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Sample records for spme measurements ranging

  1. Uptake of Radionuclide Metals by SPME Fibers

    International Nuclear Information System (INIS)

    Duff, M; S Crump, S; Robert Ray, R; Keisha Martin, K; Donna Beals, D

    2006-08-01

    The Federal Bureau of Investigation (FBI) Laboratory currently does not have on site facilities for handling radioactive evidentiary materials and there are no established FBI methods or procedures for decontaminating high explosive (HE) and fire debris (FD) evidence while maintaining evidentiary value. One experimental method for the isolation of HE and FD residue involves using solid phase microextraction or SPME fibers to remove residue of interest. Due to their high affinity for organics, SPME fibers should have little affinity for most metals. However, no studies have measured the affinity of radionuclides for SPME fibers. The focus of this research was to examine the affinity of dissolved radionuclide ( 239/240 Pu, 238 U, 237 Np, 85 Sr, 133 Ba, 137 Cs, 60 Co and 226 Ra) and stable radionuclide surrogate metals (Sr, Co, Ir, Re, Ni, Ba, Cs, Nb, Zr, Ru, and Nd) for SPME fibers at the exposure conditions that favor the uptake of HE and FD residues. Our results from radiochemical and mass spectrometric analyses indicate these metals have little measurable affinity for these SPME fibers during conditions that are conducive to HE and FD residue uptake with subsequent analysis by liquid or gas phase chromatography with mass spectrometric detection

  2. Further research on the photo-SPME of triclosan

    Energy Technology Data Exchange (ETDEWEB)

    Sanchez-Prado, Lucia; Llompart, Maria; Lores, Marta; Fernandez-Alvarez, Maria; Garcia-Jares, Carmen; Cela, Rafael [Universidad de Santiago de Compostela, Departamento de Quimica Analitica, Nutricion y Bromatologia. Facultad de Quimica, Instituto de Investigacion y Analisis Alimentario, Santiago de Compostela (Spain)

    2006-04-15

    In this study the photoinduced degradation of triclosan has been investigated by photo-solid-phase microextraction (photo-SPME). In photo-SPME, photodegradation is carried out on the SPME fibre containing the target compound. Triclosan was extracted from aqueous solutions by use of polydimethylsiloxane SPME fibres and these were subsequently exposed to UV irradiation (power 8 W, wavelength 254 nm) for different times (from 2 to 60 min). The photodegradation kinetics of triclosan were investigated, the photoproducts generated were tentatively identified, and the photochemical behaviour of these products was studied by use of this on-fibre approach followed by gas chromatographic-mass spectrometric analysis. Eight photoproducts were tentatively identified, including chlorinated phenols, chlorohydroxydiphenyl ethers, 2,8-dichlorodibenzo-p-dioxin, and a possible dichlorodibenzodioxin isomer or dichlorohydroxydibenzofuran. The main photodegradation mechanisms were postulated and photodegradation pathways proposed. The effect of pH on triclosan degradation and on triclosan-to-dioxin conversion was also investigated. Triclosan degradation occurred, and generation of 2,8-dichlorodibenzo-p-dioxin was confirmed, throughout the pH range studied (from 3 to 9). (orig.)

  3. 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.

  4. SPME-Based Ca-History Method for Measuring SVOC Diffusion Coefficients in Clothing Material.

    Science.gov (United States)

    Cao, Jianping; Liu, Ningrui; Zhang, Yinping

    2017-08-15

    Clothes play an important role in dermal exposure to indoor semivolatile organic compounds (SVOCs). The diffusion coefficient of SVOCs in clothing material (D m ) is essential for estimating SVOC sorption by clothing material and subsequent dermal exposure to SVOCs. However, few studies have reported the measured D m for clothing materials. In this paper, we present the solid-phase microextraction (SPME) based C a -history method. To the best of our knowledge, this is the first try to measure D m with known relative standard deviation (RSD). A thin sealed chamber is formed by a circular ring and two pieces of flat SVOC source materials that are tightly covered by the targeted clothing materials. D m is obtained by applying an SVOC mass transfer model in the chamber to the history of gas-phase SVOC concentrations (C a ) in the chamber measured by SPME. D m 's of three SVOCs, di-iso-butyl phthalate (DiBP), di-n-butyl phthalate (DnBP), and tris(1-chloro-2-propyl) phosphate (TCPP), in a cotton T-shirt can be obtained within 16 days, with RSD less than 3%. This study should prove useful for measuring SVOC D m in various sink materials. Further studies are expected to facilitate application of this method and investigate the effects of temperature, relative humidity, and clothing material on D m .

  5. Scalable improvement of SPME multipolar electrostatics in anisotropic polarizable molecular mechanics using a general short-range penetration correction up to quadrupoles.

    Science.gov (United States)

    Narth, Christophe; Lagardère, Louis; Polack, Étienne; Gresh, Nohad; Wang, Qiantao; Bell, David R; Rackers, Joshua A; Ponder, Jay W; Ren, Pengyu Y; Piquemal, Jean-Philip

    2016-02-15

    We propose a general coupling of the Smooth Particle Mesh Ewald SPME approach for distributed multipoles to a short-range charge penetration correction modifying the charge-charge, charge-dipole and charge-quadrupole energies. Such an approach significantly improves electrostatics when compared to ab initio values and has been calibrated on Symmetry-Adapted Perturbation Theory reference data. Various neutral molecular dimers have been tested and results on the complexes of mono- and divalent cations with a water ligand are also provided. Transferability of the correction is adressed in the context of the implementation of the AMOEBA and SIBFA polarizable force fields in the TINKER-HP software. As the choices of the multipolar distribution are discussed, conclusions are drawn for the future penetration-corrected polarizable force fields highlighting the mandatory need of non-spurious procedures for the obtention of well balanced and physically meaningful distributed moments. Finally, scalability and parallelism of the short-range corrected SPME approach are addressed, demonstrating that the damping function is computationally affordable and accurate for molecular dynamics simulations of complex bio- or bioinorganic systems in periodic boundary conditions. Copyright © 2016 Wiley Periodicals, Inc.

  6. Method for covering a spme fibre with carbon nanotubes and resulting spme fibre

    OpenAIRE

    Bertrán, Enric; Jover Comas, Eric; García Céspedes, Jordi; Bayona Termens, Josep María

    2010-01-01

    [EN] The invention relates to a method for covering solid phase microextraction (SPME) fibres with carbon nanotubes (CNT), comprising the following operations: (i) depositing a layer of a metal material on the SPME fibre; (ii) applying a heat treatment in order to form catalytic metal nanoparticles in a reducing atmosphere; and (iii) applying carbon using chemical deposition techniques, thereby forming CNT on top ofthe metal nanoparticles. The invention also relates to a fibre obtain...

  7. Determination of benzene, toluene, ethylbenzene and xylene in field and laboratory by means of cold fiber SPME equipped with thermoelectric cooler and GC/FID method

    Directory of Open Access Journals (Sweden)

    Tajik Leila

    2017-09-01

    Full Text Available A simple and effective cooling device based on a thermoelectric cooler was applied to cool the SPME fiber. The device was used for quantitative extraction of aromatic hydrocarbons in the air. Several factors such as coating temperature, extraction temperature and relative humidity in the laboratory setting were optimized. Comparison of the results between the cold fiber SPME (CF-SPME and NIOSH 1501 method on standard test atmosphere indicated a satisfactory agreement. The CF-SPME and SPME method were also compared. The results revealed that CF-SPME has the most appropriate outcome for the extraction of aromatic hydrocarbons from the ambient air. The cold fiber SPME technique showed good results for several validation parameters. Under the optimized conditions, the limits of detection (LOD and the limits of quantification (LOQ ranged from 0.00019 to 0.00033 and 0.0006 to 0.001 ng ml−1, respectively. The intra-day relative standard deviation (RSD showed ranging from 4.8 to 10.5%.

  8. Direct determination of anabolic steroids in pig urine by a new SPME-GC-MS method.

    Science.gov (United States)

    Zhang, Zhuomin; Duan, Hongbin; Zhang, Lan; Chen, Xi; Liu, Wei; Chen, Guonan

    2009-05-15

    A new solid phase microextraction (SPME) method coupled with gas chromatography-mass spectrometry (GC-MS) was developed for rapid determination of four anabolic steroids such as 3alpha-hydroxy-5alpha-androstane-17-one (HA), dihydrotestosterone (DHT), androstenedione (AD) and methyltestosterone (MT) in pig urine. SPME was used to extract the four anabolic compounds directly without derivatization. The optimum SPME sampling conditions were based on the home-made carbowax-divinylbenzene (CW-DVB) fiber coating during extraction at 40 degrees C for 50 min with 0.18 g/mL NaCl solution and 750 rpm stirring speed. The linear ranges of the proposed method were in the range of 8-640 pg/mL for HA and DHT and 16-510 pg/mL for AD and MT, respectively. The detection limits (S/N=3) were from 2 to 8 pg/mL for the four anabolic steroids. This SPME method provided very high enrichment factors for the four anabolic steroids, which were 1063-fold and 965-fold for HA and DHT at the concentration of 8 pg/mL and 207-fold and 451-fold for AD and MT at the concentration of 16 pg/mL, respectively. The recoveries ranged from 71.3 to 121%, and the RSDs were lower than 12.9%. The method was sensitive and reliable for determination of trace anabolic steroids in biological samples.

  9. Is Solid Phase Microextraction (SPME) an appropriate method for extraction of volatile oxidation products from complex food systems

    DEFF Research Database (Denmark)

    Jacobsen, Charlotte; Horn, Anna Frisenfeldt; Lu, Henna Fung Sieng

    Volatile secondary lipid oxidation products can be identified and quantified by GC-FID or GC-MS. An extraction step is, however, needed before GC analysis. A range of different extraction methods are available such as static headspace, dynamic headspace and SPME. Each of these methods has its...... advantages and drawbacks. Among the advantages of the SPME method are its high sensitivity compared to static headspace and that it is less laborious than the dynamic headspace method. For these reasons, the use of SPME has increased in both academia and industry during the last decade. The extraction...... for analysis of lipid oxidation during storage of complex food matrices. Examples on how uncontrollable factors have affected results obtained with the SPME method in the authors’ lab will be given and the appropriateness of the SPME method for the analysis of volatile oxidation products in selected food...

  10. Solid phase microextraction (SPME) for extraction of volatile oxidation products from complex food systems – Pros and cons

    DEFF Research Database (Denmark)

    Jacobsen, Charlotte; Horn, Anna Frisenfeldt; Lu, Henna Fung Sieng

    Volatile secondary lipid oxidation products can be identified and quantified by GC-FID or GC-MS. An extraction step is, however, needed before GC analysis. A range of different extraction methods are available such as static headspace, dynamic headspace and SPME. Each of these methods has its...... advantages and drawbacks. Among the advantages of the SPME method are its high sensitivity compared to static headspace and that it is less laborious than the dynamic headspace method. For these reasons, the use of SPME has increased in both academia and industry during the last decade. The extraction...... for analysis of lipid oxidation during storage of complex food matrices. Examples on how uncontrollable factors have affected results obtained with the SPME method in the authors’ lab will be given and the appropriateness of the SPME method for the analysis of volatile oxidation products in selected food...

  11. Role of nanoparticles in analytical solid phase microextraction (SPME)

    NARCIS (Netherlands)

    Zielinska, K.; Leeuwen, van H.P.

    2013-01-01

    Solid phase microextraction (SPME) is commonly used to measure the free concentration of fairly hydrophobic substances in aqueous media on the basis of their partitioning between sample solution and a solid phase. Here we study the role of nanoparticles that may sorb the analyte in the sample

  12. Phytoscreening with SPME: Variability Analysis.

    Science.gov (United States)

    Limmer, Matt A; Burken, Joel G

    2015-01-01

    Phytoscreening has been demonstrated at a variety of sites over the past 15 years as a low-impact, sustainable tool in delineation of shallow groundwater contaminated with chlorinated solvents. Collection of tree cores is rapid and straightforward, but low concentrations in tree tissues requires sensitive analytics. Solid-phase microextraction (SPME) is amenable to the complex matrix while allowing for solvent-less extraction. Accurate quantification requires the absence of competitive sorption, examined here both in laboratory experiments and through comprehensive examination of field data. Analysis of approximately 2,000 trees at numerous field sites also allowed testing of the tree genus and diameter effects on measured tree contaminant concentrations. Collectively, while these variables were found to significantly affect site-adjusted perchloroethylene (PCE) concentrations, the explanatory power of these effects was small (adjusted R(2) = 0.031). 90th quantile chemical concentrations in trees were significantly reduced by increasing Henry's constant and increasing hydrophobicity. Analysis of replicate tree core data showed no correlation between replicate relative standard deviation (RSD) and wood type or tree diameter, with an overall median RSD of 30%. Collectively, these findings indicate SPME is an appropriate technique for sampling and analyzing chlorinated solvents in wood and that phytoscreening is robust against changes in tree type and diameter.

  13. Sampling atmospheric pesticides with SPME: Laboratory developments and field study

    International Nuclear Information System (INIS)

    Wang Junxia; Tuduri, Ludovic; Mercury, Maud; Millet, Maurice; Briand, Olivier; Montury, Michel

    2009-01-01

    To estimate the atmospheric exposure of the greenhouse workers to pesticides, solid phase microextraction (SPME) was used under non-equilibrium conditions. Using Fick's law of diffusion, the concentrations of pesticides in the greenhouse can be calculated using pre-determined sampling rates (SRs). Thus the sampling rates (SRs) of two modes of SPME in the lab and in the field were determined and compared. The SRs for six pesticides in the lab were 20.4-48.3 mL min -1 for the exposed fiber and 0.166-0.929 mL min -1 for the retracted fiber. In field sampling, two pesticides, dichlorvos and cyprodinil were detected with exposed SPME. SR with exposed SPME for dichlorvos in the field (32.4 mL min -1 ) was consistent with that in the lab (34.5 mL min -1 ). SR for dichlorvos in the field (32.4 mL min -1 ) was consistent with that in the lab (34.5 mL min -1 ). The trends of temporal concentration and the inhalation exposure were also obtained. - SPME was proved to be a powerful and simple tool for determining pesticides' atmospheric concentration

  14. Selective molecularly imprinted polymer combined with restricted access material for in-tube SPME/UHPLC-MS/MS of parabens in breast milk samples

    International Nuclear Information System (INIS)

    Souza, Israel D.; Melo, Lidervan P.; Jardim, Isabel C.S.F.; Monteiro, Juliana C.S.; Nakano, Ana Marcia S.; Queiroz, Maria Eugênia C.

    2016-01-01

    A new molecularly imprinted polymer modified with restricted access material (a hydrophilic external layer), (MIP-RAM) was synthesized via polymerization in situ in an open fused silica capillary. This stationary phase was used as sorbent for in-tube solid phase microextraction (in-tube SPME) to determine parabens in breast milk samples by ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Scanning electron micrographs (SEM) illustrate MIP surface modification after glycerol dimethacrylate (hydrophilic monomer) incorporation. The interaction between parabens and MIP-RAM was investigated by Fourier-transform infrared (FTIR) spectroscopy. The Scatchard plot for MIP-RAM presented two linear parts with different slopes, illustrating binding sites with high- and low-affinity. Endogenous compounds exclusion from the MIP-RAM capillary was demonstrated by in-tube SPME/LC-UV assays carried out with blank milk samples. The in-tube SPME/UHPLC-MS/MS method presented linear range from 10 ng mL"−"1 (LLOQ) to 400 ng mL"−"1 with coefficients of determination higher than 0.99, inter-assay precision with coefficient of variation (CV) values ranging from 2 to 15%, and inter-assay accuracy with relative standard deviation (RSD) values ranging from −1% to 19%. Analytical validation parameters attested that in-tube SPME/UHPLC-MS/MS is an appropriate method to determine parabens in human milk samples to assess human exposure to these compounds. Analysis of breast milk samples from lactating women demonstrated that the proposed method is effective. - Highlights: • Molecularly imprinted polymer modified with a hydrophilic external layer (RAM-MIP) was synthesized in a silica capillary. • RAM-MIP capillary, used as sorbent for in-tube SPME, established specific interaction with parabens present in milk samples. • The matrix components that interacted only with the hydrophilic external layer (non-adsorptive network) were excluded. • The

  15. Selective molecularly imprinted polymer combined with restricted access material for in-tube SPME/UHPLC-MS/MS of parabens in breast milk samples

    Energy Technology Data Exchange (ETDEWEB)

    Souza, Israel D.; Melo, Lidervan P. [Departamento de Química, Faculdade de Filosofia Ciências e Letras de Ribeirão Preto, Universidade de São Paulo, Ribeirão Preto, SP (Brazil); Jardim, Isabel C.S.F. [Instituto de Química, Universidade Estadual de Campinas, Campinas, SP (Brazil); Monteiro, Juliana C.S.; Nakano, Ana Marcia S. [Escola de Enfermagem de Ribeirão Preto, Universidade de São Paulo, Ribeirão Preto, SP (Brazil); Queiroz, Maria Eugênia C., E-mail: mariaeqn@ffclrp.usp.br [Departamento de Química, Faculdade de Filosofia Ciências e Letras de Ribeirão Preto, Universidade de São Paulo, Ribeirão Preto, SP (Brazil)

    2016-08-17

    A new molecularly imprinted polymer modified with restricted access material (a hydrophilic external layer), (MIP-RAM) was synthesized via polymerization in situ in an open fused silica capillary. This stationary phase was used as sorbent for in-tube solid phase microextraction (in-tube SPME) to determine parabens in breast milk samples by ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Scanning electron micrographs (SEM) illustrate MIP surface modification after glycerol dimethacrylate (hydrophilic monomer) incorporation. The interaction between parabens and MIP-RAM was investigated by Fourier-transform infrared (FTIR) spectroscopy. The Scatchard plot for MIP-RAM presented two linear parts with different slopes, illustrating binding sites with high- and low-affinity. Endogenous compounds exclusion from the MIP-RAM capillary was demonstrated by in-tube SPME/LC-UV assays carried out with blank milk samples. The in-tube SPME/UHPLC-MS/MS method presented linear range from 10 ng mL{sup −1} (LLOQ) to 400 ng mL{sup −1} with coefficients of determination higher than 0.99, inter-assay precision with coefficient of variation (CV) values ranging from 2 to 15%, and inter-assay accuracy with relative standard deviation (RSD) values ranging from −1% to 19%. Analytical validation parameters attested that in-tube SPME/UHPLC-MS/MS is an appropriate method to determine parabens in human milk samples to assess human exposure to these compounds. Analysis of breast milk samples from lactating women demonstrated that the proposed method is effective. - Highlights: • Molecularly imprinted polymer modified with a hydrophilic external layer (RAM-MIP) was synthesized in a silica capillary. • RAM-MIP capillary, used as sorbent for in-tube SPME, established specific interaction with parabens present in milk samples. • The matrix components that interacted only with the hydrophilic external layer (non-adsorptive network) were excluded.

  16. Microextração por fase sólida SPME, Solid Phase Micro-Extration

    Directory of Open Access Journals (Sweden)

    Antonio Luiz Pires Valente

    2000-08-01

    Full Text Available Fundamental aspects of Solid Phase Micro-Extraction (SPME are discussed in the present paper. The application of SPME as a microtechnique of sample preparation for gas chromatographic analysis is considered and related to existing theoretical models. Both research prototypes and commercial SPME devices are considered.

  17. Analysis of flavor-related compounds from tabacco using SPME-GC-MS

    Energy Technology Data Exchange (ETDEWEB)

    Park, G.B.; Lee, S.G. [Korea Research Institute of Chemical Technology, Taejeon (Korea)

    2001-04-01

    The flavor-related compounds contained in tobacco were analyzed by selected ion monitoring (SIM) method using headspace SPME gas chromatography-mass spectrometry (GC-MS). Flavor-related compounds were estragole, pulegone, trans-anethole, safrole, piperonal, eugenol, methyleugenol, coumarin, trans-isoeugenol, trans-methyleugenol and myristicin More than one of the flavor-related compounds were detected in the range of 0.001-1.3 {mu}g/g from all brands of tobacco studied. The recovery was ranged from 89.1 to 102.9% and relative standard deviation was ranged from 2.6 to 25.2%. (author). 19 refs., 4 tabs., 2 figs.

  18. Differentiation of wines according to grape variety and geographical origin based on volatiles profiling using SPME-MS and SPME-GC/MS methods.

    Science.gov (United States)

    Ziółkowska, Angelika; Wąsowicz, Erwin; Jeleń, Henryk H

    2016-12-15

    Among methods to detect wine adulteration, profiling volatiles is one with a great potential regarding robustness, analysis time and abundance of information for subsequent data treatment. Volatile fraction fingerprinting by solid-phase microextraction with direct analysis by mass spectrometry without compounds separation (SPME-MS) was used for differentiation of white as well as red wines. The aim was to differentiate between varieties used for wine production and to also differentiate wines by country of origin. The results obtained were compared to SPME-GC/MS analysis in which compounds were resolved by gas chromatography. For both approaches the same type of statistical procedure was used to compare samples: principal component analysis (PCA) followed by linear discriminant analysis (LDA). White wines (38) and red wines (41) representing different grape varieties and various regions of origin were analysed. SPME-MS proved to be advantageous in use due to better discrimination and higher sample throughput. Copyright © 2016 Elsevier Ltd. All rights reserved.

  19. Measurement of the isotope ratio of acetic acid in vinegar by HS-SPME-GC-TC/C-IRMS.

    Science.gov (United States)

    Hattori, Ryota; Yamada, Keita; Shibata, Hiroki; Hirano, Satoshi; Tajima, Osamu; Yoshida, Naohiro

    2010-06-23

    Acetic acid is the main ingredient of vinegar, and the worth of vinegar often depends on the fermentation of raw materials. In this study, we have developed a simple and rapid method for discriminating the fermentation of the raw materials of vinegar by measuring the hydrogen and carbon isotope ratio of acetic acid using head space solid-phase microextraction (HS-SPME) combined with gas chromatography-high temperature conversion or combustion-isotope ratio mass spectrometry (GC-TC/C-IRMS). The measurement of acetic acid in vinegar by this method was possible with repeatabilities (1sigma) of +/-5.0 per thousand for hydrogen and +/-0.4 per thousand for carbon, which are sufficient to discriminate the origin of acetic acid. The fermentation of raw materials of several vinegars was evaluated by this method.

  20. Quantitative and enantioselective analysis of monoterpenes from plant chambers and in ambient air using SPME

    Directory of Open Access Journals (Sweden)

    N. Yassaa

    2010-11-01

    Full Text Available A headspace solid-phase microextraction (HS-SPME and gas chromatography/mass spectrometry (GC/MS system has been developed for quantifying enantiomeric and nonenantiomeric monoterpenes in plant chamber studies and ambient air. Performance of this system was checked using a capillary diffusion system to produce monoterpene standards. The adsorption efficiency, competitive adsorption and chromatographic peak resolution of monoterpene enantiomer pairs were compared for three SPME fibre coatings: 75 μm Carboxen-PDMS (CAR-PDMS, 50/30 μm divinylbenzene-carboxen-polydimethylsiloxane (DVB-CAR-PDMS and 65 μm divinylbenzene-polydimethylsiloxane (DVB-PDMS. Key parameters such as the linearity and reproducibility of the SPME system have been investigated in this work. The best compromise between the enantiomeric separation of monoterpenes and competitive adsorption of the isoprenoids on the solid SPME fibre coating was found for DVB-PDMS fibres. The optimum conditions using DVB-PDMS fibres were applied to measure the exchange rates of monoterpenes in the emission of Quercus ilex using a laboratory whole plant enclosure under light and dark conditions, as well as in ambient air. With 592 and 223 ng m−2 s−1 respectively, β-myrcene and limonene were the predominant monoterpenes in the emission of Q. ilex. These values were closely comparable to those obtained using a zNose and cartridge GC-FID systems.

  1. Quantitative and enantioselective analysis of monoterpenes from plant chambers and in ambient air using SPME

    Science.gov (United States)

    Yassaa, N.; Custer, T.; Song, W.; Pech, F.; Kesselmeier, J.; Williams, J.

    2010-11-01

    A headspace solid-phase microextraction (HS-SPME) and gas chromatography/mass spectrometry (GC/MS) system has been developed for quantifying enantiomeric and nonenantiomeric monoterpenes in plant chamber studies and ambient air. Performance of this system was checked using a capillary diffusion system to produce monoterpene standards. The adsorption efficiency, competitive adsorption and chromatographic peak resolution of monoterpene enantiomer pairs were compared for three SPME fibre coatings: 75 μm Carboxen-PDMS (CAR-PDMS), 50/30 μm divinylbenzene-carboxen-polydimethylsiloxane (DVB-CAR-PDMS) and 65 μm divinylbenzene-polydimethylsiloxane (DVB-PDMS). Key parameters such as the linearity and reproducibility of the SPME system have been investigated in this work. The best compromise between the enantiomeric separation of monoterpenes and competitive adsorption of the isoprenoids on the solid SPME fibre coating was found for DVB-PDMS fibres. The optimum conditions using DVB-PDMS fibres were applied to measure the exchange rates of monoterpenes in the emission of Quercus ilex using a laboratory whole plant enclosure under light and dark conditions, as well as in ambient air. With 592 and 223 ng m-2 s-1 respectively, β-myrcene and limonene were the predominant monoterpenes in the emission of Q. ilex. These values were closely comparable to those obtained using a zNose and cartridge GC-FID systems.

  2. SDE and SPME Analysis of Flavor Compounds in Jin Xuan Oolong Tea.

    Science.gov (United States)

    Sheibani, Ershad; Duncan, Susan E; Kuhn, David D; Dietrich, Andrea M; O'Keefe, Sean F

    2016-02-01

    Simultaneous distillation-extraction (SDE) and solid phase micro extraction (SPME) are procedures used for the isolation of flavor compounds in foods. The purpose of this study was to optimize SDE conditions (solvent and time) and to compare SDE with SPME for the isolation of flavor compounds in Jin Xuan oolong tea using GC-MS and GC-O. The concentration of volatile compounds isolated with diethyl ether was higher (P < 0.05) than for dichloromethane and concentration was higher at 40 min (P < 0.05) than 20 or 60 min extractions. For SDE, 128 volatiles were identified using GC-MS and 45 aroma active compounds using GC-O. Trans-nerolidol was the most abundant compound in oolong tea. The number of volatiles identified using GC-MS was lower in SPME than SDE. For SPME, 59 volatiles and 41 aroma active compounds were identified. The composition of the volatiles isolated by the 2 methods differed considerably but provided complementary information. © 2016 Institute of Food Technologists®

  3. Modified application of HS-SPME for quality evaluation of essential oil plant materials.

    Science.gov (United States)

    Dawidowicz, Andrzej L; Szewczyk, Joanna; Dybowski, Michal P

    2016-01-01

    The main limitation in the standard application of head space analysis employing solid phase microextraction (HS-SPME) for the evaluation of plants as sources of essential oils (EOs) are different quantitative relations of EO components from those obtained by direct analysis of EO which was got in the steam distillation (SD) process from the same plant (EO/SD). The results presented in the paper for thyme, mint, sage, basil, savory, and marjoram prove that the quantitative relations of EO components established by HS-SPME procedure and direct analysis of EO/SD are similar when the plant material in the HS-SPME process is replaced by its suspension in oil of the same physicochemical character as that of SPME fiber coating. The observed differences in the thyme EO composition estimated by both procedures are insignificant (F(exp)SPME procedure proposed in this paper substantially shortens the evaluation time of plant material quality and thus may improve the efficiency of analytical laboratories. Copyright © 2015 Elsevier B.V. All rights reserved.

  4. Determination of volatile organic compounds (VOCs) using tedlar bag/solid-phase microextraction/gas chromatography/mass spectrometry (SPME/GC/MS) in ambient and workplace air

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Jae Hwan; Lee, Dai Woon [Yonsei Univ., Seoul (Korea, Republic of); Hwang, Seung Man; Heo, Gwi Suk [Korea Research Institute of Standards and Science, Taejon (Korea, Republic of)

    2002-03-01

    SPME techniques have proven to be very useful tools in the analysis of wide VOCs in the air. In this study, we estimated VOCs in ambient and workplace air using a Tedlar ba/SPME/GC/MS system. The calibration curve was set to be linear over the range of 1-30 ppbv. The detection limits ranged from 10 pptv 0.93 ppbv for all VOCs. Reproducibility of TO-14 target gas mixtures by SPME/GC/MS averaged at 8.8 R.S.D (%). Air toxic VOCs (hazardous air pollutants, HAPs) containing a total of forty halohydrocarbons, aromatics, and haloaro-matic carbons could be analyzed with significant accuracy, detection limit and linearity at low ppbv level. Only reactive VOCs with low molecular weight, such as chloromethane, vinylchloride, ethylchloride and 1,2-dichloro-ethane, yielded relatively poor results using this technique. In ambient air samples, ten VOCs were identified and quantified after external calibration. VOC concentration in ambient and workplace air ranged from 0.04 to 1.85 ppbv. The overall process was successfully applied to identify and quantify VOCs in ambient/workplace air.

  5. Determination of volatile organic compounds (VOCs) using tedlar bag/solid-phase microextraction/gas chromatography/mass spectrometry (SPME/GC/MS) in ambient and workplace air

    International Nuclear Information System (INIS)

    Lee, Jae Hwan; Lee, Dai Woon; Hwang, Seung Man; Heo, Gwi Suk

    2002-01-01

    SPME techniques have proven to be very useful tools in the analysis of wide VOCs in the air. In this study, we estimated VOCs in ambient and workplace air using a Tedlar ba/SPME/GC/MS system. The calibration curve was set to be linear over the range of 1-30 ppbv. The detection limits ranged from 10 pptv 0.93 ppbv for all VOCs. Reproducibility of TO-14 target gas mixtures by SPME/GC/MS averaged at 8.8 R.S.D (%). Air toxic VOCs (hazardous air pollutants, HAPs) containing a total of forty halohydrocarbons, aromatics, and haloaro-matic carbons could be analyzed with significant accuracy, detection limit and linearity at low ppbv level. Only reactive VOCs with low molecular weight, such as chloromethane, vinylchloride, ethylchloride and 1,2-dichloro-ethane, yielded relatively poor results using this technique. In ambient air samples, ten VOCs were identified and quantified after external calibration. VOC concentration in ambient and workplace air ranged from 0.04 to 1.85 ppbv. The overall process was successfully applied to identify and quantify VOCs in ambient/workplace air

  6. Application of solid phase micro extraction (SPME) in profiling hydrocarbons in oil spill cases

    International Nuclear Information System (INIS)

    Zuraidah Abdullah Munir; Norashikin Saim; Nurul Huda Mamat Ghani

    2008-01-01

    In environmental forensic, it is extremely important to have a fast and reliable method in identifying sources of spilled oil and petroleum products. In this study, solid phase micro extraction (SPME) method coupled to gas chromatography-mass spectrometry was developed for the analysis of hydrocarbons in diesel and petroleum contaminated soil samples. Optimization of SPME parameters such as extraction time, extraction temperature and desorption time, was performed using 100-μm poly dimethylsiloxane (PDMS) fiber. These parameters were studied at three levels by means of a central composite experimental design and the optimum experimental conditions were determined using response surface method. The developed SPME method was applied to determine the profiles of hydrocarbons in several oil contaminated soil sample. The SPME method was also used to study the effects of weathering on the profiles of hydrocarbons in unleaded gasoline, diesel and kerosene contaminated soil samples. After several days, significant losses of the lighter hydrocarbons were observed compared to the heavier ones. From these data, SPME method can be used to differentiate possible candidate sources in oil spill cases. (author)

  7. Selective molecularly imprinted polymer combined with restricted access material for in-tube SPME/UHPLC-MS/MS of parabens in breast milk samples.

    Science.gov (United States)

    Souza, Israel D; Melo, Lidervan P; Jardim, Isabel C S F; Monteiro, Juliana C S; Nakano, Ana Marcia S; Queiroz, Maria Eugênia C

    2016-08-17

    A new molecularly imprinted polymer modified with restricted access material (a hydrophilic external layer), (MIP-RAM) was synthesized via polymerization in situ in an open fused silica capillary. This stationary phase was used as sorbent for in-tube solid phase microextraction (in-tube SPME) to determine parabens in breast milk samples by ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Scanning electron micrographs (SEM) illustrate MIP surface modification after glycerol dimethacrylate (hydrophilic monomer) incorporation. The interaction between parabens and MIP-RAM was investigated by Fourier-transform infrared (FTIR) spectroscopy. The Scatchard plot for MIP-RAM presented two linear parts with different slopes, illustrating binding sites with high- and low-affinity. Endogenous compounds exclusion from the MIP-RAM capillary was demonstrated by in-tube SPME/LC-UV assays carried out with blank milk samples. The in-tube SPME/UHPLC-MS/MS method presented linear range from 10 ng mL(-1) (LLOQ) to 400 ng mL(-1) with coefficients of determination higher than 0.99, inter-assay precision with coefficient of variation (CV) values ranging from 2 to 15%, and inter-assay accuracy with relative standard deviation (RSD) values ranging from -1% to 19%. Analytical validation parameters attested that in-tube SPME/UHPLC-MS/MS is an appropriate method to determine parabens in human milk samples to assess human exposure to these compounds. Analysis of breast milk samples from lactating women demonstrated that the proposed method is effective. Copyright © 2016 Elsevier B.V. All rights reserved.

  8. Measurement of Activity Coefficients at Infinite Dilution for Alcohols in [BMIM][CH3SO4] using HS-SPME/GC-FID

    Directory of Open Access Journals (Sweden)

    A. M. Elias

    Full Text Available ABSTRACT The activity coefficient at infinite dilution (&IN1 and distribution ratios at infinite dilution (&IN2 were determined for alkanols (methanol, ethanol, 1-propanol, 1-butanol, 2-butanol, and 2-methyl-2-propanol in the ionic liquid (IL 1-butyl-3-methylimidazolium methyl sulfate ([BMIM][CH3SO4] by HS-SPME (Headspace - Solid Phase Micro Extraction at four temperatures (298.15, 313.15, 333.15, and 353.15K using headspace - solid phase microextraction (SPME-HS. The results showed significant agreement with literature data. In addition, partial molar excess enthalpies at infinite dilution (&IN3, excess Gibbs energies (&IN4, and excess entropies (&IN5 were calculated from the (&IN6 values.

  9. Determination of fatty acids and volatile compounds in fruits of rosehip(Rosa L.) species by HS-SPME/GC-MS and Im-SPME/GC-MS techniques

    OpenAIRE

    MURATHAN, ZEHRA TUĞBA; ZARIFIKHOSROSHAHI, MOZGAN; KAFKAS, NESİBE EBRU

    2016-01-01

    In this study, we aimed to compare fatty acid and volatile compound compositions of four rosehip species, namely Rosa pimpinellifolia, R. Villosa, R. Canina, and R. Dumalis, by gas chromatography with flame ionization detector (GC/FID) and headspace and immersion solid-phase microextraction gas chromatography-mass spectrometry (HS-SPME/GC-MS and Im-SPME/GC-MS) techniques. The total lipid contents in fruits of the rosehip species varied from 5.83% (R. Villosa) to 7.84% (R. Dumalis). A total of...

  10. 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.

  11. SPME GC/MS Analysis of Three Ornithogalum L. species from Turkey

    Directory of Open Access Journals (Sweden)

    Gülin Renda

    2016-01-01

    Full Text Available In this study, a solid phase micro extraction (SPME method with gas chromatography-mass spectrometry (GC-MS was used for analysis of volatile compounds in flowers and bulbs of three Ornithogalum species. The samples of flowers and bulbs of Ornithogalum sigmoideum, Ornithogalum orthophyllum, Ornithogalum oligophyllum was separately analyzed by SPME-GC-MS. A comparison of volatile compounds was made between species and the parts studied. A total of 70 compounds were identified and different volatile compounds were determined in distinct parts of the species. The major volatile organic compound of the flowers of O. sigmoideum and O. ornithogalum was furan (54.5% and 57.0% respectively. For O. oligophyllum the major volatile organic compound was nonanal (19.2%. Analyses revealed that SPME-GC-MS method is appropriate for the analysis of volatile compounds of Ornithogalum species.

  12. Fast quantitation of opioid isomers in human plasma by differential mobility spectrometry/mass spectrometry via SPME/open-port probe sampling interface.

    Science.gov (United States)

    Liu, Chang; Gómez-Ríos, Germán Augusto; Schneider, Bradley B; Le Blanc, J C Yves; Reyes-Garcés, Nathaly; Arnold, Don W; Covey, Thomas R; Pawliszyn, Janusz

    2017-10-23

    Mass spectrometry (MS) based quantitative approaches typically require a thorough sample clean-up and a decent chromatographic step in order to achieve needed figures of merit. However, in most cases, such processes are not optimal for urgent assessments and high-throughput determinations. The direct coupling of solid phase microextraction (SPME) to MS has shown great potential to shorten the total sample analysis time of complex matrices, as well as to diminish potential matrix effects and instrument contamination. In this study, we demonstrate the use of the open-port probe (OPP) as a direct and robust sampling interface to couple biocompatible-SPME (Bio-SPME) fibres to MS for the rapid quantitation of opioid isomers (i.e. codeine and hydrocodone) in human plasma. In place of chromatography, a differential mobility spectrometry (DMS) device was implemented to provide the essential selectivity required to quantify these constitutional isomers. Taking advantage of the simplified sample preparation process based on Bio-SPME and the fast separation with DMS-MS coupling via OPP, a high-throughput assay (10-15 s per sample) with limits of detection in the sub-ng/mL range was developed. Succinctly, we demonstrated that by tuning adequate ion mobility separation conditions, SPME-OPP-MS can be employed to quantify non-resolved compounds or those otherwise hindered by co-extracted isobaric interferences without further need of coupling to other separation platforms. Copyright © 2017 Elsevier B.V. All rights reserved.

  13. Optimization of Solid Phase Micro-Extraction (SPME for Monitoring Occupational Exposure to Ethyl Benzene

    Directory of Open Access Journals (Sweden)

    H. Heidari

    2009-08-01

    Full Text Available AbstractBackground and Objectives: Analytical methods for volatile organic compounds (VOCs in different samples need extraction of compounds, by applying hazardous solvents. Solid phase micro-extraction (SPME is a solvent-free equilibrium extraction method, in which proper calibration can allow quantitative determinations of VOCs at a very good sensitivity without the use of any organic solvent. VOCs are generally present in urine only at trace levels, therefore, a sensitive procedure is needed for their trace determinations. Throughout this study, headspace solid phase micro-extraction (HS-SPME was followed by GC-FID for ethyl benzene in spiked urine was optimized.Methods: In this study, the parameters influencing SPME and gas chromatography of ethyl benzene, including extraction time, temperature, desorption temperature, desorption time, salt addition, sample pH, sample volume and sample agitation were investigated. Results: Extraction procedure was performed at 30°C for 6 min, using 0.2 gml-1 of NaCl in the sample solution. The sample volume and sample pH were optimized at 5 ml and 7 (neutral pH, respectively. Desorption of the ethyl benzene was carried out for 60 sec. at 250°C. The method was also validated with three different spiked urine samples and illustrated an appropriate reproducibility over six consecutive days as well as six within-day experiments. During this investigation, parameters of accuracy, linearity, and detection limits of the procedure were also evaluated.Conclusion: The developed method of HS- SPME-GC-FID proved to be a simple, convenient, and practical procedure, and was successfully used for measuring of ethyl benzene in spiked urine.

  14. Analysis of Volatile Markers for Virgin Olive Oil Aroma Defects by SPME-GC/FID: Possible Sources of Incorrect Data.

    Science.gov (United States)

    Oliver-Pozo, Celia; Aparicio-Ruiz, Ramón; Romero, Inmaculada; García-González, Diego L

    2015-12-09

    The need to explain virgin olive oil (VOO) aroma descriptors by means of volatiles has raised interest in applying analytical techniques for trapping and quantitating volatiles. Static headspace sampling with solid phase microextraction (SPME) as trapping material is one of the most applied solutions for analyzing volatiles. The use of an internal standard and the determination of the response factors of the main volatiles seem to guarantee the correct determination of volatile concentrations in VOOs by SPME-GC/FID. This paper, however, shows that the competition phenomena between volatiles in their adsorption to the SPME fiber, inherent in static headspace sampling, may affect the quantitation. These phenomena are more noticeable in the particular case of highly odorant matrices, such as rancid and vinegary VOOs with high intensity of defect. The competition phenomena can modify the measurement sensitivity, which can be observed in volatile quantitation as well as in the recording of internal standard areas in different matrices. This paper analyzes the bias of the peak areas and concentrations of those volatiles that are markers for each sensory defect of VOOs (rancid, vinegary, musty, and fusty) when the intensity and complexity of aroma are increased. Of the 17 volatile markers studied in this work, 10 presented some anomalies in the quantitation in highly odorant matrices due the competition phenomena. However, quantitation was not affected in the concentration ranges at which each volatile marker is typically found in the defective oils they were characteristic of, validating their use as markers.

  15. Comparative analysis of the aroma chemicals of Melissa officinalis using hydrodistillation and HS-SPME techniques

    Directory of Open Access Journals (Sweden)

    Shakeel-u- Rehman

    2017-05-01

    Full Text Available Headspace solid-phase micro extraction (HS-SPME coupled with gas chromatography–mass spectrometry (GC–MS has been used for the chemical analysis of Melissa officinalis (leaves cultivated in Institute Germplasm. The HS-SPME analysis led to the identification of 22 components constituting 99.1% of the total volatile constituents present in the leaves whereas its hydrodistillate led to the identification of 24 volatile constituents constituting 98.1% of the volatile material. The chemical composition of the SPME and hydrodistilled extract of M. officinalis leaves comprised mainly of oxygenated monoterpenes (78.5% and 57.8% respectively and sesquiterpene hydrocarbons (14.9% and 29.7% respectively. The major components identified in the HS-SPME extract were citronellal (31.1%, citronellol (18.3%, β-caryophyllene (12.0%, (E-citral (11.9%, (Z-citral (9.6%, geraniol (3.6%, (Z-β-ocimene (3.1% and 1-octen-3-ol (2.0% whereas hydrodistilled essential oil was rich in (Z-citral (19.6%, β-caryophyllene (13.2%, (E-citral (11.2%, citronellal (10.2%, germacrene-d (8.3%, δ-3-carene (5.0%, 6-methyl-5-hepten-2-one (3.7% and citronellyl acetate (3.7%. The comparative analysis of volatile constituents of M. officinalis leaf extract using HS-SPME and hydrodistillation techniques shows both qualitative as well as quantitative differences. The current study is the first report involving rapid analysis of volatile components of M. officinalis by HS-SPME.

  16. A rapid screening procedure for the analysis of proliferation compounds in complex matrices using solid phase microextraction (SPME) and SPME with in-situ derivatization

    International Nuclear Information System (INIS)

    Alcaraz, A.; Hulsey, S.S.; Andresen, B.D.

    1995-01-01

    A variety of methods have been established using advanced chromatographic techniques and new detection systems for the analysis of chemical signatures associated with nuclear and chemical weapon (CW) proliferation. Most of these analytical methods are used in the laboratory and seldom applied in the field. The Chemical Weapons Convention (an international treaty to ban chemical weapons) may require the rapid on-site analysis of environmental samples which contain CW agents, their precursors, and/or their degradation products. In addition to the fact that certain countries are involved in CW non-compliance, there is a current uncertainty regarding nuclear proliferation. This also creates new demands on sample work-up and analytical instrumentation use in the field. The isolation and identification of unique chemical signatures in complex samples such as soils, waste tanks, and decontamination solutions would determine non-compliance. However, a primary area of detection research continues to be sample preparation. Most of the established sample cleanup technologies involve liquid/liquid, Soxhlet, or most recently, solid phase extraction (SPE). Despite the success of these traditional sample preparation techniques, they are time consuming and require multi-step procedures (especially when preparing samples for gas chromatographic mass-spectrometric analysis). The goal of this work is to demonstrate the advantages of utilizing SPME and SPME in-situ derivatization techniques to eliminate time consuming steps necessary to prepare a sample for on-site GC-MS. The authors' approach was to compare two SPME fibers and to develop methods to facilitate the isolation of polar and moderately polar proliferation compounds from complex environmental samples. This work will help to evaluate current SPME technologies for use during on-site environmental monitoring analysis

  17. HS-SPME-GC-MS Analysis of onion (Allium cepa L. and shallot (Allium ascalonicum L.

    Directory of Open Access Journals (Sweden)

    D’Auria, M.

    2017-06-01

    Full Text Available The volatile organic compounds of onion and shallot were determined via HS-SPME-GC-MS. The main components were dipropyldisulphide and allylpropyldisulphide. Thiopropanal S-oxide were detected only in onion volatiles. In shallot is interesting the presence of 2-methyl-2-pentenal, a compound with an intense fruity aroma, that can characterize the different aroma between onion and shallot. The SPME-GC-MS analysis of shallot after absorption on the SPME fiber at 50°C showed the presence of new compounds, whose structures have been discussed.

  18. Optimization of Solid Phase Micro-Extraction (SPME for Monitoring Occupational Exposure to Ethyl Benzene

    Directory of Open Access Journals (Sweden)

    H Heidari

    2012-05-01

    Full Text Available

    Background and Objectives: Analytical methods for volatile organic compounds (VOCs in different samples need extraction of compounds, by applying hazardous solvents. Solid phase micro-extraction (SPME is a solvent-free equilibrium extraction method, in which proper calibration can allow quantitative determinations of VOCs at a very good sensitivity without the use of any organic solvent. VOCs are generally present in urine only at trace levels, therefore, a sensitive procedure is needed for their trace determinations. Throughout this study, headspace solid phase micro-extraction (HS-SPME was followed by GC-FID for ethyl benzene in spiked urine was optimized.

    Methods: In this study, the parameters influencing SPME and gas chromatography of ethyl benzene, including extraction time, temperature, desorption temperature, desorption time, salt addition, sample pH, sample volume and sample agitation were investigated.

    Results: Extraction procedure was performed at 30°C for 6 min, using 0.2 gml-1 of NaCl in the sample solution. The sample volume and sample pH were optimized at 5 ml and 7 (neutral pH, respectively. Desorption of the ethyl benzene was carried out for 60 sec. at 250°C. The method was also validated with three different spiked urine samples and illustrated an appropriate reproducibility over six consecutive days as well as six within-day experiments. During this investigation, parameters of accuracy, linearity, and detection limits of the procedure were also evaluated.

    Conclusion: The developed method of HS- SPME-GC-FID proved to be a simple, convenient, and practical procedure, and was successfully used for measuring of ethyl benzene in spiked urine.

  19. Analysis of aldehydes in human exhaled breath condensates by in-tube SPME-HPLC.

    Science.gov (United States)

    Wang, ShuLing; Hu, Sheng; Xu, Hui

    2015-11-05

    In this paper, polypyrrole/graphene (PPy/G) composite coating was prepared by a facile electrochemical polymerization strategy on the inner surface of a stainless steel (SS) tube. Based on the coating tube, a novel online in-tube solid-phase microextraction -high performance liquid chromatography (IT-SPME-HPLC) was developed and applied for the extraction of aldehydes in the human exhaled breath condensates (EBC). The hybrid PPy/G nanocomposite exhibits remarkable chemical and mechanical stability, high selectivity, and satisfactory extraction performance toward aldehyde compounds. Moreover, the proposed online IT-SPME-HPLC method possesses numerous superiorities, such as time and cost saving, process simplicity, high precision and sensitivity. Some parameters related to extraction efficiency were optimized systematically. Under the optimal conditions, the recoveries of the aldehyde compounds at three spiked concentration levels varied in the range of 85%-117%. Good linearity was obtained with excellent correlation coefficients (R(2)) being larger than 0.994. The relative standard deviations (n = 5) of the method ranged from 1.8% to 11.3% and the limits of detection were between 2.3 and 3.3 nmol L(-1). The successful application of the proposed method in human EBC indicated that it is a promising approach for the determination of trace aldehyde metabolites in complex EBC samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  20. Prediction of Partition Coefficients of Organic Compounds for SPME/PDMS

    Directory of Open Access Journals (Sweden)

    Liao Hsuan-Yu

    2016-01-01

    Full Text Available The partition coefficients of 51 organic compounds between SPME/PDMS and gas were compiled from the literature sources in this study. The effect of physicochemical properties and descriptors on the partitioning process of partition coefficients was explicated by the correlation analysis. The PDMS-gas partition coefficients were well correlated to the molecular weight of organic compounds (r = 0.832, p < 0.05. An empirical model, consisting of the molecular weight and the polarizability, was developed to appropriately predict the partition coefficients of organic compounds. The empirical model for estimating the PDMS-gas partition coefficient will contribute to the practical applications of the SPME technique.

  1. A comparison study on a sulfonated graphene-polyaniline nanocomposite coated fiber for analysis of nicotine in solid samples through the traditional and vacuum-assisted HS-SPME.

    Science.gov (United States)

    Ghiasvand, Alireza; Koonani, Samira; Yazdankhah, Fatemeh; Farhadi, Saeid

    2018-02-05

    A simple, rapid, and reliable headspace solid-phase microextraction (HS-SPME) procedure, reinforced by applying vacuum in the extraction vial, was developed. It was applied for the extraction of nicotine in solid samples prior to determination by gas chromatography-flame ionization detection (GC-FID). First, the surface of a narrow stainless steel wire was made porous and adhesive by platinization to obtain a durable, higher surface area, and resistant fiber. Then, a thin film of sulfonated graphene/polyaniline (Sulf-G/PANI) nanocomposite was synthesized and simultaneously coated on the platinized fiber using the electrophoretic deposition (EPD) method. It was demonstrated that the extraction efficiency remarkably increased by applying the reduced-pressure condition in the extraction vial. To evaluate the conventional HS-SPME and vacuum-assisted HS-SPME (VA-HS-SPME) platforms, all experimental parameters affecting the extraction efficiency including desorption time and temperature, extraction time and temperature and moisture content of sample matrix were optimized. The highest extraction efficiency was obtained at 60°C, 10min (extraction temperature and time) and 280°C, 2min (desorption condition), for VA-HS-SPME strategy, while for conventional HS-SPME the extraction and desorption conditions found to be 100°C, 30min and 280°C, 2min, respectively. The Sulf-G/PANI coated fiber showed high thermal stability, good chemical/mechanical resistance, and long lifetime. For analysis of nicotine in solid samples using VA-HS-SPME-GC-FID, linear dynamic range (LDR) was 0.01-30μgg -1 (R 2 =0.996), the relative standard deviation (RSD%, n=6), for analyses of 1μgg -1 nicotine was calculated 3.4% and limit of detection (LOD) found to be 0.002μgg -1 . The VA-HS-SPME-GC-FID strategy was successfully carried out for quantitation of nicotine in hair and tobacco real samples. Copyright © 2017 Elsevier B.V. All rights reserved.

  2. Quantitation of (R)- and (S)-linalool in beer using solid phase microextraction (SPME) in combination with a stable isotope dilution assay (SIDA).

    Science.gov (United States)

    Steinhaus, Martin; Fritsch, Helge T; Schieberle, Peter

    2003-11-19

    A stable isotope dilution assay (SIDA) was developed for the quantitation of both linalool enantiomers using synthesized [2H(2)]R/S-linalool as the internal standard. For enrichment of the target compound from beer, a solid phase microextraction method (SPME) was developed. In comparison to the more time-consuming extraction/distillation cleanup of the beer samples, the results obtained by SPME/SIDA were very similar, even under nonequilibration conditions. Analysis of five different types of beer showed significant differences in the linalool concentrations, which were clearly correlated with the intensity of the hoppy aroma note as evaluated by a sensory panel. In addition, significant differences in the R/S ratios were measured in the beers. The SPME/SIDA yielded exact data independently from headspace sampling parameters, such as exposure time or ionic strength of the solution.

  3. Field measurements of biogenic volatile organic compounds in the atmosphere using solid-phase microextraction Arrow

    Science.gov (United States)

    Feijó Barreira, Luís Miguel; Duporté, Geoffroy; Rönkkö, Tuukka; Parshintsev, Jevgeni; Hartonen, Kari; Hyrsky, Lydia; Heikkinen, Enna; Jussila, Matti; Kulmala, Markku; Riekkola, Marja-Liisa

    2018-02-01

    Biogenic volatile organic compounds (BVOCs) emitted by terrestrial vegetation participate in a diversity of natural processes. These compounds impact both short-range processes, such as on plant protection and communication, and long-range processes, for example by participating in aerosol particle formation and growth. The biodiversity of plant species around the Earth, the vast assortment of emitted BVOCs, and their trace atmospheric concentrations contribute to the substantial remaining uncertainties about the effects of these compounds on atmospheric chemistry and physics, and call for the development of novel collection devices that can offer portability with improved selectivity and capacity. In this study, a novel solid-phase microextraction (SPME) Arrow sampling system was used for the static and dynamic collection of BVOCs from a boreal forest, and samples were subsequently analyzed on site by gas chromatography-mass spectrometry (GC-MS). This system offers higher sampling capacity and improved robustness when compared to traditional equilibrium-based SPME techniques, such as SPME fibers. Field measurements were performed in summer 2017 at the Station for Measuring Ecosystem-Atmosphere Relations (SMEAR II) in Hyytiälä, Finland. Complementary laboratory tests were also performed to compare the SPME-based techniques under controlled experimental conditions and to evaluate the effect of temperature and relative humidity on their extraction performance. The most abundant monoterpenes and aldehydes were successfully collected. A significant improvement on sampling capacity was observed with the new SPME Arrow system over SPME fibers, with collected amounts being approximately 2 × higher for monoterpenes and 7-8 × higher for aldehydes. BVOC species exhibited different affinities for the type of sorbent materials used (polydimethylsiloxane (PDMS)-carbon wide range (WR) vs. PDMS-divinylbenzene (DVB)). Higher extraction efficiencies were obtained with dynamic

  4. A quantitative approach for pesticide analysis in grape juice by direct interfacing of a matrix compatible SPME phase to dielectric barrier discharge ionization-mass spectrometry.

    Science.gov (United States)

    Mirabelli, Mario F; Gionfriddo, Emanuela; Pawliszyn, Janusz; Zenobi, Renato

    2018-02-12

    We evaluated the performance of a dielectric barrier discharge ionization (DBDI) source for pesticide analysis in grape juice, a fairly complex matrix due to the high content of sugars (≈20% w/w) and pigments. A fast sample preparation method based on direct immersion solid-phase microextraction (SPME) was developed, and novel matrix compatible SPME fibers were used to reduce in-source matrix suppression effects. A high resolution LTQ Orbitrap mass spectrometer allowed for rapid quantification in full scan mode. This direct SPME-DBDI-MS approach was proven to be effective for the rapid and direct analysis of complex sample matrices, with limits of detection in the parts-per-trillion (ppt) range and inter- and intra-day precision below 30% relative standard deviation (RSD) for samples spiked at 1, 10 and 10 ng ml -1 , with overall performance comparable or even superior to existing chromatographic approaches.

  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. Method for sampling and analysis of volatile biomarkers in process gas from aerobic digestion of poultry carcasses using time-weighted average SPME and GC-MS.

    Science.gov (United States)

    Koziel, Jacek A; Nguyen, Lam T; Glanville, Thomas D; Ahn, Heekwon; Frana, Timothy S; Hans van Leeuwen, J

    2017-10-01

    A passive sampling method, using retracted solid-phase microextraction (SPME) - gas chromatography-mass spectrometry and time-weighted averaging, was developed and validated for tracking marker volatile organic compounds (VOCs) emitted during aerobic digestion of biohazardous animal tissue. The retracted SPME configuration protects the fragile fiber from buffeting by the process gas stream, and it requires less equipment and is potentially more biosecure than conventional active sampling methods. VOC concentrations predicted via a model based on Fick's first law of diffusion were within 6.6-12.3% of experimentally controlled values after accounting for VOC adsorption to the SPME fiber housing. Method detection limits for five marker VOCs ranged from 0.70 to 8.44ppbv and were statistically equivalent (p>0.05) to those for active sorbent-tube-based sampling. The sampling time of 30min and fiber retraction of 5mm were found to be optimal for the tissue digestion process. Copyright © 2017 Elsevier Ltd. All rights reserved.

  7. Determination of Pyrethroids in Tea Brew by GC-MS Combined with SPME with Multiwalled Carbon Nanotube Coated Fiber.

    Science.gov (United States)

    Ren, Dongxia; Sun, Chengjun; Ma, Guanqun; Yang, Danni; Zhou, Chen; Xie, Jiayu; Li, Yongxin

    2018-01-01

    A new method has been developed to simultaneously determine 7 pyrethroid residues in tea brew using gas chromatography-mass spectrometry (GC-MS) combined with solid phase microextraction (SPME) with multiwalled carbon nanotubes (MWCNTs) coated fiber. The MWCNTs coated fiber of SPME was homemade by using stainless steel wire as coating carrier and polyacrylonitrile (PAN) solution as adhesive glue. Under the optimized conditions, a good linearity was shown for bifenthrin, fenpropathrin, permethrin, and cyfluthrin in 1-50 ng mL -1 and for cypermethrin, fenvalerate, and deltamethrin in 5-50 ng mL -1 . The correlation coefficients were in the range of 0.9948-0.9999. The average recoveries of 7 pyrethroids were 94.2%-107.3% and the relative standard deviations (RSDs) were less than 15%. The detection limit of the method ranged from 0.12 to 1.65 ng mL -1 . The tea brew samples made from some commercial tea samples were analyzed. Among them, bifenthrin, fenpropathrin, and permethrin were found. The results show that the method is rapid and sensitive and requires low organic reagent consumption, which can be well used for the detection of the pyrethroids in tea brew.

  8. Comparison of the atmospheric- and reduced-pressure HS-SPME strategies for analysis of residual solvents in commercial antibiotics using a steel fiber coated with a multiwalled carbon nanotube/polyaniline nanocomposite.

    Science.gov (United States)

    Ghiasvand, Ali Reza; Nouriasl, Kolsoum; Yazdankhah, Fatemeh

    2018-01-01

    A low-cost, sensitive and reliable reduced-pressure headspace solid-phase microextraction (HS-SPME) setup was developed and evaluated for direct extraction of residual solvents in commercial antibiotics, followed by determination by gas chromatography with flame ionization detection (GC-FID). A stainless steel narrow wire was made porous and adhesive by platinization by a modified electrophoretic deposition method and coated with a polyaniline/multiwalled carbon nanotube nanocomposite. All experimental variables affecting the extraction efficiency were investigated for both atmospheric-pressure and reduced-pressure conditions. Comparison of the optimal experimental conditions and the results demonstrated that the reduced-pressure strategy leads to a remarkable increase in the extraction efficiency and reduction of the extraction time and temperature (10 min, 25 °Ϲ vs 20 min, 40 °Ϲ). Additionally, the reduced-pressure strategy showed better analytical performances compared with those obtained by the conventional HS-SPME-GC-FID method. Limit of detections, linear dynamic ranges, and relative standard deviations of the reduced-pressure HS-SPME procedure for benzene, toluene, ethylbenzene, and xylene (BTEX) in injectable solid drugs were obtained over the ranges of 20-100 pg g -1 , 0.02-40 μg g -1 , and 2.8-10.2%, respectively. The procedure developed was successful for the analysis of BTEX in commercial containers of penicillin, ampicillin, ceftriaxone, and cefazolin. Graphical abstract Schematic representation of the developed RP-HS-SPME setup.

  9. Comparison of Spot and Time Weighted Averaging (TWA Sampling with SPME-GC/MS Methods for Trihalomethane (THM Analysis

    Directory of Open Access Journals (Sweden)

    Don-Roger Parkinson

    2016-02-01

    Full Text Available Water samples were collected and analyzed for conductivity, pH, temperature and trihalomethanes (THMs during the fall of 2014 at two monitored municipal drinking water source ponds. Both spot (or grab and time weighted average (TWA sampling methods were assessed over the same two day sampling time period. For spot sampling, replicate samples were taken at each site and analyzed within 12 h of sampling by both Headspace (HS- and direct (DI- solid phase microextraction (SPME sampling/extraction methods followed by Gas Chromatography/Mass Spectrometry (GC/MS. For TWA, a two day passive on-site TWA sampling was carried out at the same sampling points in the ponds. All SPME sampling methods undertaken used a 65-µm PDMS/DVB SPME fiber, which was found optimal for THM sampling. Sampling conditions were optimized in the laboratory using calibration standards of chloroform, bromoform, bromodichloromethane, dibromochloromethane, 1,2-dibromoethane and 1,2-dichloroethane, prepared in aqueous solutions from analytical grade samples. Calibration curves for all methods with R2 values ranging from 0.985–0.998 (N = 5 over the quantitation linear range of 3–800 ppb were achieved. The different sampling methods were compared for quantification of the water samples, and results showed that DI- and TWA- sampling methods gave better data and analytical metrics. Addition of 10% wt./vol. of (NH42SO4 salt to the sampling vial was found to aid extraction of THMs by increasing GC peaks areas by about 10%, which resulted in lower detection limits for all techniques studied. However, for on-site TWA analysis of THMs in natural waters, the calibration standard(s ionic strength conditions, must be carefully matched to natural water conditions to properly quantitate THM concentrations. The data obtained from the TWA method may better reflect actual natural water conditions.

  10. Using SPME fibers and Tenax to predict the bioavailability of pyrethroids and chlorpyrifos in field sediments

    International Nuclear Information System (INIS)

    Harwood, Amanda D.; Landrum, Peter F.; Weston, Donald P.; Lydy, Michael J.

    2013-01-01

    The presence of pyrethroids in both urban and agricultural sediments at levels lethal to invertebrates has been well documented. However, variations in bioavailability among sediments make accurate predictions of toxicity based on whole sediment concentrations difficult. A proposed solution to this problem is the use of bioavailability-based estimates, such as solid phase microextraction (SPME) fibers and Tenax beads. This study compared three methods to assess the bioavailability and ultimately toxicity of pyrethroid pesticides including field-deployed SPME fibers, laboratory-exposed SPME fibers, and a 24-h Tenax extraction. The objective of the current study was to compare the ability of these methods to quantify the bioavailable fraction of pyrethroids in contaminated field sediments that were toxic to benthic invertebrates. In general, Tenax proved a more sensitive method than SPME fibers and a correlation between Tenax extractable concentrations and mortality was observed. - Highlights: ► Can use bioavailability-based methods for pyrethroids in sediments. ► Tenax was a more sensitive technique. ► Tenax extractable concentrations relate to invertebrate mortality. - This research provides an important first step in using bioavailability-based techniques for estimating the bioavailability and toxicity of hydrophobic pesticides in field sediments.

  11. Partitioning of the pesticide trifluralin between dissolved organic matter and water using automated SPME-GC/MS

    KAUST Repository

    Caupos, Emilie

    2014-10-04

    Solid-phase microextraction (SPME) was used to determine the equilibrium association constant for a pesticide, trifluralin (TFR), with dissolved organic matter (DOM). After optimization of the SPME method for the analysis of TFR, partition coefficients (K DOM) with three different sources of DOM were determined in buffered solutions at pH 7. Commercial humic acids and DOM fractions isolated from two surface waters were used. The values of log K DOMvaried from 4.3 to 5.8, depending on the nature of the organic material. A good correlation was established between log K DOMand DOM properties (as measured with the H/O atomic ratio and UV absorbance), in agreement with literature data. This is consistent with the effect of polarity and aromaticity for governing DOM-pollutant associations, regardless of the origin of DOM. This association phenomenon is relevant to better understand the behavior of pesticides in the environment since it controls part of pesticide leaching and fate in aquatic systems.

  12. HS-SPME-GC-MS ANALYSIS OF VOLATILE AND SEMI-VOLATILE COMPOUNDS FROM DRIED LEAVES OF Mikania glomerata Sprengel

    Directory of Open Access Journals (Sweden)

    Esmeraldo A. Cappelaro

    2015-03-01

    Full Text Available This paper reports on the identification of volatile and semi-volatile compounds and a comparison of the chromatographic profiles obtained by Headspace Solid-Phase Microextraction/Gas Chromatography with Mass Spectrometry detection (HS-SPME-GC-MS of dried leaves of Mikania glomerata Sprengel (Asteraceae, also known as 'guaco.' Three different types of commercial SPME fibers were tested: polydimethylsiloxane (PDMS, polydimethylsiloxane/divinylbenzene (PDMS/DVB and polyacrylate (PA. Fifty-nine compounds were fully identified by HS-SPME-HRGC-MS, including coumarin, a marker for the quality control of guaco-based phytomedicines; most of the other identified compounds were mono- and sesquiterpenes. PA fibers performed better in the analysis of coumarin, while PDMS-DVB proved to be the best choice for a general and non-selective analysis of volatile and semi-volatile guaco-based compounds. The SPME method is faster and requires a smaller sample than conventional hydrodistillation of essential oils, providing a general overview of the volatile and semi-volatile compounds of M. glomerata.

  13. A SPME-based method for rapidly and accurately measuring the characteristic parameter for DEHP emitted from PVC floorings.

    Science.gov (United States)

    Cao, J; Zhang, X; Little, J C; Zhang, Y

    2017-03-01

    Semivolatile organic compounds (SVOCs) are present in many indoor materials. SVOC emissions can be characterized with a critical parameter, y 0 , the gas-phase SVOC concentration in equilibrium with the source material. To reduce the required time and improve the accuracy of existing methods for measuring y 0 , we developed a new method which uses solid-phase microextraction (SPME) to measure the concentration of an SVOC emitted by source material placed in a sealed chamber. Taking one typical indoor SVOC, di-(2-ethylhexyl) phthalate (DEHP), as the example, the experimental time was shortened from several days (even several months) to about 1 day, with relative errors of less than 5%. The measured y 0 values agree well with the results obtained by independent methods. The saturated gas-phase concentration (y sat ) of DEHP was also measured. Based on the Clausius-Clapeyron equation, a correlation that reveals the effects of temperature, the mass fraction of DEHP in the source material, and y sat on y 0 was established. The proposed method together with the correlation should be useful in estimating and controlling human exposure to indoor DEHP. The applicability of the present approach for other SVOCs and other SVOC source materials requires further study. © 2016 John Wiley & Sons A/S. Published by John Wiley & Sons Ltd.

  14. Solid Phase Microextraction (SPME in Determination of Pesticide Residues in Soil Samples

    Directory of Open Access Journals (Sweden)

    Rada Đurović

    2011-01-01

    Full Text Available The basic principles and application possibilities of the methods based on solid phase microextraction (SPME in the analysis of pesticide residues in soil samples are presented in the paper. The most important experimental parameters which affect SPME efficacy inpesticide determination (type and thickness of microextraction fiber, duration of microextraction,temperature at which it is conducted, effect of addition of salts (the effect of efflorescence,temperature and time of desorption, the choice of optimal solvent for pesticide exctraction from the soil and the optimal number of extraction steps, as well as general guidelines for their optimization are also shown. In the end, current applications of SPMEmethods in the analysis of pesticide residues in soil samples are presented.

