solvents are volatile organic compounds which can be present in pharmaceutical substances. A generic static headspace-gas chromatography analysis method for the identification and control of residual solvents is described in the European Pharmacopoeia. Although this method is proved to be suitable for the majority of samples and residual solvents, the method may lack sensitivity for high boiling point residual solvents such as N,N-dimethylformamide, N,N-dimethylacetamide, dimethyl sulfoxide and benzyl alcohol. In this study, liquid paraffin was investigated as new dilution medium for the analysis of these residual solvents. The headspace-gas chromatography method was developed and optimized taking the official Pharmacopoeia method as a starting point. The optimized method was validated according to ICH criteria. It was found that the detection limits were below 1μg/vial for each compound, indicating a drastically increased sensitivity compared to the Pharmacopoeia method, which failed to detect the compounds at their respective limit concentrations. Linearity was evaluated based on the R(2) values, which were above 0.997 for all compounds, and inspection of residual plots. Instrument and method precision were examined by calculating the relative standard deviations (RSD) of repeated analyses within the linearity and accuracy experiments, respectively. It was found that all RSD values were below 10%. Accuracy was checked by a recovery experiment at three different levels. Mean recovery values were all in the range 95-105%. Finally, the optimized method was applied to residual DMSO analysis in four different Kollicoat(®) sample batches. Copyright © 2011 Elsevier B.V. All rights reserved.

  10. Headspace vapor characterization of Hanford Waste Tank 241-T-110: Results from samples collected on August 31, 1995. Tank Vapor Characterization Project

    International Nuclear Information System (INIS)

    McVeety, B.D.; Thomas, B.L.; Evans, J.C.

    1996-05-01

    This report describes the results of vapor samples taken from the headspace of waste storage tank 241-T-110 (Tank T-110) at the Hanford Site in Washington State. Pacific Northwest National Laboratory (PNNL) contracted with Westinghouse Hanford Company (WHC) to provide sampling devices and analyze samples for inorganic and organic analytes collected from the tank headspace and ambient air near the tank. The analytical work was performed by the PNNL Vapor Analytical Laboratory (VAL) by the Tank Vapor Characterization Project. Work performed was based on a sample and analysis plan (SAP) prepared by WHC. The SAP provided job-specific instructions for samples, analyses, and reporting. The SAP for this sample job was open-quotes Vapor Sampling and Analysis Planclose quotes, and the sample job was designated S5056. Samples were collected by WHC on August 31, 1995, using the Vapor Sampling System (VSS), a truck-based sampling method using a heated probe inserted into the tank headspace

  11. Headspace vapor characterization of Hanford Waste Tank 241-TX-111: Results from samples collected on October 12, 1995. Tank Vapor Characterization Project

    International Nuclear Information System (INIS)

    Pool, K.H.; Clauss, T.W.; Evans, J.C.

    1996-06-01

    This report describes the results of vapor samples taken from the headspace of waste storage tank 241-TX-111 (Tank TX-111) at the Hanford Site in Washington State. Pacific Northwest National Laboratory (PNNL) contracted with Westinghouse Hanford Company (WHC) to provide sampling devices and analyze samples for inorganic and organic analytes collected from the tank headspace and ambient air near the tank. The analytical work was performed by the PNNL Vapor Analytical Laboratory (VAL) by the Tank Vapor Characterization Project. Work performed was based on a sample and analysis plan (SAP) prepared by WHC. The SAP provided job-specific instructions for samples, analyses, and reporting. The SAP for this sample job was open-quotes Vapor Sampling and Analysis Planclose quotes, and the sample job was designated S5069. Samples were collected by WHC on October 12, 1995, using the Vapor Sampling System (VSS), a truck-based sampling method using a heated probe inserted into the tank headspace

  12. Headspace vapor characterization of Hanford Waste Tank 241-SX-109: Results from samples collected on August 1, 1995. Tank Vapor Characterization Project

    International Nuclear Information System (INIS)

    Pool, K.H.; Clauss, T.W.; Evans, J.C.

    1996-05-01

    This report describes the results of vapor samples taken from the headspace of waste storage tank 241-SX-109 (Tank SX-109) at the Hanford Site in Washington State. Pacific Northwest National Laboratory (PNNL) contracted with Westinghouse Hanford Company (WHC) to provide sampling devices and analyze samples for inorganic and organic analytes collected from the tank headspace and ambient air near the tank. The analytical work was performed by the PNNL Vapor Analytical Laboratory (VAL) by the Tank Vapor Characterization Project. Work performed was based on a sample and analysis plan (SAP) prepared by WHC. The SAP provided job-specific instructions for samples, analyses, and reporting. The SAP for this sample job was open-quotes Vapor Sampling and Analysis Planclose quotes, and the sample job was designated S5048. Samples were collected by WHC on August 1, 1995, using the Vapor Sampling System (VSS), a truck-based sampling method using a heated probe inserted into the tank headspace

  13. Headspace vapor characterization of Hanford Waste Tank 241-SX-104: Results from samples collected on July 25, 1995. Tank Vapor Characterization Project

    International Nuclear Information System (INIS)

    Thomas, B.L.; Clauss, T.W.; Evans, J.C.

    1996-05-01

    This report describes the results of vapor samples taken from the headspace of waste storage tank 241-SX-104 (Tank SX-104) at the Hanford Site in Washington State. Pacific Northwest National Laboratory (PNNL) contracted with Westinghouse Hanford Company (WHC) to provide sampling devices and analyze samples for inorganic and organic analytes collected from the tank headspace and ambient air near the tank. The analytical work was performed by the PNNL Vapor Analytical Laboratory (VAL) by the Tank Vapor Characterization Project. Work performed was based on a sample and analysis plan (SAP) prepared by WHC. The SAP provided job-specific instructions for samples, analyses, and reporting. The SAP for this sample job was open-quotes Vapor Sampling and Analysis Planclose quotes, and the sample job was designated S5049. Samples were collected by WHC on July 25, 1995, using the Vapor Sampling System (VSS), a truck-based sampling method using a heated probe inserted into the tank headspace

  14. Headspace vapor characterization of Hanford Waste Tank 241-S-112: Results from samples collected on July 11, 1995. Tank Vapor Characterization Project

    International Nuclear Information System (INIS)

    Clauss, T.W.; Pool, K.H.; Evans, J.C.

    1996-05-01

    This report describes the results of vapor samples taken from the headspace of waste storage Tank 241-S-112 (Tank S-112) at the Hanford. Pacific Northwest National Laboratory (PNNL) is contracted with Westinghouse Hanford Company (WHC) to provide sampling devices and analyze samples for inorganic and organic analytes collected from the tank headspace and ambient air near the tank. The analytical work was performed by the PNNL Vapor Analytical Laboratory (VAL) by the Tank Vapor Characterization Project. Work performed was based on a sample and analysis plan (SAP) prepared by WHC. The SAP provided job-specific instructions for samples, analyses, and reporting. The SAP for this sample job was open-quotes Vapor Sampling and Analysis Planclose quotes, and the sample job was designated S5044. Samples were collected by WHC on July 11, 1995, using the Vapor Sampling System (VSS), a truck-based sampling method using a heated probe inserted into the tank headspace

  15. Headspace vapor characterization of Hanford Waste Tank 241-SX-105: Results from samples collected on July 26, 1995. Tank Vapor Characterization Project

    International Nuclear Information System (INIS)

    Pool, K.H.; Clauss, T.W.; Evans, J.C.

    1996-05-01

    This report describes the results of vapor samples taken from the headspace of waste storage tank 241-SX-105 (Tank SX-105) at the Hanford Site in Washington State. Pacific Northwest National Laboratory (PNNL) contracted with Westinghouse Hanford Company (WHC) to provide sampling devices and analyze samples for inorganic and organic analytes collected from the tank headspace and ambient air near the tank. The analytical work was performed by the PNNL Vapor Analytical Laboratory (VAL) by the Tank Vapor Characterization Project. Work performed was based on a sample and analysis plan (SAP) prepared by WHC. The SAP provided job-specific instructions for samples, analyses, and reporting. The SAP for this sample job was open-quotes Vapor Sampling and Analysis Planclose quotes, and the sample job was designated S5047. Samples were collected by WHC on July 26, 1995, using the Vapor Sampling System (VSS), a truck-based sampling method using a heated probe inserted into the tank headspace

  16. Quantitative analysis of perfumes in talcum powder by using headspace sorptive extraction.

    Science.gov (United States)

    Ng, Khim Hui; Heng, Audrey; Osborne, Murray

    2012-03-01

    Quantitative analysis of perfume dosage in talcum powder has been a challenge due to interference of the matrix and has so far not been widely reported. In this study, headspace sorptive extraction (HSSE) was validated as a solventless sample preparation method for the extraction and enrichment of perfume raw materials from talcum powder. Sample enrichment is performed on a thick film of poly(dimethylsiloxane) (PDMS) coated onto a magnetic stir bar incorporated in a glass jacket. Sampling is done by placing the PDMS stir bar in the headspace vial by using a holder. The stir bar is then thermally desorbed online with capillary gas chromatography-mass spectrometry. The HSSE method is based on the same principles as headspace solid-phase microextraction (HS-SPME). Nevertheless, a relatively larger amount of extracting phase is coated on the stir bar as compared to SPME. Sample amount and extraction time were optimized in this study. The method has shown good repeatability (with relative standard deviation no higher than 12.5%) and excellent linearity with correlation coefficients above 0.99 for all analytes. The method was also successfully applied in the quantitative analysis of talcum powder spiked with perfume at different dosages. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Rapid and sensitive analysis of polychlorinated biphenyls and acrylamide in food samples using ionic liquid-based in situ dispersive liquid-liquid microextraction coupled to headspace gas chromatography.

    Science.gov (United States)

    Zhang, Cheng; Cagliero, Cecilia; Pierson, Stephen A; Anderson, Jared L

    2017-01-20

    A simple and rapid ionic liquid (IL)-based in situ dispersive liquid-liquid microextraction (DLLME) method was developed and coupled to headspace gas chromatography (HS-GC) employing electron capture (ECD) and mass spectrometry (MS) detection for the analysis of polychlorinated biphenyls (PCBs) and acrylamide at trace levels from milk and coffee samples. The chemical structures of the halide-based ILs were tailored by introducing various functional groups to the cations to evaluate the effect of different structural features on the extraction efficiency of the target analytes. Extraction parameters including the molar ratio of IL to metathesis reagent and IL mass were optimized. The effects of HS oven temperature and the HS sample vial volume on the analyte response were also evaluated. The optimized in situ DLLME method exhibited good analytical precision, good linearity, and provided detection limits down to the low ppt level for PCBs and the low ppb level for acrylamide in aqueous samples. The matrix-compatibility of the developed method was also established by quantifying acrylamide in brewed coffee samples. This method is much simpler and faster compared to previously reported GC-MS methods using solid-phase microextraction (SPME) for the extraction/preconcentration of PCBs and acrylamide from complex food samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  18. Headspace solid-phase microextraction for the determination of volatile organic sulphur and selenium compounds in beers, wines and spirits using gas chromatography and atomic emission detection.

    Science.gov (United States)

    Campillo, Natalia; Peñalver, Rosa; López-García, Ignacio; Hernández-Córdoba, Manuel

    2009-09-25

    A rapid and solvent-free method for the determination of eight volatile organic sulphur and two selenium compounds in different beverage samples using headspace solid-phase microextraction and gas chromatography with atomic emission detection has been developed. The bonded carboxen/polydimethylsiloxane fiber was the most suitable for preconcentrating the analytes from the headspace of the sample solution. Volumes of 20 mL of undiluted beer were used while, in the case of wines and spirits, sample:water ratios of 5:15 and 2:18, respectively, were used, in order to obtain the maximum sensitivity. Quantitation was carried out by using synthetic matrices of beer and wine, and a spiked sample for spirits, and using ethyl methyl sulphide and isopropyl disulphide as internal standards. Detection limits ranged from 8 ng L(-1) to 40 ng mL(-1), depending on the compound and the beverage sample analyzed, with a fiber time exposure of 20 min at ambient temperature. The optimized method was successfully applied to different samples, some of the studied compounds being detected at concentration levels in the 0.04-152 ng mL(-1) range.

  19. Bromination of Aromatic Compounds by Residual Bromide in Sodium Chloride Matrix Modifier Salt During Heated Headspace GC/MS Analysis

    Science.gov (United States)

    Analytical artifacts attributed to the bromination of toluene, xylenes, and trimethylbenzenes were found during the heated headspace gas chromatography/mass spectrometry (GC/MS) analysis of aqueous samples. The aqueous samples were produced from Fenton-like chemical oxidation rea...

  20. 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

  1. Direct thermal desorption in the analysis of cheese volatiles by gas chromatography and gas chromatography-mass spectrometry: comparison with simultaneous distillation-extraction and dynamic headspace.

    Science.gov (United States)

    Valero, E; Sanz, J; Martínez-Castro, I

    2001-06-01

    Direct thermal desorption (DTD) has been used as a technique for extracting volatile components of cheese as a preliminary step to their gas chromatographic (GC) analysis. In this study, it is applied to different cheese varieties: Camembert, blue, Chaumes, and La Serena. Volatiles are also extracted using other techniques such as simultaneous distillation-extraction and dynamic headspace. Separation and identification of the cheese components are carried out by GC-mass spectrometry. Approximately 100 compounds are detected in the examined cheeses. The described results show that DTD is fast, simple, and easy to automate; requires only a small amount of sample (approximately 50 mg); and affords quantitative information about the main groups of compounds present in cheeses.

  2. Rapid analysis of dissolved methane, ethylene, acetylene and ethane using partition coefficients and headspace-gas chromatography.

    Science.gov (United States)

    Lomond, Jasmine S; Tong, Anthony Z

    2011-01-01

    Analysis of dissolved methane, ethylene, acetylene, and ethane in water is crucial in evaluating anaerobic activity and investigating the sources of hydrocarbon contamination in aquatic environments. A rapid chromatographic method based on phase equilibrium between water and its headspace is developed for these analytes. The new method requires minimal sample preparation and no special apparatus except those associated with gas chromatography. Instead of Henry's Law used in similar previous studies, partition coefficients are used for the first time to calculate concentrations of dissolved hydrocarbon gases, which considerably simplifies the calculation involved. Partition coefficients are determined to be 128, 27.9, 1.28, and 96.3 at 30°C for methane, ethylene, acetylene, and ethane, respectively. It was discovered that the volume ratio of gas-to-liquid phase is critical to the accuracy of the measurements. The method performance can be readily improved by reducing the volume ratio of the two phases. Method validation shows less than 6% variation in accuracy and precision except at low levels of methane where interferences occur in ambient air. Method detection limits are determined to be in the low ng/L range for all analytes. The performance of the method is further tested using environmental samples collected from various sites in Nova Scotia.

  3. Simultaneous Determination of Alkoxyalcohols in Wet Wipes Using Static Headspace Gas Chromatography and Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Lee, So Jin; Pyo, Hee Soo; Chung, Bong Chul; Lee, Jeon Gae [KIST, Seoul (Korea, Republic of); Kim, Hai Dong [Kyung Hee University, Seoul (Korea, Republic of)

    2014-09-15

    Alkoxyalcohols are used as solvents or preservatives in various consumer products such as wet wipes. The metabolites of alkoxyalcohols are known to be chronically toxic and carcinogenic to animals. Thus, an analytical method is needed to monitor alkoxyalcohols in wet wipes. The aim of this study was to develop a simultaneous analytical method for 14 alkoxyalcohols using headspace gas chromatography coupled with mass spectrometry to analyze the wet wipes. This method was developed by comparing with various headspace extraction parameters. The linear calibration curves were obtained for the method (r2 > 0.995). The limit of detection of alkoxyalcohols ranged from 2 to 200 ng mL-1. The precision of the determinative method was less than 18.20% coefficient of variation both intra and inter days. The accuracy of the method ranged from 82.86% to 119.83%. (2-Methoxymethylethoxy)propanol, 2-phenoxyethanol, and 1-phenoxy-2-propanol were mainly detected in wet wipes.

  4. Identification of volatiles by headspace gas chromatography with simultaneous flame ionization and mass spectrometric detection.

    Science.gov (United States)

    Tiscione, Nicholas B; Yeatman, Dustin Tate; Shan, Xiaoqin; Kahl, Joseph H

    2013-10-01

    Volatiles are frequently abused as inhalants. The methods used for identification are generally nonspecific if analyzed concurrently with ethanol or require an additional analytical procedure that employs mass spectrometry. A previously published technique utilizing a capillary flow technology splitter to simultaneously quantitate and confirm ethyl alcohol by flame ionization and mass spectrometric detection after headspace sampling and gas chromatographic separation was evaluated for the detection of inhalants. Methanol, isopropanol, acetone, acetaldehyde, toluene, methyl ethyl ketone, isoamyl alcohol, isobutyl alcohol, n-butyl alcohol, 1,1-difluoroethane, 1,1,1-trifluoroethane, 1,1,1,2-tetrafluoroethane (Norflurane, HFC-134a), chloroethane, trichlorofluoromethane (Freon®-11), dichlorodifluoromethane (Freon®-12), dichlorofluoromethane (Freon®-21), chlorodifluoromethane (Freon®-22) and 1,2-dichlorotetrafluoroethane (Freon®-114) were validated for qualitative identification by this method. The validation for qualitative identification included evaluation of matrix effects, sensitivity, carryover, specificity, repeatability and ruggedness/robustness.

  5. Ethanol analysis by headspace gas chromatography with simultaneous flame-ionization and mass spectrometry detection.

    Science.gov (United States)

    Tiscione, Nicholas B; Alford, Ilene; Yeatman, Dustin Tate; Shan, Xiaoqin

    2011-09-01

    Ethanol is the most frequently identified compound in forensic toxicology. Although confirmation involving mass spectrometry is desirable, relatively few methods have been published to date. A novel technique utilizing a Dean's Switch to simultaneously quantitate and confirm ethyl alcohol by flame-ionization (FID) and mass spectrometric (MS) detection after headspace sampling and gas chromatographic separation is presented. Using 100 μL of sample, the limits of detection and quantitation were 0.005 and 0.010 g/dL, respectively. The zero-order linear range (r(2) > 0.990) was determined to span the concentrations of 0.010 to 1.000 g/dL. The coefficient of variation of replicate analyses was less than 3.1%. Quantitative accuracy was within ±8%, ±6%, ±3%, and ±1.5% at concentrations of 0.010, 0.025, 0.080, and 0.300 g/dL, respectively. In addition, 1,1-difluoroethane was validated for qualitative identification by this method. The validated FID-MS method provides a procedure for the quantitation of ethyl alcohol in blood by FID with simultaneous confirmation by MS and can also be utilized as an identification method for inhalants such as 1,1-difluoroethane.

  6. Effects of headspace fraction and aqueous alkalinity on subcritical hydrothermal gasification of cellulose

    Energy Technology Data Exchange (ETDEWEB)

    Dolan, Ryan; Yin, Sudong; Tan, Zhongchao [Department of Mechanical and Manufacturing Engineering, Centre for Environmental Engineering Research and Education, Schulich School of Engineering, University of Calgary, 2500 University Dr. N.W. Calgary, AB (Canada)

    2010-07-15

    In order to better understand the pathways of hydrothermal gasification of cellulose, the effect of headspace fraction and alkalinity on the hydrothermal gasification of cellulose has been studied at 315 C in the presence of Pt/Al{sub 2}O{sub 3} as catalyst. It was found that regardless of alkalinity the headspace fraction had a large impact on gasification yield, with larger headspace fractions resulting in considerably more gas product. Without the addition of sodium carbonate, the effect of headspace fraction became more pronounced, with gas increasing by approximately a factor of forty from the lowest to highest headspace fraction. On the other hand, for the same residence time the addition of sodium carbonate co-catalyst dampened the magnitude of the effect, to a factor of 2.5 and 1.5, for 50 and 100 mM sodium carbonate solutions, respectively. These results indicated that the headspace fraction affected the phase behaviour, and that this altered the pathway of the cellulose decomposition. While furfural alcohol was the major product obtained with a 49% headspace fraction, it was effectively suppressed by using 78% or greater headspace fractions. Based on the effects of phase behaviour and previous literature, the reduced effect occurring upon the addition of sodium carbonate may relate to catalysis of the Lobry de-bruyn Van Eckenstein transform to produce lactic acid rather than intermediates proceeding through glycolaldehyde. (author)

  7. Headspace solid phase microextraction (HSSPME) for the determination of volatile and semivolatile pollutants in soils

    Energy Technology Data Exchange (ETDEWEB)

    Llompart, Maria [Departamento de Quimica Analitica Nutricion y Bromatologia, Facultad de Quimica, Universidad de Santiago de Compostela, E-15706 Santiago de Compostela (Spain); Li, Ken; Fingas, Merv [Emergencies Science Division, Environment Canada, Environmental Technology Centre, 3439 River Road, Ottawa, ON (Canada)

    1999-02-08

    We have investigated the use of headspace solid phase microextraction (HSSPME) as a sample concentration and preparation technique for the analysis of volatile and semivolatile pollutants in soil samples. Soil samples were suspended in solvent and the SPME fibre suspended in the headspace above the slurry. Finally, the fibre was desorbed in the Gas Chromatograph (GC) injection port and the analysis of the samples was carried out. Since the transfer of contaminants from the soil to the SPME fibre involves four separate phases (soil-solvent-headspace and fibre coating), parameters affecting the distribution of the analytes were investigated. Using a well-aged artificially spiked garden soil, different solvents (both organic and aqueous) were used to enhance the release of the contaminants from the solid matrix to the headspace. It was found that simple addition of water is adequate for the purpose of analysing the target volatile organic chemicals (VOCs) in soil. The addition of 1 ml of water to 1 g of soil yielded maximum response. Without water addition, the target VOCs were almost not released from the matrix and a poor response was observed. The effect of headspace volume on response as well as the addition of salt were also investigated. Comparison studies between conventional static headspace (HS) at high temperature (95C) and the new technology HSSPME at room temperature (=20C) were performed. The results obtained with both techniques were in good agreement. HSSPME precision and linearity were found to be better than automated headspace method and HSSPME also produced a significant enhancement in response. The detection and quantification limits for the target VOCs in soils were in the sub-ng g{sup -1} level. Finally, we tried to extend the applicability of the method to the analysis of semivolatiles. For these studies, two natural soils contaminated with diesel fuel and wood preservative, as well as a standard urban dust contaminated with polyaromatic

  8. Comments on “innovative method for carbon dioxide determination in human postmortem cardiac gas samples using headspace-gas chromatography–mass spectrometry and stable labeled isotope as internal standard” by Varlet et al

    Energy Technology Data Exchange (ETDEWEB)

    Saffaj, T., E-mail: taoufiq.saffaj@usmba.ac.ma [Centre Universitaire Régional d’Interface, Université Sidi Mohamed Ben Abdellah, BP 2626, route d’Imouzzer, Fes Morocco (Morocco); Laboratoire de Chimie Organique Appliquée, Faculté des Sciences et Techniques, BP 2202, route d’Imouzzer, Fes Morocco (Morocco); Ihssane, B. [Laboratoire de Chimie Organique Appliquée, Faculté des Sciences et Techniques, BP 2202, route d’Imouzzer, Fes Morocco (Morocco)

    2014-01-31

    Graphical abstract: -- Highlights: •We comment on the validation results of the method for CO{sub 2} analysis in cardiac samples. •We demonstrate that the total error of the method exceeds the acceptance limits. •We show that the method is not valid according to the new SFSTP guideline. -- Abstract: Varlet et al. recently proposed a headspace-gas chromatography–mass spectrometry (HS-GC–MS) method applicable for the routine determination of CO{sub 2} in gaseous biologic matrices. This developed bioanalytical method was fully validated according to the SFSTP 1997 guidelines using the accuracy profile as a graphical decision-making tool.In this letter, we discuss the validity of HS-GC–MS method based on the newest SFSTP guideline. In particular, we demonstrate by the estimation of the β-expectation tolerance interval that the error total exceeds the acceptance limits (30%) for the second concentration level (0.5 μmol mL{sup −1} vial HS). Furthermore, we show through the risk profile that the probability to have future results inside the ±30% acceptance limits is smaller than 95%.

  9. Simple and sensitive analysis of nereistoxin and its metabolites in human serum using headspace solid-phase microextraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Namera, A; Watanabe, T; Yashiki, M; Kojima, T; Urabe, T

    1999-03-01

    A simple method for the analysis of nereistoxin and its metabolites in human serum using headspace solid-phase microextraction (SPME) and gas chromatography-mass spectrometry (GC-MS) is developed. A vial containing a serum sample, 5M sodium hydroxide, and benzylacetone (internal standard) is heated to 70 degrees C, and an SPME fiber is exposed for 30 min in the headspace of the vial. The compounds extracted by the fiber are desorbed by exposing the fiber in the injection port of the GC-MS. The calibration curves show linearity in the range of 0.05-5.0 micrograms/mL for nereistoxin and N-methyl-N-(2-methylthio-1-methylthiomethyl)ethylamine, 0.01-5.0 micrograms/mL for S,S'-dimethyl dihydronereistoxin, and 0.5-10 micrograms/mL for 2-methylthio-1-methylthiomethylethylamine in serum. No interferences are found, and the analysis time is 50 min for one sample. In addition, this proposed method is applied to a patient who attempted suicide by ingesting Padan 4R, a herbicide. Padan 4R contains 4% cartap hydrochloride, which is an analogue of nereistoxin. Nereistoxin and its metabolites are detected in the serum samples collected from the patient during hospitalization. The concentration ranges of nereistoxin in the serum are 0.09-2.69 micrograms/mL.

  10. Determination of residual acetone and acetone related impurities in drug product intermediates prepared as Spray Dried Dispersions (SDD) using gas chromatography with headspace autosampling (GCHS).

    Science.gov (United States)

    Quirk, Emma; Doggett, Adrian; Bretnall, Alison

    2014-08-05

    Spray Dried Dispersions (SDD) are uniform mixtures of a specific ratio of amorphous active pharmaceutical ingredient (API) and polymer prepared via a spray drying process. Volatile solvents are employed during spray drying to facilitate the formation of the SDD material. Following manufacture, analytical methodology is required to determine residual levels of the spray drying solvent and its associated impurities. Due to the high level of polymer in the SDD samples, direct liquid injection with Gas Chromatography (GC) is not a viable option for analysis. This work describes the development and validation of an analytical approach to determine residual levels of acetone and acetone related impurities, mesityl oxide (MO) and diacetone alcohol (DAA), in drug product intermediates prepared as SDDs using GC with headspace (HS) autosampling. The method development for these analytes presented a number of analytical challenges which had to be overcome before the levels of the volatiles of interest could be accurately quantified. GCHS could be used after two critical factors were implemented; (1) calculation and application of conversion factors to 'correct' for the reactions occurring between acetone, MO and DAA during generation of the headspace volume for analysis, and the addition of an equivalent amount of polymer into all reference solutions used for quantitation to ensure comparability between the headspace volumes generated for both samples and external standards. This work describes the method development and optimisation of the standard preparation, the headspace autosampler operating parameters and the chromatographic conditions, together with a summary of the validation of the methodology. The approach has been demonstrated to be robust and suitable to accurately determine levels of acetone, MO and DAA in SDD materials over the linear concentration range 0.008-0.4μL/mL, with minimum quantitation limits of 20ppm for acetone and MO, and 80ppm for DAA. Copyright

  11. Vanguard/rearguard strategy for the evaluation of the degradation of yoghurt samples based on the direct analysis of the volatiles profile through headspace-gas chromatography-mass spectrometry.

    Science.gov (United States)

    Carrillo-Carrión, C; Cárdenas, S; Valcárcel, M

    2007-02-02

    A vanguard/rearguard analytical strategy for the monitoring of the degradation of yoghurt samples is proposed. The method is based on the headspace-gas chromatography-mass spectrometry (HS-GC-MS) instrumental coupling. In this combination, the chromatographic column is firstly used as an interface between the HS and the MS (vanguard mode) avoiding separation of the volatile components by maintaining the chromatographic oven at high, constant temperature. By changing the thermal conditions of the oven, the aldehydes can be properly separated for individual identification/quantification (rearguard mode). In the vanguard method, the quantification of the volatile aldehydes was calculated through partial least square and given as a total index. The rearguard method permits the detection of the aldehydes at concentrations between 12 and 35 ng/g. Both methods were applied to the study of the environmental factors favouring the presence of the volatile aldehydes (C(5)-C(9)) in the yoghurt samples. Principal component analysis of the total concentration of aldehydes with the time (from 0 to 30 days) demonstrates the capability of the HS-MS coupling for the estimation of the quality losses of the samples. The results were corroborated by the HS-GC-MS which also indicates that pentanal was present in the yoghurt from the beginning of the study and the combination of light/oxygen was the most negative influence for sample conservation.

  12. Tank Vapor Characterization Project: Headspace vapor characterization of Hanford waste tank 241-S-101: Results from samples collected on 06/06/96

    International Nuclear Information System (INIS)

    Thomas, B.L.; Evans, J.C.; Pool, K.H.; Olsen, K.B.; Fruchter, J.S.; Silvers, K.L.

    1997-01-01

    This report describes the analytical results of vapor samples taken from the headspace of the waste storage tank 241-S-101. The results described in this report were obtained to characterize the vapors present in the tank headspace and to support safety evaluations and tank farm operations. The results include air concentrations of selected inorganic and organic analytes and grouped compounds from samples obtained. Analyte concentrations were based on analytical results and sample volumes provided by WHC. A summary of the inorganic analytes, permanent gases, and total non-methane organic compounds is listed

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

    Science.gov (United States)

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

    2017-05-05

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

  14. Tank 241-C-103 headspace flammability

    International Nuclear Information System (INIS)

    Huckaby, J.L.

    1994-01-01

    Information regarding flammable vapors, gases, and aerosols is presented for the purpose of resolving the tank 241-C-103 headspace flammability issue. Analyses of recent vapor and liquid samples, as well as visual inspections of the tank headspace, are discussed in the context of tank dynamics. This document is restricted to issues regarding the flammability of gases, vapors, and an aerosol that may exist in the headspace of tank 241-C-103. While discussing certain information about the organic liquid present in tank 241-C-103, this document addresses neither the potential for, nor consequences of, a pool fire involving this organic liquid; they will be discussed in a separate report

  15. Tank 241-C-103 headspace flammability

    Energy Technology Data Exchange (ETDEWEB)

    Huckaby, J.L.

    1994-01-01

    Information regarding flammable vapors, gases, and aerosols is presented for the purpose of resolving the tank 241-C-103 headspace flammability issue. Analyses of recent vapor and liquid samples, as well as visual inspections of the tank headspace, are discussed in the context of tank dynamics. This document is restricted to issues regarding the flammability of gases, vapors, and an aerosol that may exist in the headspace of tank 241-C-103. While discussing certain information about the organic liquid present in tank 241-C-103, this document addresses neither the potential for, nor consequences of, a pool fire involving this organic liquid; they will be discussed in a separate report.

  16. Headspace vapor characterization of Hanford waste tank 241-B-107: Results from samples collected on 7/23/96

    International Nuclear Information System (INIS)

    Evans, J.C.; Pool, K.H.; Thomas, B.L.; Olsen, K.B.; Fruchter, J.S.; Silvers, K.L.

    1997-01-01

    This report describes the analytical results of vapor samples taken from the headspace of the waste storage tank 241-B-107 (Tank B-107) at the Hanford Site in Washington State. The results described in this report were obtained to characterize the vapors present in the tank headspace and to support safety evaluations and tank farm operations. The results include air concentrations of selected inorganic and organic analytes and grouped compounds from samples obtained by Westinghouse Hanford Company (WHC) and provided for analysis to Pacific Northwestern National Laboratory (PNNL). A summary of the inorganic analytes, permanent gases, and total non-methane organic compounds is listed in a table. The three highest concentration analytes detected in SUMMA trademark canister and triple sorbent trap samples are also listed in the same table. Detailed descriptions of the analytical results appear in the appendices

  17. Headspace vapor characterization of Hanford waste tank 241-S-106: Results from samples collected on 06/13/96

    International Nuclear Information System (INIS)

    Evans, J.C.; Pool, K.H.; Thomas, B.L.; Olsen, K.B.; Fruchter, J.S.; Silvers, K.L.

    1997-01-01

    This report describes the analytical results of vapor samples taken from the headspace of the waste storage tank 241-S-106 (Tank S-106) at the Hanford Site in Washington State. The results described in this report were obtained to characterize the vapors present in the tank headspace and to support safety evaluations and tank farm operations. The results include air concentrations of selected inorganic and organic analytes and grouped compounds from samples obtained by Westinghouse Hanford Company (WHC) and provided for analysis to Pacific Northwest National Laboratory (PNNL). A summary of the inorganic analytes, permanent gases, and total non-methane organic compounds is listed in a table. The three highest concentration analytes detected in SUMMA trademark canister and triple sorbent trap samples are also listed in the same table. Detailed descriptions of the analytical results appear in the appendices

  18. Headspace vapor characterization of Hanford waste Tank 241-BX-110: Results from samples collected on 04/30/96

    International Nuclear Information System (INIS)

    Evans, J.C.; Pool, K.H.; Thomas, B.L.; Olsen, K.B.; Fruchter, J.S.; Silvers, K.L.

    1997-01-01

    This report describes the analytical results of vapor samples taken from the headspace of the waste storage tank 241-BX-110 (Tank BX-110) at the Hanford Site in Washington State. The results described in this report were obtained to characterize the vapors present in the tank headspace and to support safety evaluations and tank farm operations. The results include air concentrations of selected inorganic and organic analytes and grouped compounds from samples obtained by Westinghouse Hanford Company (WHC) and provided for analysis to Pacific Northwest National Laboratory (PNNL). Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. Analyte concentrations were based on analytical results and, where appropriate, sample volumes provided by WHC. A summary of the inorganic analytes, permanent gases, and total non-methane organic compounds is listed in a table. The three highest concentration analytes detected in SUMMA trademark canister and triple sorbent trap samples are also listed in the table. Detailed descriptions of the analytical results appear in the appendices

  19. Screening for γ-Nonalactone in the Headspace of Freshly Cooked Non-Scented Rice Using SPME/GC-O and SPME/GC-MS

    Directory of Open Access Journals (Sweden)

    Jie Yu Chen

    2009-08-01

    Full Text Available The determination of γ-nonalactone as one of the important odor-active compounds in freshly cooked non-scented rice is reported. It was evaluated by gas chromatography-olfactometry (GC-O analysis and identified by gas chromatography-mass spectrometry (GC-MS analysis in the headspace above the freshly cooked non-scented rice samples extracted by using a modified headspace solid-phase microextraction (SPME method. This component had a mass spectrum with a characteristic ion peak at m/z 85 (100% and a linear retention index (RI of 2,023 on a DB Wax column, consistent with those of an authentic sample of γ-nonalactone. The odor characterization of a strong, sweet, coconut-like aroma of this compound was also validated by GC-O comparison with the authentic compound.

  20. Headspace Hanging Drop Liquid Phase Microextraction and Gas Chromatography-Mass Spectrometry for the Analysis of Flavors from Clove Buds

    Energy Technology Data Exchange (ETDEWEB)

    Jung, Mi Jin; Shin, Yeon Jae; Oh, Se Yeon; Kim, Nam Sun; Kim, Kun; Lee, Dong Sun [Seoul Women' s University, Seoul (Korea, Republic of)

    2006-02-15

    A novel sample pretreatment technique, headspace hanging drop liquid phase microextraction (HS-LPME) was studied and applied to the determination of flavors from solid clove buds by gas chromatography-mass spectrometry (GC-MS). Several parameters affecting on HS-LPME such as organic solvent drop volume, extraction time, extraction temperature and phase ratio were investigated. 1-Octanol was selected as the extracting solvent, drop size was fixed to 0.6 μL. 60 min extraction time at 25 .deg. C was chosen. HS-LPME has the good efficiency demonstrated by the higher partition equilibrium constant (K{sub lh}) values and concentration factor (CF) values. The limits of detection (LOD) were 1.5-3.2 ng. The amounts of eugenol, β-caryophyllene and eugenol acetate from the clove bud sample were 1.90 mg/g, 1.47 mg/g and 7.0 mg/g, respectively. This hanging drop based method is a simple, fast and easy sample enrichment technique using minimal solvent. HSLPME is an alternative sample preparation method for the analysis of volatile aroma compounds by GC-MS.

  1. Headspace vapor characterization of Hanford waste Tank 241-C-201: Results from samples collected on 06/19/96

    International Nuclear Information System (INIS)

    Thomas, B.L.; Evans, J.C.; Pool, K.H.; Olsen, K.B.; Fruchter, J.S.; Silvers, K.L.

    1997-01-01

    This report describes the analytical results of vapor samples taken from the headspace of the waste storage tank 241-C-201 (Tank C-201) at the Hanford Site in Washington State. The results described in this report were obtained to characterize the vapors present in the tank headspace and to support safety evaluations and tank farm operations. The results include air concentrations of selected inorganic and organic analytes and grouped compounds from samples obtained by Westinghouse Hanford Company (WHC) and provided for analysis to Pacific Northwest National Laboratory (PNNL). Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. Analyte concentrations were based on analytical results and, where appropriate, on sample volumes provided by WHC. A summary, of the inorganic analytes, permanent gases, and total non-methane organic compounds is listed in a table. Detailed descriptions of the analytical results appear in the appendices

  2. Quantification of liquid products from the electroreduction of CO2 and CO using static headspace-gas chromatography and nuclear magnetic resonance spectroscopy

    DEFF Research Database (Denmark)

    Bertheussen, Erlend; Abghoui, Younes; Jovanov, Zarko P.

    2017-01-01

    Static headspace-gas chromatography (HS-GC) useful for ex-situ liquid product analysis. Could complement high-performance liquid chromatography and NMR spectroscopy. Particularly high sensitivity towards compounds with high vapor pressure. Detection limits below 0.5μM were shown for acetaldehyde...

  3. Simplex Optimization of Headspace-Enrichment Conditions of Residual Petroleum Distillates Used by Arsonists

    Science.gov (United States)

    Warnke, Molly M.; Erickson, Angela E.; Smith, Eugene T.

    2005-01-01

    A forensic project is described that is suitable for an undergraduate instrumental methods lab. Accelerants commonly used by arsonists are analyzed by static headspace enrichment followed by gas chromatography. The conditions used for headspace enrichment (e.g., time and temperature) are known to influence the distribution of hydrocarbons…

  4. Rapid determination of the volatile components in tobacco by ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction with gas chromatography-mass spectrometry.

    Science.gov (United States)

    Yang, Yanqin; Chu, Guohai; Zhou, Guojun; Jiang, Jian; Yuan, Kailong; Pan, Yuanjiang; Song, Zhiyu; Li, Zuguang; Xia, Qian; Lu, Xinbo; Xiao, Weiqiang

    2016-03-01

    An ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction was first employed to determine the volatile components in tobacco samples. The method combined the advantages of ultrasound, microwave, and headspace solid-phase microextraction. The extraction, separation, and enrichment were performed in a single step, which could greatly simplify the operation and reduce the whole pretreatment time. In the developed method, several experimental parameters, such as fiber type, ultrasound power, and irradiation time, were optimized to improve sampling efficiency. Under the optimal conditions, there were 37, 36, 34, and 36 components identified in tobacco from Guizhou, Hunan, Yunnan, and Zimbabwe, respectively, including esters, heterocycles, alkanes, ketones, terpenoids, acids, phenols, and alcohols. The compound types were roughly the same while the contents were varied from different origins due to the disparity of their growing conditions, such as soil, water, and climate. In addition, the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction method was compared with the microwave-assisted extraction coupled to headspace solid-phase microextraction and headspace solid-phase microextraction methods. More types of volatile components were obtained by using the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction method, moreover, the contents were high. The results indicated that the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction technique was a simple, time-saving and highly efficient approach, which was especially suitable for analysis of the volatile components in tobacco. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Determination of N,N-dimethyltryptamine in beverages consumed in religious practices by headspace solid-phase microextraction followed by gas chromatography ion trap mass spectrometry.

    Science.gov (United States)

    Gaujac, Alain; Dempster, Nicola; Navickiene, Sandro; Brandt, Simon D; de Andrade, Jailson Bittencourt

    2013-03-15

    A novel analytical approach combining solid-phase microextraction (SPME)/gas chromatography ion trap mass spectrometry (GC-IT-MS) was developed for the detection and quantification N,N-dimethyltryptamine (DMT), a powerful psychoactive indole alkaloid present in a variety of South American indigenous beverages, such as ayahuasca and vinho da jurema. These particular plant products, often used within a religious context, are increasingly consumed throughout the world following an expansion of religious groups and the availability of plant material over the Internet and high street shops. The method described in the present study included the use of SPME in headspace mode combined GC-IT-MS and included the optimization of the SPME procedure using multivariate techniques. The method was performed with a polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber in headspace mode (70 min at 60 °C) which resulted in good precision (RSDvinho da jurema samples, obtained from Brazilian religious groups, which revealed DMT concentration levels between 0.10 and 1.81 g L(-1). Copyright © 2013 Elsevier B.V. All rights reserved.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2018-01-01

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

  7. The potential of head-space gas chromatography for VLE measurements

    International Nuclear Information System (INIS)

    Luis, Patricia; Wouters, Christine; Sweygers, Nick; Creemers, Claude; Van der Bruggen, Bart

    2012-01-01

    Highlights: ► HS-GC is a potential technique to obtain VLE data in a high throughput scenario. ► We applied HS-GC and evaluate the main issues to consider. ► Four azeotropic mixtures of industrial interest are studied. ► The thermodynamic analysis of VLE shows the strong non-ideality of the mixtures. - Abstract: Head-space gas chromatography (HS-GC) is thought to allow the performance of (vapour + liquid) equilibrium (VLE) measurements in a fast and automated way. However, two decades after the first applications of HS-GC for this purpose, the potential of this technique is not fully developed yet. Measurements of isothermal VLE and activity coefficients of mixtures can be obtained in a high throughput scenario. However, several considerations have to be taken into account before starting the analysis, such as the equilibration time or the minimum sample volume and the GC response factors. These aspects can strongly influence on the validity of the results and should therefore be determined for each mixture. In this paper, four azeotropic mixtures of interest in the pharmaceutical and chemical industry, i.e., (ethylacetate + water), which forms a heterogeneous azeotrope, (ethylacetate + isooctane), (acetonitrile + toluene) and the ternary mixture (acetonitrile + toluene + tetrahydrofuran), are considered to show the potential of HS-GC for VLE measurements. The thermodynamic analysis of VLE data leads to activity coefficients for the mixtures at (35, 50, and 70) °C. In addition, the experimental data are compared with thermodynamic models and data from the literature, when available.

  8. Headspace analysis gas-phase infrared spectroscopy: a study of xanthate decomposition on mineral surfaces

    Science.gov (United States)

    Vreugdenhil, Andrew J.; Brienne, Stephane H. R.; Markwell, Ross D.; Butler, Ian S.; Finch, James A.

    1997-03-01

    The O-ethyldithiocarbonate (ethyl xanthate, CH 3CH 2OCS -2) anion is a widely used reagent in mineral processing for the separation of sulphide minerals by froth flotation. Ethyl xanthate interacts with mineral powders to produce a hydrophobic layer on the mineral surface. A novel infrared technique, headspace analysis gas-phase infrared spectroscopy (HAGIS) has been used to study the in situ thermal decomposition products of ethyl xanthate on mineral surfaces. These products include CS 2, COS, CO 2, CH 4, SO 2, and higher molecular weight alkyl-containing species. Decomposition pathways have been proposed with some information determined from 2H- and 13C-isotope labelling experiments.

  9. Tank 241-C-101 vapor sampling and analysis tank characterization report

    International Nuclear Information System (INIS)

    Huckaby, J.L.

    1995-01-01

    Tank C-101 headspace gas and vapor samples were collected and analyzed to help determine the potential risks of fugitive emissions to tank farm workers. Gas and vapor samples from the Tank C-101 headspace were collected on July 7, 1994 using the in situ sampling (ISS) method, and again on September 1, 1994 using the more robust vapor sampling system (VSS). Gas and vapor concentrations in Tank C-101 are influenced by its connections to other tanks and its ventilation pathways. At issue is whether the organic vapors in Tank C-101 are from the waste in that tank, or from Tanks C-102 or C-103. Tank C-103 is on the Organic Watch List; the other two are not. Air from the Tank C-101 headspace was withdrawn via a 7.9-m long heated sampling probe mounted in riser 8, and transferred via heated tubing to the VSS sampling manifold. The tank headspace temperature was determined to be 34.0 C, and all heated zones of the VSS were maintained at approximately 50 C. Sampling media were prepared and analyzed by WHC, Oak Ridge National Laboratories, Pacific Northwest Laboratories, and Oregon Graduate Institute of Science and Technology through a contract with Sandia National Laboratories. The 39 tank air samples and 2 ambient air control samples collected are listed in Table X-1 by analytical laboratory. Table X-1 also lists the 14 trip blanks and 2 field blanks provided by the laboratories

  10. Magnetic solid phase extraction and static headspace gas chromatography-mass spectrometry method for the analysis of polycyclic aromatic hydrocarbons.

    Science.gov (United States)

    Cai, Ying; Yan, Zhihong; Wang, Lijia; NguyenVan, Manh; Cai, Qingyun

    2016-01-15

    A magnetic solid phase extraction (MSPE) protocol combining a static headspace gas chromatography coupled to mass spectrometry (HS-GC-MS) method has been developed for extraction, and determination of 16 polycyclic aromatic hydrocarbons (PAHs) in drinking water samples. Magnetic nanoparticles (MNPs) were coated with 3-aminopropyltriethoxysilane and modified by cholesterol chloroformate. Transmission electron microscope, vibrating sample magnetometer, Fourier transform infrared spectrometry and X-ray photoelectron spectroscopy were used to characterize the cholesterol-functionalized sorbents, and the main parameters affecting the extraction as well as HS sampling, such as sorbent amount, extraction time, oven temperature and equilibration time have been investigated and established. Combination with HS sampling, the MSPE procedure was simple, fast and environmentally friendly, without need of any organic solvent. Method validation proved the feasibility of the developed sorbents for the quantitation of the investigated analytes at trace levels obtaining the limit of detection (S/N=3) ranging from 0.20 to 7.8 ng/L. Good values for intra and inter-day precision were obtained (RSDs ≤ 9.9%). The proposed method was successfully applied to drinking water samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  11. Headspace vapor characterization of Hanford waste tank 241-U-109: Results from samples collected on 8/10/95

    International Nuclear Information System (INIS)

    Evans, J.C.; Thomas, B.L.; Pool, K.H.; Olsen, K.B.; Fruchter, J.S.; Silvers, K.L.

    1996-05-01

    This report describes the analytical results of vapor samples taken from the headspace of the waste storage tank 241-U-109 (Tank U-109) At the Hanford Site in Washington State. The results described in this report were obtained to characterize the vapors present in the tank headspace and to support safety evaluations and tank farm operations. This tank is on the Hydrogen Waste List. The results include air concentrations of selected inorganic and organic analytes and grouped compounds from samples obtained by Westinghouse Hanford Company (WHC) and provided for analysis to Pacific Northwest National Laboratory (PNNL). Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. Analyte concentrations were based on analytical results and, where appropriate, sample volumes provided by WHC. A summary of the inorganic analytes, permanent gases and total non-methane hydrocarbons is listed in a table. The three highest concentration analytes detected in SUMMA trademark canister and triple sorbent trap samples is also listed in the table. Detailed descriptions of the analytical results appear in the text

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

    International Nuclear Information System (INIS)

    Lockrem, L.L.

    1997-01-01

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

  13. Tank Vapor Characterization Project. Headspace vapor characterization of Hanford Waste Tank AX-102: Results from samples collected on June 27, 1995

    International Nuclear Information System (INIS)

    Clauss, T.W.; Pool, K.H.; Evans, J.C.; McVeety, B.D.; Thomas, B.L.; Olsen, K.B.; Fruchter, J.S.; Ligotke, M.W.