  15. Development of an SPME-GC-MS/MS method for the determination of pesticides in rainwater: Laboratory and field experiments

    International Nuclear Information System (INIS)

    Sauret-Szczepanski, Nathalie; Mirabel, Philippe; Wortham, Henri

    2006-01-01

    A solid-phase microextraction - coupled to a gas chromatography - ion trap tandem mass spectrometry (SPME-GC-MS/MS) method was developed for the quantitative determination in rainwater of 8 pesticides amongst the most used in France and 3 triazines metabolites. The main factors affecting the SPME process were studied. Using a 3 mL sample, the method developed showed good linearity for concentrations ranging from 0.05 to 50 μg L -1 with correlation coefficients between 0.997 and 0.9999 and relative standard deviations (% RSD) below 14%. The study of matrix effects showed that rainwater was too diluted to have any significant influence on the extraction efficiency. To validate the method, a field campaign was carried out on the rain events, which occurred in Strasbourg during a one-year period. The rain concentrations showed patterns of high pesticide concentrations during spring months, which were correlated to the spraying periods of most of these substances. - Solid-phase microextraction efficiency of pesticides in rainwater was optimized

  16. Determination of Pyrethroids in Tea Brew by GC-MS Combined with SPME with Multiwalled Carbon Nanotube Coated Fiber

    Directory of Open Access Journals (Sweden)

    Dongxia Ren

    2018-01-01

    Full Text Available A new method has been developed to simultaneously determine 7 pyrethroid residues in tea brew using gas chromatography-mass spectrometry (GC-MS combined with solid phase microextraction (SPME with multiwalled carbon nanotubes (MWCNTs coated fiber. The MWCNTs coated fiber of SPME was homemade by using stainless steel wire as coating carrier and polyacrylonitrile (PAN solution as adhesive glue. Under the optimized conditions, a good linearity was shown for bifenthrin, fenpropathrin, permethrin, and cyfluthrin in 1–50 ng mL−1 and for cypermethrin, fenvalerate, and deltamethrin in 5–50 ng mL−1. The correlation coefficients were in the range of 0.9948–0.9999. The average recoveries of 7 pyrethroids were 94.2%–107.3% and the relative standard deviations (RSDs were less than 15%. The detection limit of the method ranged from 0.12 to 1.65 ng mL−1. The tea brew samples made from some commercial tea samples were analyzed. Among them, bifenthrin, fenpropathrin, and permethrin were found. The results show that the method is rapid and sensitive and requires low organic reagent consumption, which can be well used for the detection of the pyrethroids in tea brew.

  17. Recent Developments and Applications of Solid Phase Microextraction (SPME in Food and Environmental Analysis—A Review

    Directory of Open Access Journals (Sweden)

    Sybille Merkle

    2015-06-01

    Full Text Available Solid-phase microextraction (SPME is a simple, sensitive, rapid and solvent-free technique for the extraction of analytes from gaseous, liquid and solid samples and takes a leading position among microextraction methods. Application of SPME in sample preparation has been increasing continuously over the last decade. It is most often used as an automatized fiber injection system coupled to chromatographic separation modules for the extraction of volatile and semivolatile organic compounds and also allows for the trace analysis of compounds in complex matrices. Since SPME was first introduced in the early 1990s, several modifications have been made to adapt the procedure to specific application requirements. More robust fiber assemblies and coatings with higher extraction efficiencies, selectivity and stability have been commercialized. Automation and on-line coupling to analytical instruments have been achieved in many applications and new derivatization strategies as well as improved calibration procedures have been developed to overcome existing limitations regarding quantitation. Furthermore, devices using tubes, needles or tips for extraction instead of a fiber have been designed. In the field of food analysis, SPME has been most often applied to fruit/vegetables, fats/oils, wine, meat products, dairy and beverages whereas environmental applications focus on the analysis of air, water, soil and sediment samples.

  18. Improving the On-Line Extraction of Polar Compounds by IT-SPME with Silica Nanoparticles Modified Phases

    Directory of Open Access Journals (Sweden)

    Pascual Serra-Mora

    2018-02-01

    Full Text Available In the present work the extraction efficiency of in-tube solid-phase microextraction (IT-SPME for polar herbicides has been evaluated using extractive capillaries coated with different polymeric sorbents. For this purpose, aqueous solutions of herbicides with a wide range of polarities, including some highly polar compounds (log Kow < 1, have been directly processed by IT-SPME coupled on-line to capillary liquid chromatography with UV-diode array detection. For extraction, commercially available capillary columns coated with polydimethylsiloxane (PDMS and polyetilenglicol (PEG-based phases have been used, and the results have been compared with those obtained with a synthesized tetraethyl orthosilicate (TEOS-trimethoxyethylsilane (MTEOS polymer, as well as the same polymer reinforced with silica nanoparticles (SiO2 NPs. The SiO2 NPs functionalized TEOS-MTEOS coating provided the best results for most herbicides, especially for the most polar compounds. On the basis of the results obtained, conditions for the quantification of the herbicides tested are described using a SiO2 NPs reinforced TEOS-MTEOS coated capillary. The proposed method provided satisfactory linearity up to concentrations of 200 μg/L. The precision was also suitable, with relative standard deviations (RSDs values ≤9% (n = 3, and the limits of detection (LODs were within the 0.5–7.5 µg/L range. The method has been applied to different water samples and the extract obtained from an agricultural soil.

  19. Quantification of transformation products of rocket fuel unsymmetrical dimethylhydrazine in soils using SPME and GC-MS.

    Science.gov (United States)

    Bakaikina, Nadezhda V; Kenessov, Bulat; Ul'yanovskii, Nikolay V; Kosyakov, Dmitry S

    2018-07-01

    Determination of transformation products (TPs) of rocket fuel unsymmetrical dimethylhydrazine (UDMH) in soil is highly important for environmental impact assessment of the launches of heavy space rockets from Kazakhstan, Russia, China and India. The method based on headspace solid-phase microextraction (HS SPME) and gas chromatography-mass spectrometry is advantageous over other known methods due to greater simplicity and cost efficiency. However, accurate quantification of these analytes using HS SPME is limited by the matrix effect. In this research, we proposed using internal standard and standard addition calibrations to achieve proper combination of accuracies of the quantification of key TPs of UDMH and cost efficiency. 1-Trideuteromethyl-1H-1,2,4-triazole (MTA-d3) was used as the internal standard. Internal standard calibration allowed controlling matrix effects during quantification of 1-methyl-1H-1,2,4-triazole (MTA), N,N-dimethylformamide (DMF), and N-nitrosodimethylamine (NDMA) in soils with humus content < 1%. Using SPME at 60 °C for 15 min by 65 µm Carboxen/polydimethylsiloxane fiber, recoveries of MTA, DMF and NDMA for sandy and loamy soil samples were 91-117, 85-123 and 64-132%, respectively. For improving the method accuracy and widening the range of analytes, standard addition and its combination with internal standard calibration were tested and compared on real soil samples. The combined calibration approach provided greatest accuracies for NDMA, DMF, N-methylformamide, formamide, 1H-pyrazole, 3-methyl-1H-pyrazole and 1H-pyrazole. For determination of 1-formyl-2,2-dimethylhydrazine, 3,5-dimethylpyrazole, 2-ethyl-1H-imidazole, 1H-imidazole, 1H-1,2,4-triazole, pyrazines and pyridines, standard addition calibration is more suitable. However, the proposed approach and collected data allow using both approaches simultaneously. Copyright © 2018 Elsevier B.V. All rights reserved.

  20. Cannabinoids determination in oral fluid by SPME-GC/MS and UHPLC-MS/MS and its application on suspected drivers.

    Science.gov (United States)

    Anzillotti, Luca; Castrignanò, Erika; Strano Rossi, Sabina; Chiarotti, Marcello

    2014-12-01

    The confirmation of Δ9-tetrahydrocannabinol (THC) in oral fluid (OF) is an important issue for assessing Driving Under the Influence of Drugs (DUID). The aim of this research was to develop a highly sensitive method with minimal sample pre-treatment suitable for the analysis of small OF volumes (100 μL) for the confirmation of cannabinoids in DUID cases. Two methods were compared for the confirmation of THC in residual OF samples, obtained from a preliminary on-site screening with commercial devices. An ultra high performance LC-MS (UHPLC-MS/MS) method and an SPME-GC/MS method were hence developed. 100 μL of the residual mixture OF/preservative buffer or neat OF was simply added to 10 μL of THC-D3 (1 μg/mL) and submitted to the two different analyses: A - direct injection of 10 μL in UHPLC-MS/MS in positive electrospray ionisation (ESI) mode and B - sampling for 30 min with SPME (100 μm polydimethylsiloxane or PDMS fibre) and direct injection by desorption of the fibre in the GC injection port. The lowest limit of detection (LLOD) of THC was 2 ng/mL in UHPLC-MS/MS and 0.5 ng/mL in SPME-GC/MS. In addition, cannabidiol (CBD) and cannabinol (CBN) could be detected in GC/MS equipment at 2 ng/mL, whilst in UHPLC-MS/MS the LLOD was 20 ng/mL. Both methods were applied to 70 samples coming from roadside tests. By SPME-GC/MS analysis, THC was confirmed in 42 samples, whilst CBD was detected in 21 of them, along with CBN in 14 samples. THC concentrations ranged from traces below the lowest limit of quantification or LLOQ (2 ng/mL) up to 690 ng/mL. Copyright © 2014 Forensic Science Society. Published by Elsevier Ireland Ltd. All rights reserved.

  1. pH-dependent equilibrium isotope fractionation associated with the compound specific nitrogen and carbon isotope analysis of substituted anilines by SPME-GC/IRMS.

    Science.gov (United States)

    Skarpeli-Liati, Marita; Turgeon, Aurora; Garr, Ashley N; Arnold, William A; Cramer, Christopher J; Hofstetter, Thomas B

    2011-03-01

    Solid-phase microextraction (SPME) coupled to gas chromatography/isotope ratio mass spectrometry (GC/IRMS) was used to elucidate the effects of N-atom protonation on the analysis of N and C isotope signatures of selected aromatic amines. Precise and accurate isotope ratios were measured using polydimethylsiloxane/divinylbenzene (PDMS/DVB) as the SPME fiber material at solution pH-values that exceeded the pK(a) of the substituted aniline's conjugate acid by two pH-units. Deviations of δ(15)N and δ(13)C-values from reference measurements by elemental analyzer IRMS were small (IRMS. Under these conditions, the detection limits for accurate isotope ratio measurements were between 0.64 and 2.1 mg L(-1) for δ(15)N and between 0.13 and 0.54 mg L(-1) for δ(13)C, respectively. Substantial inverse N isotope fractionation was observed by SPME-GC/IRMS as the fraction of protonated species increased with decreasing pH leading to deviations of -20‰ while the corresponding δ(13)C-values were largely invariant. From isotope ratio analysis at different solution pHs and theoretical calculations by density functional theory, we derived equilibrium isotope effects, EIEs, pertinent to aromatic amine protonation of 0.980 and 1.001 for N and C, respectively, which were very similar for all compounds investigated. Our work shows that N-atom protonation can compromise accurate compound-specific N isotope analysis of aromatic amines.

  2. A home-made SPME fiber coating for Arson Analysis

    International Nuclear Information System (INIS)

    Umi Khairul Ahmad; Abdul Rahim Yacob; Selvaraju, Geetha

    2008-01-01

    A number of adsorbents are available commercially as coatings for SPME fibers but some analytical methodologies might demand specific properties for the extraction of selected compounds, special coatings that have particular volume and a selectivity towards particular analytes. This paper presents a simple, fast, effective and environmental friendly methodology for the determination of accelerants in arson samples using headspace solid-phase micro extraction coupled to gas chromatography. A new fiber prepared by sol-gel method, containing 1:1 molar ratio of octyltriethoxysilane (C 8 -TEOS): methyltrimethoxysilane (MTMOS) was employed in this technique. The efficiency of the new fiber coating prepared by sol-gel technology for the determination of accelerants was compared to that of commercial PDMS/ DVB fibers. Poly dimethylsiloxane divinylbenzene (PDMS/ DVB) is the most common fiber coating for the extraction of hydrocarbon compounds. Compared with commercial PDMS/ DVB fiber, the new homemade fiber exhibited higher extraction capability and good selectivity for accelerants. The homemade fiber was also applied for the simulated arson samples. The home-made SPME adsorbent was shown to be a good alternative to commercially available fiber for the determination of accelerants in arson cases. (author)

  3. Application of Microextraction Techniques Including SPME and MESI to the Thermal Degradation of Polymers: A Review.

    Science.gov (United States)

    Kaykhaii, Massoud; Linford, Matthew R

    2017-03-04

    Here, we discuss the newly developed micro and solventless sample preparation techniques SPME (Solid Phase Microextraction) and MESI (Membrane Extraction with a Sorbent Interface) as applied to the qualitative and quantitative analysis of thermal oxidative degradation products of polymers and their stabilizers. The coupling of these systems to analytical instruments is also described. Our comprehensive literature search revealed that there is no previously published review article on this topic. It is shown that these extraction techniques are valuable sample preparation tools for identifying complex series of degradation products in polymers. In general, the number of products identified by traditional headspace (HS-GC-MS) is much lower than with SPME-GC-MS. MESI is particularly well suited for the detection of non-polar compounds, therefore number of products identified by this technique is not also to the same degree of SPME. Its main advantage, however, is its ability of (semi-) continuous monitoring, but it is more expensive and not yet commercialized.

  4. Why do Ladybugs Smell Bad? In-vivo Quantification of Odorous Insect Kairomones with SPME and Multidimensional GC-MS-Olfactometry

    International Nuclear Information System (INIS)

    Cai Lingshuang; Koziel, Jacek A.; O'Neal, Matthew E.

    2009-01-01

    Winemakers, small fruit growers, and homeowners are concerned with noxious compounds released by multicolored Asian ladybird beetles (Harmonia axyridis, Coleoptera: Coccinellidae). New method based on headspace solid phase microextraction (HS-SPME) coupled with multidimensional gas chromatography mass spectrometry--olfactometry (MDGC-MS-O) system was developed for extraction, isolation and simultaneous identification of compounds responsible for the characteristic odor of live H. axyridis. Four methoxypyrazines (MPs) were identified in headspace volatiles of live H. axyridis as those responsible for the characteristic odor: 2, 5-dimethy1-3-methoxypyrazine (DMMP), 2-isopropy1-3-methoxypyrazine (IPMP), 2-sec-buty1-3-methoxypyrazine (SBMP), and 2-isobuty1-3-methoxypyrazine (IBMP). To the best of our knowledge this is the first report of H. axyridis releasing DMMP and the first report of this compound being a component of the H. axyridis characteristic odor. Quantification of three MPs (IPMP, SBMP and IBMP) emitted from live H. axyridis were performed using external calibration with HS-SPME and direct injections. A linear relationship (R 2 >0.9958 for all 3 MPs) between MS response and concentration of standard was observed over a concentration range from 0.1 ng L -1 to 0.05 μg L -1 for HS-SPME-GC-MS. The method detection limits (MDL) based on multidimensional GC-MS approach for three MPs were estimated to be between 0.020 ng L -1 . to 0.022 ng L -1 . This methodology is applicable for in vivo determination of odor-causing chemicals associated with emissions of volatiles from insects.

  5. A high area, porous and resistant platinized stainless steel fiber coated by nanostructured polypyrrole for direct HS-SPME of nicotine in biological samples prior to GC-FID quantification.

    Science.gov (United States)

    Abdolhosseini, Sana; Ghiasvand, Alireza; Heidari, Nahid

    2017-09-01

    The surface of a stainless steel fiber was made porous, resistant and cohesive using electrophoretic deposition and coated by the nanostructured polypyrrole using an amended in-situ electropolymerization method. The coated fiber was applied for direct extraction of nicotine in biological samples through a headspace solid-phase microextraction (HS-SPME) method followed by GC-FID determination. The effects of the important experimental variables on the efficiency of the developed HS-SPME-GC-FID method, including pH of sample solution, extraction temperature and time, stirring rate, and ionic strength were evaluated and optimized. Under the optimal experimental conditions, the calibration curve was linear over the range of 0.1-20μgmL -1 and the detection limit was obtained 20ngmL -1 . Relative standard deviation (RSD, n=6) was calculated 7.6%. The results demonstrated the superiority of the proposed fiber compared with the most used commercial types. The proposed HS-SPME-GC-FID method was successfully used for the analysis of nicotine in urine and human plasma samples. Copyright © 2017 Elsevier B.V. All rights reserved.

  6. Optimization of HS-SPME/GC-MS analysis and its use in the profiling of illicit ecstasy tablets (Part 1).

    Science.gov (United States)

    Bonadio, Federica; Margot, Pierre; Delémont, Olivier; Esseiva, Pierre

    2009-05-30

    A headspace solid-phase microextraction procedure (HS-SPME) was developed for the profiling of traces present in 3,4-methylenedioxymethylampethamine (MDMA). Traces were first extracted using HS-SPME and then analyzed by gas chromatography-mass spectroscopy (GC-MS). The HS-SPME conditions were optimized using varying conditions. Optimal results were obtained when 40 mg of crushed MDMA sample was heated at 80 degrees C for 15 min, followed by extraction at 80 degrees C for 15 min with a polydimethylsiloxane/divinylbenzene coated fibre. A total of 31 compounds were identified as traces related to MDMA synthesis, namely precursors, intermediates or by-products. In addition some fatty acids used as tabletting materials and caffeine used as adulterant, were also detected. The use of a restricted set of 10 target compounds was also proposed for developing a screening tool for clustering samples having close profile. 114 seizures were analyzed using an SPME auto-sampler (MultiPurpose Samples MPS2), purchased from Gerstel GMBH & Co. (Germany), and coupled to GC-MS. The data was handled using various pre-treatment methods, followed by the study of similarities between sample pairs based on the Pearson correlation. The results show that HS-SPME, coupled with the suitable statistical method is a powerful tool for distinguishing specimens coming from the same seizure and specimens coming from different seizures. This information can be used by law enforcement personnel to visualize the ecstasy distribution network as well as the clandestine tablet manufacturing.

  7. Polyelectrolyte coatings prevent interferences from charged nanoparticles in SPME speciation analysis

    International Nuclear Information System (INIS)

    Zielińska, Katarzyna; Leeuwen, Herman P. van

    2014-01-01

    Highlights: • For the first time SPME fiber is coated with polyelectrolyte layer. • Sorption of nanoparticles on the solid phase surface is prevented. • Polyelectrolyte-modified fiber enables extraction of free analyte in presence of sorbing nanoparticles. - Abstract: In this work we present a new approach for protection of the fiber in solid phase microextraction (SPME) from interfering charged particles present in the sample medium. It involves coating of commercial poly(dimethylsiloxane) extraction phase with polyelectrolyte layer composed of poly(diallyldimethylammonium chloride), and poly(sodium 4-styrenesulfonate). The modified fiber provides reproducible, convenient and fast extraction capabilities toward the model analyte, triclosan (TCS). A negatively charged polyelectrolyte coating prevents sorbing oxidic nanoparticles from both partitioning into the PDMS phase and aggregation at its surface. The results for the TCS/nanoparticle sample show that the polyelectrolyte layer-modified solid phase extracts just the free form of the organic compound and enables dynamic speciation analysis of the nanoparticulate target analyte complex

  8. Quantitative Analysis of Bisphenol A Leached from Household Plastics by Solid-Phase Microextraction and Gas Chromatography-Mass Spectrometry (SPME-GC-MS)

    Science.gov (United States)

    Johnson, Bettie Obi; Burke, Fernanda M.; Harrison, Rebecca; Burdette, Samantha

    2012-01-01

    The measurement of trace levels of bisphenol A (BPA) leached out of household plastics using solid-phase microextraction (SPME) with gas chromatography-mass spectrometry (GC-MS) is reported here. BPA is an endocrine-disrupting compound used in the industrial manufacture of polycarbonate plastic bottles and epoxy resin can liners. This experiment…

  9. Multivariate statistical analysis of hemlock (Tsuga) volatiles by SPME/GC/MS: insights into the phytochemistry of the hemlock woolly adelgid (Adelges tsugae Annand)

    Science.gov (United States)

    Anthony Lagalante; Frank Calvosa; Michael Mirzabeigi; Vikram Iyengar; Michael Montgomery; Kathleen Shields

    2007-01-01

    A previously developed single-needle, SPME/GC/MS technique was used to measure the terpenoid content of T. canadensis growing in a hemlock forest at Lake Scranton, PA (Lagalante and Montgomery 2003). The volatile terpenoid composition was measured over a 1-year period from June 2003 to May 2004 to follow the annual cycle of foliage development from...

  10. 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.

  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. Polycyclic aromatic hydrocarbons bioavailability in industrial and agricultural soils: Linking SPME and Tenax extraction with bioassays.

    Science.gov (United States)

    Guo, Meixia; Gong, Zongqiang; Li, Xiaojun; Allinson, Graeme; Rookes, James; Cahill, David

    2017-06-01

    The aims of this study were to evaluate the bioavailability of polycyclic aromatic hydrocarbons (PAHs) in industrial and agricultural soils using chemical methods and a bioassay, and to study the relationships between the methods. This was conducted by comparing the quantities of PAHs extracted from two manufactured gas plant (MGP) soils and an agricultural soil with low level contamination by solid-phase micro-extraction (SPME) and Tenax-TA extraction with the quantities taken up by the earthworm (Eisenia fetida). In addition, a biodegradation experiment was conducted on one MGP soil (MGP-A) to clarify the relationship between PAH removal by biodegradation and the variation in PAH concentrations in soil pore water. Results demonstrated that the earthworm bioassay could not be used to examine PAH bioavailability in the tested MGP soils; which was the case even in the diluted MGP-A soils after biodegradation. However, the bioassay was successfully applied to the agricultural soil. These results suggest that earthworms can only be used for bioassays in soils with low toxicity. In general, rapidly desorbing concentrations extracted by Tenax-TA could predict PAH concentrations accumulated in earthworms (R 2 =0.66), while SPME underestimated earthworm concentrations by a factor of 2.5. Both SPME and Tenax extraction can provide a useful tool to predict PAH bioavailability for earthworms, but Tenax-TA extraction was proven to be a more sensitive and precise method than SPME for the prediction of earthworm exposure in the agricultural soil. Copyright © 2017. Published by Elsevier Inc.

  13. Validace HPLC metody stanovení piroxikamu v plasmě s využitím SPME a deproteinace

    OpenAIRE

    Kuželová, Kristýna

    2015-01-01

    Validation of HPLC evaluatoin of piroxicam in plasma using SPME and precipitation Rigorous Thesis Mgr. Kristýna Kuželová Charles University in Prague, Faculty of Pharmacy in Hradec Kralove, Department of Pharmaceutical Chemistry and Drug Control, Heyrovského 1203, Hradec Králové The purpose of this thesis was bioanalytical evalution of piroxicam using High Performance Liquid Chromatagraphy (HPLC). Piroxicam was isolated from plasma using SPME and protein precipitacion. Plasma was adjusted to ...

  14. Evaluation of the volatile profile of Tuber liyuanum by HS-SPME with GC-MS.

    Science.gov (United States)

    Liu, Changjiao; Li, Yu

    2017-04-01

    The volatile components of Tuber liyuanum were determined by HS-SPME with GC-MS for the first time. The effects of different fibre coating, extraction time, extraction temperature and sample amount were studied to get optimal extraction conditions. The optimal conditions were SPME fibre of Carboxen/PDMS, extraction time of 40 min, extraction temperature of 80 °C, sample amount of 2 g. Under these conditions 57 compounds in volatile of T. liyuanum were detected with a resemblance percentage above 80%. Aldehydes and aromatics were the main chemical families identified. The contribution of 3-Octanone(11.67%), phenylethyl alcohol (10.60%), isopentana (9.29%) and methylbutana (8.06%) for the total volatile profile were more significant in T. liyuanum than other compounds.

  15. Rapid sampling of BTEX in air by SPME in the city of Nice and at the Nice-Cote d'Azur airport

    International Nuclear Information System (INIS)

    Tumbiolo, S.; Gal, J.F.; Maria, P.Ch.; Laborde, P.; Teton, S.

    2006-01-01

    This article presents the results of a tentative application of Solid Phase Micro Extraction (SPME) to the analysis of BTEX (benzene, toluene, ethyl-benzene and xylenes) at the μg/m 3 level in indoor and outdoor air. The salient features of the method validation are reported. Sampling by QUALITAIR using Radiello passive samplers, was carried out from 2001 to 2004 in the city of Nice and its airport. Urban traffic impact was proved, but a link between BTX concentrations and the variations of airport activities was not clearly established. During the same period, several samplings were performed using SPME. Taking into account the short (30 minutes) sampling time, rapid changes of BTEX concentrations were evidenced, as for example the start of airplane engines. As field studies have shown, SPME technique appears as a method of choice for fast qualitative analysis and quantitative determination of Volatile Organic Compounds (VOC). The small dimensions of the SPME sampling system and the short sampling time let envisage its utilisation for the rapid diagnostic and the monitoring of indoor air quality. (author)

  16. Nuevos desarrollos metodológicos en SPME

    OpenAIRE

    Ríos Acevedo, John Jairo

    2016-01-01

    La Microextracción en fase sólida (SPME) ha experimentado un rápido desarrollo desde su introducción hace más de 20 años teniendo un gran impacto sobre las prácticas de muestreo y preparación de muestra en áreas como análisis químico, bioanálisis, los alimentos y las ciencias ambientales. Sin embargo, en otras áreas como análisis clínico, ciencias farmacéuticas y médicas, se espera un crecimiento en sus aplicaciones. El objetivo fundamental de la presente investigación ha sido la implementaci...

  17. Using disposable solid-phase microextraction (SPME) to determine the freely dissolved concentration of polybrominated diphenyl ethers (PBDEs) in sediments

    International Nuclear Information System (INIS)

    Jia Fang; Cui Xinyi; Wang Wei; Delgado-Moreno, Laura; Gan, Jay

    2012-01-01

    Polybrominated diphenyl ethers (PBDEs) are brominated flame retardants (BFRs). The ubiquity and persistence of PBDEs in sediment have raised concerns over their environmental fate and ecological risks. Due to strong affinity for sediment organic matter, environmental fate and bioavailability of PBDEs closely depend on their phase distribution. In this study, disposable polydimethylsiloxane (PDMS) fiber was used to derive the freely dissolved concentration (C free ) of PBDEs in sediment porewater as a measurement of bioavailability. The PDMS-to-water partition coefficient (log K PDMS ) was 5.46–5.83 for BDE 47, 99, and 153. In sediments, PBDEs were predominantly sorbed to the sediment phase, with C free accounting for free of PBDEs decreased as their bromination or sediment organic carbon content increased. The strong association with dissolved organic matter (DOM) implies a potential for facilitated offsite transport and dispersion in the environment that depends closely on the stability of sediment aggregates. - Highlights: ► A disposable SPME method was developed for measuring C free of PBDEs in sediment. ► C free decreased with increasing congener bromination or sediment OC content. ► C free of PBDEs accounted for DOC values suggest a high probability for DOM-facilitated offsite transport. - A SPME method based on disposable PDMS fibers was developed for measuring the freely dissolved concentration of PBDEs (C free ) in sediment porewater.

  18. 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...

  19. Simple and accurate quantification of BTEX in ambient air by SPME and GC-MS.

    Science.gov (United States)

    Baimatova, Nassiba; Kenessov, Bulat; Koziel, Jacek A; Carlsen, Lars; Bektassov, Marat; Demyanenko, Olga P

    2016-07-01

    Benzene, toluene, ethylbenzene and xylenes (BTEX) comprise one of the most ubiquitous and hazardous groups of ambient air pollutants of concern. Application of standard analytical methods for quantification of BTEX is limited by the complexity of sampling and sample preparation equipment, and budget requirements. Methods based on SPME represent simpler alternative, but still require complex calibration procedures. The objective of this research was to develop a simpler, low-budget, and accurate method for quantification of BTEX in ambient air based on SPME and GC-MS. Standard 20-mL headspace vials were used for field air sampling and calibration. To avoid challenges with obtaining and working with 'zero' air, slope factors of external standard calibration were determined using standard addition and inherently polluted lab air. For polydimethylsiloxane (PDMS) fiber, differences between the slope factors of calibration plots obtained using lab and outdoor air were below 14%. PDMS fiber provided higher precision during calibration while the use of Carboxen/PDMS fiber resulted in lower detection limits for benzene and toluene. To provide sufficient accuracy, the use of 20mL vials requires triplicate sampling and analysis. The method was successfully applied for analysis of 108 ambient air samples from Almaty, Kazakhstan. Average concentrations of benzene, toluene, ethylbenzene and o-xylene were 53, 57, 11 and 14µgm(-3), respectively. The developed method can be modified for further quantification of a wider range of volatile organic compounds in air. In addition, the new method is amenable to automation. Copyright © 2016 Elsevier B.V. All rights reserved.

  20. Use of solid-phase microextraction (SPME) for the determination of methadone and EDDP in human hair by GC-MS.

    Science.gov (United States)

    Lucas, A C; Bermejo, A M; Tabernero, M J; Fernández, P; Strano-Rossi, S

    2000-01-10

    Solid-phase microextraction (SPME) is a new extraction technique with many advantages: small sample volume, simplicity, quickness and solvent-free. It is mainly applied to environmental analysis, but is also useful for the extraction of drugs from biological samples. In this paper the use of SPME is proposed for the determination of methadone and its main metabolite EDDP in hair by GC-MS. The hair samples were washed, cut into 1-mm segments, and incubated with Pronase E for 12 h. A 100-micron polydimethylsiloxane (PDMS) film fibre was submerged for 30 min in a diluted solution of the hydrolysis liquid (1:4 with borax buffer) containing methadone-d3 and EDDP-d3 as internal standards. Once the microextraction was concluded the fibre was directly inserted into the CG injection port. Linearity was found for methadone and EDDP in the range studied, 1.0-50 ng/mg hair, with correlation coefficients higher than 0.99. Interassay relative standard deviation (R.S.D) was determined to be less than 13.30% for methadone and less than 8.94% for EDDP, at 3.0 and 30.0 ng/mg. Analytical recoveries were close to 100% for both compounds on spiked samples. The method was applied to the analysis of real hair samples from eight patients of a methadone maintenance programme. The concentration of methadone in hair ranged from 2.45 to 78.10 ng/mg, and for EDDP from 0.98 to 7.76 ng/mg of hair.

  1. Sol-gel-based SPME fiber as a reliable sampling technique for studying biogenic volatile organic compounds released from Clostridium tetani.

    Science.gov (United States)

    Ghader, Masoud; Shokoufi, Nader; Es-Haghi, Ali; Kargosha, Kazem

    2017-11-01

    A novel and efficient headspace solid-phase microextraction (HS-SPME) method, followed by gas chromatography mass spectrometry (GC-MS), was developed to study volatile organic compounds (VOCs) emerging from microorganisms. Two homemade SPME fibers, a semi-polar poly (dimethylsiloxane) (PDMS) fiber, and a polar polyethylene glycol (PEG) fiber, along with two commercial fibers (PDMS and PDMS/DVB) were used to collect VOCs emerging from Clostridium tetani which was cultured in different media. The adsorbed VOCs were desorbed and identified, in vitro, using GC-MS. The adsorption efficiency was improved by optimizing the time duration of adsorption and desorption. About 50 components were identified by the proposed method. The main detected compounds appeared to be sulfur containing compounds such as butanethioic acid S-methyl ester, dimethyl trisulfide, and dimethyl tetrasulfide. These volatile sulfur containing compounds are derived from amino acids containing the sulfur element, which probably coexist in the mentioned bacterium or are added to the culture media. The developed HS-SPME-GC-MS method allowed the determination of the chemical fingerprint of Clostridium tetani volatile constituents, and thus provides a new, simple, and reliable tool for studying the growth of microorganisms. Graphical abstract Investigation of biogenic VOCs released from Clostridium tetani using SPME-GC-MS.

  2. Prediction of Partition Coefficients of Organic Compounds for SPME/PDMS

    OpenAIRE

    Liao Hsuan-Yu; Huang Miao-Ling; Lu Yu-Ting; Chao Keh-Ping

    2016-01-01

    The partition coefficients of 51 organic compounds between SPME/PDMS and gas were compiled from the literature sources in this study. The effect of physicochemical properties and descriptors on the partitioning process of partition coefficients was explicated by the correlation analysis. The PDMS-gas partition coefficients were well correlated to the molecular weight of organic compounds (r = 0.832, p < 0.05). An empirical model, consisting of the molecular weight and the polarizability, was ...

  3. Soliton microcomb range measurement

    Science.gov (United States)

    Suh, Myoung-Gyun; Vahala, Kerry J.

    2018-02-01

    Laser-based range measurement systems are important in many application areas, including autonomous vehicles, robotics, manufacturing, formation flying of satellites, and basic science. Coherent laser ranging systems using dual-frequency combs provide an unprecedented combination of long range, high precision, and fast update rate. We report dual-comb distance measurement using chip-based soliton microcombs. A single pump laser was used to generate dual-frequency combs within a single microresonator as counterpropagating solitons. We demonstrated time-of-flight measurement with 200-nanometer precision at an averaging time of 500 milliseconds within a range ambiguity of 16 millimeters. Measurements at distances up to 25 meters with much lower precision were also performed. Our chip-based source is an important step toward miniature dual-comb laser ranging systems that are suitable for photonic integration.

  4. Essential oil from Rhaponticum acaule L. roots: Comparative study using HS-SPME/GC/GC–MS and hydrodistillation techniques

    Directory of Open Access Journals (Sweden)

    Batoul Benyelles

    2014-12-01

    Full Text Available The composition of essential oil extracted from Rhaponticum acaule L. roots growing wild in Algeria was studied by hydrodistillation (HD and by Head-Space Solid Phase Micro-Extraction (HS-SPME. Quantitative but not qualitative differences have been found in the chemical composition of both analysed samples depending on the extraction method. However, the oil obtained from R. acaule roots shows that aliphatic alcohols were found to be the major class (69.2%, followed by the terpenes (5.5%, alkenes (5.2% and alkynes (4.0%. In both cases the analysis were carried out using Gas Chromatography (GC and Gas Chromatography–Mass Spectrometry (GC–MS. Our study shows that HS-SPME extraction could be considered as an alternative technique for the isolation of volatiles from plant. 25 components were identified in oil vs. 39 in the HS-SPME. However the oil composition of roots was mainly represented by a variety of aliphatic hydrocarbons (alcohols, aldehydes and ketones and terpenes which are known for their antimicrobial activities.

  5. Nanoparticle-Incorporated PDMS Film as an Improved Performance SPME Fiber for Analysis of Volatile Components of Eucalyptus Leaf

    Directory of Open Access Journals (Sweden)

    Parviz Aberoomand Azar

    2013-01-01

    Full Text Available A new fabrication strategy was proposed to prepare polydimethylsiloxane (PDMS- coated solid-phase microextraction (SPME on inexpensive and unbreakable Cu fiber. PDMS was covalently bonded to the Cu substrate using self-assembled monolayer (SAM of (3-mercaptopropyltrimethoxysilane (3MPTS as binder. To increase the performance of the fiber, the incorporation effect of some nanomaterials including silica nanoparticles (NPs, carbon nanotubes (CNTs, and carboxylated carbon nanotubes (CNT-COOH to PDMS coating was compared. The surface morphology of the prepared fibers was characterized by scanning electron microscopy (SEM, and their applicability was evaluated through the extraction of some volatile organic compounds (VOCs of Eucalyptus leaf in headspace mode, and parameters affecting the extraction efficiency including extraction temperature and extraction time were optimized. Extracted compounds were analyzed by GC-MS instrument. The results obtained indicated that prepared fibers have some advantages relative to previously prepared SPME fibers, such as higher thermal stability and improved performance of the fiber. Also, results showed that SPME is a fast, simple, quick, and sensitive technique for sampling and sample introduction of Eucalyptus VOCs.

  6. SPME as a tool in WEA - CONCAWE Contribution to OSPAR Demonstration Project 2005 - 2006

    NARCIS (Netherlands)

    Leslie, H.A.

    2006-01-01

    This document represents a compilation of various data and deliverables from the study programme. An executive summary is followed by the presentation of data generated in an interlaboratory study of effluents assessed using both EGOM-LLE and biomimetic SPME methods.

  7. Development of a GC-MS-SPME Method for the Determination of Amines in Meteorites

    Science.gov (United States)

    Hilts, R. W.; Skelhorne, A. W.; Simkus, D.; Herd, C. D. K.

    2016-08-01

    A GC-MS-SPME analytical method for the direct determination of amines in aqueous solution has been developed. The key step in the procedure is the conversion of the amines into their non-volatile ammonium salts by protonation with HCl.

  8. Determinação do coeficiente de atividade em diluição infinita de hidrocarbonetos em furfural a 298,15 K por SPME-GC/FID

    Directory of Open Access Journals (Sweden)

    Filipe Arantes Furtado

    2010-01-01

    Full Text Available In this work a new method (SPME-GC/FID was developed to analyze the activity of binary liquid mixtures. The purpose is to demonstrate that SPME is capable to be used to determinate activity coefficients at infinite dilution knowing the fiber properties, with a lower cost than the conventional methods encountered in literature such as GLC. The activity coefficients at infinite dilution in furfural for n-hexane, n-heptane and cyclohexane at 298.15 K was determined using SPME and deviations of literature data was about 7%.

  9. Determination of Sesquiterpenes in Wines by HS-SPME Coupled with GC-MS

    OpenAIRE

    Cincotta, Fabrizio; Verzera, Antonella; Tripodi, Gianluca; Condurso, Concetta

    2015-01-01

    The sesquiterpene compounds present in red wines were characterized and quantified by Headspace Solid-Phase Microextraction in combination with Gas Chromatography–Mass Spectrometry (HS-SPME-GC-MS). Sixteen sesquiterpenes were identified, mainly hydrocarbons but also derived oxygenated compounds. Sesquiterpenes were acyclic, monocyclic, byciclic and tryciclic. Sesquiterpenes were detected in SIM (selected ion monitoring) mode using their characteristics ions. All the sesquiterpenes were identi...

  10. Passive Sampling and Analysis of Naphthalene in Internal Combustion Engine Exhaust with Retracted SPME Device and GC-MS

    Directory of Open Access Journals (Sweden)

    Nassiba Baimatova

    2017-07-01

    Full Text Available Exhaust gases from internal combustion engines are the main source of urban air pollution. Quantification of Polycyclic aromatic hydrocarbons (PAHs in the exhaust gases is needed for emissions monitoring, enforcement, development, and testing of control technologies. The objective was to develop quantification of gaseous naphthalene in diesel engine exhaust based on diffusion-controlled extraction onto a retracted solid-phase microextraction (SPME fiber coating and analysis on gas chromatography-mass spectrometry (GC-MS. Extraction of naphthalene with retracted fibers followed Fick’s law of diffusion. Extracted mass of naphthalene was proportional to Cg, t, Dg, T and inversely proportional to Z. Method detection limit (p = 0.95 was 11.5 ppb (0.06 mg·m−3 at t = 9 h, Z = 10 mm and T = 40 °C, respectively. It was found that the % mass extracted of naphthalene by SPME needle assembly depended on the type of fiber. Storage time at different temperatures did not affect analyte losses extracted by polydimethylsiloxane (PDMS 100 µm fiber. The developed method was tested on exhaust gases from idling pickup truck and tractor, and compared side-by-side with a direct injection of sampled exhaust gas method. Time-weighted average (TWA concentrations of naphthalene in exhaust gases from idling pickup truck and a tractor ranged from 0.08 to 0.3 mg·m−3 (15.3–53.7 ppb.

  11. SPME as a promising tool in translational medicine and drug discovery: From bench to bedside.

    Science.gov (United States)

    Goryński, Krzysztof; Goryńska, Paulina; Górska, Agnieszka; Harężlak, Tomasz; Jaroch, Alina; Jaroch, Karol; Lendor, Sofia; Skobowiat, Cezary; Bojko, Barbara

    2016-10-25

    Solid phase microextraction (SPME) is a technology where a small amount of an extracting phase dispersed on a solid support is exposed to the sample for a well-defined period of time. The open-bed geometry and biocompatibility of the materials used for manufacturing of the devices makes it very convenient tool for direct extraction from complex biological matrices. The flexibility of the formats permits tailoring the method according the needs of the particular application. Number of studies concerning monitoring of drugs and their metabolites, analysis of metabolome of volatile as well as non-volatile compounds, determination of ligand-protein binding, permeability and compound toxicity was already reported. All these applications were performed in different matrices including biological fluids and tissues, cell cultures, and in living animals. The low invasiveness of in vivo SPME, ability of using very small sample volumes and analysis of cell cultures permits to address the rule of 3R, which is currently acknowledged ethical standard in R&D labs. In the current review systematic evaluation of the applicability of SPME to studies required to be conduct at different stages of drug discovery and development and translational medicine is presented. The advantages and challenges are discussed based on the examples directly showing given experimental design or on the studies, which could be translated to the models routinely used in drug development process. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. Improving Student Understanding of Qualitative and Quantitative Analysis via GC/MS Using a Rapid SPME-Based Method for Determination of Trihalomethanes in Drinking Water

    Science.gov (United States)

    Huang, Shu Rong; Palmer, Peter T.

    2017-01-01

    This paper describes a method for determination of trihalomethanes (THMs) in drinking water via solid-phase microextraction (SPME) GC/MS as a means to develop and improve student understanding of the use of GC/MS for qualitative and quantitative analysis. In the classroom, students are introduced to SPME, GC/MS instrumentation, and the use of MS…

  13. Development of a Direct Headspace Collection Method from Arabidopsis Seedlings Using HS-SPME-GC-TOF-MS Analysis

    Directory of Open Access Journals (Sweden)

    Kazuki Saito

    2013-04-01

    Full Text Available Plants produce various volatile organic compounds (VOCs, which are thought to be a crucial factor in their interactions with harmful insects, plants and animals. Composition of VOCs may differ when plants are grown under different nutrient conditions, i.e., macronutrient-deficient conditions. However, in plants, relationships between macronutrient assimilation and VOC composition remain unclear. In order to identify the kinds of VOCs that can be emitted when plants are grown under various environmental conditions, we established a conventional method for VOC profiling in Arabidopsis thaliana (Arabidopsis involving headspace-solid-phase microextraction-gas chromatography-time-of-flight-mass spectrometry (HS-SPME-GC-TOF-MS. We grew Arabidopsis seedlings in an HS vial to directly perform HS analysis. To maximize the analytical performance of VOCs, we optimized the extraction method and the analytical conditions of HP-SPME-GC-TOF-MS. Using the optimized method, we conducted VOC profiling of Arabidopsis seedlings, which were grown under two different nutrition conditions, nutrition-rich and nutrition-deficient conditions. The VOC profiles clearly showed a distinct pattern with respect to each condition. This study suggests that HS-SPME-GC-TOF-MS analysis has immense potential to detect changes in the levels of VOCs in not only Arabidopsis, but other plants grown under various environmental conditions.

  14. Comparison of SPME Methods for Determining Volatile Compounds in Milk, Cheese, and Whey Powder

    Directory of Open Access Journals (Sweden)

    Michael H. Tunick

    2013-11-01

    Full Text Available Solid phase microextraction and gas chromatography-mass spectrometry (SPME-GC-MS are commonly used for qualitative and quantitative analysis of volatile compounds in various dairy products, but conditions have to be adjusted to maximize release while not generating new compounds that are absent in the original sample. Queso Fresco, a fresh non-melting cheese, may be heated at 60 °C for 30 min; in contrast, compounds are produced in milk when exposed to light and elevated temperatures, so milk samples are heated as little as possible. Products such as dehydrated whey protein are more stable and can be exposed to longer periods (60 min of warming at lower temperature (40 °C without decomposition, allowing for capture and analysis of many minor components. The techniques for determining the volatiles in dairy products by SPME and GC-MS have to be optimized to produce reliable results with minimal modifications and analysis times.

  15. Monitoring of persistent organic pollutants in seawater of the Pearl River Estuary with rapid on-site active SPME sampling technique

    International Nuclear Information System (INIS)

    Huang, Siming; He, Shuming; Xu, Hao; Wu, Peiyan; Jiang, Ruifen; Zhu, Fang; Luan, Tiangang; Ouyang, Gangfeng

    2015-01-01

    An on-site active solid-phase microextraction (SPME) sampling technique coupled with gas chromatography-mass spectrometry (GC–MS) for sampling and monitoring 16 polycyclic aromatic hydrocarbons (PAHs) and 8 organochlorine pesticides (OCPs) in seawater was developed. Laboratory experiments demonstrated that the sampling-rate calibration method was practical and could be used for the quantification of on-site sampling. The proposed method was employed for field tests which covered large amounts of water samples in the Pearl River Estuary in rainy and dry seasons. The on-site SPME sampling method can avoid the contamination of sample, the losses of analytes during sample transportation, as well as the usage of solvent and time-consuming sample preparation process. Results indicated that the technique with the designed device can address the requirement of modern environment water analysis. In addition, the sources, bioaccumulation and potential risk to human of the PAHs and OCPs in seawater of the Pearl River Estuary were discussed. - Highlights: • SPME on-site active sampling technique was developed and validated. • The technique was employed for field tests in the Pearl River Estuary. • 16 PAHs and 8 OCPs in the seawater of Pearl River Estuary were monitored. • The potential risk of the PAHs and OCPs in Pearl River Estuary were discussed. - An on-site active SPME sampling technique was developed and successfully applied for sampling and monitoring 16 PAHs and 8 OCPs in the Pearl River Estuary

  16. 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.)

  17. Determination of infinite dilution activity coefficients using HS-SPME/GC/FID for hydrocarbons in furfural at temperatures of (298.15, 308.15, and 318.15) K

    International Nuclear Information System (INIS)

    Arantes Furtado, Filipe; Vieira Coelho, Gerson Luiz

    2012-01-01

    Highlights: ► Two approaches were proposed using SPME on determination of infinite dilution activity coefficients. ► Infinite dilution activity coefficients of nine solutes in solvent furfural at T = (298.15, 308.15, and 318.15) K. ► Fiber–gas partition coefficients of nine solutes on PDMS at T = (298.15, 308.15, and 318.15) K. ► Optical microscopy analysis and statistical tests to measure possible damages on fiber coating. ► Advantages and limitations of methodology proposed were discussed. - Abstract: A new methodology using the headspace solid phase microextraction (HS-SPME) technique has been used to evaluate the infinite dilution activity coefficient (γ 12 ∞ ) of nine hydrocarbons (alkanes, cycloalkanes, and aromatics) in furfural solvent. The main objective of this study was to validate a faster and lower cost methodology expanding the use of HS-SPME to determine infinite dilution activity of solutes in organic solvents. Two approaches were proposed for the determination of γ 12 ∞ in order to use this technique (HS-SPME). In addition, the fiber–gas partition coefficients (K fg ) for each analyte at each of the studied temperatures were determined. The activity and partition coefficients have been reported at temperatures of (298.15, 308.15, and 318.15) K. The data were compared with the literature infinite dilution data determined by other methods such as liquid–gas chromatography (GLC) and gas stripping. Partial molar excess enthalpies of mixing at infinite dilution for each solute have been determined. The fibers were tested before and after each experiment, using statistical methods to ensure that their properties do not change during the experiments. The fibers were also analyzed by optical microscopy to evaluate possible surface damage by comparing them with new fibers. The activity coefficient values correlated well with the data in the literature and showed average deviations less than 10%.

  18. EVALUACIÓN DE DES, FSC Y SPME/CG-MS PARA LA EXTRACCIÓN Y DETERMINACIÓN DE COMPUESTOS RESPONSABLES DEL AROMA DE CAFÉ TOSTADO DE VILCABAMBA - ECUADOR

    Directory of Open Access Journals (Sweden)

    Jorge G. Figueroa

    2016-07-01

    Full Text Available The aim of this study was to compare the usefulness of three extraction methods: solid-phase microextraction (SPME with four different coating (PDMS, PDMS/DVB, DVB/CAR/PDMS and PA, supercritical fluid extraction with carbon dioxide (SCF and simultaneous distillation and extraction (SDE for isolation of flavor compounds from roasted ground coffee (Coffea arabica L. var. Typica of Vilcabamba (Ecuador. Identification and characterization of volatile compounds were achieved using gas chromatography / mass spectrometry (GC-MS. Analysis of variance and principal components analysis was done. For the SPME method the coating material affect the amount and concentration of compounds extracted, the DVB/CAR/PDMS coating provided the most representative aroma extract (44 compounds were identified. The SCF method allowed extracting a higher amount of compounds and also their identification by GC-MS (72 that SDE (64 and SPME (57, in addition provide higher extractions. The acetic acid, caffeine, furfuryl alcohol, furfural, 5-methylfurfural, butylated hydroxytoluene and maltol were the compounds with higher concentrations found with SPME and SDE, with SCF were found higher concentration to compounds with high molecular weights (> 194 g mol-1. Preferably SPME-DVB/CAR/PDMS method should be used for a characterization of coffee aroma compounds.

  19. Elucidating the sorption mechanism of “mixed-mode” SPME using the basic drug amphetamine as a model compound

    International Nuclear Information System (INIS)

    Peltenburg, Hester; Groothuis, Floris A.; Droge, Steven T.J.; Bosman, Ingrid J.; Hermens, Joop L.M.

    2013-01-01

    Graphical abstract: -- Highlights: •C18/propylsulfonic acid “mixed-mode” SPME fiber is efficient in sampling amphetamine. •Both protonated and neutral species of amphetamine sorb to the mixed-mode fiber. •Sorption of organic cations to this mixed-mode fiber depends on pH and salinity. •Amphetamine has a 20× higher affinity to the mixed-mode coating than to polyacrylate. -- Abstract: We studied the sorption of amphetamine as a model drug to represent small, polar organic cations to a new SPME coating combining C18 and propylsulfonic acid. This combination of hydrophobic and strong cation exchange (SCX) groups was compared to conventional SPME fibers with polyacrylate (PA) or C18 coating. The affinity of amphetamine at physiological pH (PBS) was 20 to 180 times greater for the new C18/SCX coating than for C18 alone and PA of different coating thickness. As amphetamine is a base and >99% protonated at physiological pH, this enhanced affinity is attributed to the ion-exchange phase in the coating. Tests at pH above the pK a of amphetamine show that, when normalized to the coating volume, neutral amphetamine also has a higher affinity compared to PA. As ion-exchange groups are not unlimitedly present in the coating, amphetamine isotherms level off to a saturation concentration on the C18/SCX fiber at the highest tested aqueous concentrations. Also, other cations (Na + , K + , Ca 2+ ) compete for the SCX sites and decrease the sorption coefficients, e.g. by 1.7 log units when comparing Milli-Q water with PBS. The C18/SCX fiber provides improved sensitivity over some of the classic SPME fibers. However, care should be taken near the cation exchange capacity of the fiber and the fiber should be calibrated in an appropriate matrix so as to eliminate competition effects

  20. 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.

  1. Critical micelle concentration values for different surfactants measured with solid-phase microextraction fibers

    NARCIS (Netherlands)

    Haftka, Joris J H; Scherpenisse, Peter; Oetter, G??nter; Hodges, Geoff; Eadsforth, Charles V.; Kotthoff, Matthias; Hermens, Joop L M

    The amphiphilic nature of surfactants drives the formation of micelles at the critical micelle concentration (CMC). Solid-phase microextraction (SPME) fibres were used in the present study to measure CMC values of twelve nonionic, anionic, cationic and zwitterionic surfactants. The SPME derived CMC

  2. HP-SPME of volatile polycyclic aromatic hydrocarbons from water using multiwalled carbon nanotubes coated on a steel fiber through electrophoretic deposition

    Energy Technology Data Exchange (ETDEWEB)

    Maghsoudi, S.; Noroozian, E. [Shahid Bahonar Univ., Kerman (Iran, Islamic Republic of). Dept. of Chemistry

    2012-08-15

    A headspace solid-phase microextraction (SPME) method using a stainless steel wire electrophoretically coated with dodecylsulfate modified multiwalled carbon nanotubes was used for the gas chromatographic (GC) determination of polycyclic aromatic hydrocarbons (PAHs) in aqueous samples. Electrophoretic deposition was easily carried out from an aqueous sodium dodecylsulfate medium. The effects of various parameters on the efficiency of SPME process, such as extraction time, extraction temperature, ionic strength, desorption time, and desorption temperature were studied. Under optimized conditions, the detection limits for the various PAHs studied varied from 0.03 to 0.07 ng mL{sup -1}. The inter-day and intra-day relative standard deviations at a 10 ng mL{sup -1} concentration level (n = 7) using a single-fiber were from 5.5 to 9.7 and 4.1 to 8.5 %, respectively. The fiber-to-fiber RSD% (n = 3) was between 7.3 and 11.1 %. The linear ranges were between 0.1 and 100 ng mL{sup -1}. The method was successfully applied to the analysis of a real sample with the recoveries from 88 to 105 % for 5 ng mL{sup -1} and 89 to 101 % for 0.5 ng mL{sup -1} samples. (orig.)

  3. HS-SPME AS AN EFFICIENT TOOL FOR DISCRIMINATING CHEMOTYPES OF Lippia alba (Mill. N. E. Brown

    Directory of Open Access Journals (Sweden)

    Aiêrta C. C. da Silva

    Full Text Available Lippia alba (Mill. N. E. Brown (Verbenaceae is a medicinal plant for which several biological activities are reported, such as sedative, anxiolytic, anti-ulcer, antifungal, antimicrobial, antioxidant, antispasmodic, anti-nociceptive and anti-inflammatory. It is characterized by the production of essential oils which have been used to classify the plant in different chemotypes. In the Northeast region of Brazil, the presence of three chemotypes are reported: myrcene-citral (chemotype I, limonene-citral (chemotype II and carvone-limonene (chemotype III. In this work, headspace-solid phase microextraction (HS-SPME was used on the analysis of the volatile organic compounds (VOCs of three chemotypes of L. alba from the Northeast region of Brazil, and compared to the essential oils of the plants extracted by hydrodistillation. Volatile compounds from each chemotype were more effectively differentiated when extracted by HS-SPME than by hydrodistillation.

  4. Optimization of total vaporization solid-phase microextraction (TV-SPME) for the determination of lipid profiles of Phormia regina, a forensically important blow fly species.

    Science.gov (United States)

    Kranz, William; Carroll, Clinton; Dixon, Darren; Picard, Christine; Goodpaster, John

    2017-11-01

    A new method has been developed for the determination of fatty acids, sterols, and other lipids which naturally occur within pupae of the blow fly Phormia regina. The method relies upon liquid extraction in non-polar solvent, followed by derivatization using N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) w/ 1% trimethylchlorsilane (TMCS) carried out inside the sample vial. The analysis is facilitated by total vaporization solid-phase microextraction (TV-SPME), with gas chromatography-mass spectrometry (GC-MS) serving as the instrumentation for analysis. The TV-SPME delivery technique is approximately a factor of five more sensitive than traditional liquid injection, which may alleviate the need for rotary evaporation, reconstitution, collection of high performance liquid chromatography fractions, and many of the other pre-concentration steps that are commonplace in the current literature. Furthermore, the ability to derivatize the liquid extract in a single easy step while increasing sensitivity represents an improvement over current derivatization methods. The most common lipids identified in fly pupae were various saturated and unsaturated fatty acids ranging from lauric acid (12:0) to arachinoic acid (20:4), as well as cholesterol. The concentrations of myristic acid (14:0), palmitelaidic acid (16:2), and palmitoleic acid (16:1) were the most reliable indicators of the age of the pupae. Graphical abstract Blow fly pupae were extracted prior to emerging as adults. The extracts were analyzed via total vaporization solid-phase microextraction (TV-SPME), revealing a complex mixture of lipids that could be associated with the age of the insect. This information may assist in determining a post-mortum interval (PMI) in a death investigation.

  5. Dynamic speciation analysis of atrazine in aqueous latex nanoparticle dispersions using solid phase microextraction (SPME)

    NARCIS (Netherlands)

    Benhabib, K.; Town, R.M.; Leeuwen, van H.P.

    2009-01-01

    Solid phase microextraction (SPME) is applied in the dynamic speciation analysis of the pesticide atrazine in an aqueous medium containing sorbing latex nanoparticles. It is found that the overall rate of extraction of the analyte is faster than in the absence of nanoparticles and governed by the

  6. Potential semiochemicals in urine from free ranging wolverines (Gulo gulo Pallas, 1780)

    Science.gov (United States)

    William F. Wood; Jeffrey P. Copeland; Richard E. Yates; Iman K. Horsey; Lynne R. McGreevy

    2009-01-01

    Urine deposition has been observed as an important scent-marking behaviour among wolverines (Gulo gulo, Mustelinae, Mustelidae). Solid phase microextraction (SPME) of headspace volatiles of the urine from free ranging wolverines were examined by gas chromatography-mass spectrometry (GC-MS). Urine samples were collected directly from the bladder of live-trapped animals...

  7. Multiple internal standard normalization for improving HS-SPME-GC-MS quantitation in virgin olive oil volatile organic compounds (VOO-VOCs) profile.

    Science.gov (United States)

    Fortini, Martina; Migliorini, Marzia; Cherubini, Chiara; Cecchi, Lorenzo; Calamai, Luca

    2017-04-01

    The commercial value of virgin olive oils (VOOs) strongly depends on their classification, also based on the aroma of the oils, usually evaluated by a panel test. Nowadays, a reliable analytical method is still needed to evaluate the volatile organic compounds (VOCs) and support the standard panel test method. To date, the use of HS-SPME sampling coupled to GC-MS is generally accepted for the analysis of VOCs in VOOs. However, VOO is a challenging matrix due to the simultaneous presence of: i) compounds at ppm and ppb concentrations; ii) molecules belonging to different chemical classes and iii) analytes with a wide range of molecular mass. Therefore, HS-SPME-GC-MS quantitation based upon the use of external standard method or of only a single internal standard (ISTD) for data normalization in an internal standard method, may be troublesome. In this work a multiple internal standard normalization is proposed to overcome these problems and improving quantitation of VOO-VOCs. As many as 11 ISTDs were used for quantitation of 71 VOCs. For each of them the most suitable ISTD was selected and a good linearity in a wide range of calibration was obtained. Except for E-2-hexenal, without ISTD or with an unsuitable ISTD, the linear range of calibration was narrower with respect to that obtained by a suitable ISTD, confirming the usefulness of multiple internal standard normalization for the correct quantitation of VOCs profile in VOOs. The method was validated for 71 VOCs, and then applied to a series of lampante virgin olive oils and extra virgin olive oils. In light of our results, we propose the application of this analytical approach for routine quantitative analyses and to support sensorial analysis for the evaluation of positive and negative VOOs attributes. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. Application of robust NiTi-ZrO2-PEG SPME fiber in the determination of haloanisoles in cork stopper samples

    International Nuclear Information System (INIS)

    Budziak, Dilma; Martendal, Edmar; Carasek, Eduardo

    2008-01-01

    In this study, a novel solid-phase microextraction (SPME) fiber obtained using sol-gel technology was applied in the determination of off-flavor compounds (2,4,6-trichloroanisole (TCA), 2,4,6-tribromoanisole (TBA) and pentachloroanisole (PCA)) present in cork stopper samples. A NiTi alloy previously electrodeposited with zirconium oxide was used as the substrate for a poly(ethylene glycol) (PEG) coating. Scanning electronic microscopy showed good uniformity of the coating and allowed the coating thickness to be estimated as around 17 μm. The optimization of the main parameters influencing the extraction efficiency, such as cork sample mass, sodium chloride mass, extraction temperature and extraction time were optimized using a full factorial design, followed by a Doehlert design. The optimum conditions were: 20 min of extraction at 70 deg. C using 60 mg of the cork sample and 10 mL of water saturated with sodium chloride in a 20 mL amber vial with constant magnetic stirring. Satisfactory detection limits between 2.5 and 5.1 ng g -1 were obtained, as well as good precision (R.S.D. in the range of 5.8-12.0%). Recovery tests were performed on three different cork samples, and values between 83 and 119% were obtained. The proposed SPME fiber was compared with commercially available fibers and good results were achieved, demonstrating its applicability

  9. Screening of transformation products in soils contaminated with unsymmetrical dimethylhydrazine using headspace SPME and GC-MS

    NARCIS (Netherlands)

    Kenessov, B.N.; Koziel, J.A.; Grotenhuis, J.T.C.; Carlsen, L.

    2010-01-01

    The paper describes a novel SPME-based approach for sampling and analysis of transformation products of highly reactive and toxic unsymmetrical dimethylhydrazine (UDMH) which is used as a fuel in many Russian, European, Indian, and Chinese heavy cargo carrier rockets. The effects of several

  10. 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.

  11. Determinação de herbicidas usados no cultivo de arroz irrigado na região sul do estado de Santa Catarina através da SPME-GC-ECD Determination of herbicides used in irrigated rice cultivation in the south of Santa Catarina using SPME-GC-ECD

    Directory of Open Access Journals (Sweden)

    Léa L. F. Costa

    2008-01-01

    Full Text Available Evaluation of the pollution by the herbicides alachlor, propanil and atrazine in water samples from four rivers in the cities of Turvo and Meleiro, south of Santa Catarina State, was made using the SPME-GC-ECD method. The proposed method was optimized and validated. The correlation coefficients were higher than 0.997 and linear ranges of the analytical curves were 0.1-4; 0.1-2.5 and 0.1-5 µg L-1 for atrazine, alachlor and propanil, respectively. The herbicides were quantified by GC-ECD and identified by GC-MS. Both of the selected rivers presented contamination by at least one of the studied herbicides.

  12. Optimization of Biochemical Screening Methods for Volatile and Unstable Sesquiterpenoids Using HS-SPME-GC-MS

    Directory of Open Access Journals (Sweden)

    Trine Bundgaard Andersen

    2015-06-01

    Full Text Available HS-SPME-GC-MS has been suggested as a fast and robust analytical platform for the product characterization of sesquiterpene synthases. The choice of fiber and injection temperature can have a significant effect on the observed product profile, due to the chemical rearrangements that can occur on the fiber material. Here we present a systematic study on the effects of fiber choice and injection port temperature on the observed sesquiterpenoid profile of four sesquiterpene synthases expressed in Nicotiana benthamiana. We found that the absorbent material PDMS was much less likely to support acid-induced rearrangement of sesquiterpenoids when compared to the adsorbent materials PDMS/DVB, PDMS/CAR, and PDMS/CAR/DVB. Furthermore, utilizing an injection port temperature at 160 °C almost eliminated the inherent thermal instability of germacrene sesquiterpenoids. Thus, for fast screening of sesquiterpene synthases, the results suggest that PDMS fibers and an injection temperature of 160 °C provide a fast and reproducible HS-SPME GC-MS method when using H2 as carrier gas.

  13. A quantum inspired model of radar range and range-rate measurements with applications to weak value measurements

    Science.gov (United States)

    Escalante, George

    2017-05-01

    Weak Value Measurements (WVMs) with pre- and post-selected quantum mechanical ensembles were proposed by Aharonov, Albert, and Vaidman in 1988 and have found numerous applications in both theoretical and applied physics. In the field of precision metrology, WVM techniques have been demonstrated and proven valuable as a means to shift, amplify, and detect signals and to make precise measurements of small effects in both quantum and classical systems, including: particle spin, the Spin-Hall effect of light, optical beam deflections, frequency shifts, field gradients, and many others. In principal, WVM amplification techniques are also possible in radar and could be a valuable tool for precision measurements. However, relatively limited research has been done in this area. This article presents a quantum-inspired model of radar range and range-rate measurements of arbitrary strength, including standard and pre- and post-selected measurements. The model is used to extend WVM amplification theory to radar, with the receive filter performing the post-selection role. It is shown that the description of range and range-rate measurements based on the quantum-mechanical measurement model and formalism produces the same results as the conventional approach used in radar based on signal processing and filtering of the reflected signal at the radar receiver. Numerical simulation results using simple point scatterrer configurations are presented, applying the quantum-inspired model of radar range and range-rate measurements that occur in the weak measurement regime. Potential applications and benefits of the quantum inspired approach to radar measurements are presented, including improved range and Doppler measurement resolution.

  14. Volatile emerging contaminants in melon fruits, analysed by HS-SPME-GC-MS.

    Science.gov (United States)

    Cincotta, Fabrizio; Verzera, Antonella; Tripodi, Gianluca; Condurso, Concetta

    2018-03-01

    The aim of this research was to develop and validate a headspace-solid phase micro-extraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS) method for the determination of volatile emerging contaminants in fruit. The method showed good precision (RSD ≤ 14%) and satisfactory recoveries (99.1-101.7%) and LOD and LOQ values ranging between 0.011-0.033 μg kg -1 and 0.037-0.098 μg kg -1 , respectively. The method was applied to investigate the content of volatile emerging contaminants in two varieties of melon fruit (Cucumis melo L.) cultivated adjoining high-risk areas. Glycol ethers, BHT, BHA and BTEX (benzene, toluene, ethylbenzene and xylene) were determined in melon fruit pulps for the first time, with different sensitivities depending on sample and variety. Although the amount of the volatile contaminants in the melon samples were in the order of µg kg -1 , the safety of vegetable crops cultivated near risk areas should be more widely considered. The results showed that this accurate and reproducible method can be useful for routine safety control of fruits and vegetables.

  15. Ultrafast Screening and Quantitation of Pesticides in Food and Environmental Matrices by Solid-Phase Microextraction-Transmission Mode (SPME-TM) and Direct Analysis in Real Time (DART).

    Science.gov (United States)

    Gómez-Ríos, Germán Augusto; Gionfriddo, Emanuela; Poole, Justen; Pawliszyn, Janusz

    2017-07-05

    The direct interface of microextraction technologies to mass spectrometry (MS) has unquestionably revolutionized the speed and efficacy at which complex matrices are analyzed. Solid Phase Micro Extraction-Transmission Mode (SPME-TM) is a technology conceived as an effective synergy between sample preparation and ambient ionization. Succinctly, the device consists of a mesh coated with polymeric particles that extracts analytes of interest present in a given sample matrix. This coated mesh acts as a transmission-mode substrate for Direct Analysis in Real Time (DART), allowing for rapid and efficient thermal desorption/ionization of analytes previously concentrated on the coating, and dramatically lowering the limits of detection attained by sole DART analysis. In this study, we present SPME-TM as a novel tool for the ultrafast enrichment of pesticides present in food and environmental matrices and their quantitative determination by MS via DART ionization. Limits of quantitation in the subnanogram per milliliter range can be attained, while total analysis time does not exceed 2 min per sample. In addition to target information obtained via tandem MS, retrospective studies of the same sample via high-resolution mass spectrometry (HRMS) were accomplished by thermally desorbing a different segment of the microextraction device.

  16. Analysis of organic micropollutants in drinking water using SPME and GC-MS

    International Nuclear Information System (INIS)

    Guidotti, M.; Ravaioli, G.

    1999-01-01

    In this work the purpose was to develop accurate and reproducible methods for the qualitative and quantitative analysis of pesticides/herbicides, phthalates, chlorinated solvents, trihalomethanes, polycyclic aromatic hydrocarbons (PAHs) and chlorophenols in drinking waters, using solid-phase micro extraction and GC-MS techniques. The SPME developed by J. Pawliszyn and co-workers, consists of an fused silica fibre, coated with an appropriate absorbent phase, hosted inside the needle of a holder that looks like a GC-syringe; the needle pierces the septum of a sealed vial and the fibre is lowered, by depressing the plunger of the holder, into the liquid (or in the headspace, if that is the case) that contains the analytes of interest. After a set period of time, necessary to reach the partitioning equilibrium, the fibre is retracted inside the needle, the needle is inserted into the GC injector port and the fibre pushed in the heated injector. Here the compounds of interest (that have adsorbed onto the fibre) are thermally desorbed and analysed by GC-MS. After three minutes the fibre is extracted and is ready for a new analysis. The SPME technique has already found many applications in food and environmental analysis. Many of the analytes investigated in this research are listed Italian legislation as possible pollutants of drinking waters and their presence and concentrations require monitoring. The list of compounds included in this work is reported in Table 1

  17. Solid-phase microextraction (SPME) as a tool to predict the bioavailability and toxicity of pyrene to the springtail, Folsomia candida, under various soil conditions

    DEFF Research Database (Denmark)

    Styrishave, Bjarne; Mortensen, Mads; Krogh, Paul Henning

    2008-01-01

    The porewater concentrations of pyrene were estimated by a negligible depletive solid-phase microextraction (SPME) method. The effects of organic matter (OM) and soil aging on the bioavailability of pyrene in soil were investigated by generation of reproductive effect concentrations (EC50...... increased with increasing OM and aging of the soil. The increase of the OM content in the soil reduced the extractability of pyrene by SPME, as well as the toxicity of pyrene. An aging effect was demonstrated in Askov soil, EC50 values increased with increased contact time. The amounts of pyrene extracted...

  18. Stable isotope dilution assay (SIDA) and HS-SPME-GCMS quantification of key aroma volatiles for fruit and sap of Australian mango cultivars.

    Science.gov (United States)

    San, Anh T; Joyce, Daryl C; Hofman, Peter J; Macnish, Andrew J; Webb, Richard I; Matovic, Nicolas J; Williams, Craig M; De Voss, James J; Wong, Siew H; Smyth, Heather E

    2017-04-15

    Reported herein is a high throughput method to quantify in a single analysis the key volatiles that contribute to the aroma of commercially significant mango cultivars grown in Australia. The method constitutes stable isotope dilution analysis (SIDA) in conjunction with headspace (HS) solid-phase microextraction (SPME) coupled with gas-chromatography mass spectrometry (GCMS). Deuterium labelled analogues of the target analytes were either purchased commercially or synthesised for use as internal standards. Seven volatiles, hexanal, 3-carene, α-terpinene, p-cymene, limonene, α-terpinolene and ethyl octanoate, were targeted. The resulting calibration functions had determination coefficients (R 2 ) ranging from 0.93775 to 0.99741. High recovery efficiencies for spiked mango samples were also achieved. The method was applied to identify the key aroma volatile compounds produced by 'Kensington Pride' and 'B74' mango fruit and by 'Honey Gold' mango sap. This method represents a marked improvement over current methods for detecting and measuring concentrations of mango fruit and sap volatiles. Copyright © 2016 Elsevier Ltd. All rights reserved.

  19. Characterization of Fish Sauce Aroma Impact Compounds Using GC-MS, SPME-Osme-GCO, and Stevens' Power Law Exponents

    Science.gov (United States)

    The objectives of this study were to characterize volatile compounds and to determine the characteristic aromas associated with impact compounds in 4 fish sauces using solid-phase micro-extraction, gas chromatography-mass spectrometry, Osme, and gas chromatography olfactometry (SPME-Osme-GCO) couple...

  20. Modified HS-SPME for determination of quantitative relations between low-molecular oxygen compounds in various matrices.

    Science.gov (United States)

    Dawidowicz, Andrzej L; Szewczyk, Joanna; Dybowski, Michal P

    2016-09-07

    Similar quantitative relations between individual constituents of the liquid sample established by its direct injection can be obtained applying Polydimethylsiloxane (PDMS) fiber in the headspace solid phase microextraction (HS-SPME) system containing the examined sample suspended in methyl silica oil. This paper proves that the analogous system composed of sample suspension/emulsion in polyethylene glycol (PEG) and Carbowax fiber allows to get similar quantitative relations between components of the mixture as those established by its direct analysis, but only for polar constituents. It is demonstrated for essential oil (EO) components of savory, sage, mint and thyme, and of artificial liquid mixture of polar constituents. The observed differences in quantitative relations between polar constituents estimated by both applied procedures are insignificant (Fexp < Fcrit). The presented results indicates that wider applicability of the system composed of a sample suspended in the oil of the same physicochemical character as that of used SPME fiber coating strongly depends on the character of interactions between analytes-suspending liquid and analytes-fiber coating. Copyright © 2016 Elsevier B.V. All rights reserved.

  1. JV Task 92 - Alcoa/Retec SFE and SPME

    Energy Technology Data Exchange (ETDEWEB)

    Steven Hawthorne

    2009-02-15

    This report summarizes the work performed by the Energy & Environmental Research Center (EERC) under the U.S. Department of Energy Jointly Sponsored Research Program JV Task 92, which is a continuation of JV9. Successful studies performed in 1999 through the end of 2008 demonstrated the potential for using selective supercritical fluid extraction (SFE) and a solid-phase microextraction (SPME) method for measuring sediment pore water polycyclic aromatic hydrocarbons (PAHs) to mimic the bioavailability of PAHs from manufactured gas plant and aluminum smelter soils and sediments both in freshwater and saltwater locations. The studies that the EERC has performed with the commercial partners have continued to generate increased interest in both the regulatory communities and in the industries that have historically produced or utilized coal tar products. Both ASTM International and the U.S. Environmental Protection Agency (EPA) have accepted the pore water method developed at the EERC as standard methods. The studies have demonstrated the effectiveness of our techniques in predicting bioavailability of PAHs from ca. 250 impacted and background field sediments and soils. The field demonstrations from the final years of the project continued to build the foundation data for acceptance of our methods by the regulatory communities. The JV92 studies provide the single largest database in the world that includes measures of PAH bioavailability along with biological end points. These studies clearly demonstrated that present regulatory paradigms based on equilibrium partitioning greatly overpredict bioavailability. These investigations also laid the foundation for present (non-JV) studies being applied to PAHs and polychlorinated biphenyls (PCBs) at EPA Superfund sites, investigations into PAH and PCB bioavailability at U.S Department of Defense sites, and the application of the techniques to investigating the bioavailability of chlorinated dioxins and furans from impacted

  2. Analysis of High Quality Agar wood Oil Chemical Compounds By Means Of SPME/ GC-MS and Z-Score Technique

    International Nuclear Information System (INIS)

    Nurlaila Ismail; Mohd Ali Nor Azah; Mailina Jamil; Saiful Nizam Tajuddin; Mohd Nasir Taib

    2013-01-01

    Currently, the grading of the agar wood oil to the high and low quality is done using manually such as human trained grader. It was performed based on the agar wood oil physical properties such as human experience and perception and the oil colour, odor and long lasting aroma. Several researchers found that chemical profiles of the oil should be utilized to overcome the problem facing by manual techniques for example human nose cannot tolerate with the many oils at the same time, so that accurate result can be obtained in grading the agar wood oil. The analysis involved of SPME/ GC-MS and Z-score techniques have been proposed in this study to analyze the chemical compounds especially from the high quality samples of agar wood oil (Aquilariamalaccensis) from Malaysia. Two SPME fibers were used such as divinylbenzene-carbogen-polydimethylsiloxane (DVB-CAR-PDMS) and polydimethylsiloxane (PDMS) in extracting the oils compound under three different sampling temperature conditions such as 40, 60 and 80 degree Celsius. The chemical compounds extracted by SPME/ GC-MS were analyzed. The chemical compounds as identified by Z-score as significant compounds were discussed before the conclusion is made. It was found that 10-epi-γ-eudesmol, aromadendrene, β-agar ofuran, α-agar ofuran and γ-eudesmol were highlighted as significant for high quality agar wood oil and can be used as a marker compounds in classifying the agar wood oil. (author)

  3. VOLATILE COMPOUNDS OF LITHRAEA CAUSTICA (LITRE) DETERMINATED BY SOLID PHASE MICRO-EXTRACTION (SPME)

    OpenAIRE

    GARBARINO, JUAN A; SALVATORE, GIUSEPPE; PIVANOVO, MARISA; CHAMY, MARÍA CRISTINA; NICOLETTI, MARCELLO; DE IOANNES, ALFREDO

    2002-01-01

    The head space of the aerial parts of Lithraea caustica was analyzed by Solid Phase Micro-Extraction (SPME) technique, obtaining as main volatile compounds the monoterpenes, myrcene, a -pinene, , p-cymene and limonene, as well as the sesquiterpene caryophylene. De las partes áereas de Lithraea caustica y usando la técnica de Micro-Extracción en Fase Sólida (MEFS), fueron identificados y cuantificados los principales compuestos volátiles: los monoterpenos, mirceno, a -pineno, p-cimeno y lim...

  4. Changes in SPME-extracted volatile compounds from Iberian ham during ripening

    Directory of Open Access Journals (Sweden)

    García, Carmen

    2009-07-01

    Full Text Available A headspace SPME procedure was tested to study the evolution of volatile compounds during the ripening of Iberian hams from pigs reared in a Montanera system (outdoorbased, with acorn and pasture available and a HO-Pienso system (indoor-based, with a high oleic acid concentrate. The effect of the ripening time on volatile compounds was more marked than the effect of feeding system. Most volatile compounds affected by the ripening time were compounds that come from Strecker and Maillard reactions, which increased significantly ( p Un procedimiento de microextración en fase sólida (SPME en espacio de cabeza fue ensayado para estudiar la evolución de los compuestos volátiles durante la curación de Jamones Ibéricos de cerdos criados en régimen de montanera (en libertad, con bellotas y pasto disponible y un sistema OH-Pienso (estabulados, con un pienso alto en ácido oléico. El efecto del tiempo de curación en los compuestos volátiles fue más marcado que el efecto de la alimentación. La mayoría de los compuestos volátiles afectados por el tiempo de curación fueron compuestos que proceden de la reacción de Strecker y Maillard, que se incrementaron significativamente (p p < 0.05. Algunos de ellos (ácido butanoico, 2,6- dimetilpiracina y 1-octen-3-ol fueron más abundantes en jamones de Montanera que en jamones de Pienso. Estas pequeñas diferencias podrían ser importantes porque los compuestos involucrados han sido identificados como aromas del jamón Ibérico.

  5. 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.

  6. An Innovative Rapid Method for Analysis of 10 Organophosphorus Pesticide Residues in Wheat by HS-SPME-GC-FPD/MSD.

    Science.gov (United States)

    Du, Xin; Ren, YongLin; Beckett, Stephen J

    2016-01-01

    The rapid detection of pesticide residues in wheat has become a top food security priority. A solvent-free headspace solid-phase microextraction (HS-SPME) has been evaluated for rapid screening of organophosphorus pesticide (OPP) residues in wheat with high sensitivity. Individual wheat samples (1.7 g), spiked with 10 OPPs, were placed in a 4 mL sealed amber glass vial and heated at 60°C for 45 min. During this time, the OPP residues were extracted with a 50 μm/30 μm divinylbenzene (DVB)/carboxen (CAR)/plasma desorption mass spectroscopy polydimethylsiloxane (PDMS) fiber from the headspace above the sample. The fiber was then removed and injected into the GC injection port at 250°C for desorption of the extracted chemicals. The multiple residues were identified by a GC mass spectrometer detector (GC-MSD) and quantified with a GC flame photometric detector (GC-FPD). Seven spiked levels of 10 OPPs on wheat were analyzed. The GC responses for a 50 μm/30 μm DVB/CAR/PDMS fiber increased with increasing spiking levels, yielding significant (R(2) > 0.98) linear regressions. The lowest LODs of the multiple pesticide standards were evaluated under the conditions of the validation study in a range of levels from 0 (control) to 100 ng of pesticide residue per g of wheat that separated on a low-polar GC capillary column (Agilent DB-35UI). The results of the HS-SPME method were compared with the QuEChERS AOAC 2007.01 method and they showed several advantages over the latter. These included improved sensitivity, selectivity, and simplicity.

  7. Analysis of Organic Volatile Flavor Compounds in Fermented Stinky Tofu Using SPME with Different Fiber Coatings

    Directory of Open Access Journals (Sweden)

    Wei Guan

    2012-03-01

    Full Text Available The organic volatile flavor compounds in fermented stinky tofu (FST were studied using SPME-GC/MS. A total of 39 volatile compounds were identified, including nine esters, seven alcohols, five alkenes, four sulfides, three heterocycles, three carboxylic acids, three ketones, two aldehydes, one phenol, one amine and one ether. These compounds were determined by MS, and conformed by comparison of the retention times of the separated constituents with those of authentic samples and by comparison of retention indexes (RIs of separated constituents with the RIs reported in the literature. The predominant volatile compound in FST was indole, followed by dimethyl trisulfide, phenol, dimethyl disulfide and dimethyl tetrasulfide. In order to find a better extraction time, the extraction times was optimized for each type of SPME fiber; the results show that the best extraction time for Carboxen/PDMS is 60 min, for PDMS/DVB 30 min, for DVB/CAR/PDMS 60 min and for PDMS 75 min. Of the four fibers used in this work, Carboxen/PDMS is found to be the most suitable to extract the organic volatile flavor compounds in fermented stinky tofu.

  8. Application of HS-SPME and GC-MS to characterization of volatile compounds emitted from Osmanthus flowers.

    Science.gov (United States)

    Deng, Chunhui; Song, Guoxin; Hu, Yaoming

    2004-12-01

    Headspace solid-phase microextraction (HS-SPME) combined with gas chromatography-mass spectrometry (GC-MS) was developed for characterization of volatile compounds emitted from two varieties Osmanthus flowers of O. fragrans var. latifolius and O. fragrans var. thunbergii. The SPME parameters were studied, the optimum conditions of a 65 microm carbowax/divinylbenzene (CW/DVB), extraction temperature of 22 degrees C and extraction time of 10 min were obtained and applied to extraction of the volatile emissions. Fourteen compounds released from both varieties of Osmanthus flowers were separated and identified by GC-MS, which mainly included alpha-linalool, beta-linalool, trans-linalool oxide, cis-linalool oxide, alpha-lonone, beta-lonone, capraldehyde and decalactone. By comparing their peak areas, we found that the sums of the fourteen compounds from the two Osmanthus flowers were very close, while the relative contents of individual volatile compounds in the two emissions were very different. The relative content of alpha-linalool and beta-linalool in O. fragrans var. latifolius were 39.46% and 0.51%, while in O. fragrans var. thunbergii were 9.53% and 27.71%. Due to their different relative contents, the two varieties of flower have different fragrances.

  9. Applications of Solid-Phase Microextraction and Gas Chromatography/Mass Spectrometry (SPME-GC/MS in the Study of Grape and Wine Volatile Compounds

    Directory of Open Access Journals (Sweden)

    Annarita Panighel

    2014-12-01

    Full Text Available Volatile compounds are responsible for the wine “bouquet”, which is perceived by sniffing the headspace of a glass, and of the aroma component (palate-aroma of the overall flavor, which is perceived on drinking. Grape aroma compounds are transferred to the wine and undergo minimal alteration during fermentation (e.g., monoterpenes and methoxypyrazines; others are precursors of aroma compounds which form in winemaking and during wine aging (e.g., glycosidically-bound volatile compounds and C13-norisoprenoids. Headspace solid phase microextraction (HS-SPME is a fast and simple technique which was developed for analysis of volatile compounds. This review describes some SPME methods coupled with gas chromatography/mass spectrometry (GC/MS used to study the grape and wine volatiles.

  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. Headspace-SPME-GC/MS as a simple cleanup tool for sensitive 2,6-diisopropylphenol analysis from lipid emulsions and adaptable to other matrices.

    Science.gov (United States)

    Pickl, Karin E; Adamek, Viktor; Gorges, Roland; Sinner, Frank M

    2011-07-15

    Due to increased regulatory requirements, the interaction of active pharmaceutical ingredients with various surfaces and solutions during production and storage is gaining interest in the pharmaceutical research field, in particular with respect to development of new formulations, new packaging material and the evaluation of cleaning processes. Experimental adsorption/absorption studies as well as the study of cleaning processes require sophisticated analytical methods with high sensitivity for the drug of interest. In the case of 2,6-diisopropylphenol - a small lipophilic drug which is typically formulated as lipid emulsion for intravenous injection - a highly sensitive method in the concentration range of μg/l suitable to be applied to a variety of different sample matrices including lipid emulsions is needed. We hereby present a headspace-solid phase microextraction (HS-SPME) approach as a simple cleanup procedure for sensitive 2,6-diisopropylphenol quantification from diverse matrices choosing a lipid emulsion as the most challenging matrix with regard to complexity. By combining the simple and straight forward HS-SPME sample pretreatment with an optimized GC-MS quantification method a robust and sensitive method for 2,6-diisopropylphenol was developed. This method shows excellent sensitivity in the low μg/l concentration range (5-200μg/l), good accuracy (94.8-98.8%) and precision (intraday-precision 0.1-9.2%, inter-day precision 2.0-7.7%). The method can be easily adapted to other, less complex, matrices such as water or swab extracts. Hence, the presented method holds the potential to serve as a single and simple analytical procedure for 2,6-diisopropylphenol analysis in various types of samples such as required in, e.g. adsorption/absorption studies which typically deal with a variety of different surfaces (steel, plastic, glass, etc.) and solutions/matrices including lipid emulsions. Copyright © 2011 Elsevier B.V. All rights reserved.

  12. Development and validation of an SPME-GC method for a degradation kinetics study of propiconazole I, propiconazole II and tebuconazole in blueberries in Concordia, the main production area of Argentina.

    Science.gov (United States)

    Munitz, Martín S; Medina, María B; Montti, María I T

    2017-05-01

    An analytical method for the simultaneous determination of propiconazole isomers and tebuconazole residues in blueberries was developed using solid-phase microextraction (SPME) coupled to gas chromatography. Confirmation was performed by gas chromatography-mass spectrometry in selected-ion monitoring mode. The SPME fibre coating selected was CWX-DVB, and the pH was adjusted to 7 with NaOH. The method is selective with adequate precision and high accuracy and sensitivity. Recoveries ranged between 97.4% and 98.9% for all compounds; and detection and quantification limits were respectively 0.21 and 0.49 μg kg -1 for propiconazole I; 0.16 and 0.22 μg kg -1 for propiconazole II; and 0.16 and 0.48 μg kg -1 for tebuconazole. The degradation of these fungicides in blueberries followed first-order rate kinetics. The half-life times for flowering and fruit set applications were respectively 4.0 and 10.3 days for propiconazole I, 4.0 and 11.4 days for propiconazole II, and 3.5 and 12.4 days for tebuconazole.

  13. Development of a Microfluidic Open Interface with Flow Isolated Desorption Volume for the Direct Coupling of SPME Devices to Mass Spectrometry.

    Science.gov (United States)

    Tascon, Marcos; Alam, Md Nazmul; Gómez-Ríos, Germán Augusto; Pawliszyn, Janusz

    2018-02-20

    Technologies that efficiently integrate the sampling and sample preparation steps with direct introduction to mass spectrometry (MS), providing simple and sensitive analytical workflows as well as capabilities for automation, can generate a great impact in a vast variety of fields, such as in clinical, environmental, and food-science applications. In this study, a novel approach that facilitates direct coupling of Bio-SPME devices to MS using a microfluidic design is presented. This technology, named microfluidic open interface (MOI), which operates under the concept of flow-isolated desorption volume, consists of an open-to-ambient desorption chamber (V ≤ 7 μL) connected to an ionization source. Subsequently, compounds of interest are transported to the ionization source by means of the self-aspiration process intrinsic of these interfaces. Thus, any ionization technology that provides a reliable and constant suction, such as electrospray ionization (ESI), atmospheric-pressure chemical ionization (APCI), or inductively coupled plasma ionization (ICP), can be hyphenated to MOI. Using this setup, the desorption chamber is used to release target compounds from the coating, while the isolation of the flow enables the ionization source to be continuously fed with solvent, all without the necessity of employment of additional valves. As a proof of concept, the design was applied to an ESI-MS/MS system for experimental validation. Furthermore, numerical simulations were undertaken to provide a detailed understanding of the fluid flow pattern inside the interface, then used to optimize the system for better efficiency. The analytical workflow of the developed Bio-SPME-MOI-MS setup consists of the direct immersion of SPME fibers into the matrix to extract/enrich analytes of interest within a short period of time, followed by a rinsing step with water to remove potentially adhering proteins, salts, and/or other interfering compounds. Next, the fiber is inserted into the

  14. Quantification of Polyfunctional Thiols in Wine by HS-SPME-GC-MS Following Extractive Alkylation.

    Science.gov (United States)

    Musumeci, Lauren E; Ryona, Imelda; Pan, Bruce S; Loscos, Natalia; Feng, Hui; Cleary, Michael T; Sacks, Gavin L

    2015-07-06

    Analyses of key odorous polyfunctional volatile thiols in wines (3-mercaptohexanol (3-MH), 3-mercaptohexylacetate (3-MHA), and 4-mercapto-4-methyl-2-pentanone (4-MMP)) are challenging due to their high reactivity and ultra-trace concentrations, especially when using conventional gas-chromatography electron impact mass spectrometry (GC-EI-MS). We describe a method in which thiols are converted to pentafluorobenzyl (PFB) derivatives by extractive alkylation and the organic layer is evaporated prior to headspace solid phase microextraction (HS-SPME) and GC-EI-MS analysis. Optimal parameters were determined by response surface area modeling. The addition of NaCl solution to the dried SPME vials prior to extraction resulted in up to less than fivefold improvement in detection limits. Using 40 mL wine samples, limits of detection for 4-MMP, 3-MH, and 3-MHA were 0.9 ng/L, 1 ng/L, and 17 ng/L, respectively. Good recovery (90%-109%) and precision (5%-11% RSD) were achieved in wine matrices. The new method was used to survey polyfunctional thiol concentrations in 61 commercial California and New York State wines produced from V. vinifera (Riesling, Gewürztraminer, Cabernet Sauvignon, Sauvignon blanc and non-varietal rosé wines), V. labruscana (Niagara), and Vitis spp. (Cayuga White). Mean 4-MMP concentrations in New York Niagara (17 ng/L) were not significantly different from concentrations in Sauvignon blanc, but were significantly higher than 4-MMP in other varietal wines.

  15. Quantification of Polyfunctional Thiols in Wine by HS-SPME-GC-MS Following Extractive Alkylation

    Directory of Open Access Journals (Sweden)

    Lauren E. Musumeci

    2015-07-01

    Full Text Available Analyses of key odorous polyfunctional volatile thiols in wines (3-mercaptohexanol (3-MH, 3-mercaptohexylacetate (3-MHA, and 4-mercapto-4-methyl-2-pentanone (4-MMP are challenging due to their high reactivity and ultra-trace concentrations, especially when using conventional gas-chromatography electron impact mass spectrometry (GC-EI-MS. We describe a method in which thiols are converted to pentafluorobenzyl (PFB derivatives by extractive alkylation and the organic layer is evaporated prior to headspace solid phase microextraction (HS-SPME and GC-EI-MS analysis. Optimal parameters were determined by response surface area modeling. The addition of NaCl solution to the dried SPME vials prior to extraction resulted in up to less than fivefold improvement in detection limits. Using 40 mL wine samples, limits of detection for 4-MMP, 3-MH, and 3-MHA were 0.9 ng/L, 1 ng/L, and 17 ng/L, respectively. Good recovery (90%–109% and precision (5%–11% RSD were achieved in wine matrices. The new method was used to survey polyfunctional thiol concentrations in 61 commercial California and New York State wines produced from V. vinifera (Riesling, Gewürztraminer, Cabernet Sauvignon, Sauvignon blanc and non-varietal rosé wines, V. labruscana (Niagara, and Vitis spp. (Cayuga White. Mean 4-MMP concentrations in New York Niagara (17 ng/L were not significantly different from concentrations in Sauvignon blanc, but were significantly higher than 4-MMP in other varietal wines.

  16. 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.

  17. HS-SPME analysis of volatile organic compounds of coniferous needle litter

    Science.gov (United States)

    Isidorov, V. A.; Vinogorova, V. T.; Rafałowski, K.

    The composition of volatile emission of Scots pine ( Pinus sylvestris) and spruce ( Picea exelsa) litter was studied by gas chromatography-mass spectrometry (GC-MS) and samples were collected by solid-phase microextraction (SPME) method. The list of identified compounds includes over 60 organic substances of different classes. It was established that volatile emission contain not only components of essential oils of pine and spruce needles but also a large number of organic compounds which are probably secondary metabolites of litter-decomposing fungi. They include lower carbonyl compounds and alcohols as well as products of terpene dehydration and oxidation. These data show that the processes of litter decomposition are an important source of reactive organic compounds under canopy of coniferous forests.

  18. A sensitive method using SPME pre-concentration for the quantification of aromatic amines in indoor air.

    Science.gov (United States)

    Lucaire, Vincent; Schwartz, Jean-Jacques; Delhomme, Olivier; Ocampo-Torres, Ruben; Millet, Maurice

    2018-03-01

    Monitoring the levels of aliphatic and aromatic amines (AA) in indoor air is important to protect human health because of exposure to these compounds through diet and inhalation. A sampling and analytical method using XAD-2 cartridges and gas chromatography coupled to mass spectrometry used for assessing 25 AA in different smoking and non-smoking indoor environment was developed. After sampling and delivering 1 m 3 of air (6-8 h sampling), an adsorbent was ultrasonically extracted with acetonitrile, concentrated to 1 mL and diluted in 25 mL of water (pH = 9; 5% NaCl), and then extracted for 40 min at 80 °C using a divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) fiber and injected in a GC/MS system. With this method, 22 of the 25 AA can be analyzed with detection limits up to five times lower than that of classic liquid injection. Benzylamine, 3-aminophenol, and 4-aminophenol were not detected with the solid-phase micro-extraction (SPME) method. It can be assumed that aminophenols required a derivatization step for their analysis by GC as these molecules were not detected regardless of the injection mode used. Graphical abstract Analysis of aromatic amines in indoor air by SPME-GC/MS.

  19. Sampling and analytical procedures for the determination of VOCs released into air from natural and anthropogenic sources: A comparison between SPME (Solid Phase Micro Extraction) and ST (Solid Trap) methods

    International Nuclear Information System (INIS)

    Tassi, F.; Capecchiacci, F.; Buccianti, A.; Vaselli, O.

    2012-01-01

    In the present study, two sampling and analytical methods for VOC determination in fumarolic exhalations related to hydrothermal-magmatic reservoirs in volcanic and geothermal areas and biogas released from waste landfills were compared: (a) Solid Traps (STs), consisting of three phase (Carboxen B, Carboxen C and Carbosieve S111) absorbent stainless steel tubes and (b) Solid Phase Micro Extraction (SPME) fibers, composed of DiVinylBenzene (DVB), Carboxen and PolyDimethylSiloxane. These techniques were applied to pre-concentrate VOCs discharged from: (i) low-to-high temperature fumaroles collected at Vulcano Island, Phlegrean Fields (Italy), and Nisyros Island (Greece), (ii) recovery wells in a solid waste disposal site located near Florence (Italy). A glass condensing system cooled with water was used to collect the dry fraction of the fumarolic gases, in order to allow more efficient VOC absorption avoiding any interference by water vapor and acidic gases, such as SO 2 , H 2 S, HF and HCl, typically present at relatively high concentrations in these fluids. Up to 37 organic species, in the range of 40–400 m/z, were determined by coupling gas chromatography to mass spectrometry (GC–MS). This study shows that the VOC compositions of fumaroles and biogas determined via SPME and ST are largely consistent and can be applied to the analysis of VOCs in gases released from different natural and anthropogenic environments. The SPME method is rapid and simple and more appropriate for volcanic and geothermal emissions, where VOCs are present at relatively high concentrations and prolonged gas sampling may be hazardous for the operator. The ST method, allowing the collection of large quantities of sample, is to be preferred to analyze the VOC composition of fluids from diffuse emissions and air, where these compounds are present at relatively low concentrations.

  20. Development of a HS-SPME-GC-MS/MS Method for the Quantitation of Thymol and Carvacrol in Bovine Matrices and To Determine Residue Depletion in Milk and Tissues.

    Science.gov (United States)

    Armorini, Sara; Yeatts, James E; Mullen, Keena A E; Mason, Sharon E; Mehmeti, Elmira; Anderson, Kevin L; Washburn, Steve P; Baynes, Ronald E

    2016-10-11

    Thymol and carvacrol may be present in several phytoceutical products but there are no well-defined methods to measure these compounds in meat and milk from treated animals. U.S. regulatory authorities deem their presence as an adulteration of food. A rapid and sensitive HS-SPME-GC-MS/MS method was developed for the detection of thymol and carvacrol in bovine milk, plasma, liver, kidney, and fat. Inter- and intraday precision values were all less than 15.7 and 20.2% for thymol and carvacrol, respectively. The accuracy was in ranges of 69.9-111.8% for thymol and 74.0-119.2% for carvacrol. With the exception of fat tissue, stability studies showed that both compounds are stable over a 2 month period. A pilot pharmacokinetic study was conducted to evaluate the developed analytical method and to provide initial estimates of thymol and carvacrol depletion in plasma, milk, and several tissues. Treatment of lactating dairy cattle with phytoceutical products containing these substances resulted in low but measurable residue levels at 96 h for liver and 36 h for milk with very short apparent plasma and milk half-lives (<3.0 h).

  1. Extraction with SPME and Synthesis of 2-Methyl-6-vinylpyrazine by a ‘One Pot’ Reaction Using Microwaves

    Directory of Open Access Journals (Sweden)

    René Arzuffi

    2009-06-01

    Full Text Available A synthesis of 2-methyl-6-vinylpyrazine was carried out by way of a ‘one pot’ reaction. In order to establish the efficiency of this synthesis the extraction of the volatiles released by male papaya fruit flies was performed by SPME (solid phase micro-extraction. The compound was separated and identified using GC/MSD (gas chromatography/mass spectrometry detector.

  2. New insight on biological interaction analysis: new nanocrystalline mixed metal oxide SPME fiber for GC-FID analysis of BTEX and its application in human hemoglobin-benzene interaction studies.

    Directory of Open Access Journals (Sweden)

    Reza Hosseinzadeh

    Full Text Available Nanocrystalline mixed metal oxides (MMO of various metal cations were synthesized and were used for coating a piece of copper wire as a new high sensitive solid phase micro extraction (SPME fiber in extraction and determination of BTEX compounds from the headspace of aqueous samples prior to GC-FID analysis. Under optimum extraction conditions, the proposed fiber exhibited low detection limits, and quantification limits, good reproducibility, simple and fast preparation method, high fiber capacity and high thermal and mechanical durability. These are some of the most important advantages of the new fiber. The proposed fiber was used for human hemoglobin upon interaction with benzene. Binding isotherm, Scatchard and Klotz logarithmic plots were constructed using HS-SPME-GC data, accurately. The obtained binding isotherm analyzed using Hill method. The Hill parameters have been obtained by calculating saturation parameter from the ratio of measured chromatographic peak areas in the presence and absence of hemoglobin. In this interaction, Hill coefficient and Hill constant determined as (nH = 6.14 and log KH = 6.47 respectively. These results reveal the cooperativity of hemoglobin upon interaction with benzene.

  3. Rapid measurement of 13C-enrichment of acetic, propionic and butyric acids in plasma with solid phase microextraction coupled to gas chromatography-mass spectrometry

    International Nuclear Information System (INIS)

    Moreau, N.M.; Delepee, R.; Maume, D.; Le Bizec, B.; Nguyen, P.G.; Champ, M.M.; Martin, L.J.; Dumon, H.J.

    2004-01-01

    An analytical procedure based on solid phase microextraction (SPME) has been developed to quantify [1- 13 C]-labelled short-chain fatty acids (SCFAs)--mainly acetic, propionic and butyric acids--in a small volume (120 μl) of deproteinised plasma (corresponding to 200 μl of raw plasma) by gas chromatography-mass spectrometry (GC-MS) analysis. Simultaneous SCFA extraction was optimal after 5 min using a 75 μm Carboxen/polydimethylsiloxane-coated fiber. The base peak of the three analytes has been characterised by middle-resolution mass spectrometry (R>6000). All these data allowed the specificity reinforcement of the measure. The validation of the method also considered the linearity and the repeatability of the [ 13 C]SCFA measurements by SPME-GC-MS. Results were linear in a range from 5 to 100 mol% of [ 13 C]SCFA enrichment and the method provided a good intra-day (R.S.D. 13 C]butyric acid) by cecal infusion before blood sampling in portal vein. Results of [1- 13 C]butyric acid enrichment showed an excellent correlation (r 2 =0.9832; n=30) with data obtained on the same samples using a previously published procedure based on diethyl extraction and derivatisation before GC-MS analyses. SPME coupled to GC-MS appears to be a powerful analytical tool for the direct isotopic measurements of low deproteinised plasma volume avoiding consequently preliminary treatment such as extraction or derivatisation. The presented method could be of great interest for real time [ 13 C]SCFA plasma determination of in metabolic in vivo studies in small animal models

  4. Assessing bioavailability of DDT and metabolites in marine sediments using solid-phase microextraction with performance reference compounds.

    Science.gov (United States)

    Bao, Lian-Jun; Jia, Fang; Crago, J; Zeng, Eddy Y; Schlenk, D; Gan, Jay

    2013-09-01

    Solid-phase microextraction (SPME) has often been used to estimate the freely dissolved concentration (Cfree ) of organic contaminants in sediments. A significant limitation in the application of SPME for Cfree measurement is the requirement for attaining equilibrium partition, which is often difficult for strongly hydrophobic compounds such as DDT. A method was developed using SPME with stable isotope-labeled analogues as performance reference compounds (PRCs) to measure Cfree of DDT and metabolites (DDTs) in marine sediments. Six (13) C-labeled or deuterated PRCs were impregnated into polydimethylsiloxane (PDMS) fiber before use. Desorption of PRCs from PDMS fibers and absorption of DDTs from sediment were isotropic in a range of sediments evaluated ex situ under well-mixed conditions. When applied to a historically contaminated marine sediment from a Superfund site, the PRC-SPME method yielded Cfree values identical to those found by using a conventional equilibrium SPME approach (Eq-SPME), whereas the time for mixing was reduced from 9 d to only 9 h. The PRC-SPME method was further evaluated against bioaccumulation of DDTs by Neanthes arenaceodentata in the contaminated sediment with or without amendment of activated carbon or sand. Strong correlations were consistently found between the derived equilibrium concentrations on the fiber and lipid-normalized tissue residues for DDTs in the worms. Results from the present study clearly demonstrated the feasibility of coupling PRCs with SPME sampling to greatly shorten sampling time, thus affording much improved flexibility in the use of SPME for bioavailability evaluation. Copyright © 2013 SETAC.

  5. Experimental design-based isotope-dilution SPME-GC/MS method development for the analysis of smoke flavouring products.

    Science.gov (United States)

    Giri, Anupam; Zelinkova, Zuzana; Wenzl, Thomas

    2017-12-01

    For the implementation of Regulation (EC) No 2065/2003 related to smoke flavourings used or intended for use in or on foods a method based on solid-phase micro extraction (SPME) GC/MS was developed for the characterisation of liquid smoke products. A statistically based experimental design (DoE) was used for method optimisation. The best general conditions to quantitatively analyse the liquid smoke compounds were obtained with a polydimethylsiloxane/divinylbenzene (PDMS/DVB) fibre, 60°C extraction temperature, 30 min extraction time, 250°C desorption temperature, 180 s desorption time, 15 s agitation time, and 250 rpm agitation speed. Under the optimised conditions, 119 wood pyrolysis products including furan/pyran derivatives, phenols, guaiacol, syringol, benzenediol, and their derivatives, cyclic ketones, and several other heterocyclic compounds were identified. The proposed method was repeatable (RSD% <5) and the calibration functions were linear for all compounds under study. Nine isotopically labelled internal standards were used for improving quantification of analytes by compensating matrix effects that might affect headspace equilibrium and extractability of compounds. The optimised isotope dilution SPME-GC/MS based analytical method proved to be fit for purpose, allowing the rapid identification and quantification of volatile compounds in liquid smoke flavourings.

  6. Development and Validation of a SPME-GC-MS Method for In situ Passive Sampling of Root Volatiles from Glasshouse-Grown Broccoli Plants Undergoing Below-Ground Herbivory by Larvae of Cabbage Root Fly, Delia radicum L.

    Science.gov (United States)

    Deasy, William; Shepherd, Tom; Alexander, Colin J; Birch, A Nicholas E; Evans, K Andrew

    2016-11-01

    Research on plant root chemical ecology has benefited greatly from recent developments in analytical chemistry. Numerous reports document techniques for sampling root volatiles, although only a limited number describe in situ collection. To demonstrate a new method for non-invasive in situ passive sampling using solid phase micro extraction (SPME), from the immediate vicinity of growing roots. SPME fibres inserted into polyfluorotetrafluoroethylene (PTFE) sampling tubes located in situ which were either perforated, covered with stainless steel mesh or with microporous PTFE tubing, were used for non-invasive sub-surface sampling of root volatiles from glasshouse-grown broccoli. Sampling methods were compared with above surface headspace collection using Tenax TA. The roots were either mechanically damaged or infested with Delia radicum larvae. Principal component analysis (PCA) was used to investigate the effect of damage on the composition of volatiles released by broccoli roots. Analyses by gas chromatography-mass spectrometry (GC-MS) with SPME and automated thermal desorption (ATD) confirmed that sulphur compounds, showing characteristic temporal emission patterns, were the principal volatiles released by roots following insect larval damage. Use of SPME with in situ perforated PTFE sampling tubes was the most robust method for out-of-lab sampling. This study describes a new method for non-invasive passive sampling of volatiles in situ from intact and insect damaged roots using SPME. The method is highly suitable for remote sampling and has potential for wide application in chemical ecology/root/soil research. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  7. Development of a simple and sensitive method for the characterization of odorous waste gas emissions by means of solid-phase microextraction (SPME) and GC-MS/olfactometry.

    Science.gov (United States)

    Kleeberg, K K; Liu, Y; Jans, M; Schlegelmilch, M; Streese, J; Stegmann, R

    2005-01-01

    A solid-phase microextraction (SPME) method has been developed for the extraction of odorous compounds from waste gas. The enriched compounds were characterized by gas chromatography-mass spectrometry (GC-MS) and gas chromatography followed by simultaneous flame ionization detection and olfactometry (GC-FID/O). Five different SPME fiber coatings were tested, and the carboxen/polydimethylsiloxane (CAR/PDMS) fiber showed the highest ability to extract odorous compounds from the waste gas. Furthermore, parameters such as exposure time, desorption temperature, and desorption time have been optimized. The SPME method was successfully used to characterize an odorous waste gas from a fat refinery prior to and after waste gas treatment in order to describe the treatment efficiency of the used laboratory scale plant which consisted of a bioscrubber/biofilter combination and an activated carbon adsorber. The developed method is a valuable approach to provide detailed information of waste gas composition and complements existing methods for the determination of odors. However, caution should be exercised if CAR/PDMS fibers are used for the quantification of odorous compounds in multi-component matrices like waste gas emissions since the relative affinity of each analyte was shown to differ according to the total amount of analytes present in the sample.

  8. Ultra trace analysis of PAHs by designing simple injection of large amounts of analytes through the sample reconcentration on SPME fiber after magnetic solid phase extraction.

    Science.gov (United States)

    Khodaee, Nader; Mehdinia, Ali; Esfandiarnejad, Reyhaneh; Jabbari, Ali

    2016-01-15

    A simple solventless injection method was introduced based on the using of a solid-phase microextraction (SPME) fiber for injection of large amounts of the analytes extracted by the magnetic solid phase extraction (MSPE) procedure. The resulted extract from MSPE procedure was loaded on a G-coated SPME fiber, and then the fiber was injected into the gas chromatography (GC) injection port. This method combines the advantages of exhaustive extraction property of MSPE and the solvent-less injection of SPME to improve the sensitivity of the analysis. In addition, the analytes were re-concentrated prior to inject into the gas chromatography (GC) inlet because of the organic solvent removing from the remaining extract of MSPE technique. Injection of the large amounts of analytes was made possible by using the introduced procedure. Fourteen polycyclic aromatic hydrocarbons (PAHs) with different volatility were used as model compounds to investigate the method performance for volatile and semi-volatile compounds. The introduced method resulted in the higher enhancement factors (5097-59376), lower detection limits (0.29-3.3pgmL(-1)), and higher sensitivity for the semi-volatile compounds compared with the conventional direct injection method. Copyright © 2015 Elsevier B.V. All rights reserved.

  9. Development and validation of automatic HS-SPME with a gas chromatography-ion trap/mass spectrometry method for analysis of volatiles in wines.

    Science.gov (United States)

    Paula Barros, Elisabete; Moreira, Nathalie; Elias Pereira, Giuliano; Leite, Selma Gomes Ferreira; Moraes Rezende, Claudia; Guedes de Pinho, Paula

    2012-11-15

    An automated headspace solid-phase microextraction (HS-SPME) combined with gas chromatography-ion trap/mass spectrometry (GC-IT/MS) was developed in order to quantify a large number of volatile compounds in wines such as alcohols, ester, norisoprenoids and terpenes. The procedures were optimized for SPME fiber selection, pre-incubation temperature and time, extraction temperature and time, and salt addition. A central composite experimental design was used in the optimization of the extraction conditions. The volatile compounds showed optimal extraction using a DVB/CAR/PDMS fiber, incubation of 5 ml of wine with 2g NaCl at 45 °C during 5 min, and subsequent extraction of 30 min at the same temperature. The method allowed the identification of 64 volatile compounds. Afterwards, the method was validated successfully for the most significant compounds and was applied to study the volatile composition of different white wines. Copyright © 2012 Elsevier B.V. All rights reserved.

  10. Natural Variation of Volatile Compounds in Virgin Olive Oil Analyzed by HS-SPME/GC-MS-FID

    Directory of Open Access Journals (Sweden)

    Carlos Sanz

    2018-04-01

    Full Text Available Virgin olive oil is unique among plant oils for its high levels of oleic acid, and the presence of a wide range of minor components, which are responsible for both its health-promoting properties and characteristic aroma, and only produced when olives are crushed during the industrial process used for oil production. The genetic variability of the major volatile compounds comprising the oil aroma was studied in a representative sample of olive cultivars from the World Olive Germplasm Collection (IFAPA, Cordoba, Spain, by means of the headspace solid-phase microextraction/gas chromatography–mass spectrometry–flame ionization detection (HS-SPME/GC-MS-FID. The analytical data demonstrated that a high variability is found for the content of volatile compounds in olive species, and that most of the volatile compounds found in the oils were synthesized by the enzymes included in the so-called lipoxygenase pathway. Multivariate analysis allowed the identification of cultivars that are particularly interesting, in terms of volatile composition and presumed organoleptic quality, which can be used both to identify old olive cultivars that give rise to oils with a high organoleptic quality, and in parent selection for olive breeding programs.

  11. Characterization of the volatile components in green tea by IRAE-HS-SPME/GC-MS combined with multivariate analysis.

    Science.gov (United States)

    Yang, Yan-Qin; Yin, Hong-Xu; Yuan, Hai-Bo; Jiang, Yong-Wen; Dong, Chun-Wang; Deng, Yu-Liang

    2018-01-01

    In the present work, a novel infrared-assisted extraction coupled to headspace solid-phase microextraction (IRAE-HS-SPME) followed by gas chromatography-mass spectrometry (GC-MS) was developed for rapid determination of the volatile components in green tea. The extraction parameters such as fiber type, sample amount, infrared power, extraction time, and infrared lamp distance were optimized by orthogonal experimental design. Under optimum conditions, a total of 82 volatile compounds in 21 green tea samples from different geographical origins were identified. Compared with classical water-bath heating, the proposed technique has remarkable advantages of considerably reducing the analytical time and high efficiency. In addition, an effective classification of green teas based on their volatile profiles was achieved by partial least square-discriminant analysis (PLS-DA) and hierarchical clustering analysis (HCA). Furthermore, the application of a dual criterion based on the variable importance in the projection (VIP) values of the PLS-DA models and on the category from one-way univariate analysis (ANOVA) allowed the identification of 12 potential volatile markers, which were considered to make the most important contribution to the discrimination of the samples. The results suggest that IRAE-HS-SPME/GC-MS technique combined with multivariate analysis offers a valuable tool to assess geographical traceability of different tea varieties.

  12. Characterization of the volatile components in green tea by IRAE-HS-SPME/GC-MS combined with multivariate analysis.

    Directory of Open Access Journals (Sweden)

    Yan-Qin Yang

    Full Text Available In the present work, a novel infrared-assisted extraction coupled to headspace solid-phase microextraction (IRAE-HS-SPME followed by gas chromatography-mass spectrometry (GC-MS was developed for rapid determination of the volatile components in green tea. The extraction parameters such as fiber type, sample amount, infrared power, extraction time, and infrared lamp distance were optimized by orthogonal experimental design. Under optimum conditions, a total of 82 volatile compounds in 21 green tea samples from different geographical origins were identified. Compared with classical water-bath heating, the proposed technique has remarkable advantages of considerably reducing the analytical time and high efficiency. In addition, an effective classification of green teas based on their volatile profiles was achieved by partial least square-discriminant analysis (PLS-DA and hierarchical clustering analysis (HCA. Furthermore, the application of a dual criterion based on the variable importance in the projection (VIP values of the PLS-DA models and on the category from one-way univariate analysis (ANOVA allowed the identification of 12 potential volatile markers, which were considered to make the most important contribution to the discrimination of the samples. The results suggest that IRAE-HS-SPME/GC-MS technique combined with multivariate analysis offers a valuable tool to assess geographical traceability of different tea varieties.

  13. Range-Measuring Video Sensors

    Science.gov (United States)

    Howard, Richard T.; Briscoe, Jeri M.; Corder, Eric L.; Broderick, David

    2006-01-01

    Optoelectronic sensors of a proposed type would perform the functions of both electronic cameras and triangulation- type laser range finders. That is to say, these sensors would both (1) generate ordinary video or snapshot digital images and (2) measure the distances to selected spots in the images. These sensors would be well suited to use on robots that are required to measure distances to targets in their work spaces. In addition, these sensors could be used for all the purposes for which electronic cameras have been used heretofore. The simplest sensor of this type, illustrated schematically in the upper part of the figure, would include a laser, an electronic camera (either video or snapshot), a frame-grabber/image-capturing circuit, an image-data-storage memory circuit, and an image-data processor. There would be no moving parts. The laser would be positioned at a lateral distance d to one side of the camera and would be aimed parallel to the optical axis of the camera. When the range of a target in the field of view of the camera was required, the laser would be turned on and an image of the target would be stored and preprocessed to locate the angle (a) between the optical axis and the line of sight to the centroid of the laser spot.

  14. Extração em fase sólida (SPE e micro extração em fase sólida (SPME de piretróides em água Solid-phase extraction (SPE and solid-phase microextraction of pyrethroids in water

    Directory of Open Access Journals (Sweden)

    Wilma Regina Barrionuevo

    2001-04-01

    Full Text Available The pyrethroids bifenthrin, permethrin, cypermethrin and deltamethrin were extracted by solid phase extraction (SPE and solid phase microextraction (SPME. The analysis were performed on a gas chromatograph with electron capture detection (GC-ECD. Octadecil Silano-C18, Florisil and Silica stationary phases were studied for SPE. Better results were obtained for Florisil which gave recoveries from 80% to 108%. Pyrethroids extraction by SPME showed a linear response and a detection limit of 10 pg ml-1. Although the data showed that the two extraction methods were able to isolate the pesticide residues from water samples, the best results were obtained by using SPME which is more sensitive, faster, cheeper, being a more useful technique for the analysis of pyrethroids in drinking water.

  15. Differentiation of Toxic Molds via Headspace SPME-GC/MS and Canine Detection

    Directory of Open Access Journals (Sweden)

    Kenneth G. Furton

    2007-08-01

    Full Text Available Indoor mold growth has recently become a concern in the legal world in regards to insurance litigation. Hazardous mold exposure to humans has been linked to many acute and chronic adverse health effects including death. As it grows, mold produces several types of primary and secondary metabolites, including microbial volatile organic compounds (MVOCs. Microbial volatile organic compound emission may be used as a preliminary indication of a mold infestation that is invisible to the unaided eye. The objective of the study is to identify the unique odor signatures of three species of molds, Aspergillus versicolor, Penicillium chrysogenum, and Stachybotrys chartarum by SPME-GC/MS analysis. Determining the compounds that are emitted by the selected species has made it possible to conduct validation studies of canine detection of these mold species through a series of field tests.

  16. Compound-specific nitrogen and carbon isotope analysis of nitroaromatic compounds in aqueous samples using solid-phase microextraction coupled to GC/IRMS.

    Science.gov (United States)

    Berg, Michael; Bolotin, Jakov; Hofstetter, Thomas B

    2007-03-15

    Solid-phase microextraction (SPME) coupled to gas chromatography/isotope ratio mass spectrometry was used to determine the delta15N and delta13C signatures of selected nitroaromatic contaminants such as the explosive 2,4,6-trinitrotoluene (TNT) for derivation of isotopic enrichment factors of contaminant transformation. Parameters for efficient extraction of nitroaromatic compounds (NACs) and substituted anilines from water samples were evaluated by SPME-GC/MS. delta13C signatures determined by SPME-GC/IRMS and elemental analyzer IRMS (EA-IRMS) were in good agreement, generally within +/-0.7 per thousand, except for 2,4-dinitrotoluene (2,4-DNT) and TNT, which showed slight deviations (IRMS were between 73 and 780 microg L-1 and correlated with the extraction efficiencies of the compounds determined by SPME-GC/MS. Nitrogen isotope measurements by SPME-GC/IRMS were of similar precision (standard deviations IRMS within +/-1.3 per thousand (+2.5 per thousand for TNT), but no systematic trend was found for the deviations. LODs of delta15N measurements ranged from 1.6 to 9.6 mg L-1 for nitrotoluenes, chlorinated NACs and DNTs (22 mg L-1 for TNT). The SPME-GC/IRMS method is well suited for the determination of isotopic enrichment factors of various NAC transformation processes and provides so far unexplored possibilities to elucidate behavior and degradation mechanisms of nitroaromatic contaminants in soils and groundwaters.

  17. Characterisation of the volatile profile of coconut water from five varieties using an optimised HS-SPME-GC analysis.

    Science.gov (United States)

    Prades, Alexia; Assa, Rebecca Rachel Ablan; Dornier, Manuel; Pain, Jean-Pierre; Boulanger, Renaud

    2012-09-01

    Coconut (Cocos nucifera L.) water is a refreshing tropical drink whose international market has recently been growing. However, little is yet known about its physicochemical composition, particularly its aroma. This study set out to characterise the volatile profile of water from five coconut varieties. Aroma compounds were characterised by headspace solid phase microextraction gas chromatography (HS-SPME-GC) analysis. An experimental design was established to optimise SPME conditions, leading to an equilibration time of 10 min followed by an extraction time of 60 min at 50 °C. Accordingly, immature coconut water from WAT (West African Tall), PB121 (MYD × WAT Hybrid), MYD (Malayan Yellow Dwarf), EGD (Equatorial Guinea Green Dwarf) and THD (Thailand Aromatic Green Dwarf) palms was analysed and described. Ketones were mainly present in the Tall and Hybrid varieties, whereas aldehydes were most abundant in the Dwarf palms. Tall coconut water was characterised by a high lactone content. THD exhibited a high ethyl octanoate level. The cluster analysis of the volatile fraction from the five coconut cultivars was found to be related to their genetic classification. The volatile compounds of immature coconut water from five varieties were characterised for the first time. Volatile profile analysis could be a useful tool for the selection of Dwarf coconut varieties, which are mainly consumed as a beverage. Copyright © 2012 Society of Chemical Industry.

  18. Simultaneous analysis of organochlorine pesticides and polychlorinated biphenyls in air samples by using accelerated solvent extraction (ASE) and solid-phase micro-extraction (SPME) coupled to gas chromatography dual electron capture detection.

    Science.gov (United States)

    Mokbel, Haifaa; Al Dine, Enaam Jamal; Elmoll, Ahmad; Liaud, Céline; Millet, Maurice

    2016-04-01

    An analytical method associating accelerated solvent extraction (ASE) and solid-phase micro-extraction (SPME) in immersion mode combined with gas chromatography dual electrons capture detectors (SPME-GC-2ECD) has been developed and studied for the simultaneous determination of 19 organochlorine pesticides (OCPs) and 22 polychlorinated biphenyls (PCBs) in air samples (active and XAD-2 passive samplers). Samples were extracted with ASE with acetonitrile using the following conditions: temperature, 150 °C; pressure, 1500 psi; static, 15 min; cycles, 3; purge, 300 s; flush, 100 %. Extracts were reduced to 1 mL, and 500 μL of this extract, filled with deionised water, was subject to SPME extraction. Experimental results indicated that the proposed method attained the best extraction efficiency under the optimised conditions: extraction of PCB-OCP mixture using 100-μm PDMS fibre at 80 °C for 40 min with no addition of salt. The performance of the proposed ASE-SPME-GC-2ECD methodology with respect to linearity, limit of quantification and detection was evaluated by spiking of XAD-2 resin with target compounds. The regression coefficient (R (2)) of most compounds was found to be high of 0.99. limits of detection (LODs) are between 0.02 and 4.90 ng m(-3), and limits of quantification (LOQs) are between 0.05 and 9.12 ng m(-3) and between 0.2 and 49 ng/sampler and 0.52 and 91 ng/sampler, respectively, for XAD-2 passive samplers. Finally, a developed procedure was applied to determine selected PCBs and OCPs in the atmosphere.

  19. An approach to determination of phenolic compounds in seawater using SPME-GC-MS based on SWCNTs coating

    Science.gov (United States)

    Zhu, Jia; Wang, Ying; Zeng, Lin

    2016-08-01

    Phenolic compounds have become one kind of the important pollutants of the marine environment. Single-walled Carbon nanotubes, as one-dimensional nano materials, have light weight and perfect hexagonal structure of connections, with many unusual mechanical, chemical and electrical properties. In recent years, with the research of carbon nanotubes and other nano materials, the application prospect is also constantly discussed. In this paper, homemade single-walled carbon nanotubes (SWCNTs) coating was used for establishing an analytical approach to the determination of five kinds of phenolic compounds in seawater using SPME-GC-MS. Optimal conditions: After saturation was conducted with NaCl, and pH was adjusted to 2.0 with H2SO4, the extract was immersed in a water bath at 40°C for GC-MS determination through 40-min agitating extraction at 500 rmin-1 and 3-min desorption at 280°C. The liniearities ranged between 0.01-100 μg L-1, and the determination limits ranged between 1.5-10 ng L-1. The relative standard deviation (RSD, n = 5) was less than 6.5%. For the phenolic compounds obtained from the spiked recovery test for actual seawater samples, the rates of recovery were 87.5%-101.7%, and the RSDs were less than 8.8%, which met the requirements of determination. Due to its simplicity, high efficiency and low consumption, this approach is suitable for the analysis of trace amounts of phenolic compounds in marine waters.

  20. Authenticity of raspberry flavor in food products using SPME-chiral-GC-MS

    DEFF Research Database (Denmark)

    Hansen, Anne-Mette Sølvbjerg; Frandsen, Henrik Lauritz; Fromberg, Arvid

    2015-01-01

    A fast and simple method for authenticating raspberry flavors from food products was developed. The two enantiomers of the compound (E)-α-ionone from raspberry flavor were separated on a chiral gas chromatographic column. Based on the ratio of these two enantiomers the naturalness of a raspberry...... flavor can be evaluated due to the fact that a natural flavor will consist almost exclusively of the R enantiomer, while a chemical synthesis of the same compound will result in a racemic mixture. 27 food products containing raspberry flavors where investigated using SPME-chiral-GC-MS. We found raspberry...... distribution of the R and S isomer. Two products were labelled to contain natural raspberry flavors but were found to contain almost equal amounts of both enantiomers indicating a presence of synthetic raspberry flavors only. Additionally, two products labelled to contain both raspberry juice and flavor showed...

  1. Analysis of volatile compounds in gluten-free bread crusts with an optimised and validated SPME-GC/QTOF methodology.

    Science.gov (United States)

    Pico, Joana; Antolín, Beatriz; Román, Laura; Gómez, Manuel; Bernal, José

    2018-04-01

    The aroma of bread crust, as one of the first characteristics perceived, is essential for bread acceptance. However, gluten-free bread crusts exhibit weak aroma. A SPME-GC/QTOF methodology was optimised with PCA and RSM and validated for the quantification of 44 volatile compounds in bread crust, extracting 0.75 g of crust at 60 °C for 51 min. LODs ranged between 3.60 and 1760 μg Kg -1 , all the R 2 were higher than 0.99 and %RSD for precision and %Er for accuracy were lower than 9% and 12%, respectively. A commercial wheat bread crust was quantified, and furfural was the most abundant compound. Bread crusts of wheat starch and of japonica rice, basmati rice and teff flours were also quantified. Teff flour and wheat starch crusts were very suitable for improving gluten-free bread crust aroma, due to their similar content in 2-acetyl-1-pyrroline and 4-hydroxy-2,5-dimethyl-3(2H)-furanone compared to wheat flour crust and also for their high content in pyrazines. Copyright © 2018 Elsevier Ltd. All rights reserved.

  2. Measurements of Capture Efficiency of Range Hoods in Homes

    DEFF Research Database (Denmark)

    Simone, Angela; Sherman, Max H.; Walker, Iain S.

    2015-01-01

    mapped the pollution distribution in the room, and showed that the pollutants escape more at the sides of the cooktop. These preliminary results suggest that more measurements should be conducted investigating the capture efficiency at different pollutant source temperature, size and location...... want a range hood to use little energy and have high capture efficiency to minimize the required air flow to capture the cooking pollutants. Currently there are no standards for rating range hoods for capture efficiency In this study, measurements of range hood capture efficiency were made a tight...... kitchen-room built in a laboratory chamber, and a methodology for standardizing measurement of capture efficiency was developed. The results for a wall mounted range hood, showed that up to half of the cooking pollutants were not captured at a flow rate of 230 m3/h. A more detailed set of measurements...

  3. Use of solid phase microextraction (SPME) for profiling the volatile metabolites produced by Glomerella cingulata.

    Science.gov (United States)

    Miyazawa, Mitsuo; Kimura, Minako; Yabe, Yoshito; Tsukamoto, Daisuke; Sakamoto, Masaya; Horibe, Isao; Okuno, Yoshiharu

    2008-01-01

    The profile of volatile organic compounds (VOCs) released from Glomerella cingulata using solid phase microextraction (SPME) with different fibers, Polydimethylsiloxane (PDMS), Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), Carboxen/Polydimethylsiloxane (CAR/PDMS) and Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), was investigated. C4-C6 aliphatic alcohols were the predominant fraction of VOCs isolated by CAR/PDMS fiber. Sesquiterpene hydrocarbons represented 20.3% of VOCs isolated by PDMS fiber. During the growth phase, Ochracin was produced in the large majority of VOCs. 3-Methylbutanol and phenylethyl alcohol were found in the log phase of it. Alcohols were found in cultures of higher age, while sesquiterpenes were found to be characteristic of initial growth stage of G. cingulata.

  4. Method of high precision interval measurement in pulse laser ranging system

    Science.gov (United States)

    Wang, Zhen; Lv, Xin-yuan; Mao, Jin-jin; Liu, Wei; Yang, Dong

    2013-09-01

    Laser ranging is suitable for laser system, for it has the advantage of high measuring precision, fast measuring speed,no cooperative targets and strong resistance to electromagnetic interference,the measuremen of laser ranging is the key paremeters affecting the performance of the whole system.The precision of the pulsed laser ranging system was decided by the precision of the time interval measurement, the principle structure of laser ranging system was introduced, and a method of high precision time interval measurement in pulse laser ranging system was established in this paper.Based on the analysis of the factors which affected the precision of range measure,the pulse rising edges discriminator was adopted to produce timing mark for the start-stop time discrimination,and the TDC-GP2 high precision interval measurement system based on TMS320F2812 DSP was designed to improve the measurement precision.Experimental results indicate that the time interval measurement method in this paper can obtain higher range accuracy. Compared with the traditional time interval measurement system,the method simplifies the system design and reduce the influence of bad weather conditions,furthermore,it satisfies the requirements of low costs and miniaturization.

  5. Determinação do coeficiente de atividade na diluição infinita (g¥ através da micro-extração em fase sólida (SPME Determination of activity coefficients at infinite dilution through solid phase microextraction (SPME

    Directory of Open Access Journals (Sweden)

    Douglas B. Fonseca

    2007-01-01

    Full Text Available In this study a new approach, solid phase micro extraction (SPME, is used in the evaluation of the infinite dilution activity coefficient of the solute in a given solvent. It is the purpose of the current work to demonstrate a different approach to obtain the data needed for studying the solution thermodynamics of binary liquid mixtures as well as for designing multi-component separations. The solutes investigated at the temperature 298.15 K were toluene, ethyl benzene and xylene in the solvent methanol.

  6. Determination of Sesquiterpenes in Wines by HS-SPME Coupled with GC-MS

    Directory of Open Access Journals (Sweden)

    Fabrizio Cincotta

    2015-07-01

    Full Text Available The sesquiterpene compounds present in red wines were characterized and quantified by Headspace Solid-Phase Microextraction in combination with Gas Chromatography–Mass Spectrometry (HS-SPME-GC-MS. Sixteen sesquiterpenes were identified, mainly hydrocarbons but also derived oxygenated compounds. Sesquiterpenes were acyclic, monocyclic, byciclic and tryciclic. Sesquiterpenes were detected in SIM (selected ion monitoring mode using their characteristics ions. All the sesquiterpenes were identified by mass spectral data, linear retention indices (LRI, literature data and injection of standards where available. Quantitative results were obtained using the method of standard additions. The method showed an average LOD = 0.05 µg L−1 and LOQ = 0.15 µg L−1. The monocyclic sesquiterpene with the germacrene skeleton, Germacrene D and the bicyclic sesquiterpene with the muurolane skeleton, α-muurolene were present in all the wine samples analysed. Syrah wines were the samples richest in sesquiterpenes in agreement with their typical spicy and woody notes. The results evidenced the possibility to use sesquiterpenes for wine authenticity and traceability.

  7. ANALYTICAL APPROACH OF THE VOLATILE FRACTION OF Solanum quitoense BY HS-SPME/GC-MS

    Directory of Open Access Journals (Sweden)

    EDUARDO CORPAS IGUARÁN

    2017-07-01

    Full Text Available The species of lulo fruit (Solanum quitoense, predominant in Colombia, is a promising fruit for both national and international market due to its flavor and nutritional characteristics, which generated the interest to know the volatile composition of its pulp. After adjusting, the chromatographic conditions necessary to analyze volatile fraction of this fruit, the effect of the temperature and time of adsorption was measured through the headspace - solid phase microextraction (HS-SPME and gas chromatography - mass spectrometry (GC-MS, on the area of volatile compounds of S. quitoense, by applying the experimental design of a factor. The descriptive analysis suggested that the adsorption at 60°C and 30 minutes promoted optimal recovery of volatiles as well as internal standard (1-Octanol, with recovery of 99,66% at 60ºC, while the non-parametric test Kruskal-Wallis showed statistical differences in the effect of time (P= 0,018, but not of the temperature adsorption (P= 0,058 upon the volatiles compounds area. A predominance of esters (48,98%, aldehydes (18,37%, and alcohols (14,29% was observed and also were found compounds of greatest area such as 3-hexen-1-ol acetate, acetic acid methyl ester, and acetic acid hexyl ester. These metabolites determine the characteristic aroma from lulo pulp and influence the consumer preference.

  8. 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.

  9. High Precision Ranging and Range-Rate Measurements over Free-Space-Laser Communication Link

    Science.gov (United States)

    Yang, Guangning; Lu, Wei; Krainak, Michael; Sun, Xiaoli

    2016-01-01

    We present a high-precision ranging and range-rate measurement system via an optical-ranging or combined ranging-communication link. A complete bench-top optical communication system was built. It included a ground terminal and a space terminal. Ranging and range rate tests were conducted in two configurations. In the communication configuration with 622 data rate, we achieved a two-way range-rate error of 2 microns/s, or a modified Allan deviation of 9 x 10 (exp -15) with 10 second averaging time. Ranging and range-rate as a function of Bit Error Rate of the communication link is reported. They are not sensitive to the link error rate. In the single-frequency amplitude modulation mode, we report a two-way range rate error of 0.8 microns/s, or a modified Allan deviation of 2.6 x 10 (exp -15) with 10 second averaging time. We identified the major noise sources in the current system as the transmitter modulation injected noise and receiver electronics generated noise. A new improved system will be constructed to further improve the system performance for both operating modes.

  10. Development of a HS-SPME-GC/MS protocol assisted by chemometric tools to study herbivore-induced volatiles in Myrcia splendens.

    Science.gov (United States)

    Souza Silva, Érica A; Saboia, Giovanni; Jorge, Nina C; Hoffmann, Camila; Dos Santos Isaias, Rosy Mary; Soares, Geraldo L G; Zini, Claudia A

    2017-12-01

    A headspace solid phase microextraction (HS-SPME) method combined with gas chromatography-mass spectrometry (GC/MS) was developed and optimized for extraction and analysis of volatile organic compounds (VOC) of leaves and galls of Myrcia splendens. Through a process of optimization of main factors affecting HS-SPME efficiency, the coating divivnilbenzene-carboxen-polydimethylsiloxane (DVB/Car/PDMS) was chosen as the optimum extraction phase, not only in terms of extraction efficiency, but also for its broader analyte coverage. Optimum extraction temperature was 30°C, while an extraction time of 15min provided the best compromise between extraction efficiencies of lower and higher molecular weight compounds. The optimized protocol was demonstrated to be capable of sampling plant material with high reproducibility, considering that most classes of analytes met the 20% RSD FDA criterion. The optimized method was employed for the analysis of three classes of M. splendens samples, generating a final list of 65 tentatively identified VOC, including alcohols, aldehydes, esters, ketones, phenol derivatives, as well as mono and sesquiterpenes. Significant differences were evident amongst the volatile profiles obtained from non-galled leaves (NGL) and leaf-folding galls (LFG) of M. splendens. Several differences pertaining to amounts of alcohols and aldehydes were detected between samples, particularly regarding quantities of green leaf volatiles (GLV). Alcohols represented about 14% of compounds detected in gall samples, whereas in non-galled samples, alcohol content was below 5%. Phenolic derived compounds were virtually absent in reference samples, while in non-galled leaves and galls their content ranged around 0.2% and 0.4%, respectively. Likewise, methyl salicylate, a well-known signal of plant distress, amounted for 1.2% of the sample content of galls, whereas it was only present in trace levels in reference samples. Chemometric analysis based on Heatmap associated

  11. Measuring the relativistic perigee advance with satellite laser ranging

    CERN Document Server

    Iorio, L; Pavlis, E C

    2002-01-01

    The pericentric advance of a test body by a central mass is one of the classical tests of general relativity. Today, this effect is measured with radar ranging by the perihelion shift of Mercury and other planets in the gravitational field of the Sun, with a relative accuracy of the order of 10 sup - sup 2 -10 sup - sup 3. In this paper, we explore the possibility of a measurement of the pericentric advance in the gravitational field of Earth by analysing the laser-ranged data of some orbiting, or proposed, laser-ranged geodetic satellites. Such a measurement of the perigee advance would place limits on hypothetical, very weak, Yukawa-type components of the gravitational interaction with a finite range of the order of 10 sup 4 km. Thus, we show that, at the present level of knowledge of the orbital perturbations, the relative accuracy, achievable with suitably combined orbital elements of LAGEOS and LAGEOS II, is of the order of 10 sup - sup 3. With the corresponding measured value of (2 + 2 gamma - beta)/3, ...

  12. Development of SPME-LC-MS method for screening of eight beta-blockers and bronchodilators in plasma and urine samples.

    Science.gov (United States)

    Goryński, Krzysztof; Kiedrowicz, Alicja; Bojko, Barbara

    2016-08-05

    The current work describes the development and validation of a simple, efficient, and fast method using solid phase microextraction coupled to liquid chromatography-tandem mass spectrometry (SPME-LC-MS/MS) for the concomitant measurement of eight beta-blockers and bronchodilators in plasma and urine. The presented assay enables quantitative determination of acebutolol, atenolol, fenoterol, nadolol, pindolol, procaterol, sotalol, and timolol. In this work, samples were prepared on a high-throughput platform using the 96-well plate format of the thin film solid phase microextraction (TFME) system, and a biocompatible extraction phase made of hydrophilic-lipophilic balance particles. Analytes were separated on a pentafluorophenyl column (100mm×2.1mm, 3μm) by gradient elution using an UPLC Nexera coupled with an LCMS-8060 mass spectrometer. The mobile phase consisted of water-acetonitrile (0.1% formic acid) at a flow rate of 0.4mLmin(-1). The linearity of the method was checked within therapeutic blood-plasma concentrations, and shown to adequately reflect typically expected concentrations of future study samples. Post-extraction addition experiments showed that the matrix effect ranged in plasma from 98% for procaterol to 115% for nadolol, and in urine, from 85% for nadolol and pindolol to 119% for atenolol. The method was successfully validated using Food and Drug Administration (FDA) guidelines, and met all acceptance criteria for bioanalytical assays at five concentration levels for all selected drugs. The final protocol can be successfully applied for monitoring concentrations of the selected drugs in both plasma and urine matrices obtained from patients or athletes. Copyright © 2016 Elsevier B.V. All rights reserved.

  13. 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.