    1995-11-01

    This report describes the analytical results of vapor samples taken from the headspace of the waste storage tank 241-AX-102 (Tank AX-102) at the Hanford Site in Washington State. The results described in this report were obtained to characterize the vapors present in the tank headspace and to support safety evaluations and tank-farm operations. The results include air concentrations of selected inorganic and organic analytes and grouped compounds from samples obtained by Westinghouse Hanford Company (WHC) and provided for analysis to Pacific Northwest Laboratory (PNL). Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNL. Analyte concentrations were based on analytical results and, where appropriate, sample volumes provided by WHC. Detailed descriptions of the analytical results appear in the text

  14. Determination of Lactones in Wines by Headspace Solid-Phase Microextraction and Gas Chromatography Coupled with Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    S. J. Pérez-Olivero

    2014-01-01

    Full Text Available Application of headspace solid-phase microextraction (HS-SPME coupled with high-resolution gas chromatographic (HRGC analysis was studied for determining lactones in wines. Six different SPME fibers were tested, and the influence of different factors such as temperature and time of desorption, ionic strength, time of extraction, content of sugar, ethanol, tannins and anthocyanins, and pH and influence of SO2 were studied. The proposed HS-SPME-GC method is an appropriate technique for the quantitative analysis of γ-butyrolactone, γ-hexalactone, trans-whiskey lactone, γ-octalactone, cis-whiskey lactone, γ-nonalactone, γ-decalactone, δ-decalactone, and γ-undecalactone in wines. Method reproducibility and repeatability ranged between 0.6 and 5.2% for all compounds. Detection limit for γ-butyrolactone was 0.17 mg/L and a few μg/L for the rest of the compounds. The optimized method has been applied to several wine samples.

  15. Determination of 1,3-dichloro-2-propanol and 3-chloro-1,2-propandiol in soy sauce by headspace derivatization solid-phase microextraction combined with gas chromatography-mass spectrometry.

    Science.gov (United States)

    Lee, Maw-Rong; Chiu, Tzu-Chun; Dou, Jianpeng

    2007-05-22

    This study proposes a method for identifying 1,3-dichloro-2-propanol and 3-chloro-1,2-propandiol in aqueous matrices by using headspace on-fiber derivatization following solid-phase microextraction combined with gas chromatography-mass spectrometry. The optimized SPME experimental procedures for extracting 1,3-dichloro-2-propanol and 3-chloro-1,2-propandiol in aqueous solutions involved a 85 microm polyacrylate-coated fiber at pH 6, a sodium chloride concentration of 0.36 g mL(-1), extraction at 50 degrees C for 15 min and desorption of analytes at 260 degrees C for 3 min. Headspace derivatization was conducted in a laboratory-made design with N-methyl-N-(trimethylsilyl)-trifluoroacetamide vapor following solid-phase microextraction by using 3 microL N-methyl-N-(trimethylsilyl)-trifluoroacetamide at an oil bath temperature of 230 degrees C for 40 s. This method had good repeatability (R.S.D.s or = 0.9972) for ultrapure water and soy sauce samples that were spiked with two analytes. Detection limits were obtained at the ng mL(-1). The result demonstrated that headspace on-fiber derivatization following solid-phase microextraction was a simple, fast and accurate technique for identifying trace 1,3-dichloro-2-propanol and 3-chloro-1,2-propandiol in soy sauce.

  16. Heat-flow patterns in Tian-Calvet microcalorimeters: Conductive, convective, and radiative transport in gas dosing experiments

    International Nuclear Information System (INIS)

    Vilchiz, Luis Enrique; Pacheco-Vega, Arturo; Handy, Brent E.

    2005-01-01

    Mathematical models of a Tian-Calvet microcalorimeter were solved numerically by the finite-element method in an effort to understand the relative importance of the three basic heat transfer mechanisms operative during gas dosing experiments typically used to determine heats of adsorption on catalysts and adsorbents. The analysis pays particular attention to the quantitative release of heat through various elements of the cell and sensor cups to assess time delays and the deg.ree of thermal shunting that may result in inaccuracies in calorimetric measurements. Conductive transfer predominates in situations where there is high gas headspace pressure. The convection currents that arise when dosing with considerable gas pressure in the cell headspace region are not sufficiently strong to shunt significant amounts of sample heat away from being sensed by the surrounding thermopiles. Therefore, the heat capture fraction (heat sensed/heat produced) does not vary significantly with gas headspace pressure. During gas dosing under very low gas headspace pressure, radiation losses from the top of the sample bed may significantly affect the heat capture fraction, leading to underestimations of adsorption heats, unless the heat radiated from the top of the catalyst bed is effectively reflected back to the sample region or absorbed by an inert packing layer also in thermal contact with the thermopile wall

  17. Tank 241-U-106 vapor sampling and analysis tank characterization report

    International Nuclear Information System (INIS)

    Huckaby, J.L.

    1995-01-01

    This report presents the details of the Hanford waste tank characterization study for tank 241-U-106. The drivers and objectives of the headspace vapor sampling and analysis were in accordance with procedures that were presented in other reports. The vapor and headspace gas samples were collected to determine the potential risks to tank farm workers due to fugitive emissions from the tank

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

    Science.gov (United States)

    Zhang, Chun-Yun; Chai, Xin-Sheng

    2015-03-13

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

  19. Tank Vapor Characterization Project: Headspace vapor characterization of Hanford Waste Tank U-203, Results from samples collected on August 8, 1995

    International Nuclear Information System (INIS)

    Pool, K.H.; Clauss, T.W.; Evans, J.C.; McVeety, B.D.; Thomas, B.L.; Olsen, K.B.; Fruchter, J.S.; Ligotke, M.W.

    1995-11-01

    This report describes the analytical results of vapor samples taken from the headspace of the waste storage tank 241-U-203 (Tank U-203) at the Hanford Site in Washington State. The results described in this report were obtained to characterize the vapors present in the tank headspace and to support safety evaluations and tank-farm operations. The results include air concentrations of selected inorganic and organic analytes and grouped compounds from samples obtained by Westinghouse Hanford Company (WHC) and provided for analysis to Pacific Northwest Laboratory (PNL). Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNL. Analyte concentrations were based on analytical results and, where appropriate, sample volumes provided by WHC. A summary of the results is listed. Detailed descriptions of the analytical results appear in the text

  20. Tank Vapor Characterization Project: Headspace vapor characterization of Hanford Waste Tank U-204, Results from samples collected on August 8, 1995

    International Nuclear Information System (INIS)

    Clauss, T.W.; Evans, J.C.; McVeety, B.D.; Pool, K.H.; Thomas, B.L.; Olsen, K.B.; Fruchter, J.S.; Ligotke, M.W.

    1995-11-01

    This report describes the analytical results of vapor samples taken from the headspace of the waste storage tank 241-U-204 (Tank U-204) at the Hanford Site in Washington State. The results described in this report were obtained to characterize the vapors present in the tank headspace and to support safety evaluations and tank-farm operations. The results include air concentrations of selected inorganic and organic analytes and grouped compounds from samples obtained by Westinghouse Hanford Company (WHC) and provided for analysis to Pacific Northwest National Laboratory (PNL). Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNL. Analyte concentrations were based on analytical results and, where appropriate, sample volumes provided by WHC. A summary of the results is listed. Detailed descriptions of the analytical results appear in the text

  1. A novel poly(3,4-ethylenedioxythiophene)-ionic liquid composite coating for the headspace solid-phase microextraction and gas chromatography determination of several alcohols in soft drinks.

    Science.gov (United States)

    Wu, Mian; Zhang, Haibo; Zhao, Faqiong; Zeng, Baizhao

    2014-11-19

    A novel poly(3,4-ethylenedioxythiophene)-ionic liquid (i.e., 1-hydroxyethyl-3-methyl imidazolium-bis[(trifluoromethyl)sulfonyl]imide) composite film was electrodeposited on a Pt wire for headspace solid-phase microextraction. The film showed nodular structure and had large specific surface. In addition, it displayed high thermal stability (up to 300°C) and durable property (could be used for more than 200 times). Coupled with gas chromatography-flame ionization detection, the resulting fiber was applied to the headspace solid-phase microextraction and determination of several alcohols (i.e., linalool, nonanol, terpineol, geraniol, decanol and dodecanol). It presented higher extraction capability in comparison with the poly(3,4-ethylenedioxythiophene) and commercial polydimethylsiloxane/divinylbenzene fiber. Under the optimized conditions, the linear ranges exceeded three magnitudes with correlation coefficients above 0.9952 and the low limits of detection were 34.2-81.3ng L(-1). For different alcohols the repeatabilities (defined as RSD) were alcohols in real samples with acceptable recoveries from 81.1% to 106.6%. Copyright © 2014 Elsevier B.V. All rights reserved.

  2. (Vapour + liquid) equilibria of ternary systems with ionic liquids using headspace gas chromatography

    International Nuclear Information System (INIS)

    Mokhtarani, Babak; Gmehling, Juergen

    2010-01-01

    (Vapour + liquid) equilibrium (VLE) data for the ternary systems (hexane + benzene), (hexane + cyclohexane), (benzene + cyclohexane), and (ethanol + water) with an ionic liquid as entrainer for extractive distillation were measured by headspace gas chromatography. As ionic liquids, 1-hexyl-3-methyl-imidazolium bis (trifluoromethyl-sulfonyl) imide [HMIM][BTI], 1-octyl-3-methyl-imidazolium bis (trifluoromethyl-sulfonyl) imide [OMIM][BTI], 1-octyl-3-methyl-imidazolium trifluoro-methanesulfonate [OMIM][OTF], and 1-butyl-3-methyl-imidazolium trifluoro-methanesulfonate [BMIM][OTF] were used. The experimental data show that the ionic liquids investigated have a great influence on the separation factors of the systems (hexane + benzene), (hexane + cyclohexane), and (benzene + cyclohexane). The experimental data were compared with the predicted results using mod. UNIFAC (Do). The predicted results are in good agreement with the experimental data.

  3. (Vapour + liquid) equilibria of ternary systems with ionic liquids using headspace gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Mokhtarani, Babak [Chemistry and Chemical Engineering Research Center of Iran, P.O. Box 14335-186, Tehran (Iran, Islamic Republic of); Gmehling, Juergen, E-mail: gmehling@tech.chem.uni-oldenburg.d [Carl von Ossietzky Universitaet Oldenburg, Technische Chemie, D-26111 Oldenburg (Germany)

    2010-08-15

    (Vapour + liquid) equilibrium (VLE) data for the ternary systems (hexane + benzene), (hexane + cyclohexane), (benzene + cyclohexane), and (ethanol + water) with an ionic liquid as entrainer for extractive distillation were measured by headspace gas chromatography. As ionic liquids, 1-hexyl-3-methyl-imidazolium bis (trifluoromethyl-sulfonyl) imide [HMIM][BTI], 1-octyl-3-methyl-imidazolium bis (trifluoromethyl-sulfonyl) imide [OMIM][BTI], 1-octyl-3-methyl-imidazolium trifluoro-methanesulfonate [OMIM][OTF], and 1-butyl-3-methyl-imidazolium trifluoro-methanesulfonate [BMIM][OTF] were used. The experimental data show that the ionic liquids investigated have a great influence on the separation factors of the systems (hexane + benzene), (hexane + cyclohexane), and (benzene + cyclohexane). The experimental data were compared with the predicted results using mod. UNIFAC (Do). The predicted results are in good agreement with the experimental data.

  4. Tank 241-TY-101 vapor sampling and analysis tank characterization report

    International Nuclear Information System (INIS)

    Huckaby, J.L.

    1995-01-01

    This report presents the details of the Hanford waste tank characterization study for tank 241-TY-101. The drivers and objectives of the headspace vapor sampling and analysis were in accordance with procedure that were presented in other reports. The vapor and headspace gas samples were collected and analyzed to determine the potential risks to tank farm workers due to fugitive emissions from the tank

  5. Tank 241-C-107 vapor sampling and analysis tank characterization report

    International Nuclear Information System (INIS)

    Huckaby, J.L.

    1995-01-01

    This report presents the details of the Hanford waste tank characterization study for tank 241-C-107. The drivers and objectives of the headspace vapor sampling and analysis were in accordance with procedures that were presented in other reports. The vapor and headspace gas samples were collected and analyzed to determine the potential risks to tank farm workers due to fugitive emissions from the tank

  6. Tank 241-C-102 vapor sampling and analysis tank characterization report

    International Nuclear Information System (INIS)

    Huckaby, J.L.

    1995-01-01

    This report presents the details of the Hanford waste tank characterization study for tank 241-C-102. The drivers and objectives of the headspace vapor sampling and analysis were in accordance with procedures that were presented in other reports. The vapor and headspace gas samples were collected and analyzed to determine the potential risks to tank farm workers due to fugitive emissions from the tank

  7. Tank 241-B-103 vapor sampling and analysis tank characterization report

    International Nuclear Information System (INIS)

    Huckaby, J.L.

    1995-01-01

    This report presents the details of the Hanford waste tank characterization study for tank 241-B-103. The drivers and objectives of the headspace vapor sampling and analysis were in accordance with procedure that were presented in other reports. The vapor and headspace gas samples were collected and analyzed to determine the potential risks to tank farm workers due to fugitive emissions from the tank

  8. Tank 241-BX-104 vapor sampling and analysis tank characterization report

    International Nuclear Information System (INIS)

    Huckaby, J.L.

    1995-01-01

    This report presents the details of the Hanford waste tank characterization study for tank 241-BX-104. The drivers and objectives of the headspace vapor sampling and analysis were in accordance with procedure that were presented in other reports. The vapor and headspace gas samples were collected and analyzed to determine the potential risks to tank farm workers due to fugitive emissions from the tank

  9. Tank 241-SX-106 vapor sampling and analysis tank characterization report

    International Nuclear Information System (INIS)

    Huckaby, J.L.

    1995-01-01

    This report presents the details of the Hanford waste tank characterization study for tank 241-SX-106. The drivers and objectives of the headspace vapor sampling and analysis were in accordance with procedure that were presented in other reports. The vapor and headspace gas samples were collected and analyzed to determine the potential risks to tank farm workers due to fugitive emissions from the tank

  10. Tank 241-T-107 vapor sampling and analysis tank characterization report

    International Nuclear Information System (INIS)

    Huckaby, J.L.

    1995-01-01

    This report presents the details of the Hanford waste tank characterization study for tank 241-T-107. The drivers and objectives of the headspace vapor sampling and analysis were in accordance with procedure that were presented in other reports. The vapor and headspace gas samples were collected and analyzed to determine the potential risks to tank farm workers due to fugitive emissions from the tank

  11. Automated determination of aliphatic primary amines in wastewater by simultaneous derivatization and headspace solid-phase microextraction followed by gas chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Llop, Anna; Pocurull, Eva; Borrull, Francesc

    2010-01-22

    This paper presents a fully automated method for determining ten primary amines in wastewater at ng/L levels. The method is based on simultaneous derivatization with pentafluorobenzaldehyde (PFBAY) and headspace solid-phase microextraction (HS-SPME) followed by gas chromatography coupled to ion trap tandem mass spectrometry (GC-IT-MS-MS). The influence of main factors on the efficiency of derivatization and of HS-SPME is described in detail and optimized by a central composite design. For all species, the highest enrichment factors were achieved using a 85 microm polyacrylate (PA) fiber exposed in the headspace of stirred water samples (750 rpm) at pH 12, containing 360 g/L of NaCl, at 40 degrees C for 15 min. Under optimized conditions, the proposed method achieved detection limits ranging from 10 to 100 ng/L (except for cyclohexylamine). The optimized method was then used to determine the presence of primary amines in various types of wastewater samples, such as influent and effluent wastewater from municipal and industrial wastewater treatment plants (WWTPs) and a potable water treatment plant. Although the analysis of these samples revealed the presence of up to 1500 microg/L of certain primary amines in influent industrial wastewater, the concentration of these compounds in the effluent and in municipal and potable water was substantially lower, at low microg/L levels. The new derivatization-HS-SPME-GC-IT-MS-MS method is suitable for the fast, reliable and inexpensive determination of primary amines in wastewater in an automated procedure. Copyright 2009 Elsevier B.V. All rights reserved.

  12. Tank 24-C-103 headspace flammability

    International Nuclear Information System (INIS)

    Huckaby, J.L.

    1994-05-01

    Information regarding flammable vapors, gases, and aerosols is presented and interpreted to help resolve the tank 241-C-103 headspace flammability issue. Analyses of recent vapor and liquid samples, as well as visual inspections of the tank headspace, are discussed in the context of tank dynamics. Concern that the headspace of tank 241-C-103 may contain a flammable mixture of organic vapors and an aerosol of combustible organic liquid droplets arises from the presence of a layer of organic liquid in the tank. This organic liquid is believed to have originated in the plutonium-uranium extraction (PUREX) process, having been stored initially in tank 241-C-102 and apparently transferred to tank 241-C-103 in 1975 (Carothers 1988). Analyses of samples of the organic liquid collected in 1991 and 1993 indicate that the primary constituents are tributyl phosphate (TBP) and several semivolatile hydrocarbons (Prentice 1991, Pool and Bean 1994). This is consistent with the premise that the organic waste came from the PUREX process, because the PUREX process used a solution of TBP in a diluent composed of the n-C 11 H 24 to n-C 15 H 32 normal paraffinic hydrocarbons (NPH)

  13. Characterization of the Key Aroma Compounds in Proso Millet Wine Using Headspace Solid-Phase Microextraction and Gas Chromatography-Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Jingke Liu

    2018-02-01

    Full Text Available The volatile compounds in proso millet wine were extracted by headspace solid-phase microextraction (85 μm polyacrylate (PA, 100 μm polydimethylsiloxane (PDMS, 75 μm Carboxen (CAR/PDMS, and 50/30 μm divinylbenzene (DVB/CAR/PDMS fibers, and analyzed using gas chromatography-mass spectrometry; the odor characteristics and intensities were analyzed by the odor activity value (OAV. Different sample preparation factors were used to optimize this method: sample amount, extraction time, extraction temperature, and content of NaCl. A total of 64 volatile compounds were identified from the wine sample, including 14 esters, seven alcohols, five aldehydes, five ketones, 12 benzene derivatives, 12 hydrocarbons, two terpenes, three phenols, two acids, and two heterocycles. Ethyl benzeneacetate, phenylethyl alcohol, and benzaldehyde were the main volatile compounds found in the samples. According to their OAVs, 14 volatile compounds were determined to be odor-active compounds (OAV > 1, and benzaldehyde, benzeneacetaldehyde, 1-methyl-naphthalene, 2-methyl-naphthalene, and biphenyl were the prominent odor-active compounds (OAV > 50, having a high OAV. Principal component analysis (PCA showed the difference of distribution of the 64 volatile compounds and 14 odor-active compounds with four solid-phase microextraction (SPME fibers.

  14. Determinação de metil-etil-cetona em amostras de urina com amostragem por micro extração em fase sólida (MEFS em headspace associada à cromatografia gasosa com detector de ionização de chama (CG-DIC Determination of methyl ethyl ketone in urine samples by headspace solid phase micro extraction (SPME sampling associated to gas chromatography with flame-ionization detectoR (GC-FID

    Directory of Open Access Journals (Sweden)

    Marina Venzon Antunes

    2008-01-01

    Full Text Available Methyl ethyl ketone (MEK is a solvent commonly used in chemical, paint and shoe industry. The aim of this study was to develop and validate a method for urinary quantification of MEK, employing headspace solid phase micro extraction sampling (SPME coupled to gas chromatography with flame ionization detection (GC-FID. The calibration curve (y=4.6851x-0.0011 presented good linearity with r²=0.9993. Accuracy (94-109%, intra-assay precision (4.07-5.91% and inter-assay precision (3.03-5.62% were acceptable. The quantification limit was 0.19 mg/L. This low cost method can be used routinely in the biological monitoring of occupational exposure to MEK, according to the requirements of the Brazilian legislation.

  15. Tank Vapor Characterization Project: Headspace vapor characterization of Hanford Tank 241-TY-102: Results from samples collected on 04/12/96

    International Nuclear Information System (INIS)

    Evans, J.C.; Pool, K.H.; Thomas, B.L.

    1997-01-01

    This report describes the analytical results of vapor samples taken from the headspace of the waste storage tank 241-TY-102 (Tank TY-102) at the Hanford Site in Washington State. The results described in this report were obtained to'characterize the vapors present in the tank headspace and to support safety evaluations and tank farm operations. The results include air concentrations of selected inorganic and organic analytes, and grouped compounds from samples obtained by Westinghouse Hanford Company (WHC) and provided for analysis to Pacific Northwest National Laboratory (PNNL). Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. Analyte concentrations were based on analytical results and, where appropriate, sample volumes provided by WHC. A summary of the inorganic analytes, permanent gases, and total non-methane organic compounds is listed in Table S.1. The three highest concentration analytes detected in SUMMA trademark canister and triple sorbent trap samples are also listed in Table S.1. Detailed descriptions of the analytical results appear in the appendices

  16. Tank Vapor Characterization Project: Headspace vapor characterization of Hanford Tank 241-B-105: Results from samples collected on 07/30/96

    International Nuclear Information System (INIS)

    Pool, K.H.; Evans, J.C.; Thomas, B.L.

    1997-01-01

    This report describes the analytical results of vapor samples taken from the headspace of the waste storage tank 241-B-105 (Tank B-105) at the Hanford Site in Washington State. The results described in this report were obtained to characterize the vapors present in the tank headspace and to support safety evaluations and tank farm operations. The results include air concentrations of selected inorganic and organic analytes and grouped compounds from samples obtained by Westinghouse Hanford Company (WHC) and provided for analysis to Pacific Northwest National Laboratory (PNNL). Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. Analyte concentrations were based on analytical results and, where appropriate, sample volumes provided by WHC. A summary of the inorganic analytes, permanent gases, and total non-methane organic compounds is listed in Table S.1. The three highest concentration analytes detected in SUMMA trademark canister and triple sorbent trap samples are also listed in Table S.1. Detailed descriptions of the analytical results appear in the appendices

  17. Tank Vapor Characterization Project: Headspace vapor characterization of Hanford Tank 241-S-107: Results from samples collected on 06/18/96

    International Nuclear Information System (INIS)

    Pool, K.H.; Evans, J.C.; Thomas, B.L.

    1997-01-01

    This report describes the analytical results of vapor samples taken from the headspace of the waste storage tank 241-S-107 (Tank S-107) at the Hanford Site in Washington State. The results described in this report were obtained to characterize the vapors present in the tank headspace and to support safety evaluations and tank farm operations. The results include air concentrations of selected inorganic and organic analytes and grouped compounds from samples obtained by Westinghouse Hanford Company (WHC) and provided for analysis to Pacific Northwest National. Laboratory (PNNL). Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. Analyte concentrations were based on analytical results and, where appropriate, on sample volumes provided by WHC. A summary of the inorganic analytes, permanent gases, and total non-methane organic compounds is listed in Table S.1. Detailed descriptions of the analytical results appear in the appendices

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

    Science.gov (United States)

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

    2017-08-05

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

  19. Uncertainty of Blood Alcohol Concentration (BAC Results as Related to Instrumental Conditions: Optimization and Robustness of BAC Analysis Headspace Parameters

    Directory of Open Access Journals (Sweden)

    Haleigh A. Boswell

    2015-12-01

    Full Text Available Analysis of blood alcohol concentration is a routine analysis performed in many forensic laboratories. This analysis commonly utilizes static headspace sampling, followed by gas chromatography combined with flame ionization detection (GC-FID. Studies have shown several “optimal” methods for instrumental operating conditions, which are intended to yield accurate and precise data. Given that different instruments, sampling methods, application specific columns and parameters are often utilized, it is much less common to find information on the robustness of these reported conditions. A major problem can arise when these “optimal” conditions may not also be robust, thus producing data with higher than desired uncertainty or potentially inaccurate results. The goal of this research was to incorporate the principles of quality by design (QBD in the adjustment and determination of BAC (blood alcohol concentration instrumental headspace parameters, thereby ensuring that minor instrumental variations, which occur as a matter of normal work, do not appreciably affect the final results of this analysis. This study discusses both the QBD principles as well as the results of the experiments, which allow for determination of more favorable instrumental headspace conditions. Additionally, method detection limits will also be reported in order to determine a reporting threshold and the degree of uncertainty at the common threshold value of 0.08 g/dL. Furthermore, the comparison of two internal standards, n-propanol and t-butanol, will be investigated. The study showed that an altered parameter of 85 °C headspace oven temperature and 15 psi headspace vial pressurization produces the lowest percent relative standard deviation of 1.3% when t-butanol is implemented as an internal standard, at least for one very common platform. The study also showed that an altered parameter of 100 °C headspace oven temperature and 15-psi headspace vial pressurization

  20. Tank 241-C-111 vapor sampling and analysis tank characterization report. Revision 1

    International Nuclear Information System (INIS)

    Huckaby, J.L.

    1995-01-01

    This report presents the details of the Hanford waste tank characterization study for tank 241-C-111. The drivers and objectives of the headspace vapor sampling and analysis were in accordance with procedures that were presented in other reports. The vapor and headspace gas samples were collected and analyzed to determine the potential risks to tank farm workers due to fugitive emissions from the tank

  1. Tank 241-BY-110 vapor sampling and analysis tank characterization report. Revision 1

    International Nuclear Information System (INIS)

    Huckaby, J.L.

    1995-01-01

    This report presents the details of the Hanford waste tank characterization study for tank 241-BY-110. The drivers and objectives of the headspace vapor sampling and analysis were in accordance with procedures that were presented in other reports. The vapor and headspace gas samples were collected and analyzed to determine the potential risks to the tank farm workers due to fugitive emissions from the tank

  2. Tank 241-TX-105 vapor sampling and analysis tank characterization report

    International Nuclear Information System (INIS)

    Huckaby, J.L.

    1995-01-01

    Tank 241-TX-105 headspace gas and vapor samples were collected and analyzed to help determine the potential risks to tank farm workers due to fugitive emissions from the tank. The drivers and objectives of waste tank headspace sampling and analysis are discussed in open-quotes Program Plan for the Resolution of Tank Vapor Issues.close quotes Tank 241-TX-105 was vapor sampled in accordance with open-quotes Data Quality Objectives for Generic In-Tank Health and Safety Issue Resolution.close quotes

  3. Tank 241-BY-107 vapor sampling and analysis tank characterization report

    International Nuclear Information System (INIS)

    Huckaby, J.L.

    1995-01-01

    Tank 241-BY-107 headspace gas and vapor samples were collected and analyzed to help determine the potential risks to tank farm workers due to fugitive emissions from the tank. The drivers and objectives of waste tank headspace sampling and analysis are discussed in open-quotes Program Plan for the Resolution of Tank Vapor Issuesclose quotes. Tank 241-BY-107 was vapor sampled in accordance with open-quotes Data Quality Objectives for Generic In-Tank Health and Safety Issue Resolutionclose quotes

  4. Tank 241-BY-111 vapor sampling and analysis tank characterization report

    International Nuclear Information System (INIS)

    Huckaby, J.L.

    1995-01-01

    Tank 241-BY-111 headspace gas and vapor samples were collected and analyzed to help determine the potential risks to tank farm workers due to fugitive emissions from the tank. The drivers and objectives of waste tank headspace sampling and analysis are discussed in open-quotes Program Plan for the Resolution of Tank Vapor Issues.close quotes Tank 241-BY-111 was vapor sampled in accordance with open-quotes Data Quality Objectives for Generic In-Tank Health and Safety Issue Resolution.close quotes

  5. Tank 241-C-108 vapor sampling and analysis tank characterization report

    International Nuclear Information System (INIS)

    Huckaby, J.L.

    1995-01-01

    Tank 241-C-108 headspace gas and vapor samples were collected and analyzed to help determine the potential risks to tank farm workers due to fugitive emissions from the tank. The drivers and objectives of waste tank headspace sampling and analysis are discussed in Program Plan for the Resolution of Tank Vapor Issues (Osborne and Huckaby 1994). Tank 241-C-108 was vapor sampled in accordance with Data Quality Objectives for Generic In-Tank Health and Safety Issue Resolution (Osborne et al., 1994)

  6. Tank 241-TX-118 vapor sampling and analysis tank characterization report

    International Nuclear Information System (INIS)

    Huckaby, J.L.

    1995-01-01

    Tank 241-TX-118 headspace gas and vapor samples were collected and analyzed to help determine the potential risks to tank farm workers due to fugitive emissions from the tank. The drivers and objectives of waste tank headspace sampling and analysis are discussed in open-quotes Program Plan for the Resolution of Tank Vapor Issues.close quotes Tank 241-TX-118 was vapor sampled in accordance with open-quotes Data Quality Objectives for Generic In-Tank Health and Safety Issue Resolution.close quotes

  7. Tank 241-BY-112 vapor sampling and analysis tank characterization report

    International Nuclear Information System (INIS)

    Huckaby, J.L.

    1995-01-01

    Tank 241-BY-112 headspace gas and vapor samples were collected and analyzed to help determine the potential risks to tank farm workers due to fugitive emissions from the tank. The drivers and objectives of waste tank headspace sampling and analysis are discussed in open-quotes Program Plan for the Resolution of Tank Vapor Issues.close quotes Tank 241-BY-112 was vapor sampled in accordance with open-quotes Data Quality Objectives for Generic In-Tank Health and Safety Issue Resolution.close quotes

  8. Tank 241-C-104 vapor sampling and analysis tank characterization report

    International Nuclear Information System (INIS)

    Huckaby, J.L.

    1995-01-01

    Tank 241-C-104 headspace gas and vapor samples were collected and analyzed to help determine the potential risks to tank farm workers due to fugitive emissions from the tank. The drivers and objectives of waste tank headspace sampling and analysis are discussed in open-quotes Program Plan for the Resolution of Tank Vapor Issues.close quotes Tank 241-C-104 was vapor sampled in accordance with open-quotes Data Quality Objectives for Generic In-Tank Health and Safety Issue Resolution.close quotes

  9. Tank 241-BY-103 vapor sampling and analysis tank characterization report

    International Nuclear Information System (INIS)

    Huckaby, J.L.

    1995-01-01

    Tank 241-BY-103 headspace gas and vapor samples were collected and analyzed to help determine the potential risks to tank farm workers due to fugitive emissions from the tank. The drivers and objectives of waste tank headspace sampling and analysis are discussed in open-quotes Program Plan for the Resolution of Tank Vapor Issues.close quotes Tank 241-BY-103 was vapor sampled in accordance with open-quotes Data Quality Objectives for Generic In-Tank Health and Safety Issue Resolution.close quotes

  10. Tank 241-U-107 vapor sampling and analysis tank characterization report

    Energy Technology Data Exchange (ETDEWEB)

    Huckaby, J.L.

    1995-05-31

    Tank 241-U-107 headspace gas and vapor samples were collected and analyzed to help determine the potential risks to tank farm workers due to fugitive emissions from the tank. The drivers and objectives of waste tank headspace sampling and analysis are discussed in {open_quotes}Program Plan for the Resolution of Tank Vapor Issues.{close_quotes} Tank 241-U-107 was vapor sampled in accordance with {open_quotes}Data Quality Objectives for Generic In-Tank Health and Safety Issue Resolution.{close_quotes}

  11. Headspace mass spectrometry methodology: application to oil spill identification in soils

    Energy Technology Data Exchange (ETDEWEB)

    Perez Pavon, J.L.; Garcia Pinto, C.; Moreno Cordero, B. [Universidad de Salamanca, Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias Quimicas, Salamanca (Spain); Guerrero Pena, A. [Universidad de Salamanca, Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias Quimicas, Salamanca (Spain); Laboratorio de Suelos, Plantas y Aguas, Campus Tabasco, Colegio de Postgraduados, Cardenas, Tabasco (Mexico)

    2008-05-15

    In the present work we report the results obtained with a methodology based on direct coupling of a headspace generator to a mass spectrometer for the identification of different types of petroleum crudes in polluted soils. With no prior treatment, the samples are subjected to the headspace generation process and the volatiles generated are introduced directly into the mass spectrometer, thereby obtaining a fingerprint of volatiles in the sample analysed. The mass spectrum corresponding to the mass/charge ratios (m/z) contains the information related to the composition of the headspace and is used as the analytical signal for the characterization of the samples. The signals obtained for the different samples were treated by chemometric techniques to obtain the desired information. The main advantage of the proposed methodology is that no prior chromatographic separation and no sample manipulation are required. The method is rapid, simple and, in view of the results, highly promising for the implementation of a new approach for oil spill identification in soils. (orig.)

  12. A comparative study of three tissue-cultured Dendrobium species and their wild correspondences by headspace gas chromatography-mass spectrometry combined with chemometric methods.

    Science.gov (United States)

    Chen, Nai-Dong; You, Tao; Li, Jun; Bai, Li-Tao; Hao, Jing-Wen; Xu, Xiao-Yuan

    2016-10-01

    Plant tissue culture technique is widely used in the conservation and utilization of rare and endangered medicinal plants and it is crucial for tissue culture stocks to obtain the ability to produce similar bioactive components as their wild correspondences. In this paper, a headspace gas chromatography-mass spectrometry method combined with chemometric methods was applied to analyze and evaluate the volatile compounds in tissue-cultured and wild Dendrobium huoshanense Cheng and Tang, Dendrobium officinale Kimura et Migo and Dendrobium moniliforme (Linn.) Sw. In total, 63 volatile compounds were separated, with 53 being identified from the three Dendrobium spp. Different provenances of Dendrobiums had characteristic chemicals and showed remarkable quantity discrepancy of common compositions. The similarity evaluation disclosed that the accumulation of volatile compounds in Dendrobium samples might be affected by their provenance. Principal component analysis showed that the first three components explained 85.9% of data variance, demonstrating a good discrimination between samples. Gas chromatography-mass spectrometry techniques, combined with chemometrics, might be an effective strategy for identifying the species and their provenance, especially in the assessment of tissue-cultured Dendrobium quality for use in raw herbal medicines. Copyright © 2016. Published by Elsevier B.V.

  13. Determination of styrene migration from food-contact polymers into margarine, using azeotropic distillation and headspace gas chromatography.

    Science.gov (United States)

    Varner, S L; Breder, C V; Fazio, T

    1983-09-01

    Migration studies were conducted to determine the quantity of styrene that migrates from polymers into fatty foods, specifically margarine. Azeotropic distillation was used to isolate styrene from the margarine. Headspace gas chromatography with a Chromosorb 104 column and a flame ionization detector was used for quantitation. The quantitation limit for the method was about 25 ppb (wt/wt) styrene in margarine. On the average, greater than 90% of the styrene was recovered. Several commercial margarines were examined. The method and results of the migration studies are presented. There was no detectable migration of styrene into margarine.

  14. Speciation analysis of organotin compounds in human urine by headspace solid-phase micro-extraction and gas chromatography with pulsed flame photometric detection.

    Science.gov (United States)

    Valenzuela, Aníbal; Lespes, Gaëtane; Quiroz, Waldo; Aguilar, Luis F; Bravo, Manuel A

    2014-07-01

    A new headspace solid-phase micro-extraction (HS-SPME) method followed by gas chromatography with pulsed flame photometric detection (GC-PFPD) analysis has been developed for the simultaneous determination of 11 organotin compounds, including methyl-, butyl-, phenyl- and octyltin derivates, in human urine. The methodology has been validated by the analysis of urine samples fortified with all analytes at different concentration levels, and recovery rates above 87% and relative precisions between 2% and 7% were obtained. Additionally, an experimental-design approach has been used to model the storage stability of organotin compounds in human urine, demonstrating that organotins are highly degraded in this medium, although their stability is satisfactory during the first 4 days of storage at 4 °C and pH=4. Finally, this methodology was applied to urine samples collected from harbor workers exposed to antifouling paints; methyl- and butyltins were detected, confirming human exposure in this type of work environment. Copyright © 2014 Elsevier B.V. All rights reserved.

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

  16. Speciation of mercury compounds by gas chromatography with atomic emission detection. Simultaneous optimization of a headspace solid-phase microextraction and derivatization procedure by use of chemometric techniques

    Energy Technology Data Exchange (ETDEWEB)

    Carro, A.M.; Neira, I.; Rodil, R.; Lorenzo, R. A. [Univ. Santiago de Compostela (Spain). Dpto. Quimica Analitica, Nutricion y Bromatologia

    2003-06-01

    A method is proposed for the extraction and determination of organomercury compounds and Hg(II) in seawater samples by headspace solid-phase microextraction (HS-SPME) combined with capillary gas chromatography-microwave-induced plasma atomic emission spectrometry. The mercury species were derivatized with sodium tetraphenylborate, sorbed on a polydimethylsiloxane-coated fused-silica fibre, and desorbed in the injection port of the GC, in splitless mode. Experimental design methodology was used to evaluate the effect of six HS-SPME-derivatization variables: sample volume, NaBPh{sub 4} volume, pH, sorption time, extraction-derivatization temperature, and rate of stirring. Use of a multicriterion decision-making approach, with the desirability function, enabled determination of the optimum working conditions of the procedure for simultaneous analysis of three mercury species. (orig.)

  17. Comparação entre injeção na coluna ("on-column" e headspace dinâmico na determinação de benzeno, tolueno e xilenos (BTX em amostras de água

    Directory of Open Access Journals (Sweden)

    Gobato Elaine A. A. F.

    2001-01-01

    Full Text Available The analysis of water samples containing volatile organic compounds has become an important task in analytical chemistry. Gas chromatography has been widely used for the analysis of volatile organic compounds in water. The headspace analysis shows as a principal characteristic the possibility of determination of the volatile components in drinking water. Benzene, Toluene and Xylene (BTX are important compounds usually present in drinking water, from contamination by petroleum derivatives. Since they are toxic compounds even when present in low concentration levels, their determination is important in order to define the quality of the water. The sampling technique using headspace, coupled with gas chromatography as the separation method, showed to be suitable for BTX analysis in several samples at the mug/L (ppb level.

  18. Headspace solid-phase microextraction coupled to gas chromatography for the analysis of aldehydes in edible oils.

    Science.gov (United States)

    Ma, Chunhua; Ji, Jiaojiao; Tan, Connieal; Chen, Dongmei; Luo, Feng; Wang, Yiru; Chen, Xi

    2014-03-01

    Oxidation has important effects on the quality of edible oils. In particular, the generation of aldehydes produced by the oxidation of oils is one of the deteriorative factors to their quality. The aim of this study was to develop a method to determine the aldehydes as lipid oxidation markers in edible oils. Seven aldehydes generated from lipid oxidation were studied using headspace solid-phase microextraction coupled to gas chromatography with a flame ionization detector. The extraction efficiency of five commercial fibers was investigated and the influence of extraction temperature, extraction time, desorption temperature, and desorption time were optimized. The best result was obtained with 85 μm carboxen/polydimethylsiloxane, extraction at 50 °C for 15 min and desorption in the gas chromatography injector at 250 °C for 2 min. Under the optimized conditions, the content of hexanal was the highest of the seven aldehydes in all edible oils. The limits of detection for hexanal in the three oils were found to range from 4.6 to 10.2 ng L(-1). The reproducibility of the method was evaluated and the relative standard deviations were less than 8.9%. This developed approach was successfully applied to analyze hexanal in peanut oil, soy oil, and olive oil samples, and these results were compared with those obtained using the thiobarbituric acid-reactive substances (TBARs) method. © 2013 The Authors. Published by Elsevier B.V. All rights reserved.

  19. Tank Vapor Characterization Project: Headspace vapor characterization of Hanford Waste Tank 241-C-204: Results from samples collected on 07/02/96

    International Nuclear Information System (INIS)

    Thomas, B.L.; Evans, J.C.; Pool, K.H.

    1997-01-01

    This report describes the analytical results of vapor samples taken from the headspace of the waste storage tank 241-C-204 (Tank C-204) at the Hanford Site in Washington State. The results described in this report were obtained to characterize the vapors present in the tank headspace and to support safety evaluations and tank farm operations. The results include air concentrations of selected inorganic and organic analytes and grouped compounds from samples obtained by Westinghouse Hanford Company (WHC) and provided for analysis to Pacific Northwest National Laboratory (PNNL). Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. Analyte concentrations were based on analytical results and, where appropriate, sample volumes provided by WHC. A summary of the inorganic analytes, permanent gases, and total non-methane organic compounds is listed in Table S.1. The three highest concentration analytes detected in SUMMA trademark canister and triple sorbent trap samples are also listed in Table S.1. Detailed descriptions of the analytical results appear in the appendices

  20. Tank Vapor Characterization Project: Headspace vapor characterization of Hanford Waste Tank 241-S-103: Results from samples collected on 06/12/96

    International Nuclear Information System (INIS)

    Evans, J.C.; Pool, K.H.; Thomas, B.L.

    1997-01-01

    This report describes the analytical results of vapor samples taken from the headspace of the waste storage tank 241-S-103 (Tank S-103) at the Hanford Site in Washington State. The results described in this report were obtained to characterize the vapors present in the tank headspace and to support safety evaluations and tank farm operations. The results include air concentrations of selected inorganic and organic analytes and grouped compounds from samples obtained by Westinghouse Hanford Company (WHC) and provided for analysis to Pacific Northwest National Laboratory (PNNL). Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. Analyte concentrations were based on analytical results and, where appropriate, sample volumes provided by WHC. A summary of the inorganic analytes, permanent gases, and total non-methane organic compounds is listed in Table S.1. The three highest concentration analytes detected in SUMMA trademark canister and triple sorbent trap samples are also listed in Table S.1. Detailed descriptions of the analytical results appear in the appendices

  1. Dynamic headspace-gas-chromatography-olfactometry analysis of different anatomical parts of lovage (Levisticum officinale Koch.) at eight growing stages

    NARCIS (Netherlands)

    Bylaite, E.; Roozen, J.P.; Legger, A.; Venskutonis, R.P.; Posthumus, M.A.

    2000-01-01

    Volatiles of five different parts of lovage (leaves, stems, flowers, seeds, and roots) were isolated by dynamic headspace (DHS) method and analyzed by GC-FID and GC-olfactometry (GC-O) techniques. In total, 98 compounds were identified in the samples, of which 41 are reported as lovage volatiles for

  2. Developed a needle trap device with PDMS sorbent for microextraction of toluene and methyl ethyl ketone from aquatic samples using dynamic headspace

    Directory of Open Access Journals (Sweden)

    Sara Karimi Zeverdegani

    2016-09-01

    Full Text Available Introduction: Due to the widespread use of toxic chemicals in most workplaces that can lead to toxic effects on human, various chemical extraction technique have been defined for analysis these toxic substances in air, water and biological samples. The purpose of this research is extraction of  toluene and methyl ethyl ketone from aquatic samples with needle trap device and  one commercial sorbent. Methods: In this research, needle trap device was used to extraction of  toluene and methyl ethyl ketone in aquatic samples, so needles(size 20 were packed with PDMS and extraction was done with dynamic headspace needle trap device. Gas chromatography with - flame ionization detector was used to analysis and optimized extraction of two substances were obtained. Results: Results show that the optimum temperature and time extraction was similar for toluene and methyl ethyl ketone (30 ° C, 30 min, but the reproducibility of results and calibration curve that obtained for toluene was better than methyl ethyl ketone. Conclusion: Needle trap technique is inexpensive, sensitive and portable also this method has good recovery to extract small amounts of  toluene and methyl ethyketon from aquatic samples with polydimethylsiloxane.

  3. Determination of perfluorobutane in rat blood by automatic headspace capillary gas chromatography and selected ion monitoring mass spectrometry.

    Science.gov (United States)

    Hvattum, E; Normann, P T; Oulie, I; Uran, S; Ringstad, O; Skotland, T

    2001-01-01

    A new contrast agent (Sonazoid; NC100100) for ultrasound imaging has been developed. It is an aqueous suspension of lipid stabilised perfluorobutane (PFB) gas microbubbles. An automatic headspace capillary gas-chromatographic mass spectrometric method using electron impact ionisation was developed for analysis of Sonazoid PFB in rat blood. The calibration standards were gaseous PFB dissolved in ethanol in the range of 0.5-5000 ng PFB. Fluorotrichloromethane (CFC 11) was used as an internal standard of the method and the MS detector was set to single ion monitoring of the base fragment ions of PFB (m/z 69 and 119) and CFC 11 (m/z 101). The calibration graph, made by plotting the peak area ratios of PFB (m/z 69) to CFC 11(m/z 101) against the amount of PFB, was fitted to a second-order polynomial equation with weighting 1/y2 and found to be reproducible. The limit of quantification of the method was set to 0.4 ng PFB. The between-day variation of the method was below 9.2% relative standard deviation (RSD) and the within-day variation of the method was below 7.6% RSD. The accuracy of the method, as compared to Coulter counter, was estimated by determination of PFB in samples where Sonazoid was added to saline and found to range from 91.5% to 105.2%. PFB, added as Sonazoid, was found to be stable for at least 7 months in rat blood samples when stored at -20 degrees C.

  4. Grains colonised by moulds: fungal identification and headspace analysis of produced volatile metabolites

    Directory of Open Access Journals (Sweden)

    Maria Paola Tampieri

    2010-01-01

    Full Text Available The aim of this work was to verify if the headspace analysis of fungal volatile compounds produced by some species of Fusarium can be used as a marker of mould presence on maize. Eight samples of maize (four yellow maize from North Italy and four white maize from Hungary, naturally contaminated by Fusarium and positive for the presence of fumonisins, were analyzed to detect moisture content, Aw, volatile metabolites and an enumeration of viable moulds was performed by means of a colony count technique. Headspace samples were analysed using a gas-chromatograph equipped with a capillary column TR-WAX to detect volatile metabolites of moulds. Furthermore macro and microscopic examination of the colonies was performed in order to distinguish, according to their morphology, the genera of the prevalent present moulds. Prevalent mould of eight samples was Fusarium, but other fungi, like Aspergillus, Penicillum and Mucoraceae, were observed. The metabolites produced by F.graminearum and F. moniliforme were Isobutyl-acetate, 3-Methyl-1-butanol and, only at 8 days, 3-Octanone. The incubation time can affect off flavour production in consequence of the presence of other moulds. Further studies on maize samples under different conditions are needed in order to establish the presence of moulds using the count technique and through the identification of volatile compounds.

  5. Tank 241-C-108 vapor sampling and analysis tank characterization report. Revision 1

    International Nuclear Information System (INIS)

    Huckaby, J.L.

    1995-01-01

    Tank 241-C-108 headspace gas and vapor samples were collected and analyzed to help determine the potential risks to tank farm workers due to fugitive emissions from the tank. The drivers and objectives of waste tank headspace sampling and analysis are discussed in open-quotes Program Plan for the Resolution of Tank Vapor Issues.close quotes Tank 241-C-108 was vapor sampled in accordance with open-quotes Data Quality Objectives for Generic In-Tank Health and Safety Issue Resolution.close quotes

  6. Tank 241-BY-107 vapor sampling and analysis tank characterization report. Revision 1

    International Nuclear Information System (INIS)

    Huckaby, J.L.

    1995-01-01

    Tank 241-BY-107 headspace gas and vapor samples were collected and analyzed to help determine the potential risks to tank farm workers due to fugitive emissions from the tank. The drivers and objectives of waste tank headspace sampling and analysis are discussed in open-quotes Program Plan for the Resolution of Tank Vapor Issues.close quotes Tank 241-BY-107 was vapor sampled in accordance with open-quotes Data Quality Objectives for Generic In-Tank Health and Safety Issue Resolution.close quotes

  7. Tank 241-BY-108 vapor sampling and analysis tank characterization report. Revision 1

    International Nuclear Information System (INIS)

    Huckaby, J.L.

    1995-01-01

    Tank 241-BY-108 headspace gas and vapor samples were collected and analyzed to help determine the potential risks to tank farm workers due to fugitive emissions from the tank. The drivers and objectives of waste tank headspace sampling and analysis are discussed in ''Program Plan for the Resolution of Tank Vapor Issues'' (Osborne and Huckaby 1994). Tank 241-BY-108 was vapor sampled in accordance with ''Data Quality Objectives for Generic In-Tank Health and Safety Issue Resolution (Osborne et al., 1994)

  8. Tank 241-BY-106 vapor sampling and analysis tank characterization report. Revision 1

    International Nuclear Information System (INIS)

    Huckaby, J.L.

    1995-01-01

    Tank 241-BY-106 headspace gas and vapor samples were collected and analyzed to help determine the potential risks to tank farm workers due to fugitive emissions from the tank. The drivers and objectives of waste tank headspace sampling and analysis are discussed in open-quotes Program Plan for the Resolution of Tank Vapor Issues.close quotes Tank 241-BY-106 was vapor sampled in accordance with open-quotes Data Quality Objectives for Generic In-Tank Health and Safety Issue Resolution.close quotes

  9. Tank vapor characterization project - headspace vapor characterization of Hanford Waste Tank 241-C-107: Second comparison study results from samples collected on 3/26/96

    International Nuclear Information System (INIS)

    Evans, J.C.; Pool, K.H.; Thomas, B.L.

    1997-01-01

    This report describes the analytical results of vapor samples taken from the headspace of waste storage tank 241-C-107 (Tank C-107) at the Hanford Site in Washington State. The results described in this report is the second in a series comparing vapor sampling of the tank headspace using the Vapor Sampling System (VSS) and In Situ Vapor Sampling (ISVS) system without high efficiency particulate air (HEPA) prefiltration. The results include air concentrations of water (H 2 O) and ammonia (NH 3 ), permanent gases, total non-methane organic compounds (TO-12), and individual organic analytes collected in SUMMA trademark canisters and on triple sorbent traps (TSTs). Samples were collected by Westinghouse Hanford Company (WHC) and analyzed by Pacific Northwest National Laboratory (PNNL). Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. Analyte concentrations were based on analytical results and, where appropriate, sample volume measurements provided by WHC

  10. Tank vapor characterization project. Headspace vapor characterization of Hanford waste tank 241-BY-108: Second comparison study results from samples collected on 3/28/96

    International Nuclear Information System (INIS)

    Thomas, B.L.; Pool, K.H.; Evans, J.C.