  14. SOLID PHASE MICRO EXTRACTION (SPME) FLAVOR ANALYSIS OF APPLE JUICE AND COFFEE MIXTURES USING GAS CHROMATOGRAPHY-MASS SPECTROMETRY (GC-MS)

    OpenAIRE

    Mi Ja Kim; Jeehyun Lee; Jaeyoung Byun; Sunmi Choi; Wonsik Choi

    2016-01-01

    This research was conducted to evaluate the flavor of apple juice and coffee mixtures and the sensory quality of SPME extracts using gas chromatography-mass spectrometry (GC-MS). Three samples with different compositions were examined. Sample A1 contained85% apple juiceand 15% coffee, sample A2 had87.5% apple and 12.5% coffee, and sample A3 had90% apple juiceand 10% coffee. The sensory analysis involved 100 panelists and a sequential monadic test. Sample presentation orders were balanced in ...

  15. Phytoscreening for chlorinated solvents using rapid in vitro SPME sampling: Application to urban plume in Verl, Germany

    Science.gov (United States)

    Limmer, M.A.; Balouet, J.-C.; Karg, F.; Vroblesky, D.A.; Burken, J.G.

    2011-01-01

    Rapid detection and delineation of contaminants in urban settings is critically important in protecting human health. Cores from trees growing above a plume of contaminated groundwater in Verl, Germany, were collected in 1 day, with subsequent analysis and plume mapping completed over several days. Solid-phase microextraction (SPME) analysis was applied to detect tetrachloroethene (PCE) and trichloroethene (TCE) to below nanogram/liter levels in the transpiration stream of the trees. The tree core concentrations showed a clear areal correlation to the distribution of PCE and TCE in the groundwater. Concentrations in tree cores were lower than the underlying groundwater, as anticipated; however, the tree core water retained the PCE:TCE signature of the underlying groundwater in the urban, populated area. The PCE:TCE ratio can indicate areas of differing degradation activity. Therefore, the phytoscreening analysis was capable not only of mapping the spatial distribution of groundwater contamination but also of delineating zones of potentially differing contaminant sources and degradation. The simplicity of tree coring and the ability to collect a large number of samples in a day with minimal disruption or property damage in the urban setting demonstrates that phytoscreening can be a powerful tool for gaining reconnaissance-level information on groundwater contaminated by chlorinated solvents. The use of SPME decreases the detection level considerably and increases the sensitivity of phytoscreening as an assessment, monitoring, and phytoforensic tool. With rapid, inexpensive, and noninvasive methods of detecting and delineating contaminants underlying homes, as in this case, human health can be better protected through screening of broader areas and with far faster response times. ?? 2011 American Chemical Society.

  16. Caracterización de los compuestos del aroma en rones colombianos por HS-SPME-GC-MS-O

    Directory of Open Access Journals (Sweden)

    Jazmín Osorio Monsalve

    2016-11-01

    Full Text Available Se identificaron por primera vez 46 compuestos volátiles olfativamente activos con actividad aromática significativa presentes en rones comerciales de Colombia. Lo anterior, mediante microextracción en fase sólida en modo espacio de cabeza (HS-SPME, acoplada a cromatografía de gases con detectores de espectrometría de masas y olfatometría (GC-MS-O. Dentro de los compuestos identificados se encuentran ésteres, compuestos aromáticos, alcoholes, acetales, lactonas y furfural. De esos 46 compuestos, nueve están presentes en todos los rones estudiados y algunos otros son característicos solo de la marca.

  17. Field-based Evaluation of a Novel SPME-GC-MS Method for Investigation of Below-ground Interaction between Brassica Roots and Larvae of Cabbage Root Fly, Delia radicum L.

    Science.gov (United States)

    Deasy, William; Shepherd, Tom; Alexander, Colin J; Birch, A Nicholas E; Evans, K Andrew

    2016-11-01

    Collection of volatiles from plant roots poses technical challenges due to difficulties accessing the soil environment without damaging the roots. To validate a new non-invasive method for passive sampling of root volatiles in situ, from plants grown under field conditions, using solid phase micro-extraction (SPME). SPME fibres were inserted into perforated polytetrafluoroethene (PTFE) tubes positioned in the soil next to broccoli plants for collection of root volatiles pre- and post-infestation with Delia radicum larvae. After sample analysis by gas chromatography-mass spectrometry (GC-MS), principal component analysis (PCA) was applied to determine differences in the profiles of volatiles between samples. GC-MS analysis revealed that this method can detect temporal changes in root volatiles emitted before and after Delia radicum damage. PCA showed that samples collected pre- and post-infestation were compositionally different due to the presence of root volatiles induced by D. radicum feeding. Sulphur containing compounds, in particular, accounted for the differences observed. Root volatiles emission patterns post-infestation are thought to follow the feeding and developmental progress of larvae. This study shows that volatiles released by broccoli roots can be collected in situ using SPME fibres within perforated PTFE tubes under field conditions. Plants damaged by Delia radicum larvae could be distinguished from plants sampled pre-infestation and soil controls on the basis of larval feeding-induced sulphur-containing volatiles. These results show that this new method is a powerful tool for non-invasive sampling of root volatiles below-ground. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  18. High-throughput analysis using non-depletive SPME: challenges and applications to the determination of free and total concentrations in small sample volumes.

    Science.gov (United States)

    Boyacı, Ezel; Bojko, Barbara; Reyes-Garcés, Nathaly; Poole, Justen J; Gómez-Ríos, Germán Augusto; Teixeira, Alexandre; Nicol, Beate; Pawliszyn, Janusz

    2018-01-18

    In vitro high-throughput non-depletive quantitation of chemicals in biofluids is of growing interest in many areas. Some of the challenges facing researchers include the limited volume of biofluids, rapid and high-throughput sampling requirements, and the lack of reliable methods. Coupled to the above, growing interest in the monitoring of kinetics and dynamics of miniaturized biosystems has spurred the demand for development of novel and revolutionary methodologies for analysis of biofluids. The applicability of solid-phase microextraction (SPME) is investigated as a potential technology to fulfill the aforementioned requirements. As analytes with sufficient diversity in their physicochemical features, nicotine, N,N-Diethyl-meta-toluamide, and diclofenac were selected as test compounds for the study. The objective was to develop methodologies that would allow repeated non-depletive sampling from 96-well plates, using 100 µL of sample. Initially, thin film-SPME was investigated. Results revealed substantial depletion and consequent disruption in the system. Therefore, new ultra-thin coated fibers were developed. The applicability of this device to the described sampling scenario was tested by determining the protein binding of the analytes. Results showed good agreement with rapid equilibrium dialysis. The presented method allows high-throughput analysis using small volumes, enabling fast reliable free and total concentration determinations without disruption of system equilibrium.

  19. Measuring the relativistic perigee advance with satellite laser ranging

    International Nuclear Information System (INIS)

    Iorio, Lorenzo; Ciufolini, Ignazio; Pavlis, Erricos C

    2002-01-01

    The pericentric advance of a test body by a central mass is one of the classical tests of general relativity. Today, this effect is measured with radar ranging by the perihelion shift of Mercury and other planets in the gravitational field of the Sun, with a relative accuracy of the order of 10 -2 -10 -3 . In this paper, we explore the possibility of a measurement of the pericentric advance in the gravitational field of Earth by analysing the laser-ranged data of some orbiting, or proposed, laser-ranged geodetic satellites. Such a measurement of the perigee advance would place limits on hypothetical, very weak, Yukawa-type components of the gravitational interaction with a finite range of the order of 10 4 km. Thus, we show that, at the present level of knowledge of the orbital perturbations, the relative accuracy, achievable with suitably combined orbital elements of LAGEOS and LAGEOS II, is of the order of 10 -3 . With the corresponding measured value of (2 + 2γ - β)/3, by using η = 4β - γ - 3 from lunar laser ranging, we could get an estimate of the PPN parameters γ and β with an accuracy of the order of 10 -2 -10 -3 . Nevertheless, these accuracies would be substantially improved in the near future with the new Earth gravity field models by the CHAMP and GRACE missions. The use of the perigee of LARES (LAser RElativity Satellite), with a suitable combination of orbital residuals including also the node and the perigee of LAGEOS II, would also further improve the accuracy of the proposed measurement

  20. Optimization of the Extraction of the Volatile Fraction from Honey Samples by SPME-GC-MS, Experimental Design, and Multivariate Target Functions

    Directory of Open Access Journals (Sweden)

    Elisa Robotti

    2017-01-01

    Full Text Available Head space (HS solid phase microextraction (SPME followed by gas chromatography with mass spectrometry detection (GC-MS is the most widespread technique to study the volatile profile of honey samples. In this paper, the experimental SPME conditions were optimized by a multivariate strategy. Both sensitivity and repeatability were optimized by experimental design techniques considering three factors: extraction temperature (from 50°C to 70°C, time of exposition of the fiber (from 20 min to 60 min, and amount of salt added (from 0 to 27.50%. Each experiment was evaluated by Principal Component Analysis (PCA that allows to take into consideration all the analytes at the same time, preserving the information about their different characteristics. Optimal extraction conditions were identified independently for signal intensity (extraction temperature: 70°C; extraction time: 60 min; salt percentage: 27.50% w/w and repeatability (extraction temperature: 50°C; extraction time: 60 min; salt percentage: 27.50% w/w and a final global compromise (extraction temperature: 70°C; extraction time: 60 min; salt percentage: 27.50% w/w was also reached. Considerations about the choice of the best internal standards were also drawn. The whole optimized procedure was than applied to the analysis of a multiflower honey sample and more than 100 compounds were identified.

  1. Comparison of common components analysis with principal components analysis and independent components analysis: Application to SPME-GC-MS volatolomic signatures.

    Science.gov (United States)

    Bouhlel, Jihéne; Jouan-Rimbaud Bouveresse, Delphine; Abouelkaram, Said; Baéza, Elisabeth; Jondreville, Catherine; Travel, Angélique; Ratel, Jérémy; Engel, Erwan; Rutledge, Douglas N

    2018-02-01

    The aim of this work is to compare a novel exploratory chemometrics method, Common Components Analysis (CCA), with Principal Components Analysis (PCA) and Independent Components Analysis (ICA). CCA consists in adapting the multi-block statistical method known as Common Components and Specific Weights Analysis (CCSWA or ComDim) by applying it to a single data matrix, with one variable per block. As an application, the three methods were applied to SPME-GC-MS volatolomic signatures of livers in an attempt to reveal volatile organic compounds (VOCs) markers of chicken exposure to different types of micropollutants. An application of CCA to the initial SPME-GC-MS data revealed a drift in the sample Scores along CC2, as a function of injection order, probably resulting from time-related evolution in the instrument. This drift was eliminated by orthogonalization of the data set with respect to CC2, and the resulting data are used as the orthogonalized data input into each of the three methods. Since the first step in CCA is to norm-scale all the variables, preliminary data scaling has no effect on the results, so that CCA was applied only to orthogonalized SPME-GC-MS data, while, PCA and ICA were applied to the "orthogonalized", "orthogonalized and Pareto-scaled", and "orthogonalized and autoscaled" data. The comparison showed that PCA results were highly dependent on the scaling of variables, contrary to ICA where the data scaling did not have a strong influence. Nevertheless, for both PCA and ICA the clearest separations of exposed groups were obtained after autoscaling of variables. The main part of this work was to compare the CCA results using the orthogonalized data with those obtained with PCA and ICA applied to orthogonalized and autoscaled variables. The clearest separations of exposed chicken groups were obtained by CCA. CCA Loadings also clearly identified the variables contributing most to the Common Components giving separations. The PCA Loadings did not

  2. Headspace solid phase microextraction--GC/C-IRMS for delta13CVPDB measurements of mono-aromatic hydrocarbons using EA-IRMS calibration.

    Science.gov (United States)

    Ebongué, Véronique Woule; Geypens, Benny; Berglund, Michael; Taylor, Philip

    2009-03-01

    This work aims at comparing the delta(13)C(VPDB) of mono-aromatic hydrocarbons benzene, toluene, ethylbenzene and xylene isomers (BTEX) measured by elemental analyser (EA)-isotope ratio mass spectrometer (IRMS) with the delta(13)C(VPDB) measured on the same compounds by headspace solid phase microextraction - GC/C-IRMS (hSPME - GC/C-IRMS) with the final goal of using these compounds as internal standards on the latter system. The EA-IRMS measurements were done using calcium and lithium carbonate isotopic reference materials: NBS19 and L-SVEC for establishing the delta(13)C(VPDB) scale. The EA-IRMS measurements with helium dilution of a set of five reference materials (USGS40, USGS41, IAEA-CH-6, IAEA-CH-3 and IAEA-601) show systematic bias of 1 per thousand relative to their assigned values. This bias due to the dilution mechanism in the used ConfloII interface device could not be avoided. As the selected hydrocarbons: BTEX could not be analysed by EA-IRMS without helium dilution, their delta(13)C(VPDB) must be corrected from this observed bias using an external calibration. The CO(2) gas calibrated using EA-IRMS without helium dilution, was used as an in-house reference for the delta(13)C(VPDB) measurements of the BTEX by the hSPME - GC/C-IRMS system. The comparison made between the delta(13)C(VPDB) measured on the same BTEX compounds by EA-IRMS (with external calibration) and by hSPME - GC/C-IRMS techniques showed good agreement.

  3. Use of passive samplers for improving oil toxicity and spill effects assessment

    International Nuclear Information System (INIS)

    Letinski, Daniel; Parkerton, Thomas; Redman, Aaron; Manning, Ryan; Bragin, Gail; Febbo, Eric; Palandro, David; Nedwed, Tim

    2014-01-01

    Highlights: • Methods to quantify dissolved hydrocarbons needed to link oil exposures to toxicity. • Solid phase microextraction (SPME) fibers used to measure dissolved hydrocarbons. • SPME results reliably predicted acute toxicity for range of dispersed oils. • Oil droplets and chemical dispersant did not significantly contribute to toxicity. • SPME analysis improves oil exposure assessment in lab and field studies. - Abstract: Methods that quantify dissolved hydrocarbons are needed to link oil exposures to toxicity. Solid phase microextraction (SPME) fibers can serve this purpose. If fibers are equilibrated with oiled water, dissolved hydrocarbons partition to and are concentrated on the fiber. The absorbed concentration (C polymer ) can be quantified by thermal desorption using GC/FID. Further, given that the site of toxic action is hypothesized as biota lipid and partitioning of hydrocarbons to lipid and fibers is well correlated, C polymer is hypothesized to be a surrogate for toxicity prediction. To test this method, toxicity data for physically and chemically dispersed oils were generated for shrimp, Americamysis bahia, and compared to test exposures characterized by C polymer . Results indicated that C polymer reliably predicted toxicity across oils and dispersions. To illustrate field application, SPME results are reported for oil spills at the Ohmsett facility. SPME fibers provide a practical tool to improve characterization of oil exposures and predict effects in future lab and field studies

  4. Estudio analítico de MTA-Angelus® y Biodentine® con técnicas SPME-GCMS y AFM

    OpenAIRE

    Díaz-Flores García, Víctor; Martínez Pérez, Lucía; Escribano Otero, Amparo; Kayali Sayadi, Nour

    2016-01-01

    Introducción: El objetivo del estudio fue obtener información analítica sobre la pureza química y homogeneidad de los materiales de uso endodóntico MTA-Angelus® y Biodentine®. Material y métodos: Se analizaron ambos materiales mediante la técnica de microextracción en fase sólida (SPME), combinada con cromatografía de gases acoplada a espectrómetro de masas (GC-MS) para separar e identificar los compuestos orgánicos volátiles (COVs) contenidos. Por otro lado, utilizando microscopía de f...

  5. HS-SPME-GC-MS/MS Method for the Rapid and Sensitive Quantitation of 2-Acetyl-1-pyrroline in Single Rice Kernels.

    Science.gov (United States)

    Hopfer, Helene; Jodari, Farman; Negre-Zakharov, Florence; Wylie, Phillip L; Ebeler, Susan E

    2016-05-25

    Demand for aromatic rice varieties (e.g., Basmati) is increasing in the US. Aromatic varieties typically have elevated levels of the aroma compound 2-acetyl-1-pyrroline (2AP). Due to its very low aroma threshold, analysis of 2AP provides a useful screening tool for rice breeders. Methods for 2AP analysis in rice should quantitate 2AP at or below sensory threshold level, avoid artifactual 2AP generation, and be able to analyze single rice kernels in cases where only small sample quantities are available (e.g., breeding trials). We combined headspace solid phase microextraction with gas chromatography tandem mass spectrometry (HS-SPME-GC-MS/MS) for analysis of 2AP, using an extraction temperature of 40 °C and a stable isotopologue as internal standard. 2AP calibrations were linear between the concentrations of 53 and 5380 pg/g, with detection limits below the sensory threshold of 2AP. Forty-eight aromatic and nonaromatic, milled rice samples from three harvest years were screened with the method for their 2AP content, and overall reproducibility, observed for all samples, ranged from 5% for experimental aromatic lines to 33% for nonaromatic lines.

  6. Measurement of positron range in matter in strong magnetic fields

    International Nuclear Information System (INIS)

    Hammer, B.E.; Christensen, N.L.

    1995-01-01

    Positron range is one factor that places a limitation on Positron Emission Tomography (PET) resolution. The distance a positron travels through matter before it annihilates with an electron is a function of its initial energy and the electron density of the medium. A strong magnetic field limits positron range when momentum components are transverse to the field. Measurement of positron range was determined by deconvolving the effects of detector response and radioactive distribution from the measured annihilation spread function. The annihilation spread function for a 0.5 mm bead of 68 Ga was measured with 0.2 and 1.0 mm wide slit collimators. Based on the annihilation spread function FWHM (Full Width at Half Maximum) for a 1.0 mm wide slit the median positron range in tissue equivalent material is 0.87, 0.50, 0.22 mm at 0, 5.0 and 9.4 T, respectively

  7. Coherent change detection and interferometric ISAR measurements in the folded compact range

    Energy Technology Data Exchange (ETDEWEB)

    Sorensen, K.W.

    1996-08-01

    A folded compact range configuration has been developed ant the Sandia National Laboratories` compact range antenna and radar-cross- section measurement facility as a means of performing indoor, environmentally-controlled, far-field simulations of synthetic aperture radar (SAR) measurements of distributed target samples (i.e. gravel, sand, etc.). The folded compact range configuration has previously been used to perform coherent-change-detection (CCD) measurements, which allow disturbances to distributed targets on the order of fractions of a wavelength to be detected. This report describes follow-on CCD measurements of other distributed target samples, and also investigates the sensitivity of the CCD measurement process to changes in the relative spatial location of the SAR sensor between observations of the target. Additionally, this report describes the theoretical and practical aspects of performing interferometric inverse-synthetic-aperture-radar (IFISAR) measurements in the folded compact range environment. IFISAR measurements provide resolution of the relative heights of targets with accuracies on the order of a wavelength. Several examples are given of digital height maps that have been generated from measurements performed at the folded compact range facility.

  8. An emittance measurement system for a wide range of bunch charges

    International Nuclear Information System (INIS)

    Dunham, B.; Engwall, D.; Hofler, A.; Keesee, M.; Legg, R.

    1997-01-01

    As a part of the emittance measurements planned for the FEL injector at the Thomas Jefferson National Accelerator Facility (Jefferson Lab), the authors have developed an emittance measurement system that covers the wide dynamic range of bunch charges necessary to fully characterize the high-DC-voltage photocathode gun. The measurements are carried out with a variant of the classical two-slit method using a slit to sample the beam in conjunction with a wire scanner to measure the transmitted beam profile. The use of commercial, ultra-low noise picoammeters makes it possible to cover the wide range of desired bunch charges, with the actual measurements made over the range of 0.25 pC to 125 pC. The entire system, including its integration into the EPICS control system, is discussed

  9. Analysis of enantiomeric and non-enantiomeric monoterpenes in plant emissions using portable dynamic air sampling/solid-phase microextraction (PDAS-SPME) and chiral gas chromatography/mass spectrometry

    Science.gov (United States)

    Yassaa, Noureddine; Williams, Jonathan

    A portable dynamic air sampler (PDAS) using a porous polymer solid-phase microextraction (SPME) fibre has been validated for the determination of biogenic enantiomeric and non-enantiomeric monoterpenes in air. These compounds were adsorbed in the field, and then thermally desorbed at 250 °C in a gas chromatograph injector port connected via a β-cyclodextrin capillary separating column to a mass spectrometer. The optimized method has been applied for investigating the emissions of enantiomeric monoterpenes from Pseudotsuga menziesii (Douglas-fir), Rosmarinus officinalis (Rosemary) and Lavandula lanata (Lavender) which were selected as representative of coniferous trees and aromatic plants, respectively. The enantiomers of α-pinene, sabinene, camphene, δ-3-carene, β-pinene, limonene, β-phellandrene, 4-carene and camphor were successfully determined in the emissions from the three plants. While Douglas-fir showed a strong predominance toward (-)-enantiomers, Rosemary and Lavender demonstrated a large variation in enantiomeric distribution of monoterpenes. The simplicity, rapidity and sensitivity of dynamic sampling with porous polymer coated SPME fibres coupled to chiral capillary gas chromatography/mass spectrometry (GC/MS) makes this method potentially useful for in-field investigations of atmosphere-biosphere interactions and studies of optically explicit atmospheric chemistry.

  10. Degradation product emission from historic and modern books by headspace SPME/GC-MS: evaluation of lipid oxidation and cellulose hydrolysis.

    Science.gov (United States)

    Clark, Andrew J; Calvillo, Jesse L; Roosa, Mark S; Green, David B; Ganske, Jane A

    2011-04-01

    Volatile organic compounds emitted from a several decade series of bound periodicals (1859-1939) printed on ground wood paper, as well as historical books dating from the 1500s to early 1800s made from cotton/linen rag, were studied using an improved headspace SPME/GC-MS method. The headspace over the naturally aging books, stored upright in glass chambers, was monitored over a 24-h period, enabling the identification of a wide range of organic compounds emanating from the whole of the book. The detection of particular straight chain aldehydes, as well as characteristic alcohols, alkenes and ketones is correlated with oxidative degradation of the C(18) fatty acid constituency of paper. The relative importance of hydrolytic and oxidative chemistry involved in paper aging in books published between 1560 and 1939 was examined by comparing the relative abundances of furfural (FUR) a known cellulose hydrolysis product, and straight chain aldehydes (SCA) produced from the oxidation of fatty acids in paper. The relative abundance of furfural is shown to increase across the 379-year publication time span. A comparison of relative SCA peak areas across the series of books examined reveals that SCA emission is more important in the cotton/linen rag books than in the ground wood books.

  11. Development of source range measurement instrument in Xi'an pulsed reactor

    CERN Document Server

    Wang Li

    2002-01-01

    Source range measurement instrument in Xi'an pulsed reactor is key equipment of low-side measuring in source range. At the same time, it is also weighty component of out-of-pile neutron-flux level observation system. The authors have done some researching and renovating based on the similar type devices used in nuclear reactor to improve the meter sensitivity, measuring range, noise proof features, reliability in running and maintainability which belong to the main performance index of the instrument. The design ideas, configurations, working principle, performance indexes, technique features and effect in utilizing are introduced briefly

  12. Assessment of Volatile Chemical Composition of the Essential Oil of Jatropha ribifolia (Pohl Baill by HS-SPME-GC-MS Using Different Fibers

    Directory of Open Access Journals (Sweden)

    Celia Eliane de Lara da Silva

    2013-01-01

    Full Text Available The chemical composition of essential oil and volatile obtained from the roots of Jatropha ribifolia (Pohl Baill was performed in this work. The Clevenger extractor was utilized in hydrodistillation of oil and chemical composition determined by gas chromatography coupled with mass spectrometry detector (GC-MS. The identification of compounds was confirmed by retention index (Kovats index obtained from a series of straight chain alkanes (C7–C30 and by comparison with NIST and ADAMS library. A total of 61 compounds were identified in essential oil by GC-MS. The extraction of volatile was performed also by the use of the solid phase microextraction (SPME with four different fibers. The essential oil extraction was extremely rapid (15 s to avoid saturation of the fiber and the MS detector. The majority of the composition of essential oil is the terpenes: β-pinene (major compound 9.16%, β-vatirene (8.34%, α-gurjunene (6.98%, α-pinene (6.35%, camphene (4.34%, tricyclene (3.79% and dehydro aromadendrene (3.52% it and aldehydes and alcohols. Through the SPME it was possible to determine the nine volatile compounds not identified in oil 2,3,4-trimethyl-2-cyclopenten-1-one, α-phellandrene, 3-carene, trans-p-mentha-2,8-dienol, pinocamphone, D-verbenon, 1,3,3-trimethyl-2-(2-methyl-cyclopropyl-cyclohexene, 2,4-diisocyanato-1-methylbenzene, and (6-hydroxymethyl-2,3-dimethylehenyl methanol.

  13. Otimização dos parâmetros de extração para determinação multiresíduo de pesticidas em amostras de água empregando microextração em fase sólida Parameter optimization for pesticide multiresidue determination using SPME in water samples

    Directory of Open Access Journals (Sweden)

    Emy Komatsu

    2004-10-01

    Full Text Available In this study the factors that affect the extraction of pesticide residues from water samples for their determination by solid-phase micro-extraction (SPME and GC/MS were optimized. The fiber polymer, the extraction mode, the ionic strength, the stirring rate, the pH and the extraction time were the most significant parameters evaluated. The recovery obtained with the proposed method ranged from 94 to 110% and the sensitivity of the method, determined by calculating the detection limit (DL, ranged from 0.004 to 0.1 mug l-1. The results obtained with spiked real samples, at the 0.1 mug l-1 level, showed acceptable conformity with the expected values.

  14. Measurement of natural carbon isotopic composition of acetone in human urine.

    Science.gov (United States)

    Yamada, Keita; Ohishi, Kazuki; Gilbert, Alexis; Akasaka, Mai; Yoshida, Naohiro; Yoshimura, Ryoko

    2016-02-01

    The natural carbon isotopic composition of acetone in urine was measured in healthy subjects using gas chromatography-combustion-isotope ratio mass spectrometry combined with headspace solid-phase microextraction (HS-SPME-GC-C-IRMS). Before applying the technique to a urine sample, we optimized the measurement conditions of HS-SPME-GC-C-IRMS using aqueous solutions of commercial acetone reagents. The optimization enabled us to determine the carbon isotopic compositions within ±0.2 ‰ of precision and ±0.3‰ of error using 0.05 or 0.2 mL of aqueous solutions with acetone concentrations of 0.3-121 mg/L. For several days, we monitored the carbon isotopic compositions and concentrations of acetone in urine from three subjects who lived a daily life with no restrictions. We also monitored one subject for 3 days including a fasting period of 24 h. These results suggest that changes in the availability of glucose in the liver are reflected in changes in the carbon isotopic compositions of urine acetone. Results demonstrate that carbon isotopic measurement of metabolites in human biological samples at natural abundance levels has great potential as a tool for detecting metabolic changes caused by changes in physiological states and disease.

  15. Spatial filtering velocimeter for vehicle navigation with extended measurement range

    Science.gov (United States)

    He, Xin; Zhou, Jian; Nie, Xiaoming; Long, Xingwu

    2015-05-01

    The idea of using spatial filtering velocimeter is proposed to provide accurate velocity information for vehicle autonomous navigation system. The presented spatial filtering velocimeter is based on a CMOS linear image sensor. The limited frame rate restricts high speed measurement of the vehicle. To extend measurement range of the velocimeter, a method of frequency shifting is put forward. Theoretical analysis shows that the frequency of output signal can be reduced and the measurement range can be doubled by this method when the shifting direction is set the same with that of image velocity. The approach of fast Fourier transform (FFT) is employed to obtain the power spectra of the spatially filtered signals. Because of limited frequency resolution of FFT, a frequency spectrum correction algorithm, called energy centrobaric correction, is used to improve the frequency resolution. The correction accuracy energy centrobaric correction is analyzed. Experiments are carried out to measure the moving surface of a conveyor belt. The experimental results show that the maximum measurable velocity is about 800deg/s without frequency shifting, 1600deg/s with frequency shifting, when the frame rate of the image is about 8117 Hz. Therefore, the measurement range is doubled by the method of frequency shifting. Furthermore, experiments were carried out to measure the vehicle velocity simultaneously using both the designed SFV and a laser Doppler velocimeter (LDV). The measurement results of the presented SFV are coincident with that of the LDV, but with bigger fluctuation. Therefore, it has the potential of application to vehicular autonomous navigation.

  16. Measurements of short-range ordering in Ni3Al

    International Nuclear Information System (INIS)

    Okamoto, J.K.; Ahn, C.C.

    1992-01-01

    This paper reports on extended electron energy-loss fine structure (EXELFS) that has been used to measure short-range ordering in Ni 3 Al. Films of fcc Ni 3 Al with suppressed short-range order synthesized by vacuum evaporation of Ni 3 Al onto room temperature substrates. EXELFS data were taken from both Al K and Ni L 23 edges. The development of short-range order was observed after the samples were annealed for various times at temperatures below 350 degrees C. Upon comparison with ab initio planewave EXELFS calculations, it was found that the Warren-Cowley short-range order parameter a(1nn) changed by about -0.1 after 210 minutes of annealing at 150 degrees C

  17. 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.

  18. Fingerprint of volatiles from plant extracts based on SPME-GC-MS

    Directory of Open Access Journals (Sweden)

    Ezequias P. Siqueira

    Full Text Available The Laboratory of Chemistry of Natural Products has an ex situ collection of extracts from organisms of the biodiversity aiming at bioprospecting. Nowadays the collection has about 4000 extracts from 1000 different species. Extracts are used to identify new bioactive compounds that could be useful for developing new drugs against neglected diseases like leishmaniosis, Chagas disease, malaria and tuberculosis. After biologic assays, the bioactive extracts need to be prepared in larger quantity to allow isolation and characterization of the bioactive component. At this time, it is important to not only confirm the bioactivity of new extract but also check if its composition is similar to the old one. It was evaluated the ability of Solid Phase Microextraction and Gas Chromatography-Mass Spectrometry analysis (SPME-GC-MS. It was used the AMDIS (Automatic Mass Spectral Deconvolution and Identification System software as tools to collect and to compare the chromatographic profiles of each extract (fingerprint. Forty six samples were analyzed, it was possible to infer from the composition of each sample and common compounds. Nine groups of samples, collected at different time, were analyzed and seasonal modifications between then could be elucidated. The results showed that this methodology can be used to monitor the composition of extracts, allowing to monitor chemical changes that may occur during storage periods and to investigate the occurrence of a determined component in different extracts.

  19. Range measurements of keV hydrogen ions in solid oxygen and carbon monoxide

    International Nuclear Information System (INIS)

    Schou, J.; Soerensen, H.; Andersen, H.H.; Nielsen, M.; Rune, J.

    1984-01-01

    Ranges of 1.3-3.5 keV/atom hydrogen and deuterium molecular ions have been measured by a thin-film reflection method. The technique, used here for range measurements in solid oxygen and carbon monoxide targets, is identical to the one used previously for range measurements in hydrogen and nitrogen. The main aim was to look for phase-effects, i.e. gas-solid differences in the stopping processes. While measured ranges in solid oxygen were in agreement with known gas data, the ranges in solid carbon monoxide were up to 50% larger than those calculated from gas-stopping data. The latter result agrees with that previously found for solid nitrogen. (orig.)

  20. HS-SPME GC/MS characterization of volatiles in raw and dry-roasted almonds (Prunus dulcis).

    Science.gov (United States)

    Xiao, Lu; Lee, Jihyun; Zhang, Gong; Ebeler, Susan E; Wickramasinghe, Niramani; Seiber, James; Mitchell, Alyson E

    2014-05-15

    A robust HS-SPME and GC/MS method was developed for analyzing the composition of volatiles in raw and dry-roasted almonds. Almonds were analyzed directly as ground almonds extracted at room temperature. In total, 58 volatiles were identified in raw and roasted almonds. Straight chain aldehydes and alcohols demonstrated significant but minimal increases, while the levels of branch-chain aldehydes, alcohols, heterocyclic and sulfur containing compounds increased significantly (500-fold) in response to roasting (palmonds) to 315.8±70.0 ng/g (averaged across the roasting treatments evaluated i.e. 28, 33 and 38 min at 138 °C) after roasting. Pyrazines were detected in only the roasted almonds, with the exception of 2,5-dimethylpyrazine, which was also found in raw almonds. The concentration of most alcohols increased in the roasted samples with the exception of 2-methyl-1-propanol, 3-methyl-1-butanol and 2-phenylethyl alcohol, which decreased 68%, 80%, and 86%, respectively. Copyright © 2013 Elsevier Ltd. All rights reserved.

  1. Application of HS-SPME-GC-MS method for the detection of active moulds on historical parchment.

    Science.gov (United States)

    Sawoszczuk, Tomasz; Syguła-Cholewińska, Justyna; Del Hoyo-Meléndez, Julio M

    2017-03-01

    The goal of this work was to analyse the profile of microbial volatile organic compounds (MVOCs) emitted by moulds growing on parchment samples, in search of particular volatiles mentioned in the literature as indicators of active mould growth. First, the growth of various moulds on samples of parchment was assessed. Those species that showed collagenolytic activity were then inoculated on two types of media: samples of parchment placed on media and on media containing amino acids that are elements of the structure of collagen. All samples were prepared inside 20-ml vials (closed system). In the first case, the media did not contain any sources of organic carbon, nitrogen, or sulphur, i.e. parchment was the only nutrient for the moulds. A third type of sample was historical parchment prepared in a Petri dish without a medium and inoculated with a collagenolytically active mould (open system). The MVOCs emitted by moulds were sampled with the headspace-SPME method. Volatiles extracted on DVB/CAR/PDMS fibres were analysed in a gas chromatography-mass spectrometry system. Qualitative and quantitative analyses of chromatograms were carried out in search of indicators of metabolic activity. The results showed that there are three groups of volatiles that can be used for the detection of active forms of moulds on parchment objects. To the best of our knowledge, this is the first work to measure MVOCs emitted by moulds growing on parchment.

  2. Characterization of fish sauce aroma-impact compounds using GC-MS, SPME-Osme-GCO, and Stevens' power law exponents.

    Science.gov (United States)

    Pham, A J; Schilling, M W; Yoon, Y; Kamadia, V V; Marshall, D L

    2008-05-01

    The objectives of this study were to characterize volatile compounds and to determine the characteristic aromas associated with impact compounds in 4 fish sauces using solid-phase micro-extraction, gas chromatography-mass spectrometry, Osme, and gas chromatography olfactometry (SPME-Osme-GCO) coupled with Stevens' Power Law. Compounds were separated using GCMS and GCO and were identified with the mass spectral database, aroma perceived at the sniffing port, retention indices, and verification of compounds by authentic standards in the GCMS and GCO. Aromas that were isolated and present in all 4 fish sauce samples at all concentrations included fishy (trimethylamine), pungent and dirty socks (combination of butanoic, pentanoic, hexanoic, and heptanoic acids), cooked rice and buttery popcorn (2,6-dimethyl pyrazine), and sweet and cotton candy (benzaldehyde). All fish sauces contained the same aromas as determined by GCO and GCMS (verified using authentic standard compounds), but the odor intensity associated with each compound or group of compounds was variable for different fish sauce samples. Stevens' Power Law exponents were also determined using this analytical technique, but exponents were not consistent for the same compounds that were found in all fish sauces. Stevens' Power Law exponents ranged from 0.14 to 0.37, 0.24 to 0.34, 0.09 to 0.21, and 0.10 to 0.35 for dirty socks, fishy, buttery popcorn, and sweet aromas, respectively. This demonstrates that there is variability in Stevens' Power Law exponents for odorants within fish sauce samples.

  3. Authenticity of raspberry flavor in food products using SPME-chiral-GC-MS.

    Science.gov (United States)

    Hansen, Anne-Mette S; Frandsen, Henrik L; Fromberg, Arvid

    2016-05-01

    A fast and simple method for authenticating raspberry flavors from food products was developed. The two enantiomers of the compound (E)-α-ionone from raspberry flavor were separated on a chiral gas chromatographic column. Based on the ratio of these two enantiomers, the naturalness of a raspberry flavor can be evaluated due to the fact that a natural flavor will consist almost exclusively of the R enantiomer, while a chemical synthesis of the same compound will result in a racemic mixture. Twenty-seven food products containing raspberry flavors where investigated using SPME-chiral-GC-MS. We found raspberry jam, dried raspberries, and sodas declared to contain natural aroma all contained almost only R-(E)-α-ionone supporting the content of natural raspberry aroma. Six out of eight sweets tested did not indicate a content of natural aroma on the labeling which was in agreement with the almost equal distribution of the R and S isomer. Two products were labeled to contain natural raspberry flavors but were found to contain almost equal amounts of both enantiomers indicating a presence of synthetic raspberry flavors only. Additionally, two products that were labeled to contain both raspberry juice and flavor showed equal amounts of both enantiomers, indicating the presence of synthetic flavor.

  4. 1H NMR and SPME-GC/MS study of hydrolysis, oxidation and other reactions occurring during in vitro digestion of non-oxidized and oxidized sunflower oil. Formation of hydroxy-octadecadienoates.

    Science.gov (United States)

    Nieva-Echevarría, Bárbara; Goicoechea, Encarnación; Manzanos, María J; Guillén, María D

    2017-01-01

    Both fresh and slightly oxidized sunflower oils, as models of omega-6 rich lipids, were submitted to in vitro gastrointestinal digestion and studied by 1 H NMR and SPME-GC/MS. Changes in lipolysis degree, lipid composition and oxidative level were studied by 1 H NMR. Three quantitative approaches were used and several equations were newly developed. In oxidized oil digestates slightly lower hydrolysis and a higher advance of oxidation took place during digestion. This latter was evidenced by a greater decrease of lipid unsaturation degree and enhanced generation of oxidation products (cis,trans-hydroperoxy-octadecadienoates, cis,trans- and trans,trans-hydroxy-octadecadienoates). For the first time, the generation of hydroxy-octadecadienoates during in vitro digestion is reported. Furthermore, SPME-GC/MS study of non-digested and digested samples headspaces confirmed that lipid oxidation occurred: abundances of volatile markers increased (including potentially toxic alpha,beta-unsaturated aldehydes), especially in oxidized oils digestates. Markers of Maillard-type and esterification reactions were also detected in the digestates. Copyright © 2016 Elsevier Ltd. All rights reserved.

  5. Oxidative Stress Biomarkers in Exhaled Breath of Workers Exposed to Crystalline Silica Dust by SPME-GC-MS.

    Science.gov (United States)

    Jalali, Mahdi; Zare Sakhvidi, Mohammad Javad; Bahrami, Abdulrahman; Berijani, Nima; Mahjub, Hussein

    2016-01-01

    Silicosis is considered an oxidative stress related disease that can lead to the development of lung cancer. In this study, our purpose was to analysis of volatile organic compounds (VOCs) in the exhaled breath of workers exposed to silica containing dust and compare peak area of these compounds with silicosis patients and healthy volunteers (smokers and nonsmokers) groups. In this cross sectional case-control study, the exhaled breath of 69 subjects including workers exposed to silica (n=20), silicosis patient (n=4), healthy non-smoker (n=20) and healthy smoker (n=25) were analyzed. We collected breath samples using 3-liter Tedlar bags. The VOCs were extracted with solid phase micro-extraction (SPME) and analyzed by gas chromatography-mass spectrometry (GC-MS). Personal exposure intensity was measured according to NIOSH 7601 method. Respiratory parameters were measured using spirometry. Seventy percent and 100% of the exposures to crystalline silica dust exceeded from 8 h TWA ACGIH TLVs in case and positive control groups, respectively. A significant negative correlation was found between dust exposure intensity and FEV1/FVC when exposure and positive control groups were studied in a group (r2=-0.601, P<0.001). Totally, forty VOCs were found in all exhaled breath samples. Among the VOCs, the mean of peak area acetaldehyde, hexanal, nonanal, decane, pentad cane, 2-propanol and 3-hydroxy-2-butanone were higher in exhaled breath of the workers exposed to silica and silicosis patient compared to the healthy smoker and nonsmoker controls. In some cases the difference was significant (P<0.05). The analysis of some VOCs in exhaled breath of subjects is appropriate biomarker to determine of exposure to silica.

  6. Preparation and evaluation of molecularly imprinted solid-phase micro-extraction fibers for selective extraction of phthalates in an aqueous sample

    International Nuclear Information System (INIS)

    He Juan; Lv Ruihe; Zhan Haijun; Wang Huizhi; Cheng Jie; Lu Kui; Wang Fengcheng

    2010-01-01

    A novel molecularly imprinted polymer (MIP) that was applied to a solid-phase micro-extraction (SPME) device, which could be coupled directly to gas chromatograph and mass spectrometer (GC/MS), was prepared using dibutyl phthalate (DBP) as the template molecule. The characteristics and application of this fiber were investigated. Electron microscope images indicated that the MIP-coated solid-phase micro-extraction (MI-SPME) fibers were homogeneous and porous. The extraction yield of DBP with the MI-SPME fibers was higher than that of the non-imprinted polymer (NIP)-coated SPME (NI-SPME) fibers. The MI-SPME fibers had a higher selectivity to other phthalates that had similar structures as DBP. A method was developed for the determination of phthalates using MI-SPME fibers coupled with GC/MS. The extraction conditions were optimized. Detection limits for the phthalate samples were within the range of 2.17-20.84 ng L -1 . The method was applied to five kinds of phthalates dissolved in spiked aqueous samples and resulted in recoveries of up to 94.54-105.34%, respectively. Thus, the MI-SPME fibers are suitable for the extraction of trace phthalates in complicated samples.

  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. Smartphone photography utilized to measure wrist range of motion.

    Science.gov (United States)

    Wagner, Eric R; Conti Mica, Megan; Shin, Alexander Y

    2018-02-01

    The purpose was to determine if smartphone photography is a reliable tool in measuring wrist movement. Smartphones were used to take digital photos of both wrists in 32 normal participants (64 wrists) at extremes of wrist motion. The smartphone measurements were compared with clinical goniometry measurements. There was a very high correlation between the clinical goniometry and smartphone measurements, as the concordance coefficients were high for radial deviation, ulnar deviation, wrist extension and wrist flexion. The Pearson coefficients also demonstrated the high precision of the smartphone measurements. The Bland-Altman plots demonstrated 29-31 of 32 smartphone measurements were within the 95% confidence interval of the clinical measurements for all positions of the wrists. There was high reliability between the photography taken by the volunteer and researcher, as well as high inter-observer reliability. Smartphone digital photography is a reliable and accurate tool for measuring wrist range of motion. II.

  9. MTF measurement of IR optics in different temperature ranges

    Science.gov (United States)

    Bai, Alexander; Duncker, Hannes; Dumitrescu, Eugen

    2017-10-01

    Infrared (IR) optical systems are at the core of many military, civilian and manufacturing applications and perform mission critical functions. To reliably fulfill the demanding requirements imposed on today's high performance IR optics, highly accurate, reproducible and fast lens testing is of crucial importance. Testing the optical performance within different temperature ranges becomes key in many military applications. Due to highly complex IR-Applications in the fields of aerospace, military and automotive industries, MTF Measurement under realistic environmental conditions become more and more relevant. A Modulation Transfer Function (MTF) test bench with an integrated thermal chamber allows measuring several sample sizes in a temperature range from -40 °C to +120°C. To reach reliable measurement results under these difficult conditions, a specially developed temperature stable design including an insulating vacuum are used. The main function of this instrument is the measurement of the MTF both on- and off-axis at up to +/-70° field angle, as well as measurement of effective focal length, flange focal length and distortion. The vertical configuration of the system guarantees a small overall footprint. By integrating a high-resolution IR camera with focal plane array (FPA) in the detection unit, time consuming measurement procedures such as scanning slit with liquid nitrogen cooled detectors can be avoided. The specified absolute accuracy of +/- 3% MTF is validated using internationally traceable reference optics. Together with a complete and intuitive software solution, this makes the instrument a turn-key device for today's state-of- the-art optical testing.

  10. Lifetime measurements in the picosecond range: Achievements and Perspectives

    International Nuclear Information System (INIS)

    Kruecken, Reiner

    1999-01-01

    This contribution will review the recoil distance method (RDM), its current range of applications as well as future perspectives for the measurement of lifetimes in the picosecond range of excited nuclear levels. Recent Doppler-shift lifetime experiments with large gamma-ray spectrometers have achieved a new level of precision and sensitivity, providing new insights into nuclear structure physics. High precision RDM measurements of near-yrast states in various mass regions have revealed dynamic shape effects beyond the framework of collective models and have also allowed to study the interaction between coexisting shapes. The measurement of lifetimes in superdeformed bands has shown that lifetimes can be measured for nuclear excitations, which are only populated with a few percent of the production cross-section of a nucleus. These experiments have also enabled us to study the mechanism of the decay-out of superdeformed bands. Another example for the need of precise lifetime measurements is the recent verifications of the concept of 'magnetic rotation' in nuclei by the experimental observation of the characteristic drop of B(M1) values as a function of angular momentum. These recent breakthroughs have also opened new perspectives for the use of the RDM technique for more exotic regions of nuclei and nuclear excitations. Here the measurement of lifetimes in neutron rich nuclei, which are not accessible with conventional nuclear reactions using stable beams and targets, is of special interest. Possible experimental approaches and simple estimates for the feasibility of such experiments will be presented. (author)

  11. The Development of a Tactical-Level Full Range Leadership Measurement Instrument

    Science.gov (United States)

    2010-03-01

    full range leadership theory has become established as the predominant and most widely researched theory on leadership . The most commonly used survey...instrument to assess full range leadership theory is the Multifactor Leadership Questionnaire, originally developed by Bass in 1985. Although much...existing literature to develop a new full range leadership theory measurement instrument that effectively targets low- to mid-level supervisors, or

  12. High-temperature absorbed dose measurements in the megagray range

    International Nuclear Information System (INIS)

    Balian, P.; Ardonceau, J.; Zuppiroli, L.

    1988-01-01

    Organic conductors of the tetraselenotetracene family have been tested as ''high-temperature'' absorbed dose dosimeters. They were heated up to 120 0 C and irradiated at this temperature with 1-MeV electrons in order to simulate, in a short time, a much longer γ-ray irradiation. The electric resistance increase of the crystal can be considered a good measurement of the absorbed dose in the range 10 6 Gy to a few 10 8 Gy and presumably one order of magnitude more. This dosimeter also permits on-line (in-situ) measurements of the absorbed dose without removing the sensor from the irradiation site. The respective advantages of organic and inorganic dosimeters at these temperature and dose ranges are also discussed. In this connection, we outline new, but negative, results concerning the possible use of silica as a high-temperature, high-dose dosimeter. (author)

  13. Optimisation and validation of a HS-SPME-GC-IT/MS method for analysis of carbonyl volatile compounds as biomarkers in human urine: Application in a pilot study to discriminate individuals with smoking habits.

    Science.gov (United States)

    Calejo, Isabel; Moreira, Nathalie; Araújo, Ana Margarida; Carvalho, Márcia; Bastos, Maria de Lourdes; de Pinho, Paula Guedes

    2016-02-01

    A new and simple analytical approach consisting of an automated headspace solid-phase microextraction (HS-SPME) sampler coupled to gas chromatography-ion trap/mass spectrometry detection (GC-IT/MS) with a prior derivatization step with O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine hydrochloride (PFBHA) was developed to detect volatile carbonyl metabolites with low molecular weights in human urine. A central composite design (CCD) was used to optimise the PFBHA concentration and extraction conditions that affect the efficiency of the SPME procedure. With a sample volume of 1 mL, optimal conditions were achieved by adding 300 mg/L of PFBHA and allowing the sample to equilibrate for 6 min at 62°C and then extracting the samples for 51 min at the same temperature, using a divinylbenzene/polydimethylsiloxane (DVB/PDMS) fibre. The method allowed the simultaneous identification and quantification of 44 carbonyl compounds consisting of aldehydes, dialdehydes, heterocyclic aldehydes and ketones. The method was validated with regards to the linearity, inter- and intra-day precision and accuracy. The detection limits ranged from 0.009 to 0.942 ng/mL, except for 4-hydroxy-2-nonenal (15 ng/mL), and the quantification limits varied from 0.029 to 1.66 ng/mL, except for butanal (2.78 ng/mL), 2-butanone (2.67 ng/mL), 4-heptanone (3.14 ng/mL) and 4-hydroxy-2-nonenal (50.0 ng/mL). The method accuracy was satisfactory, with recoveries ranging from 90 to 107%. The proof of applicability of the methodology was performed in a pilot target analysis of urine samples obtained from 18 healthy smokers and 18 healthy non-smokers (control group). Chemometric supervised analysis was performed using the volatile patterns acquired for these samples and clearly showed the potential of the volatile carbonyl profiles to discriminate urine from smoker and non-smoker subjects. 5-Methyl-2-furfural (p<0.0001), 2-methylpropanal, nonanal and 2-methylbutanal (p<0.05) were identified as potentially useful

  14. An overview of Broadband Laser Ranging Architecture and Measurement Considerations

    Science.gov (United States)

    Daykin, Edward; La Lone, Brandon; Miller, Edward; Younk, Patrick; Bennett, Corey; Catenacci, Jared; LLNL BLR Development Group Collaboration; LANL BLR Development Group Collaboration

    2017-06-01

    Broadband Laser Ranging (BLR) is a developmental diagnostic intended to measure the position of rapidly moving surfaces in combination with optical velocimetry. Design and employment of a BLR diagnostic on dynamic experiments requires consideration for both the inherent measurement system tradeoffs as well as architectural choices appropriate to the nature of investigation. The diagnostic uses spectral interferometry to measure distance by mapping femtosecond laser pulses to the time domain via chromatic dispersion within the fiber-optic architecture. The system parameters and governing equations that describe measurement range, resolution, and Doppler sensitivity will be discussed. We will also briefly review the impact of diagnostic architectural choices including: nature of interferometer, Interferometric dispersion matching, optical amplification, integration of optical velocimetry, BLR calibration, and field operability. To summarize we will present the architectural and operational approach currently being pursued by NSTec within an on-going collaboration between NSTec, Lawrence Livermore and Los Alamos National Labs. This work was done by National Security Technologies, LLC, under Contract No. DE-AC52-06NA25946 with the U.S. Department of Energy.

  15. Study of flavour compounds from orange juices by HS-SPME and GC-MS

    Science.gov (United States)

    Schmutzer, G.; Avram, V.; Covaciu, F.; Feher, I.; Magdas, A.; David, L.; Moldovan, Z.

    2013-11-01

    The flavour of the orange juices, which gives the taste and odour of the product, is an important criterion about the products quality for consumers. A fresh single strength and two commercial orange juices (obtained from concentrate) flavour profile were studied using a selective and sensitive gas chromatography - mass spectrometry (GC-MS) analytical system, after a solvent free, single step preconcentration and extraction technique, the headspace solid phase microextraction (HP-SPME). In the studied orange juices 55 flavour compounds were detected and classified as belonging to the esters, alcohols, ketones, monoterpenes and sesquiterpenes chemical families. The fresh single strength orange juice was characterized by high amount of esters, monoterpenes and sesquiterpenes. Limonene and valencene were the most abundant flavours in this fresh natural orange juice. Alcohols and ketones were found in higher concentration in the commercial orange juices made from concentrate, than in the single strength products. Nevertheless, in commercial juices the most abundant flavour was limonene and α-terpineol. The results highlight clear differences between fresh singles strength orange juice and juice from concentrate. The orange juices reconstructed from concentrate, made in Romania, present low quantity of flavour compounds, suggesting the absence or a low rearomatization process, but extraneous components were not detected.

  16. Optimization of biological and instrumental detection of explosives and ignitable liquid residues including canines, SPME/ITMS and GC/MSn

    Science.gov (United States)

    Furton, Kenneth G.; Harper, Ross J.; Perr, Jeannette M.; Almirall, Jose R.

    2003-09-01

    A comprehensive study and comparison is underway using biological detectors and instrumental methods for the rapid detection of ignitable liquid residues (ILR) and high explosives. Headspace solid phase microextraction (SPME) has been demonstrated to be an effective sampling method helping to identify active odor signature chemicals used by detector dogs to locate forensic specimens as well as a rapid pre-concentration technique prior to instrumental detection. Common ignitable liquids and common military and industrial explosives have been studied including trinitrotoluene, tetryl, RDX, HMX, EGDN, PETN and nitroglycerine. This study focuses on identifying volatile odor signature chemicals present, which can be used to enhance the level and reliability of detection of ILR and explosives by canines and instrumental methods. While most instrumental methods currently in use focus on particles and on parent organic compounds, which are often involatile, characteristic volatile organics are generally also present and can be exploited to enhance detection particularly for well-concealed devices. Specific examples include the volatile odor chemicals 2-ethyl-1-hexanol and cyclohexanone, which are readily available in the headspace of the high explosive composition C-4; whereas, the active chemical cyclo-1,3,5-trimethylene-2,4,6-trinitramine (RDX) is not. The analysis and identification of these headspace 'fingerprint' organics is followed by double-blind dog trials of the individual components using certified teams in an attempt to isolate and understand the target compounds to which dogs are sensitive. Studies to compare commonly used training aids with the actual target explosive have also been undertaken to determine their suitability and effectiveness. The optimization of solid phase microextraction (SPME) combined with ion trap mobility spectrometry (ITMS) and gas chromatography/mass spectrometry/mass spectrometry (GC/MSn) is detailed including interface development

  17. Odor Profile of Different Varieties of Extra-Virgin Olive Oil During Deep Frying Using an Electronic Nose and SPME-GC-FID

    Science.gov (United States)

    Messina, Valeria; Biolatto, Andrea; Sancho, Ana; Descalzo, Adriana; Grigioni, Gabriela; de Reca, Noemí Walsöe

    2011-09-01

    The aim of the performed work was to evaluate with an electronic nose changes in odor profile of Arauco and Arbequina varieties of extra-virgin olive oil during deep-frying. Changes in odor were analyzed using an electronic nose composed of 16 sensors. Volatile compounds were analyzed by SPME-GC-FID. Principal Component Analysis was applied for electronic results. Arauco variety showed the highest response for sensors. Statistical analysis for volatile compounds indicated a significant (P<0.001) interaction between variety and time of frying processes. Arauco variety showed the highest production of volatile compounds at 60 min of deep frying. The two varieties presented distinct patterns of volatile products, being clearly identified with the electronic nose.

  18. Broadband Laser Ranging for Position Measurements in Shock Physics Experiments

    Science.gov (United States)

    Rhodes, Michelle; Bennett, Corey; Daykin, Edward; Younk, Patrick; Lalone, Brandon; Kostinski, Natalie

    2017-06-01

    Broadband laser ranging (BLR) is a recently developed measurement system that provides an attractive option for determining the position of shock-driven surfaces. This system uses broadband, picosecond (or femtosecond) laser pulses and a fiber interferometer to measure relative travel time to a target and to a reference mirror. The difference in travel time produces a delay difference between pulse replicas that creates a spectral beat frequency. The spectral beating is recorded in real time using a dispersive Fourier transform and an oscilloscope. BLR systems have been designed that measure position at 12.5-40 MHz with better than 100 micron accuracy over ranges greater than 10 cm. We will give an overview of the basic operating principles of these systems. Prepared by LLNL under Contract DE-AC52-07NA27344, by LANL under Contract DE-AC52-06NA25396, and by NSTec Contract DE-AC52-06NA25946.

  19. Characterisation of volatile profiles in 50 native Peruvian chili pepper using solid phase microextraction-gas chromatography mass spectrometry (SPME-GCMS).

    Science.gov (United States)

    Patel, Kirti; Ruiz, Candy; Calderon, Rosa; Marcelo, Mavel; Rojas, Rosario

    2016-11-01

    The volatiles were characterised by headspace solid phase micro extraction (HS-SPME), gas chromatography mass spectrometry (GC-FID/MS). A total of 127 compounds were identified with terpenes (including mono terpenes and sesquiterpenes - a total of 45 compounds), esters (31 compounds) and hydrocarbons (20 compounds) were the predominant volatile compounds. Principal component analysis (PCA) of the volatile compounds yielded 2 significant PC's, which together accounted for 90.3% of the total variance in the data set and the scatter plot generated between PC1 and PC2 successfully segregated the 50 chili pepper samples into 7 groups. Clusters of hydrocarbons, esters, terpenes, aldehyde and ketones formed the major determinants of the difference. Copyright © 2016 Elsevier Ltd. All rights reserved.

  20. Microextraction by Packed Sorbent (MEPS and Solid-Phase Microextraction (SPME as Sample Preparation Procedures for the Metabolomic Profiling of Urine

    Directory of Open Access Journals (Sweden)

    Catarina Silva

    2014-01-01

    Full Text Available For a long time, sample preparation was unrecognized as a critical issue in the analytical methodology, thus limiting the performance that could be achieved. However, the improvement of microextraction techniques, particularly microextraction by packed sorbent (MEPS and solid-phase microextraction (SPME, completely modified this scenario by introducing unprecedented control over this process. Urine is a biological fluid that is very interesting for metabolomics studies, allowing human health and disease characterization in a minimally invasive form. In this manuscript, we will critically review the most relevant and promising works in this field, highlighting how the metabolomic profiling of urine can be an extremely valuable tool for the early diagnosis of highly prevalent diseases, such as cardiovascular, oncologic and neurodegenerative ones.

  1. Small Device For Short-Range Antenna Measurements Using Optics

    DEFF Research Database (Denmark)

    Yanakiev, Boyan Radkov; Nielsen, Jesper Ødum; Christensen, Morten

    2011-01-01

    This paper gives a practical solution for implementing an antenna radiation pattern measurement device using optical fibers. It is suitable for anechoic chambers as well as short range channel sounding. The device is optimized for small size and provides a cheap and easy way to make optical antenna...

  2. Methodical evaluation and improvement of matrix compatible PDMS-overcoated coating for direct immersion solid phase microextraction gas chromatography (DI-SPME-GC)-based applications.

    Science.gov (United States)

    Souza-Silva, Érica A; Gionfriddo, Emanuela; Shirey, Robert; Sidisky, Len; Pawliszyn, Janusz

    2016-05-12

    The main quest for the implementation of direct SPME to complex matrices has been the development of matrix compatible coatings that provide sufficient sensitivity towards the target analytes. In this context, we present here a thorough evaluation of PDMS-overcoated fibers suitable for simultaneous extraction of different polarities analytes, while maintaining adequate matrix compatibility. For this, eleven analytes were selected, from various application classes (pesticides, industrial chemicals and pharmaceuticals) and with a wide range of log P values (ranging from 1.43 to 6). The model matrix chosen was commercial Concord grape juice, which is rich in pigments such as anthocyanins, and contains approximately 20% of sugar (w/w). Two types of PDMS, as well as other intrinsic factors associated with the PDMS-overcoated fiber fabrication are studied. The evaluation showed that the PDMS-overcoated fibers considerably slowed down the coating fouling process during direct immersion in complex matrices of high sugar content. Longevity differences could be seen between the two types of PDMS tested, with a proprietary Sylgard(®) giving superior performance because of lesser amount of reactive groups and enhanced hydrophobicity. Conversely, the thickness of the outer layer did not seem to have a significant effect on the fiber lifetime. We also demonstrate that the uniformity of the overcoated PDMS layer is paramount to the achievement of reliable data and extended fiber lifetime. Employing the optimum overcoated fiber, limits of detection (LOD) in the range of 0.2-1.3 ng/g could be achieved. Additional improvement is attainable by introducing washing of the coatings after desorption, so that any carbon build-up (fouling) left on the coating surface after thermal desorption can be removed. Copyright © 2016 Elsevier B.V. All rights reserved.

  3. Second Order Kinetic Modeling of Headspace Solid Phase Microextraction of Flavors Released from Selected Food Model Systems

    Directory of Open Access Journals (Sweden)

    Jiyuan Zhang

    2014-09-01

    Full Text Available The application of headspace-solid phase microextraction (HS-SPME has been widely used in various fields as a simple and versatile method, yet challenging in quantification. In order to improve the reproducibility in quantification, a mathematical model with its root in psychological modeling and chemical reactor modeling was developed, describing the kinetic behavior of aroma active compounds extracted by SPME from two different food model systems, i.e., a semi-solid food and a liquid food. The model accounted for both adsorption and release of the analytes from SPME fiber, which occurred simultaneously but were counter-directed. The model had four parameters and their estimated values were found to be more reproducible than the direct measurement of the compounds themselves by instrumental analysis. With the relative standard deviations (RSD of each parameter less than 5% and root mean square error (RMSE less than 0.15, the model was proved to be a robust one in estimating the release of a wide range of low molecular weight acetates at three environmental temperatures i.e., 30, 40 and 60 °C. More insights of SPME behavior regarding the small molecule analytes were also obtained through the kinetic parameters and the model itself.

  4. Measured long-range repulsive Casimir-Lifshitz forces.

    Science.gov (United States)

    Munday, J N; Capasso, Federico; Parsegian, V Adrian

    2009-01-08

    Quantum fluctuations create intermolecular forces that pervade macroscopic bodies. At molecular separations of a few nanometres or less, these interactions are the familiar van der Waals forces. However, as recognized in the theories of Casimir, Polder and Lifshitz, at larger distances and between macroscopic condensed media they reveal retardation effects associated with the finite speed of light. Although these long-range forces exist within all matter, only attractive interactions have so far been measured between material bodies. Here we show experimentally that, in accord with theoretical prediction, the sign of the force can be changed from attractive to repulsive by suitable choice of interacting materials immersed in a fluid. The measured repulsive interaction is found to be weaker than the attractive. However, in both cases the magnitude of the force increases with decreasing surface separation. Repulsive Casimir-Lifshitz forces could allow quantum levitation of objects in a fluid and lead to a new class of switchable nanoscale devices with ultra-low static friction.

  5. The Use of Headspace Solid-Phase Microextraction (HS-SPME to Assess the Quality and Stability of Fruit Products: An Example Using Red Mombin Pulp (Spondias purpurea L.

    Directory of Open Access Journals (Sweden)

    Katieli Martins Todisco

    2014-10-01

    Full Text Available The present study aimed to evaluate the volatiles profile of red mombin (Spondias purpurea pulp and its powder produced by spray-drying (SD as an example to show utility of headspace solid-phase microextraction (HS-SPME in the analysis of parameters such as the quality and stability of fruit products. Volatiles profiles of the pulp were identified by gas chromatography-mass spectrometry (GC-MS, quantified by gas chromatography-flame ionization detector (GC-FID and compared to the profile of the powder stored at 0, 60 and 120 days in plastic (PP or laminated packages (LP. The results showed that the technique was able to identify 36 compounds in the red mombin pulp, 17 out of which have been described for the first time in this fruit, showing that red mombin fresh pulp appears to be unique in terms of volatiles composition. However, only 24 compounds were detected in the powder. This decrease is highly correlated (r2 = 0.99, at least for the majority of compounds, to the degree of volatility of compounds. Furthermore, the powder stored in PP or LP showed no statistical differences in the amounts of its components for a period of 120 days of storage. Finally, this work shows how HS-SPME analysis can be a valuable tool to assess the quality and stability of fruit products.

  6. Development of an SPME-GC-MS method for the specific quantification of dimethylamine and trimethylamine: use of a new ratio for the freshness monitoring of cod fillets.

    Science.gov (United States)

    Dehaut, Alexandre; Duthen, Simon; Grard, Thierry; Krzewinski, Frédéric; N'Guessan, Assi; Brisabois, Anne; Duflos, Guillaume

    2016-08-01

    Fish is a highly perishable food, so it is important to be able to estimate its freshness to ensure optimum quality for consumers. The present study describes the development of an SPME-GC-MS technique capable of quantifying both trimethylamine (TMA) and dimethylamine (DMA), components of what has been defined as partial volatile basic nitrogen (PVB-N). This method was used, together with other reference methods, to monitor the storage of cod fillets (Gadus morhua) conserved under melting ice. Careful optimisation enabled definition of the best parameters for extracting and separating targeted amines and an internal standard. The study of cod spoilage by sensory analysis and TVB-N assay led to the conclusion that the shelf-life of cod fillet was between 6 and 7 days. Throughout the study, TMA and DMA were specifically quantified by SPME-GC-MS; the first was found to be highly correlated with the values returned by steam distillation assays. Neither TMA-N nor DMA-N were able to successfully characterise the decrease in early freshness, unlike dimethylamine/trimethylamine ratio (DTR), whose evolution is closely related to the results of sensory analysis until the stage where fillets need to be rejected. DTR was proposed as a reliable indicator for the early decrease of freshness until fish rejection. © 2015 Society of Chemical Industry. © 2015 Society of Chemical Industry.

  7. Comprehensive Measurement of Atmospheric Aerosols with a Wide Range Aerosol Spectrometer

    International Nuclear Information System (INIS)

    Keck, L; Pesch, M; Grimm, H

    2011-01-01

    A wide range aerosol spectrometer (WRAS) was used for comprehensive long term measurements of aerosol size distributions. The system combines the results of an optical aerosol spectrometer with the results of a Scanning Mobility Particle Sizer (SMPS) to record essentially the full size range (5 nm - 32 μm) of atmospheric particles in 72 channels. Measurements were carried out over one year (2009) at the Global Atmospheric Watch (GAW)-Station Hohenpeissenberg, Bavaria. Total particle number concentrations obtained from the aerosol size distributions were compared to the total number concentrations measured by a Condensation Particle Counter (CPC). The comparison showed an excellent agreement of the data. The high time resolution of 5 minutes allows the combination of the measured size distributions with meteorological data and correlations to gaseous pollutants (CO, NOx and SO2). A good correlation of particle number and CO concentrations was found for long distance transported small particles, which were probably mainly soot particles. Correlations to NOx were observed for aerosols from local sources such as traffic emissions. The formation of secondary aerosols from gaseous precursors was also observed. Episodes of relatively high concentration of particles in the range of 2-3 μm were probably caused by pollen.

  8. Expanding the dynamic measurement range for polymeric nanoparticle pH sensors

    DEFF Research Database (Denmark)

    Sun, Honghao; Almdal, Kristoffer; Andresen, Thomas Lars

    2011-01-01

    Conventional optical nanoparticle pH sensors that are designed for ratiometric measurements in cells have been based on utilizing one sensor fluorophore and one reference fluorophore in each nanoparticle, which results in a relatively narrow dynamic measurement range. This results in substantial...

  9. NMR, HS-SPME-GC/MS, and HPLC/MSn Analyses of Phytoconstituents and Aroma Profile of Rosmarinus eriocalyx.

    Science.gov (United States)

    Bendif, Hamdi; Miara, Mohamed Djamel; Peron, Gregorio; Sut, Stefania; Dall'Acqua, Stefano; Flamini, Guido; Maggi, Filippo

    2017-10-01

    In this work, a comprehensive study on the chemical constituents of the aerial parts of Rosmarinus eriocalyx (Lamiaceae), an aromatic shrub traditionally consumed as a food and herbal remedy in Algeria, is presented. The aroma profile was analysed by headspace solid phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC/MS), whereas the crude extract constituents were analyzed by 1 H-NMR and by high performance liquid chromatography coupled with mass spectrometry (HPLC/MS n ). Thirty-nine volatile compounds, most of them being monoterpenes, have been identified, with camphor, camphene, and α-pinene as the most abundant constituents. 1 H-NMR analysis revealed the presence of phenolic compounds and betulinic acid while HPLC/MS n allowed the identification of glycosilated and aglyconic flavonoids as well as phenylpropanoid derivatives. Some of these constituents, namely as betulinic acid, rosmanol, and cirsimaritin were reported for the first time in R. eriocalyx. © 2017 Wiley-VHCA AG, Zurich, Switzerland.

  10. Calibration Standards for Surface Topography Measuring Systems down to Nanometric Range

    DEFF Research Database (Denmark)

    Trumpold, H.; De Chiffre, Leonardo; Andreasen, Jan Lasson

    compression and injection moulded plastic negatives and Ni-negatives have been made from which again Ni-positives were produced. The replication processes showed negligible deviations from the Pt and Pa values compared to the primary standards. An important prerequisite is the cleanliness of the surfaces......Background For the precise and accurate measurement of surface topography a whole range of surface detection systems is available. With their application in research and production problems arise due to the lack of traceable standard artefacts for the instrument calibration in X, Y and Z directions...... and for the calibration of filters. Existing ISO standards on calibration specimens are inadequate and limited in that they only cover contacting instruments and only partially the measuring ranges for these instruments. The whole range of non-contacting instruments are not covered despite their increasing use...