    1997-01-01

    This report describes the analytical results of vapor samples taken from the headspace of waste storage tank 241-BY-108 (Tank BY-108) at the Hanford Site in Washington State. The results described in this report is the second in a series comparing vapor sampling of the tank headspace using the Vapor Sampling System (VSS) and In Situ Vapor Sampling (ISVS) system without high efficiency particulate air (HEPA) prefiltration. The results include air concentrations of water (H 2 O) and ammonia (NH 3 ), permanent gases, total non-methane organic compounds (TO-12), and individual organic analytes collected in SUMMA trademark canisters and on triple sorbent traps (TSTs). Samples were collected by Westinghouse Hanford Company (WHC) and analyzed by Pacific Northwest National Laboratory (PNNL). Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. Analyte concentrations were based on analytical results and, where appropriate, sample volume measurements provided by WHC

  11. Multiple headspace-solid-phase microextraction: An application to quantification of mushroom volatiles

    Energy Technology Data Exchange (ETDEWEB)

    Costa, Rosaria; Tedone, Laura; De Grazia, Selenia [Dipartimento Farmaco-chimico, University of Messina, viale Annunziata, 98168 Messina (Italy); Dugo, Paola [Dipartimento Farmaco-chimico, University of Messina, viale Annunziata, 98168 Messina (Italy); Centro Integrato di Ricerca (C.I.R.), Università Campus-Biomedico, Via Álvaro del Portillo, 21, 00128 Roma (Italy); Mondello, Luigi, E-mail: lmondello@unime.it [Dipartimento Farmaco-chimico, University of Messina, viale Annunziata, 98168 Messina (Italy); Centro Integrato di Ricerca (C.I.R.), Università Campus-Biomedico, Via Álvaro del Portillo, 21, 00128 Roma (Italy)

    2013-04-03

    Highlights: ► Multiple headspace extraction-solid phase microextraction (MHS-SPME) has been applied to the analysis of Agaricus bisporus. ► Mushroom flavor is characterized by the presence of compounds with a 8-carbon atoms skeleton. ► Formation of 8-carbon compounds involves a unique fungal biochemical pathway. ► The MHS-SPME allowed to determine quantitatively 5 target analytes of A. bisporus for the first time. -- Abstract: Multiple headspace-solid phase microextraction (MHS-SPME) followed by gas chromatography/mass spectrometry (GC–MS) and flame ionization detection (GC–FID) was applied to the identification and quantification of volatiles released by the mushroom Agaricus bisporus, also known as champignon. MHS-SPME allows to perform quantitative analysis of volatiles from solid matrices, free of matrix interferences. Samples analyzed were fresh mushrooms (chopped and homogenized) and mushroom-containing food dressings. 1-Octen-3-ol, 3-octanol, 3-octanone, 1-octen-3-one and benzaldehyde were common constituents of the samples analyzed. Method performance has been tested through the evaluation of limit of detection (LoD, range 0.033–0.078 ng), limit of quantification (LoQ, range 0.111–0.259 ng) and analyte recovery (92.3–108.5%). The results obtained showed quantitative differences among the samples, which can be attributed to critical factors, such as the degree of cell damage upon sample preparation, that are here discussed. Considerations on the mushrooms biochemistry and on the basic principles of MHS analysis are also presented.

  12. Multiple headspace-solid-phase microextraction: An application to quantification of mushroom volatiles

    International Nuclear Information System (INIS)

    Costa, Rosaria; Tedone, Laura; De Grazia, Selenia; Dugo, Paola; Mondello, Luigi

    2013-01-01

    Highlights: ► Multiple headspace extraction-solid phase microextraction (MHS-SPME) has been applied to the analysis of Agaricus bisporus. ► Mushroom flavor is characterized by the presence of compounds with a 8-carbon atoms skeleton. ► Formation of 8-carbon compounds involves a unique fungal biochemical pathway. ► The MHS-SPME allowed to determine quantitatively 5 target analytes of A. bisporus for the first time. -- Abstract: Multiple headspace-solid phase microextraction (MHS-SPME) followed by gas chromatography/mass spectrometry (GC–MS) and flame ionization detection (GC–FID) was applied to the identification and quantification of volatiles released by the mushroom Agaricus bisporus, also known as champignon. MHS-SPME allows to perform quantitative analysis of volatiles from solid matrices, free of matrix interferences. Samples analyzed were fresh mushrooms (chopped and homogenized) and mushroom-containing food dressings. 1-Octen-3-ol, 3-octanol, 3-octanone, 1-octen-3-one and benzaldehyde were common constituents of the samples analyzed. Method performance has been tested through the evaluation of limit of detection (LoD, range 0.033–0.078 ng), limit of quantification (LoQ, range 0.111–0.259 ng) and analyte recovery (92.3–108.5%). The results obtained showed quantitative differences among the samples, which can be attributed to critical factors, such as the degree of cell damage upon sample preparation, that are here discussed. Considerations on the mushrooms biochemistry and on the basic principles of MHS analysis are also presented

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

    Science.gov (United States)

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

    2017-08-01

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

  14. Headspace volume and percentage of carbon monoxide affects carboxymyoglobin layer development of modified atmosphere packaged beef steaks.

    Science.gov (United States)

    Raines, Christopher R; Hunt, Melvin C

    2010-01-01

    Carboxymyoglobin (COMb) development of beef Longissimus lumborum as related to molecular CO availability and package headspace volume was evaluated. Steaks from six pairs of USDA Select strip loins were packaged in modified atmosphere packages with 0.2%, 0.4%, or 0.8% CO and 30% CO(2) and balanced with N(2) to obtain meat-to-gas ratios of 0.4, 0.7, and 1.1, and CO molar concentrations of 0.07, 0.10, and 0.20 mMol. Steak redness (CIE a*), COMb layer thickness, percentage of CO in the headspace, visual display color, and bloom intensity scores were evaluated 4 and 7 d after packaging. Greater concentration of CO in a smaller headspace resulted in a thicker COMb layer compared with lesser concentration of CO in a larger headspace, regardless of moles CO available. The combined effects of concentration of CO and headspace volume had a greater impact on COMb development than millimoles of CO in the package headspace. Package headspace can be reduced and the concentration of CO can be increased without detriment to fresh beef color or consumer safety.

  15. Time since discharge of 9mm cartridges by headspace analysis, part 1: Comprehensive optimisation and validation of a headspace sorptive extraction (HSSE) method.

    Science.gov (United States)

    Gallidabino, M; Romolo, F S; Weyermann, C

    2017-03-01

    Estimating the time since discharge of spent cartridges can be a valuable tool in the forensic investigation of firearm-related crimes. To reach this aim, it was previously proposed that the decrease of volatile organic compounds released during discharge is monitored over time using non-destructive headspace extraction techniques. While promising results were obtained for large-calibre cartridges (e.g., shotgun shells), handgun calibres yielded unsatisfying results. In addition to the natural complexity of the specimen itself, these can also be attributed to some selective choices in the methods development. Thus, the present series of paper aimed to more systematically evaluate the potential of headspace analysis to estimate the time since discharge of cartridges through the use of more comprehensive analytical and interpretative techniques. Specifically, in this first part, a method based on headspace sorptive extraction (HSSE) was comprehensively optimised and validated, as the latter recently proved to be a more efficient alternative than previous approaches. For this purpose, 29 volatile organic compounds were preliminary selected on the basis of previous works. A multivariate statistical approach based on design of experiments (DOE) was used to optimise variables potentially involved in interaction effects. Introduction of deuterated analogues in sampling vials was also investigated as strategy to account for analytical variations. Analysis was carried out by selected ion mode, gas chromatography coupled to mass spectrometry (GC-MS). Results showed good chromatographic resolution as well as detection limits and peak area repeatability. Application to 9mm spent cartridges confirmed that the use of co-extracted internal standards allowed for improved reproducibility of the measured signals. The validated method will be applied in the second part of this work to estimate the time since discharge of 9mm spent cartridges using multivariate models. Copyright

  16. Determination of antioxidants in new and used lubricant oils by headspace-programmed temperature vaporization-gas chromatography-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Nogal Sanchez, Miguel del; Perez Pavon, Jose Luis; Garcia Pinto, Carmelo; Moreno Cordero, Bernardo [Universidad de Salamanca, Departamento de Quimica Analitica, Nutricion y Bromatologia, Salamanca (Spain); Glanzer, Paul [University of Vienna, Department of Analytical Chemistry, Vienna (Austria)

    2010-12-15

    A sensitive method is presented to determine antioxidants (2-, 3-, and 4-tert-butylphenol, 2,6-di-tert-butylphenol, 3-tert-butyl-4-hydroxyanisol, 2,6-di-tert-butyl-4-methylphenol, 1-naphthol, and diphenylamine) in new and used lubricant oil samples. Research was carried out on a GC device equipped with a headspace sampler, a programmed temperature vaporizer, and an MS detector unit. The proposed method does not require sample treatment prior to analyses, hence eliminating possible errors occurring in this step. Sample preparation is reduced when placing the oil sample (2.0 g) in the vial and adding propyl acetate (20 {mu}L). Solvent vent injection mode permits a pre-concentration of the compounds of interest in the liner filled with Tenax-TA {sup registered}, while venting other species present in the headspace. Thereby, both the life of the liner and the capillary column is prolonged, and unnecessary contamination of the detector unit is avoided. Calibration was performed by adding different concentrations of analytes to a new oil which did not contain any of the studied compounds. Limits of detection as low as 0.57 {mu}g/L (2-tert-butylphenol) with a precision lower or equal to 5.3% were achieved. Prediction of the antioxidants in new oil samples of different viscosities (5W40, 10W40, and 15W40) was accomplished with the previous calibration, and the results were highly satisfactory. To determine antioxidants in used engine oils, standard addition method was used due to the matrix effect. (orig.)

  17. Tank 241-BY-108 vapor sampling and analysis tank characterization report

    International Nuclear Information System (INIS)

    Huckaby, J.L.

    1995-01-01

    Tank BY-108 headspace gas and vapor samples were collected and analyzed to help determine the potential risks to tank farm workers due to fugitive emissions from the tank. Tank BY-108 is on the Ferrocyanide Watch List. Samples were collected from Tank BY-108 using the vapor sampling system (VSS) on october 27, 1994 by WHC Sampling and Mobile Laboratories. The tank headspace temperature was determined to be 25.7 C. Air from the Tank BY-108 headspace was withdrawn via a 7.9 m-long heated sampling probe mounted in riser 1, and transferred via heated tubing to the VSS sampling manifold. All heated zones of the VSS were maintained at approximately 50 C. Sampling media were prepared and analyzed by WHC, Oak Ridge National Laboratories, and Pacific Northwest Laboratories. The 40 tank air samples and 2 ambient air control samples collected are listed in Table X-1 by analytical laboratory. Table X-1 also lists the 14 trip blanks and 2 field blanks that accompanied the samples

  18. Tank 241-BY-110 vapor sampling and analysis tank characterization report

    International Nuclear Information System (INIS)

    Huckaby, J.L.

    1995-01-01

    Tank BY-110 headspace gas and vapor samples were collected and analyzed to help determine the potential risks to tank farm workers due to fugitive emissions from the tank. Tank BY-110 is on the Ferrocyanide Watch List. Samples were collected from Tank BY-110 using the vapor sampling system (VSS) on November 11, 1994 by WHC Sampling and Mobile Laboratories. The tank headspace temperature was determined to be 27 C. Air from the Tank BY-110 headspace was withdrawn via a 7.9 m-long heated sampling probe mounted in riser 12B, and transferred via heated tubing to the VSS sampling manifold. All heated zones of the VSS were maintained at approximately 50 C. Sampling media were prepared and analyzed by WHC, Oak Ridge National Laboratories, and Pacific Northwest Laboratories. The 40 tank air samples and 2 ambient air control samples collected are listed in Table X-1 by analytical laboratory. Table X-1 also lists the 14 trip blanks and 2 field blanks that accompanied the samples

  19. Tank 241-BY-105 vapor sampling and analysis tank characterization report

    International Nuclear Information System (INIS)

    Huckaby, J.L.

    1995-01-01

    Tank BY-105 headspace gas and vapor samples were collected and analyzed to help determine the potential risks to tank farm workers due to fugitive emissions from the tank. Tank BY-105 is on the Ferrocyanide Watch List. Samples were collected from Tank BY-105 using the vapor sampling system (VSS) on July 7, 1994 by WHC Sampling and Mobile Laboratories. The tank headspace temperature was determined to be 26 C. Air from the Tank BY-105 headspace was withdrawn via a heated sampling probe mounted in riser 10A, and transferred via heated tubing to the VSS sampling manifold. All heated zones of the VSS were maintained at approximately 65 C. Sampling media were prepared and analyzed by WHC, Oak Ridge National Laboratories, Pacific Northwest Laboratories, and Oregon Graduate Institute of Science and Technology through a contract with Sandia National Laboratories. The 46 tank air samples and 2 ambient air control samples collected are listed in Table X-1 by analytical laboratory. Table X-1 also lists the 10 trip blanks provided by the laboratories

  20. Factors controlling headspace pressure in a manual manometric BMP method can be used to produce a methane output comparable to AMPTS.

    Science.gov (United States)

    Himanshu, H; Voelklein, M A; Murphy, J D; Grant, J; O'Kiely, P

    2017-08-01

    The manual manometric biochemical methane potential (mBMP) test uses the increase in pressure to calculate the gas produced. This gas production may be affected by the headspace volume in the incubation bottle and by the overhead pressure measurement and release (OHPMR) frequency. The biogas and methane yields of cellulose, barley, silage and slurry were compared with three incubation bottle headspace volumes (50, 90 and 180ml; constant 70ml total medium) and four OHPMR frequencies (daily, each third day, weekly and solely at the end of experiment). The methane yields of barley, silage and slurry were compared with those from an automated volumetric method (AMPTS). Headspace volume and OHPMR frequency effects on biogas yield were mediated mainly through headspace pressure, with the latter having a negative effect on the biogas yield measured and relatively little effect on methane yield. Two mBMP treatments produced methane yields equivalent to AMPTS. Copyright © 2017 Elsevier Ltd. All rights reserved.

  1. Selective determination of semi-volatile thiophene compounds in water by molecularly imprinted polymer thin films with direct headspace gas chromatography sulfur chemiluminescence detection.

    Science.gov (United States)

    Hijazi, Hassan Y; Bottaro, Christina S

    2018-02-26

    Water-compatible molecularly imprinted polymer (MIP) thin films are coupled with headspace gas chromatography sulfur chemiluminescence detection (HS-GC-SCD) to create a new approach for the determination of trace concentrations of thiophene compounds in water samples. Thiophene compounds are persistent, typically petrogenic, organic pollutants of concern due to their potential for biomagnification and bioaccumulation, mutagenicity, and carcinogenicity in terrestrial and aquatic fauna. Identification and quantitation in water, particularly following oil spills, is a priority. Following adsorption of the thiophenes to the MIPs, the MIP-bound analytes are analyzed directly by HS-GC-SCD, with minimal sample manipulation and virtually no organic solvent. Calibration curves of spiked seawater were linear from 5 μg L -1 to 100 μg L -1 and limits of detection (LOD) were in the range of 0.24-0.82 μg L -1 . Low matrix effects were observed in the analysis of thiophene compounds in seawater making the method suitable for use in fresh and saline waters without modification. Acceptable reproducibility was obtained for analysis of thiophene compounds from spiked seawater samples at RSDs ≤7.0% (n = 3).

  2. Determination of Muscone in Rats Plasma following Oral Administration of Artificial Musk: Using of Combined Headspace Gas Chromatography-Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Qibiao Wu

    2014-01-01

    Full Text Available To develop an analytical method for determination of plasma concentrations of muscone in rats following oral administration of artificial musk, with the aim of investigating the pharmacokinetic profile of artificial musk. Plasma samples were pretreated with acetonitrile to precipitate proteins. Headspace injection coupled with gas chromatography-mass spectrometry was used for quantitative analysis of muscone concentrations. A strong linear relationship was obtained for plasma muscone concentrations ranging from 75.6 to 7560 ng·mL−1  R2=0.9998, with the minimum detectable concentration being 25 ng·mL−1. The within-day and interday precision for determination of three different concentrations of muscone were favorable (RSD < 25%. The average absolute recovery ranged from 83.7 to 88.6%, with an average relative recovery of 100.5 to 109.8%. The method described was characterized by stability and reliability, and in the present study showed significant specificity and high sensitivity. This method would be applicable to the analysis of plasma concentrations of muscone in preclinical contexts, where artificial musk is used.

  3. Microbes a Tool for the Remediation of Organotin Pollution Determined by Static Headspace Gas Chromatography-Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Christopher Finnegan

    2018-03-01

    Full Text Available Tributyltin (TBT is one of the most toxic anthropogenic compounds introduced into the marine environment. Despite its global ban in 2008, TBT is still a problem of great concern due to its high affinity for particulate matter, providing a direct and potentially persistent route of entry into benthic sediments. Bioremediation strategies may constitute an alternative approach to conventional physicochemical methods, benefiting from the microorganism’s potential to metabolize anthropogenic compounds. In this work, a simple, precise and accurate static headspace gas chromatography method was developed to investigate the ability of TBT degrading microbes in sedimentary microcosms over a period of 120 days. The proposed method was validated for linearity, repeatability, accuracy, specificity, limit of detection and limit of quantification. The method was subsequently successfully applied for the detection and quantification of TBT and degradation compounds in sediment samples on day 0, 30, 60, 90 and 120 of the experiment employing the principles of green chemistry. On day 120 the concentration of TBT remaining in the microcosms ranged between 91.91 ng/g wet wt for the least effective microbial inoculant to 52.73 ng/g wet wt for the most effective microbial inoculant from a starting concentration of 100 ng/g wet wt.

  4. Determination of chlorophenols in landfill leachate using headspace sampling with ionic liquid-coated solid-phase microextraction fibers combined with gas chromatography–mass spectrometry

    International Nuclear Information System (INIS)

    Ho, Tse-Tsung; Chen, Chung-Yu; Li Zuguang; Yang, Thomas Ching-Cherng; Lee, Maw-Rong

    2012-01-01

    Highlights: ► Ionic liquid (IL), ([C 4 MIM][PF 6 ]), was rapid synthesized by microwave radiation. ► Trace chlorophenols in landfill leachate were extract by SPME coated IL. ► The IL-coated SPME-GC/MS method is low-cost, solvent-free and sensitive. - Abstract: A new microextraction technique based on ionic liquid solid-phase microextraction (IL-SPME) was developed for determination of trace chlorophenols (CPs) in landfill leachate. The synthesized ionic liquid, 1-butyl-3-methylimidazolium hexafluorophosphate ([C 4 MIM][PF 6 ]), was coated onto the spent fiber of SPME for extraction of trace CPs. After extraction, the absorbed analytes were desorbed and quantified using gas chromatography–mass spectrometry (GC/MS). The term of the proposed method is as ionic liquid-coated of solid-phase microextraction combined with gas chromatography–mass spectrometry (IL-SPME-GC/MS). No carryover effect was found, and every laboratory-made ionic liquids-coated-fiber could be used for extraction at least eighty times without degradation of efficiency. The chlorophenols studied were 2,4-dichlorophenol (2,4-DP), 2,4,6-trichlorophenol (2,4,6-TCP), 2,3,4,6-tetrachlorophenol (2,3,4,6-TeCP), and pentachlorophenol (PCP). The best results of chlorophenols analysis were obtained with landfill leachate at pH 2, headspace extraction for 4 min, and thermal desorption with the gas chromatograph injector at 240 °C for 4 min. Linearity was observed from 0.1 to 1000 μg L −1 with relative standard deviations (RSD) less than 7% and recoveries were over 87%. The limit of detection (LOD) for pentachlorophenol was 0.008 μg L −1 . The proposed method was tested by analyzing landfill leachate from a sewage farm. The concentrations of chlorophenols were detected to range from 1.1 to 1.4 μg L −1 . The results demonstrate that the IL-SPME-GC/MS method is highly effective in analyzing trace chlorophenols in landfill leachate.

  5. Determination of chlorophenols in landfill leachate using headspace sampling with ionic liquid-coated solid-phase microextraction fibers combined with gas chromatography-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Ho, Tse-Tsung; Chen, Chung-Yu [Department of Chemistry, National Chung Hsing University, Taichung 40227, Taiwan (China); Li Zuguang [Department of Chemistry, National Chung Hsing University, Taichung 40227, Taiwan (China); College of Chemical Engineering and Materials Science, Zhejiang University of Technology, Hangzhou 310014, Zhejiang (China); Yang, Thomas Ching-Cherng [Department of Chemistry, National Kaohsiung Normal University, Kaohsiung 82444, Taiwan (China); Lee, Maw-Rong, E-mail: mrlee@dragon.nchu.edu.tw [Department of Chemistry, National Chung Hsing University, Taichung 40227, Taiwan (China)

    2012-01-27

    Highlights: Black-Right-Pointing-Pointer Ionic liquid (IL), ([C{sub 4}MIM][PF{sub 6}]), was rapid synthesized by microwave radiation. Black-Right-Pointing-Pointer Trace chlorophenols in landfill leachate were extract by SPME coated IL. Black-Right-Pointing-Pointer The IL-coated SPME-GC/MS method is low-cost, solvent-free and sensitive. - Abstract: A new microextraction technique based on ionic liquid solid-phase microextraction (IL-SPME) was developed for determination of trace chlorophenols (CPs) in landfill leachate. The synthesized ionic liquid, 1-butyl-3-methylimidazolium hexafluorophosphate ([C{sub 4}MIM][PF{sub 6}]), was coated onto the spent fiber of SPME for extraction of trace CPs. After extraction, the absorbed analytes were desorbed and quantified using gas chromatography-mass spectrometry (GC/MS). The term of the proposed method is as ionic liquid-coated of solid-phase microextraction combined with gas chromatography-mass spectrometry (IL-SPME-GC/MS). No carryover effect was found, and every laboratory-made ionic liquids-coated-fiber could be used for extraction at least eighty times without degradation of efficiency. The chlorophenols studied were 2,4-dichlorophenol (2,4-DP), 2,4,6-trichlorophenol (2,4,6-TCP), 2,3,4,6-tetrachlorophenol (2,3,4,6-TeCP), and pentachlorophenol (PCP). The best results of chlorophenols analysis were obtained with landfill leachate at pH 2, headspace extraction for 4 min, and thermal desorption with the gas chromatograph injector at 240 Degree-Sign C for 4 min. Linearity was observed from 0.1 to 1000 {mu}g L{sup -1} with relative standard deviations (RSD) less than 7% and recoveries were over 87%. The limit of detection (LOD) for pentachlorophenol was 0.008 {mu}g L{sup -1}. The proposed method was tested by analyzing landfill leachate from a sewage farm. The concentrations of chlorophenols were detected to range from 1.1 to 1.4 {mu}g L{sup -1}. The results demonstrate that the IL-SPME-GC/MS method is highly effective in

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

    International Nuclear Information System (INIS)

    Lockrem, L.L.

    1997-01-01

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

  7. Gas formation in drum waste packages of Paks NPP

    International Nuclear Information System (INIS)

    Molnar, M.; Palcsu, L.; Svingor, E.; Szanto, Z.; Futo, I.; Ormai, P.

    2000-01-01

    Gas composition measurements have been carried out by mass spectrometry analysis of samples taken from the headspace of ten drum waste packages generated and temporarily stored at Paks NPP. Four drums contained compacted solid waste, three drums were filled with grouted (solidified) sludge and three drums contained solid waste without compaction. The drums have been equipped with a special gas outlet system to make repeated sampling possible. Based on the first measurements significant differences in the gas composition and the rate of gas generation among the drums were found. (author)

  8. Analysis of Cyanide in Blood by Headspace-Isotope-Dilution-GC-MS

    DEFF Research Database (Denmark)

    Løbger, Lise Lotte; Petersen, Henning Willads; Andersen, Jens Enevold Thaulov

    2008-01-01

    An uncomplicated, rapid, automated procedure for the analysis of low cyanide concentrations in whole blood is reported. The analysis was performed by headspace gas chromatography and mass spectrometry in the (1H12C14N) and m/z 29 (1H13C15N). Carryover from cyanide adsorption onto the surface...

  9. Determination of residual volatile organic compounds migrated from polystyrene food packaging into food simulant by headspace solid phase micro extraction-gas chromatography

    International Nuclear Information System (INIS)

    Mohd Marsin Sanagi; Ling, Susie Lu; Zalilah Nasir; Wan Aini Wan Ibrahim; Abu Naim, Ahmedy

    2008-01-01

    The residual styrene and other volatile organic compounds (VOCs) present in the polystyrene food packaging are of concern as these compounds have the potential to migrate into the food in contact. This work describes a method for quantitative determination of VOCs, namely styrene, toluene, ethyl benzene, iso-propylbenzene and n-propylbenzene that have migrated from polystyrene food packaging into food stimulant by gas chromatography-flame ionization detection (GC-FID). Headspace solid phase micro extraction (HS-SPME) technique was applied for migration test using water as food stimulant. The effects of extraction variables including sample volume, eluotropic strength, extraction temperature, extraction time, desorption time, sample agitation, and salt addition on the amounts of the extracted analyses were studied to obtain the optimal HS-SPME conditions. The optimized method was applied to test the VOCs migrated from polystyrene bowls and cups at storage temperatures ranging from 24 to 80 degree Celsius for 30 min. Styrene and ethyl benzene were found to migrate from the samples into the food stimulant. The migration of analyze was found to be strongly dependent upon the storage temperature. The HS-SPME is useful as an alternative method to determine the migration of VOCs from food packaging material into food stimulant. (author)

  10. Study of gas generation in drum L/ILW packages using hermetic containers

    International Nuclear Information System (INIS)

    Molnar, M.; Palcsu, L.; Svingor, E.; Futo, I.; Major, Z.; Veres, M.

    2005-01-01

    Complete text of publication follows. During the storage of low and intermediate level radioactive waste (L/ILW) significant quantities of gas may be produced. It is likely that a small proportion of the generated gas will be radioactive as a result of the incorporation of the isotopes 3 H and 14 C that are present within the waste. To obtain reliable estimates of the quantities and rates of the gas production in L/ILWa series of measurements was carried out of waste packages produced and temporarily stored at the site of Paks Nuclear Power Plant (NPP). Ten drums filled with selected original L/ILW were placed into hermetic containers equipped with sampling valves for repeated sampling. These hermetic containers were stored at the same site where the L/ILW is stored primarily in the Paks NPP. The pressure and the temperature of the headspace gas in the containers were monitored continuously. Qualitative gas component analyses of headspace gases of drums and their containers were executed by quadrupole mass spectrometer. The gas generation rate in the stored L/ILW was calculated by the measured state parameters and the composition variation of the gas in the closed containers. Stable isotope measurements were executed from the CO 2 , CH 4 and N 2 fractions by stable isotope ratio mass spectrometer. Helium measurements were done by noble gas mass spectrometer. The tritium content of the vapour, H 2 and CH 4 fractions was measured by a low background liquid scintillation counter. 14 C content of the CO 2 and CH 4 fractions was measured by a low background gas proportional counter system (ATOMKI). Our results showed that the main generated gases in L/ILW are carbon dioxide, methane, hydrogen and nitrogen. The typical rates were 0.05-0.2 normal litre gas/day for CO 2 and CH 4 generation, and less than 0.02 normal litre gas/day for H 2 . Because of the typical vanishing of the O 2 from the headspace gases no explosive gas mixture was indicated in the L/ILW drums during

  11. Position for determining gas-phase volatile organic compound concentrations in transuranic waste containers. Revision 2

    Energy Technology Data Exchange (ETDEWEB)

    Connolly, M.J.; Liekhus, K.J. [Lockheed Martin Idaho Technologies Co., Idaho Falls, ID (United States). Idaho National Engineering and Environmental Lab.; Djordjevic, S.M.; Loehr, C.A.; Spangler, L.R. [Benchmark Environmental Corp. (United States)

    1998-06-01

    In the conditional no-migration determination (NMD) for the test phase of the Waste Isolation Pilot Plant (WIPP), the US Environmental Protection Agency (EPA) imposed certain conditions on the US Department of Energy (DOE) regarding gas phase volatile organic compound (VOC) concentrations in the void space of transuranic (TRU) waste containers. Specifically, the EPA required the DOE to ensure that each waste container has no layer of confinement that contains flammable mixtures of gases or mixtures of gases that could become flammable when mixed with air. The EPA also required that sampling of the headspace of waste containers outside inner layers of confinement be representative of the entire void space of the container. The EPA stated that all layers of confinement in a container would have to be sampled until DOE can demonstrate to the EPA that sampling of all layers is either unnecessary or can be safely reduced. A test program was conducted at the Idaho National Engineering and Environmental Laboratory (INEEL) to demonstrate that the gas phase VOC concentration in the void space of each layer of confinement in vented drums can be estimated from measured drum headspace using a theoretical transport model and that sampling of each layer of confinement is unnecessary. This report summarizes the studies performed in the INEEL test program and extends them for the purpose of developing a methodology for determining gas phase VOC concentrations in both vented and unvented TRU waste containers. The methodology specifies conditions under which waste drum headspace gases can be said to be representative of drum gases as a whole and describes a method for predicting drum concentrations in situations where the headspace concentration is not representative. The methodology addresses the approach for determining the drum VOC gas content for two purposes: operational period drum handling and operational period no-migration calculations.

  12. Position for determining gas phase volatile organic compound concentrations in transuranic waste containers. Revision 1

    International Nuclear Information System (INIS)

    Connolly, M.J.; Liekhus, K.J.; Djordjevic, S.M.; Loehr, C.A.; Spangler, L.R.

    1995-08-01

    In the conditional no-migration determination (NMD) for the test phase of the Waste Isolation Pilot Plant (WIPP), the US Environmental Protection Agency (EPA) imposed certain conditions on the US Department of Energy (DOE) regarding gas phase volatile organic compound (VOC) concentrations in the void space of transuranic (TRU) waste containers. Specifically, the EPA required the DOE to ensure that each waste container has no layer of confinement that contains flammable mixtures of gases or mixtures of gases that could become flammable when mixed with air. The EPA also required that sampling of the headspace of waste containers outside inner layers of confinement be representative of the entire void space of the container. The EPA stated that all layers of confinement in a container would have to be sampled until DOE can demonstrate to the EPA that sampling of all layers is either unnecessary or can be safely reduced. A test program was conducted at the Idaho National Engineering Laboratory (INEL) to demonstrate that the gas phase VOC concentration in the void space of each layer of confinement in vented drums can be estimated from measured drum headspace using a theoretical transport model and that sampling of each layer of confinement is unnecessary. This report summarizes the studies performed in the INEL test program and extends them for the purpose of developing a methodology for determining gas phase VOC concentrations in both vented and unvented TRU waste containers. The methodology specifies conditions under which waste drum headspace gases can be said to be representative of drum gases as a whole and describes a method for predicting drum concentrations in situations where the headspace concentration is not representative. The methodology addresses the approach for determining the drum VOC gas content for two purposes: operational period drum handling and operational period no-migration calculations

  13. Position for determining gas-phase volatile organic compound concentrations in transuranic waste containers. Revision 2

    International Nuclear Information System (INIS)

    Connolly, M.J.; Liekhus, K.J.

    1998-06-01

    In the conditional no-migration determination (NMD) for the test phase of the Waste Isolation Pilot Plant (WIPP), the US Environmental Protection Agency (EPA) imposed certain conditions on the US Department of Energy (DOE) regarding gas phase volatile organic compound (VOC) concentrations in the void space of transuranic (TRU) waste containers. Specifically, the EPA required the DOE to ensure that each waste container has no layer of confinement that contains flammable mixtures of gases or mixtures of gases that could become flammable when mixed with air. The EPA also required that sampling of the headspace of waste containers outside inner layers of confinement be representative of the entire void space of the container. The EPA stated that all layers of confinement in a container would have to be sampled until DOE can demonstrate to the EPA that sampling of all layers is either unnecessary or can be safely reduced. A test program was conducted at the Idaho National Engineering and Environmental Laboratory (INEEL) to demonstrate that the gas phase VOC concentration in the void space of each layer of confinement in vented drums can be estimated from measured drum headspace using a theoretical transport model and that sampling of each layer of confinement is unnecessary. This report summarizes the studies performed in the INEEL test program and extends them for the purpose of developing a methodology for determining gas phase VOC concentrations in both vented and unvented TRU waste containers. The methodology specifies conditions under which waste drum headspace gases can be said to be representative of drum gases as a whole and describes a method for predicting drum concentrations in situations where the headspace concentration is not representative. The methodology addresses the approach for determining the drum VOC gas content for two purposes: operational period drum handling and operational period no-migration calculations

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

    International Nuclear Information System (INIS)

    Lockrem, L.L.

    1997-01-01

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

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

    International Nuclear Information System (INIS)

    Lockrem, L.L.

    1997-01-01

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

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

    International Nuclear Information System (INIS)

    Lockrem, L.L.

    1997-01-01

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

  17. Analysis of neutral volatile aroma components in Tilsit cheese using a combination of dynamic headspace technique, capillary gas chromatography and mass spectrometry

    International Nuclear Information System (INIS)

    Dillinger, K.H.

    2000-03-01

    Tilsit cheese is made by the influence of lab ferment and starter cultures on milk. The ripening is done by repeated inoculation of the surface of the Tilsit cheese with yeasts and read smear cultures. This surface flora forms the typical aroma of the Tilsit cheese during the ripening process. The aim of the work was to receive general knowledge about the kind and amount of the neutral volatile aroma components of Tilsit cheese. Beyond this the ability of forming aroma components by read smear cultures and the dispersion of these components in cheese was to be examined. The results were intended to evaluate the formation of aroma components in Tilsit cheese. The semi-quantitative analyses of the aroma components of all samples were done by combining dynamic headspace extraction, gas chromatography and mass spectrometry. In this process the neutral volatile aroma components were extracted by dynamic headspace technique, adsorbed on a trap, thermally desorbed, separated by gas chromatography, detected and identified by mass spectrometry. 63 components belonging to the chemical classes of esters, ketones, aldehydes, alcohols and sulfur containing substances as well as aromatic hydrocarbons, chlorinated hydrocarbons and hydrocarbons were found in the analysed cheese samples of different Austrian Tilsit manufacturing plants. All cheese samples showed a qualitative equal but quantitative varied spectrum of aroma components. The cultivation of pure cultures on a cheese agar medium showed all analysed aroma components to be involved in the biochemical metabolism of these cultures. The ability to produce aroma components greatly differed between the strains and it was not possible to correlate this ability with the taxonomic classification of the strains. The majority of the components had a non-homogeneous concentration profile in the cheese body. This was explained by effects of diffusion and temporal and spatial different forming of components by the metabolism of the

  18. Headspace liquid-phase microextraction of methamphetamine and amphetamine in urine by an aqueous drop

    International Nuclear Information System (INIS)

    He Yi; Vargas, Angelica; Kang, Youn-Jung

    2007-01-01

    This study developed a headspace liquid-phase microextraction (LPME) method by using a single aqueous drop in combination with high performance liquid chromatography (HPLC)-UV detection for the determination of methamphetamine (MAP) and amphetamine (AP) in urine samples. The analytes, volatile and basic, were released from sample matrix into the headspace first, and then protonated and dissolved in an aqueous H 3 PO 4 drop hanging in the headspace by a HPLC syringe. After extraction, this drop was directly injected into HPLC. Parameters affecting extraction efficiency were investigated and optimized. This method showed good linearity in the investigated concentration range of 1.0-1500 μg L -1 , repeatability of the extraction (R.S.D. -1 for both analytes). Enrichment factors of about 400-fold and 220-fold were achieved for MAP and AP, respectively, at optimum conditions. The feasibility of the method was demonstrated by analyzing human urine samples

  19. Determination of some volatile compounds in alcoholic beverage by headspace solid-phase microextraction gas chromatography - mass spectrometry

    Science.gov (United States)

    Schmutzer, G.; Avram, V.; Feher, I.; David, L.; Moldovan, Z.

    2012-02-01

    The volatile composition of alcoholic beverage was studied by headspace solid-phase microextraction (HSSPME) method and gas chromatography - mass spectrometry (GC-MS). Some volatile compounds, such as alcohols, esters, terpenes and other are mainly responsible for the flavor of fortified wines and their amounts specify the quality of the alcoholic beverages. From this perspective it is interesting to develop a rapid, selective and sensitive analytical method suitable for simultaneous quantification of the main molecules being responsible for the organoleptic characteristic of alcoholic beverages. Vermouth fortified drink was analyzed in order to characterize the volatile profile. Using the HS-SPME/GC-MS a number of twenty-six volatile compounds from a commercial market alcoholic beverage were identified. The most abundant compounds were m-thymol, o-thymol and eugenol, alongside of the ethyl ester compounds.

  20. Headspace Analysis of Philippine Civet Coffee Beans Using Gas Chromatography-Mass Spectrometry and Electronic Nose

    Science.gov (United States)

    Ongo, E.; Sevilla, F.; Antonelli, A.; Sberveglieri, G.; Montevecchi, G.; Sberveglieri, V.; de Paola, E. L.; Concina, I.; Falasconi, M.

    2011-11-01

    Civet coffee, the most expensive and best coffee in the world, is an economically important export product of the Philippines. With a growing threat of food adulteration and counterfeiting, a need for quality authentication is essential to protect the integrity and strong market value of Philippine civet coffee. At present, there is no internationally accepted method of verifying whether a bean is an authentic civet coffee. This study presented a practical and promising approach to identify and establish the headspace qualitative profile of Philippine civet coffee using electronic nose (E-nose) and gas chromatography-mass spectrometry (GC-MS). E-nose analysis revealed that aroma characteristic is one of the most important quality indicators of civet coffee. The findings were supported by GC-MS analysis. Principal component analysis (PCA) exhibited a clearly separated civet coffees from their control beans. The chromatographic fingerprints indicated that civet coffees differed with their control beans in terms of composition and concentration of individual volatile constituents.

  1. 32-Week Holding-Time Study of SUMMA Polished Canisters and Triple Sorbent Traps Used To Sample Organic Constituents in Radioactive Waste Tank Vapor Headspace

    International Nuclear Information System (INIS)

    Evans, John C.; Huckaby, James L.; Mitroshkov, Alexandre V.; Julya, Janet L.; Hayes, James C.; Edwards, Jeffrey A.; Sasaki, Leela M.

    1997-01-01

    Two sampling methods[SUMMA polished canisters and triple sorbent traps (TSTs)] were compared for long-term storage of trace organic vapor samples collected from the headspaces of high-level radioactive waste tanks at the U.S. Department of Energy's Hanford Site in Washington State. Because safety, quality assurance, radiological controls, the long-term stability of the sampling media during storage needed to be addressed. Samples were analyzed with a gas chromatograph/mass spectrometer (GC/MS) using cryogenic reconcentration or thermal desorption sample introduction techniques. SUMMA canister samples were also analyzed for total non-methane organic compounds (TNMOC) by GC/flame ionization detector (FID) using EPA Compendium Method TO-12 . To verify the long-term stability of the sampling media, multiple samples were collected in parallel from a typical passively ventilated radioactive waste tank known to contain moderately high concentrations of both polar and nonpolar organic compounds. Analyses for organic analytes and TNMOC were conducted at increasing intervals over a 32-week period to determine whether any systematic degradation of sample integrity occurred. Analytes collected in the SUMMA polished canisters generally showed good stability over the full 32 weeks with recoveries at the 80% level or better for all compounds studied. The TST data showed some loss (50-80% recovery) for a few high-volatility compounds even in the refrigerated samples; losses for unrefrigerated samples were far more pronounced with recoveries as low as 20% observed in a few cases

  2. Determination of the solubility of low volatility liquid organic compounds in water using volatile-tracer assisted headspace gas chromatography.

    Science.gov (United States)

    Zhang, Shu-Xin; Chai, Xin-Sheng; Barnes, Donald G

    2016-02-26

    This study reports a new headspace gas chromatographic method (HS-GC) for the determination of water solubility of low volatility liquid organic compounds (LVLOs). The HS-GC analysis was performed on a set of aqueous solutions containing a range of concentrations of toluene-spiked (as a tracer) LVLOs, from under-saturation to over-saturation. A plot of the toluene tracer GC signal vs. the concentration of the LVLO results in two lines of different slopes that intersect at the concentration corresponding to the compound's solubility in water. The results showed that the HS-GC method has good precision (RSD waters of environmental and biological systems. Copyright © 2016 Elsevier B.V. All rights reserved.

  3. Headspace liquid-phase microextraction of methamphetamine and amphetamine in urine by an aqueous drop

    Energy Technology Data Exchange (ETDEWEB)

    He Yi [Department of Sciences, John Jay College of Criminal Justice, City University of New York, 445 W 59th Street, New York, NY 10019 (United States)]. E-mail: yhe@jjay.cuny.edu; Vargas, Angelica [Department of Sciences, John Jay College of Criminal Justice, City University of New York, 445 W 59th Street, New York, NY 10019 (United States); Kang, Youn-Jung [Department of Sciences, John Jay College of Criminal Justice, City University of New York, 445 W 59th Street, New York, NY 10019 (United States)

    2007-04-25

    This study developed a headspace liquid-phase microextraction (LPME) method by using a single aqueous drop in combination with high performance liquid chromatography (HPLC)-UV detection for the determination of methamphetamine (MAP) and amphetamine (AP) in urine samples. The analytes, volatile and basic, were released from sample matrix into the headspace first, and then protonated and dissolved in an aqueous H{sub 3}PO{sub 4} drop hanging in the headspace by a HPLC syringe. After extraction, this drop was directly injected into HPLC. Parameters affecting extraction efficiency were investigated and optimized. This method showed good linearity in the investigated concentration range of 1.0-1500 {mu}g L{sup -1}, repeatability of the extraction (R.S.D. < 5%, n = 6), and low detection limits (0.3 {mu}g L{sup -1} for both analytes). Enrichment factors of about 400-fold and 220-fold were achieved for MAP and AP, respectively, at optimum conditions. The feasibility of the method was demonstrated by analyzing human urine samples.

  4. Wet gas sampling

    Energy Technology Data Exchange (ETDEWEB)

    Welker, T.F.

    1997-07-01

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

  5. Liquid-liquid extraction/headspace/gas chromatographic/mass spectrometric determination of benzene, toluene, ethylbenzene, (o-, m- and p-)xylene and styrene in olive oil using surfactant-coated carbon nanotubes as extractant.

    Science.gov (United States)

    Carrillo-Carrión, Carolina; Lucena, Rafael; Cárdenas, Soledad; Valcárcel, Miguel

    2007-11-09

    BTEX-S compounds are widely distributed in the environment and can be present in different foodstuffs, including olive oil. Taking into account the risks of the exposure to these compounds, analytical methods for their determination in different matrices are mandatory. In this paper, the use of surfactant-coated multiwalled carbon nanotubes as additive in liquid-liquid extraction is applied for the determination of single-ring aromatic compounds in olive oil samples. After sample treatment, the aqueous extracts are subsequently analyzed by headspace/gas chromatography/mass spectrometry allowing the determination of BTEX-S within ca. 15 min. Each stage of the proposed LLE/HS/GC/MS configuration involves a selectivity enhancement avoiding the interference of other compounds of the sample matrix. Limits of detection were in the range 0.25 ng mL(-1) (obtained for ethylbenzene) and 0.43 ng mL(-1) (for benzene). The repeatability of the proposed method expressed as RSD varied between 1.9% (styrene) and 3.3% (benzene) (n=11).

  6. Comparison of direct, headspace and headspace cold fiber modes in solid phase microextraction of polycyclic aromatic hydrocarbons by a new coating based on poly(3,4-ethylenedioxythiophene)/graphene oxide composite.

    Science.gov (United States)

    Banitaba, Mohammad Hossein; Hosseiny Davarani, Saied Saeed; Kazemi Movahed, Siyavash

    2014-01-17

    A novel nanocomposite coating made of poly(3,4-ethylenedioxythiophene) (PEDOT) and graphene oxide was electrochemically prepared on gold wire. The prepared fiber was applied to the solid-phase microextraction (SPME) and gas chromatographic analysis of six polycyclic aromatic hydrocarbons (PAHs). Three modes of extraction i.e. direct immersion (DI), headspace (HS) and headspace cold fiber (HS-CF) in SPME were investigated. The results were compared under optimized conditions of each mode, considering the effects of the three most important parameters which are extraction temperature, extraction time and ionic strength. The comparison showed that HS-CF-SPME results in the best outcome for the extraction of PAHs from water samples. Under the optimized conditions of this mode, the calibration curves were linear within the range of 0.4-600μgL(-1) and the detection limits were between 0.05 and 0.13μgL(-1). The intra-day and inter-day relative standard deviations obtained at 10μgL(-1) (n=5), using a single fiber, were 4.1-6.8% and 4.8-8.4%, respectively. The fiber-to-fiber repeatabilities (n=4), expressed as the relative standard deviations (RSD%), were between 6.5% and 10.7% at a 10μgL(-1) concentration level. The method was successfully applied to the analysis of PAHs in seawater samples showing recoveries from 85% to 107%. Copyright © 2013 Elsevier B.V. All rights reserved.

  7. A short review of headspace extraction and ultrasonic solvent extraction for honey volatiles fingerprinting

    Directory of Open Access Journals (Sweden)

    Z. Marijanović

    2009-01-01

    Full Text Available Honey volatiles exhibit a potential role in distinguishing honeys as a function of botanical origin, but heating of honey generates artefacts such as compounds of Strecker degradation and Maillard reaction products. This short review is focused on the most recently applied methods for honey volatiles fingerprinting (without generation of thermal artefacts: headspace extraction (dynamic headspace extraction (DHE, headspace solid-phase microextraction (HS-SPME and ultrasonic solvent extraction (USE. These methods display a varying degree of selectivity and effectiveness depending upon the compounds involved and the extraction conditions. Recent developments of these methods are discussed, with application examples drawn from the literature as well from our own research. Flavour qualities of the honey are very much dependent on the volatile and semivolatile organic compounds present in both the sample matrix and the headspace aroma. Therefore the use of one single technique is not adequate for reliable honey volatiles profiling, but combined use of headspace extraction and ultrasonic solvent extraction could be a useful tool for the characterization of the honey and identification of its botanical source through typical volatile marker compounds.

  8. Multiple headspace-solid-phase microextraction: an application to quantification of mushroom volatiles.

    Science.gov (United States)

    Costa, Rosaria; Tedone, Laura; De Grazia, Selenia; Dugo, Paola; Mondello, Luigi

    2013-04-03

    Multiple headspace-solid phase microextraction (MHS-SPME) followed by gas chromatography/mass spectrometry (GC-MS) and flame ionization detection (GC-FID) was applied to the identification and quantification of volatiles released by the mushroom Agaricus bisporus, also known as champignon. MHS-SPME allows to perform quantitative analysis of volatiles from solid matrices, free of matrix interferences. Samples analyzed were fresh mushrooms (chopped and homogenized) and mushroom-containing food dressings. 1-Octen-3-ol, 3-octanol, 3-octanone, 1-octen-3-one and benzaldehyde were common constituents of the samples analyzed. Method performance has been tested through the evaluation of limit of detection (LoD, range 0.033-0.078 ng), limit of quantification (LoQ, range 0.111-0.259 ng) and analyte recovery (92.3-108.5%). The results obtained showed quantitative differences among the samples, which can be attributed to critical factors, such as the degree of cell damage upon sample preparation, that are here discussed. Considerations on the mushrooms biochemistry and on the basic principles of MHS analysis are also presented. Copyright © 2013 Elsevier B.V. All rights reserved.

  9. 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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2008-06-09

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

  11. [Simultaneous determination of seven residual solvents in bovis calculus artifactus by headspace gas chromatography].

    Science.gov (United States)

    Chi, Shuyao; Wu, Dike; Sun, Jinhong; Ye, Ruhan; Wang, Xiaoyan

    2014-05-01

    A headspace gas chromatography (HS-GC) method was developed for the simultaneous determination of seven residual solvents (petroleum ether (60-90 degrees C), acetone, ethyl acetate, methanol, methylene chloride, ethanol and butyl acetate) in bovis calculus artifactus. The DB-WAX capillary column and flame ionization detector (FID) were used for the separation and detection of the residual solvents, and the internal standard method was used for the quantification. The chromatographic conditions, such as equilibrium temperature and equilibrium time, were optimized. Under the optimized conditions, all of the seven residual solvents showed good linear relationships with good correlation coefficients (not less than 0.999 3) in the prescribed concentration range. At three spiked levels, the recoveries for the seven residual solvents were 94.7%-105.2% with the relative standard deviations (RSDs) less than 3.5%. The limits of detection (LODs) of the method were 0.43-5.23 mg/L, and the limits of quantification (LOQs) were 1.25-16.67 mg/L. The method is simple, rapid, sensitive and accurate, and is suitable for the simultaneous determination of the seven residual solvents in bovis calculus artifactus.