  11. Enhanced Strain Measurement Range of an FBG Sensor Embedded in Seven-Wire Steel Strands.

    Science.gov (United States)

    Kim, Jae-Min; Kim, Chul-Min; Choi, Song-Yi; Lee, Bang Yeon

    2017-07-18

    FBG sensors offer many advantages, such as a lack of sensitivity to electromagnetic waves, small size, high durability, and high sensitivity. However, their maximum strain measurement range is lower than the yield strain range (about 1.0%) of steel strands when embedded in steel strands. This study proposes a new FBG sensing technique in which an FBG sensor is recoated with polyimide and protected by a polyimide tube in an effort to enhance the maximum strain measurement range of FBG sensors embedded in strands. The validation test results showed that the proposed FBG sensing technique has a maximum strain measurement range of 1.73% on average, which is 1.73 times higher than the yield strain of the strands. It was confirmed that recoating the FBG sensor with polyimide and protecting the FBG sensor using a polyimide tube could effectively enhance the maximum strain measurement range of FBG sensors embedded in strands.

  12. Multiwall carbon nanotube- zirconium oxide nanocomposite hollow fiber solid phase microextraction for determination of polyaromatic hydrocarbons in water, coffee and tea samples.

    Science.gov (United States)

    Yazdi, Mahnaz Nozohour; Yamini, Yadollah; Asiabi, Hamid

    2018-06-15

    The purpose of this study was to evaluate the application of hollow fiber solid-phase microextraction (HF-SPME) followed by HPLC-UV to determine the ultra-trace amounts of polycyclic aromatic hydrocarbons (PAHs) as model analytes in complex coffee and tea samples. HF-SPME can be effectively used as an alternative to the direct immersion SPME (DI-SPME) method in complex matrices. The DI-SPME method suffers from serious limitation in dirty and complicated matrices with low sample clean-up, while the HF-SPME method has high clean-up and selectivity due to the high porosity of hollow fiber that can pick out analyte from complicated matrices. As a hollow fiber sorbent, a novel multiwall carbon nanotube/zirconium oxide nanocomposite (MWCNT/ZrO 2 ) was fabricated. The excellent adsorption of PAHs on the sorbent was attributed to the dominant roles of π-π stacking interaction and hydrophobic interaction. Under the optimized extraction conditions, the wide linear range of 0.1-200 μg L -1 with coefficients of determination better than 0.998 and low detection limits of 0.033-0.16 μg L -1 with satisfactory precision (RSD tea samples were in the range of 92.0-106.0%. Compared to other methods, MWCNT/ZrO 2 hollow fiber solid phase microextraction demonstrated a good capability for determination of PAHs in complex coffee and tea samples. Copyright © 2018 Elsevier B.V. All rights reserved.

  13. Measured long-range repulsive Casimir–Lifshitz forces

    Science.gov (United States)

    Munday, J. N.; Capasso, Federico; Parsegian, V. Adrian

    2014-01-01

    Quantum fluctuations create intermolecular forces that pervade macroscopic bodies1–3. At molecular separations of a few nanometres or less, these interactions are the familiar van der Waals forces4. However, as recognized in the theories of Casimir, Polder and Lifshitz5–7, at larger distances and between macroscopic condensed media they reveal retardation effects associated with the finite speed of light. Although these long-range forces exist within all matter, only attractive interactions have so far been measured between material bodies8–11. Here we show experimentally that, in accord with theoretical prediction12, the sign of the force can be changed from attractive to repulsive by suitable choice of interacting materials immersed in a fluid. The measured repulsive interaction is found to be weaker than the attractive. However, in both cases the magnitude of the force increases with decreasing surface separation. Repulsive Casimir–Lifshitz forces could allow quantum levitation of objects in a fluid and lead to a new class of switchable nanoscale devices with ultra-low static friction13–15. PMID:19129843

  14. Recoil range distribution measurement in 20Ne + 181Ta reaction

    International Nuclear Information System (INIS)

    Tripathi, R.; Sudarshan, K.; Goswami, A.; Guin, R.; Reddy, A.V.R.

    2005-01-01

    In order to investigate linear momentum transfer in various transfer channels in 20 Ne + 181 Ta, recoil range distribution measurements have been carried out at E lab = 180 MeV, populating significant number of l-waves above l crit

  15. Alpha Beam Energy Determination Using a Range Measuring Device for Radioisotope Production

    Energy Technology Data Exchange (ETDEWEB)

    Choi, Jun Yong; Kim, Byeon Gil; Hong, Seung Pyo; Kim, Ran Young; Chun, Kwon Soo [Korea Institute of Radiological and Medical Sciences, Seoul (Korea, Republic of)

    2016-05-15

    The threshold energy of the {sup 209}Bi(α,3n){sup 210} At reaction is at about 30MeV. Our laboratory suggested an energy measurement method to confirm the proton-beam's energy by using a range measurement device. The experiment was performed energy measurement of alpha beam. The alpha beam of energy 29 MeV has been extracted from the cyclotron for the production of {sup 211}At. This device was composed of four parts: an absorber, a drive shaft, and a servo motor and a Faraday cup. The drive shaft was mounted on the absorber and connects with the axis of the servo motor and rotates linearly and circularly by this servo motor. A Faraday cup is for measuring the beam flux. As this drive shaft rotates, the thickness of the absorber varies depending on the rotation angle of the absorber. The energy of the alpha particle accelerated and extracted from MC-50 cyclotron was calculated with the measurement of the particle range in Al foil and using ASTAR, SRIM, MCNPX software. There were a little discrepancy between the expected energy and the calculated energy within the 0.5MeV error range. We have a plan to make an experiment with various alpha particle energies and another methodology, for example, the cross section measurement of the nuclear reaction.

  16. Evaluation of needle trap micro-extraction and solid-phase micro-extraction: Obtaining comprehensive information on volatile emissions from in vitro cultures.

    Science.gov (United States)

    Oertel, Peter; Bergmann, Andreas; Fischer, Sina; Trefz, Phillip; Küntzel, Anne; Reinhold, Petra; Köhler, Heike; Schubert, Jochen K; Miekisch, Wolfram

    2018-05-14

    Volatile organic compounds (VOCs) emitted from in vitro cultures may reveal information on species and metabolism. Owing to low nmol L -1 concentration ranges, pre-concentration techniques are required for gas chromatography-mass spectrometry (GC-MS) based analyses. This study was intended to compare the efficiency of established micro-extraction techniques - solid-phase micro-extraction (SPME) and needle-trap micro-extraction (NTME) - for the analysis of complex VOC patterns. For SPME, a 75 μm Carboxen®/polydimethylsiloxane fiber was used. The NTME needle was packed with divinylbenzene, Carbopack X and Carboxen 1000. The headspace was sampled bi-directionally. Seventy-two VOCs were calibrated by reference standard mixtures in the range of 0.041-62.24 nmol L -1 by means of GC-MS. Both pre-concentration methods were applied to profile VOCs from cultures of Mycobacterium avium ssp. paratuberculosis. Limits of detection ranged from 0.004 to 3.93 nmol L -1 (median = 0.030 nmol L -1 ) for NTME and from 0.001 to 5.684 nmol L -1 (median = 0.043 nmol L -1 ) for SPME. NTME showed advantages in assessing polar compounds such as alcohols. SPME showed advantages in reproducibility but disadvantages in sensitivity for N-containing compounds. Micro-extraction techniques such as SPME and NTME are well suited for trace VOC profiling over cultures if the limitations of each technique is taken into account. Copyright © 2018 John Wiley & Sons, Ltd.

  17. ZnO nanorod array polydimethylsiloxane composite solid phase micro-extraction fiber coating: fabrication and extraction capability.

    Science.gov (United States)

    Wang, Dan; Wang, Qingtang; Zhang, Zhuomin; Chen, Guonan

    2012-01-21

    ZnO nanorod array coating is a novel kind of solid-phase microextraction (SPME) fiber coating which shows good extraction capability due to the nanostructure. To prepare the composite coating is a good way to improve the extraction capability. In this paper, the ZnO nanorod array polydimethylsiloxane (PDMS) composite SPME fiber coating has been prepared and its extraction capability for volatile organic compounds (VOCs) has been studied by headspace sampling the typical volatile mixed standard solution of benzene, toluene, ethylbenzene and xylene (BTEX). Improved detection limit and good linear ranges have been achieved for this composite SPME fiber coating. Also, it is found that the composite SPME fiber coating shows good extraction selectivity to the VOCs with alkane radicals.

  18. Analysis of Five Earthy-Musty Odorants in Environmental Water by HS-SPME/GC-MS

    Directory of Open Access Journals (Sweden)

    Zhen Ding

    2014-01-01

    Full Text Available The pressing issue of earthy and musty odor compounds in natural waters, which can affect the organoleptic properties of drinking water, makes it a public health concern. A simple and sensitive method for simultaneous analysis of five odorants in environmental water was developed by headspace solid-phase microextraction (HS-SPME coupled to chromatography-mass spectrometry (GC-MS, including geosmin (GSM and 2-methylisoborneol (2-MIB, as well as dimethyl trisulfide (DMTS, β-cyclocitral, and β-ionone. Based on the simple modification of original magnetic stirrer purchased from CORNING (USA, the five target compounds can be separated within 23 min, and the calibration curves show good linearity with a correlation coefficient above 0.999 (levels = 5. The limits of detection (LOD are all below 1.3 ng L−1, and the relative standard deviation (%RSD is between 4.4% and 9.9% (n = 7 and recoveries of the analytes from water samples are between 86.2% and 112.3%. In addition, the storage time experiment indicated that the concentrations did not change significantly for GSM and 2-MIB if they were stored in canonical environment. In conclusion, the method in this study could be applied for monitoring these five odorants in natural waters.

  19. Sensitive multiresidue method by HS-SPME/GC-MS for 10 volatile organic compounds in urine matrix: a new tool for biomonitoring studies on children.

    Science.gov (United States)

    Antonucci, Arianna; Vitali, Matteo; Avino, Pasquale; Manigrasso, Maurizio; Protano, Carmela

    2016-08-01

    A HS-SPME method coupled with GC-MS analysis has been developed for simultaneously measuring the concentration of 10 volatile organic compounds (VOCs) (benzene, toluene, ethylbenzene, o-, m-, and p-xylene, methyl tert-butyl ether, ethyl tert-butyl ether, 2-methyl-2-butyl methyl ether, and diisopropyl ether) in urine matrix as a biomonitoring tool for populations at low levels of exposure to such VOCs. These compounds, potentially toxic for human health, are common contaminants of both outdoor and indoor air, as they are released by autovehicular traffic; some of them are also present in environmental tobacco smoke (ETS). Thus, the exposure to these pollutants cannot be neglected and should be assessed. The low limits of detection and quantification (LODs and LOQs <6.5 and 7.5 ng L(-1), respectively) and the high reproducibility (CVs <4 %) make the developed method suited for biomonitoring populations exposed at low levels such as children. Further, the method is cost-effective and low in time-consumption; therefore, it is useful for investigating large populations. It has been applied to children exposed to traffic pollution and/or ETS; the relevant results are reported, and the relevant implications are discussed.

  20. Fast electrostatic force calculation on parallel computer clusters

    International Nuclear Information System (INIS)

    Kia, Amirali; Kim, Daejoong; Darve, Eric

    2008-01-01

    The fast multipole method (FMM) and smooth particle mesh Ewald (SPME) are well known fast algorithms to evaluate long range electrostatic interactions in molecular dynamics and other fields. FMM is a multi-scale method which reduces the computation cost by approximating the potential due to a group of particles at a large distance using few multipole functions. This algorithm scales like O(N) for N particles. SPME algorithm is an O(NlnN) method which is based on an interpolation of the Fourier space part of the Ewald sum and evaluating the resulting convolutions using fast Fourier transform (FFT). Those algorithms suffer from relatively poor efficiency on large parallel machines especially for mid-size problems around hundreds of thousands of atoms. A variation of the FMM, called PWA, based on plane wave expansions is presented in this paper. A new parallelization strategy for PWA, which takes advantage of the specific form of this expansion, is described. Its parallel efficiency is compared with SPME through detail time measurements on two different computer clusters

  1. Development of a solid-phase microextraction-based method for sampling of persistent chlorinated hydrocarbons in an urbanized coastal environment.

    Science.gov (United States)

    Zeng, Eddy Y; Tsukada, David; Diehl, Dario W

    2004-11-01

    Solid-phase microextraction (SPME) has been used as an in situ sampling technique for a wide range of volatile organic chemicals, but SPME field sampling of nonvolatile organic pollutants has not been reported. This paper describes the development of an SPME-based sampling method employing a poly(dimethylsiloxane) (PDMS)-coated (100-microm thickness) fiber as the sorbent phase. The laboratory-calibrated PDMS-coated fibers were used to construct SPME samplers, and field tests were conducted at three coastal locations off southern California to determine the equilibrium sampling time and compare the efficacy of the SPME samplers with that of an Infiltrex 100 water pumping system (Axys Environmental Systems Ltd., Sidney, British Columbia, Canada). p,p'-DDE and o,p'-DDE were the components consistently detected in the SPME samples among 42 polychlorinated biphenyl congeners and 17 chlorinated pesticidestargeted. SPME samplers deployed attwo locations with moderate and high levels of contamination for 18 and 30 d, respectively, attained statistically identical concentrations of p,p'-DDE and o,p'-DDE. In addition, SPME samplers deployed for 23 and 43 d, respectively, at a location of low contamination also contained statistically identical concentrations of p,p'-DDE. These results indicate that equilibrium could be reached within 18 to 23 d. The concentrations of p,p'-DDE, o,p'-DDE, or p,p'-DDD obtained with the SPME samplers and the Infiltrex 100 system were virtually identical. In particular, two water column concentration profiles of p,p'-DDE and o,p'-DDE acquired by the SPME samplers at a highly contaminated site on the Palos Verdes Shelf overlapped with the profiles obtained by the Infiltrex 100 system in 1997. The field tests not only reveal the advantages of the SPME samplers compared to the Infiltrex 100 system and other integrative passive devices but also indicate the need to improve the sensitivity of the SPME-based sampling technique.

  2. Establishment of Exposure to Organophosphorus Warfare Agents by Means of SPME-GSMS Analysis of Bodily Fluids

    International Nuclear Information System (INIS)

    Saveleva, E. I.; Koryagina, N. L.; Radilov, A. S.; Khlebnikova, N. S.; Khrustaleva, V. S.; Feld, V. E.

    2007-01-01

    Reliable chemical analytical procedures for revealing an exposure to toxic chemicals, identifying the active substance, and assessing the degree of exposure are necessary as a component of medical and forensic activities in cases of the possible use of highly toxic chemicals in war conflicts and terrorism acts, as well as emergency situations in chemical industry, specifically at chemical weapons storage and destruction facilities. According to Chemical Weapons Convention, Part XI, Appendix 4, e-17, 'samples of importance in the investigation of alleged use include biomedical samples from human or animal sources (blood, urine, excreta, tissue etc.)'. Urinary metabolites, O-alkyl esters of methylphosphic acid, offer one of the simplest means of confirming an exposure to organophosphorus warfare agents (OPWA). Urine, unlike blood or tissues, does not require invasive collection demanding in terms of sterility. Excretion with urine is the major route of elimination of OPWA from an organism. According to published data, 90% of OPWA metabolites are excreted within 48-72 h after intoxication. We developed an SPME-GCMS procedure for the determination of O-alkyl esters methylphosphonic acid in urine, with the following detection limits,: isopropyl and isobutyl esters 5 ng/ml and pinacolyl ester 1 ng/ml. The procedure involves derivatization of the target compounds directly on the microfiber. The total analysis time is 1-1.5 h. In animal experiments in vivo we could establish the exposure to OPWA at a half-LD50 level within no less than 48 h after intoxication. In principle, OPWA metabolites could be detected in urine within two weeks after intoxication but at higher doses. Retrospective analysis of urinary metabolites in cases of the exposure to low doses of OPWA requires lower detection limits (0.1-1 ng/ml). Optimal objects for the retrospective analysis of OPWA in an organism are long-lived blood protein adducts. We developed a procedure for revealing an exposure to

  3. Utilization of long duration high-volume sampling coupled to SPME-GC-MS/MS for the assessment of airborne pesticides variability in an urban area (Strasbourg, France) during agricultural application.

    Science.gov (United States)

    Liaud, Céline; Brucher, Michel; Schummer, Claude; Coscollà, Clara; Wolff, Hélène; Schwartz, Jean-Jacques; Yusà, Vicent; Millet, Maurice

    2016-10-02

    Atmospheric samples have been collected between 14 March and 12 September 2012 on a 2-week basis (15 days of sampling and exchange of traps each 7 days) in Strasbourg (east of France) for the analysis of 43 pesticides. Samples (particle and gas phases) were separately extracted using Accelerated Solvent Extraction (ASE) and pre-concentrated by Solid Phase Micro-Extraction (SPME) before analysis by gas chromatography coupled to tandem mass spectrometry (GC-MS/MS). Four SPME consecutive injections at distinct temperatures were made in order to increase the sensitivity of detection for the all monitored pesticides. Currently used detected pesticides can be grouped in four classes; those used in maize crops (acetochlor, benoxacor, dicamba, s-metolachlor, pendimethalin, and bromoxynil), in cereal crops (benoxacor, chlorothalonil, fenpropimorph, and propiconazole), in vineyards (tebuconazole), and as herbicides for orchards, meadows of green spaces (2,4-MCPA, trichlopyr). This is in accordance with the diversity of crops found in the Alsace region and trends observed are in accordance with the period of application of these pesticides. Variations observed permit also to demonstrate that the long time sampling duration used in this study is efficient to visualize temporal variations of airborne pesticides concentrations. Then, long time high-volume sampling could be a simple method permitting atmospheric survey of atmospheric contamination without any long analysis time and consequently low cost.

  4. Adaptive digital fringe projection technique for high dynamic range three-dimensional shape measurement.

    Science.gov (United States)

    Lin, Hui; Gao, Jian; Mei, Qing; He, Yunbo; Liu, Junxiu; Wang, Xingjin

    2016-04-04

    It is a challenge for any optical method to measure objects with a large range of reflectivity variation across the surface. Image saturation results in incorrect intensities in captured fringe pattern images, leading to phase and measurement errors. This paper presents a new adaptive digital fringe projection technique which avoids image saturation and has a high signal to noise ratio (SNR) in the three-dimensional (3-D) shape measurement of objects that has a large range of reflectivity variation across the surface. Compared to previous high dynamic range 3-D scan methods using many exposures and fringe pattern projections, which consumes a lot of time, the proposed technique uses only two preliminary steps of fringe pattern projection and image capture to generate the adapted fringe patterns, by adaptively adjusting the pixel-wise intensity of the projected fringe patterns based on the saturated pixels in the captured images of the surface being measured. For the bright regions due to high surface reflectivity and high illumination by the ambient light and surfaces interreflections, the projected intensity is reduced just to be low enough to avoid image saturation. Simultaneously, the maximum intensity of 255 is used for those dark regions with low surface reflectivity to maintain high SNR. Our experiments demonstrate that the proposed technique can achieve higher 3-D measurement accuracy across a surface with a large range of reflectivity variation.

  5. Error Analysis of Relative Calibration for RCS Measurement on Ground Plane Range

    Directory of Open Access Journals (Sweden)

    Wu Peng-fei

    2012-03-01

    Full Text Available Ground plane range is a kind of outdoor Radar Cross Section (RCS test range used for static measurement of full-size or scaled targets. Starting from the characteristics of ground plane range, the impact of environments on targets and calibrators is analyzed during calibration in the RCS measurements. The error of relative calibration produced by the different illumination of target and calibrator is studied. The relative calibration technique used in ground plane range is to place the calibrator on a fixed and auxiliary pylon somewhere between the radar and the target under test. By considering the effect of ground reflection and antenna pattern, the relationship between the magnitude of echoes and the position of calibrator is discussed. According to the different distances between the calibrator and target, the difference between free space and ground plane range is studied and the error of relative calibration is calculated. Numerical simulation results are presented with useful conclusions. The relative calibration error varies with the position of calibrator, frequency and antenna beam width. In most case, set calibrator close to the target may keep the error under control.

  6. Comparative study of volatile components from male and female flower buds of Populus × tomentosa by HS-SPME-GC-MS.

    Science.gov (United States)

    Xu, Liang; Liu, Haiping; Ma, Yucui; Wu, Cui; Li, Ruiqi; Chao, Zhimao

    2018-06-13

    The differences of volatile components in male (MFB) and female flower buds (FFB) of Populus × tomentosa were analysed and compared by HS-SPME with GC-MS for the first time. A total of 34 compounds were identified. Two clusters were clearly divided into male and female by hierarchical clustering analysis. Both the male and female flower buds showed methyl salicylate (22.83 and 24.09%, respectively) and 2-hydroxy-benzaldehyde (10.05 and 12.41%, respectively) as the main volatile constituents. The content of 2-cyclohexen-1-one, benzyl benzoate, and methyl benzoate in FFB was remarkably higher than in MFB. In contrast, the content of ethyl benzoate in MFB was greater than that in FFB. The phenomena showed the characteristic differences between MFB and FFB of P. × tomentosa, which enriched the basic studies on dioecious plant.

  7. Determination of steroids, caffeine and methylparaben in water using solid phase microextraction-comprehensive two dimensional gas chromatography-time of flight mass spectrometry.

    Science.gov (United States)

    Lima Gomes, Paulo C F; Barnes, Brian B; Santos-Neto, Álvaro J; Lancas, Fernando M; Snow, Nicholas H

    2013-07-19

    Analysis of several emerging contaminants (steroids, caffeine and methylparaben) in water using automated solid-phase microextraction with comprehensive two dimensional gas chromatography coupled to time of flight mass spectrometry (SPME-GCxGC-ToF/MS) is presented. Experimental design was used to determine the best SPME extraction conditions and the steroids were not derivatized prior to injection. SPME-GCxGC-ToF/MS provided linear ranges from 0.6 to 1200μgL(-1) and limits of detection and quantitation from 0.02 to 100μgL(-1). A series of river water samples obtained locally were subjected to analysis. SPME-GCxGC-ToF/MS is readily automated, straightforward and competitive with other methods for low level analysis of emerging contaminants. Copyright © 2013 Elsevier B.V. All rights reserved.

  8. Comparison and characterization of volatile compounds as markers of oils stability during frying by HS-SPME-GC/MS and Chemometric analysis.

    Science.gov (United States)

    Ben Hammouda, Ibtissem; Freitas, Flavia; Ammar, Sonda; Da Silva, M D R Gomes; Bouaziz, Mohamed

    2017-11-15

    The formation and emission of volatile compounds, including the aldehydes and some toxic compounds of oil samples, ROPO pure (100%) and the blended ROPO/RCO (80-20%), were carried out during deep frying at 180°C. The volatile profile of both oil samples was evaluated by an optimized HS-SPME-GC/MS method, before and after 20, 40 and 60 successive sessions of deep-frying. Actually, from 100 detected compounds, aldehydes were found to be the main group formed. In addition, the oil degradation under thermal treatment regarding the volatile compounds were evaluated and compared. Consequently, the blended ROPO/RCO revealed fewer formations of unsaturated aldehydes, including toxic ones, such as acrolein, and showed a greater stability against oxidative thermal degradation compared to ROPO pure. Copyright © 2017 Elsevier B.V. All rights reserved.

  9. Model-based cartilage thickness measurement in the submillimeter range

    International Nuclear Information System (INIS)

    Streekstra, G. J.; Strackee, S. D.; Maas, M.; Wee, R. ter; Venema, H. W.

    2007-01-01

    Current methods of image-based thickness measurement in thin sheet structures utilize second derivative zero crossings to locate the layer boundaries. It is generally acknowledged that the nonzero width of the point spread function (PSF) limits the accuracy of this measurement procedure. We propose a model-based method that strongly reduces PSF-induced bias by incorporating the PSF into the thickness estimation method. We estimated the bias in thickness measurements in simulated thin sheet images as obtained from second derivative zero crossings. To gain insight into the range of sheet thickness where our method is expected to yield improved results, sheet thickness was varied between 0.15 and 1.2 mm with an assumed PSF as present in the high-resolution modes of current computed tomography (CT) scanners [full width at half maximum (FWHM) 0.5-0.8 mm]. Our model-based method was evaluated in practice by measuring layer thickness from CT images of a phantom mimicking two parallel cartilage layers in an arthrography procedure. CT arthrography images of cadaver wrists were also evaluated, and thickness estimates were compared to those obtained from high-resolution anatomical sections that served as a reference. The thickness estimates from the simulated images reveal that the method based on second derivative zero crossings shows considerable bias for layers in the submillimeter range. This bias is negligible for sheet thickness larger than 1 mm, where the size of the sheet is more than twice the FWHM of the PSF but can be as large as 0.2 mm for a 0.5 mm sheet. The results of the phantom experiments show that the bias is effectively reduced by our method. The deviations from the true thickness, due to random fluctuations induced by quantum noise in the CT images, are of the order of 3% for a standard wrist imaging protocol. In the wrist the submillimeter thickness estimates from the CT arthrography images correspond within 10% to those estimated from the anatomical

  10. Characterization of Volatile Compounds with HS-SPME from Oxidized n-3 PUFA Rich Oils via Rancimat Tests.

    Science.gov (United States)

    Yang, Kai-Min; Cheng, Ming-Ching; Chen, Chih-Wei; Tseng, Chin-Yin; Lin, Li-Yun; Chiang, Po-Yuan

    2017-02-01

    Algae oil and fish oil are n-3 PUFA mainstream commercial products. The various sources for the stability of n-3 PUFA oxidation are influenced by the fatty acid composition, extraction and refined processing. In this study, the oil stability index (OSI) occurs within 2.3 to 7.6 hours with three different n-3 PUFA rich oil. To set the OSI in the Rancimat test as the oil stability limit and observed various degrees of oxidation (0, 25, 50, 75, 100 and 125%). The volatile oxidation compounds were analyzed via headspace-solid phase microextraction (HS-SPME) and GC/MS. We detected 51 volatile compound variations during the oxidation, which were composed of aldehydes, hydrocarbons, cyclic compounds, alcohols, benzene compounds, ketones, furans, ester and pyrrolidine. The off-flavor characteristics can be strongly influenced by the synergy effects of volatile oxidation compounds. Chemometric analysis (PCA and AHC) was applied to identify the sensitive oxidation marker compounds, which included a (E,E)-2,4-heptadienal appropriate marker, via lipid oxidation in the n-3 PUFA rich oil.

  11. An Observability Metric for Underwater Vehicle Localization Using Range Measurements

    Directory of Open Access Journals (Sweden)

    Filippo Arrichiello

    2013-11-01

    Full Text Available The paper addresses observability issues related to the general problem of single and multiple Autonomous Underwater Vehicle (AUV localization using only range measurements. While an AUV is submerged, localization devices, such as Global Navigation Satellite Systems, are ineffective, due to the attenuation of electromagnetic waves. AUV localization based on dead reckoning techniques and the use of affordable motion sensor units is also not practical, due to divergence caused by sensor bias and drift. For these reasons, localization systems often build on trilateration algorithms that rely on the measurements of the ranges between an AUV and a set of fixed transponders using acoustic devices. Still, such solutions are often expensive, require cumbersome calibration procedures and only allow for AUV localization in an area that is defined by the geometrical arrangement of the transponders. A viable alternative for AUV localization that has recently come to the fore exploits the use of complementary information on the distance from the AUV to a single transponder, together with information provided by on-board resident motion sensors, such as, for example, depth, velocity and acceleration measurements. This concept can be extended to address the problem of relative localization between two AUVs equipped with acoustic sensors for inter-vehicle range measurements. Motivated by these developments, in this paper, we show that both the problems of absolute localization of a single vehicle and the relative localization of multiple vehicles can be treated using the same mathematical framework, and tailoring concepts of observability derived for nonlinear systems, we analyze how the performance in localization depends on the types of motion imparted to the AUVs. For this effect, we propose a well-defined observability metric and validate its usefulness, both in simulation and by carrying out experimental tests with a real marine vehicle during which the

  12. 10.23  Mcps laser pseudo-code ranging system with 0.33  mm (1σ) pseudo-range measurement precision.

    Science.gov (United States)

    Yu, Xiaonan; Tong, Shoufeng; Zhang, Lei; Dong, Yan; Zhao, Xin; Qiao, Yue

    2017-07-01

    The inter-satellite laser link is the backbone of the next inter-satellite information network, and ranging and communication are the main functions of the inter-satellite laser link. This study focuses on the inter-satellite laser ranging based on the pseudo-code correlation technology. In this paper, several typical laser-ranging methods have been compared and we determined that the laser pseudo-code ranging architecture is more suitable for the inter-satellite laser communication link. The pseudo-code ranging system is easy to combine with a digital communication system, and we used it to calculate integer ambiguity by modulating the time information. The main challenge of the ranging system is range precision, which is the main focus of this paper. First, the framework of the pseudo-code ranging system is introduced; the ranging architecture of dual one-way ranging is used to eliminate the clock error between the two transceivers, and then the uncertainty of the phase detector is analyzed. In the analysis, the carrier to noise ratio and the ranging code rate are constrained by the laser communication link margin and the electronic hardware limitation. Therefore, the relationship between the sampling depth and the phase detector uncertainty is verified. A series of optical fiber channel laser pseudo-code ranging experiments demonstrated the effects of sampling depth on the ranging precision. By adjusting the depth of storage, such as the depth of 1.6 Mb, we obtained a pseudo-range measurement precision of 0.33 mm (1σ), which is equivalent to 0.0001 times code subdivision of 10.23 Mcps pseudo-code. This paper has achieved high precision in a pseudo-range measurements, which is the foundation of the inter-satellite laser link.

  13. Quantification of benzene, toluene, ethylbenzene and o-xylene in internal combustion engine exhaust with time-weighted average solid phase microextraction and gas chromatography mass spectrometry.

    Science.gov (United States)

    Baimatova, Nassiba; Koziel, Jacek A; Kenessov, Bulat

    2015-05-11

    A new and simple method for benzene, toluene, ethylbenzene and o-xylene (BTEX) quantification in vehicle exhaust was developed based on diffusion-controlled extraction onto a retracted solid-phase microextraction (SPME) fiber coating. The rationale was to develop a method based on existing and proven SPME technology that is feasible for field adaptation in developing countries. Passive sampling with SPME fiber retracted into the needle extracted nearly two orders of magnitude less mass (n) compared with exposed fiber (outside of needle) and sampling was in a time weighted-averaging (TWA) mode. Both the sampling time (t) and fiber retraction depth (Z) were adjusted to quantify a wider range of Cgas. Extraction and quantification is conducted in a non-equilibrium mode. Effects of Cgas, t, Z and T were tested. In addition, contribution of n extracted by metallic surfaces of needle assembly without SPME coating was studied. Effects of sample storage time on n loss was studied. Retracted TWA-SPME extractions followed the theoretical model. Extracted n of BTEX was proportional to Cgas, t, Dg, T and inversely proportional to Z. Method detection limits were 1.8, 2.7, 2.1 and 5.2 mg m(-3) (0.51, 0.83, 0.66 and 1.62 ppm) for BTEX, respectively. The contribution of extraction onto metallic surfaces was reproducible and influenced by Cgas and t and less so by T and by the Z. The new method was applied to measure BTEX in the exhaust gas of a Ford Crown Victoria 1995 and compared with a whole gas and direct injection method. Copyright © 2015 Elsevier B.V. All rights reserved.

  14. Discrimination of cherry wines based on their sensory properties and aromatic fingerprinting using HS-SPME-GC-MS and multivariate analysis.

    Science.gov (United States)

    Xiao, Zuobing; Liu, Shengjiang; Gu, Yongbo; Xu, Na; Shang, Yi; Zhu, Jiancai

    2014-03-01

    Volatiles of cherry wines were extracted by headspace solid phase microextraction (HS-SPME) and analyzed by gas chromatography mass spectrometry (GC-MS), multivariate statistical techniques (such as principal component analysis (PCA) and cluster analysis (CA) and correlation analysis) to differentiate sensory attributes of 3 groups of the wines through characterization of volatiles of cherry wine. Seventy-five volatiles were identified in 9 samples, including 29 esters, 22 alcohols, 8 acids, 3 ketones, 5 aldehydes, and 8 miscellaneous compounds. The PCA results showed that the cherry wines were mainly differentiated by 8 sensory attributes. The samples W2, W4, and W7 were grouped around sweet aromatic and the samples W1, W5, and W9 were highly associated with the sweet, esters, green, bitter, and fermented. Nevertheless, the samples W3, W6, and W8 were located close to the sour, alcoholic, and fruity. The final result of correlation analysis was in conformity with the conclusion of PCA. The CA results showed that the group of W2, W4, and W7, and the group of W1, W5, and W9 had less difference than the group of W3, W6, and W8. The reason should be that esterification reactions and fermentation process during the ageing period was more extended. The results of analyzing revealed that HS-SPME-GC-MS coupled with chemometrics could give an appropriate way of characterizing and classifying the cherry wines. Attributes that represent and discriminate among cherry wines might be made use of a better comprehending of the wines and for being utilized in future work. In addition, several chemometrics were used to classify the type of wines and try to install the relationship between volatiles and sensory property. Especially, PCA clearly revealed that the most contributing compounds for sensory attributes of cherry wines, CA was a more applicable way to distinguish types of cherry wines. Therefore, a feasible method that would be helpful to promote the quality of the wines by

  15. Picosecond X-ray streak camera dynamic range measurement

    Energy Technology Data Exchange (ETDEWEB)

    Zuber, C., E-mail: celine.zuber@cea.fr; Bazzoli, S.; Brunel, P.; Gontier, D.; Raimbourg, J.; Rubbelynck, C.; Trosseille, C. [CEA, DAM, DIF, F-91297 Arpajon (France); Fronty, J.-P.; Goulmy, C. [Photonis SAS, Avenue Roger Roncier, BP 520, 19106 Brive Cedex (France)

    2016-09-15

    Streak cameras are widely used to record the spatio-temporal evolution of laser-induced plasma. A prototype of picosecond X-ray streak camera has been developed and tested by Commissariat à l’Énergie Atomique et aux Énergies Alternatives to answer the Laser MegaJoule specific needs. The dynamic range of this instrument is measured with picosecond X-ray pulses generated by the interaction of a laser beam and a copper target. The required value of 100 is reached only in the configurations combining the slowest sweeping speed and optimization of the streak tube electron throughput by an appropriate choice of high voltages applied to its electrodes.

  16. A modified multiscale peak alignment method combined with trilinear decomposition to study the volatile/heat-labile components in Ligusticum chuanxiong Hort - Cyperus rotundus rhizomes by HS-SPME-GC/MS.

    Science.gov (United States)

    He, Min; Yan, Pan; Yang, Zhi-Yu; Zhang, Zhi-Min; Yang, Tian-Biao; Hong, Liang

    2018-03-15

    Head Space/Solid Phase Micro-Extraction (HS-SPME) coupled with Gas Chromatography/Mass Spectrometer (GC/MS) was used to determine the volatile/heat-labile components in Ligusticum chuanxiong Hort - Cyperus rotundus rhizomes. Facing co-eluting peaks in k samples, a trilinear structure was reconstructed to obtain the second-order advantage. The retention time (RT) shift with multi-channel detection signals for different samples has been vital in maintaining the trilinear structure, thus a modified multiscale peak alignment (mMSPA) method was proposed in this paper. The peak position and peak width of representative ion profile were firstly detected by mMSPA using Continuous Wavelet Transform with Haar wavelet as the mother wavelet (Haar CWT). Then, the raw shift was confirmed by Fast Fourier Transform (FFT) cross correlation calculation. To obtain the optimal shift, Haar CWT was again used to detect the subtle deviations and be amalgamated in calculation. Here, to ensure there is no peaks shape alternation, the alignment was performed in local domains of data matrices, and all data points in the peak zone were moved via linear interpolation in non-peak parts. Finally, chemical components of interest in Ligusticum chuanxiong Hort - Cyperus rotundus rhizomes were analyzed by HS-SPME-GCMS and mMSPA-alternating trilinear decomposition (ATLD) resolution. As a result, the concentration variation between herbs and their pharmaceutical products can provide a scientific basic for the quality standard establishment of traditional Chinese medicines. Copyright © 2018 Elsevier B.V. All rights reserved.

  17. Greek Salvia sclarea L. Essential Oils: Effect of Hydrodistillation Time, Comparison of the Aroma Chemicals Using Hydrodistillation and HS-SPME Techniques

    Directory of Open Access Journals (Sweden)

    Aikaterini Koutsaviti

    2016-05-01

    Full Text Available Since the essential oil of Salvia sclarea is used as a flavouring agent, the effect of different extraction techniques (hydrodistillation & HS-SPME and duration of hydrodistillation (2, 3 and 4 h with respect to yield, composition and identification rate of extracted essential oils from Greek cultivated S. sclarea aerial blooming parts were investigated. Linalool and linalyl acetate levels seemed to decrease with increasing duration of hydrodistillation, while diterpenes increased dramatically, while the head space analysis showed significantly lower levels of linalool in comparison to its ester. Thus, linalool (5.1-35.8%, linalyl acetate (11.3-37.6% and sclareol (0.0-41.8%, concerning the oils obtained by hydrodistillation, were the most important metabolites. Solid-phase microextraction yielded mainly oxygenated monoterpenes, especially linalyl acetate (59.3%, followed by cis-linalool oxide (8.6% and linalool (7.8%.

  18. Ground based mobile isotopic methane measurements in the Front Range, Colorado

    Science.gov (United States)

    Vaughn, B. H.; Rella, C.; Petron, G.; Sherwood, O.; Mielke-Maday, I.; Schwietzke, S.

    2014-12-01

    Increased development of unconventional oil and gas resources in North America has given rise to attempts to monitor and quantify fugitive emissions of methane from the industry. Emission estimates of methane from oil and gas basins can vary significantly from one study to another as well as from EPA or State estimates. New efforts are aimed at reconciling bottom-up, or inventory-based, emission estimates of methane with top-down estimates based on atmospheric measurements from aircraft, towers, mobile ground-based vehicles, and atmospheric models. Attributing airborne measurements of regional methane fluxes to specific sources is informed by ground-based measurements of methane. Stable isotopic measurements (δ13C) of methane help distinguish between emissions from the O&G industry, Confined Animal Feed Operations (CAFO), and landfills, but analytical challenges typically limit meaningful isotopic measurements to individual point sampling. We are developing a toolbox to use δ13CH4 measurements to assess the partitioning of methane emissions for regions with multiple methane sources. The method was applied to the Denver-Julesberg Basin. Here we present data from continuous isotopic measurements obtained over a wide geographic area by using MegaCore, a 1500 ft. tube that is constantly filled with sample air while driving, then subsequently analyzed at slower rates using cavity ring down spectroscopy (CRDS). Pressure, flow and calibration are tightly controlled allowing precise attribution of methane enhancements to their point of collection. Comparisons with point measurements are needed to confirm regional values and further constrain flux estimates and models. This effort was made in conjunction with several major field campaigns in the Colorado Front Range in July-August 2014, including FRAPPÉ (Front Range Air Pollution and Photochemistry Experiment), DISCOVER-AQ, and the Air Water Gas NSF Sustainability Research Network at the University of Colorado.

  19. Optimization of an analytical methodology for the determination of alkyl- and methoxy-phenolic compounds by HS-SPME in biomass smoke

    Energy Technology Data Exchange (ETDEWEB)

    Conde, Francisco J.; Afonso, Ana M.; Gonzalez, Venerando; Ayala, Juan H. [University of La Laguna, Campus de Anchieta, Department of Analytical Chemistry, Nutrition and Food Science, La Laguna (Spain)

    2006-08-15

    A sampling and analysis method for the determination of 21 phenolic compounds in smoke samples from biomass combustion has been developed. The smoke is used to make smoked foods, following an artisanal procedure used in some parts of the Canary Islands. The sampling system consists of a Bravo H air sampler, two impingers, each one containing an aqueous solution of sodium hydroxide 0.1 mol L{sup -1}, followed by a silica gel trap. The variables optimized to reach the best sampling conditions were volume of absorbent solution and sampling flow. Under the optimum conditions, 100 mL of absorbent solution of NaOH 0.10 mol L{sup -1} and 2 L min{sup -1} for the sampling flow, sampling efficiencies are higher than 80%. Analysis of phenolic compounds was carried out by headspace solid-phase microextraction (HS-SPME) coupled to gas chromatography-mass spectrometry (GC-MS). Five different fiber coatings were employed in this study. By means of a central composite design, extraction time, salt concentration, and pH of the solution were optimized: 65-{mu}m carbowax-divinylbenzene, extraction time 90 min, concentration in NaCl of 35% (m/v), and pH 2 yielded the highest response. Detection limits of phenol and their alkyl derivatives, guaiacol and eugenol, are between 1.13 and 4.60 ng mL{sup -1}. 3-Methoxyphenol, 2,6-dimethoxyphenol, and vanillin have detection limits considerably higher. Good linearity (R {sup 2}{>=}0.98) was observed for all calibration curves in the established ranges. The reproducibility of the method (RSD, relative standard deviation) was found to oscillate between 7 and 18% (generally close or lower than 10%). (orig.)

  20. An extended set-value observer for position estimation using single range measurements

    DEFF Research Database (Denmark)

    Marcal, Jose; Jouffroy, Jerome; Fossen, Thor I.

    the observability of the system is briefly discussed and an extended set-valued observer is presented, with some discussion about the effect of the measurements noise on the final solution. This observer estimates bounds in the errors assuming that the exogenous signals are bounded, providing a safe region......The ability of estimating the position of an underwater vehicle from single range measurements is important in applications where one transducer marks an important geographical point, when there is a limitation in the size or cost of the vehicle, or when there is a failure in a system...... of transponders. The knowledge of the bearing of the vehicle and the range measurements from a single location can provide a solution which is sensitive to the trajectory that the vehicle is following, since there is no complete constraint on the position estimate with a single beacon. In this paper...

  1. Optimisation of recovery protocols for double-base smokeless powder residues analysed by total vaporisation (TV) SPME/GC-MS.

    Science.gov (United States)

    Sauzier, Georgina; Bors, Dana; Ash, Jordan; Goodpaster, John V; Lewis, Simon W

    2016-09-01

    The investigation of explosive events requires appropriate evidential protocols to recover and preserve residues from the scene. In this study, a central composite design was used to determine statistically validated optimum recovery parameters for double-base smokeless powder residues on steel, analysed using total vaporisation (TV) SPME/GC-MS. It was found that maximum recovery was obtained using isopropanol-wetted swabs stored under refrigerated conditions, then extracted for 15min into acetone on the same day as sample collection. These parameters were applied to the recovery of post-blast residues deposited on steel witness surfaces following a PVC pipe bomb detonation, resulting in detection of all target components across the majority of samples. Higher overall recoveries were obtained from plates facing the sides of the device, consistent with the point of first failure occurring in the pipe body as observed in previous studies. The methodology employed here may be readily applied to a variety of other explosive compounds, and thus assist in establishing 'best practice' procedures for explosive investigations. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. Metabolome based volatiles profiling in 13 date palm fruit varieties from Egypt via SPME GC-MS and chemometrics.

    Science.gov (United States)

    Khalil, Mohammed N A; Fekry, Mostafa I; Farag, Mohamed A

    2017-02-15

    Dates (Phoenix dactylifera L.) are distributed worldwide as major food complement providing a source of sugars and dietary fiber as well as macro- and micronutrients. Although phytochemical analyses of date fruit non-volatile metabolites have been reported, much less is known about the aroma given off by the fruit, which is critical for dissecting sensory properties and quality traits. Volatile constituents from 13 date varieties grown in Egypt were profiled using SPME-GCMS coupled to multivariate data analysis to explore date fruit aroma composition and investigate potential future uses by food industry. A total of 89 volatiles were identified where lipid-derived volatiles and phenylpropanoid derivatives were the major components of date fruit aroma. Multivariate data analyses revealed that 2,3-butanediol, hexanal, hexanol and cinnamaldehyde contributed the most to classification of different varieties. This study provides the most complete map of volatiles in Egyptian date fruit, with Siwi and Sheshi varieties exhibiting the most distinct aroma among studied date varieties. Copyright © 2016 Elsevier Ltd. All rights reserved.

  3. Solid phase microextraction sampling of high explosive residues in the presence of radionuclides and radionuclide surrogate metals

    International Nuclear Information System (INIS)

    Duff, M.C.; Crump, S.L.; Ray, R.J.; Beals, D.; Cotham, W.E.; Mount, K.; Koons, R.D.; Leggitt, J.

    2008-01-01

    The Federal Bureau of Investigation (FBI) Laboratory currently does not have on site facilities for handling radioactive evidentiary materials and there are no established FBI methods or procedures for decontaminating high explosive (HE) evidence while maintaining evidentiary value. One experimental method for the isolation of HE residue involves using solid phase microextraction (SPME) fibers to remove residue of interest. Due to their high affinity for organics, SPME fibers should have little affinity for most metals. However, no studies have measured the affinity of radionuclides for SPME fibers. The focus of this research was to examine the affinity of dissolved radionuclide ( 239/240 Pu, 238 U, 237 Np, 85 Sr, 133 Ba, 137 Cs, 60 Co and 226 Ra) and stable radionuclide surrogate metals (Sr, Co, Ir, Re, Ni, Ba, Cs, Nb, Ru, and Nd) for SPME fibers at the exposure conditions that favor the uptake of HE residues. Our results from radiochemical and mass spectrometric analyses indicate these metals have little measurable affinity for these SPME fibers during conditions that are conducive to HE residue uptake with subsequent analysis by liquid or gas phase chromatography with mass spectrometric detection. (author)

  4. Spin motion determination of the Envisat satellite through laser ranging measurements from a single pass measured by a single station

    Science.gov (United States)

    Pittet, Jean-Noël; Šilha, Jiří; Schildknecht, Thomas

    2018-02-01

    The Satellite Laser Ranging (SLR) technology is used to accurately determine the position of space objects equipped with so-called retro-reflectors or retro-reflector arrays (RRA). This type of measurement allows to measure the range to the spacecraft with high precision, which leads to determination of very accurate orbits for these targets. Non-active spacecraft, which are not attitude controlled any longer, tend to start to spin or tumble under influence of the external and internal torques and forces. If the return signal is measured for a non-spherical non-active rotating object, the signal in the range residuals with respect to the reference orbit is more complex. For rotating objects the return signal shows an oscillating pattern or patterns caused by the RRA moving around the satellite's centre of mass. This behaviour is projected onto the radial component measured by the SLR. In our work, we demonstrate how the SLR ranging technique from one sensor to a satellite equipped with a RRA can be used to precisely determine its spin motion during one passage. Multiple SLR measurements of one target over time allow to accurately monitor spin motion changes which can be further used for attitude predictions. We show our solutions of the spin motion determined for the non-active ESA satellite Envisat obtained from measurements acquired during years 2013-2015 by the Zimmerwald SLR station, Switzerland. All the necessary parameters are defined for our own so-called point-like model which describes the motion of a point in space around the satellite centre of mass.

  5. NMR investigation of acrolein stability in hydroalcoholic solution as a foundation for the valid HS-SPME/GC–MS quantification of the unsaturated aldehyde in beverages

    International Nuclear Information System (INIS)

    Kächele, Martin; Monakhova, Yulia B.; Kuballa, Thomas; Lachenmeier, Dirk W.

    2014-01-01

    Highlights: • Acrolein in hydroalcoholic solution degrades to 1,3,3-propanetriol and 3-hydroxypropionaldehyde. • Hydroquinone (0.2%) at pH 3.0 stabilizes acrolein solutions. • Quantitative HS-SPME/GC–MS determination of acrolein in alcoholic beverages was developed (LOD 14 μg L −1 ). • 6 of 117 samples had acrolein levels above the WHO threshold (1500 μg L −1 ). - Abstract: Acrolein (propenal) is found in many foods and beverages and may pose a health hazard due to its cytotoxicity. Considerable knowledge gaps regarding human exposure to acrolein exist, and there is a lack of reliable analytical methods. Hydroalcoholic dilutions prepared for calibration purposes from pure acrolein show considerable degradation of the compound and nuclear magnetic resonance (NMR) spectroscopy showed that 1,3,3-propanetriol and 3-hydroxypropionaldehyde are formed. The degradation can be prevented by addition of hydroquinone as stabilizer to the calibration solutions, which then show linear concentration-response behaviour required for quantitative analysis. The stabilized calibration solutions were used for quantitative headspace solid-phase microextraction/gas chromatography–mass spectrometry (HS-SPME/GC–MS) determination of acrolein in alcoholic beverages with a detection limit of 14 μg L −1 . Of 117 tested alcoholic beverages, 64 were tested positive with the highest incidence in grape marc spirits and whiskey (100%, mean 252 μg L −1 ), followed by fruit spirits (86%, mean 591 μg/L −1 ), tequila (86%, mean 404 μg L −1 ), Asian spirits (43%, mean 54 μg L −1 ) and wine (9%, mean 0.7 μg L −1 ). Acrolein could not be detected in beer, vodka, absinthe and bottled water. Six of the fruit and grape marc spirits had acrolein levels above the World Health Organization (WHO) provisional tolerable concentration of 1.5 mg L −1

  6. NMR investigation of acrolein stability in hydroalcoholic solution as a foundation for the valid HS-SPME/GC–MS quantification of the unsaturated aldehyde in beverages

    Energy Technology Data Exchange (ETDEWEB)

    Kächele, Martin [Chemisches und Veterinäruntersuchungsamt (CVUA) Karlsruhe, Weissenburger Strasse 3, D-76187 Karlsruhe (Germany); Hochschule Mannheim, Paul-Wittsack-Strasse 10, D-68163 Mannheim (Germany); Monakhova, Yulia B. [Chemisches und Veterinäruntersuchungsamt (CVUA) Karlsruhe, Weissenburger Strasse 3, D-76187 Karlsruhe (Germany); Bruker Biospin GmbH, Silbersteifen, 76287 Rheinstetten (Germany); Department of Chemistry, Saratov State University, Astrakhanskaya Street 83, 410012 Saratov (Russian Federation); Kuballa, Thomas [Chemisches und Veterinäruntersuchungsamt (CVUA) Karlsruhe, Weissenburger Strasse 3, D-76187 Karlsruhe (Germany); Lachenmeier, Dirk W., E-mail: lachenmeier@web.de [Chemisches und Veterinäruntersuchungsamt (CVUA) Karlsruhe, Weissenburger Strasse 3, D-76187 Karlsruhe (Germany); Ministry of Rural Affairs and Consumer Protection, Kernerplatz 10, 70182 Stuttgart (Germany)

    2014-04-01

    Highlights: • Acrolein in hydroalcoholic solution degrades to 1,3,3-propanetriol and 3-hydroxypropionaldehyde. • Hydroquinone (0.2%) at pH 3.0 stabilizes acrolein solutions. • Quantitative HS-SPME/GC–MS determination of acrolein in alcoholic beverages was developed (LOD 14 μg L⁻¹. • 6 of 117 samples had acrolein levels above the WHO threshold (1500 μg L⁻¹). Abstract: Acrolein (propenal) is found in many foods and beverages and may pose a health hazard due to its cytotoxicity. Considerable knowledge gaps regarding human exposure to acrolein exist, and there is a lack of reliable analytical methods. Hydroalcoholic dilutions prepared for calibration purposes from pure acrolein show considerable degradation of the compound and nuclear magnetic resonance (NMR) spectroscopy showed that 1,3,3-propanetriol and 3-hydroxypropionaldehyde are formed. The degradation can be prevented by addition of hydroquinone as stabilizer to the calibration solutions, which then show linear concentration-response behaviour required for quantitative analysis. The stabilized calibration solutions were used for quantitative headspace solid-phase microextraction/gas chromatography–mass spectrometry (HS-SPME/GC–MS) determination of acrolein in alcoholic beverages with a detection limit of 14 μg L⁻¹. Of 117 tested alcoholic beverages, 64 were tested positive with the highest incidence in grape marc spirits and whiskey (100%, mean 252 μg L⁻¹), followed by fruit spirits (86%, mean 591 μg/L⁻¹), tequila (86%, mean 404 μg L⁻¹), Asian spirits (43%, mean 54 μg L⁻¹) and wine (9%, mean 0.7 μg L⁻¹). Acrolein could not be detected in beer, vodka, absinthe and bottled water. Six of the fruit and grape marc spirits had acrolein levels above the World Health Organization (WHO) provisional tolerable concentration of 1.5 mg L⁻¹.

  7. Scintillator-CCD camera system light output response to dosimetry parameters for proton beam range measurement

    Energy Technology Data Exchange (ETDEWEB)

    Daftari, Inder K., E-mail: idaftari@radonc.ucsf.edu [Department of Radiation Oncology, 1600 Divisadero Street, Suite H1031, University of California-San Francisco, San Francisco, CA 94143 (United States); Castaneda, Carlos M.; Essert, Timothy [Crocker Nuclear Laboratory,1 Shields Avenue, University of California-Davis, Davis, CA 95616 (United States); Phillips, Theodore L.; Mishra, Kavita K. [Department of Radiation Oncology, 1600 Divisadero Street, Suite H1031, University of California-San Francisco, San Francisco, CA 94143 (United States)

    2012-09-11

    The purpose of this study is to investigate the luminescence light output response in a plastic scintillator irradiated by a 67.5 MeV proton beam using various dosimetry parameters. The relationship of the visible scintillator light with the beam current or dose rate, aperture size and the thickness of water in the water-column was studied. The images captured on a CCD camera system were used to determine optimal dosimetry parameters for measuring the range of a clinical proton beam. The method was developed as a simple quality assurance tool to measure the range of the proton beam and compare it to (a) measurements using two segmented ionization chambers and water column between them, and (b) with an ionization chamber (IC-18) measurements in water. We used a block of plastic scintillator that measured 5 Multiplication-Sign 5 Multiplication-Sign 5 cm{sup 3} to record visible light generated by a 67.5 MeV proton beam. A high-definition digital video camera Moticam 2300 connected to a PC via USB 2.0 communication channel was used to record images of scintillation luminescence. The brightness of the visible light was measured while changing beam current and aperture size. The results were analyzed to obtain the range and were compared with the Bragg peak measurements with an ionization chamber. The luminescence light from the scintillator increased linearly with the increase of proton beam current. The light output also increased linearly with aperture size. The relationship between the proton range in the scintillator and the thickness of the water column showed good linearity with a precision of 0.33 mm (SD) in proton range measurement. For the 67.5 MeV proton beam utilized, the optimal parameters for scintillator light output response were found to be 15 nA (16 Gy/min) and an aperture size of 15 mm with image integration time of 100 ms. The Bragg peak depth brightness distribution was compared with the depth dose distribution from ionization chamber measurements

  8. Smartphone Photography as a Tool to Measure Knee Range of Motion.

    Science.gov (United States)

    Mica, Megan Conti; Wagner, Eric R; Shin, Alexander Y

    2018-01-01

    The objective of this study was to validate measuring knee range of motion (ROM) from smartphone photography. Thirty-two participants (64 knees) obtained smartphone photographs of knee flexion and extension. Surgeons obtained the same photographs and goniometric measurement of ROM. ROM was measured using Adobe Photoshop. Goniometer versus digital measurements, participant versus surgeon photographs, and interobserver measurements were analyzed. The average difference in goniometer and digital photograph measurements was 5°. The interclass correlation was .642(L) and .656(R). The Bland-Altman plots demonstrated that 29/32 digital measurements were within the 95% confidence interval (CI). Participants' versus researchers' photographs averaged a 2° difference. The interclass correlation was .924(L) and .91(R). Bland-Altman plots demonstrated that 31/32 measurements were within the 95% CI. Interobserver reliability averaged aROMdifference of 5°. The concordance coefficients were .647(L) and .723(R). Bland-Altman plots demonstrated that 30 of 32 digital measurements were within the 95% CI. Measuring knee ROM using smartphone digital photography is valid and reliable. (Journal of Surgical Orthopaedic Advances 27(1):52-57, 2018).

  9. Potentiometric Measurement of Transition Ranges and Titration Errors for Acid/Base Indicators

    Science.gov (United States)

    Flowers, Paul A.

    1997-07-01

    Sophomore analytical chemistry courses typically devote a substantial amount of lecture time to acid/base equilibrium theory, and usually include at least one laboratory project employing potentiometric titrations. In an effort to provide students a laboratory experience that more directly supports their classroom discussions on this important topic, an experiment involving potentiometric measurement of transition ranges and titration errors for common acid/base indicators has been developed. The pH and visually-assessed color of a millimolar strong acid/base system are monitored as a function of added titrant volume, and the resultant data plotted to permit determination of the indicator's transition range and associated titration error. Student response is typically quite positive, and the measured quantities correlate reasonably well to literature values.

  10. Locating industrial VOC sources with aircraft observations

    International Nuclear Information System (INIS)

    Toscano, P.; Gioli, B.; Dugheri, S.; Salvini, A.; Matese, A.; Bonacchi, A.; Zaldei, A.; Cupelli, V.; Miglietta, F.

    2011-01-01

    Observation and characterization of environmental pollution, focussing on Volatile Organic Compounds (VOCs), in a high-risk industrial area, are particularly important in order to provide indications on a safe level of exposure, indicate eventual priorities and advise on policy interventions. The aim of this study is to use the Solid Phase Micro Extraction (SPME) method to measure VOCs, directly coupled with atmospheric measurements taken on a small aircraft environmental platform, to evaluate and locate the presence of VOC emission sources in the Marghera industrial area. Lab analysis of collected SPME fibres and subsequent analysis of mass spectrum and chromatograms in Scan Mode allowed the detection of a wide range of VOCs. The combination of this information during the monitoring campaign allowed a model (Gaussian Plume) to be implemented that estimates the localization of emission sources on the ground. - Highlights: → Flight plan aimed at sampling industrial area at various altitudes and locations. → SPME sampling strategy was based on plume detection by means of CO 2 . → Concentrations obtained were lower than the limit values or below the detection limit. → Scan mode highlighted presence of γ-butyrolactone (GBL) compound. → Gaussian dispersion modelling was used to estimate GBL source location and strength. - An integrated strategy based on atmospheric aircraft observations and dispersion modelling was developed, aimed at estimating spatial location and strength of VOC point source emissions in industrial areas.

  11. Is goniometry suitable for measuring ankle range of motion in female ballet dancers? An initial comparison with radiographic measurement.

    Science.gov (United States)

    Russell, Jeffrey A; Shave, Ruth M; Kruse, David W; Nevill, Alan M; Koutedakis, Yiannis; Wyon, Matthew A

    2011-06-01

    Female ballet dancers require extreme ankle motion to attain the demi-plié (weight-bearing full dorsiflexion [DF]) and en pointe (weight-bearing full plantar flexion [PF]) positions of ballet. However, techniques for assessing this amount of motion have not yet received sufficient scientific scrutiny. Therefore, the purpose of this study was to examine possible differences between weight-bearing goniometric and radiographic ankle range of motion measurements in female ballet dancers. Ankle range of motion in 8 experienced female ballet dancers was assessed by goniometry and 2 radiographic measurement methods. The latter were performed on 3 mediolateral x-rays, in demi-plié, neutral, and en pointe positions; one of them used the same landmarks as goniometry. DF values were not significantly different among the methods, but PF values were (P ballet dancers and suggest that goniometry may not be ideal for assessing ankle range of motion in these individuals. Therefore, further research is needed to standardize how DF and PF are measured in ballet dancers. Diagnostic, Level I.

  12. Biodegradation testing of chemicals with high Henry’s constants – separating mass and effective concentration reveals higher rate constants

    DEFF Research Database (Denmark)

    Birch, Heidi; Andersen, Henrik Rasmus; Comber, Mike

    Microextraction (HS-SPME) was applied directly on the test systems to measure substrate depletion by biodegradation relative to abiotic controls. HS-SPME was also applied to determine air to water partitioning ratios. Water phase biodegradation rate constants, kwater, were up to 72 times higher than test system...

  13. A comparison on radar range profiles between in-flight measurements and RCS-predictions

    NARCIS (Netherlands)

    Heiden, R. van der; Ewijk, L.J. van; Groen, F.C.A.

    1998-01-01

    The validation of Radar Cross Section (RCS) prediction techniques against real measurements is crucial to acquire confidence in predictions when measurements are nut available. In this paper we present the results of a comparison on one-dimensional signatures, i.e. radar range profiles. The profiles

  14. Analytic escrutineo for plaguicidas organofosforados in blood in forensic cases by means of SPME-GC/NPD

    International Nuclear Information System (INIS)

    Fernandez Quesada, K.; Saenz Ugalde, M. F.

    2003-01-01

    The plaguicidas organophosphorus represent one of the most important causes of intoxication in Costa Rica; 20% of the cases received in the Section of Toxicology of the Department of Forensic Sciences of the Organism of Judicial Investigation (OIJ) are related to these plaguicidas. At the present time, the employed techniques in this institution to carry out the organophosphorus analyses in blood, present important limitations in their analytic potential. As a consequence, it is necessary to look for new methodologies, with the purpose to obtain a great specificity, and to diminish the limits of detection. This would allow a more qualified service that assures the validity and reliability of the results. Besides, it is an ideal instrument for the correct administration of justice of the Judicial Authorities. In this final work of graduation, it develops a methodology for the scrutiny of pesticides organophosphorus, in which a sample of biological origin of forensic importance is used. This employs a technique of quick, simple and clean extraction, using a separation method of detection of high analytic sensibility. In the methodology's development, samples of total blood, and the microextraccion techniques in solid phase will be used (SPME), and detection with gas chromatography by a specific instrumental detector of match and nitrogen (GCINPD) [es

  15. Laser Ranging in Solar System: Technology Developments and New Science Measurement Capabilities

    Science.gov (United States)

    Sun, X.; Smith, D. E.; Zuber, M. T.; Mcgarry, J.; Neumann, G. A.; Mazarico, E.

    2015-12-01

    Laser Ranging has played a major role in geodetic studies of the Earth over the past 40 years. The technique can potentially be used in between planets and spacecrafts within the solar system to advance planetary science. For example, a direct measurement of distances between planets, such as Mars and Venus would make significant improvements in understanding the dynamics of the whole solar system, including the masses of the planets and moons, asteroids and their perturbing interactions, and the gravity field of the Sun. Compared to the conventional radio frequency (RF) tracking systems, laser ranging is potentially more accurate because it is much less sensitive to the transmission media. It is also more efficient because the laser beams are much better focused onto the targets than RF beams. However, existing laser ranging systems are all Earth centric, that is, from ground stations on Earth to orbiting satellites in near Earth orbits or lunar orbit, and to the lunar retro-reflector arrays deployed by the astronauts in the early days of lunar explorations. Several long distance laser ranging experiments have been conducted with the lidar in space, including a two-way laser ranging demonstration between Earth and the Mercury Laser Altimeter (MLA) on the MESSENGER spacecraft over 24 million km, and a one way laser transmission and detection experiment over 80 million km between Earth and the Mars Orbiting Laser Altimeter (MOLA) on the MGS spacecraft in Mars orbit. A one-way laser ranging operation has been carried out continuously from 2009 to 2014 between multiple ground stations to LRO spacecraft in lunar orbit. The Lunar Laser Communication Demonstration (LLCD) on the LADEE mission has demonstrated that a two way laser ranging measurements, including both the Doppler frequency and the phase shift, can be obtained from the subcarrier or the data clocks of a high speed duplex laser communication system. Plans and concepts presently being studied suggest we may be

  16. Smartphone-based accelerometry is a valid tool for measuring dynamic changes in knee extension range of motion

    DEFF Research Database (Denmark)

    Støve, Morten Pallisgaard; Palsson, Thorvaldur Skuli; Hirata, Rogerio Pessoto

    2018-01-01

    Introduction: Measurement of static joint range of motion is used extensively in orthopaedic and rehabilitative communities to benchmark treatment efficacy. Static measures are, however, insufficient in providing detailed information about patient impairments. Dynamic range of motion measures cou...

  17. Measuring Systems for Thermometer Calibration in Low-Temperature Range

    Science.gov (United States)

    Szmyrka-Grzebyk, A.; Lipiński, L.; Manuszkiewicz, H.; Kowal, A.; Grykałowska, A.; Jancewicz, D.

    2011-12-01

    The national temperature standard for the low-temperature range between 13.8033 K and 273.16 K has been established in Poland at the Institute of Low Temperature and Structure Research (INTiBS). The standard consists of sealed cells for realization of six fixed points of the International Temperature Scale of 1990 (ITS-90) in the low-temperature range, an adiabatic cryostat and Isotech water and mercury triple-point baths, capsule standard resistance thermometers (CSPRT), and AC and DC bridges with standard resistors for thermometers resistance measurements. INTiBS calibrates CSPRTs at the low-temperature fixed points with uncertainties less than 1 mK. In lower temperature range—between 2.5 K and about 25 K — rhodium-iron (RhFe) resistance thermometers are calibrated by comparison with a standard which participated in the EURAMET.T-K1.1 comparison. INTiBS offers a calibration service for industrial platinum resistance thermometers and for digital thermometers between 77 K and 273 K. These types of thermometers may be calibrated at INTiBS also in a higher temperature range up to 550°C. The Laboratory of Temperature Standard at INTiBS acquired an accreditation from the Polish Centre for Accreditation. A management system according to EN ISO/IEC 17025:2005 was established at the Laboratory and presented on EURAMET QSM Forum.

  18. Wind field reconstruction from nacelle-mounted lidar short-range measurements

    Directory of Open Access Journals (Sweden)

    A. Borraccino

    2017-05-01

    Full Text Available Profiling nacelle lidars probe the wind at several heights and several distances upstream of the rotor. The development of such lidar systems is relatively recent, and it is still unclear how to condense the lidar raw measurements into useful wind field characteristics such as speed, direction, vertical and longitudinal gradients (wind shear. In this paper, we demonstrate an innovative method to estimate wind field characteristics using nacelle lidar measurements taken within the induction zone. Model-fitting wind field reconstruction techniques are applied to nacelle lidar measurements taken at multiple distances close to the rotor, where a wind model is combined with a simple induction model. The method allows robust determination of free-stream wind characteristics. The method was applied to experimental data obtained with two different types of nacelle lidar (five-beam Demonstrator and ZephIR Dual Mode. The reconstructed wind speed was within 0.5 % of the wind speed measured with a mast-top-mounted cup anemometer at 2.5 rotor diameters upstream of the turbine. The technique described in this paper overcomes measurement range limitations of the currently available nacelle lidar technology.

  19. Baking enables McLeod gauge to measure in ultrahigh vacuum range

    Science.gov (United States)

    Kreisman, W. S.

    1965-01-01

    Accurate measurements in the ultrahigh vacuum range by a conventional McLeod gage requires degassing of the gage's glass walls. A closed system, in which mercury is forced into the gage by gravity alone, and in which the gage components are baked out for long periods, is used to achieve this degassing.

  20. Varying the item format improved the range of measurement in patient-reported outcome measures assessing physical function.

    Science.gov (United States)

    Liegl, Gregor; Gandek, Barbara; Fischer, H Felix; Bjorner, Jakob B; Ware, John E; Rose, Matthias; Fries, James F; Nolte, Sandra

    2017-03-21

    Physical function (PF) is a core patient-reported outcome domain in clinical trials in rheumatic diseases. Frequently used PF measures have ceiling effects, leading to large sample size requirements and low sensitivity to change. In most of these instruments, the response category that indicates the highest PF level is the statement that one is able to perform a given physical activity without any limitations or difficulty. This study investigates whether using an item format with an extended response scale, allowing respondents to state that the performance of an activity is easy or very easy, increases the range of precise measurement of self-reported PF. Three five-item PF short forms were constructed from the Patient-Reported Outcomes Measurement Information System (PROMIS®) wave 1 data. All forms included the same physical activities but varied in item stem and response scale: format A ("Are you able to …"; "without any difficulty"/"unable to do"); format B ("Does your health now limit you …"; "not at all"/"cannot do"); format C ("How difficult is it for you to …"; "very easy"/"impossible"). Each short-form item was answered by 2217-2835 subjects. We evaluated unidimensionality and estimated a graded response model for the 15 short-form items and remaining 119 items of the PROMIS PF bank to compare item and test information for the short forms along the PF continuum. We then used simulated data for five groups with different PF levels to illustrate differences in scoring precision between the short forms using different item formats. Sufficient unidimensionality of all short-form items and the original PF item bank was supported. Compared to formats A and B, format C increased the range of reliable measurement by about 0.5 standard deviations on the positive side of the PF continuum of the sample, provided more item information, and was more useful in distinguishing known groups with above-average functioning. Using an item format with an extended

  1. Range and number-of-levels effects in derived and stated measures of attribute importance

    NARCIS (Netherlands)

    Verlegh, PWJ; Schifferstein, HNJ; Wittink, DR

    We study how the range of variation and the number of ttribute levels affect five measures of attribute importance: full profile conjoint estimates, ranges in attribute level attractiveness ratings. regression coefficients. graded paired comparisons. and self-reported ratings, We find that all

  2. Effect of the type of frying culinary fat on volatile compounds isolated in fried pork loin chops by using SPME-GC-MS.

    Science.gov (United States)

    Ramírez, María Rosario; Estévez, Mario; Morcuende, David; Cava, Ramón

    2004-12-15

    The effect of the type of frying culinary fat (olive oil, sunflower oil, butter, and pig lard) on volatile compounds isolated from fried pork loin chops (m. Longissimus dorsi) was measured by SPME-GC-MS. Frying modified the fatty acid composition of lipids from pork loin chops, which tended to be similar to that of the culinary fat used to fry. Volatile compounds formed from the oxidation of fatty acids increased, such as aldehydes, ketones, alcohols, and hydrocarbons. Besides, each culinary fat used modified the volatile profiles in fried meat differently. Sunflower oil-fried pork loin chops presented the highest aldehyde aliphatic content, probably due to their highest content of polyunsaturated acids. Hexanal, the most abundant aldehyde in fried samples, presented the most elevated content in sunflower oil-fried pork loin chops. In addition, these samples presented more heterocyclic compounds from the Maillard reaction than other fried samples. Volatiles detected in olive oil-fried pork loin chops were mainly lipid-derived compounds such as pentan-1-ol, hexanal, hept-2-enal, nonanal, decanal, benzaldehyde, and nonan-2-one. Butter-fried pork loins were abundant in ketones with a high number of carbons (heptan-2-one, nonan-2-one, undecan-2-one, tridecanone, and heptadecan-2-one). Pig lard-fried pork loin chops presented some Strecker aldehydes isolated in only these samples, such as 2-methylbutanal and 3-(methylthio)propanal, and a sulfur compound (dimethyl disulfide) related to Strecker aldehydes.

  3. Generalized weighted ratio method for accurate turbidity measurement over a wide range.

    Science.gov (United States)

    Liu, Hongbo; Yang, Ping; Song, Hong; Guo, Yilu; Zhan, Shuyue; Huang, Hui; Wang, Hangzhou; Tao, Bangyi; Mu, Quanquan; Xu, Jing; Li, Dejun; Chen, Ying

    2015-12-14

    Turbidity measurement is important for water quality assessment, food safety, medicine, ocean monitoring, etc. In this paper, a method that accurately estimates the turbidity over a wide range is proposed, where the turbidity of the sample is represented as a weighted ratio of the scattered light intensities at a series of angles. An improvement in the accuracy is achieved by expanding the structure of the ratio function, thus adding more flexibility to the turbidity-intensity fitting. Experiments have been carried out with an 850 nm laser and a power meter fixed on a turntable to measure the light intensity at different angles. The results show that the relative estimation error of the proposed method is 0.58% on average for a four-angle intensity combination for all test samples with a turbidity ranging from 160 NTU to 4000 NTU.

  4. A hydrogel based nanosensor with an unprecedented broad sensitivity range for pH measurements in cellular compartments

    DEFF Research Database (Denmark)

    Zhang, M.; Søndergaard, Rikke Vicki; Ek, Pramod Kumar

    2015-01-01

    Optical pH nanosensors have been applied for monitoring intracellular pH in real-time for about two decades. However, the pH sensitivity range of most nanosensors is too narrow, and measurements that are on the borderline of this range may not be correct. Furthermore, ratiometric measurements...... of acidic intracellular pH (pH sensor, a fluorophore based nanosensor, with an unprecedented broad measurement range from pH 1.4 to 7.0. In this nanosensor, three p......H-sensitive fluorophores (difluoro-Oregon Green, Oregon Green 488, and fluorescein) and one pH-insensitive fluorophore (Alexa 568) were covalently incorporated into a nanoparticle hydrogel matrix. With this broad range quadruple-labelled nanosensor all physiological relevant pH levels in living cells can be measured...

  5. Thin-film microextraction coupled to LC-ESI-MS/MS for determination of quaternary ammonium compounds in water samples.

    Science.gov (United States)

    Boyacı, Ezel; Sparham, Chris; Pawliszyn, Janusz

    2014-01-01

    The dual nature of the quaternary ammonium compounds, having permanently charged hydrophilic quaternary ammonium heads and long-chain hydrophobic tails, makes the sample preparation step and analysis of these compounds challenging. A high-throughput method based on thin-film solid-phase microextraction (SPME) and liquid chromatography mass spectrometry was developed for simultaneous quantitative analysis of nine benzylic and aliphatic quaternary ammonium compounds. Chromatographic separation and detection of analytes were obtained in reverse-phase mode in 8 min using a triple quadrupole mass spectrometer. Hydrophilic lipophilic balance particle-coated blades were found to be the most suitable among the different coatings tested in terms of recoveries and carryover on the blades. For desorption solvents, 70/30, v/v (A/B) with 0.1 % formic acid (where A is 10 mM ammonium acetate in acetonitrile/water (95/5 , v/v) and B is 0.1 %  (v/v) formic acid in isopropyl alcohol) was shown to be the most efficient solvent for the desorption of the analytes from the SPME sorbent. The SPME method was optimised in terms of extraction, pH, and preconditioning, as well as extraction and desorption times. Optimum conditions were 45 min of extraction time and 15 min of desorption time, all with agitation. The extraction was found to be optimum in a range of pH 6.0 to 8.0, which is consistent with the natural pH of water samples. Wide linear dynamic ranges with the developed method were obtained for each compound, enabling the application of the method for a wide range of concentrations. The developed method was validated according to the Food and Drug Administration criteria. The proposed method is the first SPME-based approach describing the applicability of the high-throughput thin-film SPME in a 96-well system for analysis of such challenging compounds.

  6. Measurement range of phase retrieval in optical surface and wavefront metrology

    International Nuclear Information System (INIS)

    Brady, Gregory R.; Fienup, James R.

    2009-01-01

    Phase retrieval employs very simple data collection hardware and iterative algorithms to determine the phase of an optical field. We have derived limitations on phase retrieval, as applied to optical surface and wavefront metrology, in terms of the speed of beam (i.e., f-number or numerical aperture) and amount of aberration using arguments based on sampling theory and geometrical optics. These limitations suggest methodologies for expanding these ranges by increasing the complexity of the measurement arrangement, the phase-retrieval algorithm, or both. We have simulated one of these methods where a surface is measured at unusual conjugates

  7. Novel gravimetric measurement technique for quantitative volume calibration in the sub-microliter range

    International Nuclear Information System (INIS)

    Liang, Dong; Zengerle, Roland; Steinert, Chris; Ernst, Andreas; Koltay, Peter; Bammesberger, Stefan; Tanguy, Laurent

    2013-01-01

    We present a novel measurement method based on the gravimetric principles adapted from the ASTM E542 and ISO 4787 standards for quantitative volume determination in the sub-microliter range. Such a method is particularly important for the calibration of non-contact micro dispensers as well as other microfluidic devices. The novel method is based on the linear regression analysis of continuously monitored gravimetric results and therefore is referred to as ‘gravimetric regression method (GRM)’. In this context, the regression analysis is necessary to compensate the mass loss due to evaporation that is significant for very small dispensing volumes. A full assessment of the measurement uncertainty of GRM is presented and results in a standard measurement uncertainty around 6 nl for dosage volumes in the range from 40 nl to 1 µl. The GRM has been experimentally benchmarked with a dual-dye ratiometric photometric method (Artel Inc., Westbrook, ME, USA), which can provide traceability of measurement to the International System of Units (SI) through reference standards maintained by NIST. Good precision (max. CV = 2.8%) and consistency (bias around 7 nl in the volume range from 40 to 400 nl) have been observed comparing the two methods. Based on the ASTM and ISO standards on the one hand and the benchmark with the photometric method on the other hand, two different approaches for establishing traceability for the GRM are discussed. (paper)

  8. Effect of water content on thermal oxidation of oleic acid investigated by combination of EPR spectroscopy and SPME-GC-MS/MS.

    Science.gov (United States)

    Chen, Hongjian; Cao, Peirang; Li, Bo; Sun, Dewei; Wang, Yong; Li, Jinwei; Liu, Yuanfa

    2017-04-15

    Promotion of water to the thermal oxidation of oleic acid was detected by the combination of EPR, SPME-GC-MS/MS and GC. Spin-trapping technique was used to identify and quantify the radical species formed during thermal oxidation of oleic acid by using DMPO as electron spin trap. The most abundant radical species were identified as DMPO-alkyl radical adducts. EPR intensity plateau of the samples with 5% water content was 140% higher than the samples without water. It implies oleic acid samples with high water content had high level of oxidation rates. The proportion of aldehydes of the samples with 2% water content was the maximum about 59.97%. Among the formed products, (E,E)-2,4-decadienal has genotoxic and cytotoxic effects, whose percentage was nearly twice comparing with that of 5-0% water content. This study demonstrated that higher water content in frying systems would contribute to seriously oxidation and degradation of oleic acids. Copyright © 2016 Elsevier Ltd. All rights reserved.

  9. Solid-phase microextraction of Methylene Blue using carboxy graphene-modified steel wires, and its detection by electrochemiluminescence

    International Nuclear Information System (INIS)

    Wang, Sui; Lv, Shasha; Guo, Zhiyong; Jiang, Feng

    2014-01-01

    We report on a new solid phase for microextraction (SPME) of Methylene Blue (MB). It was obtained by immobilizing carboxy graphene (G-COOH) on a stainless steel wire. Scanning electron micrography showed the surface to be homogeneous, porous and wrinkled. The effects of sample solution pH, extraction time, stirring rate, desorption time and of desorption solvent on the efficiency of extraction of MB were optimized. The new SPME was coupled to electrochemiluminescence detection of MB and gave a linear analytical range from 2.7 nM to 1.3 μM, and the detection limit is 0.89 nM which is better than other methods. When considering the enrichment factor of ∼20, the resulting detection limit is estimated to be 45 pM. The new SPME fiber was successfully applied to the analysis of MB in spiked real water samples. Recoveries range from 95.7 % to 113.0 %, and relative standard deviations are <5.0 %, which showed the good reproducibility of the method. (author)

  10. EVALUACIÓN DE PLAGUICIDAS 0RGAN0CL0RAD0S POR HS-SPME - GC/ECD EN LECHE PASTEURIZADA COMERCIALIZADA EN LA CIUDAD DE CARTAGENA (COLOMBIA A AVALIAQÁO DOS PESTICIDAS ORGANOCLORADOS POR HS-SPME - GC/ECD EM LEITE PASTEURIZADO COMERCIALIZADAS NA CIDADE CARTAGENA (COLOMBIA EVALUATION OF PESTICIDES BY HS-SPME ORGANOCHLORINE - GC / ECD IN PASTEURIZED MILK MARKETED IN THE CITY CARTAGENA (COLOMBIA

    Directory of Open Access Journals (Sweden)

    DENILES DEL CARMEN DE ARCO R

    2011-12-01

    Full Text Available Los plaguicidas han sido utilizados en todo el mundo desde mediados del siglo XX, en campañas de Salud Pública y en prácticas agrícolas. Los Plaguicidas Organoclorados (POCs presentan mayor impacto sobre el ambiente porque no son biodegradables, son lipofílicos, tienen gran movilidad por todo el planeta y gran tendencia a la bioacumulación, através de la cadena trófica. Con el objetivo de identificar y cuantificar plaguicidas organoclorados en leche entera pasteurizada de dos marcas (A y B, que se comercializan en la ciudad de Cartagena de Indias, se realizó la presente investigación, utilizando Microextracción en Fase Sólida en Espacio de Cabeza y Cromatografía de Gases con Detector de Captura de Electrones (HS-SPME-GC/ECD. Fueron analizadas 36 muestras (n=36, 18 de cada marca. El 100% de las muestras (n=36 resultaron positivas para el plaguicida lindano (γ-HCH, superando el Límite Máximo Residual (LMR de 0,01 mg/kg, establecido por la Food and Agriculture Organization y la Organización Mundial de la Salud (FAO/OMS. Las concentraciones promedio de lindano obtenidas para la marca A fueron de 0,042 mg/kg ± 0,003 y 0,062 ± 0,0016 mg/kg (base grasa para la marca B, no superando la Ingesta Diaria Admisible (IDA de 0,001 mg/kg de peso corporal.Os pesticidas têm sido usados em todo o mundo desde meados do século XX, as campanhas de saúde pública e práticas agrícolas. Os inseticidas organoclorados (AP têm maior impacto sobre o meio ambiente porque não são biodegradáveis, são lipofílicas, têm grande mobilidade ao redor do mundo e maior tendencia para a bioacumulação através da cadeia alimentar. A fim de identificar e quantificar pesticidas organoclorados em leite integral, duas marcas (A e B, comercializada na cidade de Cartagena das Índias, a presente investigação foi realizada por cromatografia em Fase Sólida, Microextração Headspace Gás com Detector de Captura de Elétrons(HS-SPME-GC/ECD. 36 amostras foram

  11. An impedance bridge measuring the capacitance ratio in the high frequency range up to 1 MHz

    International Nuclear Information System (INIS)

    Kim, Dan Bee; Lee, Hyung Kew; Kim, Wan-Seop

    2017-01-01

    This paper describes a 2-terminal-pair impedance bridge, measuring the capacitance ratio in the high frequency range up to 1 MHz. The bridge was configured with two voltage sources and a phase control unit which enabled the bridge balance by synchronizing the voltage sources with an enhanced phase resolution. Without employing the transformers such as inductive voltage divider, injection and detection transformers, etc, the bridge system is quite simple to set up, and the balance procedure is quick and easy. Using this dual-source coaxial bridge, the 1:1 and 10:1 capacitance ratios were measured with 1 pF–1 nF capacitors in the frequency range from 1 kHz to 1 MHz. The measurement values obtained by the dual-source bridge were then compared with reference values measured using a commercial precision capacitance bridge of AH2700A, the Z -matrix method developed by ourselves, and the 4-terminal-pair coaxial bridge by the Czech Metrological Institute. All the measurements agreed within the reference uncertainty range of an order of 10 −6 –10 −5 , proving the bridge ability as a trustworthy tool for measuring the capacitance ratio in the high frequency range. (paper)

  12. Varying the item format improved the range of measurement in patient-reported outcome measures assessing physical function

    DEFF Research Database (Denmark)

    Liegl, Gregor; Gandek, Barbara; Fischer, H. Felix

    2017-01-01

    precision between the short forms using different item formats. Results: Sufficient unidimensionality of all short-form items and the original PF item bank was supported. Compared to formats A and B, format C increased the range of reliable measurement by about 0.5 standard deviations on the positive side...

  13. Human-Induced Effects on RSS Ranging Measurements for Cooperative Positioning

    DEFF Research Database (Denmark)

    Della Rosa, Francescantonio; Pelosi, Mauro; Nurmi, Jari

    2012-01-01

    of human-induced perturbations for enhancing the final positioning accuracy through cooperative schemes has been assessed. It has been proved that the effect of cooperation is very limited if human factors are not taken into account when performing experimental activities.......We present experimental evaluations of human-induced perturbations on received-signal-strength-(RSS-) based ranging measurements for cooperative mobile positioning. To the best of our knowledge, this work is the first attempt to gain insight and understand the impact of both body loss and hand grip...... on the RSS for enhancing proximity measurements among neighbouring devices in cooperative scenarios. Our main contribution is represented by experimental investigations. Analysis of the errors introduced in the distance estimation using path-loss-based methods has been carried out. Moreover, the exploitation...

  14. New Methyltrimethoxysilane-(3-Mercaptopropyl)- Trimethoxysilane Coated Hollow Fiber-Solid Phase Micro extraction for Hexanal and Heptanal Analysis

    International Nuclear Information System (INIS)

    Siti Munirah Abd Wahib; Mohd Marsin Sanagi

    2016-01-01

    Determination of volatile organic compounds (VOCs) in various matrices is often accomplished using solid phase micro extraction (SPME) as a superior mode of extraction. Alternatively, another configuration of solid phase micro extraction (SPME) namely hollow fiber-solid phase micro extraction (HF-SPME) is a great approach to redress some limitations of the ordinary SPME fibers including fiber breakage, coating stripping and sample carry over. The HF-SPME technique highlights the use of hollow polypropylene (PP) membrane to hold and protect the adsorbent inside its lumen. Unlike the conventional SPME, the inexpensive HF device can be disposed after single use. Introducing extracting phase via sol-gel technology has gained great interest owing to its simple preparation method and promising way to obtain materials with good characteristics. In the present work, a new hybrid silica material based on methyltrimethoxysilane-(3-mercaptopropyl)trimethoxysilane (MTMOS-MPTMOS) was introduced as a new extractant of HF-SPME and the effectiveness of the proposed method was tested for analysis of hexanal and heptanal as the target VOC analytes. Preparation of the HF-SPME MTMOS-MPTMOS was simple in which the hybrid material was synthesized via sol-gel method and was self-polymerized in small segments of HF. Parameters affecting the efficiency of the HF-SPME MTMOS-MPTMOS in extracting both aldehydes were thoroughly investigated and analyzed by gas chromatography-flame ionization detection (GC-FID). It was found that the highest efficiency was achieved as the extraction was conducted in 30 min at a stirring rate of 1000 rpm in a 10 mL of sample solution whereby the back-extraction was performed via vortex for 3 min using 100 μL methanol as desorption solvent. Under the optimal conditions, linearity was observed over a range of 0.020-10.00 μg mL"-"1 with detection limits of 0.015 μg mL"-"1 and 0.010 μg mL"-"1 for hexanal and heptanal, respectively. The applicability of the HF-SPME

  15. Farmed and wild sea bass (Dicentrarchus labrax) volatile metabolites: a comparative study by SPME-GC/MS.

    Science.gov (United States)

    Vidal, Natalia P; Manzanos, María J; Goicoechea, Encarnación; Guillén, María D

    2016-03-15

    Farmed and wild European sea bass (Dicentrarchus labrax) could be distinguished by its volatile metabolites, an issue not addressed until now. The aim of this work was to study these metabolites by solid-phase microextraction followed by gas chromatography/mass spectrometry (SPME-GC/MS). Both farmed and wild sea bass have a great number of volatile metabolites, most of them being in low concentrations. These include alcohols, aldehydes, ketones, alkylfurans, acids, aliphatic and aromatic hydrocarbons, terpenes, sulfur and nitrogen derivatives, 2,6-di-tert-butyl-4-methylphenol and one derived compound, as well as 2,4,7,9-tetramethyl-5-decyne-4,7-diol, this latter compound presumably resulting from environmental contamination. Important differences have been detected between both types of sea bass, and also among individuals inside each group. Farmed specimens are richer in volatile metabolites than the wild counterparts; however, these latter, in general, contain a high number and abundance of metabolites resulting from microbial and enzymatic non-oxidative activity than the former. Clear differences in the volatile metabolites of wild and farmed sea bass have been found. A great deal of valuable information on sea bass volatile metabolites has been obtained, which can be useful in understanding certain aspects of the quality and safety of raw and processed sea bass. © 2015 Society of Chemical Industry.

  16. Measurement based scenario analysis of short-range distribution system planning

    DEFF Research Database (Denmark)

    Chen, Peiyuan; Bak-Jensen, Birgitte; Chen, Zhe

    2009-01-01

    This paper focuses on short-range distribution system planning using a probabilistic approach. Empirical probabilistic distributions of load demand and distributed generations are derived from the historical measurement data and incorporated into the system planning. Simulations with various...... feasible scenarios are performed based on a local distribution system at Støvring in Denmark. Simulation results provide more accurate and insightful information for the decision-maker when using the probabilistic analysis than using the worst-case analysis, so that a better planning can be achieved....

  17. Improved measurement linearity and precision for AMCW time-of-flight range imaging cameras.

    Science.gov (United States)

    Payne, Andrew D; Dorrington, Adrian A; Cree, Michael J; Carnegie, Dale A

    2010-08-10

    Time-of-flight range imaging systems utilizing the amplitude modulated continuous wave (AMCW) technique often suffer from measurement nonlinearity due to the presence of aliased harmonics within the amplitude modulation signals. Typically a calibration is performed to correct these errors. We demonstrate an alternative phase encoding approach that attenuates the harmonics during the sampling process, thereby improving measurement linearity in the raw measurements. This mitigates the need to measure the system's response or calibrate for environmental changes. In conjunction with improved linearity, we demonstrate that measurement precision can also be increased by reducing the duty cycle of the amplitude modulated illumination source (while maintaining overall illumination power).

  18. CFD comparison with centrifugal compressor measurements on a wide operating range

    Directory of Open Access Journals (Sweden)

    Arnou D.

    2013-04-01

    Full Text Available Centrifugal compressors are widely used in industrial applications thanks to their high efficiency. They are able to provide a wide operating range before reaching the flow barrier or surge limits. Performances and range are described by compressor maps obtained experimentally. After a description of performance test rig, this article compares measured centrifugal compressor performances with computational fluid dynamics results. These computations are performed at steady conditions with R134a refrigerant as fluid. Navier-Stokes equations, coupled with k-ε turbulence model, are solved by the commercial software ANSYS-CFX by means of volume finite method. Input conditions are varied in order to calculate several speed lines. Theoretical isentropic efficiency and theoretical surge line are finally compared to experimental data.

  19. Effect of hot air drying on volatile compounds of Flammulina velutipes detected by HS-SPME-GC-MS and electronic nose.

    Science.gov (United States)

    Yang, Wenjian; Yu, Jie; Pei, Fei; Mariga, Alfred Mugambi; Ma, Ning; Fang, Yong; Hu, Qiuhui

    2016-04-01

    Volatile compounds are important factors that affect the flavor quality of Flammulina velutipes, but the changes occurring during hot air drying is still unclear. To clarify the dynamic changes of flavor components during hot air drying, comprehensive flavor characterization and volatile compounds of F. velutipes were evaluated using electronic nose technology and headspace solid phase micro-extraction combined with gas chromatography-mass spectrometry (HS-SPME-GC-MS), respectively. Results showed that volatile components in F. velutipes significantly changed during hot air drying according to the principal component analysis and radar fingerprint chart of electronic nose. Volatile compounds of fresh F. velutipes consisted mainly of ketones, aldehydes and alcohols, and 3-octanone was the dominant compound. Drying process could significantly decrease the relative content of ketones and promoted the generation of alcohols, acids, and esters, which became the main volatile compounds of dried F. velutipes. These may provide a theoretical basis for the formation mechanism of flavor substances in dried F. velutipes. Copyright © 2015 Elsevier Ltd. All rights reserved.

  20. Rapid evaluation technique to differentiate mushroom disease-related moulds by detecting microbial volatile organic compounds using HS-SPME-GC-MS.

    Science.gov (United States)

    Radványi, Dalma; Gere, Attila; Jókai, Zsuzsa; Fodor, Péter

    2015-01-01

    Headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC-MS) was used to analyse microbial volatile organic compounds (MVOCs) of mushroom disease-related microorganisms. Mycogone perniciosa, Lecanicillum fungicola var. fungicola, and Trichoderma aggressivum f. europaeum species, which are typically harmful in mushroom cultivation, were examined, and Agaricus bisporus (bisporic button mushroom) was also examined as a control. For internal standard, a mixture of alkanes was used; these were introduced as the memory effect of primed septa in the vial seal. Several different marker compounds were found in each sample, which enabled us to distinguish the different moulds and the mushroom mycelium from each other. Monitoring of marker compounds enabled us to investigate the behaviour of moulds. The records of the temporal pattern changes were used to produce partial least squares regression (PLS-R) models that enabled determination of the exact time of contamination (the infection time of the media). Using these evaluation techniques, the presence of mushroom disease-related fungi can be easily detected and monitored via their emitted MVOCs.

  1. Characterization of volatile profile from ten different varieties of Chinese jujubes by HS-SPME/GC-MS coupled with E-nose.

    Science.gov (United States)

    Chen, Qinqin; Song, Jianxin; Bi, Jinfeng; Meng, Xianjun; Wu, Xinye

    2018-03-01

    Volatile profile of ten different varieties of fresh jujubes was characterized by HS-SPME/GC-MS (headspace solid phase micro-extraction combined with gas chromatography-mass spectrometry) and E-nose (electronic nose). GC-MS results showed that a total of 51 aroma compounds were identified in jujubes, hexanoic acid, hexanal, (E)-2-hexenal, (Z)-2-heptenal, benzaldehyde and (E)-2-nonenal were the main aroma components with contributions that over 70%. Differentiation of jujube varieties was conducted by cluster analysis of GC-MS data and principal component analysis & linear discriminant analysis of E-nose data. Both results showed that jujubes could be mainly divided into two groups: group A (JZ, PDDZ, JSXZ and LWZZ) and group B (BZ, YZ, MZ, XZ and DZ). There were significant differences in contents of alcohols, acids and aromatic compounds between group A and B. GC-MS coupled with E-nose could be a fast and accurate method to identify the general flavor difference in different varieties of jujubes. Copyright © 2017 Elsevier Ltd. All rights reserved.

  2. Lifetime measurements in the picosecond range: achievements and perspectives

    International Nuclear Information System (INIS)

    Kruecken, R.

    2000-01-01

    Recent developments in the measurement of lifetimes in the picosecond range using the recoil distance method (RDM) are reviewed. Results from recent RDM experiments on superdeformed bands in the mass-190 region, shears, bands in the neutron deficient lead isotopes, and ground state bands in the mass-130 region are presented. New experimental devices for lifetime experiments at Yale, such as the New Yale Plunger Device (N.Y.P.D.), the SPEctrometer for Doppler-shift Experiments at Yale (SPEEDY) and the plans for the gas-filled recoil separator SASSYER are presented. Perspectives for the use of the RDM technique in the study of exotic nuclei and its potential use with radioactive beams are discussed. (author)

  3. Investigation of fractional momentum transfer: measurement of forward recoil ranges in 16O + natTm collisions

    International Nuclear Information System (INIS)

    Singh, Pushpendra P.; Unnati; Sharma, Manoj Kumar; Singh, B.P.; Prasad, R.; Rakesh Kumar; Golda, K.S.; Bhardwaj, H.D.

    2006-01-01

    For better understanding of complete fusion and incomplete fusion in heavy ion reactions a programme of precise measurements of excitation functions, recoil range distribution and angular distributions of recoils has been undertaken. In the present contribution the recoil range distribution for the residues have been measured at ≅ 6 MeV/nucleon, using recoil-catcher technique followed by off-line gamma-spectroscopy

  4. Detection of DDT and its metabolites in two estuaries of South China using a SPME-based device: First report of p,p'-DDMU in water column

    International Nuclear Information System (INIS)

    Xing Yuanna; Guo Ying; Xie Mei; Shen Rulang; Zeng, Eddy Y.

    2009-01-01

    A solid-phase microextration-based sampling method was employed to determine the concentrations of 1,1,1-trichloro-2,2-bis(p-chlorophenyl)ethane (DDT) and its metabolites, 1,1-dichloro-2,2-bis(p-chlorophenyl)ethane (DDD), 1,1-dichloro-2,2-bis(p-chlorophenyl)ethene (DDE) and 1-chloro-2,2-bis(p-chlorophenyl)ethene (DDMU), in two estuarine bays, Daya Bay and Hailing Bay, of South China. Six DDT components including p,p'-DDT, o,p'-DDD, p,p'-DDD, o,p'-DDE, p,p'-DDE, and p,p'-DDMU were detected in Hailing Bay, while only p,p'-DDD was found in Daya Bay. p,p'-DDD was the most abundant DDT component in both bays, sharply different from the previous finding in the water column of the Palos Verdes Shelf, California, USA that p,p'-DDE was prevalent. In addition, the occurrence of p,p'-DDMU (with a range of 0.047-0.21 ng/L in Hailing Bay) has not been reported around the globe, and its presence in our study region appeared to stem from dehydrochlorination of p,p'-DDD, favored under aerobic conditions, but further investigations are clearly needed to confirm the mechanism for generation of DDMU in estuarine environments. - DDT and its metabolites, particularly p,p'-DDMU, are detected in the water column of two estuarine bays in South China using a SPME-based sampler

  5. Differentiation of Commercial PDO Wines Produced in Istria (Croatia) According to Variety and Harvest Year Based on HS-SPME-GC/MS Volatile Aroma Compound Profiling.

    Science.gov (United States)

    Lukić, Igor; Horvat, Ivana

    2017-03-01

    To differentiate monovarietal wines made from native and introduced varieties in Istria (Croatia), samples of Malvazija istarska, Chardonnay and Muscat yellow from two harvest years (2013 and 2014) were subjected to headspace solid-phase microextraction and gas chromatographic/mass spectrometric analysis (HS-SPME-GC/MS) of volatile aroma compounds. Significant effects of variety and harvest year were determined, but their interaction complicated the differentiation. Particular compounds were consistent as markers of variety in both years: nerol for Malvazija, ethyl cinnamate and a tentatively identified isomer of dimethylbenzaldehyde for Chardonnay, and terpenes for Muscat yellow. Wines from 2013 contained higher concentrations of the majority of important volatiles. A 100% correct differentiation of Malvazija istarska and Chardonnay wines according to both variety and harvest year was achieved by stepwise linear discriminant analysis.

  6. Application of solid-phase microextraction in analytical toxicology.

    Science.gov (United States)

    Pragst, Fritz

    2007-08-01

    Solid-phase microextraction (SPME) is a miniaturized and solvent-free sample preparation technique for chromatographic-spectrometric analysis by which the analytes are extracted from a gaseous or liquid sample by absorption in, or adsorption on, a thin polymer coating fixed to the solid surface of a fiber, inside an injection needle or inside a capillary. In this paper, the present state of practical performance and of applications of SPME to the analysis of blood, urine, oral fluid and hair in clinical and forensic toxicology is reviewed. The commercial coatings for fibers or needles have not essentially changed for many years, but there are interesting laboratory developments, such as conductive polypyrrole coatings for electrochemically controlled SPME of anions or cations and coatings with restricted-access properties for direct extraction from whole blood or immunoaffinity SPME. In-tube SPME uses segments of commercial gas chromatography (GC) capillaries for highly efficient extraction by repeated aspiration-ejection cycles of the liquid sample. It can be easily automated in combination with liquid chromatography but, as it is very sensitive to capillary plugging, it requires completely homogeneous liquid samples. In contrast, fiber-based SPME has not yet been performed automatically in combination with high-performance liquid chromatography. The headspace extractions on fibers or needles (solid-phase dynamic extraction) combined with GC methods are the most advantageous versions of SPME because of very pure extracts and the availability of automatic samplers. Surprisingly, substances with quite high boiling points, such as tricyclic antidepressants or phenothiazines, can be measured by headspace SPME from aqueous samples. The applicability and sensitivity of SPME was essentially extended by in-sample or on-fiber derivatization. The different modes of SPME were applied to analysis of solvents and inhalation narcotics, amphetamines, cocaine and metabolites

  7. Determinação de pesticidas organofosforados em água usando microextração em fase sólida e CGAR-EM Determination of organophosphorus pesticides in water using SPME-GC-MS

    Directory of Open Access Journals (Sweden)

    Fernando Carvalho Silva

    1999-04-01

    Full Text Available Solid-phase microextraction (SPME has been applied to direct extraction of 11 organophosphorus pesticides in water using a 100 mm fiber polydimethylsiloxane. The method was evaluated with respect time of exposure, detection limits (LODs, linearity and precision. The detection limits (S/N = 3 depend of each pesticide and varie about ng/L levels. The linearity was satisfactory with coefficients of correlation usually greater than 0.993. The precision of the method was determined by extraction from 4.0 mg/L aqueous standard with coefficients of variation between 5.7 to 17.2%.

  8. Quantitative Profiling of Ester Compounds Using HS-SPME-GC-MS and Chemometrics for Assessing Volatile Markers of the Second Fermentation in Bottle.

    Science.gov (United States)

    Muñoz-Redondo, José Manuel; Cuevas, Francisco Julián; León, Juan Manuel; Ramírez, Pilar; Moreno-Rojas, José Manuel; Ruiz-Moreno, María José

    2017-04-05

    A quantitative approach using HS-SPME-GC-MS was performed to investigate the ester changes related to the second fermentation in bottle. The contribution of the type of base wine to the final wine style is detailed. Furthermore, a discriminant model was developed based on ester changes according to the second fermentation (with 100% sensitivity and specificity values). The application of a double-check criteria according to univariate and multivariate analyses allowed the identification of potential volatile markers related to the second fermentation. Some of them presented a synthesis-ratio around 3-fold higher after this period and they are known to play a key role in wine aroma. Up to date, this is the first study reporting the role of esters as markers of the second fermentation. The methodology described in this study confirmed its suitability for the wine aroma field. The results contribute to enhance our understanding of this fermentative step.

  9. Optimization of the HS-SPME-GC/MS technique for the analysis of volatile compounds in caprine Coalho cheese using response surface methodology

    Directory of Open Access Journals (Sweden)

    Taliana Kênia Alves BEZERRA

    2016-03-01

    Full Text Available Abstract Caprine Coalho cheese presents great potential for a typical protected designation of origin, considering that this traditional Brazilian cheese presents a slightly salty and acid flavor, combined with a unique texture. This study optimized the HS-SPME-GC-MS methodology for volatile analysis of Coalho cheese, which can be used as a tool to help in the identification of the distinctive aroma profile of this cheese. The conditions of equilibrium time, extraction temperature and time were optimized using the statistical tool factorial experimental design 23, and applying the desirability function. After the evaluation, it was concluded that the optimum extraction conditions comprised equilibrium and extraction time of 20 and 40 minutes, respectively; and ideal extraction temperature of 45 °C. The optimum extraction of volatile compounds in goat Coalho cheese captured 32 volatile compounds: 5 alcohols, 5 esters, 3 ketones, 6 acids, 3 aldehydes, 3 terpenes, and 7 hydrocarbons.

  10. Characterization of French and Spanish dry-cured hams: influence of the volatiles from the muscles and the subcutaneous fat quantified by SPME-GC.

    Science.gov (United States)

    Sánchez-Peña, Carolina M; Luna, Guadalupe; García-González, Diego L; Aparicio, Ramón

    2005-04-01

    The influence of the volatile compounds on the characterization of Spanish and French dry-cured hams was studied. Thirty volatiles were quantified in each one of four locations (biceps femoris, semimembranosus and semitendinosus muscles and subcutaneous fat) of 29 dry-cured hams by solid-phase microextraction gas-chromatography (SPME-GC). The Brown-Forsythe univariate test allowed determination of the volatiles that individually could characterize (p0.95), then selected the most remarkable volatile compounds. Four compounds from the subcutaneous fat (methyl benzene and octanol) and the semitendinosus muscle (2-butanone and 2-octanone) allowed 100% correct classifications by geographic origin. On the other hand, only two compounds from the subcutaneous fat (octanol) and the biceps femoris muscle (3-methyl 1-butanol) correctly classified all the samples by the breed type. The ability of these variables to classify the samples was checked by the unsupervised procedure of principal components.

  11. Polymeric pH nanosensor with extended measurement range bearing octaarginine as cell penetrating peptide

    DEFF Research Database (Denmark)

    Ke, Peng; Sun, Honghao; Liu, Mingxing

    2016-01-01

    A synthetic peptide octaarginine which mimics human immunodeficiency virus-1, Tat protein is used as cell penetrating moiety for new pH nanosensors which demonstrate enhanced cellular uptake and expanded measurement range from pH 3.9 to pH 7.3 by simultaneously incorporating two complemental pH-s......H-sensitive fluorophores in a same nanoparticle. The authors believe that this triple fluorescent pH sensor provides a new tool to pH measurements that can have application in cellular uptake mechanism study and new nanomedicine design.......A synthetic peptide octaarginine which mimics human immunodeficiency virus-1, Tat protein is used as cell penetrating moiety for new pH nanosensors which demonstrate enhanced cellular uptake and expanded measurement range from pH 3.9 to pH 7.3 by simultaneously incorporating two complemental p...

  12. A Newly Designed Fiber-Optic Based Earth Pressure Transducer with Adjustable Measurement Range

    Directory of Open Access Journals (Sweden)

    Hou-Zhen Wei

    2018-03-01

    Full Text Available A novel fiber-optic based earth pressure sensor (FPS with an adjustable measurement range and high sensitivity is developed to measure earth pressures for civil infrastructures. The new FPS combines a cantilever beam with fiber Bragg grating (FBG sensors and a flexible membrane. Compared with a traditional pressure transducer with a dual diaphragm design, the proposed FPS has a larger measurement range and shows high accuracy. The working principles, parameter design, fabrication methods, and laboratory calibration tests are explained in this paper. A theoretical solution is derived to obtain the relationship between the applied pressure and strain of the FBG sensors. In addition, a finite element model is established to analyze the mechanical behavior of the membrane and the cantilever beam and thereby obtain optimal parameters. The cantilever beam is 40 mm long, 15 mm wide, and 1 mm thick. The whole FPS has a diameter of 100 mm and a thickness of 30 mm. The sensitivity of the FPS is 0.104 kPa/με. In addition, automatic temperature compensation can be achieved. The FPS’s sensitivity, physical properties, and response to applied pressure are extensively examined through modeling and experiments. The results show that the proposed FPS has numerous potential applications in soil pressure measurement.

  13. A High Dynamic-Range Beam Position Measurement System for ELSA-2

    CERN Document Server

    Balleyguier, P; Guimbal, P; Borrion, H

    2003-01-01

    New beamlines are presently under construction for ELSA, a 20 MeV electron linac located at Bruyères-le-Châtel. These lines need a beam position measurement system filling the following requirements: small footprint, wide dynamic range, single-bunch/multi-bunch capability, simple design. We designed a compact 4-stripline sensor and an electronic treatment chain based on logarithmic amplifiers. This paper presents the design, cold and hot test results.

  14. Comparison of two methods of surface profile extraction from multiple ultrasonic range measurements

    NARCIS (Netherlands)

    Barshan, B; Baskent, D

    Two novel methods for surface profile extraction based on multiple ultrasonic range measurements are described and compared. One of the methods employs morphological processing techniques, whereas the other employs a spatial voting scheme followed by simple thresholding. Morphological processing

  15. Measurement of the Lense-Thirring drag on high-altitude, laser-ranged artificial satellites

    International Nuclear Information System (INIS)

    Ciufolini, I.

    1986-01-01

    We describe a new method of measuring the Lense-Thirring relativistic nodal drag using LAGEOS together with another high-altitude, laser-ranged, similar satellite with appropriately chosen orbital parameters. We propose, for this purpose, that a future satellite such as LAGEOS II have an inclination supplementary to that of LAGEOS. The experiment proposed here would provide a method for experimental verification of the general relativistic formulation of Mach's principle and measurement of the gravitomagnetic field

  16. Aplicação de SPME (Solid Phase Micro-Extraction na análise de águas potáveis de três localidades do estado de São Paulo

    Directory of Open Access Journals (Sweden)

    Valente Antonio Luiz Pires

    1998-01-01

    Full Text Available The technique of solid phase microextraction (SPME was used for the extraction of halogenated contaminants of water samples from three cities of the State of São Paulo and the extracts were submitted to gas chromatographic analysis with electron capture detection (GC-ECD. In the samples of water collected at the city of São Paulo the detected level of trihalomethanes (THM expressed as the sum of chloroform, dibromochloromethane and dichlorobromomethane, were higher than the permissible limit established by the Brazilian regulation. In the samples collected at the two other cities the level of any of the three THM remained below the sensitivity of the ECD.

  17. Sensitivity analysis of nacelle lidar free stream wind speed measurements to wind-induction reconstruction model and lidar range configuration

    DEFF Research Database (Denmark)

    Svensson, Elin; Borraccino, Antoine; Meyer Forsting, Alexander Raul

    The sensitivity of nacelle lidar wind speed measurements to wind-induction models and lidar range configurations is studied using experimental data from the Nørrekær Enge (NKE) measurement campaign and simulated lidar data from Reynold-Averaged Navier Stokes (RANS) aerodynamic computational fluid...... the ZDM was configured to measure at five distances. From the configured distances, a large number of range configurations were created and systematically tested to determine the sensitivity of the reconstructed wind speeds to the number of ranges, minimum range and maximum range in the range......) of the fitting residuals. The results demonstrate that it is not possible to use RANS CFD simulated lidar data to determine optimal range configurations for real-time nacelle lidars due to their perfect (unrealistic) representation of the simulated flow field. The recommended range configurations are therefore...

  18. Preparation and characterization of sodium dodecyl sulfate doped polypyrrole solid phase micro extraction fiber and its application to endocrine disruptor pesticide analysis.

    Science.gov (United States)

    Korba, Korcan; Pelit, Levent; Pelit, Füsun Okçu; Ozdokur, K Volkan; Ertaş, Hasan; Eroğlu, Ahmet E; Ertaş, F Nil

    2013-06-15

    A robust in house solid-phase micro extraction (SPME) surface has been developed for the headspace (HS)-SPME determination of endocrine disruptor pesticides, namely, Chlorpyrifos, Penconazole, Procymidone, Bromopropylate and Lambda-Cyhalothrin in wine sample by using sodium dodecylsulfate doped polypyrrole SPME fiber. Pyrrole monomer was electrochemically polymerized on a stainless steel wire in laboratory conditions in virtue of diminishing the cost and enhancing the analyte retention on its surface to exert better selectivity and hence the developed polymerized surface could offer to analyst to exploit it as a fiber in headspace SPME analysis. The parameters, mainly, adsorption temperature and time, desorption temperature, stirring rate and salt amount were optimized to be as 70°C and 45min, 200°C, 600rpm and 10gL(-1), respectively. Limit of detection was estimated in the range of 0.073-1.659ngmL(-1) for the pesticides studied. The developed method was applied in to red wine sample with acceptable recovery values (92-107%) which were obtained for these selected pesticides. Copyright © 2013 Elsevier B.V. All rights reserved.

  19. Approach for measuring the chemistry of individual particles in the size range critical for cloud formation.

    Science.gov (United States)

    Zauscher, Melanie D; Moore, Meagan J K; Lewis, Gregory S; Hering, Susanne V; Prather, Kimberly A

    2011-03-15

    Aerosol particles, especially those ranging from 50 to 200 nm, strongly impact climate by serving as nuclei upon which water condenses and cloud droplets form. However, the small number of analytical methods capable of measuring the composition of particles in this size range, particularly at the individual particle level, has limited our knowledge of cloud condensation nuclei (CCN) composition and hence our understanding of aerosols effect on climate. To obtain more insight into particles in this size range, we developed a method which couples a growth tube (GT) to an ultrafine aerosol time-of-flight mass spectrometer (UF-ATOFMS), a combination that allows in situ measurements of the composition of individual particles as small as 38 nm. The growth tube uses water to grow particles to larger sizes so they can be optically detected by the UF-ATOFMS, extending the size range to below 100 nm with no discernible changes in particle composition. To gain further insight into the temporal variability of aerosol chemistry and sources, the GT-UF-ATOFMS was used for online continuous measurements over a period of 3 days.

  20. Preparation of molecularly imprinted solid-phase microextraction fiber for the selective removal and extraction of the antiviral drug abacavir in environmental and biological matrices

    Energy Technology Data Exchange (ETDEWEB)

    Terzopoulou, Zoi [Laboratory of Polymer Chemistry and Technology, Department of Chemistry, Aristotle University of Thessaloniki, GR-541 24, Thessaloniki (Greece); Papageorgiou, Myrsini [Laboratory of Environmental Pollution Control, Department of Chemistry, Aristotle University of Thessaloniki, GR–541 24, Thessaloniki (Greece); Kyzas, George Z.; Bikiaris, Dimitrios N. [Laboratory of Polymer Chemistry and Technology, Department of Chemistry, Aristotle University of Thessaloniki, GR-541 24, Thessaloniki (Greece); Lambropoulou, Dimitra A., E-mail: dlambro@chem.auth.gr [Laboratory of Environmental Pollution Control, Department of Chemistry, Aristotle University of Thessaloniki, GR–541 24, Thessaloniki (Greece)

    2016-03-24

    In the present study, a molecularly imprinted solid-phase microextraction fiber (MIP-SPME{sub f}) was synthesized and applied for the selective removal and extraction of the antiviral drug, abacavir (ABA). Morphology and structure characterization of fibers were performed by scanning electron microscopy and Fourier transform infrared spectra, respectively. The effects on the adsorption behavior of the process parameters were studied and the equilibrium data were fitted by the Langmuir, Freundlich and Langmuir-Freundlich models. The maximum adsorption capability (Q{sub max}) was determined by Langmuir- Freundlich model and was 149 mg/g for MIP-SPME{sub f}. In the next step, SPME methodology followed by liquid desorption and liquid chromatography with mass spectrometry (LC/MS) has been developed and evaluated for the determination of the target compound in environmental and biological matrices (surface waters, wastewaters and urine). Parameters that could influence SPME efficiency were investigated. Then, optimization of stirring speed, extraction time and salt content was carried out by using a central composite design (CCD) and response surface methodology (RSM). A quadratic model between dependent and independent variables was built. Under the optimum conditions (extraction time 40 min, stirring rate 650 rpm and salt content 0.3% NaCl w/v) the validated method presented a high sensitivity and selectivity with LODs and LOQs in the range of 10.1–13.6 and 33.3–43.9 ng/L, respectively. The developed method was successfully applied to the analysis of ABA in real samples. The percentage extraction efficiency ranged from 88 to 99% revealing good accuracy and absence of matrix effects. - Highlights: • Preparation of a novel SPME MIP fiber with remarkable recognition properties. • Selective removal and extraction of abacavir from environmental & biological media. • Detailed adsorbent characterization and adsorption studies. • Successful application of

  1. Preparation of molecularly imprinted solid-phase microextraction fiber for the selective removal and extraction of the antiviral drug abacavir in environmental and biological matrices

    International Nuclear Information System (INIS)

    Terzopoulou, Zoi; Papageorgiou, Myrsini; Kyzas, George Z.; Bikiaris, Dimitrios N.; Lambropoulou, Dimitra A.

    2016-01-01

    In the present study, a molecularly imprinted solid-phase microextraction fiber (MIP-SPME_f) was synthesized and applied for the selective removal and extraction of the antiviral drug, abacavir (ABA). Morphology and structure characterization of fibers were performed by scanning electron microscopy and Fourier transform infrared spectra, respectively. The effects on the adsorption behavior of the process parameters were studied and the equilibrium data were fitted by the Langmuir, Freundlich and Langmuir-Freundlich models. The maximum adsorption capability (Q_m_a_x) was determined by Langmuir- Freundlich model and was 149 mg/g for MIP-SPME_f. In the next step, SPME methodology followed by liquid desorption and liquid chromatography with mass spectrometry (LC/MS) has been developed and evaluated for the determination of the target compound in environmental and biological matrices (surface waters, wastewaters and urine). Parameters that could influence SPME efficiency were investigated. Then, optimization of stirring speed, extraction time and salt content was carried out by using a central composite design (CCD) and response surface methodology (RSM). A quadratic model between dependent and independent variables was built. Under the optimum conditions (extraction time 40 min, stirring rate 650 rpm and salt content 0.3% NaCl w/v) the validated method presented a high sensitivity and selectivity with LODs and LOQs in the range of 10.1–13.6 and 33.3–43.9 ng/L, respectively. The developed method was successfully applied to the analysis of ABA in real samples. The percentage extraction efficiency ranged from 88 to 99% revealing good accuracy and absence of matrix effects. - Highlights: • Preparation of a novel SPME MIP fiber with remarkable recognition properties. • Selective removal and extraction of abacavir from environmental & biological media. • Detailed adsorbent characterization and adsorption studies. • Successful application of synthesized MIPs

  2. Desenvolvimento de um método de MEFS com CG-DIC para determinação de 1,4 dioxana em amostras de cosméticos

    Directory of Open Access Journals (Sweden)

    Silva Fernando C.

    2001-01-01

    Full Text Available A headspace solid-phase microextraction (HS-SPME for the determination of 1,4 dioxane in cosmetics by gas chromatography is described. A manual SPME holder with 85 µm polyacrylate coating is utilized. The method is determined to have good resolution, satisfactory linerity (correlation coefficient r=0.997 for 0.20-10.00 mg Kg-1 range, a relative standard deviation of 6.3% and a detection limit of 5.00 µg Kg-1. Some cosmectic products were analyzed.

  3. Air sampling with solid phase microextraction

    Science.gov (United States)

    Martos, Perry Anthony

    There is an increasing need for simple yet accurate air sampling methods. The acceptance of new air sampling methods requires compatibility with conventional chromatographic equipment, and the new methods have to be environmentally friendly, simple to use, yet with equal, or better, detection limits, accuracy and precision than standard methods. Solid phase microextraction (SPME) satisfies the conditions for new air sampling methods. Analyte detection limits, accuracy and precision of analysis with SPME are typically better than with any conventional air sampling methods. Yet, air sampling with SPME requires no pumps, solvents, is re-usable, extremely simple to use, is completely compatible with current chromatographic equipment, and requires a small capital investment. The first SPME fiber coating used in this study was poly(dimethylsiloxane) (PDMS), a hydrophobic liquid film, to sample a large range of airborne hydrocarbons such as benzene and octane. Quantification without an external calibration procedure is possible with this coating. Well understood are the physical and chemical properties of this coating, which are quite similar to those of the siloxane stationary phase used in capillary columns. The log of analyte distribution coefficients for PDMS are linearly related to chromatographic retention indices and to the inverse of temperature. Therefore, the actual chromatogram from the analysis of the PDMS air sampler will yield the calibration parameters which are used to quantify unknown airborne analyte concentrations (ppb v to ppm v range). The second fiber coating used in this study was PDMS/divinyl benzene (PDMS/DVB) onto which o-(2,3,4,5,6- pentafluorobenzyl) hydroxylamine (PFBHA) was adsorbed for the on-fiber derivatization of gaseous formaldehyde (ppb v range), with and without external calibration. The oxime formed from the reaction can be detected with conventional gas chromatographic detectors. Typical grab sampling times were as small as 5 seconds

  4. Inertial sensors as measurement tools of elbow range of motion in gerontology

    Science.gov (United States)

    Sacco, G; Turpin, JM; Marteu, A; Sakarovitch, C; Teboul, B; Boscher, L; Brocker, P; Robert, P; Guerin, O

    2015-01-01

    Background and purpose Musculoskeletal system deterioration among the aging is a major reason for loss of autonomy and directly affects the quality of life of the elderly. Articular evaluation is part of physiotherapeutic assessment and helps in establishing a precise diagnosis and deciding appropriate therapy. Reference instruments are valid but not easy to use for some joints. The main goal of our study was to determine reliability and intertester reproducibility of the MP-BV, an inertial sensor (the MotionPod® [MP]) combined with specific software (BioVal [BV]), for elbow passive range-of-motion measurements in geriatrics. Methods This open, monocentric, randomized study compared inertial sensor to inclinometer in patients hospitalized in an acute, post-acute, and long-term-care gerontology unit. Results Seventy-seven patients (mean age 83.5±6.4 years, sex ratio 1.08 [male/female]) were analyzed. The MP-BV was reliable for each of the three measurements (flexion, pronation, and supination) for 24.3% (CI 95% 13.9–32.8) of the patients. Separately, the percentages of reliable measures were 59.7% (49.2–70.5) for flexion, 68.8% (58.4–79.5) for pronation, and 62.3% (51.2–73.1) for supination. The intraclass correlation coefficients were 0.15 (0.07–0.73), 0.46 (0.27–0.98), and 0.50 (0.31–40 0.98) for flexion, pronation, and supination, respectively. Conclusion This study shows the convenience of the MP-BV in terms of ease of use and of export of measured data. However, this instrument seems less reliable and valuable compared to the reference instruments used to measure elbow range of motion in gerontology. PMID:25759568

  5. CENTIMETER COSMO-SKYMED RANGE MEASUREMENTS FOR MONITORING GROUND DISPLACEMENTS

    Directory of Open Access Journals (Sweden)

    F. Fratarcangeli

    2016-06-01

    Full Text Available The SAR (Synthetic Aperture Radar imagery are widely used in order to monitor displacements impacting the Earth surface and infrastructures. The main remote sensing technique to extract sub-centimeter information from SAR imagery is the Differential SAR Interferometry (DInSAR, based on the phase information only. However, it is well known that DInSAR technique may suffer for lack of coherence among the considered stack of images. New Earth observation SAR satellite sensors, as COSMO-SkyMed, TerraSAR-X, and the coming PAZ, can acquire imagery with high amplitude resolutions too, up to few decimeters. Thanks to this feature, and to the on board dual frequency GPS receivers, allowing orbits determination with an accuracy at few centimetres level, the it was proven by different groups that TerraSAR-X imagery offer the capability to achieve, in a global reference frame, 3D positioning accuracies in the decimeter range and even better just exploiting the slant-range measurements coming from the amplitude information, provided proper corrections of all the involved geophysical phenomena are carefully applied. The core of this work is to test this methodology on COSMO-SkyMed data acquired over the Corvara area (Bolzano – Northern Italy, where, currently, a landslide with relevant yearly displacements, up to decimeters, is monitored, using GPS survey and DInSAR technique. The leading idea is to measure the distance between the satellite and a well identifiable natural or artificial Persistent Scatterer (PS, taking in account the signal propagation delays through the troposphere and ionosphere and filtering out the known geophysical effects that induce periodic and secular ground displacements. The preliminary results here presented and discussed indicate that COSMO-SkyMed Himage imagery appear able to guarantee a displacements monitoring with an accuracy of few centimetres using only the amplitude data, provided few (at least one stable PS’s are

  6. 110. PTB seminar: Dose rate measurements of ionizing radiation in the range of natural ambient radiation. Proceedings

    International Nuclear Information System (INIS)

    Lauterbach, U.; Pessara, W.; Woehler-Figgen, S.

    1997-12-01

    Measuring instruments for radiation dose measurement in the range of natural ambient radiation are not subject to legal obligations for calibration and the PTB received numerous requests in the past, asking for measures to be taken in order to ensure reliability of measuring results in this range of radiation. This has induced PTB to organise the seminar, intended to present the current status of measuring technology in this field, reveal problems encountered in practical applications, and discuss suitable ction for quality assurance. The papers of the seminar report the measuring performance and capabilities of the available instruments, results of comparative analyses of measurements, and resulting proposed action for quality assurance. Discussions concluding the sessions are also presented in the processdings volume. (orig./CB) [de

  7. AN INDUCTION SENSOR FOR MEASURING CURRENTS OF NANOSECOND RANGE

    Directory of Open Access Journals (Sweden)

    S. P. Shalamov

    2016-11-01

    Full Text Available Purpose. A current meter based on the principle of electromagnetic induction is designed to register the current flowing in the rod lightning. The aim of the article is to describe the way of increasing the sensitivity of the converter by means of their serial communication. Methodology. The recorded current is in the nanosecond range. If compared with other methods, meters based on the principle of electromagnetic induction have several advantages, such as simplicity of construction, reliability, low cost, no need in a power source, relatively high sensitivity. Creation of such a meter is necessary, because in some cases there is no possibility to use a shunt. Transient properties of a meter are determined by the number of turns and the constant of integration. Sensitivity is determined by measuring the number of turns, the coil sectional area, the core material and the integration constant. For measuring the magnetic field pulses with a rise time of 5 ns to 50 ns a meter has turns from 5 to 15. The sensitivity of such a meter is low. When the number of turns is increased, the output signal and the front increase. Earlier described dependencies were used to select the main parameters of the converter. It was based on generally accepted and widely known equivalent circuit. The experience of created earlier pulse magnetic field meters was considered both for measuring the magnetic fields, and large pulse current. Originality. Series connection of converters has the property of a long line. The level of the transient response of the meter is calculated. The influence of parasitic parameters on the type of meter transient response is examined. The shown construction was not previously described. Practical value. The results of meter implementation are given. The design peculiarities of the given measuring instruments are shown.

  8. Differentiation of Commercial PDO Wines Produced in Istria (Croatia According to Variety and Harvest Year Based on HS-SPME-GC/MS Volatile Aroma Compound Profiling

    Directory of Open Access Journals (Sweden)

    Igor Lukić

    2017-01-01

    Full Text Available To differentiate monovarietal wines made from native and introduced varieties in Istria (Croatia, samples of Malvazija istarska, Chardonnay and Muscat yellow from two harvest years (2013 and 2014 were subjected to headspace solid-phase microextraction and gas chromatographic/mass spectrometric analysis (HS-SPME-GC/MS of volatile aroma compounds. Significant effects of variety and harvest year were determined, but their interaction complicated the differentiation. Particular compounds were consistent as markers of variety in both years: nerol for Malvazija, ethyl cinnamate and a tentatively identified isomer of dimethylbenzaldehyde for Chardonnay, and terpenes for Muscat yellow. Wines from 2013 contained higher concentrations of the majority of important volatiles. A 100 % correct differentiation of Malvazija istarska and Chardonnay wines according to both variety and harvest year was achieved by stepwise linear discriminant analysis.

  9. A new method for the determination of short-chain fatty acids from the aliphatic series in wines by headspace solid-phase microextraction-gas chromatography-ion trap mass spectrometry.

    Science.gov (United States)

    Olivero, Sergio J Pérez; Trujillo, Juan P Pérez

    2011-06-24

    A new analytical method for the determination of nine short-chain fatty acids (acetic, propionic, isobutyric, butyric, isovaleric, 2-methylbutyric, hexanoic, octanoic and decanoic acids) in wines using the automated HS/SPME-GC-ITMS technique was developed and optimised. Five different SPME fibers were tested and the influence of different factors such as temperature and time of extraction, temperature and time of desorption, pH, strength ionic, tannins, anthocyans, SO(2), sugar and ethanol content were studied and optimised using model solutions. Some analytes showed matrix effect so a study of recoveries was performed. The proposed HS/SPME-GC-ITMS method, that covers the concentration range of the different analytes in wines, showed wide linear ranges, values of repeatability and reproducibility lower than 4.0% of RSD and detection limits between 3 and 257 μgL(-1), lower than the olfactory thresholds. The optimised method is a suitable technique for the quantitative analysis of short-chain fatty acids from the aliphatic series in real samples of white, rose and red wines. Copyright © 2011 Elsevier B.V. All rights reserved.

  10. Compressive laser ranging.

    Science.gov (United States)

    Babbitt, Wm Randall; Barber, Zeb W; Renner, Christoffer

    2011-12-15

    Compressive sampling has been previously proposed as a technique for sampling radar returns and determining sparse range profiles with a reduced number of measurements compared to conventional techniques. By employing modulation on both transmission and reception, compressive sensing in ranging is extended to the direct measurement of range profiles without intermediate measurement of the return waveform. This compressive ranging approach enables the use of pseudorandom binary transmit waveforms and return modulation, along with low-bandwidth optical detectors to yield high-resolution ranging information. A proof-of-concept experiment is presented. With currently available compact, off-the-shelf electronics and photonics, such as high data rate binary pattern generators and high-bandwidth digital optical modulators, compressive laser ranging can readily achieve subcentimeter resolution in a compact, lightweight package.

  11. Note: long range and accurate measurement of deep trench microstructures by a specialized scanning tunneling microscope.

    Science.gov (United States)

    Ju, Bing-Feng; Chen, Yuan-Liu; Zhang, Wei; Zhu, Wule; Jin, Chao; Fang, F Z

    2012-05-01

    A compact but practical scanning tunneling microscope (STM) with high aspect ratio and high depth capability has been specially developed. Long range scanning mechanism with tilt-adjustment stage is adopted for the purpose of adjusting the probe-sample relative angle to compensate the non-parallel effects. A periodical trench microstructure with a pitch of 10 μm has been successfully imaged with a long scanning range up to 2.0 mm. More innovatively, a deep trench with depth and step height of 23.0 μm has also been successfully measured, and slope angle of the sidewall can approximately achieve 67°. The probe can continuously climb the high step and exploring the trench bottom without tip crashing. The new STM could perform long range measurement for the deep trench and high step surfaces without image distortion. It enables accurate measurement and quality control of periodical trench microstructures.

  12. Spacecraft Trajectory Estimation Using a Sampled-Data Extended Kalman Filter with Range-Only Measurements

    National Research Council Canada - National Science Library

    Erwin, R. S; Bernstein, Dennis S

    2005-01-01

    .... In this paper we use a sampled-data extended Kalman Filter to estimate the trajectory or a target satellite when only range measurements are available from a constellation or orbiting spacecraft...

  13. LUMOS - A Sensitive and Reliable Optode System for Measuring Dissolved Oxygen in the Nanomolar Range

    DEFF Research Database (Denmark)

    Lehner, Philipp; Larndorfer, Christoph; Garcia-Robledo, Emilio

    2015-01-01

    Most commercially available optical oxygen sensors target the measuring range of 300 to 2 mu mol L-1. However these are not suitable for investigating the nanomolar range which is relevant for many important environmental situations. We therefore developed a miniaturized phase fluorimeter based...... for read out of less sensitive optical oxygen sensors based on the same or similar indicator dyes, for example for monitoring oxygen at physiological conditions. The presented sensor system exhibits lower noise, higher resolution and higher sensitivity than the electrochemical STOX sensor previously used...... measurement system called the LUMOS (Luminescence Measuring Oxygen Sensor). It consists of a readout device and specialized "sensing chemistry" that relies on commercially available components. The sensor material is based on palladium(II)-5,10,15,20-tetrakis-(2,3,4,5,6-pentafluorphenyl)-porphyrin embedded...

  14. Sorption of structurally different ionized pharmaceutical and illicit drugs to a mixed-mode coated microsampler.

    Science.gov (United States)

    Peltenburg, Hester; Timmer, Niels; Bosman, Ingrid J; Hermens, Joop L M; Droge, Steven T J

    2016-05-20

    neutral benzodiazepines were an order of magnitude higher than their log Kow,N. Results for anionic diclofenac species (logKow,N 4.5, pKa 4.0, log Dfw 2.9) indicate that the C18-SCX fiber might also be useful for sampling of organic anions. This data supports our theory that C18-based coatings are able to sorb ionized compounds through adsorption and demonstrates the applicability of C18-based SPME in the measurement of freely dissolved concentrations of a wide range of ionizable compounds. Copyright © 2016 Elsevier B.V. All rights reserved.

  15. Evaluation of expansion algorithm of measurement range suited for 3D shape measurement using two pitches of projected grating with light source-stepping method

    Science.gov (United States)

    Sakaguchi, Toshimasa; Fujigaki, Motoharu; Murata, Yorinobu

    2015-03-01

    Accurate and wide-range shape measurement method is required in industrial field. The same technique is possible to be used for a shape measurement of a human body for the garment industry. Compact 3D shape measurement equipment is also required for embedding in the inspection system. A shape measurement by a phase shifting method can measure the shape with high spatial resolution because the coordinates can be obtained pixel by pixel. A key-device to develop compact equipment is a grating projector. Authors developed a linear LED projector and proposed a light source stepping method (LSSM) using the linear LED projector. The shape measurement euipment can be produced with low-cost and compact without any phase-shifting mechanical systems by using this method. Also it enables us to measure 3D shape in very short time by switching the light sources quickly. A phase unwrapping method is necessary to widen the measurement range with constant accuracy for phase shifting method. A general phase unwrapping method with difference grating pitches is often used. It is one of a simple phase unwrapping method. It is, however, difficult to apply the conventional phase unwrapping algorithm to the LSSM. Authors, therefore, developed an expansion unwrapping algorithm for the LSSM. In this paper, an expansion algorithm of measurement range suited for 3D shape measurement using two pitches of projected grating with the LSSM was evaluated.

  16. Tilted Magnetic Levitation Enables Measurement of the Complete Range of Densities of Materials with Low Magnetic Permeability.

    Science.gov (United States)

    Nemiroski, Alex; Soh, Siowling; Kwok, Sen Wai; Yu, Hai-Dong; Whitesides, George M

    2016-02-03

    Magnetic levitation (MagLev) of diamagnetic or weakly paramagnetic materials suspended in a paramagnetic solution in a magnetic field gradient provides a simple method to measure the density of small samples of solids or liquids. One major limitation of this method, thus far, has been an inability to measure or manipulate materials outside of a narrow range of densities (0.8 g/cm(3) MagLev"-to increase the range of densities that can be levitated magnetically. Tilting the MagLev device relative to the gravitational vector enables the magnetic force to be decreased (relative to the magnetic force) along the axis of measurement. This approach enables many practical measurements over the entire range of densities observed in matter at ambient conditions-from air bubbles (ρ ≈ 0) to osmium and iridium (ρ ≈ 23 g/cm(3)). The ability to levitate, simultaneously, objects with a broad range of different densities provides an operationally simple method that may find application to forensic science (e.g., for identifying the composition of miscellaneous objects or powders), industrial manufacturing (e.g., for quality control of parts), or resource-limited settings (e.g., for identifying and separating small particles of metals and alloys).

  17. On the theory of SODAR measurement techniques[SOund Detection And Ranging

    Energy Technology Data Exchange (ETDEWEB)

    Antoniou, I.; Joergensen, H.E. [Risoe National Lab. (Denmark); Ormel, F. [Energy Research Center of the Netherlands (Netherlands); Bradley, S.; Huenerbein, S. von [University of Salford (United Kingdom); Emeis, S. [Forschungszentrum Karlsruhe GmbH (Germany); Warmbier, G. [GWU-Umwelttechnik Gmbh (Germany)

    2003-04-01

    The need for alternative means to measure the wind speed for wind energy purposes has increased with the increase of the size of wind turbines. The cost and the technical difficulties for performing wind speed measurements has also increased with the size of the wind turbines, since it is demanded that the wind speed has to be measured at the rotor centre of the turbine and the size of both the rotor and the hub height have grown following the increase in the size of the wind turbines. The SODAR (SOund Detection And Ranging) is an alternative to the use of cup anemometers and offers the possibility of measuring both the wind speed distribution with height and the wind direction. At the same time the SODAR presents a number of serious drawbacks such as the low number of measurements per time period, the dependence of the ability to measure on the atmospheric conditions and the difficulty of measuring at higher wind speeds due to either background noise or the neutral condition of the atmosphere. Within the WISE project (EU project number NNE5-2001-297), a number of work packages have been defined in order to deal with the SODAR. The present report is the result of the work package 1. Within this package the objective has been to present and achieve the following: 1) An accurate theoretic model that describes all the relevant aspects of the interaction of the sound beam with the atmosphere in the level of detail needed for wind energy applications. 2) Understanding of dependence of SODAR performance on hard- and software configuration. 3) Quantification of principal difference between SODAR wind measurement and wind speed measurements with cup anemometers with regard to power performance measurements.

  18. Compact range for variable-zone measurements

    Science.gov (United States)

    Burnside, Walter D.; Rudduck, Roger C.; Yu, Jiunn S.

    1988-08-02

    A compact range for testing antennas or radar targets includes a source for directing energy along a feedline toward a parabolic reflector. The reflected wave is a spherical wave with a radius dependent on the distance of the source from the focal point of the reflector.

  19. Electron density values of various human tissues: in vitro Compton scatter measurements and calculated ranges

    International Nuclear Information System (INIS)

    Shrimpton, P.C.

    1981-01-01

    Accurate direct measurements of electron density have been performed on specimens from 10 different tissue types of the human body, representing the major organs, using a Compton scatter technique. As a supplement to these experimental values, calculations have been carried out to determine the electron densities expected for these tissue types. The densities observed are in good agreement with the broad ranges deduced from the basic data previously published. The results of both the in vitro sample measurements and the approximate calculations indicate that the electron density of most normal healthy soft tissue can be expected to fall within the fairly restricted range of +- 5% around 3.4 X 10 23 electrons per cm 3 . The obvious exception to this generalisation is the result for lung tissue, which falls considerably below this range owing to the high air content inherent in its construction. In view of such an overall limited variation with little difference between tissues, it would appear that electron density alone is likely to be a rather poor clinical parameter for tissue analysis, with high accuracy and precision being essential in any in vivo Compton measurements for imaging or diagnosis on specific organs. (author)

  20. Evaluation of knee range of motion: Correlation between measurements using a universal goniometer and a smartphone goniometric application.