  12. Organic analysis of the headspace in Hanford waste tanks

    International Nuclear Information System (INIS)

    Lucke, R.B.; McVeety, B.D.; Clauss, T.W.; Fruchter, J.S.; Goheen, S.C.

    1994-01-01

    Before radioactive mixed waste in Hanford waste tanks can be isolated and permanently stored, several safety issues need to be addressed. The headspace vapors in Hanford Tank 103-C raise two issues: (1) the potential flammability of the vapor and aerosol, and (2) the potential worker health and safety hazards associated with the toxicity of the constituents. As a result, the authors have implemented organic analysis methods to characterize the headspace vapors in Hanford waste tanks. To address the flammability issue, they have used OSHA versatile sampling (OVS) tubes as the sampling method followed by solvent extraction and GC/MS analysis. For analyzing volatile organics and organic air toxins, they have implemented SUMMA trademark canisters as the collection device followed by cryogenic trapping and GC/MS analysis. Strategies for modifying existing NIOSH and EPA methods to make them applicable to vapors in Hanford waste tanks are discussed. Identification and quantification results of volatile and semivolatile organics are presented

  13. Headspace techniques in foods, fragrances and flavors: an overview.

    Science.gov (United States)

    Rouseff, R; Cadwallader, K

    2001-01-01

    Headspace techniques have traditionally involved the collection of volatiles in the vapor state under either dynamic or static conditions as a means of determining concentrations in the product of interest. A brief overview of contemporary headspace applications and recent innovations are presented from the literature and Chapters in this book. New approaches used to concentrate volatiles under static conditions such as solid phase micro extraction, SPME, are examined. Advances in purge and trap applications and automation are also presented. Innovative methods of evaluating headspace volatiles using solid state sensor arrays (electronic noses) or mass spectrometers without prior separation are referenced. Numerous food and beverage headspace techniques are also reviewed. Advantages, limitations and alternatives to headspace analysis are presented.

  14. Quantitative analysis of aldehydes in canned vegetables using static headspace-gas chromatography-mass spectrometry.

    Science.gov (United States)

    Serrano, María; Gallego, Mercedes; Silva, Manuel

    2017-11-17

    Volatile aldehydes appear in canned vegetables as constituents and some of them can also be present as disinfection by-products (DBPs) because of the contact between vegetables and treated water. This paper describes two static headspace-gas chromatography-mass spectrometry (SHS-GC-MS) methods to determine 15 aldehydes in both the solid and the liquid phases of canned vegetables. The treatment for both phases of samples was carried out simultaneously into an SHS unit, including the leaching of the aldehydes (from the vegetable), their derivatization and volatilization of the oximes formed. Detection limits were obtained within the range of 15-400μg/kg and 3-40μg/L for aldehydes in the solid and the liquid phases of the food, respectively. The relative standard deviation was lower than 7% -for the whole array of the target analytes-, the trueness evaluated by recovery experiments provided %recoveries between 89 and 99% and short- and long-term stability studies indicated there was no significant variation in relative peak areas of all aldehydes in both phases of canned vegetables after their storing at 4°C for two weeks. The study of the origin of the 15 aldehydes detected between both phases of canned vegetables showed that: i) the presence of 13 aldehydes -at average concentrations of 2.2-39μg/kg and 0.25-71μg/L for the solid and the liquid phases, respectively- is because they are natural constituents of vegetables; and ii) the presence of glyoxal and methylglyoxal -which are mainly found in the liquid phase (average values, 1.4-4.1μg/L)- is ascribed to the use of treated water, thereby being DBPs. Copyright © 2017 Elsevier B.V. All rights reserved.

  15. A novel sol-gel-based amino-functionalized fiber for headspace solid-phase microextraction of phenol and chlorophenols from environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Bagheri, Habib [Department of Chemistry, Sharif University of Technology, P.O. Box 11365-9516, Tehran (Iran, Islamic Republic of)], E-mail: Bagheri@sharif.edu; Babanezhad, Esmaeil; Khalilian, Faezeh [Department of Chemistry, Sharif University of Technology, P.O. Box 11365-9516, Tehran (Iran, Islamic Republic of)

    2008-05-26

    A novel amino-functionalized polymer was synthesized using 3-(trimethoxysilyl) propyl amine (TMSPA) as precursor and hydroxy-terminated polydimethylsiloxane (OH-PDMS) by sol-gel technology and coated on fused-silica fiber. The synthesis was designed in a way to impart polar moiety into the coating network. The scanning electron microscopy (SEM) images of this new coating showed the homogeneity and the porous surface structure of the film. The efficiency of new coating was investigated for headspace solid-phase microextraction (SPME) of some environmentally important chlorophenols from aqueous samples followed by gas chromatography-mass spectrometry (GC-MS) analysis. Effect of different parameters influencing the extraction efficiency such as extraction temperature, extraction time, ionic strength and pH was investigated and optimized. In order to improve the separation efficiency of phenolic compounds on chromatography column all the analytes were derivatized prior to extraction using acetic anhydride at alkaline condition. The detection limits of the method under optimized conditions were in the range of 0.02-0.05 ng mL{sup -1}. The relative standard deviations (R.S.D.) (n = 6) at a concentration level of 0.5 ng mL{sup -1} were obtained between 6.8 and 10%. The calibration curves of chlorophenols showed linearity in the range of 0.5-200 ng mL{sup -1}. The proposed method was successfully applied to the extraction from spiked tap water samples and relative recoveries were higher than 90% for all the analytes.

  16. Evaluation of noni (Morinda citrifolia volatile profile by dynamic headspace and gas chromatography-mass spectrometry Avaliação do perfil de voláteis em noni (Morinda citrifolia por headspace dinâmico e cromatografia gasosa-espectrometria de massas

    Directory of Open Access Journals (Sweden)

    Adriana Sousa

    2010-09-01

    Full Text Available Noni is a fruit that has interested the scientific community due to its medicinal and functional activities. Different products that contain noni are already in the market, but their consumption could be impaired by their distinctive unpleasant aroma and flavor. The aim of this work was to evaluate the noni pulp volatile profile by dynamic headspace and gas chromatography-mass spectrometry. Thirty seven volatile compounds were detected, mainly alcohols (63.3%, esters (26.9%, cetones (7.4%, and acids (1.2%.O noni é um fruto que tem interessado à comunidade científica por sua atividade funcional e medicinal. Já se encontram no mercado diferentes produtos que contêm noni em sua composição, mas seu consumo tem sido prejudicado por seu aroma e sabor desagradáveis. O objetivo deste trabalho foi o de avaliar o perfil de voláteis da polpa de noni pela técnica de headspace dinâmico e cromatografia gasosa-espectrometria de massas. Foram detectados 37 compostos voláteis, sendo os principais: alcoóis (63,3%, ésteres (26,9%, cetonas (7,4% e ácidos (1,2%.

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

    Directory of Open Access Journals (Sweden)

    LIANG Cui-cui

    2015-01-01

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

  18. Gas and porewater composition of shallow sediments in the Tuaheni Basin, New Zealand

    Science.gov (United States)

    Rose, P. S.; Coffin, R. B.; Yoza, B.; Boyd, T. J.; Crutchley, G. J.; Mountjoy, J. J.; Pecher, I. A.

    2015-12-01

    Seismic profiles collected during previous investigations on the Hikurangi Margin, off the North Island, New Zealand showed bottom simulating reflectors (BSRs), which are generally indicative of the presence of free gas. Further, double BSRs clearly identified in the Tuaheni Basin were hypothesized to result from differences in gas composition and fluid migration. During a cruise on the RV Tangaroa in June 2015 (TAN 1508) additional seismic data were collected and used to identify piston coring targets. Coring locations were selected to sample around BSR pinch-outs and possible fluid migration pathways to determine gas composition and flux. Shallow sediments collected in June 2015 in the Tuaheni Basin had relatively low sediment headspace CH4 concentrations (6000ppm. Higher molecular weight alkanes were not detected in the sediment headspace gas at any location. Sediment porewater sulfate, chloride and sulfide concentrations will be presented with CH4concentration profiles and geophysical data.

  19. [A novel vapor dynamic headspace enrichment equipment for nontarget screening of volatile organic compounds in drinking water].

    Science.gov (United States)

    Ma, Huilian; Zhang, Haijun; Tian, Yuzeng; Wang, Longxing; Chen, Jiping

    2011-09-01

    A novel vapor dynamic headspace enrichment device was set up for nontarget screening of volatile organic compounds (VOCs) in drinking water. The main operating parameters of this device, such as length of distillation tube, volume of collected condensate, and choice of absorbent, were optimized. In this device, vapor was utilized as a purge gas and water was utilized as a absorbent. With the help of the device, one liter of water sample could be concentrated to 5 mL and the sensitivity of traditional purge and trap-gas chromatography-mass spectrometry (P&T-GC-MS) could be improved 1-2 orders of magnitude. Source and disinfected water samples from a water treatment plant were analyzed with this method. Compared with the traditional P&T-GC-MS analysis without pre-enrichment, the numbers of identified VOCs were improved from 0 to 16 for source water and 5 to 35 for disinfected water samples. It is also shown that there are many halide compounds in VOCs in disinfected water which do not exist in source water.

  20. Headspace concentrations of explosive vapors in containers designed for canine testing and training: theory, experiment, and canine trials.

    Science.gov (United States)

    Lotspeich, Erica; Kitts, Kelley; Goodpaster, John

    2012-07-10

    It is a common misconception that the amount of explosive is the chief contributor to the quantity of vapor that is available to trained canines. In fact, this quantity (known as odor availability) depends not only on the amount of explosive material, but also the container volume, explosive vapor pressure and temperature. In order to better understand odor availability, headspace experiments were conducted and the results were compared to theory. The vapor-phase concentrations of three liquid explosives (nitromethane, nitroethane and nitropropane) were predicted using the Ideal Gas Law for containers of various volumes that are in use for canine testing. These predictions were verified through experiments that varied the amount of sample, the container size, and the temperature. These results demonstrated that the amount of sample that is needed to saturate different sized containers is small, predictable and agrees well with theory. In general, and as expected, once the headspace of a container is saturated, any subsequent increase in sample volume will not result in the release of more vapors. The ability of canines to recognize and alert to differing amounts of nitromethane has also been studied. In particular, it was found that the response of trained canines is independent of the amount of nitromethane present, provided it is a sufficient quantity to saturate the container in which it is held. Copyright © 2012 Elsevier Ireland Ltd. All rights reserved.

  1. Determination of dissolved methane in natural waters using headspace analysis with cavity ring-down spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Roberts, Hannah M.; Shiller, Alan M., E-mail: alan.shiller@usm.edu

    2015-01-26

    Highlights: • A method for determining low nanomolar dissolved CH{sub 4} was developed. • The methane detection utilizes cavity ring-down spectroscopy (CRDS). • Use of CRDS requires less time, materials and labor than typical of GC analysis. • Relative standard deviations of ∼4% were achieved at low nM CH{sub 4}. • Applications to seawater and river water are presented. - Abstract: Methane (CH{sub 4}) is the third most abundant greenhouse gas (GHG) but is vastly understudied in comparison to carbon dioxide. Sources and sinks to the atmosphere vary considerably in estimation, including sources such as fresh and marine water systems. A new method to determine dissolved methane concentrations in discrete water samples has been evaluated. By analyzing an equilibrated headspace using laser cavity ring-down spectroscopy (CRDS), low nanomolar dissolved methane concentrations can be determined with high reproducibility (i.e., 0.13 nM detection limit and typical 4% RSD). While CRDS instruments cost roughly twice that of gas chromatographs (GC) usually used for methane determination, the process presented herein is substantially simpler, faster, and requires fewer materials than GC methods. Typically, 70-mL water samples are equilibrated with an equivalent amount of zero air in plastic syringes. The equilibrated headspace is transferred to a clean, dry syringe and then drawn into a Picarro G2301 CRDS analyzer via the instrument’s pump. We demonstrate that this instrument holds a linear calibration into the sub-ppmv methane concentration range and holds a stable calibration for at least two years. Application of the method to shipboard dissolved methane determination in the northern Gulf of Mexico as well as river water is shown. Concentrations spanning nearly six orders of magnitude have been determined with this method.

  2. Tank vapor characterization project. Headspace vapor characterization of Hanford waste Tank SX-101: Results from samples collected on 07/21/95

    International Nuclear Information System (INIS)

    Evans, J.C.; Clauss, T.W.; McVeety, B.D.; Pool, K.H.; Olsen, K.B.; Fruchter, J.S.; Silvers, K.L.

    1996-05-01

    Results described in this report were obtained to characterize the vapors present in the tank headspace and to support safety evaluations and tank-farm operations. They include air concentrations of inorganic and organic analytes and grouped compounds from samples. The vapor concentrations are based either on whole-volume samples or on sorbent traps exposed to sample flow. No immediate notifications were needed because analytical results indicated no specific analytes exceeded notification levels. Summary of results: NH3, 3.8 ppmv; NO2, 0.10 ppmv; NO, 0.13 ppm; H2O, 11.8 mg/L; CO2, 338 ppmv; CO, 3 ; methanol, 0.060 ppmv; acetone, 0.033 ppmv; trichlorofluoromethane, 0.023 ppmv; and acetone, 0.034 ppmv

  3. Optimization of headspace experimental factors to determine chlorophenols in water by means of headspace solid-phase microextraction and gas chromatography coupled with mass spectrometry and parallel factor analysis.

    Science.gov (United States)

    Morales, Rocío; Cruz Ortiz, M; Sarabia, Luis A

    2012-11-19

    In this work an analytical procedure based on headspace solid-phase microextraction and gas chromatography coupled with mass spectrometry (HS-SPME-GC/MS) is proposed to determine chlorophenols with prior derivatization step to improve analyte volatility and therefore the decision limit (CCα). After optimization, the analytical procedure was applied to analyze river water samples. The following analytes are studied: 2,4-dichlorophenol (2,4-DCP), 2,4,6-trichlorophenol (2,4,6-TrCP), 2,3,4,6-tetrachlorophenol (2,4,6-TeCP) and pentachlorophenol (PCP). A D-optimal design is used to study the parameters affecting the HS-SPME process and the derivatization step. Four experimental factors at two levels and one factor at three levels were considered: (i) equilibrium/extraction temperature, (ii) extraction time, (iii) sample volume, (iv) agitation time and (v) equilibrium time. In addition two interactions between four of them were considered. The D-optimal design enables the reduction of the number of experiments from 48 to 18 while maintaining enough precision in the estimation of the effects. As every analysis took 1h, the design is blocked in 2 days. The second-order property of the PARAFAC (parallel factor analysis) decomposition avoids the need of fitting a new calibration model each time that the experimental conditions change. In consequence, the standardized loadings in the sample mode estimated by a PARAFAC decomposition are the response used in the design because they are proportional to the amount of analyte extracted. It has been found that block effect is significant and that 60°C equilibrium temperature together with 25min extraction time are necessary to achieve the best extraction for the chlorophenols analyzed. The other factors and interactions were not significant. After that, a calibration based in a PARAFAC2 decomposition provided the following values of CCα: 120, 208, 86, 39ngL(-1) for 2,4-DCP, 2,4,6-TrCP, 2,3,4,5-TeCP and PCP respectively for a

  4. Determination of the analytical performance of a headspace capillary gas chromatographic technique and karl Fischer coulometric titration by system calibration using oil samples containing known amounts of moisture.

    Science.gov (United States)

    Jalbert, J; Gilbert, R; Tétreault, P

    1999-08-01

    Over the past few years, concerns have been raised in the literature about the accuracy of the Karl Fischer (KF) method for assessing moisture in transformer mineral oils. To better understand this issue, the performance of a static headspace capillary gas chromatographic (HS-CGC) technique was compared to that of KF coulometric titration by analyzing moisture in samples containing known amounts of water and various samples obtained from the National Institute of Standards and Technology (NIST). Two modes of adding samples into the KF vessel were used:  direct injection and indirect injection via an azeotropic distillation of the moisture with toluene. Under the conditions used for direct injection, the oil matrix was totally dissolved in the anolyte, which allowed the moisture to be titrated in a single-phase solution rather than in a suspension. The results have shown that when HS-CGC and combined azeotropic distillation/KF titration are calibrated with moisture-in-oil standards, a linear relation is observed over 0-60 ppm H(2)O with a correlation coefficient better than 0.9994 (95% confidence), with the regression line crossing through zero. A similar relation can also be observed when calibration is achieved by direct KF addition of standards prepared with octanol-1, but in this case an intercept of 4-5 ppm is noted. The amount of moisture determined by curve interpolation in NIST reference materials by the three calibrated systems ranges from 13.0 to 14.8 ppm for RM 8506 and 42.5 to 46.4 ppm for RM 8507, and in any case, the results were as high as those reported in the literature with volumetric KF titration. However, titration of various dehydrated oil and solvent samples showed that direct KF titration is affected by a small bias when samples contain very little moisture. The source of error after correction for the large sample volume used for the determination (8 mL) is about 6 ppm for Voltesso naphthenic oil and 4 ppm for toluene, revealing a matrix

  5. Identificação e quantificação de voláteis de café através de cromatografia gasosa de alta resolução / espectrometria de massas empregando um amostrador automático de "headspace" Identification and quantification of coffee volatile components through high resolution gas chromatoghaph/mass spectrometer using a headspace automatic sampler

    Directory of Open Access Journals (Sweden)

    Leonardo César AMSTALDEN

    2001-01-01

    Full Text Available Usando um amostrador automático, os "headspaces" de três marcas comerciais de café torrado e moído foram analisados qualitativa e quantitativamente quanto a composição dos voláteis responsáveis pelo aroma através da técnica de cromatografia gasosa/espectrometria de massas. Uma vez que a metodologia não envolveu isolamento ou concentração dos aromas, suas proporções naturais foram mantidas, além de simplificar o preparo das amostras. O emprego do amostrador automático permitiu também boa resolução dos picos cromatográficos sem o emprego de criogenia, contribuindo para redução no tempo de análise. Noventa e um componentes puderam ser identificados, sendo que alguns compostos conhecidos como presentes em café como o dimetilsulfeto, metional e furfuril mercaptana não foram detectados. Os voláteis presentes em maior concentração puderam ser quantificados com o auxílio de dois padrões internos. A técnica se provou viável, tanto para caracterização como para quantificação de voláteis de café.Employing an automatic headspace sampler, the headspaces of three commercial brands of ground roasted coffee were qualitatively and quantitatively analyzed by gas chromatography / mass spectrometry. Since the methodology did not involve aroma isolation or concentration, their natural proportions were maintained, providing a more accurate composition of the flavors, and simplifying sample preparation. The automatic sampler allowed good resolution of the chromatographic peaks without cryofocusing the samples at the head of the column during injection, reducing analysis time. Ninety one compounds were identified and some known coffee volatiles, such as dimethyl sulphide, methional and furfuryl mercaptan were not detected. The more concentrated volatiles could be identified using two internal standards. The technique proved viable, for both characterization and for quantification of coffee volatiles.

  6. Polyaniline-nylon-6 electrospun nanofibers for headspace adsorptive microextraction

    International Nuclear Information System (INIS)

    Bagheri, Habib; Aghakhani, Ali

    2012-01-01

    Highlights: ► Polyaniline–polyamide nanofiber mat was fabricated by electrospinning technology. ► Electrospun nanofiber was used for extraction of chlorobenzenes from aquatic media. ► A method based on headspace adsorptive microextraction and GC–MS was developed. - Abstract: A headspace adsorptive microextraction technique was developed using a novel polyaniline-nylon-6 (PANI-N6) nanofiber sheet, fabricated by electrospinning. The homogeneity and the porosity of the prepared PANI-N6 sheet were studied using the scanning electron microscopy (SEM) and nanofibers diameters were found to be around 200 nm. The novel nanofiber sheet was examined as an extracting medium to isolate some selected chlorobenzenes (CBs), as model compounds, from aquatic media. The extracted analytes were desorbed using μL-amounts of solvent and eventually an aliquot of extractant was injected into gas chromatography–mass spectrometry (GC–MS). Various parameters affecting the extraction and desorption processes were optimized. The developed method proved to be convenient and offers sufficient sensitivity and a good reproducibility. Limits of detection achieved for CBs with the developed analytical procedure ranged from 19 to 33 ng L −1 , while limits of quantification were from 50 to 60 ng L −1 . The relative standard deviations (RSD) at a concentration level of 0.1 ng mL −1 and 1 ng mL −1 were in the range of 8–14% and 5–11% (n = 3), respectively. The calibration curves of analytes were investigated in the range of 50–1000 ng L −1 and R 2 between 0.9739 and 0.9932 were obtained. The developed method was successfully applied to the extraction of selected CBs from tap and river water samples. The relative recovery (RR) percentage obtained for the spiked real water samples at 0.1 ng mL −1 and 1 ng mL −1 level were 93–103% and 95–104%, respectively. The whole procedure showed to be conveniently applicable and quite easy to handle.

  7. Polyaniline-nylon-6 electrospun nanofibers for headspace adsorptive microextraction

    Energy Technology Data Exchange (ETDEWEB)

    Bagheri, Habib, E-mail: bagheri@sharif.edu [Environmental and Bio-Analytical Laboratories, Department of Chemistry, Sharif University of Technology, P.O. Box 11365-9516, Tehran (Iran, Islamic Republic of); Aghakhani, Ali [Environmental and Bio-Analytical Laboratories, Department of Chemistry, Sharif University of Technology, P.O. Box 11365-9516, Tehran (Iran, Islamic Republic of)

    2012-02-03

    Highlights: Black-Right-Pointing-Pointer Polyaniline-polyamide nanofiber mat was fabricated by electrospinning technology. Black-Right-Pointing-Pointer Electrospun nanofiber was used for extraction of chlorobenzenes from aquatic media. Black-Right-Pointing-Pointer A method based on headspace adsorptive microextraction and GC-MS was developed. - Abstract: A headspace adsorptive microextraction technique was developed using a novel polyaniline-nylon-6 (PANI-N6) nanofiber sheet, fabricated by electrospinning. The homogeneity and the porosity of the prepared PANI-N6 sheet were studied using the scanning electron microscopy (SEM) and nanofibers diameters were found to be around 200 nm. The novel nanofiber sheet was examined as an extracting medium to isolate some selected chlorobenzenes (CBs), as model compounds, from aquatic media. The extracted analytes were desorbed using {mu}L-amounts of solvent and eventually an aliquot of extractant was injected into gas chromatography-mass spectrometry (GC-MS). Various parameters affecting the extraction and desorption processes were optimized. The developed method proved to be convenient and offers sufficient sensitivity and a good reproducibility. Limits of detection achieved for CBs with the developed analytical procedure ranged from 19 to 33 ng L{sup -1}, while limits of quantification were from 50 to 60 ng L{sup -1}. The relative standard deviations (RSD) at a concentration level of 0.1 ng mL{sup -1} and 1 ng mL{sup -1} were in the range of 8-14% and 5-11% (n = 3), respectively. The calibration curves of analytes were investigated in the range of 50-1000 ng L{sup -1} and R{sup 2} between 0.9739 and 0.9932 were obtained. The developed method was successfully applied to the extraction of selected CBs from tap and river water samples. The relative recovery (RR) percentage obtained for the spiked real water samples at 0.1 ng mL{sup -1} and 1 ng mL{sup -1} level were 93-103% and 95-104%, respectively. The whole procedure showed

  8. Solvent-free sample preparation by headspace solid-phase microextraction applied to the tracing of n-butyl nitrite abuse.

    Science.gov (United States)

    Tytgat, J; Daenens, P

    1996-01-01

    The most common alkyl nitrites encountered in forensic toxicology are iso-butyl, n-butyl and iso-pentyl(amyl) nitrites. All have become popular as an aphrodisiac, especially among the homosexual population. Alkyl nitrites are a volatile and unstable group of compounds, which hydrolyse in aqueous matrices to the alcohol and nitrite ion. Here we describe a fast, clean and sensitive procedure for the detection of hydrolysed n-butyl nitrite in whole human blood using a new, solvent-free sampling technique, the headspace solid-phase micro-extraction (HSPME), combined with GC/FID analysis. Sample preparation was investigated using two different stationary phases (100 microns polydimethylsiloxane and 85 microns polyacrylate), coating a fused silica fibre. The effect of different sampling times at fixed temperatures was also studied. Our results demonstrate that the HSPME/GC/FID procedure allows tracing of n-butyl nitrite abuse and detects hydrolysed n-butyl nitrite, i.e., released n-butanol, in whole blood at the 1 ng/mL level.

  9. Field portable low temperature porous layer open tubular cryoadsorption headspace sampling and analysis part I: Instrumentation.

    Science.gov (United States)

    Bruno, Thomas J

    2016-01-15

    Building on the successful application in the laboratory of PLOT-cryoadsorption as a means of collecting vapor (or headspace) samples for chromatographic analysis, in this paper a field portable apparatus is introduced. This device fits inside of a briefcase (aluminum tool carrier), and can be easily transported by vehicle or by air. The portable apparatus functions entirely on compressed air, making it suitable for use in locations lacking electrical power, and for use in flammable and explosive environments. The apparatus consists of four aspects: a field capable PLOT-capillary platform, the supporting equipment platform, the service interface between the PLOT-capillary and the supporting equipment, and the necessary peripherals. Vapor sampling can be done with either a hand piece (containing the PLOT capillary) or with a custom fabricated standoff module. Both the hand piece and the standoff module can be heated and cooled to facilitate vapor collection and subsequent vapor sample removal. The service interface between the support platform and the sampling units makes use of a unique counter current approach that minimizes loss of cooling and heating due to heat transfer with the surroundings (recuperative thermostatting). Several types of PLOT-capillary elements and sampling probes are described in this report. Applications to a variety of samples relevant to forensic and environmental analysis are discussed in a companion paper. Published by Elsevier B.V.

  10. Application of head-space solid-phase microextraction for the analysis of volatile metabolites emitted by Penicillium species

    DEFF Research Database (Denmark)

    Nilsson, Torben; Larsen, Thomas Ostenfeld; Montanarella, Luca

    1996-01-01

    Head-space solid-phase microextraction (HS-SPME) has been used to collect volatile organic compounds (VOCs) emitted from fungi of the genus Penicillium. Gas chromatography combined with mass spectrometry (GC-MS) was employed for the analysis of the profiles of volatile metabolites characteristic...

  11. Identification of volatile organic compounds (VOCs in different colour carrot (Daucus carota L. cultivars using static headspace/gas chromatography/mass spectrometry

    Directory of Open Access Journals (Sweden)

    Zehra Güler

    2015-12-01

    Full Text Available Volatile organic compounds (VOCs as well as sugar and acid contents affect carrot flavour. This study compared VOCs in 11 carrot cultivars. Gas chromatography/mass spectrometry using static headspace technique was applied to analyse the VOCs. The number of VOCs per sample ranged from 17 to 31. The primarily VOCs identified in raw carrots with the exception of “Yellow Stone” were terpenes, ranging from 65 to 95%. The monoterpenes with values ranging from 31 to 89% were higher than those (from 2 to 15% of sesquiterpenes. Monoterpene α-terpinolene (with ranging from 23 to 63% and (--α-pinene (26%, and alcohol ethanol (35% was the main VOC in extracts from the nine carrot cultivars, “Purple” and “Yellow Stone”, respectively. As a result, among 16 identified monoterpenes, 7 monoterpenes (--α-pinene, (--β-pinene, β-myrcene, d-limonene, γ-terpinene, α-terpinolene and p-cymene constituted more than 60% of total VOCs identified in carrots including “Atomic Red”, “Nantes”, “Cosmic Purple”, “Red Samurai”, “Eregli Black”, “White Satin”, “Parmex” and “Baby Carrot”. Thus, these cultivars may advise to carrot breeders due to the beneficial effects of terpenes, especially monoterpenes on health.

  12. Determination of roasted pistachio (Pistacia vera L.) key odorants by headspace solid-phase microextraction and gas chromatography-olfactometry.

    Science.gov (United States)

    Aceña, Laura; Vera, Luciano; Guasch, Josep; Busto, Olga; Mestres, Montserrat

    2011-03-23

    Key odorants in roasted pistachio nuts have been determined for the first time. Two different pistachio varieties (Fandooghi and Kerman) have been analyzed by means of headspace solid-phase microextraction (HS-SPME) and gas chromatography-olfactometry (GCO). The aroma extract dilution analyses (AEDA) applied have revealed 46 and 41 odor-active regions with a flavor dilution (FD) factor≥64 for the Fandooghi and the Kerman varieties, respectively, and 39 of them were related to precisely identified compounds. These included esters, pyrazines, aldehydes, acids, furans, and phenols. The results show that the Fandooghi variety presents, not only more odor-active regions but also higher FD factors than the Kerman variety that can lead to the conclusion that the first variety has a richer aromatic profile than the second one. The descriptive sensory analysis (DSA) showed that the roasted, chocolate/coffee, and nutty attributes were rated significantly higher in the Fandooghi variety, whereas the green attribute was significantly higher in the Kerman one.

  13. Results of Vapor Space Monitoring of Flammable Gas Watch List Tanks

    Energy Technology Data Exchange (ETDEWEB)

    MCCAIN, D.J.

    2000-09-27

    This report documents the measurement of headspace gas concentrations and monitoring results from the Hanford tanks that have continuous flammable gas monitoring. The systems used to monitor the tanks are Standard Hydrogen Monitoring Systems. Further characterization of the tank off-gases was done with Gas Characterization systems and vapor grab samples. The background concentrations of all tanks are below the action level of 6250 ppm. Other information which can be derived from the measurements (such as generation rate, released rate, and ventilation rate) is also discussed.

  14. Results of vapor space monitoring of flammable gas Watch List tanks

    International Nuclear Information System (INIS)

    Wilkins, N.E.

    1997-01-01

    This report documents the measurement of headspace gas concentrations and monitoring results from the Hanford tanks that have continuous flammable gas monitoring. The systems used to monitor the tanks are Standard Hydrogen Monitoring Systems. Further characterization of the tank off-gases was done with Gas Characterization Systems and vapor grab samples. The background concentrations of all tanks are below the action level of 6250 ppm. Other information which can be derived from the measurements (such as generation rate, release rate, and ventilation rate) is also discussed

  15. 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.

  16. Determination of transformation products of unsymmetrical dimethylhydrazine in water using vacuum-assisted headspace solid-phase microextraction.

    Science.gov (United States)

    Orazbayeva, Dina; Kenessov, Bulat; Psillakis, Elefteria; Nassyrova, Dayana; Bektassov, Marat

    2018-06-22

    A new, sensitive and simple method based on vacuum-assisted headspace solid-phase microextraction (Vac-HSSPME) followed by gas chromatography-mass-spectrometry (GC-MS), is proposed for the quantification of rocket fuel unsymmetrical dimethylhydrazine (UDMH) transformation products in water samples. The target transformation products were: pyrazine, 1-methyl-1H-pyrazole, N-nitrosodimethylamine, N,N-dimethylformamide, 1-methyl-1Н-1,2,4-triazole, 1-methyl-imidazole and 1H-pyrazole. For these analytes and within shorter sampling times, Vac-HSSPME yielded detection limits (0.5-100 ng L -1 ) 3-10 times lower than those reported for regular HSSPME. Vac-HSSPME sampling for 30 min at 50 °C yielded the best combination of analyte responses and their standard deviations (24 h). Finally, multiple Vac-HSSME proved to be an efficient tool for controlling the matrix effect and quantifying UDMH transformation products. Copyright © 2018 Elsevier B.V. All rights reserved.

  17. Scientific guidelines for preservation of samples collected from Mars

    International Nuclear Information System (INIS)

    Gooding, J.L.

    1990-04-01

    The maximum scientific value of Martian geologic and atmospheric samples is retained when the samples are preserved in the conditions that applied prior to their collection. Any sample degradation equates to loss of information. Based on detailed review of pertinent scientific literature, and advice from experts in planetary sample analysis, number values are recommended for key parameters in the environmental control of collected samples with respect to material contamination, temperature, head-space gas pressure, ionizing radiation, magnetic fields, and acceleration/shock. Parametric values recommended for the most sensitive geologic samples should also be adequate to preserve any biogenic compounds or exobiological relics

  18. Determination of N-vinyl-2-pyrrolidone and N-methyl-2-pyrrolidone in drugs using polypyrrole-based headspace solid-phase microextraction and gas chromatography-nitrogen-phosphorous detection.

    Science.gov (United States)

    Mehdinia, Ali; Ghassempour, Alireza; Rafati, Hasan; Heydari, Rouhollah

    2007-03-21

    A headspace solid-phase microextraction and gas chromatography-nitrogen-phosphorous detection (HS-SPME-GC-NPD) method using polypyrrole (PPy) fibers has been introduced to determine two derivatives of pyrrolidone; N-vinyl-2-pyrrolidone (NVP) and N-methyl-2-pyrrolidone (NMP). Two types of PPy fibers, prepared using organic and aqueous media, were compared in terms of extraction efficiency and thermal stability. It was found that PPy film prepared using organic medium (i.e. acetonitrile) had higher extraction efficiency and more thermal stability compared to the film prepared in aqueous medium. To enhance the sensitivity of HS-SPME, the effects of pH, ionic strength, extraction time, extraction temperature and the headspace volume on the extraction efficiency were optimized. Using the results of this research, high sensitivity and selectivity had been achieved due to the combination of the high extraction efficiency of PPy film prepared in organic medium and the high sensitivity and selectivity of nitrogen-phosphorous detection. Linear range of the analytes was found to be between 1.0 and 1000 microg L(-1) with regression coefficients (R(2)) of 0.998 and 0.997 for NVP and NMP, consequently. Limits of detection (LODs) were 0.074 and 0.081 microg L(-1) for NVP and NMP, respectively. Relative standard deviation (R.S.D.) for five replications of analyses was found to be less than 6.0%. In real samples the mean recoveries were 94.81% and 94.15% for NVP and NMP, respectively. The results demonstrated the suitability of the HS-SPME technique for analyzing NVP and NMP in two different pharmaceutical matrices. In addition, the method was used for simultaneous detection of NVP, 2-pyrrolidone (2-Pyr), gamma-butyrolactone (GBL) and ethanolamine (EA) compounds.

  19. Rapid analysis of Fructus forsythiae essential oil by ionic liquids-assisted microwave distillation coupled with headspace single-drop microextraction followed by gas chromatography–mass spectrometry

    International Nuclear Information System (INIS)

    Jiao, Jiao; Ma, Dan-Hui; Gai, Qing-Yan; Wang, Wei; Luo, Meng; Fu, Yu-Jie; Ma, Wei

    2013-01-01

    Graphical abstract: -- Highlights: •A new ILAMD-HS-SDME method is developed for the microextraction of essential oil. •ILs used as destruction agent of plant cell walls and microwave absorption medium. •Parameters affecting the extraction efficiency are optimized by Box–Behnken design. •Procedure benefits: similar constituents, shorter duration and smaller sample amount. •ILAMD-HS-SDME followed by GC–MS is a promising technique in analytical fields. -- Abstract: A rapid, green and effective miniaturized sample preparation and analytical technique, i.e. ionic liquids-assisted microwave distillation coupled with headspace single-drop microextraction (ILAMD-HS-SDME) followed by gas chromatography–mass spectrometry (GC–MS) was developed for the analysis of essential oil (EO) in Fructus forsythiae. In this work, ionic liquids (ILs) were not only used as the absorption medium of microwave irradiation but also as the destruction agent of plant cell walls. 1-Ethyl-3-methylimidazolium acetate ([C 2 mim]OAc) was chosen as the optimal ILs. Moreover, n-heptadecane (2.0 μL) was selected as the appropriate suspended solvent for the extraction and concentration of EO. Extraction conditions of the proposed method were optimized using the relative peak area of EO constituents as the index, and the optimal operational parameters were obtained as follows: irradiation power (300 W), sample mass (0.7 g), mass ratio of ILs to sample (2.4), temperature (78 °C) and time (3.4 min). In comparison to previous reports, the proposed method was faster and required smaller sample amount but could equally monitor all EO constituents with no significant differences

  20. Rapid analysis of Fructus forsythiae essential oil by ionic liquids-assisted microwave distillation coupled with headspace single-drop microextraction followed by gas chromatography–mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Jiao, Jiao [State Key Laboratory of Tree Genetics and Breeding, Northeast Forestry University, Harbin 150040 (China); Ma, Dan-Hui [College of Life Sciences, Northeast Forestry University, Harbin 150040 (China); Gai, Qing-Yan; Wang, Wei; Luo, Meng [State Engineering Laboratory of Bio-Resource Eco-Utilization, Northeast Forestry University, Harbin 150040 (China); Fu, Yu-Jie, E-mail: yujie_fu2002@yahoo.com [State Engineering Laboratory of Bio-Resource Eco-Utilization, Northeast Forestry University, Harbin 150040 (China); Ma, Wei, E-mail: mawei@hljucm.net [State Key Laboratory of Tree Genetics and Breeding, Northeast Forestry University, Harbin 150040 (China); School of Pharmaceutical, Heilongjiang University of Chinese Medicine, Harbin 150040 (China)

    2013-12-04

    Graphical abstract: -- Highlights: •A new ILAMD-HS-SDME method is developed for the microextraction of essential oil. •ILs used as destruction agent of plant cell walls and microwave absorption medium. •Parameters affecting the extraction efficiency are optimized by Box–Behnken design. •Procedure benefits: similar constituents, shorter duration and smaller sample amount. •ILAMD-HS-SDME followed by GC–MS is a promising technique in analytical fields. -- Abstract: A rapid, green and effective miniaturized sample preparation and analytical technique, i.e. ionic liquids-assisted microwave distillation coupled with headspace single-drop microextraction (ILAMD-HS-SDME) followed by gas chromatography–mass spectrometry (GC–MS) was developed for the analysis of essential oil (EO) in Fructus forsythiae. In this work, ionic liquids (ILs) were not only used as the absorption medium of microwave irradiation but also as the destruction agent of plant cell walls. 1-Ethyl-3-methylimidazolium acetate ([C{sub 2}mim]OAc) was chosen as the optimal ILs. Moreover, n-heptadecane (2.0 μL) was selected as the appropriate suspended solvent for the extraction and concentration of EO. Extraction conditions of the proposed method were optimized using the relative peak area of EO constituents as the index, and the optimal operational parameters were obtained as follows: irradiation power (300 W), sample mass (0.7 g), mass ratio of ILs to sample (2.4), temperature (78 °C) and time (3.4 min). In comparison to previous reports, the proposed method was faster and required smaller sample amount but could equally monitor all EO constituents with no significant differences.

  1. Method detection limit determination and application of a convenient headspace analysis method for methyl tert-butyl ether in water.

    Science.gov (United States)

    O'Neill, Dennis T; Rochette, Elizabeth A; Ramsey, Philip J

    2002-11-15

    Methyl tert-butyl ether (MTBE) is a common groundwater contaminant, introduced to the environment by leaking petroleum storage tanks, urban runoff, and motorized watercraft. In this study. a simplified (static) headspace analysis method was adapted for determination of MTBE in water samples and soil water extracts. The MDL of the headspace method was calculated to be 2.0 microg L(-1) by the EPA single-concentration design method(1) and 1.2 microg L(-1) by a calibration method developed by Hubaux and Vos (Hubaux, A.; Vos, G. Anal. Chem. 1970,42, 849-855). The MDL calculated with the Hubaux and Vos method was favored because it considers both a true positive and a false positive. The static headspace method was applied to analysis of a tap water sample and a monitoring well sample from a gasoline service station, a river sample, and aqueous extracts from soil excavated during removal of a leaking underground storage tank (LUST). The water samples examined in this study had MTTBE concentrations ranging from 6 to 19 microg L(-1). Aqueous extracts of a soil sample taken from the LUST site had 8 microg L(-1) MTBE.

  2. Orthogonal Design Study on Factors Affecting the Determination of Common Odors in Water Samples by Headspace Solid-Phase Microextraction Coupled to GC/MS

    Directory of Open Access Journals (Sweden)

    Shifu Peng

    2013-01-01

    Full Text Available Geosmin and 2-MIB are responsible for the majority of earthy and musty events related to the drinking water. These two odorants have extremely low odor threshold concentrations at ng L−1 level in the water, so a simple and sensitive method for the analysis of such trace levels was developed by headspace solid-phase microextraction coupled to gas chromatography/mass spectrometry. In this study, the orthogonal experiment design L32 (49 was applied to arrange and optimize experimental conditions. The optimum was the following: temperatures of extraction and desorption, 65°C and 260°C, respectively; times of extraction and desorption, 30 min and 5 min, respectively; ionic strength, 25% (w/v; rotate-speed, 600 rpm; solution pH, 5.0. Under the optimized conditions, limits of detection (S/N=3 were 0.04 and 0.13 ng L−1 for geosmin and 2-MIB, respectively. Calculated calibration curves gave high levels of linearity with a correlation coefficient value of 0.9999 for them. Finally, the proposed method was applied to water samples, which were previously analyzed and confirmed to be free of target analytes. Besides, the proposal method was applied to test environmental water samples. The RSDs were 2.75%~3.80% and 4.35%~7.6% for geosmin and 2-MIB, respectively, and the recoveries were 91%~107% and 91%~104% for geosmin and 2-MIB, respectively.

  3. Determination of ammonium in aqueous samples using new headspace dynamic in-syringe liquid-phase microextraction with in situ derivitazation coupled with liquid chromatography-fluorescence detection.

    Science.gov (United States)

    Muniraj, Sarangapani; Yan, Cheing-Tong; Shih, Hou-Kung; Ponnusamy, Vinoth Kumar; Jen, Jen-Fon

    2012-11-19

    A new simultaneous derivatization and extraction method for the preconcentration of ammonia using new one-step headspace dynamic in-syringe liquid-phase microextraction with in situ derivatization was developed for the trace determination of ammonium in aqueous samples by liquid chromatography with fluorescence detection (LC-FLD). The acceptor phase (as derivatization reagent) containing o-phthaldehyde and sodium sulfite was held within a syringe barrel and immersed in the headspace of sample container. The gaseous ammonia from the alkalized aqueous sample formed a stable isoindole derivative with the acceptor phase inside the syringe barrel through the reciprocated movements of plunger. After derivatization-cum-extraction, the acceptor phase was directly injected into LC-FLD for analysis. Parameters affecting the ammonia evolution and the extraction/derivatization efficiency such as sample matrix, pH, temperature, sampling time, and the composition of derivatization reagent, reaction temperature, and frequency of reciprocated plunger, were studied thoroughly. Results indicated that the maximum extraction efficiency was obtained by using 100μL derivatization reagent in a 1-mL gastight syringe under 8 reciprocated movements of plunger per min to extract ammonia evolved from a 20mL alkalized aqueous solution at 70°C (preheated 4min) with 380rpm stirring for 8min. The detection was linear in the concentration range of 0.625-10μM with the correlation coefficient of 0.9967 and detection limit of 0.33μM (5.6ng mL(-1)) based on SN(-1)=3. The method was applied successfully to determine ammonium in real water samples without any prior cleanup of the samples, and has been proved to be a simple, sensitive, efficient and cost-effective procedure for trace ammonium determination in aqueous samples. Copyright © 2012 Elsevier B.V. All rights reserved.

  4. [The elaboration of gas chromatographic method of the determination of N-nitrosamines (N-nitrosodimethylamine, N-nitrosodiethylamine) in biological samples (urine)].

    Science.gov (United States)

    Zaytseva, N V; Ulanova, T S; Nurislamova, T V; Popova, N A

    2014-01-01

    The issues of the elaboration of a method for the determination of N-nitrosamines (N-nitrosodimethylamine, N-nitrosodiethylamine) in urine by means of the method of capillary gas chromatography with the use of a thermionic detector are considered. There were performed investigations on the study of the efficacy of the extraction of N-nitrosamines from the urine by steam distillation and gas chromatographic detection of headspace. With the aim of the maximal recovery of N-nitrosamines from the urine and setting parameters of the extraction two method were used to prepare the bioassay for the analysis the alkalization with potassium hydroxide and the addition of salting out reagent--neutral salts of alkali and alkaline earth metals. During the process of performed studies there was found that the greatest degree of extraction of N-nitrosamines from the urine by the method of headspace analysis is achieved if using the salting-out agent in an amount of 16 g of sodium sulfate and for N-nitrosodimethylamine is 99%, for N-nitrosodiethylamine--100%.

  5. Retained Gas Sampling Results for the Flammable Gas Program

    International Nuclear Information System (INIS)

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

    1999-01-01

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

  6. Retained Gas Sampling Results for the Flammable Gas Program

    Energy Technology Data Exchange (ETDEWEB)

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

    1999-11-18

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

  7. Novel polyamide-based nanofibers prepared by electrospinning technique for headspace solid-phase microextraction of phenol and chlorophenols from environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Bagheri, Habib, E-mail: bagheri@sharif.edu [Environmental and Bio-Analytical Laboratories, Department of Chemistry, Sharif University of Technology, Azadi Av., P.O. Box 11365-9516, Tehran (Iran, Islamic Republic of); Aghakhani, Ali; Baghernejad, Masoud; Akbarinejad, Alireza [Environmental and Bio-Analytical Laboratories, Department of Chemistry, Sharif University of Technology, Azadi Av., P.O. Box 11365-9516, Tehran (Iran, Islamic Republic of)

    2012-02-24

    A novel solid phase microextraction (SPME) fiber was fabricated by electrospinning method in which a polymeric solution was converted to nanofibers using high voltages. A thin stainless steel wire was coated by the network of polymeric nanofibers. The polymeric nanofiber coating on the wire was mechanically stable due to the fine and continuous nanofibers formation around the wire with a three dimensional structure. Polyamide (nylon 6), due to its suitable characteristics was used to prepare the unbreakable SPME nanofiber. The scanning electron microscopy (SEM) images of this new coating showed a diameter range of 100-200 nm for polyamide nanofibers with a homogeneous and porous surface structure. The extraction efficiency of new coating was investigated for headspace solid-phase microextraction (HS-SPME) of some environmentally important chlorophenols from aqueous samples followed by gas chromatography-mass spectrometry (GC-MS) analysis. Effect of different parameters influencing the extraction efficiency including extraction temperature, extraction time, ionic strength and polyamide amount were investigated and optimized. In order to improve the chromatographic behavior of phenolic compounds, all the analytes were derivatized prior to the extraction process using basic acetic anhydride. The detection limits of the method under optimized conditions were in the range of 2-10 ng L{sup -1}. The relative standard deviations (RSD) (n = 3) at the concentration level of 1.7-6.7 ng mL{sup -1} were obtained between 1 and 7.4%. The calibration curves of chlorophenols showed linearity in the range of 27-1330 ng L{sup -1} for phenol and monochlorophenols and 7-1000 ng L{sup -1} for dichloro and trichlorophenols. Also, the proposed method was successfully applied to the extraction of phenol and chlorophenols from real water samples and relative recoveries were between 84 and 98% for all the selected analytes except for 2,4,6 tricholophenol which was between 72 and 74%.

  8. The utilisation of two detectors for the determination of water in honey using headspace gas chromatography.

    Science.gov (United States)

    Frink, Lillian A; Armstrong, Daniel W

    2016-08-15

    A headspace gas chromatography (HSGC) method was developed for the determination of water content in honey. This method was shown to work with five different honey varieties which had a range of water from 14-16%. It also utilised two different detectors, the thermal conductivity detector (TCD) and the barrier discharge ionisation detector (BID). This method needs no heating pretreatment step as in the current leading method, (i.e. the measurement of refractive index). The solvent-free procedure negates the possibility of solvent-compound interactions as well as solubility limitations, as is common with Karl Fischer titrations. It was also apparent that the classic loss on drying method consistently and substantially produced results that were lower than the correct values. This approach is shown to be rapid, with an analysis time of 4 min when using the TCD detector and under 3 min when utilising the BID detector. HSGC is feasible for the determination of water due to the new PEG-linked geminal dicationic ionic-liquid-coated GC capillary column. In addition it provides accurate and precise determinations of the water content in honey. When using the sensitive BID detector, other trace volatile compounds are observed as well. Copyright © 2016 Elsevier Ltd. All rights reserved.

  9. Fabrication of novel nanoporous array anodic alumina solid-phase microextraction fiber coating and its potential application for headspace sampling of biological volatile organic compounds

    International Nuclear Information System (INIS)

    Zhang Zhuomin; Wang Qingtang; Li Gongke

    2012-01-01

    Highlights: ► Nanoporous array anodic alumina (NAAA) SPME coating was originally prepared. ► NAAA SPME coating achieved excellent enrichment capability and selectivity for VOCs. ► NAAA SPME coating can be applied for the headspace sampling of biological VOCs. - Abstract: In the study, nanoporous array anodic alumina (NAAA) prepared by a simple, rapid and stable two-step anodic oxidization method was introduced as a novel solid-phase microextraction (SPME) fiber coating. The regular nanoporous array structure and chemical composition of NAAA SPME fiber coating was characterized and validated by scanning electron microscopy and energy dispersive spectroscopy, respectively. Compared with the commercial polydimethylsiloxane (PDMS) SPME fiber coating, NAAA SPME fiber coating achieved the higher enrichment capability (1.7–4.7 folds) for the mixed standards of volatile organic compounds (VOCs). The selectivity for volatile alcohols by NAAA SPME fiber coating demonstrated an increasing trend with the increasing polarity of alcohols caused by the gradually shortening carbon chains from 1-undecanol to 1-heptanol or the isomerization of carbon chains of some typical volatile alcohols including 2-ethyl hexanol, 1-octanol, 2-phenylethanol, 1-phenylethanol, 5-undecanol, 2-undecanol and 1-undecanol. Finally, NAAA SPME fiber coating was originally applied for the analysis of biological VOCs of Bailan flower, stinkbug and orange peel samples coupled with gas chromatography–mass spectrometry (GC–MS) detection. Thirty, twenty-seven and forty-four VOCs of Bailan flower, stinkbug and orange peel samples were sampled and identified, respectively. Moreover, the contents of trace 1-octanol and nonanal of real orange peel samples were quantified for the further method validation with satisfactory recoveries of 106.5 and 120.5%, respectively. This work proposed a sensitive, rapid, reliable and convenient analytical method for the potential study of trace and small molecular

  10. Fabrication of novel nanoporous array anodic alumina solid-phase microextraction fiber coating and its potential application for headspace sampling of biological volatile organic compounds

    Energy Technology Data Exchange (ETDEWEB)

    Zhang Zhuomin [School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangzhou 510275 (China); Wang Qingtang [Key Laboratory of Analysis and Detection for Food Safety of Ministry of Education, College of Chemistry and Chemical Engineering, Fuzhou University, Fuzhou, Fujian 350002 (China); Li Gongke, E-mail: cesgkl@mail.sysu.edu.cn [School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangzhou 510275 (China)

    2012-05-21

    Highlights: Black-Right-Pointing-Pointer Nanoporous array anodic alumina (NAAA) SPME coating was originally prepared. Black-Right-Pointing-Pointer NAAA SPME coating achieved excellent enrichment capability and selectivity for VOCs. Black-Right-Pointing-Pointer NAAA SPME coating can be applied for the headspace sampling of biological VOCs. - Abstract: In the study, nanoporous array anodic alumina (NAAA) prepared by a simple, rapid and stable two-step anodic oxidization method was introduced as a novel solid-phase microextraction (SPME) fiber coating. The regular nanoporous array structure and chemical composition of NAAA SPME fiber coating was characterized and validated by scanning electron microscopy and energy dispersive spectroscopy, respectively. Compared with the commercial polydimethylsiloxane (PDMS) SPME fiber coating, NAAA SPME fiber coating achieved the higher enrichment capability (1.7-4.7 folds) for the mixed standards of volatile organic compounds (VOCs). The selectivity for volatile alcohols by NAAA SPME fiber coating demonstrated an increasing trend with the increasing polarity of alcohols caused by the gradually shortening carbon chains from 1-undecanol to 1-heptanol or the isomerization of carbon chains of some typical volatile alcohols including 2-ethyl hexanol, 1-octanol, 2-phenylethanol, 1-phenylethanol, 5-undecanol, 2-undecanol and 1-undecanol. Finally, NAAA SPME fiber coating was originally applied for the analysis of biological VOCs of Bailan flower, stinkbug and orange peel samples coupled with gas chromatography-mass spectrometry (GC-MS) detection. Thirty, twenty-seven and forty-four VOCs of Bailan flower, stinkbug and orange peel samples were sampled and identified, respectively. Moreover, the contents of trace 1-octanol and nonanal of real orange peel samples were quantified for the further method validation with satisfactory recoveries of 106.5 and 120.5%, respectively. This work proposed a sensitive, rapid, reliable and convenient

  11. Application of headspace for research volatile organic compounds emitted from building materials

    Directory of Open Access Journals (Sweden)

    Kultys Beata

    2018-01-01

    Full Text Available Headspace technique and gas chromatography method with mas detector has been used for the determination of volatile organic compounds (VOC emitted from various building and finishing materials, such as sealing foams, mounting strips, paints, varnishes, floor coverings. The tests were carried out for different temperatures (in the temperature range of 60 to 180 °C and the time of heated vials with tested materials inside. These tests were conducted to verify the possibility of use this method of determination the VOC emission. Interpretation of chromatograms and mass spectra allowed to identify the type of compounds emitted from the tested materials and the optimum time and temperature for each type of material was determined. The increase in heating temperature of the samples resulted in increase the type and number of identified compounds: for four materials the increase was in the whole temperature range, for others it was from 90 °C. On the other hand, emission from mineral wool was low in whole temperature range. 30-minutes heating of the samples was sufficient to identify emitted compounds for most of tested materials. Applying a longer time, i.e. 24 hours, significantly increased the sensitivity of the method.

  12. Multi-volatile method for aroma analysis using sequential dynamic headspace sampling with an application to brewed coffee.

    Science.gov (United States)

    Ochiai, Nobuo; Tsunokawa, Jun; Sasamoto, Kikuo; Hoffmann, Andreas

    2014-12-05

    A novel multi-volatile method (MVM) using sequential dynamic headspace (DHS) sampling for analysis of aroma compounds in aqueous sample was developed. The MVM consists of three different DHS method parameters sets including choice of the replaceable adsorbent trap. The first DHS sampling at 25 °C using a carbon-based adsorbent trap targets very volatile solutes with high vapor pressure (>20 kPa). The second DHS sampling at 25 °C using the same type of carbon-based adsorbent trap targets volatile solutes with moderate vapor pressure (1-20 kPa). The third DHS sampling using a Tenax TA trap at 80 °C targets solutes with low vapor pressure (0.9910) and high sensitivity (limit of detection: 1.0-7.5 ng mL(-1)) even with MS scan mode. The feasibility and benefit of the method was demonstrated with analysis of a wide variety of aroma compounds in brewed coffee. Ten potent aroma compounds from top-note to base-note (acetaldehyde, 2,3-butanedione, 4-ethyl guaiacol, furaneol, guaiacol, 3-methyl butanal, 2,3-pentanedione, 2,3,5-trimethyl pyrazine, vanillin, and 4-vinyl guaiacol) could be identified together with an additional 72 aroma compounds. Thirty compounds including 9 potent aroma compounds were quantified in the range of 74-4300 ng mL(-1) (RSD<10%, n=5). Copyright © 2014 The Authors. Published by Elsevier B.V. All rights reserved.

  13. Generation of sub-part-per-billion gaseous volatile organic compounds at ambient temperature by headspace diffusion of aqueous standards through decoupling between ideal and nonideal Henry's law behavior.

    Science.gov (United States)

    Kim, Yong-Hyun; Kim, Ki-Hyun

    2013-05-21

    In the analysis of volatile organic compounds in air, the preparation of their gaseous standards at low (sub-ppb) concentration levels with high reliability is quite difficult. In this study, a simple dynamic headspace-based approach was evaluated as a means of generating vapor-phase volatile organic compounds from a liquid standard in an impinger at ambient temperature (25 °C). For a given sampling time, volatile organic compound vapor formed in the headspace was swept by bypassing the sweep gas through the impinger and collected four times in quick succession in separate sorbent tubes. In each experiment, a fresh liquid sample was used for each of the four sampling times (5, 10, 20, and 30 min) at a steady flow rate of 50 mL min(-1). The air-water partitioning at the most dynamic (earliest) sweeping stage was established initially in accord with ideal Henry's law, which was then followed by considerably reduced partitioning in a steady-state equilibrium (non-ideal Henry's law). The concentrations of gaseous volatile organic compounds, collected after the steady-state equilibrium, reached fairly constant values: for instance, the mole fraction of toluene measured at a sweeping interval of 10 and 30 min averaged 1.10 and 0.99 nmol mol(-1), respectively (after the initial 10 min sampling). In the second stage of our experiment, the effect of increasing the concentrations of liquid spiking standard was also examined by collecting sweep gas samples from two consecutive 10 min runs. The volatile organic compounds, collected in the first and second 10 min sweep gas samples, exhibited ideal and nonideal Henry's law behavior, respectively. From this observation, we established numerical relationships to predict the mole fraction (or mixing ratio) of each volatile organic compound in steady-state equilibrium in relation to the concentration of standard spiked into the system. This experimental approach can thus be used to produce sub-ppb levels of gaseous volatile organic

  14. Headspace solid-phase microextraction (HS-SPME) and liquid-liquid extraction (LLE): comparison of the performance in classification of ecstasy tablets. Part 2.

    Science.gov (United States)

    Bonadio, Federica; Margot, Pierre; Delémont, Olivier; Esseiva, Pierre

    2008-11-20

    Headspace solid-phase microextraction (HS-SPME) is assessed as an alternative to liquid-liquid extraction (LLE) currently used for 3,4-methylenedioxymethampethamine (MDMA) profiling. Both methods were compared evaluating their performance in discriminating and classifying samples. For this purpose 62 different seizures were analysed using both extraction techniques followed by gas chromatography-mass spectroscopy (GC-MS). A previously validated method provided data for HS-SPME, whereas LLE data were collected applying a harmonized methodology developed and used in the European project CHAMP. After suitable pre-treatment, similarities between sample pairs were studied using the Pearson correlation. Both methods enable to distinguish between samples coming from the same pre-tabletting batches and samples coming from different pre-tabletting batches. This finding emphasizes the use of HS-SPME as an effective alternative to LLE, with additional advantages such as sample preparation and a solvent-free process.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2008-06-09

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

  16. EVIDENCE OF CORROSIVE GAS FORMED BY RADIOLYSIS OF CHLORIDE SALTS IN PLUTONIUM-BEARING MATERIALS

    Energy Technology Data Exchange (ETDEWEB)

    Dunn, K.; Louthan, M.

    2010-02-01

    Corrosion and pitting have been observed in headspace regions of stainless steel containers enclosing plutonium oxide/salt mixtures. These observations are consistent with the formation of a corrosive gas, probably HCl, and transport of that gas to the headspace regions of sealed containers. The NH{sub 4}Cl films found on the walls of the sealed containers is also indicative of the presence of HCl gas. Radiolysis of hydrated alkaline earth salts is the probable source of HCl.

  17. Sea Ice as a Sink for CO2 and Biogeochemical Material: a Novel Sampling Method and Astrobiological Applications

    Science.gov (United States)

    Wilner, J.; Hofmann, A.; Hand, K. P.

    2017-12-01

    Accurately modelling the intensification of greenhouse gas effects in the polar regions ("polar amplification") necessitates a thorough understanding of the geochemical balance between atmospheric, sea ice, and oceanic layers. Sea ice is highly permeable to CO2 and therefore represents a major sink of oceanic CO2 in winter and of atmospheric CO2 in summer, sinks that are typically either poorly constrained in or fully absent from global climate models. We present a novel method for sampling both trapped and dissolved gases (CO2, CH4 and δ13CH4) in sea ice with a Picarro 2132-i Methane Analyzer, taking the following sampling considerations into account: minimization of water and air contamination, full headspace sampling, prevention of inadvertent sample bag double-puncturing, and ease of use. This method involves melting of vacuum-sealed ice cores to evacuate trapped gases to the headspace and sampling the headspace gas with a blunt needle sheathed by a beveled puncturing needle. A gravity catchment tube prevents input of dangerous levels of liquid water to the Picarro cavity. Subsequent ultrasonic degassing allows for dissolved gas measurement. We are in the process of using this method to sample gases trapped and dissolved in Arctic autumn sea ice cores and atmospheric samples collected during the 2016 Polarstern Expedition and during a May 2017 field campaign north of Barrow, Alaska. We additionally employ this method, together with inductively coupled plasma mass spectrometry (ICP-MS), to analyze the transfer of potential biogeochemical signatures of underlying hydrothermal plumes to sea ice. This has particular relevance to Europa and Enceladus, where hypothetical hydrothermal plumes may deliver seafloor chemicals to the overlying ice shell. Hence, we are presently investigating the entrainment of methane and other hydrothermal material in sea ice cores collected along the Gakkel Ridge that may serve as biosignatures of methanogenic organisms in seafloor

  18. Expanding the use of polymeric ionic liquids in headspace solid-phase microextraction: Determination of ultraviolet filters in water samples.

    Science.gov (United States)

    Trujillo-Rodríguez, María J; Nan, He; Anderson, Jared L

    2018-03-09

    Three crosslinked polymeric ionic liquid (PIL) sorbent coatings were used in headspace solid-phase microextraction for the determination of a group of ultraviolet filters. The developed crosslinked PIL-based materials include two polycations and a double confined PIL. The method, in combination with gas chromatography-mass spectrometry, is simple, solvent free, and does not require of any derivatization step. After proper optimization of the methodologies with each developed fiber, the analytical performance was compared with a commercial polyacrylate fiber. A study of the normalized calibration slopes, obtained by dividing the calibration slope of each analyte by the coating volume, revealed that the crosslinked fibers can be used as alternatives to commercial fibers for the determination of the selected group of compounds. In particular, the coating nature of the PIL containing the 1-vinylbenzyl-3-hexadecylimidazolium bis[(trifluoromethyl)sulfonyl]imide IL as monomer and the 1,12-di(3-vinylbenzylimidazolium)dodecane bis[(trifluoromethyl)sulfonyl]imide IL as crosslinker is the most suitable for the extraction of the selected compounds despite their coating volume, being 3.6 times lower than the commercial polyacrylate fiber. For this fiber, wide linear ranges, correlation coefficients higher than 0.990, limits of detection ranging from 2.8 ng L -1 to 26 ng L -1 and relative standard deviations ranging from 2.5 to 15% were achieved. Finally, all proposed PIL-based fibers were applied towards the analysis of tap water, pool water and lake water, with the majority of the ultraviolet filters being detected and quantified in the last two types of samples. Copyright © 2018 Elsevier B.V. All rights reserved.

  19. Waste tank vapor project: Vapor space characterization of waste tank 241-BY-104: Results from samples collected on June 24, 1994

    International Nuclear Information System (INIS)

    Clauss, T.W.; Ligotke, M.W.; McVeety, B.D.; Pool, K.H.; Lucke, R.B.; Fruchter, J.S.; Goheen, S.C.

    1994-11-01

    This report describes results of the analyses of tank-headspace samples taken from Hanford waste Tank 241-BY-104 (referred to as Tank BY-104) on June 24, 1994. The Pacific Northwest Laboratory (PNL) contracted with Westinghouse Hanford Company (WHC) to provide sampling devices and analyze inorganic and organic samples collected from the tank headspace. The sample job was designated S4019 and was performed by WHC on June 24, 1994 using the vapor sampling system (VSS). The results of the analyses are expected to be used in the determination of safety and toxicological issues related to the tank-headspace gas as described in the WHC report entitled Data Quality Objectives for Generic In-Tank Health and Safety Vapor Issue Resolution, WHC-SD-WM-DQO-002, Rev. 0. Sampling devices, including 16 sorbent trains (for inorganic analyses), and 5 SUMMA trademark canisters (for organic analyses), were supplied to the WHC sampling staff on June 20, 1994. Samples were taken (by WHC) on June 24. The samples were returned from the field on June 27. The inorganic samples delivered to PNL on chain-of-custody (COC) 006893 included 16 sorbent trains as described in Tables 2.2, 2.3, and 2.4. Additional inorganic blank spikes were obtained from related sample jobs. SUMMA trademark samples delivered to PNL on COC 006896 included one ambient air sample, one ambient-air sample through the sampling system, and three tank-headspace SUMMA trademark canister samples. The samples were inspected upon delivery to the 326/23B laboratory and logged into PNL laboratory record book 55408. Custody of the sorbent trains was transferred to PNL personnel performing the inorganic analysis and stored at refrigerated (≤10 degrees C) temperature until the time of analysis. Access to the 326/23B laboratory is limited to PNL personnel working on the waste-tank safety program

  20. Subsurface Noble Gas Sampling Manual

    Energy Technology Data Exchange (ETDEWEB)

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

    2017-09-18

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

  1. Soil Gas Sampling

    Science.gov (United States)

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

  2. Discrimination of bacteria by rapid sensing their metabolic volatiles using an aspiration-type ion mobility spectrometer (a-IMS) and gas chromatography-mass spectrometry GC-MS.

    Science.gov (United States)

    Ratiu, Ileana Andreea; Bocos-Bintintan, Victor; Patrut, Adrian; Moll, Victor Hugo; Turner, Matthew; Thomas, C L Paul

    2017-08-22

    The objective of our study was to investigate whether one may quickly and reliably discriminate different microorganism strains by direct monitoring of the headspace atmosphere above their cultures. Headspace samples above a series of in vitro bacterial cultures were directly interrogated using an aspiration type ion mobility spectrometer (a-IMS), which produced distinct profiles ("fingerprints") of ion currents generated simultaneously by the detectors present inside the ion mobility cell. Data processing and analysis using principal component analysis showed net differences in the responses produced by volatiles emitted by various bacterial strains. Fingerprint assignments were conferred on the basis of product ion mobilities; ions of differing size and mass were deflected in a different degree upon their introduction of a transverse electric field, impacting finally on a series of capacitors (denominated as detectors, or channels) placed in a manner analogous to sensor arrays. Three microorganism strains were investigated - Escherichia coli, Bacillus subtilis and Staphylococcus aureus; all strains possess a relatively low pathogenic character. Samples of air with a 5 cm 3 volume from the headspace above the bacterial cultures in agar growth medium were collected using a gas-tight chromatographic syringe and injected inside the closed-loop pneumatic circuit of the breadboard a-IMS instrument model ChemPro-100i (Environics Oy, Finland), at a distance of about 1 cm from the ionization source. The resulting chemical fingerprints were produced within two seconds from the moment of injection. The sampling protocol involved to taking three replicate samples from each of 10 different cultures for a specific strain, during a total period of 72 h after the initial incubation - at 24, 48 and 72 h, respectively. Principal component analysis (PCA) was used to discriminate between the IMS fingerprints. PCA was found to successfully discriminate between bacteria at three

  3. Comparative analysis of the vapor headspace of military-grade TNT versus NESTT TNT under dynamic and static conditions

    Science.gov (United States)

    Edge, Cindy C.; Gibb, Julie; Wasserzug, Louis S.

    1998-09-01

    The Institute for Biological Detection Systems (IBDS) has developed a quantitative vapor delivery system that can aid in characterizing dog's sensitivity and ability to recognize odor signatures for explosives and contraband substances. Determining of the dog's odor signature for detection of explosives is important because it may aid in eliminating the risk of handling explosives and reducing cross-contamination. Progress is being made in the development of training aids that represent the headspace of the explosives. NESTTTM TNT materials have been proposed as an approach to developing training aid simulates. In order for such aids to be effective they must mimic the headspace of the target material. This study evaluates the NESTTTM TNT product with regard to this criterion. NESTTTM TNT vapor was generated by the IBDS vapor delivery system, which incorporates a vapor generation cell that enables the user to control the conditions under which a substance is tested. The NESTTTM TNT vapor was compared to the headspace of military-grade TNT. The findings identify and quantify major vapor constituents of military-grade TNT and NESTTTM TNT. A comparative analysis evaluated the degree to which the NESTTTM TNT mimics the headspace of an actual TNT sample.

  4. Determination of multi-class herbicides in soil by liquid-solid extraction coupled with headspace solid phase microextraction method

    Directory of Open Access Journals (Sweden)

    Đurović-Pejčev Rada

    2016-01-01

    Full Text Available A method is described for simultaneous determination of five herbicides (metribuzin, acetochlor, clomazone, oxyfluorfen and dimethenamid belonging to different pesticides groups in soil samples. Developed headspace solid phase microextraction method (HS-SPME in combination with liquid-solid sample preparation (LS was optimized and applied in the analysis of some agricultural samples. Optimization of microextraction conditions, such as temperature, extraction time and sodium chloride (NaCl content was perfor-med using 100 μm polydimethyl-siloxane (PDMS fiber. The extraction effi-ciencies of methanol, methanol:acetone=1:1 and methanol:acetone:hexane= =2:2:1 and the optimum number of extraction steps during the sample prepa-ration, were tested, as well. Gas chromatography-mass spectrometry (GC-MS was used for detection and quantification, obtaining relative standard deviation (RSD below 13%, and recovery values higher than 83% for multiple analyses of soil samples fortified at 30 μg kg-1 of each herbicide. Limits of detection (LOD were less than 1.2 μg kg-1 for all the studied herbicides. [Projekat Ministarstva nauke Republike Srbije, br. TR31043 i br. III43005

  5. Novel polyamide-based nanofibers prepared by electrospinning technique for headspace solid-phase microextraction of phenol and chlorophenols from environmental samples

    International Nuclear Information System (INIS)

    Bagheri, Habib; Aghakhani, Ali; Baghernejad, Masoud; Akbarinejad, Alireza

    2012-01-01

    A novel solid phase microextraction (SPME) fiber was fabricated by electrospinning method in which a polymeric solution was converted to nanofibers using high voltages. A thin stainless steel wire was coated by the network of polymeric nanofibers. The polymeric nanofiber coating on the wire was mechanically stable due to the fine and continuous nanofibers formation around the wire with a three dimensional structure. Polyamide (nylon 6), due to its suitable characteristics was used to prepare the unbreakable SPME nanofiber. The scanning electron microscopy (SEM) images of this new coating showed a diameter range of 100–200 nm for polyamide nanofibers with a homogeneous and porous surface structure. The extraction efficiency of new coating was investigated for headspace solid-phase microextraction (HS-SPME) of some environmentally important chlorophenols from aqueous samples followed by gas chromatography–mass spectrometry (GC–MS) analysis. Effect of different parameters influencing the extraction efficiency including extraction temperature, extraction time, ionic strength and polyamide amount were investigated and optimized. In order to improve the chromatographic behavior of phenolic compounds, all the analytes were derivatized prior to the extraction process using basic acetic anhydride. The detection limits of the method under optimized conditions were in the range of 2–10 ng L −1 . The relative standard deviations (RSD) (n = 3) at the concentration level of 1.7–6.7 ng mL −1 were obtained between 1 and 7.4%. The calibration curves of chlorophenols showed linearity in the range of 27–1330 ng L −1 for phenol and monochlorophenols and 7–1000 ng L −1 for dichloro and trichlorophenols. Also, the proposed method was successfully applied to the extraction of phenol and chlorophenols from real water samples and relative recoveries were between 84 and 98% for all the selected analytes except for 2,4,6 tricholophenol which was between 72 and 74%.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-10-31

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

  7. Full evaporation dynamic headspace in combination with selectable one-dimensional/two-dimensional gas chromatography-mass spectrometry for the determination of suspected fragrance allergens in cosmetic products.

    Science.gov (United States)

    Devos, Christophe; Ochiai, Nobuo; Sasamoto, Kikuo; Sandra, Pat; David, Frank

    2012-09-14

    Suspected fragrance allergens were determined in cosmetic products using a combination of full evaporation-dynamic headspace (FEDHS) with selectable one-dimensional/two-dimensional GC-MS. The full evaporation dynamic headspace approach allows the non-discriminating extraction and injection of both apolar and polar fragrance compounds, without contamination of the analytical system by high molecular weight non-volatile matrix compounds. The method can be applied to all classes of cosmetic samples, including water containing matrices such as shower gels or body creams. In combination with selectable (1)D/(2)D GC-MS, consisting of a dedicated heart-cutting GC-MS configuration using capillary flow technology (CFT) and low thermal mass GC (LTM-GC), a highly flexible and easy-to-use analytical solution is offered. Depending on the complexity of the perfume fraction, analyses can be performed in one-dimensional GC-MS mode or in heart-cutting two-dimensional GC-MS mode, without the need of hardware reconfiguration. The two-dimensional mode with independent temperature control of the first and second dimension column is especially useful to confirm the presence of detected allergen compounds when mass spectral deconvolution is not possible. Copyright © 2012 Elsevier B.V. All rights reserved.

  8. Automated Peak Detection and Matching Algorithm for Gas Chromatography–Differential Mobility Spectrometry

    Science.gov (United States)

    Fong, Sim S.; Rearden, Preshious; Kanchagar, Chitra; Sassetti, Christopher; Trevejo, Jose; Brereton, Richard G.

    2013-01-01

    A gas chromatography–differential mobility spectrometer (GC-DMS) involves a portable and selective mass analyzer that may be applied to chemical detection in the field. Existing approaches examine whole profiles and do not attempt to resolve peaks. A new approach for peak detection in the 2D GC-DMS chromatograms is reported. This method is demonstrated on three case studies: a simulated case study; a case study of headspace gas analysis of Mycobacterium tuberculosis (MTb) cultures consisting of three matching GC-DMS and GC-MS chromatograms; a case study consisting of 41 GC-DMS chromatograms of headspace gas analysis of MTb culture and media. PMID:21204557

  9. Australian young people's awareness of headspace, beyondblue and other mental health organizations.

    Science.gov (United States)

    Jorm, Anthony F

    2009-12-01

    Objective: The aim of this paper is to assess young people's awareness of mental health organizations supporting their age group. Of particular interest was awareness of headspace, which was created in 2006 to provide youth-oriented mental health services, and of beyondblue, which aims to raise community awareness of depression, anxiety and related disorders. Method: A telephone survey was carried out on a national sample of young people who were part of a 2-year follow-up study of youth mental health literacy. Data were analysed for those aged 13-25 years. Results: Awareness was highest for beyondblue and telephone helplines; headspace had established some awareness, particularly in areas where its services operate. However, awareness was unrelated to the participant's psychological symptoms in the past year. Conclusions: If youth-oriented services are to be successful, young people need to know about them. Awareness campaigns need to be targeted at the sub-group who have greatest need for these services, namely those with mental health problems.

  10. Determination of volatile organic compounds in water by headspace solid-phase microextraction gas chromatography coupled to tandem mass spectrometry with triple quadrupole analyzer

    International Nuclear Information System (INIS)

    Cervera, M.I.; Beltran, J.; Lopez, F.J.; Hernandez, F.

    2011-01-01

    Highlights: → Employing a statistical optimization improves results reducing experiments. → Use of MS (QqQ) allows high sensitivity determination and improves identification capabilities. → Using Q/q intensity ratios is a powerful tool to ensure compound identification. → HS SPME GC-MS/MS method allows determination of VOCs in complex matrix water samples. - Abstract: In the present work, a rapid method with little sample handling has been developed for determination of 23 selected volatile organic compounds in environmental and wastewater samples. The method is based on headspace solid-phase microextraction (SPME) followed by gas chromatography coupled to tandem mass spectrometry (GC-MS/MS) determination using triple quadrupole analyzer (QqQ) in electron ionization mode. The best conditions for extraction were optimised with a factorial design taking into account the interaction between different parameters and not only individual effects of variables. In the optimized procedure, 4 mL of water sample were extracted using a 10 mL vial and adding 0.4 g NaCl (final NaCl content of 10%). An SPME extraction with carboxen/polydimethylsiloxane 75 μm fiber for 30 min at 50 deg. C (with 5 min of previous equilibration time) with magnetic stirring was applied. Chromatographic determination was carried out by GC-MS/MS working in Selected Reaction Monitoring (SRM) mode. For most analytes, two MS/MS transitions were acquired, although for a few compounds it was difficult to obtain characteristic abundant fragments. In those cases, a pseudo selected reaction monitoring (pseudo-SRM) with three ions was used instead. The intensity ratio between quantitation (Q) and confirmation (q) signals was used as a confirmatory parameter. The method was validated by means of recovery experiments (n = 6) spiking mineral water samples at three concentration levels (0.1, 5 and 50 μg L -1 ). Recoveries between 70% and 120% were generally obtained with relative standard deviations (RSDs

  11. Determination of volatile organic compounds in water by headspace solid-phase microextraction gas chromatography coupled to tandem mass spectrometry with triple quadrupole analyzer

    Energy Technology Data Exchange (ETDEWEB)

    Cervera, M.I. [Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat, E-12071 Castellon (Spain); Beltran, J., E-mail: joaquim.beltran@uji.es [Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat, E-12071 Castellon (Spain); Lopez, F.J.; Hernandez, F. [Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat, E-12071 Castellon (Spain)

    2011-10-17

    Highlights: {yields} Employing a statistical optimization improves results reducing experiments. {yields} Use of MS (QqQ) allows high sensitivity determination and improves identification capabilities. {yields} Using Q/q intensity ratios is a powerful tool to ensure compound identification. {yields} HS SPME GC-MS/MS method allows determination of VOCs in complex matrix water samples. - Abstract: In the present work, a rapid method with little sample handling has been developed for determination of 23 selected volatile organic compounds in environmental and wastewater samples. The method is based on headspace solid-phase microextraction (SPME) followed by gas chromatography coupled to tandem mass spectrometry (GC-MS/MS) determination using triple quadrupole analyzer (QqQ) in electron ionization mode. The best conditions for extraction were optimised with a factorial design taking into account the interaction between different parameters and not only individual effects of variables. In the optimized procedure, 4 mL of water sample were extracted using a 10 mL vial and adding 0.4 g NaCl (final NaCl content of 10%). An SPME extraction with carboxen/polydimethylsiloxane 75 {mu}m fiber for 30 min at 50 deg. C (with 5 min of previous equilibration time) with magnetic stirring was applied. Chromatographic determination was carried out by GC-MS/MS working in Selected Reaction Monitoring (SRM) mode. For most analytes, two MS/MS transitions were acquired, although for a few compounds it was difficult to obtain characteristic abundant fragments. In those cases, a pseudo selected reaction monitoring (pseudo-SRM) with three ions was used instead. The intensity ratio between quantitation (Q) and confirmation (q) signals was used as a confirmatory parameter. The method was validated by means of recovery experiments (n = 6) spiking mineral water samples at three concentration levels (0.1, 5 and 50 {mu}g L{sup -1}). Recoveries between 70% and 120% were generally obtained with

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

    Science.gov (United States)

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

    2010-05-11

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

  13. Flammable gas issues in double-contained receiver tanks. Revision 2

    International Nuclear Information System (INIS)

    Peurrung, L.M.; Mahoney, L.A.; Stewart, C.W.; Gauglitz, P.A.; Pederson, L.R.; Bryan, S.A.; Shepard, C.L.

    1998-08-01

    Four double-contained receiver tanks (DCRTs) at Hanford will be used to store salt-well pumped liquids from tanks on the Flammable Gas Watch List. This document was created to serve as a reference document describing the current knowledge of flammable gas issues in DCRTs. The document identifies, describes, evaluates, and attempts to quantify potential gas carryover and release mechanisms. It estimates several key parameters needed for these calculations, such as initial aqueous concentrations and ventilation rate, and evaluates the uncertainty in those estimates. It justifies the use of the Schumpe model for estimating vapor-liquid equilibrium constants. It identifies several potential waste compatibility issues (such as mixing and pH or temperature changes) that could lead to gas release and provides a basis for calculating their effects. It evaluates the potential for gas retention in precipitated solids within a DCRT and whether retention could lead to a buoyant displacement instability (rollover) event. It discusses rates of radiolytic, thermal, and corrosive hydrogen generation within the DCRT. It also describes in detail the accepted method of calculating the lower flammability limit (LFL) for mixtures of flammable gases. The report incorporates these analyses into two models for calculating headspace flammability, one based on instantaneous equilibrium between dissolved gases and the headspace and one incorporating limited release rates based on mass-transfer considerations. Finally, it demonstrates the use of both models to estimate headspace flammable gas concentrations and minimum ventilation rates required to maintain concentrations below 25% of the LFL

  14. Test plan for measuring ventilation rates and combustible gas levels in TWRS active catch tanks

    Energy Technology Data Exchange (ETDEWEB)

    NGUYEN, D.M.

    1999-05-20

    The purpose of this test is to provide an initial screening of combustible gas concentrations in catch tanks that currently are operated by Tank Waste Remediation System (TWRS). The data will be used to determine whether or not additional data will be needed for closure of the flammable gas unreviewed safety question for these facilities. This test will involve field measurements of ammonia, organic vapor, and total combustible gas levels in the headspace of the catch tanks. If combustible gas level in a tank exceeds an established threshold, gas samples will be collected in SUMMA canisters for more extensive laboratory analysis. In addition, ventilation rates of some catch tanks will be measured to evaluate removal of flammable gas by air flow through the tanks.

  15. Test plan for measuring ventilation rates and combustible gas levels in RPP active catch tanks

    Energy Technology Data Exchange (ETDEWEB)

    NGUYEN, D.M.

    1999-06-03

    The purpose of this test is to provide an initial screening of combustible gas concentrations in catch tanks that currently are operated by River Protection Project (RPP). The data will be used to determine whether or not additional data will be needed for closure of the flammable gas unreviewed safety question for these facilities. This test will involve field measurements of ammonia, organic vapor, and total combustible gas levels in the headspace of the catch tanks. If combustible gas level in a tank exceeds an established threshold, gas samples will be collected in SUMMA canisters for more extensive laboratory analysis. In addition, ventilation rates of some catch tanks will be measured to evaluate removal of flammable gas by air flow through the tanks.

  16. Microwave-assisted decomplexation and in-situ headspace in-syringe dynamic derivatization of dimethylamine borane with high performance liquid chromatography-fluorescence detection.

    Science.gov (United States)

    Muniraj, Sarangapani; Lee, Hua-Kwang; Hsiech, Chunming; Jen, Jen-Fon

    2018-02-16

    A rapid, sensitive, selective, and simple method for monitoring dimethylamine borane (DMAB) in aqueous sample is proposed by combining microwave-assisted de-complexation, headspace liquid phase in-situ derivatization extraction, and high-performance liquid chromatography-fluorescence detection for the determination of DMAB in samples. The present procedure involves de-complexation of DMAB using microwave irradiation, evolution of dimethylamine (DMA) to the headspace from an alkalized sample solution, and dynamic headspace liquid-phase derivatization extraction (Dy-HS-LPDE) of DMA with 9-fluorenylmethyl chloroformate in a syringe barrel. In addition to the optimal Dy-HS-LPDE and chromatographic parameters described in our previous study, the de-complexation of DMAB by thermal and microwave-assisted procedures and evolution of DMA into the headspace from an alkalized solution and modification of the Dy-HS-LPDE method are thoroughly investigated. The results indicate that complete de-complexation was obtained at 70 °C for 5 min, 30 °C for 10 min, or using microwave irradiation for 30 s at any applied power. It indicates that the DMAB complex easily undergoes de-complexation under microwave irradiation. The linearity range was 0.01-0.5 mg L -1 for DMAB and 0.0077-0.38 mg L -1 for DMA, with a coefficient of determination of 0.9995, and limit of detection of 3 μg L -1 (limit of quantitation of 10 μg L -1 ) for DMAB. The recoveries of DMAB are 95.3% (3.0% RSD) for waste water when spiked 0.05 mg L -1 and 93.5% (5.4% RSD) for the samples spiked with copper and nickel salts (5 mM each in the spiked waste sample). The whole analytical procedure can be completed within 25 min. The results confirm that the present method is a rapid, sensitive, selective, automated, low-cost and eco-friendly procedure to identify DMAB in samples. Copyright © 2018 Elsevier B.V. All rights reserved.

  17. Bepaling van tetrachloor- en trichloorethyleen in olijfolie met behulp van headspace - gaschromatografie

    NARCIS (Netherlands)

    Roos, A.H.; Mazijk, van R.J.; Tuinstra, L.G.M.Th.

    1990-01-01

    De resultaten van de EEG headspace methode wijzen uit dat de herhaalbaarheid en nauwkeurigheid voldoende zijn om tetrachloor- en trichloorethyleen in olijfolie te bepalen tot een niveau van 0,01 mg/kg op produkt. De headspace techniek is door de eenvoudige procedure zeer geschikt voor routine

  18. Calibration-free sensor for pressure and H2O concentration in headspace of sterile vial using tunable diode laser absorption spectroscopy.

    Science.gov (United States)

    Cai, Tingdong; Gao, Guangzhen; Liu, Ying

    2013-11-10

    Tunable diode laser absorption measurements of pressure and H2O concentration in the headspace of vials using a distributed-feedback (DFB) diode laser near 1.4 μm are reported. A H2O line located near 7161.41 cm(-1) is selected based on its strong absorption strength and isolation from interference of neighboring transitions. Direct absorption spectra of H2O are obtained for the measurement path as well as the reference path by scanning the laser wavelength. The pressure and H2O vapor concentration in the headspace of a vial are inferred from a differential absorption signal, which is the difference between the measured and the referenced absorbance spectra. This sensor is calibration-free and no purge gas is needed. The demonstrated capability would enable measurements of pressure and H2O concentration in the headspace of vials within 2.21% and 2.86%, respectively. A precision of 1.02 Torr and 390 ppm is found for the pressure and H2O concentration, respectively. A set of measurements for commercial freeze-dried products are also performed to illustrate the usefulness of this sensor.

  19. Effect of headspace CO2 concentration on toxin production by Clostridium botulinum in MAP, irradiated fresh pork

    International Nuclear Information System (INIS)

    Lambert, A.D.; Smith, J.P.; Dodds, K.L.

    1991-01-01

    The effects of five initial levels of CO2 (15, 30, 45, 60, and 75%) and three irradiation doses (0, 0.5, and 1.0 kGy) on toxin production by Clostridium botulinum in inoculated fresh pork were studied using factorial design experiments. Headspace CO2 levels increased in all samples during storage at 15 degrees C. In most treatments, spoilage preceded toxigenesis. Toxin production occurred faster in samples initially packaged with 15 to 30% of CO2 while higher levels of CO2 (45-75%) delayed toxin production. Low-dose irradiation delayed toxin production at all levels of CO2 in the package headspace. Contrary to expectations, including a CO2 absorbent in the package enhanced toxin production by C. botulinum. This was attributed to production of H2 by the CO2 absorbent, possibly resulting in a decrease in the oxido-reduction potential of the meat

  20. Simple determination of hydrazine in waste water by headspace solid-phase micro extraction and gas chromatography-tandem mass spectrometry after derivatization with trifluoro pentanedione.

    Science.gov (United States)

    Oh, Jin-Aa; Shin, Ho-Sang

    2017-01-15

    A headspace solid-phase micro extraction (HS-SPME) and gas chromatography-tandem mass spectrometric (GC-MS/MS) method is described to detect hydrazine after derivatization with 1,1,1-trifluoro-2,4-pentanedione (1,1,1-TFPD) to 3-methyl-5-(trifluoromethyl) pyrazole in industrial waste water. The following optimal HS-SPME conditions were used: 85 μm-carboxen-polydimethylsiloxane fibre, 100 mg L -1 TFPD, saturated NaCl, an extraction/derivatization temperature of 80 °C, a heating time of 40 min, and a pH of 9.5. Under the established conditions, the detection and quantification limits were 0.002 μg L -1 and 0.007 μg L -1  by using 5 mL of waste water and the intra- and inter-day relative standard deviations were less than 10.2% at concentrations of 0.02 and 0.1 μg L -1 . The calibration curve showed good linearity, with r 2  = 0.998; the accuracy was in the range of 98.0-103%; and the precision of the assay was less than 10.2% in industrial waste water. Hydrazine was detected over a concentration range of 0.011-0.074 μg L -1 in 5 of 20 waste water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  1. Gas generation in pure and impure plutonium-bearing materials

    International Nuclear Information System (INIS)

    Mason, R.; Allen, T.; Eller, P.G.; Hagan, R.; Horrell, D.; Rink, N.

    1999-01-01

    The Los Alamos National Laboratory's (LANL's) materials identification and surveillance (MIS) project identifies materials to be stored in DOE-STD-3013-96 containers, determines the chemical and physical character of stored materials, and evaluates processing to be used to stabilize materials to meet the standard. The project has completed processing and analysis of 9 Hanford items and 24 Rocky Flats items, representing a substantial portion of the oxides to be packaged for long-term storage. The resultant data provide insight into the physical and chemical characteristics of the materials at the sites. A component of the study was to investigate gas generation for representative materials. These studies included headspace gas measurements over the 9 Hanford items, measurement of gas generation in 10-g surveillance samples of MIS powders, and pressure monitoring. Before examining the Hanford cans, sampling and analysis methods were demonstrated on HRA-905191, an item from the LANL vault. This item was not typical of materials designated to be stored in 3013 cans, as it contained plastic vials, emery cloths, paper towels, and a large percentage of thorium. However, it was one of the items that contained significant hydrogen in the headspace. A mass spectrometer was used to determine the composition of headspace gases. Oxygen was substantially depleted in all cases, and the percent of nitrogen in many items was greater than that found in air. In both cans with a high hydrogen content, the corresponding oxygen content was near zero (HRA905191 and ARF-102-85-365). In some cases, carbon dioxide was generated in the cans. Carbon monoxide was found in item BLO-39-11-85-295. This item has a high americium content, thus higher temperature than other materials examined. The only notable impurities in item BLO-39-11-85-295 were carbon at ≅0.1 wt% and chlorides at 0.2 wt%. Seven long-term surveillance vessels each holding approximately10 g of MIS powders have been monitored

  2. Headspace solid-phase microextraction coupled to gas chromatography-tandem mass spectrometry for the determination of haloanisoles in sparkling (cava and cider) and non-sparkling (wine) alcoholic beverages.

    Science.gov (United States)

    Ruiz-Delgado, Ana; Arrebola-Liébanas, Francisco Javier; Romero-González, Roberto; López-Ruiz, Rosalía; Garrido Frenich, Antonia

    2016-10-01

    A highly sensitive analytical method was developed to determine 2,4,6-trichloroanisole (TCA), 2,3,4,6-tetrachloroanisole (TeCA), 2,4,6-tribromoanisole (TBA) and 2,3,4,5,6-pentachloroanisole (PCA) in sparkling alcoholic beverages. The method was based on the use of headspace solid-phase microextraction (HS-SPME) using a polydimethylsiloxane (PDMS) fibre. It was coupled to gas chromatography-triple quadrupole tandem mass spectrometry (GC-QqQ-MS/MS) for the detection and quantification of the target haloanisoles. The method was fully automated and no sample preparation was needed. The method was validated for alcoholic beverages. The influence of CO 2 on the extraction efficiency was also evaluated for the studied sparkling drinks (cava and cider). All the calibration curves showed good linearity (R 2  > 0.98) within the tested range (1-50 ng l -1 ). Recoveries were evaluated at three different levels (1, 5 and 50 ng l -1 ) and were always between 71% and 119%. Precision was expressed as relative standard deviation (RSD), and was evaluated as intra- and inter-day precisions, with values ≤ 22% in both cases. Limits of quantitation (LOQs) were ≤ 0.91 ng l -1 , which are below the sensory threshold levels for such compounds in humans. The validated method was applied to commercial samples, 10 cavas and 10 ciders, but it was also used for the analysis of nine red wines and four white wines, demonstrating the further applicability of the proposed method to non-sparkling beverages. TCA was detected in most samples at up to 0.45 ng l -1 .

  3. Headspace solid-phase microextraction (HS-SPME) combined with GC-MS as a process analytical technology (PAT) tool for monitoring the cultivation of C. tetani.

    Science.gov (United States)

    Ghader, Masoud; Shokoufi, Nader; Es-Haghi, Ali; Kargosha, Kazem

    2018-04-15

    Vaccine production is a biological process in which variation in time and output is inevitable. Thus, the application of Process Analytical Technologies (PAT) will be important in this regard. Headspace solid - phase microextraction (HS-SPME) coupled with GC-MS can be used as a PAT for process monitoring. This method is suitable to chemical profiling of volatile organic compounds (VOCs) emitted from microorganisms. Tetanus is a lethal disease caused by Clostridium tetani (C. tetani) bacterium and vaccination is an ultimate way to prevent this disease. In this paper, SPME fiber was used for the investigation of VOCs emerging from C. tetani during cultivation. Different types of VOCs such as sulfur-containing compounds were identified and some of them were selected as biomarkers for bioreactor monitoring during vaccine production. In the second step, the portable dynamic air sampling (PDAS) device was used as an interface for sampling VOCs by SPME fibers. The sampling procedure was optimized by face-centered central composite design (FC-CCD). The optimized sampling time and inlet gas flow rates were 10 min and 2 m L s -1 , respectively. PDAS was mounted in exhausted gas line of bioreactor and 42 samples of VOCs were prepared by SPME fibers in 7 days during incubation. Simultaneously, pH and optical density (OD) were evaluated to cultivation process which showed good correlations with the identified VOCs (>80%). This method could be used for VOCs sampling from off-gas of a bioreactor to monitoring of the cultivation process. Copyright © 2018. Published by Elsevier B.V.

  4. Gas-driven pump for ground-water samples

    Science.gov (United States)

    Signor, Donald C.

    1978-01-01

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

  5. Measurements of waste tank passive ventilation rates using tracer gases

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Olsen, K.B.; Sklarew, D.S.; Evans, J.C.; Remund, K.M.

    1997-09-01

    This report presents the results of ventilation rate studies of eight passively ventilated high-level radioactive waste tanks using tracer gases. Head space ventilation rates were determined for Tanks A-101, AX-102, AX-103, BY-105, C-107, S-102, U-103, and U-105 using sulfur hexafluoride (SF 6 ) and/or helium (He) as tracer gases. Passive ventilation rates are needed for the resolution of several key safety issues. These safety issues are associated with the rates of flammable gas production and ventilation, the rates at which organic salt-nitrate salt mixtures dry out, and the estimation of organic solvent waste surface areas. This tracer gas study involves injecting a tracer gas into the tank headspace and measuring its concentration at different times to establish the rate at which the tracer is removed by ventilation. Tracer gas injection and sample collection were performed by SGN Eurisys Service Corporation and/or Lockheed Martin Hanford Corporation, Characterization Project Operations. Headspace samples were analyzed for He and SF 6 by Pacific Northwest National Laboratory (PNNL). The tracer gas method was first demonstrated on Tank S-102. Tests were conducted on Tank S-102 to verify that the tracer gas was uniformly distributed throughout the tank headspace before baseline samples were collected, and that mixing was sufficiently vigorous to maintain an approximately uniform distribution of tracer gas in the headspace during the course of the study. Headspace samples, collected from a location about 4 in away from the injection point and 15, 30, and 60 minutes after the injection of He and SF 6 , indicated that both tracer gases were rapidly mixed. The samples were found to have the same concentration of tracer gases after 1 hour as after 24 hours, suggesting that mixing of the tracer gas was essentially complete within 1 hour

  6. Composition of the C6+ Fraction of Natural Gas by Multiple Porous Layer Open Tubular Capillaries Maintained at Low Temperatures.

    Science.gov (United States)

    Burger, Jessica L; Lovestead, Tara M; Bruno, Thomas J

    2016-03-17

    As the sources of natural gas become more diverse, the trace constituents of the C 6 + fraction are of increasing interest. Analysis of fuel gas (including natural gas) for compounds with more than 6 carbon atoms (the C 6 + fraction) has historically been complex and expensive. Hence, this is a procedure that is used most often in troubleshooting rather than for day-to-day operations. The C 6 + fraction affects gas quality issues and safety considerations such as anomalies associated with odorization. Recent advances in dynamic headspace vapor collection can be applied to this analysis and provide a faster, less complex alternative for compositional determination of the C 6 + fraction of natural gas. Porous layer open tubular capillaries maintained at low temperatures (PLOT-cryo) form the basis of a dynamic headspace sampling method that was developed at NIST initially for explosives in 2009. This method has been recently advanced by the combining of multiple PLOT capillary traps into one "bundle," or wafer, resulting in a device that allows the rapid trapping of relatively large amounts of analyte. In this study, natural gas analytes were collected by flowing natural gas from the laboratory (gas out of the wall) or a prepared surrogate gas flowing through a chilled wafer. The analytes were then removed from the PLOT-cryo wafer by thermal desorption and subsequent flushing of the wafer with helium. Gas chromatography (GC) with mass spectrometry (MS) was then used to identify the analytes.

  7. Comparison of vapor sampling system (VSS) and in situ vapor sampling (ISVS) methods on Tanks C-107, BY-108, and S-102. Revision 1

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Edwards, J.A.; Evans, J.C.