    Science.gov (United States)

    Dos Santos, Rafael Aparecido; Derhon, Viviane; Brandalize, Michelle; Brandalize, Danielle; Rossi, Luciano Pavan

    2017-07-01

    Goniometers are commonly used to measure range of motion in the musculoskeletal system. Recently smartphone goniometry applications have become available to clinicians. Compare angular measures using a universal goniometer and a smartphone application. Thirty four healthy women with at least 20° of limited range of motion regarding knee extension were recruited. Knee flexion angles of the dominant limb were measured with a universal goniometer and the ROM © goniometric application for the smartphone. Three trained examiners compared the two assessment tools. Strong correlations were found between the measures of the universal goniometer and smartphone application (Pearson's correlation and interclass correlation coefficient > 0.93). The measurements with both devices demonstrated low dispersion and little variation. Measurements obtained using the smartphone goniometric application analyzed are as reliable as those of a universal goniometer. This application is therefore a useful tool for the evaluation of knee range of motion. Copyright © 2016 Elsevier Ltd. All rights reserved.

  1. Quantification of selected volatile organic compounds in human urine by gas chromatography selective reagent ionization time of flight mass spectrometry (GC-SRI-TOF-MS) coupled with head-space solid-phase microextraction (HS-SPME).

    Science.gov (United States)

    Mochalski, Paweł; Unterkofler, Karl

    2016-08-07

    Selective reagent ionization time of flight mass spectrometry with NO(+) as the reagent ion (SRI-TOF-MS(NO(+))) in conjunction with gas chromatography (GC) and head-space solid-phase microextraction (HS-SPME) was used to determine selected volatile organic compounds in human urine. A total of 16 volatiles exhibiting high incidence rates were quantified in the urine of 19 healthy volunteers. Amongst them there were ten ketones (acetone, 2-butanone, 3-methyl-2-butanone, 2-pentanone, 3-methyl-2-pentanone, 4-methyl-2-pentanone, 2-hexanone, 3-hexanone, 2-heptanone, and 4-heptanone), three volatile sulphur compounds (dimethyl sulfide, allyl methyl sulfide, and methyl propyl sulfide), and three heterocyclic compounds (furan, 2-methylfuran, 3-methylfuran). The concentrations of the species under study varied between 0.55 nmol L(-1) (0.05 nmol mmol(-1)creatinine) for allyl methyl sulfide and 11.6 μmol L(-1) (1.54 μmol mmol(-1)creatinine) for acetone considering medians. Limits of detection (LODs) ranged from 0.08 nmol L(-1) for allyl methyl sulfide to 1.0 nmol L(-1) for acetone and furan (with RSDs ranging from 5 to 9%). The presented experimental setup assists both real-time and GC analyses of volatile organic compounds, which can be performed consecutively using the same analytical system. Such an approach supports the novel concept of hybrid volatolomics, an approach which combines VOC profiles obtained from two or more body fluids to improve and complement the chemical information on the physiological status of an individual.

  2. Multiwalled carbon nanotubes coated fibers for solid-phase microextraction of polybrominated diphenyl ethers in water and milk samples before gas chromatography with electron-capture detection.

    Science.gov (United States)

    Wang, Jun-Xia; Jiang, Dong-Qing; Gu, Zhi-Yuan; Yan, Xiu-Ping

    2006-12-22

    Determination of polybrominated diphenyl ethers (PBDEs) in environmental samples has raised great concerns due to the widespread use of PBDEs and their potential risk to humans. Solid-phase microextraction (SPME) is a fast, simple, cost-effective, and green sample preparation technique and is widely used for environmental analysis, but reports on the application of SPME for determination of PBDEs are very limited, and only a few publications dealing with commercial SPME fibers are available for extraction of PBDEs. Herein, we report a novel SPME method using multiwalled carbon nanotubes (MWCNTs) as the SPME fiber coating for gas chromatography with electron-capture detection (GC-ECD) of PBDEs in environmental samples. The MWCNTs coating gave much higher enhancement factors (616-1756) than poly (5% dibenzene-95% dimethylsiloxane) coating (139-384) and activated carbon coating (193-423). Thirty-minute extraction of 10 mL of sample solution using the MWCNTs coated fiber for GC-ECD determination yielded the limits of detection of 3.6-8.6 ng L(-1) and exhibited good linearity of the calibration functions (r(2)>0.995). The precision (RSD%, n=4) for peak area and retention time at the 500 ng L(-1) level was 6.9-8.8% and 0.6-0.9%, respectively. The developed method was successfully applied for the analysis of real samples including local river water, wastewater, and milk samples. The recovery of the PBDEs at 500 ng L(-1) spiked in these samples ranged from 90 to 119%. No PBDEs were detected in the river water and skimmed milk samples, whereas in the wastewater sample, 134-215 ng L(-1) of PBDEs were found. The PBDEs were detected in all whole fat milk samples, ranging from 13 to 484 ng L(-1). In a semiskimmed milk sample, only BDE-47 was found at 21 ng L(-1).

  3. Time Biases in laser ranging measurements; impacts on geodetic products (Reference Frame and Orbitography)

    Science.gov (United States)

    Belli, A.; Exertier, P.; Lemoine, F. G.; Chinn, D. S.; Zelensky, N. P.

    2017-12-01

    The GGOS objectives are to maintain a geodetic network with an accuracy of 1 mm and a stability of 0.1 mm per year. For years, the laser ranging technique, which provide very accurate absolute distances to geodetic targets enable to determine the scale factor as well as coordinates of the geocenter. In order to achieve this goal, systematic errors appearing in the laser ranging measurements must be considered and solved. In addition to Range Bias (RB), which is the primary source of uncertainty of the technique, Time Bias (TB) has been recently detected by using the Time Transfer by Laser Link (T2L2) space instrument capability on-board the satellite Jason-2. Instead of determining TB through the precise orbit determination that is applied to commonly used geodetic targets like LAGEOS to estimate global geodetic products, we have developed, independently, a dedicated method to transfer time between remote satellite laser ranging stations. As a result, the evolving clock phase shift to UTC of around 30 stations has been determined under the form of time series of time bias per station from 2008 to 2016 with an accuracy of 3-4 ns. It demonstrated the difficulty, in terms of Time & Frequency used technologies, to locally maintain accuracy and long term stability at least in the range of 100 ns that is the current requirement for time measurements (UTC) for the laser ranging technique. Because some laser ranging stations oftently exceed this limit (from 100 ns to a few μs) we have been studying these effects first on the precision orbit determination itself, second on the station positioning. We discuss the impact of TB on LAGEOS and Jason-2 orbits, which appears to affect the along-track component essentially. We also investigate the role of TB in global geodetic parameters as the station coordinates. Finally, we propose to provide the community with time series of time bias of laser ranging stations, under the form of a data- handling-file in order to be included in

  4. Novel birefringence interrogation for Sagnac loop interferometer sensor with unlimited linear measurement range.

    Science.gov (United States)

    He, Haijun; Shao, Liyang; Qian, Heng; Zhang, Xinpu; Liang, Jiawei; Luo, Bin; Pan, Wei; Yan, Lianshan

    2017-03-20

    A novel demodulation method for Sagnac loop interferometer based sensor has been proposed and demonstrated, by unwrapping the phase changes with birefringence interrogation. A temperature sensor based on Sagnac loop interferometer has been used to verify the feasibility of the proposed method. Several tests with 40 °C temperature range have been accomplished with a great linearity of 0.9996 in full range. The proposed scheme is universal for all Sagnac loop interferometer based sensors and it has unlimited linear measurable range which overwhelming the conventional demodulation method with peak/dip tracing. Furthermore, the influence of the wavelength sampling interval and wavelength span on the demodulation error has been discussed in this work. The proposed interrogation method has a great significance for Sagnac loop interferometer sensor and it might greatly enhance the availability of this type of sensors in practical application.

  5. Analysis and suppression of reflections in far-field antenna measurement ranges

    OpenAIRE

    Sierra Castañer, Manuel; Cano Facila, Francisco Jose; Foged, Lars Jacob; Saccardi, Francesco; Nader Kawassaki, Guilherme; Raimundi, Lucas dos Reis; Vilela Rezende, Stefano Albino

    2013-01-01

    This paper presents the analysis of the reflections in two kind of spherical far field ranges: one if the classical acquisition where the AUT is rotated and the second one corresponds to the systems where the AUT is fixed and the antenna probe is rotated. In large far field systems this is not possible, but this can be used to the measurement of small antennas, for instance, with the SATIMO StarGate system. In both cases, it is assumed that only one frequency is acquired and the results shoul...

  6. Impedance measurements on a fast transition-edge sensor for optical and near-infrared range

    International Nuclear Information System (INIS)

    Taralli, E; Portesi, C; Lolli, L; Monticone, E; Rajteri, M; Novikov, I; Beyer, J

    2010-01-01

    Impedance measurements of superconducting transition-edge sensors (TESs) are a powerful tool to obtain information about the TES thermal and electrical properties. We apply this technique to a 20 μm x 20 μm Ti/Au TES, suitable for application in the optical and near-infrared range, and extend the measurements up to 250 kHz in order to obtain a complete frequency response in the complex plane. From these measurements we obtain important thermal and electrical device parameters such as heat capacity C, thermal conductance G and effective thermal time constant τ eff that will be compared with the corresponding values obtained from noise measurements.

  7. Measure of the albedo of a warm plasma in the XUV range

    Science.gov (United States)

    Busquet, Michel; Thais, Frederic; Geoffroy, Ghita; Raffestin, Didier

    2009-11-01

    It has been shown in a recent experience at PALS [1] that the radiative precursor celerity in front of a strong radiative shock is sensitive to the lateral radiative losses, thus to the albedo of the wall of a ``radiative shock tube.'' In the experiment presented here, we measure the albedo of various materials (Al, Cu, Au) heated by a Xenon gaz at temperature around 30 eV. The Xenon gas was heated by the ALISE laser in CESTA in Bordeaux (France). The emission of Xenon with and without the reflecting samples is measured with a spatially resolving XUV spectrograph in the 30-250 eV range. [4pt] [1] M. Busquet et al, HEDP 3, 8 (2007)

  8. 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.

  9. Sensitive determination of bisphenol A and bisphenol F in canned food using a solid-phase microextraction fibre coated with single-walled carbon nanotubes before GC/MS.

    Science.gov (United States)

    Rastkari, N; Ahmadkhaniha, R; Yunesian, M; Baleh, L J; Mesdaghinia, A

    2010-10-01

    A reliable and sensitive method for simultaneous determination of bisphenol A (BPA) and bisphenol F (BPF) in canned food by gas chromatography-mass spectrometry (GC/MS) is described after extraction and pre-concentration by a new solid-phase microextraction (SPME) adsorbent. The potential of single-walled carbon nanotubes (SWCNTs) as SPME adsorbent for the pre-concentration of environmental contaminants has been investigated in recent years. This work was carried out to investigate the feasibility of SWCNTs as a headspace SPME adsorbent for the determination of bisphenol derivatives in canned food. Potential factors affecting the extraction efficiency, including extraction time, extraction temperature, desorption time, desorption temperature, and salinity were optimized. Calibration curves were linear (r(2)> or = 0.994) over the concentration range from 0.30 to 60 microg kg(-1). For both target analytes, the limit of detection (LOD) at signal-to-noise (S/N) ratio of 3 was 0.10 microg kg(-1). In addition, a comparative study between the SWCNT and a commercial polydimethylsiloxane (PDMS) SPME fibre for the determination of bisphenol derivatives in canned food was conducted. SWCNT fibre showed higher extraction capacity, better thermal stability (over 350 degrees C) and longer life span (over 150 times) than the commercial PDMS fibre. The method was successfully applied to determine BPA in canned food samples which were purchased from local markets. BPA was found in some of the samples within the concentration range from 0.5 to 5.2 microg kg(-1).

  10. 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

  11. Assessing a traceability technique in fresh oranges (Citrus sinensis L. Osbeck) with an HS-SPME-GC-MS method. Towards a volatile characterisation of organic oranges.

    Science.gov (United States)

    Cuevas, Francisco Julián; Moreno-Rojas, José Manuel; Ruiz-Moreno, María José

    2017-04-15

    A targeted approach using HS-SPME-GC-MS was performed to compare flavour compounds of 'Navelina' and 'Salustiana' orange cultivars from organic and conventional management systems. Both varieties of conventional oranges showed higher content of ester compounds. On the other hand, higher content of some compounds related with the geranyl-diphosphate pathway (neryl and geranyl acetates) and some terpenoids were found in the organic samples. Furthermore, the partial least square discriminant analysis (PLS-DA) achieved an effective classification for oranges based on the farming system using their volatile profiles (90 and 100% correct classification). To our knowledge, it is the first time that a comparative study dealing with farming systems and orange aroma profile has been performed. These new insights, taking into account local databases, cultivars and advanced analytical tools, highlight the potential of volatile composition for organic orange discrimination. Copyright © 2016 Elsevier Ltd. All rights reserved.

  12. Volatile compound changes during shelf life of dried Boletus edulis: comparison between SPME-GC-MS and PTR-ToF-MS analysis.

    Science.gov (United States)

    Aprea, Eugenio; Romano, Andrea; Betta, Emanuela; Biasioli, Franco; Cappellin, Luca; Fanti, Marco; Gasperi, Flavia

    2015-01-01

    Drying process is commonly used to allow long time storage of valuable porcini mushrooms (Boletus edulis). Although considered a stable product dried porcini flavour changes during storage. Monitoring of volatile compounds during shelf life may help to understand the nature of the observed changes. In the present work two mass spectrometric techniques were used to monitor the evolution of volatile compounds during commercial shelf life of dried porcini. Solid phase microextraction (SPME) coupled to gas chromatography - mass spectrometry (GC-MS) allowed the identification of 66 volatile compounds, 36 of which reported for the first time, monitored during the commercial shelf life of dried porcini. Proton transfer reaction - time of flight - mass spectrometry (PTR-ToF-MS) , a direct injection mass spectrometric technique, was shown to be a fast and sensitive instrument for the general monitoring of volatile compound evolution during storage of dried porcini. Furthermore, PTR-ToF-MS grants access to compounds whose determination would otherwise require lengthy pre-concentration and/or derivatization steps such as ammonia and small volatile amines. The two techniques, both used for the first time to study dried porcini, provided detailed description of time evolution of volatile compounds during shelf life. Alcohols, aldehydes, ketones and monoterpenes diminish during the storage while carboxylic acids, pyrazines, lactones and amines increase. The storage temperature modifies the rate of the observed changes influencing the final quality of the dried porcini. We showed the advantages of both techniques, suggesting a strategy to be adopted to follow time evolution of volatile compounds in food products during shelf life, based on the identification of compounds by GC-MS and the rapid time monitoring by PTR-ToF-MS measurements in order to maximize the advantages of both techniques. Copyright © 2015 John Wiley & Sons, Ltd.

  13. Long-range correlations of serial FEV1 measurements in emphysematous patients and normal subjects

    DEFF Research Database (Denmark)

    Dirksen, A; Holstein-Rathlou, N H; Madsen, F

    1998-01-01

    are autocorrelated. The purpose of this study was to describe the correlation structure in time series of FEV1 measurements. Nineteen patients with severe alpha1-antitrypsin deficiency (phenotype PiZ) and moderate to severe emphysema and two subjects with normal lungs were followed for several years with daily self......In obstructive lung disease the annual change in lung function is usually estimated from serial measurements of forced expiratory volume in 1 s (FEV1). Frequent measurements in each patient may not improve this estimate because data are not statistically independent; i.e., the measurements...... measurements show long-range correlations. The practical implication is that FEV1 need not be measured more often than once every 3 mo in studies of the long-term trends in lung function....

  14. Comparison of the measurement of heart rate in adult free-range chickens (Gallus domesticus) by auscultation and electrocardiography.

    Science.gov (United States)

    Smith, C F; Gavaghan, B J; McSweeney, D; Powell, V; Lisle, A

    2014-12-01

    To compare the heart rates of adult free-range chickens (Gallus domesticus) measured by auscultation with a stethoscope with those measured simultaneously using electrocardiography (ECG). With each bird in a standing position, estimation of the heart rate was performed by placing a mark on paper for every 4 beats for roosters and 8 beats for hens as detected by auscultation over 30 s, while simultaneous ECG was performed. Heart rates measured by auscultation showed a high correlation (r = 0.97) with those measured by ECG. There was a high correlation between the heart rates of adult free-range chickens measured by auscultation with a stethoscope and those measured simultaneously using ECG. © 2014 Australian Veterinary Association.

  15. A novel method of range measuring for a mobile robot based on multi-sensor information fusion

    International Nuclear Information System (INIS)

    Zhang Yi; Luo Yuan; Wang Jifeng

    2005-01-01

    The traditional measuring range for a mobile robot is based on a sonar sensor. Because of different working environments, it is very difficult to obtain high precision by using just one single method of range measurement. So, a hybrid sonar sensor and laser scanner method is put forward to overcome these shortcomings. A novel fusion model is proposed based on basic theory and a method of information fusion. An optimal measurement result has been obtained with information fusion from different sensors. After large numbers of experiments and performance analysis, a conclusion can be drawn that the laser scanner and sonar sensor method with multi-sensor information fusion have a higher precision than the single method of sonar. It can also be the same with different environments

  16. Electrochemically modified carbon fiber bundles as selective sorbent for online solid-phase microextraction of sulfonamides

    International Nuclear Information System (INIS)

    Ling, Xu; Zhang, Wenpeng; Chen, Zilin

    2016-01-01

    The authors show that carbon fiber bundles electrochemically modified with the conducting polymer poly(3,4-ethylenedioxythiophene) (PEDOT) is a viable sorbent for online solid-phase microextraction (SPME) of the sulfonamides (sulfadiazine, sulfadimidine and sulfamethoxazole) prior to their determination by HPLC. The fibers were packed in a tube loop made from polyether ether ketone (PEEK) that was coupled to the HPLC system for online SPME. Preconcentration factors can reach values of up to 300, and the limit of detection (at an S/N ration of 3) can be as low as 0.05 ng⋅mL −1 . The method was applied to the analysis of the sulfonamides in spiked rat plasma with intra-day and inter-day RSDs of <3.33 and <4.57 %, and with recoveries in the range from 91.7 to 97.8 % in spiked plasma. The in-tube SPME was also applied to the determination of the 3 sulfonamides in rat plasma after oral administration (tablet powder) with high sensitivity. In addition to its efficient extraction, the PEEK tube based SPME has chemical and mechanical stability under even harsh conditions. (author)

  17. In situ fabrication of nanostructured titania coating on the surface of titanium wire: A new approach for preparation of solid-phase microextraction fiber

    International Nuclear Information System (INIS)

    Cao Dandan; Lue Jianxia; Liu Jingfu; Jiang Guibin

    2008-01-01

    Nanostructured titania-based solid-phase microextraction (SPME) fibers were fabricated through the in situ oxidation of titanium wires with H 2 O 2 (30%, w/w) at 80 deg. C for 24 h. The obtained SPME fibers possess a ∼1.2 μm thick nanostructured coating consisting of ∼100 nm titania walls and 100-200 nm pores. The use of these fibers for headspace SPME coupled with gas chromatography with electron capture detection (GC-ECD) resulted in improved analysis of dichlorodiphenyltrichloroethane (DDT) and its degradation products. The presented method to detect DDT and its degradation products has high sensitivity (0.20-0.98 ng L -1 ), high precision (relative standard deviation R.S.D. = 9.4-16%, n = 5), a wide linear range (5-5000 ng L -1 ), and good linearity (coefficient of estimation R 2 = 0.991-0.998). As the nanostructured titania was in situ formed on the surface of a titanium wire, the coating was uniformly and strongly adhered on the titanium wire. Because of the inherent chemical stability of the titania coating and the mechanical durability of the titanium wire substrate, this new SPME fiber exhibited long life span (over 150 times)

  18. PEEK tube-based online solid-phase microextraction-high-performance liquid chromatography for the determination of yohimbine in rat plasma and its application in pharmacokinetics study.

    Science.gov (United States)

    Xiang, Xiaowei; Shang, Bing; Wang, Xiaozheng; Chen, Qinhua

    2017-04-01

    Yohimbine is a novel compound for the treatment of erectile dysfunction derived from natural products, and pharmacokinetic study is important for its further development as a new medicine. In this work, we developed a novel PEEK tube-based solid-phase microextraction (SPME)-HPLC method for analysis of yohimbine in plasma and further for pharmacokinetic study. Poly (AA-EGDMA) was synthesized inside a PEEK tube as the sorbent for microextraction of yohimbine, and parameters that could influence extraction efficiency were systematically investigated. Under optimum conditions, the PEEK tube-based SPME method exhibits excellent enrichment efficiency towards yohimbine. By using berberine as internal standard, an online SPME-HPLC method was developed for analysis of yohimbine in human plasma sample. The method has wide linear range (2-1000 ng/mL) with an R 2 of 0.9962; the limit of detection was determined and was as low as 0.1 ng/mL using UV detection. Finally, a pharmacokinetic study of yohimbine was carried out by the online SPME-HPLC method and the results have been compared with those of reported methods. Copyright © 2016 John Wiley & Sons, Ltd.

  19. Ionospheric Coherence Bandwidth Measurements in the Lower VHF Frequency Range

    Science.gov (United States)

    Suszcynsky, D. M.; Light, M. E.; Pigue, M. J.

    2015-12-01

    The United States Department of Energy's Radio Frequency Propagation (RFProp) experiment consists of a satellite-based radio receiver suite to study various aspects of trans-ionospheric signal propagation and detection in four frequency bands, 2 - 55 MHz, 125 - 175 MHz, 365 - 415 MHz and 820 - 1100 MHz. In this paper, we present simultaneous ionospheric coherence bandwidth and S4 scintillation index measurements in the 32 - 44 MHz frequency range collected during the ESCINT equatorial scintillation experiment. 40-MHz continuous wave (CW) and 32 - 44 MHz swept frequency signals were transmitted simultaneously to the RFProp receiver suite from the Reagan Test Site at Kwajalein Atoll in the Marshall Islands (8.7° N, 167.7° E) in three separate campaigns during the 2014 and 2015 equinoxes. Results show coherence bandwidths as small as ~ 1 kHz for strong scintillation (S4 > 0.7) and indicate a high degree of ionospheric variability and irregularity on 10-m spatial scales. Spread-Doppler clutter effects arising from preferential ray paths to the satellite due to refraction off of isolated density irregularities are also observed and are dominant at low elevation angles. The results are compared to previous measurements and available scaling laws.

  20. HS-SPME optimization and extraction of volatile compounds from soursop (Annona muricata L. pulp with emphasis on their characteristic impact compounds

    Directory of Open Access Journals (Sweden)

    Karen Leticia de SANTANA

    Full Text Available Abstract Aroma and taste are decisive factors in the selection of any food. The aim of this study was to extract the volatile compounds present in soursop (Annona muricata L. pulp by Solid-phase microextraction (SPME technique using 3 different fibers (DVB/CAR/ PDMS, CAR/PDMS and PDMS/DVB. An experimental design was set up to evaluate the best extraction conditions wherein the variables were adsorption temperature, ionic strength and pulp concentration. The separation of volatiles was performed in chromatographic columns of different polarity (polar and non-polar while volatile compounds were identified by analysis in high resolution gas chromatography system coupled with mass spectrometry. The results obtained using 3 different fibers revealed the capture of about 40 compounds. The CAR/PDMS fiber was more efficient for the capture of esters and DVB/CAR/PDMS fiber for terpenes. The optimum conditions for capture of higher number of volatiles for polar column were 45 °C for extraction, 15% of ionic strength and 50% of pulp concentration which resulted in separation of 87 compounds. Among the principal character impact compounds from soursop are (E-2-hexenoate, methyl hexenoate and linalool.

  1. Measurements of long-range enhanced collisional velocity drag through plasma wave damping

    Science.gov (United States)

    Affolter, M.; Anderegg, F.; Dubin, D. H. E.; Driscoll, C. F.

    2018-05-01

    We present damping measurements of axial plasma waves in magnetized, multispecies ion plasmas. At high temperatures T ≳ 10-2 eV, collisionless Landau damping dominates, whereas, at lower temperatures T ≲ 10-2 eV, the damping arises from interspecies collisional drag, which is dependent on the plasma composition and scales roughly as T-3 /2 . This drag damping is proportional to the rate of parallel collisional slowing, and is found to exceed classical predictions of collisional drag damping by as much as an order of magnitude, but agrees with a new collision theory that includes long-range collisions. Centrifugal mass separation and collisional locking of the species occur at ultra-low temperatures T ≲ 10-3 eV, which reduce the drag damping from the T-3 /2 collisional scaling. These mechanisms are investigated by measuring the damping of higher frequency axial modes, and by measuring the damping in plasmas with a non-equilibrium species profile.

  2. Aplicação da técnica de SPME-GC-MS na determinação dos produtos voláteis gerados na degradação térmica de polímeros

    OpenAIRE

    Bortoluzzi, Janaína Heberle

    2007-01-01

    Tese (doutorado) - Universidade Federal de Santa Catarina, Centro de Ciências Físicas e Matemáticas. Programa de Pós-Graduação em Quimica. Neste trabalho a técnica de SPME aliada a GC-MS foi aplicada para o estudo da degradação térmica do poli(propileno) e do poli(estireno)-co-poli(metil metacrilato). São discutidos principalmente os produtos formados, mecanismos de formação dos principais produtos e parâmetros cinéticos de degradação. Degradaram-se os polímeros num forno tubular em divers...

  3. Investigation of complete and incomplete fusion in 20Ne + 51V system using recoil range measurement

    Directory of Open Access Journals (Sweden)

    Ali Sabir

    2015-01-01

    Full Text Available Recoil range distributions of evaporation residues, populated in 20Ne + 51V reaction at Elab ≈ 145 MeV, have been studied to determine the degree of momentum transferred through the complete and incomplete fusion reactions. Evaporation residues (ERs populated through the complete and incomplete fusion reactions have been identified on the basis of their recoil range in the Al catcher medium. Measured recoil range of evaporation residues have been compared with the theoretical value calculated using the code SRIM. Range integrated cross section of observed ERs have been compared with the value predicted by statistical model code PACE4.

  4. Solid phase microextraction: measurement of volatile organic compounds (VOCs) in Dhaka City air pollution.

    Science.gov (United States)

    Hussam, A; Alauddin, M; Khan, A H; Chowdhury, D; Bibi, H; Bhattacharjee, M; Sultana, S

    2002-08-01

    A solid phase microextraction (SPME) technique was applied for the sampling of volatile organic compounds (VOCs) in ambient air polluted by two stroke autorickshaw engines and automobile exhausts in Dhaka city, Bangladesh. Analysis was carried out by capillary gas chromatography (GC) and GC-mass spectrometry (MS). The methodology was tested by insitu sampling of an aromatic hydrocarbon mixture gas standard with a precision of +/-5% and an average accuracy of 1-20%. The accuracy for total VOCs concentration measurement was about 7%. VOC's in ambient air were collected by exposing the SPME fiber at four locations in Dhaka city. The chromatograms showed signature similar to that of unburned gasoline (petrol) and weathered diesel containing more than 200 organic compounds; some of these compounds were positively identified. These are normal hydrocarbons pentane (n-C5H2) through nonacosane (n-C29H60), aromatic hydrocarbons: benzene, toluene, ethylbenzene, n-propylbenzene, n-butylbenzene, 1,3,5-trimethylbenzene, xylenes, and 1-isocyanato-3-methoxybenzene. Two samples collected near an autorickshaw station contained 783000 and 1479000 microg/m3 of VOCs. In particular, the concentration of toluene was 50-100 times higher than the threshold limiting value of 2000 microg/m3. Two other samples collected on street median showed 135000 microg/m3 and 180000 microg/m3 of total VOCs. The method detection limit of the technique for most semi-volatile organic compounds was 1 microg/m3.

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

    Directory of Open Access Journals (Sweden)

    Xibin Wang

    2016-12-01

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

  6. Standardization of radiation protection measurements in mixed fields of an extended energy range

    International Nuclear Information System (INIS)

    Hoefert, M.; Stevenson, G.R.

    1977-01-01

    The improved ICRU concept of dose equivalent index aims at standardizing both area and personnel dose measurements so that the results on the dosimetry of external irradiations in radiation protection become compatible. It seems that for photon and neutron energies up to 3 and 20 MeV respectively the realization of dose-equivalent index is straightforward, but the inclusion of higher energies and/or other types of radiation will lead both to conceptual and practical difficulties. It will be shown that practical measurements in mixed radiation fields of an extended energy range for protection purposes will overestimate the standardized quantity. While area measurements can be performed to represent a good approximation, greater uncertainties have to be accepted in personnel dosimetry for stray radiation fields around GeV proton accelerators

  7. Recovery of phosphonate surface contaminants from glass using a simple vacuum extractor with a solid-phase microextraction fiber

    International Nuclear Information System (INIS)

    Groenewold, Gary S.; Scott, Jill R.; Rae, Catherine

    2011-01-01

    Graphical abstract: Highlights: → A field vacuum extractor (FVE) nondestructively samples surface-adsorbed organics. → The FVE creates a modest vacuum over the surface, volatilizing surface organics. → A solid phase microextraction fiber (SPME) collects volatilized organics. → The SPME is easily analyzed using GC/MS. → The FVE enables collection chemical signatures from hard-to-sample surfaces. - Abstract: Recovery of chemical contaminants from fixed surfaces for analysis can be challenging, particularly if it is not possible to acquire a solid sample to be taken to the laboratory. A simple device is described that collects semi-volatile organic compounds from fixed surfaces by creating an enclosed volume over the surface, then generating a modest vacuum. A solid-phase microextraction (SPME) fiber is then inserted into the evacuated volume where it functions to sorb volatilized organic contaminants. The device is based on a syringe modified with a seal that is used to create the vacuum, with a perforable plunger through which the SPME fiber is inserted. The reduced pressure speeds partitioning of the semi-volatile compounds into the gas phase and reduces the boundary layer around the SPME fiber, which enables a fraction of the volatilized organics to partition into the SPME fiber. After sample collection, the SPME fiber is analyzed using conventional gas chromatography/mass spectrometry. The methodology has been used to collect organophosphorus compounds from glass surfaces, to provide a simple test for the functionality of the devices. Thirty minute sampling times (ΔT vac ) resulted in fractional recovery efficiencies that ranged from 10 -3 to >10 -2 , and in absolute terms, collection of low nanograms was demonstrated. Fractional recovery values were positively correlated to the vapor pressure of the compounds being sampled. Fractional recovery also increased with increasing ΔT vac and displayed a roughly logarithmic profile, indicating that an

  8. Study of aroma formation and transformation during the manufacturing process of Biluochun green tea in Yunnan Province by HS-SPME and GC-MS.

    Science.gov (United States)

    Wang, Chen; Lv, Shidong; Wu, Yuanshuang; Lian, Ming; Gao, Xuemei; Meng, Qingxiong

    2016-10-01

    Biluochun is a typical non-fermented tea and is also famous for its unique aroma in China. Few studies have been performed to evaluate the effect of the manufacturing process on the formation and content of its aroma. The volatile components were extracted at different manufacturing process steps of Biluochun green tea using fully automated headspace solid-phase microextraction (HS-SPME) and further characterised by gas chromatography-mass spectrometry (GC-MS). Among 67 volatile components collected, the fractions of linalool oxides, β-ionone, phenylacetaldehyde, aldehydes, ketones, and nitrogen compounds were increased while alcohols and hydrocarbons declined during the manufacturing process. The aroma compounds decreased the most during the drying steps. We identified a number of significantly changed components that can be used as markers and quality control during the producing process of Biluochun. The drying step played a major role in the aroma formation of green tea products and should be the most important step for quality control. © 2016 Society of Chemical Industry. © 2016 Society of Chemical Industry.

  9. A straightforward method for measuring the range of apparent density of microplastics.

    Science.gov (United States)

    Li, Lingyun; Li, Mengmeng; Deng, Hua; Cai, Li; Cai, Huiwen; Yan, Beizhan; Hu, Jun; Shi, Huahong

    2018-10-15

    Density of microplastics has been regarded as the primary property that affect the distribution and bioavailability of microplastics in the water column. For measuring the density of microplastis, we developed a simple and rapid method based on density gradient solutions. In this study, we tested four solvents to make the density gradient solutions, i.e., ethanol (0.8 g/cm 3 ), ultrapure water (1.0 g/cm 3 ), saturated NaI (1.8 g/cm 3 ) and ZnCl 2 (1.8 g/cm 3 ). Density of microplastics was measured via observing the float or sink status in the density gradient solutions. We found that density gradient solutions made from ZnCl 2 had a larger uncertainty in measuring density than that from NaI, most likely due to a higher surface tension of ZnCl 2 solution. Solutions made from ethanol, ultrapure water, and NaI showed consistent density results with listed densities of commercial products, indicating that these density gradient solutions were suitable for measuring microplastics with a density range of 0.8-1.8 g/cm 3 . Copyright © 2018 Elsevier B.V. All rights reserved.

  10. Determination of Hazardous VOCs and Nicotine Released from Mainstream Smoke by the Combination of the SPME and GC-MS Methods

    Directory of Open Access Journals (Sweden)

    Sudhir Kumar Pandey

    2010-01-01

    Full Text Available In this study, the contents of nicotine and volatile organic compounds (VOCs in mainstream smoke (MSS were analyzed using samples of four cigarette types consisting of two common brands (R and E with full (F and light (L flavor, coded with R-F, R-L, E-F, and E-L. These cigarettes were also analyzed after removing the filter portions with the assignment of a new sample code of (N as the third letter (e.g., R-L-N. A total of 44 VOCs (including nicotine were quantified by the combination of the SPME and GC-MS methods. Out of the 44 VOCs, 10 were identified as hazardous air pollutants listed by the U.S. EPA, while their concentrations exceeded the reference exposure limits set by various agencies. A clear distinction was apparent in the concentration levels of VOCs between different brands or between full and light flavors. Nicotine concentrations varied greatly between different cigarettes types of the R brand, whereas such changes were insignificant in the counterpart E brand. This thus suggests that light-flavor cigarettes do not necessarily guarantee low doses of carcinogens (and tar than regular cigarettes, as their differences can be balanced by the inhaling behavior of the smoker.

  11. At Home Photography-Based Method for Measuring Wrist Range of Motion.

    Science.gov (United States)

    Trehan, Samir K; Rancy, Schneider K; Johnsen, Parker H; Hillstrom, Howard J; Lee, Steve K; Wolfe, Scott W

    2017-11-01

    Purpose  To determine the reliability of wrist range of motion (WROM) measurements based on digital photographs taken by patients at home compared with traditional measurements done in the office with a goniometer. Methods  Sixty-nine postoperative patients were enrolled in this study at least 3 months postoperatively. Active and passive wrist flexion/extension and radial/ulnar deviation were recorded by one of the two attending surgeons with a 1-degree resolution goniometer at the last postoperative office visit. Patients were provided an illustrated instruction sheet detailing how to take digital photographic images at home in six wrist positions (active and passive flexion/extension, and radial/ulnar deviation). Wrist position was measured from digital images by both the attending surgeons in a randomized, blinded fashion on two separate occasions greater than 2 weeks apart using the same goniometer. Reliability analysis was performed using the intraclass correlation coefficient to assess agreement between clinical and photography-based goniometry, as well as intra- and interobserver agreement. Results  Out of 69 enrolled patients, 30 (43%) patients sent digital images. Of the 180 digital photographs, only 9 (5%) were missing or deemed inadequate for WROM measurements. Agreement between clinical and photography-based measurements was "almost perfect" for passive wrist flexion/extension and "substantial" for active wrist flexion/extension and radial/ulnar deviation. Inter- and intraobserver agreement for the attending surgeons was "almost perfect" for all measurements. Discussion  This study validates a photography-based goniometry protocol allowing accurate and reliable WROM measurements without direct physician contact. Passive WROM was more accurately measured from photographs than active WROM. This study builds on previous photography-based goniometry literature by validating a protocol in which patients or their families take and submit their own

  12. SU-F-T-184: 3D Range-Modulator for Scanned Particle Therapy: Development, Monte Carlo Simulations and Measurements

    Energy Technology Data Exchange (ETDEWEB)

    Simeonov, Y; Penchev, P; Ringbaek, T Printz [University of Applied Sciences, Institute of Medical Physics and Radiation Protection, Giessen (Germany); Brons, S [Heidelberg Ion-Beam Therapy Center (HIT), Heidelberg (Germany); Weber, U [GSI Helmholtzzentrum fuer Schwerionenforschung GmbH, Darmstadt (Germany); Zink, K [University of Applied Sciences, Institute of Medical Physics and Radiation Protection, Giessen (Germany); University Hospital Giessen-Marburg, Marburg (Germany)

    2016-06-15

    Purpose: Active raster scanning in particle therapy results in highly conformal dose distributions. Treatment time, however, is relatively high due to the large number of different iso-energy layers used. By using only one energy and the so called 3D range-modulator irradiation times of a few seconds only can be achieved, thus making delivery of homogeneous dose to moving targets (e.g. lung cancer) more reliable. Methods: A 3D range-modulator consisting of many pins with base area of 2.25 mm2 and different lengths was developed and manufactured with rapid prototyping technique. The form of the 3D range-modulator was optimised for a spherical target volume with 5 cm diameter placed at 25 cm in a water phantom. Monte Carlo simulations using the FLUKA package were carried out to evaluate the modulating effect of the 3D range-modulator and simulate the resulting dose distribution. The fine and complicated contour form of the 3D range-modulator was taken into account by a specially programmed user routine. Additionally FLUKA was extended with the capability of intensity modulated scanning. To verify the simulation results dose measurements were carried out at the Heidelberg Ion Therapy Center (HIT) with a 400.41 MeV 12C beam. Results: The high resolution measurements show that the 3D range-modulator is capable of producing homogeneous 3D conformal dose distributions, simultaneously reducing significantly irradiation time. Measured dose is in very good agreement with the previously conducted FLUKA simulations, where slight differences were traced back to minor manufacturing deviations from the perfect optimised form. Conclusion: Combined with the advantages of very short treatment time the 3D range-modulator could be an alternative to treat small to medium sized tumours (e.g. lung metastasis) with the same conformity as full raster-scanning treatment. Further simulations and measurements of more complex cases will be conducted to investigate the full potential of the 3D

  13. Polymeric ionic liquid coatings versus commercial solid-phase microextraction coatings for the determination of volatile compounds in cheeses.

    Science.gov (United States)

    Trujillo-Rodríguez, María J; Yu, Honglian; Cole, William T S; Ho, Tien D; Pino, Verónica; Anderson, Jared L; Afonso, Ana M

    2014-04-01

    The extraction performance of four polymeric ionic liquid (PIL)-based solid-phase microextraction (SPME) coatings has been studied and compared to that of commercial SPME coatings for the extraction of 16 volatile compounds in cheeses. The analytes include 2 free fatty acids, 2 aldehydes, 2 ketones and 10 phenols and were determined by headspace (HS)-SPME coupled to gas chromatography (GC) with flame-ionization detection (FID). The PIL-based coatings produced by UV co-polymerization were more efficient than PIL-based coatings produced by thermal AIBN polymerization. Partition coefficients of analytes between the sample and the coating (Kfs) were estimated for all PIL-based coatings and the commercial SPME fiber showing the best performance among the commercial fibers tested: carboxen-polydimethylsyloxane (CAR-PDMS). For the PIL-based fibers, the highest K(fs) value (1.96 ± 0.03) was obtained for eugenol. The normalized calibration slope, which takes into account the SPME coating thickness, was also used as a simpler approximate tool to compare the nature of the coating within the determinations, with results entirely comparable to those obtained with estimated K(fs) values. The PIL-based materials obtained by UV co-polymerization containing the 1-vinyl-3-hexylimidazolium chloride IL monomer and 1,12-di(3-vinylimiazolium)dodecane dibromide IL crosslinker exhibited the best performance in the extraction of the select analytes from cheeses. Despite a coating thickness of only 7 µm, this copolymeric sorbent coating was capable of quantitating analytes in HS-SPME in a 30 to 2000 µg L(-1) concentration range, with correlation coefficient (R) values higher than 0.9938, inter-day precision values (as relative standard deviation in %) varying from 6.1 to 20%, and detection limits down to 1.6 µg L(-1). Copyright © 2013 Elsevier B.V. All rights reserved.

  14. Zinc oxide/polypyrrole nanocomposite as a novel solid phase microextraction coating for extraction of aliphatic hydrocarbons from water and soil samples

    International Nuclear Information System (INIS)

    Amanzadeh, Hatam; Yamini, Yadollah; Moradi, Morteza

    2015-01-01

    Highlights: • ZnO/polypyrrole (ZNO/PPY) nanocomposite coating was fabricated on stainless steel. • Nanocomposite coating morphology was evaluated using scanning electron microscopy. • It was applied for HS-SPME of aliphatic hydrocarbons in water and soil samples. • Separation and determination of the hydrocarbons were performed by GC-FID. • The method is suitable for routine analysis of n-alkanes in various environmental samples. - Abstract: In this work, ZnO/PPy nanocomposite coating was fabricated on stainless steel and evaluated as a novel headspace solid phase microextraction (HS-SPME) fiber coating for extraction of ultra-trace amounts of environmental pollutants; namely, aliphatic hydrocarbons in water and soil samples. The ZnO/PPy nanocomposite were prepared by a two-step process including the electrochemical deposition of PPy on the surface of stainless steel in the first step, and the synthesis of ZnO nanorods by hydrothermal process in the pores of PPy matrix in the second step. Porous structure together with ZnO nanorods with the average diameter of 70 nm were observed on the surface by using scanning electron microscopy (SEM). The effective parameters on HS-SPME of hydrocarbons (i.e., extraction temperature, extraction time, desorption temperature, desorption time, salt concentration, and stirring rate) were investigated and optimized by one-variable-at-a-time method. Under optimized conditions (extraction temperature, 65 ± 1 °C; extraction time, 15 min; desorption temperature, 250 °C; desorption time, 3 min; salt concentration, 10% w/v; and stirring rate, 1200 rpm), the limits of detection (LODs) were found in the range of 0.08–0.5 μg L −1 , whereas the repeatability and fiber-to-fiber reproducibility were in the range 5.4–7.6% and 8.6–10.4%, respectively. Also, the accuracies obtained for the spiked n-alkanes were in the range of 85–108%; indicating the absence of matrix effects in the proposed HS-SPME method. The results

  15. Zinc oxide/polypyrrole nanocomposite as a novel solid phase microextraction coating for extraction of aliphatic hydrocarbons from water and soil samples

    Energy Technology Data Exchange (ETDEWEB)

    Amanzadeh, Hatam; Yamini, Yadollah [Department of Chemistry, Tarbiat Modares University, P.O. Box 14115-175 Tehran (Iran, Islamic Republic of); Moradi, Morteza [Department of Semiconductors, Materials and Energy Research Center, Karaj (Iran, Islamic Republic of)

    2015-07-16

    Highlights: • ZnO/polypyrrole (ZNO/PPY) nanocomposite coating was fabricated on stainless steel. • Nanocomposite coating morphology was evaluated using scanning electron microscopy. • It was applied for HS-SPME of aliphatic hydrocarbons in water and soil samples. • Separation and determination of the hydrocarbons were performed by GC-FID. • The method is suitable for routine analysis of n-alkanes in various environmental samples. - Abstract: In this work, ZnO/PPy nanocomposite coating was fabricated on stainless steel and evaluated as a novel headspace solid phase microextraction (HS-SPME) fiber coating for extraction of ultra-trace amounts of environmental pollutants; namely, aliphatic hydrocarbons in water and soil samples. The ZnO/PPy nanocomposite were prepared by a two-step process including the electrochemical deposition of PPy on the surface of stainless steel in the first step, and the synthesis of ZnO nanorods by hydrothermal process in the pores of PPy matrix in the second step. Porous structure together with ZnO nanorods with the average diameter of 70 nm were observed on the surface by using scanning electron microscopy (SEM). The effective parameters on HS-SPME of hydrocarbons (i.e., extraction temperature, extraction time, desorption temperature, desorption time, salt concentration, and stirring rate) were investigated and optimized by one-variable-at-a-time method. Under optimized conditions (extraction temperature, 65 ± 1 °C; extraction time, 15 min; desorption temperature, 250 °C; desorption time, 3 min; salt concentration, 10% w/v; and stirring rate, 1200 rpm), the limits of detection (LODs) were found in the range of 0.08–0.5 μg L{sup −1}, whereas the repeatability and fiber-to-fiber reproducibility were in the range 5.4–7.6% and 8.6–10.4%, respectively. Also, the accuracies obtained for the spiked n-alkanes were in the range of 85–108%; indicating the absence of matrix effects in the proposed HS-SPME method. The results

  16. Head Space Solid Phase Micro-Extraction (HS - SPME of volatile organic compounds produced by Sporidiobolus salmonicolor (CBS 2636

    Directory of Open Access Journals (Sweden)

    Eunice Valduga

    2010-12-01

    Full Text Available The aim of the present study was the assessment of volatile organic compounds produced by Sporidiobolus salmonicolor (CBS 2636 using methyl and ethyl ricinoleate, ricinoleic acid and castor oil as precursors. The analysis of the volatile organic compounds was carried out using Head Space Solid Phase Micro-Extraction (HS - SPME. Factorial experimental design was used for investigating extraction conditions, verifying stirring rate (0-400 rpm, temperature (25-60 ºC, extraction time (10-30 minutes, and sample volume (2-3 mL. The identification of volatile organic compounds was carried out by Gas Chromatography with Mass Spectrum Detector (GC/MSD. The conditions that resulted in maximum extraction were: 60 ºC, 10 minutes extraction, no stirring, sample volume of 2.0 mL, and addition of saturated KCl (1:10 v/v. In the bio-production of volatile organic compounds the effect of stirring rate (120-200 rpm, temperature (23-33 ºC, pH (4.0-8.0, precursor concentration (0.02-0.1%, mannitol (0-6%, and asparagine concentration (0-0.2% was investigated. The bio-production at 28 ºC, 160 rpm, pH 6,0 and with the addition of 0.02% ricinoleic acid to the medium yielded the highest production of VOCs, identified as 1,4-butanediol, 1,2,2-trimethylciclopropilamine, beta-ionone; 2,3-butanodione, pentanal, tetradecane, 2-isononenal, 4-octen-3-one, propanoic acid, and octadecane.

  17. Simultaneous determination of salicylic, 3-methyl salicylic, 4-methyl salicylic, acetylsalicylic and benzoic acids in fruit, vegetables and derived beverages by SPME-LC-UV/DAD.

    Science.gov (United States)

    Aresta, Antonella; Zambonin, Carlo

    2016-03-20

    Salicylic and benzoic acid are phenolic acids occurring in plant cells, thus they can be present in fruit and vegetables at various levels. They possess anti-inflammatory and antimicrobial properties, however they may induce symptoms and health problems in a small percentage of the population. Therefore, a low phenolic acid diet may be of clinical benefit to such individuals. In order to achieve this goal, the concentration of these substances in different food and beverages should be assessed. The present work describes for the first time a new method, based on solid phase microextraction (polydimethylsiloxane-divinylbenzene fiber) coupled to liquid chromatography with UV diode array detection, for the simultaneous determination of salicylic acid, 3-methyl salicylic acid, 4-methyl salicylic acid, acetylsalicylic acid and benzoic acid in selected fruit, vegetables and beverages. All the aspects influencing fiber adsorption (time, temperature, pH, salt addition) and desorption (desorption and injection time, desorption solvent mixture composition) of the analytes have been investigated. An isocratic separation was performed using an acetonitrile-phosphate buffer (pH 2.8; 2 mM) mixture (70:30, v/v) as the mobile phase. The estimated LOD and LOQ values (μg/mL) were in the range 0.002-0.028 and 0.007-0.095. The within-day and day-to-day precision values (RSD%) were between 4.7-6.1 and 6.6-9.4, respectively. The method has been successfully applied to the analysis of fava beans, blueberries, kiwi, tangerines, lemons, oranges and fruit juice (lemon and blueberry) samples. The major advantage of the method is that it only requires simple homogenization and/or centrifugation and dilution steps prior to SPME and injection in the LC system. Copyright © 2016 Elsevier B.V. All rights reserved.

  18. Free and glycosidically bound volatile compounds in sun-dried raisins made from different fragrance intensities grape varieties using a validated HS-SPME with GC-MS method.

    Science.gov (United States)

    Wang, Dong; Duan, Chang-Qing; Shi, Ying; Zhu, Bao-Qing; Javed, Hafiz Umer; Wang, Jun

    2017-08-01

    The conditions of sample pretreatments and HS-SPME for extracting volatile compounds from raisins were optimized, and the method was validated in the study. Free and glycosidically bound volatile compounds in three different fragrance intensities raisins were analysed using this method. There were 91 compounds identified, and 72, 26 and 8 of these compounds came from fresh grapes, the auto-oxidation of unsaturated fatty acids (UFAO) and the Maillard reaction, respectively. The aroma profiles of Thompson Seedless raisins (TSRs) and Centennial Seedless raisins (CSRs) were similar, while the floral, fruity, green and roasted aromas of CSRs were higher than those of TSRs due to the contributions of benzeneacetaldehyde, 2-pentylfuran, (E)-2-nonenal and 3-ethyl-2,5-dimethyl pyrazine. Decanal, rose oxide, geraniol, linalool and β-damascenone made the floral and fruity aromas of Zixiang Seedless raisins (ZSRs) greater than those in TSRs and CSRs, but the green and roasted aroma intensities of ZSRs were lower. Copyright © 2017 Elsevier Ltd. All rights reserved.

  19. Measurements and correlations of turbulent burning velocities over wide ranges of fuels and elevated pressures

    KAUST Repository

    Bradley, Derek; Lawes, Malcolm; Liu, Kexin; Mansour, Morkous S.

    2013-01-01

    The implosion technique has been used to extend measurements of turbulent burning velocities over greater ranges of fuels and pressures. Measurements have been made up to 3.5 MPa and at strain rate Markstein numbers as low as 23. The implosion technique, with spark ignition at two opposite wall positions within a fan-stirred spherical bomb is capable of measuring turbulent burning velocities, at higher pressures than is possible with central ignition. Pressure records and schlieren high speed photography define the rate of burning and the smoothed area of the flame front. The first aim of the study was to extend the previous measurements with ethanol and propane-air, with further measurements over wider ranges of fuels and equivalence ratios with mixtures of hydrogen, methane, 10% hydrogen-90% methane, toluene, and i-octane, with air. The second aim was to study further the low turbulence regime in which turbulent burning co-exists with laminar flame instabilities. Correlations are presented of turbulent burning velocity normalised by the effective rms turbulent velocity acting on the flame front, ut=u0k , with the Karlovitz stretch factor, K, for different strain rate Markstein numbers, a decrease in which increases ut=u0k . Experimental correlations are presented for the present measurements, combined with previous ones. Different burning regimes are also identified, extending from that of mixed turbulence/laminar instability at low values of K to that at high values of K, in which ut=u0k is gradually reduced due to increasing localised flame extinctions. © 2012 The Combustion Institute.

  20. Chemical composition analysis of the essential oil of Solanumn nigrum L. by HS/SPME method and calculation of the biochemical coefficients of the components

    Directory of Open Access Journals (Sweden)

    Avat (Arman Taherpour

    2017-05-01

    Full Text Available The volatile constituents of the essential oil of wild Solanumn nigrum L. obtained from the Kurdistan of Iraq were extracted by head-space/solid-phase micro-extraction (HS/SPME and were analyzed by gas chromatography (GC and gas chromatography/mass spectrometry (GC/MS. Of a total of twenty compounds in the oil, all of them were identified. The main components were as follows: Dillapiole (22.22%, α-Cadinol (16.47%, para-Cymene (10.01%, (E-1-(2,6,6-Trimethyl-1,3-cyclohexadien-1-yl-2-buten-1-one or β-damascenone (9.08%, α-Phellandrene (8.48%, β-Pinene (5.93%, α-Bisabolol acetate (4.53%, (Z,E-4,6,8-Megastigmatriene (4.09%, Phytol (2.49%, Linalyl butanoate (2.13%, 8-methylene-tricyclo[3.2.1.0(2,4]octane (2.60% and Limonene (2.03%. Some physicochemical properties, such as the logarithm of calculated octanol–water partitioning coefficients (logKow and total biodegradation (TBd in mol/h were calculated for compounds 1–20 from S. nigrum L.

  1. Unitarity corrections to short-range order long-range rapidity correlations

    CERN Document Server

    Capella, A

    1978-01-01

    Although the effective hadronic forces have short range in rapidity space, one nevertheless expects long-range dynamical correlations induced by unitarity constraints. This paper contains a thorough discussion of long-range rapidity correlations in high-multiplicity events. In particular, the authors analyze in detail the forward- backward multiplicity correlations, measured recently in the whole CERN ISR energy range. They find from these data that the normalized variance of the number n of exchanged cut Pomerons, ((n/(n)-1)/sup 2/) , is most probably in the range 0.32 to 0.36. They show that such a number is obtained from Reggeon theory in the eikonal approximation. The authors also predict a very specific violation of local compensation of charge in multiparticle events: The violation should appear in the fourth-order zone correlation function and is absent in the second-order correlation function, the only one measured until now. (48 refs).

  2. Dispersive solid-phase microextraction and capillary electrophoresis separation of food colorants in beverages using diamino moiety functionalized silica nanoparticles as both extractant and pseudostationary phase.

    Science.gov (United States)

    Liu, Feng-Jie; Liu, Chuan-Ting; Li, Wei; Tang, An-Na

    2015-01-01

    In this work, a new method for the determination of food colorants in beverage samples is developed, using diamino moiety functionalized silica nanoparticles (dASNPs) as both adsorbents in dispersive solid-phase microextraction (dSPME) and pseudostationary phases (PSPs) in capillary electrophoresis (CE) separation. dASNPs were firstly used as adsorbents for the preconcentration of four colorants by the dSPME process. After that, colorants were efficiently separated by CE using 30 mM phosphate buffer (pH 6.0) containing 2 mM β-CD and 0.9 mg/mL dASNPs as additives. All factors influencing dSPME and CE separations were optimized in detail. The investigated analytes showed good linearities with correlation coefficients (R(2)) higher than 0.9932. The limits of detection for the four food colorants were between 0.030 and 0.36 mg/L, which are lower than those reported previously. The established method was also used to analyze four colorants in beverage samples with recoveries ranging from 82.7% to 114.6%. To the best of our knowledge, this is the first time to use NPs both as extractants in dSPME and pseudostationary phases in CE for the analytical purpose. Copyright © 2014 Elsevier B.V. All rights reserved.

  3. Determination of trace Cd, Cu, Fe, Pb and Zn in diesel and gasoline by inductively coupled plasma mass spectrometry after sample clean up with hollow fiber solid phase microextraction system

    International Nuclear Information System (INIS)

    Nomngongo, Philiswa N.; Ngila, J. Catherine

    2014-01-01

    This study reports a simple and efficient method for the determination of trace Cd, Cu, Fe, Pb and Zn in diesel and gasoline samples by inductively coupled plasma mass spectrometry after matrix removal and analyte pre-concentration using hollow fiber-solid phase microextraction (HF–SPME). The optimization of HF-SPME procedure was carried out using two-level full factorial and central composite designs. Four factors (variables), that are, sample solution pH, acceptor phase amount, extraction time and eluent concentration were optimized. Under the optimized experimental conditions, the precision was ≤ 3% (C = 10 μg L −1 , n = 15), limits of detection and quantification ranged from 0.1 to 0.3 μg L −1 and 0.3–0.9 μg L −1 , respectively, and the maximum preconcentration factor was 30. The HF-SPME method was applied for the determination of trace metals in real gasoline and diesel samples. - Highlights: • Hollow fiber solid phase microextraction of metal ions in diesel and gasoline • Use of hollow fiber-supported sol–gel combined with cation exchange resin • Optimization of HF-SPME using multivariate techniques • Determination of Cd, Cu, Fe, Pb and Zn using ICP–MS • Relatively low LOD and LOQ

  4. Determination of trace Cd, Cu, Fe, Pb and Zn in diesel and gasoline by inductively coupled plasma mass spectrometry after sample clean up with hollow fiber solid phase microextraction system

    Energy Technology Data Exchange (ETDEWEB)

    Nomngongo, Philiswa N.; Ngila, J. Catherine, E-mail: jcngila@uj.ac.za

    2014-08-01

    This study reports a simple and efficient method for the determination of trace Cd, Cu, Fe, Pb and Zn in diesel and gasoline samples by inductively coupled plasma mass spectrometry after matrix removal and analyte pre-concentration using hollow fiber-solid phase microextraction (HF–SPME). The optimization of HF-SPME procedure was carried out using two-level full factorial and central composite designs. Four factors (variables), that are, sample solution pH, acceptor phase amount, extraction time and eluent concentration were optimized. Under the optimized experimental conditions, the precision was ≤ 3% (C = 10 μg L{sup −1}, n = 15), limits of detection and quantification ranged from 0.1 to 0.3 μg L{sup −1} and 0.3–0.9 μg L{sup −1}, respectively, and the maximum preconcentration factor was 30. The HF-SPME method was applied for the determination of trace metals in real gasoline and diesel samples. - Highlights: • Hollow fiber solid phase microextraction of metal ions in diesel and gasoline • Use of hollow fiber-supported sol–gel combined with cation exchange resin • Optimization of HF-SPME using multivariate techniques • Determination of Cd, Cu, Fe, Pb and Zn using ICP–MS • Relatively low LOD and LOQ.

  5. In situ fabrication of nanostructured titania coating on the surface of titanium wire: A new approach for preparation of solid-phase microextraction fiber

    Energy Technology Data Exchange (ETDEWEB)

    Cao Dandan [State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, P.O. Box 2871, Beijing 100085 (China); Environmental Science Division, School of Earth and Space Science, University of Science and Technology of China, Hefei, Anhui Province 230026 (China); Lue Jianxia [State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, P.O. Box 2871, Beijing 100085 (China); Liu Jingfu [State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, P.O. Box 2871, Beijing 100085 (China)], E-mail: jfliu@rcees.ac.cn; Jiang Guibin [State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, P.O. Box 2871, Beijing 100085 (China)

    2008-03-17

    Nanostructured titania-based solid-phase microextraction (SPME) fibers were fabricated through the in situ oxidation of titanium wires with H{sub 2}O{sub 2} (30%, w/w) at 80 deg. C for 24 h. The obtained SPME fibers possess a {approx}1.2 {mu}m thick nanostructured coating consisting of {approx}100 nm titania walls and 100-200 nm pores. The use of these fibers for headspace SPME coupled with gas chromatography with electron capture detection (GC-ECD) resulted in improved analysis of dichlorodiphenyltrichloroethane (DDT) and its degradation products. The presented method to detect DDT and its degradation products has high sensitivity (0.20-0.98 ng L{sup -1}), high precision (relative standard deviation R.S.D. = 9.4-16%, n = 5), a wide linear range (5-5000 ng L{sup -1}), and good linearity (coefficient of estimation R{sup 2} = 0.991-0.998). As the nanostructured titania was in situ formed on the surface of a titanium wire, the coating was uniformly and strongly adhered on the titanium wire. Because of the inherent chemical stability of the titania coating and the mechanical durability of the titanium wire substrate, this new SPME fiber exhibited long life span (over 150 times)

  6. Apparatus intended for measuring heat capacity and heat transfer down to mK range

    International Nuclear Information System (INIS)

    Hebral, B.; Frossati, G.; Godfrin, H.; Schumacher, G.; Thoulouze, D.

    1978-01-01

    A cryogenic apparatus to perform heat capacity and heat transfer measurements in the range 1.5 mK-50 mK is described. Measurements are performed in an adiabatic demagnetization cell attached to a dilution refrigerator. Heat capacity measurements were effected on CMN-helium systems; the CMN specific heat was deduced above 1.6 mK when using liquid 3 He or a mixture 1.1% 3 He - 98.9% 4 He. A specific heat anomaly was observed with 4 He below 10 mK. It does not seen possible to interprete it by simple thermal equilibrium considerations. The superfluid 3 He heat capacity was also deduced from the results obtained with liquid 3 He under pressure. In heat transfer measurements at the interface CMN-mixture 3 He- 4 He, the temperature dependence of the thermal boundary resistance is in rather good agreement with other powder results. The measured resistances are larger than those predicted by the classical phonon process [fr

  7. Identification of long-range transport of aerosols over Austria using EARLINET lidar measurements

    Science.gov (United States)

    Camelia, Talianu

    2018-04-01

    The aims of the study is to identify the paths of the long-range transported aerosols over Austria and their potential origin, and to estimate their properties, using lidar measurements from EARLINET stations closest to Austria from Germany and Romania and aerosol transport models. As of now, there is no lidar station in Austria. The study is part of a project to estimate the usefulness of a lidar station located in Vienna, Austria.

  8. 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.

  9. Assessment of health status by molecular measures in adults ranging from middle-aged to old

    DEFF Research Database (Denmark)

    Waaijer, M. E. C.; Westendorp, R. G. J.; Goldeck, D.

    2017-01-01

    In addition to measures already used in clinical practice, molecular measures have been proposed to assess health status, but these have not yet been introduced into clinical practice. We aimed to test the association of functional capacity measures used in current practice and molecular measures...... with age and health status. The cohort consisted of 178 middle-aged to old participants of the Leiden Longevity Study (range 42-82years). We tested associations between functional capacity measures (physical tests: grip strength, 4-meter walk, chair stand test; cognitive tests: Stroop test, digit symbol...... substitution test and 15-picture learning test) with age and with cardiovascular or metabolic disease as a measure of the health status. These associations with age and health status were also tested for molecular measures (C reactive protein (CRP), numbers of senescent p16INK4a positive cells in the epidermis...

  10. Measurement of volatile organic compounds emitted in libraries and archives: an inferential indicator of paper decay?

    Directory of Open Access Journals (Sweden)

    Gibson Lorraine T

    2012-05-01

    Full Text Available Abstract Background A sampling campaign of indoor air was conducted to assess the typical concentration of indoor air pollutants in 8 National Libraries and Archives across the U.K. and Ireland. At each site, two locations were chosen that contained various objects in the collection (paper, parchment, microfilm, photographic material etc. and one location was chosen to act as a sampling reference location (placed in a corridor or entrance hallway. Results Of the locations surveyed, no measurable levels of sulfur dioxide were detected and low formaldehyde vapour (-3 was measured throughout. Acetic and formic acids were measured in all locations with, for the most part, higher acetic acid levels in areas with objects compared to reference locations. A large variety of volatile organic compounds (VOCs was measured in all locations, in variable concentrations, however furfural was the only VOC to be identified consistently at higher concentration in locations with paper-based collections, compared to those locations without objects. To cross-reference the sampling data with VOCs emitted directly from books, further studies were conducted to assess emissions from paper using solid phase microextraction (SPME fibres and a newly developed method of analysis; collection of VOCs onto a polydimethylsiloxane (PDMS elastomer strip. Conclusions In this study acetic acid and furfural levels were consistently higher in concentration when measured in locations which contained paper-based items. It is therefore suggested that both acetic acid and furfural (possibly also trimethylbenzenes, ethyltoluene, decane and camphor may be present in the indoor atmosphere as a result of cellulose degradation and together may act as an inferential non-invasive marker for the deterioration of paper. Direct VOC sampling was successfully achieved using SPME fibres and analytes found in the indoor air were also identified as emissive by-products from paper. Finally a new non

  11. A novel polythiophene – ionic liquid modified clay composite solid phase microextraction fiber: Preparation, characterization and application to pesticide analysis

    International Nuclear Information System (INIS)

    Pelit, Füsun Okçu; Pelit, Levent; Dizdaş, Tuğberk Nail; Aftafa, Can; Ertaş, Hasan; Yalçınkaya, E.E.; Türkmen, Hayati; Ertaş, F.N.

    2015-01-01

    Highlights: • A novel polythiophene – ionic liquid modified clay surface has been prepared. • Polymerization was performed electrochemically on a stainless steel wire. • This material was used as a SPME fiber in head space mode. • This new SPME fiber was applied for analysis of pesticides in juice samples. • Fiber adsorption properties were improved by modification of ionic liquids. - Abstract: This report comprises the novel usage of polythiophene – ionic liquid modified clay surfaces for solid phase microextraction (SPME) fiber production to improve the analysis of pesticides in fruit juice samples. Montmorillonite (Mmt) clay intercalated with ionic liquids (IL) was co-deposited with polythiophene (PTh) polymer coated electrochemically on an SPME fiber. The surface of the fibers were characterized by using scanning electron microscopy (SEM). Operational parameters effecting the extraction efficiency namely; the sample volume and pH, adsorption temperature and time, desorption temperature and time, stirring rate and salt amount were optimized. In order to reveal the major effects, these eight factors were selected and Plackett–Burman Design was constructed. The significant parameters detected; adsorption and temperature along with the stirring rate, were further investigated by Box–Behnken design. Under optimized conditions, calibration graphs were plotted and detection limits were calculated in the range of 0.002–0.667 ng mL −1 . Relative standard deviations were no higher than 18%. Overall results have indicated that this novel PTh-IL-Mmt SPME surface developed by the aid of electrochemical deposition could offer a selective and sensitive head space analysis for the selected pesticide residues

  12. A novel polythiophene – ionic liquid modified clay composite solid phase microextraction fiber: Preparation, characterization and application to pesticide analysis

    Energy Technology Data Exchange (ETDEWEB)

    Pelit, Füsun Okçu, E-mail: fusun.okcu@ege.edu.tr; Pelit, Levent; Dizdaş, Tuğberk Nail; Aftafa, Can; Ertaş, Hasan; Yalçınkaya, E.E.; Türkmen, Hayati; Ertaş, F.N.

    2015-02-15

    Highlights: • A novel polythiophene – ionic liquid modified clay surface has been prepared. • Polymerization was performed electrochemically on a stainless steel wire. • This material was used as a SPME fiber in head space mode. • This new SPME fiber was applied for analysis of pesticides in juice samples. • Fiber adsorption properties were improved by modification of ionic liquids. - Abstract: This report comprises the novel usage of polythiophene – ionic liquid modified clay surfaces for solid phase microextraction (SPME) fiber production to improve the analysis of pesticides in fruit juice samples. Montmorillonite (Mmt) clay intercalated with ionic liquids (IL) was co-deposited with polythiophene (PTh) polymer coated electrochemically on an SPME fiber. The surface of the fibers were characterized by using scanning electron microscopy (SEM). Operational parameters effecting the extraction efficiency namely; the sample volume and pH, adsorption temperature and time, desorption temperature and time, stirring rate and salt amount were optimized. In order to reveal the major effects, these eight factors were selected and Plackett–Burman Design was constructed. The significant parameters detected; adsorption and temperature along with the stirring rate, were further investigated by Box–Behnken design. Under optimized conditions, calibration graphs were plotted and detection limits were calculated in the range of 0.002–0.667 ng mL{sup −1}. Relative standard deviations were no higher than 18%. Overall results have indicated that this novel PTh-IL-Mmt SPME surface developed by the aid of electrochemical deposition could offer a selective and sensitive head space analysis for the selected pesticide residues.

  13. Comparison of three different concepts of high dynamic range and dependability optimised current measurement digitisers for beam loss systems

    CERN Document Server

    Viganò, W; Effinger, E; Venturini, G G; Zamantzas, C

    2012-01-01

    Three Different Concepts of High Dynamic Range and Dependability Optimised Current Measurement Digitisers for Beam Loss Systems will be compared on this paper. The first concept is based on Current to Frequency Conversion, enhanced with an ADC for extending the dynamic range and decreasing the response time. A summary of 3 years’ worth of operational experience with such a system for LHC beam loss monitoring will be given. The second principle is based on an Adaptive Current to Frequency Converter implemented in an ASIC. The basic parameters of the circuit are discussed and compared with measurements. Several measures are taken to harden both circuits against single event effects and to make them tolerant for operation in radioactive environments. The third circuit is based on a Fully Differential Integrator for enhanced dynamic range, where laboratory and test installation measurements will be presented. All circuits are designed to avoid any dead time in the acquisition and have reliability and fail safe...