    1996-08-01

    This report discusses comparison tests for two methods of collecting vapor samples from the Hanford Site high-level radioactive waste tank headspaces. The two sampling methods compared are the truck-mounted vapor sampling system (VSS) and the cart-mounted in-situ vapor sampling (ISVS). Three tanks were sampled by both the VSS and ISVS methods from the same access risers within the same 8-hour period. These tanks have diverse headspace compositions and they represent the highest known level of several key vapor analytes

  8. Analysis of the Volatile Profile of Core Chinese Mango Germplasm by Headspace Solid-Phase Microextraction Coupled with Gas Chromatography-Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Xiao-Wei Ma

    2018-06-01

    Full Text Available Despite abundant published research on the volatile characterization of mango germplasm, the aroma differentiation of Chinese cultivars remains unclear. Using headspace solid phase microextraction (HS-SPME coupled with gas chromatography–mass spectrometry (GC-MS, the composition and relative content of volatiles in 37 cultivars representing the diversity of Chinese mango germplasm were investigated. Results indicated that there are distinct differences in the components and content of volatile compounds among and within cultivars. In total, 114 volatile compounds, including 23 monoterpenes, 16 sesquiterpenes, 29 non-terpene hydrocarbons, 25 esters, 11 aldehydes, five alcohols and five ketones, were identified. The total volatile content among cultivars ranged from 211 to 26,022 μg/kg fresh weight (FW, with 123-fold variation. Terpene compounds were the basic background volatiles, and 34 cultivars exhibited abundant monoterpenes. On the basis of hierarchical cluster analysis (HCA and principal component analysis (PCA, terpinolene and α-pinene were important components constituting the aroma of Chinese mango cultivars. Most obviously, a number of mango cultivars with high content of various aroma components were observed, and they can serve as potential germplasms for both breeding and direct use.

  9. Determination of 2-Propenal Using Headspace Solid-Phase Microextraction Coupled to Gas Chromatography–Time-of-Flight Mass Spectrometry as a Marker for Authentication of Unrefined Sesame Oil

    Directory of Open Access Journals (Sweden)

    Ahmad Rois Mansur

    2017-01-01

    Full Text Available Ascertaining the authenticity of the unrefined sesame oil presents an ongoing challenge. Here, the determination of 2-propenal was performed by headspace solid-phase microextraction (HS-SPME under mild temperature coupled to gas chromatography with time-of-flight mass spectrometry, enabling the detection of adulteration of unrefined sesame oil with refined corn or soybean oil. Employing this coupled technique, 2-propenal was detected in all tested refined corn and soybean oils but not in any of the tested unrefined sesame oil samples. Using response surface methodology, the optimum extraction temperature, equilibrium time, and extraction time for the HS-SPME analysis of 2-propenal using carboxen/polydimethylsiloxane fiber were determined to be 55°C, 15 min, and 15 min, respectively, for refined corn oil and 55°C, 25 min, and 15 min, respectively, for refined soybean oil. Under these optimized conditions, the adulteration of unrefined sesame oil with refined corn or soybean oils (1–5% was successfully detected. The detection and quantification limits of 2-propenal were found to be in the range of 0.008–0.010 and 0.023–0.031 µg mL−1, respectively. The overall results demonstrate the potential of this novel method for the authentication of unrefined sesame oil.

  10. Gas chromatographic-mass spectrometric analysis of urinary volatile organic metabolites: Optimization of the HS-SPME procedure and sample storage conditions.

    Science.gov (United States)

    Živković Semren, Tanja; Brčić Karačonji, Irena; Safner, Toni; Brajenović, Nataša; Tariba Lovaković, Blanka; Pizent, Alica

    2018-01-01

    Non-targeted metabolomics research of human volatile urinary metabolome can be used to identify potential biomarkers associated with the changes in metabolism related to various health disorders. To ensure reliable analysis of urinary volatile organic metabolites (VOMs) by gas chromatography-mass spectrometry (GC-MS), parameters affecting the headspace-solid phase microextraction (HS-SPME) procedure have been evaluated and optimized. The influence of incubation and extraction temperatures and times, coating fibre material and salt addition on SPME efficiency was investigated by multivariate optimization methods using reduced factorial and Doehlert matrix designs. The results showed optimum values for temperature to be 60°C, extraction time 50min, and incubation time 35min. The proposed conditions were applied to investigate urine samples' stability regarding different storage conditions and freeze-thaw processes. The sum of peak areas of urine samples stored at 4°C, -20°C, and -80°C up to six months showed a time dependent decrease over time although storage at -80°C resulted in a slight non-significant reduction comparing to the fresh sample. However, due to the volatile nature of the analysed compounds, more than two cycles of freezing/thawing of the sample stored for six months at -80°C should be avoided whenever possible. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Headspace Analysis of Ammonium Nitrate

    Science.gov (United States)

    2017-01-25

    explosive ammonium nitrate produces ammonia and nitric acid in the gaseous headspace above bulk solids, but the concentrations of the products have been...and NO2-, a product of nitrate fragmentation (Figure 7). Brief spikes in the background and dips in oxalic acid signal were observed at the time of...either filtered air or experimental nitric acid vapor sources so that analyte signal could be measured directly opposite background. With oxalic

  12. Test Plan for Measuring Ventilation Rates and Combustible Gas Levels in TWRS Active Catch Tanks

    Energy Technology Data Exchange (ETDEWEB)

    NGUYEN, D.M.

    1999-10-25

    The purpose of this sampling activity is to obtain data to support an initial evaluation of potential hazards due to the presence of combustible gas in catch tanks that are currently operated by the River Protection Project (RPP). Results of the hazard analysis will be used to support closure of the flammable gas unreviewed safety question for these facilities. The data collection will be conducted in accordance with the Tank Safety Screening Data Quality Objective (Dukelow et al. 1995). Combustible gas, ammonia, and organic vapor levels in the headspace of the catch tanks will be field-measured using hand-held instruments. If a combustible gas level measurement in a tank exceeds an established threshold, gas samples will he collected in SUMMA' canisters for more extensive laboratory analysis. In addition, ventilation rates of some catch tanks will be measured to evaluate removal of flammable gas by air flowing through the tanks. This test plan identifies the sample collection, laboratory analysis, quality assurance, and reporting objectives for this data collection effort. The plan also provides the procedures for field measurement of combustible gas concentrations and ventilation rates.

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

    African Journals Online (AJOL)

    DELL

    2012-05-22

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

  14. Hydrogen gas sample environment for TOSCA

    International Nuclear Information System (INIS)

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

    2014-01-01

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

  15. Technical note: In vitro total gas and methane production measurements from closed or vented rumen batch culture systems.

    Science.gov (United States)

    Cattani, M; Tagliapietra, F; Maccarana, L; Hansen, H H; Bailoni, L; Schiavon, S

    2014-03-01

    This study compared measured gas production (GP) and computed CH4 production values provided by closed or vented bottles connected to gas collection bags. Two forages and 3 concentrates were incubated. Two incubations were conducted, where the 5 feeds were tested in 3 replicates in closed or vented bottles, plus 4 blanks, for a total of 64 bottles. Half of the bottles were not vented, and the others were vented at a fixed pressure (6.8 kPa) and gas was collected into one gas collection bag connected to each bottle. Each bottle (317 mL) was filled with 0.4000 ± 0.0010 g of feed sample and 60 mL of buffered rumen fluid (headspace volume = 257 mL) and incubated at 39.0°C for 24 h. At 24 h, gas samples were collected from the headspace of closed bottles or from headspace and bags of vented bottles and analyzed for CH4 concentration. Volumes of GP at 24 h were corrected for the gas dissolved in the fermentation fluid, according to Henry's law of gas solubility. Methane concentration (mL/100mL of GP) was measured and CH4 production (mL/g of incubated DM) was computed using corrected or uncorrected GP values. Data were analyzed for the effect of venting technique (T), feed (F), interaction between venting technique and feed (T × F), and incubation run as a random factor. Closed bottles provided lower uncorrected GP (-18%) compared with vented bottles, especially for concentrates. Correction for dissolved gas reduced but did not remove differences between techniques, and closed bottles (+25 mL of gas/g of incubated DM) had a greater magnitude of variation than did vented bottles (+1 mL of gas/g of incubated DM). Feeds differed in uncorrected and corrected GP, but the ranking was the same for the 2 techniques. The T × F interaction influenced uncorrected GP values, but this effect disappeared after correction. Closed bottles provided uncorrected CH4 concentrations 23% greater than that of vented bottles. Correction reduced but did not remove this difference. Methane

  16. A novel headspace solid-phase microextraction method using in situ derivatization and a diethoxydiphenylsilane fibre for the gas chromatography-mass spectrometry determination of urinary hydroxy polycyclic aromatic hydrocarbons.

    Science.gov (United States)

    Mattarozzi, M; Musci, M; Careri, M; Mangia, A; Fustinoni, S; Campo, L; Bianchi, F

    2009-07-24

    An innovative and simple headspace solid-phase microextraction method using a novel diethoxydiphenylsilane fibre based on in situ derivatization with acetic anhydride was optimized and validated for the gas chromatography-mass spectrometry determination of some monohydroxy metabolites of polycyclic aromatic hydrocarbons, namely 1-hydroxynaphthalene, 2-hydroxynaphtalene, 9-hydroxyfluorene, 2-hydroxyfluorene and 1-hydroxypyrene at trace levels in human urine. Enzymatic hydrolysis was applied before derivatization, whereas extraction conditions, i.e. the effects of time and temperature of extraction and salt addition were investigated by experimental design. Regression models and desirability functions were applied to find the experimental conditions providing the highest global extraction response. These conditions were found in correspondence of an extraction temperature of 90 degrees C, an extraction time of 90 min and 25% NaCl added to urine samples. The capabilities of the developed method were proved obtaining limit of quantitations in the 0.1-2 microg/l range, thus allowing the bio-monitoring of these compounds in human urine. A good precision was observed both in terms of intra-batch and inter-batch repeatability with RSD always lower than 14%. Recoveries ranging from 98(+/-3) to 121(+/-1)% and extraction yields higher than 72% were also obtained. Finally, the analysis of urine specimens of coke-oven workers revealed analytes' concentrations in the 2.2-164 microg/l range, proving the exposure to PAHs of the involved workers.

  17. Soil Gas Sampling Operating Procedure

    Science.gov (United States)

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

  18. Headspace single-drop microextraction coupled to microvolume UV-vis spectrophotometry for iodine determination

    International Nuclear Information System (INIS)

    Pena-Pereira, Francisco; Lavilla, Isela; Bendicho, Carlos

    2009-01-01

    Headspace single-drop microextraction has been combined with microvolume UV-vis spectrophotometry for iodine determination. Matrix separation and preconcentration of iodide following in situ volatile iodine generation and extraction into a microdrop of N,N'-dimethylformamide is performed. An exhaustive characterization of the microextraction system and the experimental variables affecting iodine generation from iodide was carried out. The procedure employed consisted of exposing 2.5 μL of N,N'-dimethylformamide to the headspace of a 10 mL acidic (H 2 SO 4 2 mol L -1 ) aqueous solution containing 1.7 mol L -1 Na 2 SO 4 for 7 min. Addition of 1 mL of H 2 O 2 1 mol L -1 for in situ iodine generation was performed. The limit of detection was determined as 0.69 μg L -1 . The repeatability, expressed as relative standard deviation, was 4.7% (n = 6). The calibration working range was from 5 to 200 μg L -1 (r 2 = 0.9991). The large preconcentration factor obtained, ca. 623 in only 7 min, compensate for the 10-fold loss in sensitivity caused by the decreased optical path, which results in improved detection limits as compared to spectrophotometric measurements carried out with conventional sample cells. The method was successfully applied to the determination of iodine in water, pharmaceutical and food samples

  19. High efficient ethanol and VFAs production from gas fermentation: effect of acetate, gas and inoculum microbial composition

    DEFF Research Database (Denmark)

    El-Gammal, Maie; Abou-Shanab, Reda; Angelidaki, Irini

    2017-01-01

    In bioindustry, syngas fermentation is a promising technology for biofuel production without the use of plant biomass as sugar-based feedstock. The aim of this study was to identify optimal conditions for high efficient ethanol and volatile fatty acids (VFA) production from synthetic gas...... fatty acids and ethanol was achieved by the pure culture (Clostridium ragsdalei). Depending on the headspace gas composition, VFA concentrations were up to 300% higher after fermentation with Clostridium ragsdalei compared to fermentation with mixed culture. The preferred gas composition with respect...

  20. A molybdenum disulfide/reduced graphene oxide fiber coating coupled with gas chromatography-mass spectrometry for the saponification-headspace solid-phase microextraction of polychlorinated biphenyls in food.

    Science.gov (United States)

    Lv, Fangying; Gan, Ning; Cao, Yuting; Zhou, You; Zuo, Rongjie; Dong, Youren

    2017-11-24

    In this work, the molybdenum disulfide/reduced graphene oxide (MoS 2 /RGO) composite material was synthesized as a fiber coating to extract seven indicator polychlorinated biphenyls (PCBs; PCB28, PCB52, PCB101, PCB118, PCB138, PCB153, and PCB180) present in food via a saponification-headspace solid-phase microextraction assay (saponification-HS-SPME). The MoS 2 /RGO coating was prepared and deposited on a stainless steel wire with the help of a silicone sealant and used as an SPME fiber. The alkali solution dissolved the fat and helped in releasing the PCBs present in milk to the headspace for extraction under 100°C. Following desorption in the inlet, the targets were quantified by gas chromatography-mass spectrometry. The effects of sorbent dosage, extraction time, added salts, and stirring rate on the extraction efficiency were investigated. The new coating was able to adsorb a higher amount of analytes, which was about 1.1-2.9 times in comparison with the commercially available SPME fiber (coated with divinylbenzene/carboxen/polydimethylsiloxane). It also showed the highest adsorption capability toward PCBs, which was 1.5-2.7 times that of the prepared RGO modified fiber. Moreover, MoS 2 also showed a strong affinity toward PCBs in a manner similar to its affinity for graphene. The developed method is simple and environmentally friendly as it does not require any organic solvents. Furthermore, it exhibits good sensitivity with detection limits less than 0.1ngmL -1 , linearity (0.25-100ngmL -1 ), and reproducibility (relative standard deviation below 10% for n=3). The novel SPME fibers are inexpensive, reusable, and can be easily prepared and manipulated. In addition, the saponification-HS-SPME assay was also found to be suitable for screening persistent organic pollutants in dairy products. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. Volatile profile of the headspace fraction of "assa-peixe" (Vernonia sp. honeys Perfil dos compostos voláteis presentes na fração "headspace" de méis de assa-peixe

    Directory of Open Access Journals (Sweden)

    Mariana Carvalho Ribeiro

    2008-03-01

    Full Text Available The volatile compounds were isolated from the headspace fraction of "assa-peixe" honeys by adsorptive column chromatography, eluted with acetone and analysed by GC-FID and GC-MS. Volatile compounds were separated using a polar phase column. Low- and medium-boiling point volatile compounds predominated in the headspace. A large proportion of 3-penten-2-one (80.5 ± 13.9 µg.kg-1 and benzaldehyde (25.9 ± 4.2 µg.kg-1 was found in the headspace fraction, while 2-penten-1-ol, 3-hexenyl butanoate, octadecane and hexanoic acid (Os compostos voláteis da fração "Headspace" de méis de assa-peixe foram adsorvidos pela técnica de cromatografia de adsorção, eluídos com acetona e analisados através da CG/DIC e CG/EM usando coluna polar de sílica fundida. Os compostos voláteis de baixo e médio ponto de ebulição predominaram na fração "headspace". Foi achada uma grande proporção de 3-penten-2-ona (80,5 ± 13,9 µg.kg-1 e benzaldeído (25,9 ± 4,2 µg.kg-1, enquanto o 2-penten-1-ol, o hexanoato de 3-hexenila, o octadecano e o ácido hexanóico (<0,01 µg.kg-1 foram compostos minoritários. Um total de doze compostos voláteis foi identificado, sendo cinco descritos pela primeira vez no mel de assa-peixe. Destes cinco, a 3-penten-2-ona, o dodecano, o tridecano e o benzaldeído foram definitivamente identificados na fração "headspace" dos méis de assa-peixe brasileiro.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-09-05

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

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

  4. Calculation note: project W-320 primary ventilation air flow requirements for mitigation of steady state flammable gas concentrations in the headspaces of tanks 241-C-106 and 241-AY-102

    International Nuclear Information System (INIS)

    Estey, S.D.

    1997-01-01

    This calculation note analyzes headspace concentrations of hydrogen dependent upon assumed ventilation flow rates provided for tanks 241-C-106 and 241-AY-102. The analyses are based on measured or estimated steady state hydrogen release rates. Tank 241-C-106 is analyzed prior to sluicing; tank 241-AY-102 is analyzed both prior to and after completion of sluicing. Specific analyses, using both best estimated and bounding hydrogen generation rates, include the minimum primary ventilation flow rates required in the tanks to ensure that the steady state hydrogen concentration in the respective tank headspace does not exceed 25% and 100% of the LFL. The headspace hydrogen concentration as a function of time as well as the time required to reach 25% and 100% of LFL upon complete loss of active ventilation, starting from the steady state hydrogen concentration based on a 200 CFM minimum flow rate in tank 241-C-106 and a 100 CFM minimum flow rate in tank241-AY-102. The headspace hydrogen concentration as a function of thee following partial loss of active ventilation (i.e., step changes to l60, l20, 80, and 40 CFM ventilation flow rates) in tank 241-C-106, staffing from a 200 CFM flow rate and the corresponding steady state hydrogen concentration based on the 200 CFM flow rate. The headspace hydrogen concentration as a function of the following partial loss of active ventilation i.e., step changes to 80, 60, 40, and 20 CFM ventilation flow rates) in tank 241-AY-102, starting from a 100 CFM flow rate and the corresponding steady state hydrogen concentration based on the 100 CFM flow rate

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

    African Journals Online (AJOL)

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

  6. A volatile tracer-assisted headspace analytical technique for determining the swelling capacity of superabsorbent polymers.

    Science.gov (United States)

    Zhang, Shu-Xin; Jiang, Ran; Chai, Xin-Sheng

    2017-09-01

    This paper reports on a new method for the determination of swelling capacity of superabsorbent polymers by a volatile tracer-assisted headspace gas chromatography (HS-GC). Toluene was used as a tracer and added to the solution for polymers swelling test. Based on the differences of the tracer partitioned between the vapor and hydrogel phase before and after the polymer's swelling capacity, a transition point (corresponding to the material swelling capacity) can be observed when plotting the GC signal of toluene vs. the ratio of solution added to polymers. The present method has good precision (RSDpolymers at the elevated temperatures. Copyright © 2017 Elsevier B.V. All rights reserved.

  7. Ammonia concentration modeling based on retained gas sampler data

    International Nuclear Information System (INIS)

    Terrones, G.; Palmer, B.J.; Cuta, J.M.

    1997-09-01

    The vertical ammonia concentration distributions determined by the retained gas sampler (RGS) apparatus were modeled for double-shell tanks (DSTs) AW-101, AN-103, AN-104, and AN-105 and single-shell tanks (SSTs) A-101, S-106, and U-103. One the vertical transport of ammonia in the tanks were used for the modeling. Transport in the non-convective settled solids and floating solids layers is assumed to occur primarily via some type of diffusion process, while transport in the convective liquid layers is incorporated into the model via mass transfer coefficients based on empirical correlations. Mass transfer between the top of the waste and the tank headspace and the effects of ventilation of the headspace are also included in the models. The resulting models contain a large number of parameters, but many of them can be determined from known properties of the waste configuration or can be estimated within reasonable bounds from data on the waste samples themselves. The models are used to extract effective diffusion coefficients for transport in the nonconvective layers based on the measured values of ammonia from the RGS apparatus. The modeling indicates that the higher concentrations of ammonia seen in bubbles trapped inside the waste relative to the ammonia concentrations in the tank headspace can be explained by a combination of slow transport of ammonia via diffusion in the nonconvective layers and ventilation of the tank headspace by either passive or active means. Slow transport by diffusion causes a higher concentration of ammonia to build up deep within the waste until the concentration gradients between the interior and top of the waste are sufficient to allow ammonia to escape at the same rate at which it is being generated in the waste

  8. Quantitative analysis of 2-furfural and 5-methylfurfural in different Italian vinegars by headspace solid-phase microextraction coupled to gas chromatography-mass spectrometry using isotope dilution.

    Science.gov (United States)

    Giordano, Lucia; Calabrese, Roberto; Davoli, Enrico; Rotilio, Domenico

    2003-10-31

    A new method was developed for the determination of 2-furfural (2-F) and 5-methylfurfural (5-MF), two products of Maillard reaction in vinegar, with head-space solid-phase microextraction (HS-SPME) coupled to gas chromatography-mass spectrometry (GC-MS). A divinylbenzene (DVB)/carboxen (CAR)/polydimethylsiloxane (PDMS) fibre was used and SPME conditions were optimised, studying ionic strength effect, temperature effect and adsorption time. Both analytes were determined by calibration established on 2-furfural-d4 (2-F-d4). The method showed good linearity in the range studied (from 16 to 0.12 mg/l), with a regression coefficient r2 of 0.9999. Inter-batch precision and accuracy were found between 14.9 and 6.0% and between -11.7 and 0.2%, respectively. Detection limit was 15 microg/l. The method is simple and accurate and it has been applied to a series of balsamic and non-balsamic vinegars.

  9. Análise de pesticidas organoclorados em água usando a microextração em fase sólida por headspace com cromatografia gasosa e espectrometria de massas

    Directory of Open Access Journals (Sweden)

    Crislaine Batista Prates

    2011-01-01

    Full Text Available A method based on headspace - solid phase microextraction coupled with gas chromatography - mass spectrometry was validated for the quantitative determination of 18 organochlorine pesticides in water. For the extraction conditioning some parameters as the best type of coating fiber, time and temperature of extraction, pH and ionic strength were evaluated. The method HS-SPME/GC-MS/MS showed linear coefficient above 0.9948. The repeatability of the measurements were lower than 7.6%. Relative recoveries were between 88 and 110%. Limits of detection from 0.5 x 10-3 to 1.0 mg L-1 were obtained. A total of 31 samples were analyzed and 16 presented from 1 to 5 pesticides.

  10. Radioactively induced noise in gas-sampling uranium calorimeters

    International Nuclear Information System (INIS)

    Gordon, H.A.; Rehak, P.

    1982-01-01

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

  11. Resource Conservation and Recovery Act, Part B permit application

    International Nuclear Information System (INIS)

    1993-01-01

    This volume contains appendices for the following: results of extraction procedure (EP) toxicity data analyses; summary of headspace gas analysis in Rocky Flats Plant sampling program-FY 1988; waste drum gas generation sampling program at Rocky Flats Plant during FY 1988; TRU waste sampling program waste characterization; summary of headspace gas analyses in TRU waste sampling program; summary of volatile organic compounds analyses in TRU waste sampling program; totals analysis versus toxicity characteristic leaching procedure; Waste Isolation Pilot Plant waste characterization sampling and analysis methods; Waste Isolation Pilot Plant waste characterization analytical methods; data reduction, validation and reporting; examples of waste screening checklists; and Waste Isolation Pilot Plant generator/storage site waste screening and acceptance audit program

  12. Tracer gas diffusion sampling test plan

    International Nuclear Information System (INIS)

    Rohay, V.J.

    1993-01-01

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

  13. Optimization and validation of liquid chromatography and headspace-gas chromatography based methods for the quantitative determination of capsaicinoids, salicylic acid, glycol monosalicylate, methyl salicylate, ethyl salicylate, camphor and l-menthol in a topical formulation.

    Science.gov (United States)

    Pauwels, Jochen; D'Autry, Ward; Van den Bossche, Larissa; Dewever, Cédric; Forier, Michel; Vandenwaeyenberg, Stephanie; Wolfs, Kris; Hoogmartens, Jos; Van Schepdael, Ann; Adams, Erwin

    2012-02-23

    Capsaicinoids, salicylic acid, methyl and ethyl salicylate, glycol monosalicylate, camphor and l-menthol are widely used in topical formulations to relieve local pain. For each separate compound or simple mixtures, quantitative analysis methods are reported. However, for a mixture containing all above mentioned active compounds, no assay methods were found. Due to the differing physicochemical characteristics, two methods were developed and optimized simultaneously. The non-volatile capsaicinoids, salicylic acid and glycol monosalicylate were analyzed with liquid chromatography following liquid-liquid extraction, whereas the volatile compounds were analyzed with static headspace-gas chromatography. For the latter method, liquid paraffin was selected as compatible dilution solvent. The optimized methods were validated in terms of specificity, linearity, accuracy and precision in a range of 80% to 120% of the expected concentrations. For both methods, peaks were well separated without interference of other compounds. Linear relationships were demonstrated with R² values higher than 0.996 for all compounds. Accuracy was assessed by performing replicate recovery experiments with spiked blank samples. Mean recovery values were all between 98% and 102%. Precision was checked at three levels: system repeatability, method precision and intermediate precision. Both methods were found to be acceptably precise at all three levels. Finally, the method was successfully applied to the analysis of some real samples (cutaneous sticks). Copyright © 2011 Elsevier B.V. All rights reserved.

  14. 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.

  15. Extension of a dynamic headspace multi-volatile method to milliliter injection volumes with full sample evaporation: Application to green tea.

    Science.gov (United States)

    Ochiai, Nobuo; Sasamoto, Kikuo; Tsunokawa, Jun; Hoffmann, Andreas; Okanoya, Kazunori; MacNamara, Kevin

    2015-11-20

    An extension of multi-volatile method (MVM) technology using the combination of a standard dynamic headspace (DHS) configuration, and a modified DHS configuration incorporating an additional vacuum module, was developed for milliliter injection volume of aqueous sample with full sample evaporation. A prior step involved investigation of water management by weighing of the water residue in the adsorbent trap. The extended MVM for 1 mL aqueous sample consists of five different DHS method parameter sets including choice of the replaceable adsorbent trap. An initial two DHS sampling sets at 25°C with the standard DHS configuration using a carbon-based adsorbent trap target very volatile solutes with high vapor pressure (>10 kPa) and volatile solutes with moderate vapor pressure (1-10 kPa). Subsequent three DHS sampling sets at 80°C with the modified DHS configuration using a Tenax TA trap target solutes with low vapor pressure (88%) for 17 test aroma compounds and moderate recoveries (44-71%) for 4 test compounds. The method showed good linearity (r(2)>0.9913) and high sensitivity (limit of detection: 0.1-0.5 ng mL(-1)) even with MS scan mode. The improved sensitivity of the method was demonstrated with analysis of a wide variety of aroma compounds in brewed green tea. Compared to the original 100 μL MVM procedure, this extension to 1 mL MVM allowed detection of nearly twice the number of aroma compounds, including 18 potent aroma compounds from top-note to base-note (e.g. 2,3-butanedione, coumarin, furaneol, guaiacol, cis-3-hexenol, linalool, maltol, methional, 3-methyl butanal, 2,3,5-trimethyl pyrazine, and vanillin). Sensitivity for 23 compounds improved by a factor of 3.4-15 under 1 mL MVM conditions. Copyright © 2015 Elsevier B.V. All rights reserved.

  16. Analysis of the volatiles in the headspace above the plasmodium and sporangia of the slime mould (Physarum polycephalum) by SPME-GCMS

    OpenAIRE

    Kateb, Huda al; Costello, Ben de Lacy

    2013-01-01

    Solid phase micro-extraction (SPME) coupled with Gas Chromatography Mass Spectrometry (GC-MS) was used to extract and analyse the volatiles in the headspace above the plasmodial and sporulating stages of the slime mould Physarum Polycephalum. In total 115 compounds were identified from across a broad range of chemical classes. Although more (87) volatile organic compounds (VOCs) were identified when using a higher incubation temperature of 75oC, a large number of compounds (79) were still ide...

  17. headspace - Australia's innovation in youth mental health: who are the clients and why are they presenting?

    Science.gov (United States)

    Rickwood, Debra J; Telford, Nic R; Parker, Alexandra G; Tanti, Chris J; McGorry, Patrick D

    2014-02-03

    To provide the first national profile of the characteristics of young people (aged 12-25 years) accessing headspace centre services - the Australian Government's innovation in youth mental health service delivery - and investigate whether headspace is providing early service access for adolescents and young adults with emerging mental health problems. Census of all young people accessing a headspace centre across the national network of 55 centres comprising a total of 21 274 headspace clients between 1 January and 30 June 2013. Reason for presentation, Kessler Psychological Distress Scale, stage of illness, diagnosis, functioning. Young people were most likely to present with mood and anxiety symptoms and disorders, self-reporting their reason for attendance as problems with how they felt. Client demographic characteristics tended to reflect population-level distributions, although clients from regional areas and of Aboriginal and Torres Strait Islander background were particularly well represented, whereas those who were born outside Australia were underrepresented. headspace centres are providing a point of service access for young Australians with high levels of psychological distress and need for care in the early stages of the development of mental disorder.

  18. Determination of trihalomethanes in water samples: A review

    Energy Technology Data Exchange (ETDEWEB)

    Perez Pavon, Jose Luis [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias Quimicas, Universidad de Salamanca, 37008 Salamanca (Spain)], E-mail: jlpp@usal.es; Herrero Martin, Sara; Garcia Pinto, Carmelo; Moreno Cordero, Bernardo [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias Quimicas, Universidad de Salamanca, 37008 Salamanca (Spain)

    2008-11-23

    This article reviews the most recent literature addressing the analytical methods applied for trihalomethanes (THMs) determination in water samples. This analysis is usually performed with gas chromatography (GC) combined with a preconcentration step. The detectors most widely used in this type of analyses are mass spectrometers (MS) and electron capture detectors (ECD). Here, we review the analytical characteristics, the time required for analysis, and the simplicity of the optimised methods. The main difference between these methods lies in the sample pretreatment step; therefore, special emphasis is placed on this aspect. The techniques covered are direct aqueous injection (DAI), liquid-liquid extraction (LLE), headspace (HS), and membrane-based techniques. We also review the main chromatographic columns employed and consider novel aspects of chromatographic analysis, such as the use of fast gas chromatography (FGC). Concerning the detection step, besides the common techniques, the use of uncommon detectors such as fluorescence detector, pulsed discharge photoionization detector (PDPID), dry electrolytic conductivity detector (DELCD), atomic emission detector (AED) and inductively coupled plasma-mass spectrometry (ICP-MS) for this type of analysis is described.

  19. Analyte induced water adsorbability in gas phase biosensors: the influence of ethinylestradiol on the water binding protein capacity.

    Science.gov (United States)

    Snopok, Borys; Kruglenko, Ivanna

    2015-05-07

    An ultra-sensitive gas phase biosensor/tracer/bio-sniffer is an emerging technology platform designed to provide real-time information on air-borne analytes, or those in liquids, through classical headspace analysis. The desired bio-sniffer measures gaseous 17α- ethinylestradiol (ETED) as frequency changes on a quartz crystal microbalance (QCM), which is a result of the interactions of liquid sample components in the headspace (ETED and water) with a biorecognition layer. The latter was constructed by immobilization of polyclonal antiserum against a phenolic A-ring of estrogenic receptors through protein A. The QCM response exhibited stretched exponential kinetics of negative frequency shifts with reversible and "irreversible" components of mass uptake onto the sensor surface in static headspace conditions when exposed to water solutions of ETED over the sensor working range, from 10(-10) to 10(-17) g L(-1). It was shown that the variations in the QCM response characteristics are due to the change of the water-binding capacity of the sensing layer induced by protein transformations initiated by the binding of ETED molecules. This result is well correlated with the natural physiological function of estrogens in controlling the homeostasis of body fluids in living beings.

  20. IXM gas sampling procedure

    International Nuclear Information System (INIS)

    Pingel, L.A.

    1995-01-01

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

  1. No-migration variance petition

    International Nuclear Information System (INIS)

    1990-03-01

    Volume IV contains the following attachments: TRU mixed waste characterization database; hazardous constituents of Rocky flats transuranic waste; summary of waste components in TRU waste sampling program at INEL; total volatile organic compounds (VOC) analyses at Rocky Flats Plant; total metals analyses from Rocky Flats Plant; results of toxicity characteristic leaching procedure (TCLP) analyses; results of extraction procedure (EP) toxicity data analyses; summary of headspace gas analysis in Rocky Flats Plant (RFP) -- sampling program FY 1988; waste drum gas generation--sampling program at Rocky Flats Plant during FY 1988; TRU waste sampling program -- volume one; TRU waste sampling program -- volume two; and summary of headspace gas analyses in TRU waste sampling program; summary of volatile organic compounds (V0C) -- analyses in TRU waste sampling program

  2. Measurement of dissolved hydrogen and hydrogen gas transfer in a hydrogen-producing reactor

    Energy Technology Data Exchange (ETDEWEB)

    Shizas, I.; Bagley, D.M. [Toronto Univ., ON (Canada). Dept. of Civil Engineering

    2004-07-01

    This paper presents a simple method to measure dissolved hydrogen concentrations in the laboratory using standard equipment and a series of hydrogen gas transfer tests. The method was validated by measuring hydrogen gas transfer parameters for an anaerobic reactor system that was purged with 10 per cent carbon dioxide and 90 per cent nitrogen using a coarse bubble diffuser stone. Liquid samples from the reactor were injected into vials and hydrogen was allowed to partition between the liquid and gaseous phases. The concentration of dissolved hydrogen was determined by comparing the headspace injections onto a gas chromatograph and a standard curve. The detection limit was 1.0 x 10{sup -5} mol/L of dissolved hydrogen. The gas transfer rate for hydrogen in basal medium and anaerobic digester sludge was used to validate the method. Results were compared with gas transfer models. In addition to monitoring dissolved hydrogen in reactor systems, this method can help improve hydrogen production potential. 1 ref., 4 figs.

  3. Methodology for flammable gas evaluations

    Energy Technology Data Exchange (ETDEWEB)

    Hopkins, J.D., Westinghouse Hanford

    1996-06-12

    There are 177 radioactive waste storage tanks at the Hanford Site. The waste generates flammable gases. The waste releases gas continuously, but in some tanks the waste has shown a tendency to trap these flammable gases. When enough gas is trapped in a tank`s waste matrix, it may be released in a way that renders part or all of the tank atmosphere flammable for a period of time. Tanks must be evaluated against previously defined criteria to determine whether they can present a flammable gas hazard. This document presents the methodology for evaluating tanks in two areas of concern in the tank headspace:steady-state flammable-gas concentration resulting from continuous release, and concentration resulting from an episodic gas release.

  4. Ethanol concentration in 56 refillable electronic cigarettes liquid formulations determined by headspace gas chromatography with flame ionization detector (HS-GC-FID).

    Science.gov (United States)

    Poklis, Justin L; Wolf, Carl E; Peace, Michelle R

    2017-10-01

    Personal battery-powered vaporizers or electronic cigarettes were developed as an alternative to traditional cigarettes. The modern electronic cigarettes were patented in 2004 by Hon Lik in China. In May 2016, the US Food and Drug Administration (FDA) imposed regulatory statutes on e-cigarettes and their liquid formulations (e-liquids); prior to that, they were unregulated. E-liquids are typically composed of propylene glycol and/or glycerin, flavouring component(s), and active ingredient(s), such as nicotine. Fifty-six commercially available e-liquids, purchased from various sources, contained a variety of flavours and active ingredients. A headspace gas chromatography with flame ionization detector (HS-GC-FID) method was used to analyze these e-liquids for volatiles content. Only one of the e-liquids listed ethanol as a component. The chromatographic separation of volatiles was performed on a Restek BAC-1 column. A linear calibration was generated for ethanol with limits of detection and quantification (LOD/LOQ) of 0.05 mg/mL. Ethanol concentrations in the 56 e-liquids ranged from none detected to 206 mg/mL. The ethanol determined in these products may have been used in flavourants or a solvent; the reason for inclusion cannot be fully ascertained. The implications of vaporizing ethanol as an e-liquid component are unknown. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

  5. A comparison of sample preparation methods for extracting volatile organic compounds (VOCs) from equine faeces using HS-SPME.

    Science.gov (United States)

    Hough, Rachael; Archer, Debra; Probert, Christopher

    2018-01-01

    Disturbance to the hindgut microbiota can be detrimental to equine health. Metabolomics provides a robust approach to studying the functional aspect of hindgut microorganisms. Sample preparation is an important step towards achieving optimal results in the later stages of analysis. The preparation of samples is unique depending on the technique employed and the sample matrix to be analysed. Gas chromatography mass spectrometry (GCMS) is one of the most widely used platforms for the study of metabolomics and until now an optimised method has not been developed for equine faeces. To compare a sample preparation method for extracting volatile organic compounds (VOCs) from equine faeces. Volatile organic compounds were determined by headspace solid phase microextraction gas chromatography mass spectrometry (HS-SPME-GCMS). Factors investigated were the mass of equine faeces, type of SPME fibre coating, vial volume and storage conditions. The resultant method was unique to those developed for other species. Aliquots of 1000 or 2000 mg in 10 ml or 20 ml SPME headspace were optimal. From those tested, the extraction of VOCs should ideally be performed using a divinylbenzene-carboxen-polydimethysiloxane (DVB-CAR-PDMS) SPME fibre. Storage of faeces for up to 12 months at - 80 °C shared a greater percentage of VOCs with a fresh sample than the equivalent stored at - 20 °C. An optimised method for extracting VOCs from equine faeces using HS-SPME-GCMS has been developed and will act as a standard to enable comparisons between studies. This work has also highlighted storage conditions as an important factor to consider in experimental design for faecal metabolomics studies.

  6. (E-2-Nonenal determination in brazilian beers using headspace solid-phase microextraction and gas chromatographic coupled mass spectrometry (HS-SPME-GC-MS Determinação de (E-2-nonenal em cervejas brasileiras utilizando microextração em fase sólida do headspace e cromatografia gasosa acoplada a espectrometria de massas

    Directory of Open Access Journals (Sweden)

    Rodrigo Scherer

    2010-05-01

    Full Text Available (E-2-nonenal is considered an important off-flavor of beer, related to the flavor of beer staling. In this study, a new method for determination of (E-2-nonenal in beer using headspace solid-phase microextraction and gas chromatographic coupled mass spectrometry (HS-SPME-GC-MS was developed and applied in Brazilian beer samples. The extractions were carried out in CAR-PDMS (carboxen-polydimethylsiloxane fiber and the best results were found with 15 minutes of equilibrium and 90 minutes of extraction at 50 °C. The method was linear in the range from 0.02 to 4.0 μg.L-1 with correlation coefficient of 0.9994. The limits of detection and quantification were 0.01 and 0.02 μg.L-1, respectively. 96.5% of recovery and 4% precision (RSD were obtained in the fortification of beer samples with 2.0 μg.L-1 of (E-2-nonenal. The developed method proved to be simple, efficient and highly sensitive to the determination of this analyte being easily applied in the quality control of the brewery. (E-2-nonenal was found in all beer samples analyzed with levels between 0.17 and 0.42 μg.L-1.O (E-2-nonenal é considerado um importante off-flavor da cerveja, sendo relacionado ao sabor de cerveja envelhecida. Neste estudo, um novo método para determinação de (E-2-nonenal em cerveja usando microextração em fase sólida do headspace e cromatografia a gás acoplada à espectrometria de massa (HS-SPME-GC-MS foi desenvolvido e aplicado em amostras de cerveja brasileira. As extrações foram realizadas utilizando a fibra CAR/PDMS (carboxen/polidimetilsiloxano, com 15 minutos de tempo de equilíbrio e 90 minutos de exposição da fibra a 50 °C. O método foi linear na faixa de 0,02 e 4,0 μg.L-1, com coeficiente de correlação de 0,9994. Os limites de detecção e quantificação foram 0,01 e 0,02 μg.L-1, respectivamente. Foram obtidos 96,5% de recuperação e 4% de variação entre replicatas de amostras de cerveja fortificadas com 2,0 μg.L-1 de (E-2-nonenal. O m

  7. Canonical sampling of a lattice gas

    International Nuclear Information System (INIS)

    Mueller, W.F.

    1997-01-01

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

  8. Data Base Management Plan for the remedial investigation of Waste Area Grouping 10, Operable Unit 3, at Oak Ridge National Laboratory, Oak Ridge, Tennessee

    International Nuclear Information System (INIS)

    1993-10-01

    This Data Base Management Plan describes the gathering, verifying, analyzing, reporting, and archiving of data generated during the remedial investigation of Waste Area Grouping 10, Operable Unit 3. This investigation will produce data documenting wellhead surveys, well headspace gas pressure measurements, geophysical surveys, water level measurements, and borehole geophysical logs. Close Support Laboratory analyses will be performed on well headspace gas and well water samples

  9. Diffusion probe for gas sampling in undisturbed soil

    DEFF Research Database (Denmark)

    Petersen, Søren O

    2014-01-01

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

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

    International Nuclear Information System (INIS)

    2009-11-01

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

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

    Science.gov (United States)

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

    1998-04-21

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

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

    Science.gov (United States)

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

    2015-07-15

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

  13. Method development and optimization for the determination of benzene, toluene, ethylbenzene and xylenes in water at trace levels by static headspace extraction coupled to gas chromatography-barrier ionization discharge detection.

    Science.gov (United States)

    Pascale, Raffaella; Bianco, Giuliana; Calace, Stefania; Masi, Salvatore; Mancini, Ignazio M; Mazzone, Giuseppina; Caniani, Donatella

    2018-05-04

    Benzene, toluene, ethylbenzene, and xylenes, more commonly named BTEX, represent one of the most ubiquitous and hazardous groups of atmospheric pollutants. The goal of our research was the trace quantification of BTEX in water by using a new simple, low-cost, and accurate method, based on headspace (HS) extraction and gas chromatography (GC) coupled to barrier ionization discharge detector (BID). This water application dealt with simple matrices without protein, fat, or humic material that adsorb target analytes, thus the external standard calibration was suitable to quantify each compound. The validation steps included the study of linearity, detection and quantification limits, and accuracy. LODs and LOQs varied from 0.159 to 1.845 μg/L and from 0.202 to 2.452 μg/L, respectively. The recovery was between 0.74 ± 0.13 and 1.15 ± 0.09; relative standard deviations (% RDSs) were less than 12.81% (n = 5) and 14.84% (n = 10). Also, GC performance was evaluated in term of efficiency, peak tailing and resolution. Preliminary results from practical applications to analyses of real samples are presented. The results indicate that static HS coupled to GC-BID is a successful method for BTEX analysis in water samples at the μg/L levels, provided that hydrocarbons interference occur at similar concentration levels. GC-BID may become a routine reference method alongside the official analytical techniques for quality control purposes of contaminated waters. Moreover, the new method is amenable to automation by using commercial HS units. Copyright © 2018. Published by Elsevier B.V.

  14. Approaches of aroma extraction dilution analysis (AEDA) for headspace solid phase microextraction and gas chromatography-olfactometry (HS-SPME-GC-O): Altering sample amount, diluting the sample or adjusting split ratio?

    Science.gov (United States)

    Feng, Yunzi; Cai, Yu; Sun-Waterhouse, Dongxiao; Cui, Chun; Su, Guowan; Lin, Lianzhu; Zhao, Mouming

    2015-11-15

    Aroma extract dilution analysis (AEDA) is widely used for the screening of aroma-active compounds in gas chromatography-olfactometry (GC-O). In this study, three aroma dilution methods, (I) using different test sample volumes, (II) diluting samples, and (III) adjusting the GC injector split ratio, were compared for the analysis of volatiles by using HS-SPME-AEDA. Results showed that adjusting the GC injector split ratio (III) was the most desirable approach, based on the linearity relationships between Ln (normalised peak area) and Ln (normalised flavour dilution factors). Thereafter this dilution method was applied in the analysis of aroma-active compounds in Japanese soy sauce and 36 key odorants were found in this study. The most intense aroma-active components in Japanese soy sauce were: ethyl 2-methylpropanoate, ethyl 2-methylbutanoate, ethyl 3-methylbutanoate, ethyl 4-methylpentanoate, 3-(methylthio)propanal, 1-octen-3-ol, 2-methoxyphenol, 4-ethyl-2-methoxyphenol, 2-methoxy-4-vinylphenol, 2-phenylethanol, and 4-hydroxy-5-ethyl-2-methyl-3(2H)-furanone. Copyright © 2015. Published by Elsevier Ltd.

  15. Evaluation of volatile profiles obtained for minimally-processed pineapple fruit samples during storage by headspace-solid phase microextraction gas chromatography-mass spectrometry

    Directory of Open Access Journals (Sweden)

    Francielle Crocetta TURAZZI

    Full Text Available Abstract This paper describes the application of the solid-phase microextraction (SPME technique for the determination and monitoring of the volatile profile of minimally-processed pineapple fruit stored at various temperatures (-12 °C, 4 °C and 25 °C for different periods (1, 4 and 10 days. The SPME fiber coating composed of Car/PDMS presented the best performance. The optimal extraction conditions obtained through a Doehlert design were 60 min at 35 °C. The profiles for the volatile compounds content of the fruit at each stage of storage were determined by gas chromatography-mass spectrometry (GC-MS. The variation in the volatile profile over time was greater when the fruit samples were stored at 25 °C and at -12 °C compared to 4 °C. Thus, according to the volatile profiles associated with the storage conditions evaluated in this study, packaged pineapple retains best its fresh fruit aroma when stored at 4 °C.

  16. Determination of biodegradation process of benzene, toluene, ethylbenzene and xylenes in seabed sediment by purge and trap gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Han, Dongqiang [Key Lab. for Atomic and Molecular Nanosciences of Education Ministry, Tsinghua Univ., Beijing (China). Dept. of Physics; China Pharmaceutical Univ., Nanjing (China). Physics Teaching and Research Section, Dept. of Basic Sciences; Ma, Wanyun; Chen, Dieyan [Key Lab. for Atomic and Molecular Nanosciences of Education Ministry, Tsinghua Univ., Beijing (China). Dept. of Physics

    2007-12-15

    Benzene, toluene, ethylbenzene, and xylenes (BTEX) are commonly found in crude oil and are used in geochemical investigations as direct indicators of the presence of oil and gas. BTEX are easily volatile and can be degraded by microorganisms, which affect their precise measurement seriously. A method for determining the biodegradation process of BTEX in seabed sediment using dynamic headspace (purge and trap) gas chromatography with a photoionization detector (PID) was developed, which had a detection limit of 7.3-13.2 ng L{sup -1} and a recovery rate of 91.6-95.0%. The decrease in the concentration of BTEX components was monitored in seabed sediment samples, which was caused by microorganism biodegradation. The results of BTEX biodegradation process were of great significance in the collection, transportation, preservation, and measurement of seabed sediment samples in the geochemical investigations of oil and gas. (orig.)

  17. Vapor space characterization of Waste Tank 241-TY-104: Results from samples collected on 4/27/95

    International Nuclear Information System (INIS)

    Klinger, G.S.; Olsen, K.B.; Clauss, T.W.

    1995-10-01

    This report describes inorganic and organic analyses results from samples obtained from the headspace of the Hanford waste storage Tank 241-TY-104 (referred to as Tank TY-104). The results described here were obtained to support safety and toxicological evaluations. A summary of the results for inorganic and organic analytes is listed in Table 1. Detailed descriptions of the results appear in the text. Quantitative results were obtained for the inorganic compounds ammonia (NH 3 ), nitrogen dioxide (NO 2 ), nitric oxide (NO), and water (H 2 O). Sampling for hydrogen cyanide (HCN) and sulfur oxides (SO x ) was not requested. In addition, quantitative results were obtained for the 39 TO-14 compounds plus an additional 14 analytes. Of these, 8 were observed above the 5-ppbv reporting cutoff. Five tentatively identified compounds (TICs) were observed above the reporting cutoff of (ca.) 10 ppbv and are reported with concentrations that are semiquantitative estimates based on internal-standard response factors. The 10 organic analytes with the highest estimated concentrations are listed in Table 1 and account for approximately 94% of the total organic components in Tank TY-104. Nitrous oxide (N 2 O) was the only permanent gas detected in the tank-headspace samples. Tank TY-104 is on the Ferrocyanide Watch List

  18. Vapor space characterization of Waste Tank 241-U-105: Results from samples collected on 2/24/95

    International Nuclear Information System (INIS)

    Pool, K.H.; Clauss, T.W.; Ligotke, M.W.

    1995-10-01

    This report describes inorganic and organic analyses results from samples obtained from the headspace of the Hanford waste storage Tank 241-U-105 (referred to as Tank U-105). The results described here were obtained to support safety and toxicological evaluations. A summary of the results for inorganic and organic analytes is listed in Table 1. Detailed descriptions of the results appear in the text. Quantitative results were obtained for the inorganic compounds ammonia (NH 3 ), nitrogen dioxide (NO 2 ), nitric oxide (NO), and water (H 2 O). Sampling for hydrogen cyanide (HCN) and sulfur oxides (SO x ) was not requested. In addition, quantitative results were obtained for the 39 TO-14 compounds plus an additional 14 analytes. Of these, six were observed above the 5-ppbv reporting cutoff. Three tentatively identified compounds (TICs) were observed above the reporting cutoff of (ca.) 10 ppbv and are reported with concentrations that are semiquantitative estimates based on internal-standard response factors. All nine of the organic analytes identified are listed in Table 1 and account for 100% of the total organic components in Tank U-105. Nitrous oxide (N 2 O) was the only permanent gas detected in the tank-headspace sample. Tank U-105 is on the Hydrogen Watch List

  19. Vapor space characterization of waste Tank 241-SX-103: Results from samples collected on 3/23/95

    International Nuclear Information System (INIS)

    Ligotke, M.W.; Clauss, T.W.; Pool, K.H.; McVeety, B.D.; Klinger, G.S.; Olsen, K.B.; Bredt, O.P.; Fruchter, J.S.; Goheen, S.C.

    1995-11-01

    This report describes inorganic and organic analyses results from samples obtained from the headspace of the Hanford waste storage tank 241-SX-103 (referred to as Tank SX-103). The results described here were obtained to support safety and toxicological evaluations. A summary of the results for inorganic and organic analytes is listed in Table 1. Detailed descriptions of the results appear in the text. Quantitative results were obtained for the inorganic compounds ammonia (NH 3 ), nitrogen dioxide (NO 2 ), nitric oxide (NO), and water vapor (H 2 O). Sampling for hydrogen cyanide (HCN) and sulfur oxides (SO x ) was not requested. In addition, quantitative results were obtained for the 39 TO-14 compounds plus an additional 14 analytes. Of these, two were observed above the 5-ppbv reporting cutoff. Two tentatively identified compounds (TICs) were observed above the reporting cutoff of (ca.) 10 ppbv and are reported with concentrations that are semiquantitative estimates based on internal-standard response factors. The four organic analytes identified are listed in Table 1 and account for approximately 100% of the total organic components in Tank SX-103. Carbon dioxide (CO 2 ) was the only permanent gas detected in the tank-headspace samples. Tank SX-103 is on the Hydrogen Watch List

  20. Coumarins as turn on/off fluorescent probes for detection of residual acetone in cosmetics following headspace single-drop microextraction.

    Science.gov (United States)

    Cabaleiro, N; de la Calle, I; Bendicho, C; Lavilla, I

    2014-11-01

    In this work, a new method based on headspace-single drop microextraction for the determination of residual acetone in cosmetics by microfluorospectrometry is proposed. Acetone causes fluorescence changes in a 2.5 µL-ethanolic drop (40% v/v) containing 3.10(-4) mol L(-1) 7-hydroxy-4-methylcoumarin ('turn off') or 6.10(-6) mol L(-1) 7-diethylamino-4-methylcoumarin ('turn on'). Polarity and ability to form hydrogen bonds of short chain alcohols (polar protic solvents) were crucial in order to observe these changes in the presence of acetone (polar aprotic solvent). Parameters related with the HS-SDME procedure were studied, namely headspace volume, composition, volume and temperature of drop, microextraction time, stirring rate, mass and temperature of sample, as well as the effect of potential interferents (alcohols and fragrances). The high volatility of acetone allows its extraction from an untreated cosmetic sample within 3 min. A detection limit of 0.26 µg g(-1) and repeatability, expressed as relative standard deviation, around 5% were reached. Accuracy of the proposed methodology was evaluated by means of recovery studies. The method was successfully used to analyze different cosmetics. Simplicity and high sample throughput can be highlighted. Copyright © 2014 Elsevier B.V. All rights reserved.

  1. SPME-GC-MS analysis of commercial henna samples (Lawsonia inermis L.).

    Science.gov (United States)

    Mengoni, Tamara; Peregrina, Dolores Vargas; Censi, Roberta; Cortese, Manuela; Ricciutelli, Massimo; Maggi, Filippo; Di Martino, Piera

    2016-01-01

    The aim of this work was to provide a characterisation of volatile constituents from different commercial batches of henna (Lawsonia inermis) leaves of different geographic origin. Headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC-MS) was used for the purpose. A total of 72 components were identified by GC-MS in the headspace of different henna samples which proved to differ considerably from each other, because they were characterised by different classes of components, mainly aliphatic compounds (9.0-64.7%), terpenoids (5.8-45.5%) and aromatics (7.9-45.2%), with alkanes (0.9-18.5%), aldehydes (2.1-18.8%) and carboxylic acids (3.1-29.3%), monoterpenes (3.4-30.0%) and sesquiterpenes (0.8-23.7%) and phenyl propanoids (0.6-43.1%), being the most abundant, respectively. Major representatives of these groups were n-hexadecane (0.5-4.7%), (2E)-hexenal (0.5-11.7%) and acetic acid (2.8-24.5%), limonene (0.8-14.7%), carvol (3.8-7.1%), geranyl acetone (1.4-7.9%) and (E)-caryophyllene (3.3-8.4%), and (E)-anethole (0.6-35.0%), respectively. We assume that factors such as the manufacturing process, the storage conditions and the different geographic origin of the samples may contribute to such variability.

  2. An interior needle electropolymerized pyrrole-based coating for headspace solid-phase dynamic extraction

    Energy Technology Data Exchange (ETDEWEB)

    Bagheri, Habib [Department of Chemistry, Sharif University of Technology, Azadi Av., P.O. Box 11365-9516, Tehran (Iran, Islamic Republic of)], E-mail: bagheri@sharif.edu; Babanezhad, Esmaeil; Khalilian, Faezeh [Department of Chemistry, Sharif University of Technology, Azadi Av., P.O. Box 11365-9516, Tehran (Iran, Islamic Republic of)

    2009-02-23

    A headspace solid-phase dynamic extraction (HS-SPDE) technique was developed by the use of polypyrrole (PPy) sorbent, electropolymerized inside the surface of a needle, as a possible alternative to solid-phase microextraction (SPME). Thermal desorption was subsequently, employed to transfer the extracted analytes into the injection port of a gas chromatography-mass spectrometry (GC-MS). The PPy sorbent including polypyrrole-dodecyl sulfate (PPy-DS) was deposited on the interior surface of a stainless steel needle from the corresponding aqueous electrolyte by applying a constant deposition potential. The homogeneity and the porous surface structure of the coating were examined using the scanning electron microscopy (SEM). The developed method was applied to the trace level extraction of some polycyclic aromatic hydrocarbons (PAHs) from aqueous sample. In order to enhance the extraction efficiency and increase the partition coefficient of analytes, the stainless steel needle was cooled at 5 deg. C, while the sample solution was kept at 80 deg. C. Optimization of influential experimental conditions including the voltage of power supply, the time of PPy electrodeposition, the extraction temperature, the ionic strength and the extraction time were also investigated. The detection limits of the method under optimized conditions were in the range of 0.002-0.01 ng mL{sup -1}. The relative standard deviations (R.S.D.) at a concentration level of 0.1 ng mL{sup -1} were obtained between 7.54 and 11.4% (n = 6). The calibration curves of PAHs showed linearity in the range of 0.01-10 ng mL{sup -1}. The proposed method was successfully applied to the extraction of some selected PAHs from real-life water samples and the relative recoveries were higher than 90% for all the analytes.

  3. Quality control of raw cows' milk by headspace analysis

    NARCIS (Netherlands)

    Hettinga, K.A.; Valenberg, van H.J.F.; Hooijdonk, van A.C.M.

    2008-01-01

    This study investigated whether headspace analysis of volatile components can be used for monitoring the quality of raw cows¿ milk. The detection of different quality defects caused by cows¿ feed, microbiological and chemical contamination, as well as enzymatic deterioration was studied. Fresh raw

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

    Science.gov (United States)

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

  5. SPME GC/MS determination of organochlorine pesticides in water samples

    Directory of Open Access Journals (Sweden)

    Yerbolat Sailaukhanuly

    2013-05-01

    Full Text Available Headspace solid phase microextraction (HS-SPME in combination with gas chromatography and mass-spectrometry (GC/MS was studied for analysis of water samples. The organochlorine pesticides (OCPs, p,p'-DDT, p,p'-DDD, and p,p'-DDE were collected and analyzed by GC/MS. To select of effective fiber coatings four types of SPME fibers were examined and compared. The parameters effecting the efficiency of HS-SPME such as extraction and pre-incubation time and extraction temperature, effect of solvent nature, ionic strength were studied to obtain optimal parameters. The method was developed using spiked water samples in a concentration range  10 - 500 ng/L. The calibration curve was linear over the studied concentration range with r≥0.9925. The detection limits varied from 1.57 to 2.08 ng/L. An authentic water samples from contaminated lake with OCPs were analyzed by developed method.

  6. Quantification of 2-acetyl-1-pyrroline in rice by stable isotope dilution assay through headspace solid-phase microextraction coupled to gas chromatography-tandem mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Maraval, Isabelle [UMR Qualisud, CIRAD, 73 Rue J. F. Breton, 34398 Montpellier Cedex 5 (France); UMR Qualisud, Universite Montpellier 2, place E. Bataillon, 34095 Montpellier Cedex 5 (France); Sen, Kemal [Department of Food Engineering, Faculty of Agriculture, University of Cukurova, 01330 Adana (Turkey); Agrebi, Abdelhamid; Menut, Chantal; Morere, Alain [UMR 5247, Institut des Biomolecules Max Mousseron (IBMM), CNRS, Universites Montpellier 2 et 1, Ecole Nationale Superieure de Chimie de Montpellier, 8 Rue de l' Ecole Normale, 34296 Montpellier Cedex 5 (France); Boulanger, Renaud [UMR Qualisud, CIRAD, 73 Rue J. F. Breton, 34398 Montpellier Cedex 5 (France); Gay, Frederic [CIRAD, DORAS Centre, Research and Development Building, Kasetsart University, Bangkok 10900 (Thailand); Mestres, Christian [UMR Qualisud, CIRAD, 73 Rue J. F. Breton, 34398 Montpellier Cedex 5 (France); Gunata, Ziya, E-mail: zgunata@univ-montp2.fr [UMR Qualisud, Universite Montpellier 2, place E. Bataillon, 34095 Montpellier Cedex 5 (France)

    2010-08-24

    A new and convenient synthesis of 2-acetyl-1-pyrroline (2AP), a potent flavor compound in rice, and its ring-deuterated analog, 2-acetyl-1-d{sub 2}-pyrroline (2AP-d{sub 2}), was reported. A stable isotope dilution assay (SIDA), involving headspace solid-phase microextraction (HS-SPME) combined with gas chromatography-positive chemical ionization-ion trap-tandem mass spectrometry (GC-PCI-IT-MS-MS), was developed for 2AP quantification. A divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) fiber was used for HS-SPME procedure and parameters affecting analytes recovery, such as extraction time and temperature, pH and salt, were studied. The repeatability of the method (n = 10) expressed as relative standard deviation (RSD) was 11.6%. A good linearity was observed from 5.9 to 779 ng of 2AP (r{sup 2} = 0.9989). Limits of detection (LOD) and quantification (LOQ) for 2AP were 0.1 and 0.4 ng g{sup -1} of rice, respectively. The recovery of spiked 2AP from rice matrix was almost complete. The developed method was applied to the quantification of 2AP in aerial parts and grains of scented and non-scented rice cultivars.

  7. Integrated sampling and analysis unit for the determination of sexual pheromones in environmental air using fabric phase sorptive extraction and headspace-gas chromatography-mass spectrometry.

    Science.gov (United States)

    Alcudia-León, M Carmen; Lucena, Rafael; Cárdenas, Soledad; Valcárcel, Miguel; Kabir, Abuzar; Furton, Kenneth G

    2017-03-10

    This article presents a novel unit that integrates for the first time air sampling and preconcentration based on the use of fabric phase sorptive extraction principles. The determination of Tuta absoluta sexual pheromone traces in environmental air has been selected as analytical problem. For this aim, a novel laboratory-built unit made up of commercial brass elements as holder of the sol-gel coated fabric extracting phase has been designed and optimized. The performance of the integrated unit was evaluated analyzing environmental air sampled in tomato crops. The unit can work under sampling and analysis mode which eliminates any need for sorptive phase manipulation prior to instrumental analysis. In the sampling mode, the unit can be connected to a sampling pump to pass the air through the sorptive phase at a controlled flow-rate. In the analysis mode, it is placed in the gas chromatograph autosampler without any instrumental modification. It also diminishes the risk of cross contamination between sampling and analysis. The performance of the new unit has been evaluated using the main components of the sexual pheromone of Tuta absoluta [(3E,8Z,11Z)-tetradecatrien-1-yl acetate and (3E,8Z)-tetradecadien-1-yl acetate] as model analytes. The limits of detection for both compounds resulted to be 1.6μg and 0.8μg, respectively, while the precision (expressed as relative standard deviation) was better than 3.7%. Finally, the unit has been deployed in the field to analyze a number of real life samples, some of them were found positive. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. The effect of surfactant on headspace single drop microextraction for the determination of some volatile aroma compounds in citronella grass and lemongrass leaves by gas chromatography

    Science.gov (United States)

    A rapid method for the determination of some volatile aromatic compounds (VACs), including citronellal, citronellol, neral, geranial, geraniol, and eugenol in citronella grass and lemongrass leaves, was developed using surfactant as a surface tension modifier while performing headspace single drop m...

  9. Graphene deposited onto aligned zinc oxide nanorods as an efficient coating for headspace solid-phase microextraction of gasoline fractions from oil samples.

    Science.gov (United States)

    Wen, Congying; Li, Mengmeng; Li, Wangbo; Li, Zizhou; Duan, Wei; Li, Yulong; Zhou, Jie; Li, Xiyou; Zeng, Jingbin

    2017-12-29

    The content of gasoline fraction in oil samples is not only an important indicator of oil quality, but also an indispensable fundamental data for oil refining and processing. Before its determination, efficient preconcentration and separation of gasoline fractions from complicated matrices is essential. In this work, a thin layer of graphene (G) was deposited onto oriented ZnO nanorods (ZNRs) as a SPME coating. By this approach, the surface area of G was greatly enhanced by the aligned ZNRs, and the surface polarity of ZNRs was changed from polar to less polar, which were both beneficial for the extraction of gasoline fractions. In addition, the ZNRs were well protected by the mechanically and chemically stable G, making the coating highly durable for use. With headspace SPME (HS-SPME) mode, the G/ZNRs coating can effectively extract gasoline fractions from various oil samples, whose extraction efficiency achieved 1.5-5.4 and 2.1-8.2 times higher than those of a G and commercial 7-μm PDMS coating respectively. Coupled with GC-FID, the developed method is sensitive, simple, cost effective and easily accessible for the analysis of gasoline fractions. Moreover, the method is also feasible for the detection of gasoline markers in simulated oil-polluted water, which provides an option for the monitoring of oil spill accident. Copyright © 2017 Elsevier B.V. All rights reserved.

  10. Flight attraction of Spodoptera littoralis (Lepidoptera, Noctuidae to cotton headspace and synthetic volatile blends

    Directory of Open Access Journals (Sweden)

    Felipe eBorrero-Echeverry

    2015-06-01

    Full Text Available The insect olfactory system discriminates odor signals of different biological relevance, which drive innate behavior. Identification of stimuli that trigger upwind flight attraction towards host plants is a current challenge, and is essential in developing new, sustainable plant protection methods, and for furthering our understanding of plant-insect interactions. Using behavioral, analytical and electrophysiological studies, we here show that both females and males of the Egyptian cotton leafworm, Spodoptera littoralis (Lepidoptera, Noctuidae, use blends of volatile compounds to locate their host plant, cotton, Gossypium hirsutum (Malvales, Malvaceae. Female S. littoralis were engaged in upwind orientation flight in a wind tunnel when headspace collected from cotton plants was delivered through a piezoelectric sprayer. Although males took off towards cotton headspace significantly fewer males than females flew upwind towards the sprayed headspace. Subsequent assays with antennally active synthetic compounds revealed that a blend of nonanal, (Z-3 hexenyl acetate, (E-β-ocimene, and (R-(+-limonene was as attractive as cotton headspace to females and more attractive to males. DMNT and (R-(--linalool, both known plant defense compounds may have reduced the flight attraction of both females and males; more moths were attracted to blends without these two compounds. Our findings provide a platform for further investigations on host plant signals mediating innate behavior, and for the development of novel insect plant protection strategies against S. littoralis.

  11. Multivariate analysis of volatile compounds detected by headspace solid-phase microextraction/gas chromatography: A tool for sensory classification of cork stoppers.

    Science.gov (United States)

    Prat, Chantal; Besalú, Emili; Bañeras, Lluís; Anticó, Enriqueta

    2011-06-15

    The volatile fraction of aqueous cork macerates of tainted and non-tainted agglomerate cork stoppers was analysed by headspace solid-phase microextraction (HS-SPME)/gas chromatography. Twenty compounds containing terpenoids, aliphatic alcohols, lignin-related compounds and others were selected and analysed in individual corks. Cork stoppers were previously classified in six different classes according to sensory descriptions including, 2,4,6-trichloroanisole taint and other frequent, non-characteristic odours found in cork. A multivariate analysis of the chromatographic data of 20 selected chemical compounds using linear discriminant analysis models helped in the differentiation of the a priori made groups. The discriminant model selected five compounds as the best combination. Selected compounds appear in the model in the following order; 2,4,6 TCA, fenchyl alcohol, 1-octen-3-ol, benzyl alcohol and benzothiazole. Unfortunately, not all six a priori differentiated sensory classes were clearly discriminated in the model, probably indicating that no measurable differences exist in the chromatographic data for some categories. The predictive analyses of a refined model in which two sensory classes were fused together resulted in a good classification. Prediction rates of control (non-tainted), TCA, musty-earthy-vegetative, vegetative and chemical descriptions were 100%, 100%, 85%, 67.3% and 100%, respectively, when the modified model was used. The multivariate analysis of chromatographic data will help in the classification of stoppers and provide a perfect complement to sensory analyses. Copyright © 2010 Elsevier Ltd. All rights reserved.

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

    NARCIS (Netherlands)

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

    2004-01-01

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

  13. Determination of different recreational drugs in sweat by headspace solid-phase microextraction gas chromatography mass spectrometry (HS-SPME GC/MS): Application to drugged drivers.

    Science.gov (United States)

    Gentili, Stefano; Mortali, Claudia; Mastrobattista, Luisa; Berretta, Paolo; Zaami, Simona

    2016-09-10

    A procedure based on headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography/mass spectrometry (GC/MS) has been developed for the determination of most commonly used drugs of abuse in sweat of drivers stopped during roadside controls. DrugWipe 5A sweat screening device was used to collect sweat by a specific pad rubbed gently over forehead skin surface. The procedure involved an acid hydrolysis, a HS-SPME extraction for drugs of abuse but Δ(9)-tetrahydrocannabinol, which was directly extracted in alkaline medium HS-SPME conditions, a GC separation of analytes by a capillary column and MS detection by electron impact ionisation. The method was linear from the limit of quantification (LOQ) to 50ng drug per pad (r(2)≥0.99), with an intra- and inter-assay precision and accuracy always less than 15% and an analytical recovery between 95.1% and 102.8%, depending on the considered analyte. Using the validated method, sweat from 60 apparently intoxicated drivers were found positive to one or more drugs of abuse, showing sweat patches testing as a viable economic and simple alternative to conventional (blood and/or urine) and non conventional (oral fluid) testing of drugs of abuse in drugged drivers. Copyright © 2016 Elsevier B.V. All rights reserved.

  14. Gas generation from Hanford grout samples

    International Nuclear Information System (INIS)

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

    1996-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Sriram Valavala

    2018-01-01

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

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

    International Nuclear Information System (INIS)

    Pitkoff, C.C.

    1995-01-01

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

  17. Quality Assurance Project Plan for the Gas Generation Testing Program at the INEL

    International Nuclear Information System (INIS)

    1994-10-01

    The data quality objectives (DQOs) for the Program are to evaluate compliance with the limits on total gas generation rates, establish the concentrations of hydrogen and methane in the total gas flow, determine the headspace concentration of VOCs in each drum prior to the start of the test, and obtain estimates of the concentrations of several compounds for mass balance purposes. Criteria for the selection of waste containers at the INEL and the parameters that must be characterized prior to and during the tests are described. Collection of gaseous samples from 55-gallon drums of contact-handled transuranic waste for the gas generation testing is discussed. Analytical methods and calibrations are summarized. Administrative quality control measures described in this QAPjP include the generation, review, and approval of project documentation; control and retention of records; measures to ensure that personnel, subcontractors or vendors, and equipment meet the specifications necessary to achieve the required data quality for the project

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

    OpenAIRE

    sprotocols

    2015-01-01

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

  19. Vapor space characterization of Waste Tank 241-U-107: Results from samples collected on 2/17/95

    International Nuclear Information System (INIS)

    McVeety, B.D.; Clauss, T.W.; Ligotke, M.W.

    1995-10-01

    This report describes inorganic and organic analyses results from samples obtained from the headspace of the Hanford waste storage Tank 241-U-107 (referred to as Tank U-107). The results described here were obtained to support safety and toxicological evaluations. A summary of the results for inorganic and organic analytes is listed in Table 1. Detailed descriptions of the results appear in the text. Quantitative results were obtained for the inorganic compounds ammonia (NH 3 ), nitrogen dioxide (NO 2 ), nitric oxide (NO), and water (H 2 O). Sampling for hydrogen cyanide (HCN) and sulfur oxides (SO x ) was not requested. In addition, quantitative results were obtained for the 39 TO-14 compounds plus an additional 14 analytes. Of these, 10 were observed above the 5-ppbv reporting cutoff. Sixteen organic tentatively identified compounds (TICs) were observed above the reporting cutoff of (ca.) 10 ppbv, and are reported with concentrations that are semiquantitative estimates based on internal-standard response factors. The 10 organic analytes with the highest estimated concentrations are listed in Table 1 and account for approximately 88% of the total organic components in Tank U-107. Nitrous oxide (N 2 O) was the only permanent gas detected in the tank-headspace samples. Tank U-107 is on the Organic and the Hydrogen Watch Lists

  20. PlanetVac: Sample Return with a Puff of Gas

    Science.gov (United States)

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

    2014-12-01

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

  1. Assessment of gas flammability in transuranic waste container

    International Nuclear Information System (INIS)

    Connolly, M.J.; Loehr, C.A.; Djordjevic, S.M.; Spangler, L.R.

    1995-01-01

    The Safety Analysis Report for the TRUPACT-II Shipping Package [Transuranic Package Transporter-II (TRUPACT-II) SARP] set limits for gas generation rates, wattage limits, and flammable volatile organic compound (VOC) concentrations in transuranic (TRU) waste containers that would be shipped to the Waste Isolation Pilot Plant (WIPP). Based on existing headspace gas data for drums stored at the Idaho National Engineering Laboratory (INEL) and the Rocky Flats Environmental Technology Site (RFETS), over 30 percent of the contact-handled TRU waste drums contain flammable VOC concentrations greater than the limit. Additional requirements may be imposed for emplacement of waste in the WIPP facility. The conditional no-migration determination (NMD) for the test phase of the facility required that flame tests be performed if significant levels of flammable VOCs were present in TRU waste containers. This paper describes an approach for investigating the potential flammability of TRU waste drums, which would increase the allowable concentrations of flammable VOCS. A flammability assessment methodology is presented that will allow more drums to be shipped to WIPP without treatment or repackaging and reduce the need for flame testing on drums. The approach includes experimental work to determine mixture lower explosive limits (MLEL) for the types of gas mixtures observed in TRU waste, a model for predicting the MLEL for mixtures of VOCS, hydrogen, and methane, and revised screening limits for total flammable VOCs concentrations and concentrations of hydrogen and methane using existing drum headspace gas data and the model predictions

  2. Influence of harvest maturity and fruit logistics on pineapple (Ananas comosus [L.] Merr.) volatiles assessed by headspace solid phase microextraction and gas chromatography-mass spectrometry (HS-SPME-GC/MS).

    Science.gov (United States)

    Steingass, Christof B; Grauwet, Tara; Carle, Reinhold

    2014-05-01

    Profiling of volatiles from pineapple fruits was performed at four ripening stages using headspace solid-phase microextraction and gas chromatography-mass spectrometry (HS-SPME-GC/MS). In total, 142 volatiles were detected, of which 132 were identified. Multivariate data analysis was carried out to assess the effect of post-harvest storage on volatiles composition of green-ripe sea-freighted pineapple in comparison to air-freighted fruits harvested at full maturity. The latter fruits were characterised by volatiles described as potent odorants in pineapples, such as δ-octalactone, γ-lactones, 1-(E,Z)-3,5-undecatriene and 1,3,5,8-undecatetraene, as well as various methyl esters. In contrast, post-harvest storage of green-ripe sea-freighted fruits resulted in an increased formation of ethyl esters, acetates, acetoxy esters and alcohols, thus allowing the authentication of sea- and air-freighted pineapples, respectively. Particularly, compounds presumably derived from methyl-branched amino acid catabolism were identified in the fruits at later post-harvest stages. In addition, physicochemical traits were determined to characterise the fruit maturity stages. Copyright © 2013 Elsevier Ltd. All rights reserved.

  3. 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

  4. Multivariate optimization of a headspace solid-phase microextraction method followed by gas chromatography with mass spectrometry for the determination of terpenes in Nicotiana langsdorffii.

    Science.gov (United States)

    Ardini, Francisco; Carro, Marina Di; Abelmoschi, Maria Luisa; Grotti, Marco; Magi, Emanuele

    2014-07-01

    A simple and sensitive procedure based on headspace solid-phase microextraction and gas chromatography with mass spectrometry was developed for the determination of five terpenes (α-pinene, limonene, linalool, α-terpineol, and geraniol) in the leaves of Nicotiana langsdorffii. The microextraction conditions (extraction temperature, equilibration time, and extraction time) were optimized by means of a Doehlert design. The experimental design showed that, for α-pinene and limonene, a low temperature and a long extraction time were needed for optimal extraction, while linalool, α-terpineol, and geraniol required a high temperature and a long extraction time. The chosen compromise conditions were temperature 60°C, equilibration time 15 min and extraction time 50 min. The main analytical figures of the optimized method were evaluated; LODs ranged from 0.07 ng/g (α-pinene) to 8.0 ng/g (geraniol), while intraday and interday repeatability were in the range 10-17% and 9-13%, respectively. Finally, the procedure was applied to in vitro wild-type and transgenic specimens of N. langsdorffii subjected to abiotic stresses (chemical and heat stress). With the exception of geraniol (75-374 ng/g), low concentration levels of terpenes were measured (ng/g level or lower); some interesting variations in terpene concentration induced by abiotic stress were observed. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

    Science.gov (United States)

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

    2013-12-01

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

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

    NARCIS (Netherlands)

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

    1995-01-01

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

  7. Direct analysis of volatile organic compounds in foods by headspace extraction atmospheric pressure chemical ionisation mass spectrometry.

    Science.gov (United States)

    Perez-Hurtado, P; Palmer, E; Owen, T; Aldcroft, C; Allen, M H; Jones, J; Creaser, C S; Lindley, M R; Turner, M A; Reynolds, J C

    2017-11-30

    The rapid screening of volatile organic compounds (VOCs) by direct analysis has potential applications in the areas of food and flavour science. Currently, the technique of choice for VOC analysis is gas chromatography/mass spectrometry (GC/MS). However, the long chromatographic run times and elaborate sample preparation associated with this technique have led a movement towards direct analysis techniques, such as selected ion flow tube mass spectrometry (SIFT-MS), proton transfer reaction mass spectrometry (PTR-MS) and electronic noses. The work presented here describes the design and construction of a Venturi jet-pump-based modification for a compact mass spectrometer which enables the direct introduction of volatiles for qualitative and quantitative analysis. Volatile organic compounds were extracted from the headspace of heated vials into the atmospheric pressure chemical ionization source of a quadrupole mass spectrometer using a Venturi pump. Samples were analysed directly with no prior sample preparation. Principal component analysis (PCA) was used to differentiate between different classes of samples. The interface is shown to be able to routinely detect problem analytes such as fatty acids and biogenic amines without the requirement of a derivatisation step, and is shown to be able to discriminate between four different varieties of cheese with good intra and inter-day reproducibility using an unsupervised PCA model. Quantitative analysis is demonstrated using indole standards with limits of detection and quantification of 0.395 μg/mL and 1.316 μg/mL, respectively. The described methodology can routinely detect highly reactive analytes such as volatile fatty acids and diamines without the need for a derivatisation step or lengthy chromatographic separations. The capability of the system was demonstrated by discriminating between different varieties of cheese and monitoring the spoilage of meats. © 2017 The Authors. Rapid Communications in Mass

  8. Evaluation of gas chromatography-combustion-isotope ratio mass spectrometry (GC-C-IRMS) for the quality assessment of citrus liqueurs.

    Science.gov (United States)

    Schipilliti, Luisa; Bonaccorsi, Ivana; Cotroneo, Antonella; Dugo, Paola; Mondello, Luigi

    2013-02-27

    Citrus liqueurs are alcoholic beverages obtained by maceration. The European Parliament protects these alcoholic beverages, forbidding the addition of nature-identical flavoring substances. However, for economical and technological reasons, producers often add natural and/or synthetic flavors to the alcoholic syrup, obtaining artificial spirit drinks. The aim of this study is to investigate the authenticity of Italian liqueurs, of lemon, bergamot, and mandarin (locally known as "limoncello", "bargamino", and "mandarinetto"), comparing the carbon isotope ratios with values determined in genuine cold-pressed peel oils. Authenticity assessment was performed using headspace-solid phase microextraction coupled to gas chromatography-combustion-isotope ratio mass spectrometry. Additional analyses were performed by direct enantioselective gas chromatography to determine the enantiomeric distribution of selected chiral volatiles and by gas chromatography-mass spectrometry for the qualitative analyses of the samples. The method allowed confirmation of genuineness. Enantioselective gas chromatography analyses confirmed the results, demonstrating the reliability of the method.

  9. Hydride generation coupled to microfunnel-assisted headspace liquid-phase microextraction for the determination of arsenic with UV-Vis spectrophotometry.

    Science.gov (United States)

    Hashemniaye-Torshizi, Reihaneh; Ashraf, Narges; Arbab-Zavar, Mohammad Hossein

    2014-12-01

    In this research, a microfunnel-assisted headspace liquid-phase microextraction technique has been used in combination with hydride generation to determine arsenic (As) by UV-Vis spectrophotometry. The method is based on the reduction of As to arsine (AsH3) in acidic media by sodium tetrahydroborate (NaBH4) followed by its subsequent reaction with silver diethyldithiocarbamate (AgDDC) to give an absorbing complex at 510 nm. The complexing reagent (AgDDC) has been dissolved in a 1:1 (by the volume ratio) mixture of chloroform/chlorobenzene microdroplet and exposed to the generated gaseous arsine via a reversed microfunnel in the headspace of the sample solution. Several operating parameters affecting the performance of the method have been examined and optimized. Acetonitrile solvent has been added to the working samples as a sensitivity enhancement agent. Under the optimized operating conditions, the detection limit has been measured to be 0.2 ng mL(-1) (based on 3sb/m criterion, n b = 8), and the calibration curve was linear in the range of 0.5-12 ng mL(-1). The relative standard deviation for eight replicate measurements was 1.9 %. Also, the effects of several potential interferences have been studied. The accuracy of the method was validated through the analysis of JR-1 geological standard reference material. The method has been successfully applied for the determination of arsenic in raw and spiked soft drink and water samples with the recoveries that ranged from 91 to 106 %.

  10. Evaluation of solid-phase microextraction conditions for the determination of polycyclic aromatic hydrocarbons in aquatic species using gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Aguinaga, N.; Campillo, N.; Vinas, P.; Hernandez-Cordoba, M. [University of Murcia, Department of Analytical Chemistry, Faculty of Chemistry, Murcia (Spain)

    2008-06-15

    This paper describes a headspace solid-phase microextraction (HS-SPME) procedure coupled to gas chromatography with mass spectrometric detection (GC-MS) for the determination of eight PAHs in aquatic species. The influence of various parameters on the PAH extraction efficiency was carefully examined. At 75 C and for an extraction time of 60 min, a polydimethylsiloxane-divinylbenzene (PDMS/DVB) fiber coating was found to be most suitable. Under the optimized conditions, detection limits ranged from 8 to 450 pg g{sup -1}, depending on the compound and the sample matrix. The repeatability varied between 7 and 15% (RSD). Accuracy was tested using the NIST SRM 1974b reference material. The method was successfully applied to different samples, and the studied PAHs were detected in several of the samples. (orig.)

  11. Dynamic collection and analysis of volatile organic compounds from the headspace of cell cultures.

    Science.gov (United States)

    Baranska, A; Smolinska, A; Boots, A W; Dallinga, J W; van Schooten, F J

    2015-10-15

    interactions. Measurements were performed with gas chromatography time-of-flight mass spectrometry. Multivariate data analysis allowed detection of significant altered compounds in the compared groups. We found a significant change (p  ⩽  0.001) of the composition of VOCs due to the stressing of the Caco-2 cells by H2O2. A total of ten VOCs showed either increased or decreased abundance in the headspace of the cell cultures due to the presence of the H2O2 stressor.

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

    Science.gov (United States)

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

    2012-08-21

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

  13. Determination of volatile polycyclic aromatic hydrocarbons in waters using headspace solid-phase microextraction with a benzyl-functionalized crosslinked polymeric ionic liquid coating.

    Science.gov (United States)

    Merdivan, Melek; Pino, Verónica; Anderson, Jared L

    2017-08-01

    A benzyl-functionalized crosslinked polymeric ionic liquid (PIL), produced through the co-polymerization of the 1-vinylbenzyl-3-hexadecylimidazolium bis[(trifluoromethyl)sulfonyl]imide (VBHDIM-NTf 2 ) ionic liquid (IL) monomer and 1,12-di(3-vinylbenzylimidazolium)dodecane bis[(trifluoromethyl)sulfonyl]imide ((DVBIM) 2 C 12- 2NTf 2 ) IL crosslinker, was successfully used as a sorbent coating in headspace solid-phase microextraction (SPME) coupled to gas chromatography (GC) with flame-ionization detection (FID) to determine seven volatile polycyclic aromatic hydrocarbons (PAHs) in environmental water samples. Optimum extraction conditions for the PAHs when using the novel sorbent include an extraction temperature of 50°C, an ionic strength content adjusted with 30% (w/v) NaCl in the aqueous sample, and an extraction time of 60 min. The extraction performance of the crosslinked PIL fiber was compared to the SPME commercial coating polydimethylsiloxane fiber. The calibration ranges of the studied PAHs were linear in the range of 0.02-20 µg L -1 for the crosslinked PIL fiber. The accuracy of the proposed method was demonstrated by examining the spiked recoveries of seven PAHs which produced values ranging from 67.2% to 130% (for river- and seawater samples), and precision values lower than 9.4% for a spiked level of 1 µg L -1 , and detection limits between 0.01 and 0.04 µg L -1 , which supports the sensitivity of the method using GC-FID.

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

    International Nuclear Information System (INIS)

    Donguy, R.; Drouet, J.

    1959-06-01

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

  15. Headspace screening: A novel approach for fast quality assessment of the essential oil from culinary sage.

    Science.gov (United States)

    Cvetkovikj, Ivana; Stefkov, Gjoshe; Acevska, Jelena; Karapandzova, Marija; Dimitrovska, Aneta; Kulevanova, Svetlana

    2016-07-01

    Quality assessment of essential oil (EO) from culinary sage (Salvia officinalis L., Lamiaceae) is limited by the long pharmacopoeial procedure. The aim of this study was to employ headspace (HS) sampling in the quality assessment of sage EO. Different populations (30) of culinary sage were assessed using GC/FID/MS analysis of the hydrodistilled EO (pharmacopoeial method) and HS sampling directly from leaves. Compound profiles from both procedures were evaluated according to ISO 9909 and GDC standards for sage EO quality, revealing compliance for only 10 populations. Factors to convert HS values, for the target ISO and GDC components, into theoretical EO values were calculated. Statistical analysis revealed a significant relationship between HS and EO values for seven target components. Consequently, HS sampling could be used as a complementary extraction technique for rapid screening in quality assessment of sage EOs. Copyright © 2016 Elsevier Ltd. All rights reserved.

  16. An Effective Method to Detect Volatile Intermediates Generated in the Bioconversion of Coal to Methane by Gas Chromatography-Mass Spectrometry after In-Situ Extraction Using Headspace Solid-Phase Micro-Extraction under Strict Anaerobic Conditions.

    Science.gov (United States)

    Liu, Jianmin; Wang, Baoyu; Tai, Chao; Wu, Li; Zhao, Han; Guan, Jiadong; Chen, Linyong

    2016-01-01

    Bioconversion of coal to methane has gained increased attention in recent decades because of its economic and environmental advantages. However, the mechanism of this process is difficult to study in depth, partly because of difficulties associated with the analysis of intermediates generated in coal bioconversion. In this investigation, we report on an effective method to analyze volatile intermediates generated in the bioconversion of coal under strict anaerobic conditions. We conduct in-situ extraction of intermediates using headspace solid-phase micro-extraction followed by detection by gas chromatography-mass spectrometry. Bioconversion simulation equipment was modified and combined with a solid-phase micro-extraction device. In-situ extraction could be achieved by using the combined units, to avoid a breakdown in anaerobic conditions and to maintain the experiment continuity. More than 30 intermediates were identified qualitatively in the conversion process, and the variation in trends of some typical intermediates has been discussed. Volatile organic acids (C2-C7) were chosen for a quantitative study of the intermediates because of their importance during coal bioconversion to methane. Fiber coating, extraction time, and solution acidity were optimized in the solid-phase micro-extraction procedure. The pressure was enhanced during the bioconversion process to investigate the influence of headspace pressure on analyte extraction. The detection limits of the method ranged from 0.0006 to 0.02 mmol/L for the volatile organic acids and the relative standard deviations were between 4.6% and 11.5%. The volatile organic acids (C2-C7) generated in the bioconversion process were 0.01-1.15 mmol/L with a recovery range from 80% to 105%. The developed method is useful for further in-depth research on the bioconversion of coal to methane.

  17. Electronic-nose technology using sputum samples in diagnosis of patients with tuberculosis

    NARCIS (Netherlands)

    Kolk, A.; Hoelscher, M.; Maboko, L.; Jung, J.; Kuijper, S.; Cauchi, M.; Bessant, C.; van Beers, S.; Dutta, R.; Gibson, T.; Reither, K.

    2010-01-01

    We investigated the potential of two different electronic noses (EN; code named "Rob" and "Walter") to differentiate between sputum headspace samples from tuberculosis (TB) patients and non-TB patients. Only samples from Ziehl-Neelsen stain (ZN)- and Mycobacterium tuberculosis culture-positive

  18. Methods for analysis of PAH and BTEX in groundwater from gas stations: a case study in Campo Grande, MS, Brazil

    International Nuclear Information System (INIS)

    Gebara, Samya Soler; Re-Poppi, Nilva; Nascimento, Andre Luiz Carneiro Soares; Raposo Junior, Jorge Luiz

    2013-01-01

    Two methods using headspace solid-phase microextraction and gas chromatography–mass spectrometry were developed for the determination of polycyclic aromatic hydrocarbons (PAH) and BTEX. Best results were obtained using DVB/CAR/PDMS fiber, with 10 min extraction at 25 °C and 0.15 min desorption at 260 °C (BTEX), and PDMS/DVB fiber, with 60 min extraction at 90 °C, 10% NaCl and 5 min desorption at 270 °C (PAH). LOD intervals were 3x10 -2 – 5x10 -2 μg L -1 (BTEX) and 1.6x10 -3 - 1.4 μg L -1 (PAH). The methods were applied to forty-five groundwater samples from monitoring wells of gas stations and only benzene level exceeded the limit established by Brazilian regulations. (author)

  19. 13C analyses on CO2 in air using the multiflow: Application for the monitoring of atmospheric 13CO2 over hydro-electric reservoir in Quebec's Boreal region - Canada

    International Nuclear Information System (INIS)

    Bilodeau, G.; Hillaire-Marcel, C.; Helie, J.-F.; Fourel, F.; Varfalvy, L.

    2002-01-01

    The Multiflow TM preparation system is a headspace sampling device allowing extraction, purification and introduction of a gas sample into a gas-source Isotopic Ratio Mass Spectrometer for isotopic analysis. The original device was designed for 13 C measurements on CO 2 from breath tests. It has been adapted here for 13 CO 2 analysis in atmospheric low pCO 2 -samples

  20. Analysis of Volatile Compounds from Solanumbetaceum Cav. Fruits from Panama by Head-Space Micro Extraction

    Directory of Open Access Journals (Sweden)

    Armando A. Durant

    2013-01-01

    Full Text Available The characterization of the volatile compounds of two varieties of Solanum betaceum Cav. by means of headspace solid-phase microextraction (HS-SPME coupled with gas chromatography-mass spectrometry ( GC-MS i s presented. The HS-SPME method for extraction of the volatiles compounds was optimized by using a 2 3 central composite design. Maximum extraction of volatile compounds was achieved by using a divinylbenzene-carboxen-polydimethylsiloxane (DVB/CAR/PDMS fiber, extraction temperature 76° C, incubation time 44 min, and extraction time of 46 min. The main types of compounds detected in both varieties are terpenoids, followed by aromatics, esters, and aldehydes. Golden-yellow cultivars contained higher levels of esters and terpenes, while the reddish-purple variety contained a significant amount of aromatic compounds. The data structure of the chemical information obtained as well as the relationship between variables was evaluated by means of principal component analysis and cluster analysis.

  1. Vapor space characterization of waste tank 241-C-101: Results from samples collected on 9/1/94

    International Nuclear Information System (INIS)

    Lucke, R.B.; Clauss, T.W.; Ligotke, M.W.

    1995-11-01

    This report describes results of the analyses of tank-headspace samples taken from the Hanford waste Tank 241-C-101 (referred to as Tank C-101) and the ambient air collected - 30 ft upwind near the tank and through the VSS near the tank. Pacific Northwest Laboratory (PNL) contracted with Westinghouse Hanford Company (WHC) to provide sampling devices and to analyze inorganic and organic analytes collected from the tank headspace and ambient air near the tank. The sample job was designated S4056, and samples were collected by WHC on September 1, 1994, using the vapor sampling system (VSS). The samples were inspected upon delivery to the 326/23B laboratory and logged into PNL record book 55408 before implementation of PNL Technical Procedure PNL-TVP-07. Custody of the sorbent traps was transferred to PNL personnel performing the inorganic analysis and stored at refrigerated (≤ 10 degrees C) temperature until the time of analysis. The canisters were stored in the 326/23B laboratory at ambient (25 degrees C) temperature until the time of the analysis. Access to the 326/23B laboratory is limited to PNL personnel working on the waste-tank safety program. Analyses described in this report were performed at PNL in the 300 area of the Hanford Reservation. Analytical methods that were used are described in the text. In summary, sorbent traps for inorganic analyses containing sample materials were either weighed (for water analysis) or desorbed with the appropriate aqueous solutions (for NH 3 , NO 2 , and NO analyses). The aqueous extracts were analyzed either by selective electrode or by ion chromatography (IC). Organic analyses were performed using cryogenic preconcentration followed by gas chromatography/mass spectrometry (GC/MS)

  2. FLAMMABLE GAS DIFFUSION THROUGH SINGLE SHELL TANK (SST) DOMES

    Energy Technology Data Exchange (ETDEWEB)

    MEACHAM, J.E.

    2003-11-10

    This report quantified potential hydrogen diffusion through Hanford Site Single-Shell tank (SST) domes if the SSTs were hypothetically sealed airtight. Results showed that diffusion would keep headspace flammable gas concentrations below the lower flammability limit in the 241-AX and 241-SX SST. The purpose of this document is to quantify the amount of hydrogen that could diffuse through the domes of the SSTs if they were hypothetically sealed airtight. Diffusion is assumed to be the only mechanism available to reduce flammable gas concentrations. The scope of this report is limited to the 149 SSTs.

  3. Analysis of volatiles in silver carp by headspace solid phase micro-extraction coupled with GC-MS

    International Nuclear Information System (INIS)

    Yang Yuping; Xiong Guangquan; Cheng Wei; Liao Tao; Lin Ruotai; Geng Shengrong; Li Xin; Li Xiaoding; Wu Wenjin

    2010-01-01

    In this paper, a method for the determination of volatiles using headspace solid phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS) was presented. The extraction conditions were optimized with reference to these volatiles as hexanal, heptanal, benzaldehyde, 1-Octen-3-ol, octanal, nonanal, decenal, 2,4-heptadienal and 2,4-decadienal. The extraction of fish muscle followed by incubation on a StableFlex divinyl benzene/Carboxen/polydimethylsiloxane (DVB/CAR/PDMS) fiber during 50 in at 60 obtained the most effective extraction of the analytes. The methods by HS-SPME and GC-MS were effective in detecting volatiles in the gills, scales, viscera and fish muscles. The types of volatiles in the gill were more than other organs and the number of odors compounds was 63, and the number of volatiles in scales, viscera and fish muscles was 48, 44 and 42 respectively. (authors)

  4. Vapor space characterization of waste Tank 241-TX-118 (in situ): Results from samples collected on 9/7/94

    International Nuclear Information System (INIS)

    Thomas, B.L.; Clauss, T.W.; Ligotke, M.W.; Pool, K.H.; McVeety, B.D.; Olsen, K.B.; Fruchter, J.S.; Goheen, S.C.

    1995-10-01

    This report describes inorganic and organic analyses results from in situ samples obtained from the headspace of the Hanford waste storage Tank 241-TX-118 (referred to as Tank TX-118). The results described here were obtained to support safety and toxicological evaluations. A summary of the results for inorganic and organic analytes is listed in Table 1. Detailed descriptions of the results appear in the text. Quantitative results were obtained for the inorganic compounds ammonia (NH 3 ), nitrogen dioxide (NO 2 ), nitric oxide (NO), hydrogen cyanide (CHN), and water (H 2 O). Sampling for sulfur oxides (SO x ) was not requested. In addition, quantitative results were obtained for the 39 TO-14 compounds plus an additional 13 analytes. Hexane, normally included in the additional analytes, was removed because a calibration standard was not available during analysis of Tank TX-118 SUMMA trademark canisters. Of these, 12 were observed above the 5-ppbv reporting cutoff. Fourteen tentatively identified compounds (TICs) were observed above the reporting cutoff of (ca.) 10 ppbv and are reported with concentrations that are semiquantitative estimates based on internal-standard response factors. The 10 organic analytes with the highest estimated concentrations are listed in Table 1 and account for approximately 86% of the total organic components in Tank TX-118. Permanent gas analysis was not conducted on the tank-headspace samples. Tank TX-118 is on both the Ferrocyanide and Organic Watch List

  5. Identification of volatiles from pineapple (Ananas comosus L.) pulp by comprehensive two-dimensional gas chromatography and gas chromatography/mass spectrometry.

    Science.gov (United States)

    Pedroso, Marcio P; Ferreira, Ernesto C; Hantao, Leandro W; Bogusz, Stanislau; Augusto, Fabio

    2011-07-01

    Combining qualitative data from the chromatographic structure of 2-D gas chromatography with flame ionization detection (GC×GC-FID) and that from gas chromatography-mass spectrometry (GC/MS) should result in a more accurate assignment of the peak identities than the simple analysis by GC/MS, where coelution of analytes is unavoidable in highly complex samples (rendering spectra unsuitable for qualitative purposes) or for compounds in very low concentrations. Using data from GC×GC-FID combined with GC/MS can reveal coelutions that were not detected by mass spectra deconvolution software. In addition, some compounds can be identified according to the structure of the GC×GC-FID chromatogram. In this article, the volatile fractions of fresh and dehydrated pineapple pulp were evaluated. The extraction of the volatiles was performed by dynamic headspace extraction coupled to solid-phase microextraction (DHS-SPME), a technique appropriate for slurries or solid matrices. Extracted analytes were then analyzed by GC×GC-FID and GC/MS. The results obtained using both techniques were combined to improve compound identifications. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Vented spikes improve delivery from intravenous bags with no air headspace.

    Science.gov (United States)

    Galush, William J; Horst, Travis A

    2015-07-01

    Flexible plastic bags are the container of choice for most intravenous (i.v.) infusions. Under certain circumstances, however, the air-liquid interface present in these i.v. bags can lead to physical instability of protein biopharmaceuticals, resulting in product aggregation. In principle, the air headspace present in the bags can be removed to increase drug stability, but experiments described here show that this can result in incomplete draining of solution from the bag using gravity delivery, or generation of negative pressure in the bag when an infusion pump is used. It is expected that these issues could lead to incomplete delivery of medication to patients or pump-related problems, respectively. However, here it is shown that contrary to the standard pharmacy practice of using nonvented spikes with i.v. bags, the use of vented spikes with i.v. bags that lack air headspace allows complete delivery of the dose solution without impacting the physical stability of a protein-based drug. © 2015 Wiley Periodicals, Inc. and the American Pharmacists Association.

  7. Dried sausages fermented with Staphylococcus xylosus at different temperatures and with different ingredient levels

    DEFF Research Database (Denmark)

    Stahnke, Marie Louise Heller

    1995-01-01

    headspace sampling and quantified and identified by gas chromatography and gas chromatography-mass spectrometry. The effects of temperature and different ingredients on the levels of individual volatiles were tested using multiple linear regression and analysis of variance. The study showed that sausages...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-08-15

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

  9. 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

  10. Comparative Analyses of the Volatile Components of Citrus Aurantium L. Flowers Using Ultrasonic-Assisted Headspace SPME and Hydrodistillation Combined with GC-MS and Evaluation of their Antimicrobial Activities

    Directory of Open Access Journals (Sweden)

    Akram Rahimi

    2014-12-01

    Full Text Available The volatile components of Citrus aurantium L. flowers were characterized by GC-MS with two different extraction techniques, hydrodistillation (HD and ultrasonic-assisted headspace solid phase microextraction (UA-HS-SPME. In the SPME method, the volatile components of the samples, irradiated by ultrasonic radiation, were collected on a polydimethyl siloxane (PDMS commercial fiber as well as some manually prepared nanoporous fibers from the samples headspace. To reach the better results, the extraction conditions were carefully optimized for the PDMS fiber. Under the optimized conditions (i.e. sonication time 15 min, extraction time 30 min and extraction temperature 55 ºC, 54 compounds were identified by the UA-HS-SPME-GC/MS method. The essential oil components of Citrus aurantium L. flower samples from two different regions of Iran and new and old samples from the same region were compared to one another. The major components identified for the samples with both the SPME and HD methods were linalool, linalyl acetate, limonene, β-myrcene, geranyl acetate, and neryl acetate, respectively. However, a substantial variation in the percentages of the components was identified for different samples and different extraction methods. The antimicrobial activities of the oil were also examined against six standard bacteria. There was some activity against Enterococcus fecalis, Escherichia coli, and Bacillus cereus, indicating important biological activities of the oil.

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

    International Nuclear Information System (INIS)

    Pitkoff, C.C.

    1995-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-05-01

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

  13. Simulations of the Viking Gas Exchange Experiment using palagonite and Fe-rich montmorillonite as terrestrial analogs: implications for the surface composition of Mars.

    Science.gov (United States)

    Quinn, R; Orenberg, J

    1993-10-01

    Simulations of the Gas Exchange Experiment (GEX), one of the Viking Lander Biology Experiments, were run using palagonite and Fe-rich montmorillonite as terrestrial analogs of the Martian soil. These terrestrial analogs were exposed to a nutrient solution of the same composition as that of the Viking Landers under humid (no contact with nutrient) and wet (intimate contact) conditions. The headspace gases in the GEX sample cell were sampled and then analyzed by gas chromatography under both humid and wet conditions. Five gases were monitored: CO2, N2, O2, Ar, and Kr. It was determined that in order to simulate the CO2 gas changes of the Viking GEX experiment, the mixture of soil analog mineral plus nutrient medium must be slightly (pH = 7.4) to moderately basic (pH = 8.7). This conclusion suggests constraints upon the composition of terrestrial analogs to the Mars soil; acidic components may be present, but the overall mixture must be basic in order to simulate the Viking GEX results.

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

    African Journals Online (AJOL)

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

  15. Doping of three-dimensional porous carbon nanotube-graphene-ionic liquid composite into polyaniline for the headspace solid-phase microextraction and gas chromatography determination of alcohols

    Energy Technology Data Exchange (ETDEWEB)

    Li, Lulu; Wu, Mian; Feng, Yingying; Zhao, Faqiong; Zeng, Baizhao, E-mail: bzzeng@whu.edu.cn

    2016-12-15

    In this work, ionic liquid (IL, i.e. 1-hydroxyethyl-3-methylimidazolium tetrafluoroborate), carboxyl multiwall carbon nanotubes (MWCNTs) and reduced graphene oxide (rGO) were used to prepare three-dimensional porous material (MWCNTs-rGO-IL) by one-step self-assembly, then it was co-electrodeposited with polyaniline (PANI) on stainless steel wires by cyclic voltammetry. The resulting coating (PANI-MWCNTs-rGO-IL) was characterized by using FT-IR and scanning electron microscopy etc, and it showed porous structure and had high thermal stability. Furthermore, it was found to be very suitable for the headspace solid-phase microextraction of alcohols (i.e. octanol, nonanol, geraniol, decanol, undecanol and dodecanol). By coupling with gas chromatography, wide linear ranges and low limits of detection (i.e. 2.2–28.3 ng L{sup −1}) were obtained for the alcohols. The coating also presented good repeatability and reproducibility; the relative standard deviations for intra-fiber and fiber-to-fiber were less than 5.6% (n = 5) and 7.0% (n = 5) respectively. In addition, the proposed method was successfully applied to the determination of alcohols in tea drinks, and the recoveries for standards added were 85.6–114%. - Highlights: • A three-dimensional porous material (MWCNTs-rGO-IL) was synthesized by self-assembly. • A new PANI-MWCNTs-rGO-IL composite coating was prepared by electrochemical method. • It presented high thermal stability and extraction selectivity for alcohols.

  16. Doping of three-dimensional porous carbon nanotube-graphene-ionic liquid composite into polyaniline for the headspace solid-phase microextraction and gas chromatography determination of alcohols

    International Nuclear Information System (INIS)

    Li, Lulu; Wu, Mian; Feng, Yingying; Zhao, Faqiong; Zeng, Baizhao

    2016-01-01

    In this work, ionic liquid (IL, i.e. 1-hydroxyethyl-3-methylimidazolium tetrafluoroborate), carboxyl multiwall carbon nanotubes (MWCNTs) and reduced graphene oxide (rGO) were used to prepare three-dimensional porous material (MWCNTs-rGO-IL) by one-step self-assembly, then it was co-electrodeposited with polyaniline (PANI) on stainless steel wires by cyclic voltammetry. The resulting coating (PANI-MWCNTs-rGO-IL) was characterized by using FT-IR and scanning electron microscopy etc, and it showed porous structure and had high thermal stability. Furthermore, it was found to be very suitable for the headspace solid-phase microextraction of alcohols (i.e. octanol, nonanol, geraniol, decanol, undecanol and dodecanol). By coupling with gas chromatography, wide linear ranges and low limits of detection (i.e. 2.2–28.3 ng L"−"1) were obtained for the alcohols. The coating also presented good repeatability and reproducibility; the relative standard deviations for intra-fiber and fiber-to-fiber were less than 5.6% (n = 5) and 7.0% (n = 5) respectively. In addition, the proposed method was successfully applied to the determination of alcohols in tea drinks, and the recoveries for standards added were 85.6–114%. - Highlights: • A three-dimensional porous material (MWCNTs-rGO-IL) was synthesized by self-assembly. • A new PANI-MWCNTs-rGO-IL composite coating was prepared by electrochemical method. • It presented high thermal stability and extraction selectivity for alcohols.

  17. Comparison of vapor sampling system (VSS) and in situ vapor sampling (ISVS) methods on Tanks C-107, BY-108, and S-102

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Edwards, J.A.; Evans, J.C.

    1996-05-01

    The objective of this report is to evaluate the equivalency of two methods used to sample nonradioactive gases and vapors in the Hanford Site high-level waste tank headspaces. In addition to the comparison of the two sampling methods, the effects of an in-line fine particle filter on sampling results are also examined to determine whether results are adversely affected by its presence. This report discusses data from a January 1996 sampling

  18. A selective and sensitive optical sensor for dissolved ammonia detection via agglomeration of fluorescent Ag nanoclusters and temperature gradient headspace single drop microextraction.

    Science.gov (United States)

    Dong, Jiang Xue; Gao, Zhong Feng; Zhang, Ying; Li, Bang Lin; Li, Nian Bing; Luo, Hong Qun

    2017-05-15

    In this paper, a simple sensor platform is presented for highly selective and sensitive detection of dissolved ammonia in aqueous solutions without pretreatment based on temperature gradient headspace single drop microextraction (HS-SDME) technique, and fluorescence and UV-vis spectrophotometry are utilized with the Ag nanoclusters (Ag NCs) functioned by citrate and glutathione as the probe. The sensing mechanism is based on the volatility of ammonia gas and the active response of Ag NCs to pH change caused by the introduction of ammonia. High pH can make the Ag NCs agglomerate and lead to the obvious decrease of fluorescence intensity and absorbance of Ag NCs solution. Moreover, the presented method exhibits a remarkably high selectivity toward dissolved ammonia over most of inorganic ions and amino acid, and shows a good linear range of 10-350μM (0.14-4.9mgNL -1 ) with a low detection limit of 336nM (4.70μgNL -1 ) at a signal-to-noise ratio of 3. In addition, the practical applications of the sensor have been successfully demonstrated by detecting dissolved ammonia in real samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  19. Improved enrichment culture technique for methane-oxidizing bacteria from marine ecosystems: the effect of adhesion material and gas composition.

    Science.gov (United States)

    Vekeman, Bram; Dumolin, Charles; De Vos, Paul; Heylen, Kim

    2017-02-01

    Cultivation of microbial representatives of specific functional guilds from environmental samples depends largely on the suitability of the applied growth conditions. Especially the cultivation of marine methanotrophs has received little attention, resulting in only a limited number of ex situ cultures available. In this study we investigated the effect of adhesion material and headspace composition on the methane oxidation activity in methanotrophic enrichments obtained from marine sediment. Addition of sterilized natural sediment or alternatively the addition of acid-washed silicon dioxide significantly increased methane oxidation. This positive effect was attributed to bacterial adhesion on the particles via extracellular compounds, with a minimum amount of particles required for effect. As a result, the particles were immobilized, thus creating a stratified environment in which a limited diffusive gas gradients could build up and various microniches were formed. Such diffusive gas gradient might necessitate high headspace concentrations of CH 4 and CO 2 for sufficient concentrations to reach the methane-oxidizing bacteria in the enrichment culture technique. Therefore, high concentrations of methane and carbon dioxide, in addition to the addition of adhesion material, were tested and indeed further stimulated methane oxidation. Use of adhesion material in combination with high concentrations of methane and carbon dioxide might thus facilitate the cultivation and subsequent enrichment of environmentally important members of this functional guild. The exact mechanism of the observed positive effects on methane oxidation and the differential effect on methanotrophic diversity still needs to be explored.

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

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

    Science.gov (United States)

    Carrigan, Charles R.; Tanaka, Junichi

    2010-05-01

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

  2. Characterization of the major odor-active compounds in Thai durian ( Durio zibethinus L. 'Monthong') by aroma extract dilution analysis and headspace gas chromatography-olfactometry.

    Science.gov (United States)

    Li, Jia-Xiao; Schieberle, Peter; Steinhaus, Martin

    2012-11-14

    An aroma extract dilution analysis applied on the volatile fraction isolated from Thai durian by solvent extraction and solvent-assisted flavor evaporation resulted in 44 odor-active compounds in the flavor dilution (FD) factor range of 1-16384, 41 of which could be identified and 24 that had not been reported in durian before. High FD factors were found for ethyl (2S)-2-methylbutanoate (fruity; FD 16384), ethyl cinnamate (honey; FD 4096), and 1-(ethylsulfanyl)ethanethiol (roasted onion; FD 1024), followed by 1-(ethyldisulfanyl)-1-(ethylsulfanyl)ethane (sulfury, onion), 2(5)-ethyl-4-hydroxy-5(2)-methylfuran-3(2H)-one (caramel), 3-hydroxy-4,5-dimethylfuran-2(5H)-one (soup seasoning), ethyl 2-methylpropanoate (fruity), ethyl butanoate (fruity), 3-methylbut-2-ene-1-thiol (skunky), ethane-1,1-dithiol (sulfury, durian), 1-(methylsulfanyl)ethanethiol (roasted onion), 1-(ethylsulfanyl)propane-1-thiol (roasted onion), and 4-hydroxy-2,5-dimethylfuran-3(2H)-one (caramel). Among the highly volatile compounds screened by static headspace gas chromatography-olfactometry, hydrogen sulfide (rotten egg), acetaldehyde (fresh, fruity), methanethiol (rotten, cabbage), ethanethiol (rotten, onion), and propane-1-thiol (rotten, durian) were found as additional potent odor-active compounds. Fourteen of the 41 characterized durian odorants showed an alkane-1,1-dithiol, 1-(alkylsulfanyl)alkane-1-thiol, or 1,1-bis(alkylsulfanyl)alkane structure derived from acetaldehyde, propanal, hydrogen sulfide, and alkane-1-thiols. Among these, 1-(propylsulfanyl)ethanethiol, 1-{[1-(methylsulfanyl)ethyl]sulfanyl}ethanethiol, and 1-{[1-(ethylsulfanyl)ethyl]sulfanyl}ethanethiol were reported for the first time in a natural product.

  3. Measurement of residual solvents in a drug substance by a purge-and-trap method.

    Science.gov (United States)

    Lakatos, Miklós

    2008-08-05

    The purge-and-trap (P&T) gas extraction method combined with gas chromatography was studied for its suitability for quantitative residual solvents determination in a water-soluble active pharmaceutical ingredient (API). Some analytical method performance characteristics were investigated, namely, the repeatability, the accuracy and the detection limit of determination. The results show that the P&T technique is--as expected--more sensitive than the static headspace, thus it can be used for the determination of residual solvents pertaining to the ICH Class 1 group. It was found that it could be an alternative sample preparation method besides the static headspace (HS) method.

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

    Science.gov (United States)

    Winters, W.J.

    1999-01-01

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

  5. High efficient ethanol and VFAs production from gas fermentation: effect of acetate, gas and inoculum microbial composition

    DEFF Research Database (Denmark)

    El-Gammal, Maie; Abou-Shanab, Reda; Angelidaki, Irini

    2017-01-01

    In bioindustry, syngas fermentation is a promising technology for biofuel production without the use of plant biomass as sugar-based feedstock. The aim of this study was to identify optimal conditions for high efficient ethanol and volatile fatty acids (VFA) production from synthetic gas fermenta......In bioindustry, syngas fermentation is a promising technology for biofuel production without the use of plant biomass as sugar-based feedstock. The aim of this study was to identify optimal conditions for high efficient ethanol and volatile fatty acids (VFA) production from synthetic gas...... fatty acids and ethanol was achieved by the pure culture (Clostridium ragsdalei). Depending on the headspace gas composition, VFA concentrations were up to 300% higher after fermentation with Clostridium ragsdalei compared to fermentation with mixed culture. The preferred gas composition with respect...... to highest VFA concentration was pure CO (100%) regardless of microbial composition of the inoculum and media composition. The addition of acetate had a negative impact on the VFA formation which was depending on the initial gas composition in head space....

  6. Metabolomics strategy for the mapping of volatile exometabolome from Saccharomyces spp. widely used in the food industry based on comprehensive two-dimensional gas chromatography.

    Science.gov (United States)

    Martins, Cátia; Brandão, Tiago; Almeida, Adelaide; Rocha, Sílvia M

    2017-05-01

    Saccharomyces spp. are widely used in the food and beverages industries. Their cellular excreted metabolites are important for general quality of products and can contribute to product differentiation. This exploratory study presents a metabolomics strategy for the comprehensive mapping of cellular metabolites of two yeast species, Saccharomyces cerevisiae and S. pastorianus (both collected in an industrial context) through a multidimensional chromatography platform. Solid-phase microextraction was used as a sample preparation method. The yeast viability, a specific technological quality parameter, was also assessed. This untargeted analysis allowed the putative identification of 525 analytes, distributed over 14 chemical families, the origin of which may be explained through the pathways network associated with yeasts metabolism. The expression of the different metabolic pathways was similar for both species, event that seems to be yeast genus dependent. Nevertheless, these species showed different growth rates, which led to statistically different metabolites content. This was the first in-depth approach that characterizes the headspace content of S. cerevisiae and S. pastorianus species cultures. The combination of a sample preparation method capable of providing released volatile metabolites directly from yeast culture headspace with comprehensive two-dimensional gas chromatography was successful in uncovering a specific metabolomic pattern for each species. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Tequila authenticity assessment by headspace SPME-HRGC-IRMS analysis of 13C/12C and 18O/16O ratios of ethanol.

    Science.gov (United States)

    Aguilar-Cisneros, Blanca O; López, Mercedes G; Richling, Elke; Heckel, Frank; Schreier, Peter

    2002-12-18

    By use of headspace SPME sampling and a PLOT column, on-line capillary gas chromatography-isotope ratio mass spectrometry was employed in the combustion (C) and the pyrolysis (P) modes (HRGC-C/P-IRMS) to determine the delta(13)C(VPDB) and delta(18)O(VSMOW) values of ethanol in authentic (n = 14) and commercial tequila samples (n = 15) as well as a number of other spirits (n = 23). Whereas with delta(13)C(VPDB) values ranging from -12.1 to -13.2 per thousand and from -12.5 to -14.8 per thousand similar variations were found for 100% agave and mixed tequilas, respectively, the delta(18)O(VSMOW) data differed slightly within these categories: ranges from +22.1 to +22.8 per thousand and +20.8 to +21.7 per thousand were determined for both the authentic 100% agave and mixed products, respectively. The data recorded for commercial tequilas were less homogeneous; delta(13)C(VPDB) data from -10.6 to -13.9 per thousand and delta(18)O(VSMOW) values from +15.5 to +22.7 per thousand were determined in tequilas of both categories. Owing to overlapping data, attempts to differentiate between white, rested, and aged tequilas within each of the two categories failed. In addition, discrimination of tequila samples from other spirits by means of delta(13)C(VPDB) and delta(18)O(VSMOW) data of ethanol was restricted to the products originating from C(3) as well as C(4)/CAM raw materials.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-03-26

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

  9. Microbial gas generation under expected Waste Isolation Pilot Plant repository conditions

    International Nuclear Information System (INIS)

    Francis, A.J.; Gillow, J.B.; Giles, M.R.

    1997-03-01

    Gas generation from the microbial degradation of the organic constituents of transuranic waste under conditions expected at the Waste Isolation Pilot Plant (WIPP) repository was investigated at Brookhaven National Laboratory. The biodegradation of mixed cellulosics (various types of paper) and electron-beam irradiated plastic and rubber materials (polyethylene, polyvinylchloride, neoprene, hypalon, and leaded hypalon) was examined. The rate of gas production from cellulose biodegradation in inundated samples incubated for 1,228 days at 30 C was biphasic, with an initial rapid rate up to approximately 600 days incubation, followed by a slower rate. The rate of total gas production in anaerobic samples containing mixed inoculum was as follows: 0.002 mL/g cellulose/day without nutrients; 0.004 mL/g cellulose/day with nutrients; and 0.01 mL/g cellulose/day in the presence of excess nitrate. Carbon dioxide production proceeded at a rate of 0.009 micromol/g cellulose/day in anaerobic samples without nutrients, 0.05 micromol/g cellulose/day in the presence of nutrients, and 0.2 micromol/g cellulose/day with excess nitrate. Adding nutrients and excess nitrate stimulated denitrification, as evidenced by the accumulation of N 2 O in the headspace (200 micromol/g cellulose). The addition of the potential backfill bentonite increased the rate of CO 2 production to 0.3 micromol/g cellulose/day in anaerobic samples with excess nitrate. Analysis of the solution showed that lactic, acetic, propionic, butyric, and valeric acids were produced due to cellulose degradation. Samples incubated under anaerobic humid conditions for 415 days produced CO 2 at a rate of 0.2 micromol/g cellulose/day in the absence of nutrients, and 1 micromol/g cellulose/day in the presence of bentonite and nutrients. There was no evidence of biodegradation of electron-beam irradiated plastic and rubber

  10. Neuro-genetic multioptimization of the determination of polychlorinated biphenyl congeners in human milk by headspace solid phase microextraction coupled to gas chromatography with electron capture detection

    International Nuclear Information System (INIS)

    Hoffmann Kowalski, Claudia; Silva, Gilmare Antonia da; Poppi, Ronei Jesus; Teixeira Godoy, Helena; Augusto, Fabio

    2007-01-01

    Polychlorinated biphenyls (PCB) can eventually contaminate breast milk, which is a serious issue to the newborn due to their high vulnerability. Solid phase microextraction (SPME) can be a very convenient technique for their isolation and pre-concentration prior chromatographic analysis. Here, a simultaneous multioptimization strategy based on a neuro-genetic approach was applied to a headspace SPME method for determination of 12 PCB in human milk. Gas chromatography with electron capture detection (ECD) was adopted for the separation and detection of the analytes. Experiments according to a Doehlert design were carried out with varied extraction time and temperature, media ionic strength and concentration of the methanol (co-solvent). To find the best model that simultaneously correlate all PCB peak areas and SPME extraction conditions, a multivariate calibration method based on a Bayesian Neural Network (BNN) was applied. The net output from the neural network was used as input in a genetic algorithm (GA) optimization operation (neuro-genetic approach). The GA pointed out that the best values of the overall SPME operational conditions were the saturation of the media with NaCl, extraction temperature of 95 deg. C, extraction time of 60 min and addition of 5% (v/v) methanol to the media. These optimized parameters resulted in the decrease of the detection limits and increase on the sensitivity for all tested analytes, showing that the use of neuro-genetic approach can be a promising way for optimization of SPME methods

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

    Science.gov (United States)

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

    2008-10-31

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

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

    NARCIS (Netherlands)

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

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

  13. Authentication of pineapple (Ananas comosus [L.] Merr.) fruit maturity stages by quantitative analysis of γ- and δ-lactones using headspace solid-phase microextraction and chirospecific gas chromatography-selected ion monitoring mass spectrometry (HS-SPME-GC-SIM-MS).

    Science.gov (United States)

    Steingass, Christof B; Langen, Johannes; Carle, Reinhold; Schmarr, Hans-Georg

    2015-02-01

    Headspace solid phase microextraction and chirospecific gas chromatography-mass spectrometry in selected ion monitoring mode (HS-SPME-GC-SIM-MS) allowed quantitative determination of δ-lactones (δ-C8, δ-C10) and γ-lactones (γ-C6, γ-C8, γ-C10). A stable isotope dilution assay (SIDA) with d7-γ-decalactone as internal standard was used for quantitative analysis of pineapple lactones that was performed at three progressing post-harvest stages of fully ripe air-freighted and green-ripe sea-freighted fruits, covering the relevant shelf-life of the fruits. Fresh pineapples harvested at full maturity were characterised by γ-C6 of high enantiomeric purity remaining stable during the whole post-harvest period. In contrast, the enantiomeric purity of γ-C6 significantly decreased during post-harvest storage of sea-freighted pineapples. The biogenetical background and the potential of chirospecific analysis of lactones for authentication and quality evaluation of fresh pineapple fruits are discussed. Copyright © 2014 Elsevier Ltd. All rights reserved.

  14. A screening method for polycyclic aromatic hydrocarbons determination in water by headspace SPME with GC-FID

    Energy Technology Data Exchange (ETDEWEB)

    Zuazagoitia, D.; Millan, E.; Garcia, R. [Univ. of Pais Vasco, Donostia-San Sebastian (Spain). Dept. of Applied Chemistry

    2007-11-15

    A simple method for determination of polycyclic aromatic hydrocarbons (PAHs) in water using headspace solid-phase microextraction (HS-SPME) with gas chromatography-flame ionisation detector (GC-FID) was developed. In order to obtain the convenient experimental conditions for HS-SPME extraction an experimental design with two steps was accomplished. A 2{sup 6-2} fractional factorial design and central composite design (CCD) considering three significant factors were used. Naphthalene, anthracene and fluoranthene were chosen as representatives of two, three and four aromatic rings, and the global response of three PAHs was used for the results, evaluation. The chosen extraction conditions were: 85 {mu}m polyacrylate fibre; 50 C temperature; 60 min time; 20 mL-dissolution volume (in 40 mL glass vial); without salt addition; and 2 min desorption time. The procedure was extended to other seven PAHs (acenaphthylene, acenaphthene, fluorene, phenanthrene, pyrene, chrysene and benzo(a)anthracene) and the analytical characteristics were checked. The limit of detection (LOD) was from 0.08 (anthracene) to 0.20 {mu}g L{sup -1} (naphthalene). The precision expressed as relative standard deviation (RSD in %) using 50 {mu}g L{sup -1} of each analyte ranged from 6.8 to 17 %. The method was applied to the analysis of the surface waters and leaching waters of contaminated soils from Gipuzkoa (North Spain). The PAHs were not detected in surface water samples. Most of the PAHs were found in the leachates from contaminated soils showing a maximum global value of 75.5 {mu}g L{sup -1}. (orig.)

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

    Science.gov (United States)

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

    2013-10-01

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

  16. Application of headspace and direct immersion solid-phase microextraction in the analysis of organothiophosphates related to the Chemical Weapons Convention from water and complex matrices.

    Science.gov (United States)

    Althoff, Marc André; Bertsch, Andreas; Metzulat, Manfred; Klapötke, Thomas M; Karaghiosoff, Konstantin L

    2017-11-01

    The successful application of headspace (HS) and direct immersion (DI) solid phase microextraction (SPME) for the unambiguous identification and characterization of a series of toxic thiophosphate esters, such as Amiton (I), from aqueous phases and complex matrices (e.g. grass and foliage) has been demonstrated. A Thermo Scientific gas chromatograph (GC) - tandem mass spectrometer (MS/MS) system with a TriPlus RSH® autosampler and a SPME tool was used to investigate the effect of different parameters that influence the extraction efficiency: e.g. pH of the sample matrix and extraction temperature. The developed methods were employed for the detection of several Amiton derivatives (Schedule II of the CWC) that are structurally closely related to each other; some of which are new and have not been reported in literature previously. In addition, a novel DI SPME method from complex matrices for the analysis of organophosphates related to the CWC was developed. The studies clearly show that DI SPME for complex matrices is superior to HS extraction and can potentially be applied to other related compounds controlled under the CWC. Copyright © 2017. Published by Elsevier B.V.

  17. Coupling laser desorption with gas chromatography and ion mobility spectrometry for improved olive oil characterisation.

    Science.gov (United States)

    Liedtke, Sascha; Seifert, Luzia; Ahlmann, Norman; Hariharan, Chandrasekhara; Franzke, Joachim; Vautz, Wolfgang

    2018-07-30

    The investigation of volatile compounds in the headspace of liquid samples can often be used for detailed and non-destructive characterisation of the sample. This has great potential for process control or the characterisation of food samples, such as olive oil. We investigated, for the first time, the plume of substances released from olive oil droplets by laser desorption in a feasibility study and applied ion mobility spectrometry coupled to rapid GC pre-separation to enhance selectivity. Our investigation demonstrated that significantly more substances can be detected and quantified via laser desorption than in the usual headspace, enabling a rapid (5-10 min), sensitive (low ng/g range) and comprehensive analysis of the sample, with the potential for quality control and fraud identification. Therefore, laser desorption provides a useful sampling tool for characterising liquids in many applications, requiring only a few µL of sample. Copyright © 2018 Elsevier Ltd. All rights reserved.

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

    International Nuclear Information System (INIS)

    Goles, R.W.

    1996-03-01

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

  19. Overview of Hanford Site High-Level Waste Tank Gas and Vapor Dynamics

    Energy Technology Data Exchange (ETDEWEB)

    Huckaby, James L.; Mahoney, Lenna A.; Droppo, James G.; Meacham, Joseph E.

    2004-08-31

    Hanford Site processes associated with the chemical separation of plutonium from uranium and other fission products produced a variety of volatile, semivolatile, and nonvolatile organic and inorganic waste chemicals that were sent to high-level waste tanks. These chemicals have undergone and continue to undergo radiolytic and thermal reactions in the tanks to produce a wide variety of degradation reaction products. The origins of the organic wastes, the chemical reactions they undergo, and their reaction products have recently been examined by Stock (2004). Stock gives particular attention to explaining the presence of various types of volatile and semivolatile organic species identified in headspace air samples. This report complements the Stock report by examining the storage of volatile and semivolatile species in the waste, their transport through any overburden of waste to the tank headspaces, the physical phenomena affecting their concentrations in the headspaces, and their eventual release into the atmosphere above the tanks.

  20. Volatile Hydrocarbon Analysis in Blood by Headspace Solid-Phase Microextraction: The Interpretation of VHC Patterns in Fire-Related Incidents.

    Science.gov (United States)

    Waters, Brian; Hara, Kenji; Ikematsu, Natsuki; Takayama, Mio; Kashiwagi, Masayuki; Matsusue, Aya; Kubo, Shin-Ichi

    2017-05-01

    A headspace solid-phase microextraction (HS-SPME) technique was used to quantitate the concentration of volatile hydrocarbons from the blood of cadavers by cryogenic gas chromatography-mass spectroscopy. A total of 24 compounds including aromatic and aliphatic volatile hydrocarbons were analyzed by this method. The analytes in the headspace of 0.1 g of blood mixed with 1.0 mL of distilled water plus 1 µL of an internal standard solution were adsorbed onto a 100-µm polydimethylsiloxane fiber at 0°C for 15 min, and measured using a GC-MS full scan method. The limit of quantitation for the analytes ranged from 6.8 to 10 ng per 1 g of blood. This method was applied to actual autopsy cases to quantitate the level of volatile hydrocarbons (VHCs) in the blood of cadavers who died in fire-related incidents. The patterns of the VHCs revealed the presence or absence of accelerants. Petroleum-based fuels such as gasoline and kerosene were differentiated. The detection of C8-C13 aliphatic hydrocarbons indicated the presence of kerosene; the detection of C3 alkylbenzenes in the absence of C8-C13 aliphatic hydrocarbons was indicative of gasoline; and elevated levels of styrene or benzene in the absence of C3/C4 alkylbenzenes and aliphatic hydrocarbons indicated a normal construction fire. This sensitive HS-SPME method could help aid the investigation of fire-related deaths by providing a simple pattern to use for the interpretation of VHCs in human blood. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  1. Headspace sorptive solid phase microextraction (HS-SPME) combined with a spectrophotometry system: A simple glass devise for extraction and simultaneous determination of cyanide and thiocyanate in environmental and biological samples.

    Science.gov (United States)

    Al-Saidi, H M; Al-Harbi, Sami A; Aljuhani, E H; El-Shahawi, M S

    2016-10-01

    A simple, low cost and efficient headspace sorptive solid phase microextraction (HS-SPME) method for determination of cyanide has been developed. The system comprises of a glass tube with two valves and a moveable glass slide fixed at its centre. It includes an acceptor phase polyurethane foam treated mercury (II) dithizonate [Hg(HDz)2-PUF] complex fixed inside by a septum cap in a cylindrical configuration (5.0cm length and 1.0cm diameter). The extraction is based upon the contact of the acceptor phase to the headspace and subsequently measuring the absorbance of the recovered mercury (II) dithizonate from PUFs sorbent. Unlike other HSSE, extraction and back - extractions was carried out in a closed system, thereby improving the analytical performance by preventing the analyte loss. Under the optimized conditions, a linear calibration plot in the range of 1.0-50.0µmolL(-1) was achieved with limits of detection (LOD) and quantification (LOQ) of 0.34, 1.2µmolL(-1) CN(-), respectively. Simultaneous analysis of cyanide and thiocyanate in saliva was also performed with satisfactory recoveries. Copyright © 2016. Published by Elsevier B.V.

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

    Science.gov (United States)

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

    2018-05-01

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

  3. Source identification of underground fuel spills by solid-phase microextraction/high-resolution gas chromatography/genetic algorithms.

    Science.gov (United States)

    Lavine, B K; Ritter, J; Moores, A J; Wilson, M; Faruque, A; Mayfield, H T

    2000-01-15

    Solid-phase microextraction (SPME), capillary column gas chromatography, and pattern recognition methods were used to develop a potential method for typing jet fuels so a spill sample in the environment can be traced to its source. The test data consisted of gas chromatograms from 180 neat jet fuel samples representing common aviation turbine fuels found in the United States (JP-4, Jet-A, JP-7, JPTS, JP-5, JP-8). SPME sampling of the fuel's headspace afforded well-resolved reproducible profiles, which were standardized using special peak-matching software. The peak-matching procedure yielded 84 standardized retention time windows, though not all peaks were present in all gas chromatograms. A genetic algorithm (GA) was employed to identify features (in the standardized chromatograms of the neat jet fuels) suitable for pattern recognition analysis. The GA selected peaks, whose two largest principal components showed clustering of the chromatograms on the basis of fuel type. The principal component analysis routine in the fitness function of the GA acted as an information filter, significantly reducing the size of the search space, since it restricted the search to feature subsets whose variance is primarily about differences between the various fuel types in the training set. In addition, the GA focused on those classes and/or samples that were difficult to classify as it trained using a form of boosting. Samples that consistently classify correctly were not as heavily weighted as samples that were difficult to classify. Over time, the GA learned its optimal parameters in a manner similar to a perceptron. The pattern recognition GA integrated aspects of strong and weak learning to yield a "smart" one-pass procedure for feature selection.

  4. J

    African Journals Online (AJOL)

    1987-03-13

    Mar 13, 1987 ... Institute for Chromatography, University of Pretoria, Pretoria, ... dynamic solvent effect sampling, capillary gas-liquid chroma- ... of volatiles from 10 ml of headspace above the anal gland secretion of a male lctonyx striatus.

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

    International Nuclear Information System (INIS)

    Trimble, D.J.

    1995-01-01

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

  6. Possibilities for decreasing detection limits of analytical methods for determination of transformation products of unsymmetrical dimethylhydrazine in environmental samples

    Directory of Open Access Journals (Sweden)

    Bulat Kenessov

    2015-12-01

    Full Text Available Most rockets of middle and heavy class launched from Kazakhstan, Russia, China and other countries still use highly toxic unsymmetrical dimethylhydrazine (UDMH as a liquid propellant. Study of migration, distribution and accumulation of UDMH transformation products in environment and human health impact assessment of space rocket activity are currently complicated due to the absence of analytical methods allowing detection of trace concentrations of these compounds in analyzed samples. This paper reviews methods and approaches, which can be applied for development of such methods. Detection limits at a part-per-trillion (ppt level may be achieved using most selective and sensitive methods based on gas or liquid chromatography in combination of tandem or high-resolution mass spectrometry. In addition, 1000-fold concentration of samples or integrated sample preparation methods, e.g., dynamic headspace extraction, are required. Special attention during development and application of such methods must be paid to purity of laboratory air, reagents, glassware and analytical instruments.

  7. Principle and Performance of Gas Self-inducing Reactors and Applications to Biotechnology.

    Science.gov (United States)

    Ye, Qin; Li, Zhimin; Wu, Hui

    2016-01-01

    Gas-liquid contacting is an important unit operation in chemical and biochemical processes, but the gas utilization efficiency is low in conventional gas-liquid contactors especially for sparingly soluble gases. The gas self-inducing impeller is able to recycle gas in the headspace of a reactor to the liquid without utilization of additional equipment such as a gas compressor, and thus, the gas utilization efficiency is significantly enhanced. Gas induction is caused by the low pressure or deep vortex at a sufficiently high impeller speed, and the speed at which gas induction starts is termed the critical speed. The critical impeller speed, gas-induction flow rate, power consumption, and gas-liquid mass transfer are determined by the impeller design and operation conditions. When the reactor is operated in a dead-end mode, all the introduced gas can be completely used, and this feature is especially favorable to flammable and/or toxic gases. In this article, the principles, designs, characteristics of self-inducing reactors, and applications to biotechnology are described.

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

    Science.gov (United States)

    Yokochi, Reika

    2016-09-01

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

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

    Directory of Open Access Journals (Sweden)

    Jiang-Feng Liu

    2017-01-01

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

  10. Headspace-Sampling Paper-Based Analytical Device for Colorimetric/Surface-Enhanced Raman Scattering Dual Sensing of Sulfur Dioxide in Wine.

    Science.gov (United States)

    Li, Dan; Duan, Huazhen; Ma, Yadan; Deng, Wei

    2018-05-01

    This study demonstrates a novel strategy for colorimetric/surface-enhanced Raman scattering (SERS) dual-mode sensing of sulfur dioxide (SO 2 ) by coupling headspace sampling (HS) with paper-based analytical device (PAD). The smart and multifunctional PAD is fabricated with a vacuum filtration method in which 4-mercaptopyridine (Mpy)-modified gold nanorods (GNRs)-reduced graphene oxide (rGO) hybrids (rGO/MPy-GNRs), anhydrous methanol, and starch-iodine complex are immobilized into cellulose-based filter papers. The resultant PAD exhibits a deep-blue color with a strong absorption peak at 600 nm due to the formation of an intermolecular charge-transfer complex between starch and iodine. However, the addition of SO 2 induces the Karl Fischer reaction, resulting in the decrease of color and increase of SERS signals. Therefore, the PAD can be used not only as a naked-eye indicator of SO 2 changed from blue to colorless but also as a highly sensitive SERS substrates because of the SO 2 -triggered conversion of Mpy to pyridine methyl sulfate on the GNRs. A distinguishable change in the color was observed at a SO 2 concentration of 5 μM by the naked eye, and a detection limit as low as 1.45 μM was obtained by virtue of UV-vis spectroscopy. The PAD-based SERS method is effective over a wide range of concentrations (1 μM to 2000 μM) for SO 2 , and the detection limit for SO 2 is found to be 1 μM. The HS-PAD based colorimetric/SERS method is applied for the determination of SO 2 in wine, and the detection results match well with those obtained from the traditional Monier-Williams method. This study not only offers a new method for on-site monitoring of SO 2 but also provides a new strategy for designing of paper-based sensing platform for a wide range of field-test applications.

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

    International Nuclear Information System (INIS)

    Alwardt, L.D.

    1995-01-01

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

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

    Directory of Open Access Journals (Sweden)

    J. Daryatmo

    2015-04-01

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

  13. Determination of tetrachloroethylene and other volatile halogenated organic compounds in oil wastes by headspace SPME GC-MS

    Energy Technology Data Exchange (ETDEWEB)

    Fabbri, D.; Bezzi, R.; Torri, C.; Galletti, P.; Tagliavini, E. [Bologna Univ., Ravenna (Italy). Lab. of Chemistry, C.I.R.S.A

    2007-09-15

    Oil wastes and slops are complex mixtures of hydrocarbons, which may contain a variety of contaminants including tetrachloroethylene (perchloroethylene, PCE) and other volatile halogenated organic compounds (VHOCs). The analytical determination of PCE at trace levels in petroleum-derived matrices is difficult to carry out in the presence of large amounts of hydrocarbon matrix components. In the following study, we demonstrate that headspace solid-phase microextraction (HS-SPME) combined with GC-MS analysis can be applied for the rapid measurement of PCE concentration in oil samples. The HS-SPME method was developed using liquid paraffin as matrix matching reference material for external and internal calibration and optimisation of experimental parameters. The limit of quantitation was 0.05 mg kg{sup -1}, and linearity was established up to 25 mg kg{sup -1}. The HS-SPME method was extended to several VHOCs, including trichloroethylene (TCE) in different matrices and was applied to the quantitative analysis of PCE and TCE in real samples.

  14. Kiwifruit Flower Odor Perception and Recognition by Honey Bees, Apis mellifera.

    Science.gov (United States)

    Twidle, Andrew M; Mas, Flore; Harper, Aimee R; Horner, Rachael M; Welsh, Taylor J; Suckling, David M

    2015-06-17

    Volatile organic compounds (VOCs) from male and female kiwifruit (Actinidia deliciosa 'Hayward') flowers were collected by dynamic headspace sampling. Honey bee (Apis mellifera) perception of the flower VOCs was tested using gas chromatography coupled to electroantennogram detection. Honey bees consistently responded to six compounds present in the headspace of female kiwifruit flowers and five compounds in the headspace of male flowers. Analysis of the floral volatiles by gas chromatography-mass spectrometry and microscale chemical derivatization showed the compounds to be nonanal, 2-phenylethanol, 4-oxoisophorone, (3E,6E)-α-farnesene, (6Z,9Z)-heptadecadiene, and (8Z)-heptadecene. Bees were then trained via olfactory conditioning of the proboscis extension response (PER) to synthetic mixtures of these compounds using the ratios present in each flower type. Honey bees trained to the synthetic mixtures showed a high response to the natural floral extracts, indicating that these may be the key compounds for honey bee perception of kiwifruit flower odor.

  15. Evaluation of peroxidative stress of cancer cells in vitro by real-time quantification of volatile aldehydes in culture headspace.

    Science.gov (United States)

    Shestivska, Violetta; Rutter, Abigail V; Sulé-Suso, Josep; Smith, David; Španěl, Patrik

    2017-08-30

    Peroxidation of lipids in cellular membranes results in the release of volatile organic compounds (VOCs), including saturated aldehydes. The real-time quantification of trace VOCs produced by cancer cells during peroxidative stress presents a new challenge to non-invasive clinical diagnostics, which as described here, we have met with some success. A combination of selected ion flow tube mass spectrometry (SIFT-MS), a technique that allows rapid, reliable quantification of VOCs in humid air and liquid headspace, and electrochemistry to generate reactive oxygen species (ROS) in vitro has been used. Thus, VOCs present in the headspace of CALU-1 cancer cell line cultures exposed to ROS have been monitored and quantified in real time using SIFT-MS. The CALU-1 lung cancer cells were cultured in 3D collagen to mimic in vivo tissue. Real-time SIFT-MS analyses focused on the volatile aldehydes: propanal, butanal, pentanal, hexanal, heptanal and malondialdehyde (propanedial), that are expected to be products of cellular membrane peroxidation. All six aldehydes were identified in the culture headspace, each reaching peak concentrations during the time of exposure to ROS and eventually reducing as the reactants were depleted in the culture. Pentanal and hexanal were the most abundant, reaching concentrations of a few hundred parts-per-billion by volume, ppbv, in the culture headspace. The results of these experiments demonstrate that peroxidation of cancer cells in vitro can be monitored and evaluated by direct real-time analysis of the volatile aldehydes produced. The combination of adopted methodology potentially has value for the study of other types of VOCs that may be produced by cellular damage. Copyright © 2017 John Wiley & Sons, Ltd.

  16. Classification of bacteria by simultaneous methylation-solid phase microextraction and gas chromatography/mass spectrometry analysis of fatty acid methyl esters.

    Science.gov (United States)

    Lu, Yao; Harrington, Peter B

    2010-08-01

    Direct methylation and solid-phase microextraction (SPME) were used as a sample preparation technique for classification of bacteria based on fatty acid methyl ester (FAME) profiles. Methanolic tetramethylammonium hydroxide was applied as a dual-function reagent to saponify and derivatize whole-cell bacterial fatty acids into FAMEs in one step, and SPME was used to extract the bacterial FAMEs from the headspace. Compared with traditional alkaline saponification and sample preparation using liquid-liquid extraction, the method presented in this work avoids using comparatively large amounts of inorganic and organic solvents and greatly decreases the sample preparation time as well. Characteristic gas chromatography/mass spectrometry (GC/MS) of FAME profiles was achieved for six bacterial species. The difference between Gram-positive and Gram-negative bacteria was clearly visualized with the application of principal component analysis of the GC/MS data of bacterial FAMEs. A cross-validation study using ten bootstrap Latin partitions and the fuzzy rule building expert system demonstrated 87 +/- 3% correct classification efficiency.

  17. Characterization of Volatile Compounds from Ethnic Agave Alcoholic Beverages by Gas Chromatography-Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Pilar Escalante-Minakata

    2008-01-01

    Full Text Available Ethnic Agave alcoholic beverages such as raicilla, sisal, tequila, mezcal, bacanora, sotol and pulque have been analyzed by gas chromatography and headspace solid-phase microextraction- gas chromatography-mass spectrometry (HS-SPME-GC-MS. There were 105 compounds identified, eleven were classified as major compounds and the others were classified as minor compounds. Seventeen minor compounds could be used as authenticity markers since they were beverage specific. Cluster analysis (CA showed that Agave alcoholic beverages could be distinguished by multivariate analysis of major compounds; however, the analysis of minor compounds provided a better fingerprinting.

  18. Rapid direct analysis to discriminate geographic origin of extra virgin olive oils by flash gas chromatography electronic nose and chemometrics.

    Science.gov (United States)

    Melucci, Dora; Bendini, Alessandra; Tesini, Federica; Barbieri, Sara; Zappi, Alessandro; Vichi, Stefania; Conte, Lanfranco; Gallina Toschi, Tullia

    2016-08-01

    At present, the geographical origin of extra virgin olive oils can be ensured by documented traceability, although chemical analysis may add information that is useful for possible confirmation. This preliminary study investigated the effectiveness of flash gas chromatography electronic nose and multivariate data analysis to perform rapid screening of commercial extra virgin olive oils characterized by a different geographical origin declared in the label. A comparison with solid phase micro extraction coupled to gas chromatography mass spectrometry was also performed. The new method is suitable to verify the geographic origin of extra virgin olive oils based on principal components analysis and discriminant analysis applied to the volatile profile of the headspace as a fingerprint. The selected variables were suitable in discriminating between "100% Italian" and "non-100% Italian" oils. Partial least squares discriminant analysis also allowed prediction of the degree of membership of unknown samples to the classes examined. Copyright © 2016. Published by Elsevier Ltd.

  19. Analysis of Odorants in Marking Fluid of Siberian Tiger (Panthera tigris altaica Using Simultaneous Sensory and Chemical Analysis with Headspace Solid-Phase Microextraction and Multidimensional Gas Chromatography-Mass Spectrometry-Olfactometry

    Directory of Open Access Journals (Sweden)

    Simone B. Soso

    2016-06-01

    Full Text Available Scent-marking is the most effective method of communication in the presence or absence of a signaler. These complex mixtures result in a multifaceted interaction triggered by the sense of smell. The objective was to identify volatile organic compound (VOC composition and odors emitted by total marking fluid (MF associated with Siberian tigers (Panthera tigris altaica. Siberian tiger, an endangered species, was chosen because its MF had never been analyzed. Solid phase microextraction (SPME for headspace volatile collection combined with multidimensional gas chromatography-mass spectrometry-olfactometry for simultaneous chemical and sensory analyses were used. Thirty-two VOCs emitted from MF were identified. 2-acetyl-1-pyrroline, the sole previously identified compound responsible for the “characteristic” odor of P. tigris MF, was identified along with two additional compounds confirmed with standards (urea, furfural and four tentatively identified compounds (3-methylbutanamine, (R-3-methylcyclopentanone, propanedioic acid, and 3-hydroxybutanal as being responsible for the characteristic aroma of Siberian tiger MF. Simultaneous chemical and sensory analyses improved characterization of scent-markings and identified compounds not previously reported in MF of other tiger species. This research will assist animal ecologists, behaviorists, and zookeepers in understanding how scents from specific MF compounds impact tiger and wildlife communication and improve management practices related to animal behavior. Simultaneous chemical and sensory analyses is applicable to unlocking scent-marking information for other species.

  20. Analysis of Odorants in Marking Fluid of Siberian Tiger (Panthera tigris altaica) Using Simultaneous Sensory and Chemical Analysis with Headspace Solid-Phase Microextraction and Multidimensional Gas Chromatography-Mass Spectrometry-Olfactometry.

    Science.gov (United States)

    Soso, Simone B; Koziel, Jacek A

    2016-06-25

    Scent-marking is the most effective method of communication in the presence or absence of a signaler. These complex mixtures result in a multifaceted interaction triggered by the sense of smell. The objective was to identify volatile organic compound (VOC) composition and odors emitted by total marking fluid (MF) associated with Siberian tigers (Panthera tigris altaica). Siberian tiger, an endangered species, was chosen because its MF had never been analyzed. Solid phase microextraction (SPME) for headspace volatile collection combined with multidimensional gas chromatography-mass spectrometry-olfactometry for simultaneous chemical and sensory analyses were used. Thirty-two VOCs emitted from MF were identified. 2-acetyl-1-pyrroline, the sole previously identified compound responsible for the "characteristic" odor of P. tigris MF, was identified along with two additional compounds confirmed with standards (urea, furfural) and four tentatively identified compounds (3-methylbutanamine, (R)-3-methylcyclopentanone, propanedioic acid, and 3-hydroxybutanal) as being responsible for the characteristic aroma of Siberian tiger MF. Simultaneous chemical and sensory analyses improved characterization of scent-markings and identified compounds not previously reported in MF of other tiger species. This research will assist animal ecologists, behaviorists, and zookeepers in understanding how scents from specific MF compounds impact tiger and wildlife communication and improve management practices related to animal behavior. Simultaneous chemical and sensory analyses is applicable to unlocking scent-marking information for other species.