  14. Hardware test program for evaluation of baseline range/range rate sensor concept

    Science.gov (United States)

    Pernic, E.

    1985-01-01

    The test program Phase II effort provides additional design information in terms of range and range rate (R/R) sensor performance when observing and tracking a typical spacecraft target. The target used in the test program was a one-third scale model of the Hubble Space Telescope (HST) available at the MSFC test site where the tests were performed. A modified Bendix millimeter wave radar served as the R/R sensor test bed for evaluation of range and range rate tracking performance, and generation of radar signature characteristics of the spacecraft target. A summary of program test results and conclusions are presented along with detailed description of the Bendix test bed radar with accompaning instrumentation. The MSFC test site and facilities are described. The test procedures used to establish background levels, and the calibration procedures used in the range accuracy tests and RCS (radar cross section) signature measurements, are presented and a condensed version of the daily log kept during the 5 September through 17 September test period is also presented. The test program results are given starting with the RCS signature measurements, then continuing with range measurement accuracy test results and finally the range and range rate tracking accuracy test results.

  15. Reliability of the American Medical Association guides' model for measuring spinal range of motion. Its implication for whole-person impairment rating.

    Science.gov (United States)

    Nitschke, J E; Nattrass, C L; Disler, P B; Chou, M J; Ooi, K T

    1999-02-01

    Repeated measures design for intra- and interrater reliability. To determine the intra- and interrater reliability of the lumbar spine range of motion measured with a dual inclinometer, and the thoracolumbar spine range of motion measured with a long-arm goniometer, as recommended in the American Medical Association Guides. The American Medical Association Guides (2nd and 4th editions) recommend using measurements of thoracolumbar and lumbar range of movement, respectively, to estimate the percentage of permanent impairment in patients with chronic low back pain. However, the reliability of this method of estimating impairment has not been determined. In all, 34 subjects participated in the study, 21 women with a mean age of 40.1 years (SD, +/- 11.1) and 13 men with a mean age of 47.7 years (SD, +/- 12.1). Measures of thoracolumbar flexion, extension, lateral flexion, and rotation were obtained with a long-arm goniometer. Lumbar flexion, extension, and lateral flexion were measured with a dual inclinometer. Measurements were taken by two examiners on one occasion and by one examiner on two occasions approximately 1 week apart. The results showed poor intra- and interrater reliability for all measurements taken with both instruments. Measurement error expressed in degrees showed that measurements taken by different raters exhibited systematic as well as random differences. As a result, subjects measured by two different examiners on the same day, with either instrument, could give impairment ratings ranging between 0% and 18% of the whole person (excluding rotation), in which percentage impairment is calculated using the average range of motion and the average systematic and random error in degrees for the group for each movement (flexion, extension, and lateral flexion). The poor reliability of the American Medical Association Guides' spinal range of motion model can result in marked variation in the percentage of whole-body impairment. These findings have

  16. Feasibility of RACT for 3D dose measurement and range verification in a water phantom

    Energy Technology Data Exchange (ETDEWEB)

    Alsanea, Fahed [School of Health Sciences, Purdue University, 550 Stadium Mall Drive, West Lafayette, Indiana 47907-2051 (United States); Moskvin, Vadim [Radiation Oncology, Indiana University School of Medicine, 535 Barnhill Drive, RT 041, Indianapolis, Indiana 46202-5289 (United States); Stantz, Keith M., E-mail: kstantz@purdue.edu [School of Health Sciences, Purdue University, 550 Stadium Mall Drive, West Lafayette, Indiana 47907-2051 and Radiology and Imaging Sciences, Indiana University School of Medicine, 950 West Walnut Street, Indianapolis, Indiana 46202-5289 (United States)

    2015-02-15

    Purpose: The objective of this study is to establish the feasibility of using radiation-induced acoustics to measure the range and Bragg peak dose from a pulsed proton beam. Simulation studies implementing a prototype scanner design based on computed tomographic methods were performed to investigate the sensitivity to proton range and integral dose. Methods: Derived from thermodynamic wave equation, the pressure signals generated from the dose deposited from a pulsed proton beam with a 1 cm lateral beam width and a range of 16, 20, and 27 cm in water using Monte Carlo methods were simulated. The resulting dosimetric images were reconstructed implementing a 3D filtered backprojection algorithm and the pressure signals acquired from a 71-transducer array with a cylindrical geometry (30 × 40 cm) rotated over 2π about its central axis. Dependencies on the detector bandwidth and proton beam pulse width were performed, after which, different noise levels were added to the detector signals (using 1 μs pulse width and a 0.5 MHz cutoff frequency/hydrophone) to investigate the statistical and systematic errors in the proton range (at 20 cm) and Bragg peak dose (of 1 cGy). Results: The reconstructed radioacoustic computed tomographic image intensity was shown to be linearly correlated to the dose within the Bragg peak. And, based on noise dependent studies, a detector sensitivity of 38 mPa was necessary to determine the proton range to within 1.0 mm (full-width at half-maximum) (systematic error < 150 μm) for a 1 cGy Bragg peak dose, where the integral dose within the Bragg peak was measured to within 2%. For existing hydrophone detector sensitivities, a Bragg peak dose of 1.6 cGy is possible. Conclusions: This study demonstrates that computed tomographic scanner based on ionizing radiation-induced acoustics can be used to verify dose distribution and proton range with centi-Gray sensitivity. Realizing this technology into the clinic has the potential to significantly

  17. Measurement of transparency ratios for protons from short-range correlated pairs

    Science.gov (United States)

    Hen, O.; Hakobyan, H.; Shneor, R.; Piasetzky, E.; Weinstein, L. B.; Brooks, W. K.; May-Tal Beck, S.; Gilad, S.; Korover, I.; Beck, A.; Adhikari, K. P.; Aghasyan, M.; Amaryan, M. J.; Anefalos Pereira, S.; Arrington, J. R.; Baghdasaryan, H.; Ball, J.; Battaglieri, M.; Batourine, V.; Bedlinskiy, I.; Biselli, A. S.; Bono, J.; Boiarinov, S.; Briscoe, W. J.; Burkert, V. D.; Carman, D. S.; Celentano, A.; Chandavar, S.; Cole, P. L.; Contalbrigo, M.; Crede, V.; D'Angelo, A.; Dashyan, N.; De Vita, R.; De Sanctis, E.; Deur, A.; Djalali, C.; Dodge, G. E.; Doughty, D.; Dupre, R.; Egiyan, H.; El Alaoui, A.; El Fassi, L.; Eugenio, P.; Fedotov, G.; Fegan, S.; Fleming, J. A.; Gabrielyan, M. Y.; Gevorgyan, N.; Gilfoyle, G. P.; Giovanetti, K. L.; Girod, F. X.; Goetz, J. T.; Gohn, W.; Golovatch, E.; Gothe, R. W.; Griffioen, K. A.; Guo, L.; Hafidi, K.; Harrison, N.; Heddle, D.; Hicks, K.; Holtrop, M.; Hyde, C. E.; Ilieva, Y.; Ireland, D. G.; Ishkhanov, B. S.; Isupov, E. L.; Jo, H. S.; Joo, K.; Keller, D.; Khandaker, M.; Khetarpal, P.; Kim, A.; Klein, F. J.; Koirala, S.; Kubarovsky, A.; Kubarovsky, V.; Kuhn, S. E.; Livingston, K.; Lu, H. Y.; MacGregor, I. J. D.; Martinez, D.; Mayer, M.; McKinnon, B.; Mineeva, T.; Mokeev, V.; Montgomery, R. A.; Moutarde, H.; Munevar, E.; Munoz Camacho, C.; Mustapha, B.; Nadel-Turonski, P.; Nasseripour, R.; Niccolai, S.; Niculescu, G.; Niculescu, I.; Osipenko, M.; Ostrovidov, A. I.; Pappalardo, L. L.; Paremuzyan, R.; Park, K.; Park, S.; Pasyuk, E.; Phelps, E.; Phillips, J. J.; Pisano, S.; Pivnyuk, N.; Pogorelko, O.; Pozdniakov, S.; Price, J. W.; Procureur, S.; Protopopescu, D.; Puckett, A. J. R.; Raue, B. A.; Rimal, D.; Ripani, M.; Ritchie, B. G.; Rosner, G.; Rossi, P.; Sabatié, F.; Saini, M. S.; Schott, D.; Schumacher, R. A.; Seraydaryan, H.; Sharabian, Y. G.; Smith, G. D.; Sober, D. I.; Sokhan, D.; Stepanyan, S. S.; Stepanyan, S.; Strauch, S.; Taiuti, M.; Tang, W.; Taylor, C. E.; Tian, Ye; Tkachenko, S.; Ungaro, M.; Vernarsky, B.; Vlassov, A.; Voskanyan, H.; Voutier, E.; Walford, N. K.; Watts, D. P.; Wood, M. H.; Zachariou, N.; Zana, L.; Zhang, J.; Zheng, X.; Zonta, I.

    2013-05-01

    Nuclear transparency, Tp (A), is a measure of the average probability for a struck proton to escape the nucleus without significant re-interaction. Previously, nuclear transparencies were extracted for quasi-elastic A (e ,e‧ p) knockout of protons with momentum below the Fermi momentum, where the spectral functions are well known. In this Letter we extract a novel observable, the transparency ratio, Tp (A) /Tp(12 C), for knockout of high-missing-momentum protons from the breakup of short-range correlated pairs (2N-SRC) in Al, Fe and Pb nuclei relative to C. The ratios were measured at momentum transfer Q2 ⩾ 1.5(GeV /c) 2 and xB ⩾ 1.2 where the reaction is expected to be dominated by electron scattering from 2N-SRC. The transparency ratios of the knocked-out protons coming from 2N-SRC breakup are 20-30% lower than those of previous results for low missing momentum. They agree with Glauber calculations and agree with renormalization of the previously published transparencies as proposed by recent theoretical investigations. The new transparencies scale as A - 1 / 3, which is consistent with dominance of scattering from nucleons at the nuclear surface.

  18. Multi-functional measurement systems for studying photon-hadron interactions in the intermediate energy range

    International Nuclear Information System (INIS)

    Baranov, P.S.; Vol'nov, M.I.; Eliseev, A.N.

    1983-01-01

    The PION multifunctional time-of-flight measurement system operating on-line with the D-116 computer is described. The system is designed to study proton-hadron interaction processes using the PACHRA synchrotron beam. The following devices are involved into the basic permanent system equipment: two gamma telescope counters, neutron spectrometer, scintillation mass spectrometer, and also cryogenic liquid hydrogen and liquid deuterium targets, ionization chambers, and quantometer. The time-of-flight neutron spectrometer consists of 4 coordinate-sensitive scintillation counters, before which the logic detector operating in the anticoincidence regime is placed. Information acquisition and measurement system control are accomplished by the computer using the CAMAK modules. The above system allows one to observe at the same time different physical processes and to carry out simultaneous measurements in a wide energy range

  19. Impact of Microbial Composition of Cambodian Traditional Dried Starters (Dombea on Flavor Compounds of Rice Wine: Combining Amplicon Sequencing With HP-SPME-GCMS

    Directory of Open Access Journals (Sweden)

    Sokny Ly

    2018-05-01

    Full Text Available Dombae is a traditional ferment starter which has been used for starchy based wine production in Cambodia. However, the production technology of rice wine in Cambodia is not optimized. The current study aimed to investigate the microbiota associated in five ferment starters and the effect of a traditional fermentation process using a metagenomics sequencing analysis and HS-SPME-GCMS for the characterization of the aromatic profiles at the end of fermentation. Most of bacteria identified in this study were lactic acid bacteria including Weissella cibaria, Pediococcus sp. MMZ60A, Lactobacillus fermentum, and Lactobacillus plantarum. Saccharomyces cerevisiae and Saccharomycopsis fibuligera were found to be abundant yeasts while the only amylolytic filamentous fungus was Rhizopus oryzae. A total of 25 aromatic compounds were detected and identified as esters, alcohols, acids, ketones and aldehydes. The alcohol group was dominant in each rice wine. Significant changes were observed at the level of microbial communities during fermentation, suggesting microbial succession for the assimilation of starch and subsequently assimilation of fermentation by-products leading to the production of flavor compounds. At this level, the presence of Weissella, Pediococcus, and Lactobacillus genus was strongly correlated with most of the flavor compounds detected.

  20. Impact of Microbial Composition of Cambodian Traditional Dried Starters (Dombea) on Flavor Compounds of Rice Wine: Combining Amplicon Sequencing With HP-SPME-GCMS

    Science.gov (United States)

    Ly, Sokny; Mith, Hasika; Tarayre, Cédric; Taminiau, Bernard; Daube, Georges; Fauconnier, Marie-Laure; Delvigne, Frank

    2018-01-01

    Dombae is a traditional ferment starter which has been used for starchy based wine production in Cambodia. However, the production technology of rice wine in Cambodia is not optimized. The current study aimed to investigate the microbiota associated in five ferment starters and the effect of a traditional fermentation process using a metagenomics sequencing analysis and HS-SPME-GCMS for the characterization of the aromatic profiles at the end of fermentation. Most of bacteria identified in this study were lactic acid bacteria including Weissella cibaria, Pediococcus sp. MMZ60A, Lactobacillus fermentum, and Lactobacillus plantarum. Saccharomyces cerevisiae and Saccharomycopsis fibuligera were found to be abundant yeasts while the only amylolytic filamentous fungus was Rhizopus oryzae. A total of 25 aromatic compounds were detected and identified as esters, alcohols, acids, ketones and aldehydes. The alcohol group was dominant in each rice wine. Significant changes were observed at the level of microbial communities during fermentation, suggesting microbial succession for the assimilation of starch and subsequently assimilation of fermentation by-products leading to the production of flavor compounds. At this level, the presence of Weissella, Pediococcus, and Lactobacillus genus was strongly correlated with most of the flavor compounds detected. PMID:29867806

  1. A new polyethylene glycol fiber prepared by coating porous zinc electrodeposited onto silver for solid-phase microextraction of styrene

    International Nuclear Information System (INIS)

    Sungkaew, Sakchaibordee; Thammakhet, Chongdee; Thavarungkul, Panote; Kanatharana, Proespichaya

    2010-01-01

    A new polyethylene glycol fiber was developed for solid-phase microextraction (SPME) of styrene by electrodepositing porous Zn film on Ag wire substrate followed by coating with polyethylene glycol sol-gel (Ag/Zn/PEG sol-gel fiber). The scanning electron micrographs of fibers surface revealed a highly porous structure. The extraction property of the developed fiber-to-styrene residue from polystyrene packaged food was investigated by headspace solid-phase microextraction (HS-SPME) and analyzed with a gas chromatograph coupled with flame ionization detection (GC-FID). The new Ag/Zn/PEG sol-gel fiber is simple to prepare, low cost, robust, has high thermal stability and long lifetime, up to 359 extractions. Repeatability of one fiber (n = 6) was in the range of 4.7-7.5% and fiber-to-fiber reproducibility (n = 4) for five concentration values were in the range 3.4-10%. This Ag/Zn/PEG sol-gel fiber was compared to two commercial SPME fibers, 75 μm carboxen/polydimethylsiloxane (CAR/PDMS) and 100 μm polydimethylsiloxane (PDMS). Under their optimum conditions, Ag/Zn/PEG sol-gel fiber showed the highest sensitivity and the lowest detection limit at 0.28 ± 0.01 ng mL -1 .

  2. Determination of Methyl tert-Butyl Ether and tert-Butyl Alcohol in Water by Solid-Phase Microextraction/Head Space Analysis in Comparison to EPA Method 5030/8260B

    Energy Technology Data Exchange (ETDEWEB)

    Oh, Keun-Chan; Stringfellow, William T.

    2003-10-02

    Methyl tert-butyl ether (MTBE) is now one of the most common groundwater contaminants in the United States. Groundwater contaminated with MTBE is also likely to be contaminated with tert-butyl alcohol (TBA), because TBA is a component of commercial grade MTBE, TBA can also be used as a fuel oxygenate, and TBA is a biodegradation product of MTBE. In California, MTBE is subject to reporting at concentrations greater than 3 {micro}g/L. TBA is classified as a ''contaminant of current interest'' and has a drinking water action level of 12 {micro}g/L. In this paper, we describe the development and optimization of a simple, automated solid phase microextraction (SPME) method for the analysis of MTBE and TBA in water and demonstrate the applicability of this method for monitoring MTBE and TBA contamination in groundwater, drinking water, and surface water. In this method, the headspace (HS) of a water sample is extracted with a carboxen/polydimethylsiloxane SPME fiber, the MTBE and TBA are desorbed into a gas chromatograph (GC), and detected using mass spectrometry (MS). The method is optimized for the routine analysis of MTBE and TBA with a level of quantitation of 0.3 {micro}g/L and 4 {micro}g/L, respectively, in water. MTBE quantitation was linear for over two orders of concentration (0.3 {micro}g/L -80 {micro}g/L). TBA was found to be linear within the range of 4 {micro}g/L-7,900 {micro}g/L. The lower level of detection for MTBE is 0.03 {micro}g/L using this method. This SPME method using headspace extraction was found to be advantageous over SPME methods requiring immersion of the fiber into the water samples, because it prolonged the life of the fiber by up to 400 sample analyses. This is the first time headspace extraction SPME has been shown to be applicable to the measurement of both MTBE and TBA at concentrations below regulatory action levels. This method was compared with the certified EPA Method 5030/8260B (purge-and-trap/GC/MS) using split

  3. Identification of Volatile Components of Liverwort (Porella cordaeana Extracts Using GC/MS-SPME and Their Antimicrobial Activity

    Directory of Open Access Journals (Sweden)

    Maria Elisabetta Guerzoni

    2012-06-01

    Full Text Available Chemical constituents of liverwort (Porella cordaeana extracts have been identified using solid-phase microextraction-gas chromatography mass spectrometry (SPME-GC/MS. The methanol, ethanol and ethyl acetate extracts were rich in terpenoids such as sesquiterpene hydrocarbons (53.12%, 51.68%, 23.16%, and monoterpene hydrocarbons (22.83%, 18.90%, 23.36%, respectively. The dominant compounds in the extracts were β-phellandrene (15.54%, 13.66%, 12.10% and β-caryophyllene (10.72%, 8.29%, 7.79%, respectively. The antimicrobial activity of the extracts was evaluated against eleven food microorganisms using the microdilution and disc diffusion methods. The minimum inhibitory concentration (MIC varied from 0.50 to 2.00 mg/mL for yeast strains (Saccharomyces cerevisiae 635, Zygosacharomyces bailii 45, Aerobasidium pullulans L6F, Pichia membranaefaciens OC 71, Pichia membranaefaciens OC 70, Pichia anomala CBS 5759, Pichia anomala DBVPG 3003 and Yarrowia lipolytica RO13, and from 1.00 to 3.00 mg/mL for bacterial strains (Salmonella enteritidis 155, Escherichia coli 555 and Listeria monocytogenes 56Ly. Methanol extract showed better activity in comparison with ethanol and ethyl acetate extracts. High percentages of monoterpene and sesquiterpene hydrocarbons could be responsible for the better antimicrobial activity.

  4. Análise de fármacos em material biológico: acoplamento microextração em fase sólida "no tubo" e cromatografia líquida de alta eficiência Analysis of drugs in biological samples: automated "in-tube" solid-phase microextraction and high performance liquid chromatography

    Directory of Open Access Journals (Sweden)

    Maria Eugênia C. Queiroz

    2005-10-01

    Full Text Available A new solid phase microextraction (SPME system, known as in-tube SPME, was recently developed using an open tubular fused-silica capilary column, instead of an SPME fiber, as the SPME device. On-line in-tube SPME is usually used in combination with high performance liquid chromatography. Drugs in biological samples are directly extracted and concentrated in the stationary phase of capillary columns by repeated draw/eject cycles of sample solution, and then directly transferred to the liquid chromatographic column. In-tube SPME is suitable for automation. Automated sample handling procedures not only shorten the total analysis time, but also usually provide better accuracy and precision relative to manual techniques. In-tube SPME has been demonstrated to be a very effective and highly sensitive technique to determine drugs in biological samples for various purposes such as therapeutic drug monitoring, clinical toxicology, bioavailability and pharmacokinetics.

  5. Volatiles and primary metabolites profiling in two Hibiscus sabdariffa (roselle) cultivars via headspace SPME-GC-MS and chemometrics.

    Science.gov (United States)

    Farag, Mohamed A; Rasheed, Dalia M; Kamal, Islam M

    2015-12-01

    Hibiscus sabdariffa (roselle) is a plant of considerable commercial importance worldwide as functional food due to its organic acids, mucilage, anthocyanins, macro and micro-nutrients content. Although Hibiscus flowers are emerging as very competitive targets for phytochemical studies, very little is known about their volatile composition and or aroma, such knowledge can be suspected to be relevant for understanding its olfactory and taste properties. To provide insight into Hibiscus flower aroma composition and for its future use in food and or pharmaceutical industry, volatile constituents from 2 cultivars grown in Egypt, viz. Aswan and Sudan-1 were profiled using solid-phase microextraction (SPME) coupled to GCMS. A total of 104 volatiles were identified with sugar and fatty acid derived volatiles amounting for the major volatile classes. To reveal for cultivar effect on volatile composition in an untargeted manner, multivariate data analysis was applied. Orthogonal projection to latent structures-discriminant analysis (OPLS-DA) revealed for 1-octen-3-ol versus furfural/acetic acid enrichment in Aswan and Sudan-1 cvs., respectively. Primary metabolites contributing to roselle taste and nutritional value viz. sugars and organic acids were profiled using GC-MS after silylation. The impact of probiotic bacteria on roselle infusion aroma profile was further assessed and revealed for the increase in furfural production with Lactobacillus plantarum inoculation and without affecting its anthocyanin content. This study provides the most complete map for volatiles, sugars and organic acids distribution in two Hibiscus flower cultivars and its fermented product. Copyright © 2015 Elsevier Ltd. All rights reserved.

  6. A liquid crystalline medium for measuring residual dipolar couplings over a wide range of temperatures

    Energy Technology Data Exchange (ETDEWEB)

    Wang Hong; Eberstadt, Matthias; Olejniczak, Edward T.; Meadows, Robert P.; Fesik, Stephen W. [Abbott Laboratories (United States)

    1998-10-15

    A mixture of dilauroyl phosphatidylcholine (DLPC) and 3-(cholamidopropyl)dimethylammonio-2-hydroxyl-1-propane sulfonate (CHAPSO) in water forms disc shaped bicelles that become ordered at high magnetic fields over a wide range of temperatures. As illustrated for the FK506 binding protein (FKBP), large residual dipolar couplings can be measured for proteins dissolved in low concentrations (5% w/v) of a DLPC/CHAPSO medium at a molar ratio of 4.2:1. This system is especially useful for measuring residual dipolar couplings for molecules that are only stable at low temperatures.

  7. 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.

  8. High-molecular products analysis of VOC destruction in atmospheric pressure discharge

    International Nuclear Information System (INIS)

    Grossmannova, Hana; Ciganek, Miroslav; Krcma, Frantisek

    2007-01-01

    We investigate the issue of applicability of the solid phase microextraction (SPME) in the analysis of volatile organic compounds (VOCs) destruction products in the gliding arc discharge. Our research is focused on the measurements with the simple one stage gliding arc reactor, applied voltage was varied in the range of 3.5-4 kV. As a carrier gas, the dry air and its mixtures with nitrogen and oxygen, enriched by toluene, with flow rate of 1000-3500 ml/min was used. Total decomposition of toluene of 97 % was achieved at the oxygen content in carrier gas of 60 %. For measurements with air as a carrier gas, the highest efficiency was 95 %. We also tested the SPME technique suitability for the quantitative analysis of exhausts gases and if this technique can be used efficiently in the field to extract byproducts. Carbowax/divinylbenzene and Carboxen/polydimethylsiloxane/divinylbenzene fibres were chosen for sampling. Tens of various high-molecular substances were observed, especially a large number of oxygenous compounds and further several nitrogenous and C x H y compounds. The concentrations of various generated compounds strongly depend on the oxygen content in gas mixture composition. The results showed that the fiber coated by Carbowax/divinylbenzene can extract more products independently on the used VOC compound. The Carboxen/polydimethylsiloxane/divinylbenzene fiber is useful for the analysis of oxygenous compounds and its use will be recommended especially when the destruction is done in the oxygen rich atmosphere. With the higher ratio of oxygen in the carrier gas a distinctive decline of C x H y compounds amount have been observed. We also tried to describe the significant production of some compounds like benzyl alcohol, benzeneacetaldehyde, even in oxygen content is proximate 0 %. Experimental data demonstrated that it is necessary to use several SPME fibres for full-scale high-molecular products analysis

  9. Measurement of the extreme ankle range of motion required by female ballet dancers.

    Science.gov (United States)

    Russell, Jeffrey A; Kruse, David W; Nevill, Alan M; Koutedakis, Yiannis; Wyon, Matthew A

    2010-12-01

    Female ballet dancers require extreme ankle motion, especially plantar flexion, but research about measuring such motion is lacking. The purposes of this study were to determine in a sample of ballet dancers whether non-weight-bearing ankle range of motion is significantly different from the weight-bearing equivalent and whether inclinometric plantar flexion measurement is a suitable substitute for standard plantar flexion goniometry. Fifteen female ballet dancers (5 university, 5 vocational, and 5 professional dancers; age 21 ± 3.0 years) volunteered. Subjects received 5 assessments on 1 ankle: non-weight-bearing goniometry dorsiflexion (NDF) and plantar flexion (NPF), weight-bearing goniometry in the ballet positions demi-plié (WDF) and en pointe (WPF), and non-weight-bearing plantar flexion inclinometry (IPF). Mean NDF was significantly lower than WDF (17° ± 1.3° vs 30° ± 1.8°, P ballet proficiency. The authors conclude that assessment of extreme ankle motion in female ballet dancers is challenging, and goniometry and inclinometry appear to measure plantar flexion differently.

  10. Preparation by low-temperature nonthermal plasma of graphite fiber and its characteristics for solid-phase microextraction

    International Nuclear Information System (INIS)

    Luo Fan; Wu Zucheng; Tao Ping; Cong Yanqing

    2009-01-01

    Low-temperature nonthermal plasma has been used to prepare solid-phase microextraction (SPME) fibers with high adsorbability, long-term serviceability, and high reproducibility. Graphite rods serving as fiber precursors were treated by an air plasma discharged at 15.2-15.5 kV for a duration of 8 min. Sampling results revealed that the adsorptive capacity of the homemade fiber was 2.5-34.6 times that of a polyacrylate (PA) fiber for alcohols (methanol, ethanol, isopropyl alcohol, n-butyl alcohol), and about 1.4-1.6 times and 2.5-5.1 times that of an activated carbon fiber (ACF) for alcohols and BTEX (benzene, toluene, ethylbenzene, and xylenes), respectively. It is confirmed from FTIR (Fourier transform infrared spectrophotometer) and SEM (scanning electron microscope) analyses that the improvement in the adsorptive performance attributed to increased surface energy and roughness of the graphite fiber. Using gas chromatography (GC)-flame-ionization detector (FID), the limits of detection (LODs) of the alcohols and BTEX ranged between 0.19 and 3.75 μg L -1 , the linear ranges were between 0.6 and 35619 μg L -1 with good linearity (R 2 = 0.9964-0.9997). It was demonstrated that nonthermal plasma offers a fast and simple method for preparing an efficient graphite SPME fiber, and that SPME using the homemade fiber represents a sensitive and selective extraction method for the analysis of a wide range of organic compounds

  11. Preparation by low-temperature nonthermal plasma of graphite fiber and its characteristics for solid-phase microextraction

    Energy Technology Data Exchange (ETDEWEB)

    Luo Fan [Department of Environmental Engineering, State Key Laboratory of Clean Energy Utilization, Key Laboratory of Polluted Environment Remediation and Ecological Health, MOE, Zhejiang University, Hangzhou 310027 (China); Wu Zucheng [Department of Environmental Engineering, State Key Laboratory of Clean Energy Utilization, Key Laboratory of Polluted Environment Remediation and Ecological Health, MOE, Zhejiang University, Hangzhou 310027 (China)], E-mail: wuzc@zju.edu.cn; Tao Ping [Institute of Structural Mechanics, China Academy of Engineering Physics, Mianyang 621900 (China); Cong Yanqing [College of Environmental Science and Engineering, Zhejiang Gongshang University, Hangzhou 310012 (China)

    2009-01-05

    Low-temperature nonthermal plasma has been used to prepare solid-phase microextraction (SPME) fibers with high adsorbability, long-term serviceability, and high reproducibility. Graphite rods serving as fiber precursors were treated by an air plasma discharged at 15.2-15.5 kV for a duration of 8 min. Sampling results revealed that the adsorptive capacity of the homemade fiber was 2.5-34.6 times that of a polyacrylate (PA) fiber for alcohols (methanol, ethanol, isopropyl alcohol, n-butyl alcohol), and about 1.4-1.6 times and 2.5-5.1 times that of an activated carbon fiber (ACF) for alcohols and BTEX (benzene, toluene, ethylbenzene, and xylenes), respectively. It is confirmed from FTIR (Fourier transform infrared spectrophotometer) and SEM (scanning electron microscope) analyses that the improvement in the adsorptive performance attributed to increased surface energy and roughness of the graphite fiber. Using gas chromatography (GC)-flame-ionization detector (FID), the limits of detection (LODs) of the alcohols and BTEX ranged between 0.19 and 3.75 {mu}g L{sup -1}, the linear ranges were between 0.6 and 35619 {mu}g L{sup -1} with good linearity (R{sup 2} = 0.9964-0.9997). It was demonstrated that nonthermal plasma offers a fast and simple method for preparing an efficient graphite SPME fiber, and that SPME using the homemade fiber represents a sensitive and selective extraction method for the analysis of a wide range of organic compounds.

  12. Preparation by low-temperature nonthermal plasma of graphite fiber and its characteristics for solid-phase microextraction.

    Science.gov (United States)

    Luo, Fan; Wu, Zucheng; Tao, Ping; Cong, Yanqing

    2009-01-05

    Low-temperature nonthermal plasma has been used to prepare solid-phase microextraction (SPME) fibers with high adsorbability, long-term serviceability, and high reproducibility. Graphite rods serving as fiber precursors were treated by an air plasma discharged at 15.2-15.5 kV for a duration of 8 min. Sampling results revealed that the adsorptive capacity of the homemade fiber was 2.5-34.6 times that of a polyacrylate (PA) fiber for alcohols (methanol, ethanol, isopropyl alcohol, n-butyl alcohol), and about 1.4-1.6 times and 2.5-5.1 times that of an activated carbon fiber (ACF) for alcohols and BTEX (benzene, toluene, ethylbenzene, and xylenes), respectively. It is confirmed from FTIR (Fourier transform infrared spectrophotometer) and SEM (scanning electron microscope) analyses that the improvement in the adsorptive performance attributed to increased surface energy and roughness of the graphite fiber. Using gas chromatography (GC)-flame-ionization detector (FID), the limits of detection (LODs) of the alcohols and BTEX ranged between 0.19 and 3.75 microg L(-1), the linear ranges were between 0.6 and 35,619 microg L(-1) with good linearity (R(2)=0.9964-0.9997). It was demonstrated that nonthermal plasma offers a fast and simple method for preparing an efficient graphite SPME fiber, and that SPME using the homemade fiber represents a sensitive and selective extraction method for the analysis of a wide range of organic compounds.

  13. Nanostructured polypyrrole for automated and electrochemically controlled in-tube solid-phase microextraction of cationic nitrogen compounds

    International Nuclear Information System (INIS)

    Asiabi, Hamid; Yamini, Yadollah; Rezaei, Fatemeh; Seidi, Shahram

    2015-01-01

    The authors describe an efficient method for microextraction and preconcentration of trace quantities of cationic nitrogen compounds, specifically of anilines. It relies on a combination of electrochemically controlled solid-phase microextraction and on-line in-tube solid-phase microextraction (SPME) using polypyrrole-coated capillaries. Nanostructured polypyrrole was electrically deposited on the inner surface of a stainless steel tube and used as the extraction phase. It also acts as a polypyrrole electrode that was used as a cation exchanger, and a platinum electrode that was used as the anode. The solution to be extracted is passed over the inner surface of the polypyrrole electrode, upon which cations are extracted by applying a negative potential under flow conditions. This method represents an ideal technique for SPME of protonated anilines because it is fast, easily automated, solvent-free, and inexpensive. Under optimal conditions, the limits of detection are in the 0.10–0.30 μg L -1 range. The method works in the 0.10 to 300 μg L -1 concentration range. The inter- and intra-assay precisions (RSD%; for n = 3) range from 5.1 to 7.5 % and from 4.7 to 6.0 % at the concentration levels of 2, 10 and 20 μg L -1 , respectively. The EC-in-tube SPME method was successfully applied to the analysis of methyl-, 4-chloro-, 3-chloro and 3,4-dichloroanilines in (spiked) water samples. (author)

  14. In-flight measurements and RCS-predictions: A comparison on broad-side radar range profiles of a Boeing 737

    NARCIS (Netherlands)

    Heiden, R. van der; Ewijk, L.J. van; Groen, F.C.A.

    1997-01-01

    The validation of Radar Cross Section (RCS) prediction techniques against real measurements is crucial to acquire confidence in predictions when measurements are not available. In this paper we present the first results of a comparison on one dimensional images, i.e., radar range profiles. The

  15. Outlier Detection in GNSS Pseudo-Range/Doppler Measurements for Robust Localization

    Directory of Open Access Journals (Sweden)

    Salim Zair

    2016-04-01

    Full Text Available In urban areas or space-constrained environments with obstacles, vehicle localization using Global Navigation Satellite System (GNSS data is hindered by Non-Line Of Sight (NLOS and multipath receptions. These phenomena induce faulty data that disrupt the precise localization of the GNSS receiver. In this study, we detect the outliers among the observations, Pseudo-Range (PR and/or Doppler measurements, and we evaluate how discarding them improves the localization. We specify a contrario modeling for GNSS raw data to derive an algorithm that partitions the dataset between inliers and outliers. Then, only the inlier data are considered in the localization process performed either through a classical Particle Filter (PF or a Rao-Blackwellization (RB approach. Both localization algorithms exclusively use GNSS data, but they differ by the way Doppler measurements are processed. An experiment has been performed with a GPS receiver aboard a vehicle. Results show that the proposed algorithms are able to detect the ‘outliers’ in the raw data while being robust to non-Gaussian noise and to intermittent satellite blockage. We compare the performance results achieved either estimating only PR outliers or estimating both PR and Doppler outliers. The best localization is achieved using the RB approach coupled with PR-Doppler outlier estimation.

  16. Accurate dew-point measurement over a wide temperature range using a quartz crystal microbalance dew-point sensor

    Science.gov (United States)

    Kwon, Su-Yong; Kim, Jong-Chul; Choi, Buyng-Il

    2008-11-01

    Quartz crystal microbalance (QCM) dew-point sensors are based on frequency measurement, and so have fast response time, high sensitivity and high accuracy. Recently, we have reported that they have the very convenient attribute of being able to distinguish between supercooled dew and frost from a single scan through the resonant frequency of the quartz resonator as a function of the temperature. In addition to these advantages, by using three different types of heat sinks, we have developed a QCM dew/frost-point sensor with a very wide working temperature range (-90 °C to 15 °C). The temperature of the quartz surface can be obtained effectively by measuring the temperature of the quartz crystal holder and using temperature compensation curves (which showed a high level of repeatability and reproducibility). The measured dew/frost points showed very good agreement with reference values and were within ±0.1 °C over the whole temperature range.

  17. Accurate dew-point measurement over a wide temperature range using a quartz crystal microbalance dew-point sensor

    International Nuclear Information System (INIS)

    Kwon, Su-Yong; Kim, Jong-Chul; Choi, Buyng-Il

    2008-01-01

    Quartz crystal microbalance (QCM) dew-point sensors are based on frequency measurement, and so have fast response time, high sensitivity and high accuracy. Recently, we have reported that they have the very convenient attribute of being able to distinguish between supercooled dew and frost from a single scan through the resonant frequency of the quartz resonator as a function of the temperature. In addition to these advantages, by using three different types of heat sinks, we have developed a QCM dew/frost-point sensor with a very wide working temperature range (−90 °C to 15 °C). The temperature of the quartz surface can be obtained effectively by measuring the temperature of the quartz crystal holder and using temperature compensation curves (which showed a high level of repeatability and reproducibility). The measured dew/frost points showed very good agreement with reference values and were within ±0.1 °C over the whole temperature range

  18. Inertial sensors as measurement tools of elbow range of motion in gerontology

    Directory of Open Access Journals (Sweden)

    Sacco G

    2015-02-01

    Full Text Available G Sacco,1–3,* JM Turpin,3,4,* A Marteu,5 C Sakarovitch,6 B Teboul,2 L Boscher,4,5 P Brocker,4 P Robert,1–3 O Guerin2,3,7 1Memory Center, Claude Pompidou Institut, Department of Geriatrics, University Hospital of Nice, Nice, France; 2Centre d’Innovation et d’Usages en Santé (CIU-S, University Hospital of Nice, Cimiez Hospital, Nice, France; 3CoBTeK Cognition Behaviour Technology EA 7276, Research Center Edmond and Lily Safra, Nice Sophia-Antipolis University, Nice, France; 4Rehabilitation Unit, Department of Geriatrics, University Hospital of Nice, Cimiez Hospital, Nice, France; 5Rehabilitation Unit, Department of Neurosciences, University Hospital of Nice, L’Archet Hospital, Nice, France; 6Department of Clinical Research and Innovation, University Hospital of Nice, Cimiez Hospital, Nice, France; 7Acute Geriatrics Unit, Department of Geriatrics, University Hospital of Nice, Cimiez Hospital, Nice, France *These authors contributed equally to this work Background and purpose: Musculoskeletal system deterioration among the aging is a major reason for loss of autonomy and directly affects the quality of life of the elderly. Articular evaluation is part of physiotherapeutic assessment and helps in establishing a precise diagnosis and deciding appropriate therapy. Reference instruments are valid but not easy to use for some joints. The main goal of our study was to determine reliability and intertester reproducibility of the MP-BV, an inertial sensor (the MotionPod® [MP] combined with specific software (BioVal [BV], for elbow passive range-of-motion measurements in geriatrics. Methods: This open, monocentric, randomized study compared inertial sensor to inclinometer in patients hospitalized in an acute, post-acute, and long-term-care gerontology unit. Results: Seventy-seven patients (mean age 83.5±6.4 years, sex ratio 1.08 [male/female] were analyzed. The MP-BV was reliable for each of the three measurements (flexion, pronation, and

  19. Application of solid-phase micro extraction for the determination of pesticides in vegetable samples by gas chromatography with an electron capture detector

    International Nuclear Information System (INIS)

    Chai, Mee Kin; Tan, Guan Huat; Kumari, Asha

    2008-01-01

    A solid-phase micro extraction (SPME) method has been developed for the determination of 9 pesticides in 2 vegetables -cucumber and tomato - samples, based on direct immersion mode and subsequent desorption into the injection port of a gas chromatograph with an electron capture detector (GC-ECD). The main factors affecting the SPME process such as extraction time and temperature, desorption time and temperature, the effect of salt addition and fiber depth into the liner were studied and optimized. The analytical procedure proposed consisted of a 30 minute ultrasonic extraction of the target compounds from 1.0 g vegetable samples with 5 mL of distilled water. Then, the samples were filtered and topped up with distilled water to 10 mL. The analytes in this aqueous extract were extracted for 15 minutes with a 100 μm thickness polydimethylsiloxane SPME fiber. Relative standard deviations for triplicate analyses of samples were less than 10 %. The recoveries of the pesticides studied in cucumber and tomato ranged from 52 % to 82 % and the RSD were below 10 %. Therefore, the proposed method is applicable in the analysis of pesticides in vegetable matrices. SPME has been shown to be a simple extraction technique, which has a number of advantages such as solvent free extraction, simplicity and compatibility with the chromatographic analytical system. (author)

  20. Herbs and spices: characterization and quantitation of biologically-active markers for routine quality control by multiple headspace solid-phase microextraction combined with separative or non-separative analysis.

    Science.gov (United States)

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

    2015-01-09

    Herbs and spices are used worldwide as food flavoring, thus determination of their identity, origin, and quality is mandatory for safe human consumption. An analysis strategy based on separative (HS-SPME-GC-MS) and non-separative (HS-SPME-MS) approaches is proposed for the volatile fraction of herbs and spices, for quality control and to quantify the aromatic markers with a single analysis directly on the plant material as such. Eight-to-ten lots of each of the following herbs/spices were considered: cloves (Syzygium aromaticum (L.) Merr. & Perry), American peppertree (Schinus molle L.), black pepper and white pepper (Piper nigrum L.), rosemary (Rosmarinus officinalis L.), sage (Salvia officinalis L.) and thyme (Thymus vulgaris L.). Homogeneity, origin, and chemotypes of the investigated lots of each herb/spice were defined by fingerprinting, through statistical elaboration with principal component analysis (PCA). Characterizing aromatic markers were directly quantified on the solid matrix through multiple headspace extraction-HS-SPME (MHS-SPME). Reliable results were obtained with both separative and non-separative methods (where the latter were applicable); the two were in full agreement, RSD% ranging from 1.8 to 7.7% for eugenol in cloves, 2.2-18.4% for carvacrol+thymol in thyme, and 3.1-16.8% for thujones in sage. Copyright © 2014 Elsevier B.V. All rights reserved.

  1. Wide range neutron monitoring device

    International Nuclear Information System (INIS)

    Okido, Fumiyasu; Arita, Setsuo; Ishii, Kazuhiko; Matsumiya, Shoichi; Furusato, Ken-ichiro; Nishida, Akira.

    1994-01-01

    The present invention has a function of reliably switching measuring values between a pulse method and a Cambel method even if noise level and saturated level are fluctuated. That is, a proportional range judging means always monitors neutron flux measuring values in a start-up region and neutron flux measuring values in an intermediate power region, so that the proportional range is detected depending on whether the difference or a variation coefficient of both of the measured values is constant or not. A switching value determining means determines a switching value by the result of judgement of the proportional range judging means. A selection/output means selects and outputs measuring signals at a neutron flux level in the start-up region or the intermediate power region by the output of the switching value determining means. With such procedures, since the measuring value is switched after confirming that arrival at the proportional range where the difference or a variation coefficient of the measured value between the pulse processing method and the measured value by the Cambel method is constant, an accurate neutron flux level containing neither noise level nor saturated level can be outputted. (I.S.)

  2. 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.

  3. 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

  4. Total photoabsorption cross section on nuclei measured in energy range 0.5-2.6 GeV

    International Nuclear Information System (INIS)

    Mirazita, M.

    1998-03-01

    The total photoabsorption cross section on several nuclei has been measured in the energy range 0.5 - 2.6 GeV. Nuclear data show a significant reduction of the absorption strength with respect to the free nucleon case suggesting a shadowing effect at low energies

  5. Validation of a photography-based goniometry method for measuring joint range of motion.

    Science.gov (United States)

    Blonna, Davide; Zarkadas, Peter C; Fitzsimmons, James S; O'Driscoll, Shawn W

    2012-01-01

    A critical component of evaluating the outcomes after surgery to restore lost elbow motion is the range of motion (ROM) of the elbow. This study examined if digital photography-based goniometry is as accurate and reliable as clinical goniometry for measuring elbow ROM. Instrument validity and reliability for photography-based goniometry were evaluated for a consecutive series of 50 elbow contractures by 4 observers with different levels of elbow experience. Goniometric ROM measurements were taken with the elbows in full extension and full flexion directly in the clinic (once) and from digital photographs (twice in a blinded random manner). Instrument validity for photography-based goniometry was extremely high (intraclass correlation coefficient: extension = 0.98, flexion = 0.96). For extension and flexion measurements by the expert surgeon, systematic error was negligible (0° and 1°, respectively). Limits of agreement were 7° (95% confidence interval [CI], 5° to 9°) and -7° (95% CI, -5° to -9°) for extension and 8° (95% CI, 6° to 10°) and -7° (95% CI, -5° to -9°) for flexion. Interobserver reliability for photography-based goniometry was better than that for clinical goniometry. The least experienced observer's photographic goniometry measurements were closer to the reference measurements than the clinical goniometry measurements. Photography-based goniometry is accurate and reliable for measuring elbow ROM. The photography-based method relied less on observer expertise than clinical goniometry. This validates an objective measure of patient outcome without requiring doctor-patient contact at a tertiary care center, where most contracture surgeries are done. Copyright © 2012 Journal of Shoulder and Elbow Surgery Board of Trustees. Published by Mosby, Inc. All rights reserved.

  6. Measuring Relativistic effects in the field of the Earth with Laser Ranged Satellites and the LARASE research program

    Science.gov (United States)

    Lucchesi, David; Anselmo, Luciano; Bassan, Massimo; Magnafico, Carmelo; Pardini, Carmen; Peron, Roberto; Pucacco, Giuseppe; Stanga, Ruggero; Visco, Massimo

    2017-04-01

    The main goal of the LARASE (LAser RAnged Satellites Experiment) research program is to obtain refined tests of Einstein's theory of General Relativity (GR) by means of very precise measurements of the round-trip time among a number of ground stations of the International Laser Ranging Service (ILRS) network and a set of geodetic satellites. These measurements are guaranteed by means of the powerful and precise Satellite Laser Ranging (SLR) technique. In particular, a big effort of LARASE is dedicated to improve the dynamical models of the LAGEOS, LAGEOS II and LARES satellites, with the objective to obtain a more precise and accurate determination of their orbit. These activities contribute to reach a final error budget that should be robust and reliable in the evaluation of the main systematic errors sources that come to play a major role in masking the relativistic precession on the orbit of these laser-ranged satellites. These error sources may be of gravitational and non-gravitational origin. It is important to stress that a more accurate and precise orbit determination, based on more reliable dynamical models, represents a fundamental prerequisite in order to reach a sub-mm precision in the root-mean-square of the SLR range residuals and, consequently, to gather benefits in the fields of geophysics and space geodesy, such as stations coordinates knowledge, geocenter determination and the realization of the Earth's reference frame. The results reached over the last year will be presented in terms of the improvements achieved in the dynamical model, in the orbit determination and, finally, in the measurement of the relativistic precessions that act on the orbit of the satellites considered.

  7. Linearity improvement on wide-range log signal of neutron measurement system for HANARO

    International Nuclear Information System (INIS)

    Kim, Young-Ki; Tuetken, Jeffrey S.

    1998-01-01

    This paper discusses engineering activities for improving the linearity characteristics of the Log Power signal from the neutron measurement system for HANARO. This neutron measurement system uses a fission chamber based detector which covers 10.3 decade-wide range from 10 -8 % full power(FP) up to 200%FP, The Log Power signal is designed to control the reactor at low power levels where most of the reactor physics tests are carried out. Therefore, the linearity characteristics of the Log Power signal is the major factor for accurate reactor power control. During the commissioning of the neutron measurement system, it was found that the linearity characteristics of the Log Power signal, especially near 10 -2 %FP, were not accurate enough for controlling the reactor during physics testing. Analysis of the system linearity data directly measured with reactor operating determined that the system was not operating per the design characteristics established from previous installations. The linearity data, which were taken as the reactor was increased in power, were sent to manufacturer's engineering group and a follow-up measures based on the analysis were then fed back to the field. Through step by step trouble-shooting activities, which included minor circuit modifications and alignment procedure changes, the linearity characteristics have been successfully improved and now exceed minimum performance requirements. This paper discusses the trouble-shooting techniques applied, the changes in the linearity characteristics, special circumstances in the HANARO application and the final resolution. (author)

  8. In matrix derivatization of trichloroethylene metabolites in human plasma with methyl chloroformate and their determination by solid-phase microextraction-gas chromatography-electron capture detector.

    Science.gov (United States)

    Mudiam, Mohana Krishna Reddy; Jain, Rajeev; Varshney, Meenu; Ch, Ratnasekhar; Chauhan, Abhishek; Goyal, Sudhir Kumar; Khan, Haider A; Murthy, R C

    2013-04-15

    Trichloroethylene (TCE) is a common industrial chemical that has been widely used as metal degreaser and for many industrial purposes. In humans, TCE is metabolized into dichloroacetic acid (DCA), trichloroacetic acid (TCA) and trichloroethanol (TCOH). A simple and rapid method has been developed for the quantitative determination of TCE metabolites. The procedure involves the in situ derivatization of TCE metabolites with methyl chloroformate (MCF) directly in diluted plasma samples followed by extraction and analysis with solid-phase microextraction (SPME) coupled to gas chromatography-electron capture detector (GC-ECD). Factors which can influence the efficiency of derivatization such as amount of MCF and pyridine (PYR), ratio of water/methanol were optimized. The factors which can affect the extraction efficiencies of SPME were screened using 2(7-4) Placket-Burman Design (PBD). A central composite design (CCD) was then applied to further optimize the most significant factors for optimum SPME extraction. The optimum factors for the SPME extraction were found to be 562.5mg of NaCl, pH at 1 and an extraction time of 22 min. Recoveries and detection limits of all three analytes in plasma were found to be in the range of 92.69-97.55% and 0.036-0.068 μg mL(-1) of plasma, respectively. The correlation coefficients were found to be in the range of 0.990-0.995. The intra- and inter-day precisions for TCE metabolites were found to be in the range of 2.37-4.81% and 5.13-7.61%, respectively. The major advantage of this method is that MCF derivatization allows conversion of TCE metabolites into their methyl esters in very short time (≤30 s) at room temperature directly in the plasma samples, thus makes it a solventless analysis. The method developed was successfully applied to the plasma samples of humans exposed to TCE. Copyright © 2013 Elsevier B.V. All rights reserved.

  9. Ranging behavior relates to welfare indicators pre- and post-range access in commercial free-range broilers.

    Science.gov (United States)

    Taylor, Peta S; Hemsworth, Paul H; Groves, Peter J; Gebhardt-Henrich, Sabine G; Rault, Jean-Loup

    2018-06-01

    Little is known about the effect of accessing an outdoor range on chicken welfare. We tracked individual ranging behavior of 538 mixed-sex Ross 308 chickens on a commercial farm across 4 flocks in winter and summer. Before range access, at 17 to 19 d of age, and post-range access, at 30 to 33 and 42 to 46 d of age in winter and summer flocks respectively, welfare indicators were measured on chickens (pre-range: winter N = 292; summer N = 280; post-range: winter N = 131; summer N = 140), including weight, gait score, dermatitis and plumage condition. Post-ranging autopsies were performed (winter: N = 170; summer: N = 60) to assess breast burn, leg health, and ascites. Fewer chickens accessed the range in winter flocks (32.5%) than summer flocks (82.1%). Few relationships between welfare and ranging were identified in winter, likely due to minimal ranging and the earlier age of post-ranging data collection compared to summer flocks. In summer flocks prior to range access, chickens that accessed the range weighed 4.9% less (P = 0.03) than chickens that did not access the range. Pre-ranging weight, gait score, and overall plumage cover predicted the amount of range use by ranging chickens in summer flocks (P ranging behavior. In summer flocks post-range access, ranging chickens weighed 12.8% less than non-ranging chickens (P range visits were associated with lower weight (P range was associated with lower weight (P range in summer is partly related to changes in broiler chicken welfare. Further investigations are required to determine causation.

  10. Usefulness of a PARAFAC decomposition in the fiber selection procedure to determine chlorophenols by means SPME-GC-MS.

    Science.gov (United States)

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

    2012-05-01

    In this work, a procedure based on solid-phase microextraction and gas chromatography coupled with mass spectrometry is proposed to determine chlorophenols in water without derivatization. The following chlorophenols are studied: 2,4-dichlorophenol; 2,4,6-trichlorophenol; 2,3,4,6-tetrachlorophenol and pentachlorophenol. Three kinds of SPME fibers, polyacrylate, polydimethylsiloxane, and polydimethylsiloxane/divinylbenzene are compared to identify the most suitable one for the extraction process on the basis of two criteria: (a) to select the equilibrium time studying the kinetics of the extraction, and (b) to obtain the best values of the figures of merit. In both cases, a three-way PARAllel FACtor analysis decomposition is used. For the first step, the three-way experimental data are arranged as follows: if I extraction times are considered, the tensor of data, X, of dimensions I × J × K is generated by concatenating the I matrices formed by the abundances of the J m/z ions recorded in K elution times around the retention time for each chlorophenol. The second-order property of PARAFAC (or PARAFAC2) assesses the unequivocal identification of each chlorophenol, as consequence, the loadings in the first mode estimated by the PARAFAC decomposition are the kinetic profile. For the second step, a calibration based on a PARAFAC decomposition is used for each fiber. The best figures of merit were obtained with PDMS/DVB fiber. The values of decision limit, CCα, achieved are between 0.29 and 0.67 μg L(-1) for the four chlorophenols. The accuracy (trueness and precision) of the procedure was assessed. This procedure has been applied to river water samples.

  11. Density Measurements of Waste Cooking Oil Biodiesel and Diesel Blends Over Extended Pressure and Temperature Ranges

    Directory of Open Access Journals (Sweden)

    Thanh Xuan NguyenThi

    2018-05-01

    Full Text Available Density and compressibility are primordial parameters for the optimization of diesel engine operation. With this objective, these properties were reported for waste cooking oil biodiesel and its blends (5% and 10% by volume mixed with diesel. The density measurements were performed over expanded ranges of pressure (0.1 to 140 MPa and temperature (293.15 to 353.15 K compatible with engine applications. The isothermal compressibility was estimated within the same experimental range by density differentiation. The Fatty Acid Methyl Esters (FAMEs profile of the biodiesel was determined using a Gas Chromatography–Mass Spectrometry (GC-MS technique. The storage stability of the biodiesel was assessed in terms of the reproducibility of the measured properties. The transferability of this biodiesel fuel was discussed on the basis of the standards specifications that support their use in fuel engines. Additionally, this original set of data represents meaningful information to develop new approaches or to evaluate the predictive capability of models previously developed.

  12. Determination of Selected Aromas in Marquette and Frontenac Wine Using Headspace-SPME Coupled with GC-MS and Simultaneous Olfactometry

    Directory of Open Access Journals (Sweden)

    Somchai Rice

    2018-03-01

    Full Text Available Understanding the aroma profile of wines made from cold climate grapes is needed to help winemakers produce quality aromatic wines. The current study aimed to add to the very limited knowledge of aroma-imparting compounds in wines made from the lesser-known Frontenac and Marquette cultivars. Headspace solid-phase microextraction (SPME and gas chromatography-mass spectrometry (GC-MS with simultaneous olfactometry was used to identify and quantify selected, aroma-imparting volatile organic compounds (VOC in wines made from grapes harvested at two sugar levels (22° Brix and 24° Brix. Aroma-imparting compounds were determined by aroma dilution analysis (ADA. Odor activity values (OAV were also used to aid the selection of aroma-imparting compounds. Principal component analysis and hierarchical clustering analysis indicated that VOCs in wines produced from both sugar levels of Marquette grapes are similar to each other, and more similar to wines produced from Frontenac grapes harvested at 24° Brix. Selected key aroma compounds in Frontenac and Marquette wines were ethyl hexanoate, ethyl isobutyrate, ethyl octanoate, and ethyl butyrate. OAVs >1000 were reported for three aroma compounds that impart fruity aromas to the wines. This study provides evidence that aroma profiles in Frontenac wines can be influenced by timing of harvesting the berries at different Brix. Future research should focus on whether this is because of berry development or accumulation of aroma precursors and sugar due to late summer dehydration. Simultaneous chemical and sensory analyses can be useful for the understanding development of aroma profile perceptions for wines produced from cold-climate grapes.

  13. Determination of furfural and hydroxymethylfurfural from baby formula using headspace solid phase microextraction based on nanostructured polypyrrole fiber coupled with ion mobility spectrometry.

    Science.gov (United States)

    Kamalabadi, Mahdie; Ghaemi, Elham; Mohammadi, Abdorreza; Alizadeh, Naader

    2015-08-15

    Furfural (Fu) and hydroxymethylfurfural (HMFu) are extracted using a dodecylbenzenesulfonate-doped polypyrrole coating as a fiber for headspace solid phase microextraction (HS-SPME) method in baby formula samples and detected using ion mobility spectrometry (IMS). Sample pH, salt effect, extraction time and temperature were investigated and optimized as effective parameters in HS-SPME. The calibration curves were linear in the range of 20-300 ng g(-1) (R(2)>0.99). Limits of detection for Fu and HMFu were 6 ng g(-1) and 5 ng g(-1), respectively. The RSD% of Fu and HMFu for five analyses was 4.4 and 4.9, respectively. The proposed method was successfully applied to determine of Fu and HMFu in the different baby formula samples with satisfactory result. The results were in agreement with those obtained using HPLC analysis. The HS-SPME-IMS is precise, selective and sensitive analytical method for determination of Fu and HMFu in baby formula samples, without any derivatization process. Copyright © 2015 Elsevier Ltd. All rights reserved.

  14. Comparative study of the sol-gel based solid phase microextraction fibers in extraction of naphthalene, fluorene, anthracene and phenanthrene from saffron samples extractants

    International Nuclear Information System (INIS)

    Sarafraz-Yazdi, A.; Ghaemi, F.; Amiri, A.

    2012-01-01

    We are introducing a method for the determination of some polycyclic aromatic hydrocarbons in aqueous saffron sample by direct immersion solid phase microextraction (SPME) and gas chromatography. A sol-gel technique is used for the preparation of the SPME fibers. Three kinds of sol-gel coatings on the fibers were tested and compared. They are composed of poly(dimethyl siloxane) (PDMS), poly(ethylene glycol) (PEG), and a poly(ethylene glycol) modified with multi-walled carbon nanotubes (PEG/CNTs). The effects of fiber coating, desorption time, desorption temperature, extraction time, stirring speed and salting effect were optimized. Under the optimal conditions, the detection limits (at S/N = 3) are 7-50, 5-50, and 1-10 pg mL -1 , respectively, for SPME fibers made from PDMS, PEG and PEG/CNTs. The relative standard deviations for one type of fiber are from 2.1% to 9.6% for all fibers (at n = 5), and in the range from 1.9% to 9.8% from batch to batch (for n = 3). (author)

  15. Exploring the range of energy savings likely from energy efficiency retrofit measures in Ireland's residential sector

    International Nuclear Information System (INIS)

    Dineen, D.; Ó Gallachóir, B.P.

    2017-01-01

    This paper estimates the potential energy savings in the Irish residential sector by 2020 due to the introduction of an ambitious retrofit programme. We estimate the technical energy savings potential of retrofit measures targeting energy efficiency of the space and water heating end uses of the 2011 stock of residential dwellings between 2012 and 2020. We build eight separate scenarios, varying the number of dwellings retrofitted and the depth of retrofit carried out in order to investigate the range of energy savings possible. In 2020 the estimated technical savings potential lies in the range from 1713 GWh to 10,817 GWh, but is more likely to fall within the lower end of this range, i.e. between 1700 and 4360 GWh. When rebound effects are taken into account this reduces further to 1100 GWh and 2800 GWh per annum. The purpose of this paper was to test the robustness of the NEEAP target savings for residential retrofit, i.e. 3000 GWh by 2020. We conclude that this target is technically feasible but very challenging and unlikely to be achieved based on progress to date. It will require a significant shift towards deeper retrofit measures compared to what has been achieved by previous schemes. - Highlights: • Paper estimates range of energy savings likely from Irish residential retrofit. • Achieving NEEAP target savings of 3000 GWh by 2020 is feasible but very challenging. • Likely savings of 1100–2800 GWh per annum in 2020, including rebound. • NEEAP target unlikely to be achieved based on current trends.

  16. Determination of Trichloroethylene in Water by Liquid–Liquid Microextraction Assisted Solid Phase Microextraction

    Directory of Open Access Journals (Sweden)

    Mengliang Zhang

    2015-02-01

    Full Text Available A method for the determination of trichloroethylene (TCE in water using portable gas chromatography/mass spectrometry (GC/MS was developed. A novel sample preparation method, liquid–liquid microextraction assisted solid phase microextraction (LLME–SPME, is introduced. In this method, 20 µL of hexane was added to 10 mL of TCE contaminated aqueous samples to assist headspace SPME. The extraction efficiency of SPME was significantly improved with the addition of minute amounts of organic solvents (i.e., 20 µL hexane. The absolute recoveries of TCE at different concentrations were increased from 11%–17% for the samples extracted by SPME to 29%–41% for the samples extracted by LLME–SPME. The method was demonstrated to be linear from 10 to 1000 ng mL−1 for TCE in water. The improvements on extraction efficiencies were also observed for toluene and 1, 2, 4-trichlorobenzene in water by using LLME–SPME method. The LLME–SPME method was optimized by using response surface modeling (RSM.

  17. Small-Chamber Measurements of Chemical-Specific Emission Factors for Drywall

    Energy Technology Data Exchange (ETDEWEB)

    Maddalena, Randy; Russell, Marion; Apte, Michael G.

    2010-06-01

    Imported drywall installed in U.S. homes is suspected of being a source of odorous and potentially corrosive indoor pollutants. To support an investigation of those building materials by the Consumer Products Safety Commission (CPSC), Lawrence Berkeley National Laboratory (LBNL) measured chemical-specific emission factors for 30 samples of drywall materials. Emission factors are reported for 75 chemicals and 30 different drywall samples encompassing both domestic and imported stock and incorporating natural, synthetic, or mixed gypsum core material. CPSC supplied all drywall materials. First the drywall samples were isolated and conditioned in dedicated chambers, then they were transferred to small chambers where emission testing was performed. Four sampling and analysis methods were utilized to assess (1) volatile organic compounds, (2) low molecular weight carbonyls, (3) volatile sulfur compounds, and (4) reactive sulfur gases. LBNL developed a new method that combines the use of solid phase microextraction (SPME) with small emission chambers to measure the reactive sulfur gases, then extended that technique to measure the full suite of volatile sulfur compounds. The testing procedure and analysis methods are described in detail herein. Emission factors were measured under a single set of controlled environmental conditions. The results are compared graphically for each method and in detailed tables for use in estimating indoor exposure concentrations.

  18. Physical measurements for ion range verification in charged particle therapy

    International Nuclear Information System (INIS)

    Testa, M.

    2010-10-01

    This PhD thesis reports on the experimental investigation of the prompt photons created during the fragmentation of the carbon beam used in particle therapy. Two series of experiments have been performed at the GANIL and GSI facilities with 95 MeV/u and 305 MeV/u 12 C 6+ ion beams stopped in PMMA and water phantoms. In both experiments a clear correlation was obtained between the C-ion range and the prompt photon profile. A major issue of these measurements is the discrimination between the prompt photon signal (which is correlated with the ion path) and a vast neutron background uncorrelated with the Bragg-Peak position. Two techniques are employed to allow for this photon-neutron discrimination: the time-of-flight (TOF) and the pulse-shape-discrimination (PSD). The TOF technique allowed demonstrating the correlation of the prompt photon production and the primary ion path while the PSD technique brought great insights to better understand the photon and neutron contribution in TOF spectra. In this work we demonstrated that a collimated set-up detecting prompt photons by means of TOF measurements, could allow real-time control of the longitudinal position of the Bragg-peak under clinical conditions. In the second part of the PhD thesis a simulation study was performed with Geant4 Monte Carlo code to assess the influence of the main design parameters on the efficiency and spatial resolution achievable with a multidetector and multi-collimated Prompt Gamma Camera. Several geometrical configurations for both collimators and stack of detectors have been systematically studied and the considerations on the main design constraints are reported. (author)

  19. Measurements on the extended range of the wake

    International Nuclear Information System (INIS)

    Kumbartzki, G.J.; Kroesing, G; Neuburger, H.

    1981-01-01

    The Coulomb explosion of H 2 + -ions at 28 MeV is used to probe the wake over a range of about 400 A in Al. Preliminary results give food agreement with the wavelength prediction of the simple plasma oscillation wake model. (author)

  20. Relationship between welfare and individual ranging behaviour in commercial free-range laying hens.

    Science.gov (United States)

    Larsen, H; Hemsworth, P H; Cronin, G M; Gebhardt-Henrich, S G; Smith, C L; Rault, J-L

    2018-01-24

    Laying hens housed in free-range systems have access to an outdoor range, and individual hens within a flock differ in their ranging behaviour. Whether there is a link between ranging and laying hen welfare remains unclear. We analysed the relationships between ranging by individual hens on a commercial free-range layer farm and behavioural, physiological and health measures of animal welfare. We hypothesised that hens that access the range more will be (1) less fearful in general and in response to novelty and humans, (2) have better health in terms of physical body condition and (3) have a reduced physiological stress response to behavioural tests of fear and health assessments than hens that use the range less. Using radio frequency identification tracking across two flocks, we recorded individual hens' frequency, duration and consistency of ranging. We also assessed how far hens ventured into the range based on three zones: 0 to 2.4, 2.4 to 11.4 or >11.4 m from the shed. We assessed hen welfare using a variety of measures including: tonic immobility, open field, novel object, human approach, and human avoidance (HAV) behavioural tests; stress-induced plasma corticosterone response and faecal glucocorticoid metabolites; live weight, comb colour, and beak, plumage, footpad, and keel bone condition. Range use was positively correlated with plasma corticosterone response, faecal glucocorticoid metabolites, and greater flight distance during HAV. Hens that used the range more, moved towards rather than away from the novel object more often than hens that ranged less. Distance ranged from the shed was significantly associated with comb colour and beak condition, in that hens with darker combs and more intact beaks ranged further. Overall the findings suggest that there is no strong link between outdoor range usage and laying hen welfare. Alternatively, it may be that hens that differed in their ranging behaviour showed few differences in measures of welfare because

  1. Measuring sensitivity in pharmacoeconomic studies. Refining point sensitivity and range sensitivity by incorporating probability distributions.

    Science.gov (United States)

    Nuijten, M J

    1999-07-01

    The aim of the present study is to describe a refinement of a previously presented method, based on the concept of point sensitivity, to deal with uncertainty in economic studies. The original method was refined by the incorporation of probability distributions which allow a more accurate assessment of the level of uncertainty in the model. In addition, a bootstrap method was used to create a probability distribution for a fixed input variable based on a limited number of data points. The original method was limited in that the sensitivity measurement was based on a uniform distribution of the variables and that the overall sensitivity measure was based on a subjectively chosen range which excludes the impact of values outside the range on the overall sensitivity. The concepts of the refined method were illustrated using a Markov model of depression. The application of the refined method substantially changed the ranking of the most sensitive variables compared with the original method. The response rate became the most sensitive variable instead of the 'per diem' for hospitalisation. The refinement of the original method yields sensitivity outcomes, which greater reflect the real uncertainty in economic studies.

  2. An adaptive scheme for robot localization and mapping with dynamically configurable inter-beacon range measurements.

    Science.gov (United States)

    Torres-González, Arturo; Martinez-de Dios, Jose Ramiro; Ollero, Anibal

    2014-04-25

    This work is motivated by robot-sensor network cooperation techniques where sensor nodes (beacons) are used as landmarks for range-only (RO) simultaneous localization and mapping (SLAM). This paper presents a RO-SLAM scheme that actuates over the measurement gathering process using mechanisms that dynamically modify the rate and variety of measurements that are integrated in the SLAM filter. It includes a measurement gathering module that can be configured to collect direct robot-beacon and inter-beacon measurements with different inter-beacon depth levels and at different rates. It also includes a supervision module that monitors the SLAM performance and dynamically selects the measurement gathering configuration balancing SLAM accuracy and resource consumption. The proposed scheme has been applied to an extended Kalman filter SLAM with auxiliary particle filters for beacon initialization (PF-EKF SLAM) and validated with experiments performed in the CONET Integrated Testbed. It achieved lower map and robot errors (34% and 14%, respectively) than traditional methods with a lower computational burden (16%) and similar beacon energy consumption.

  3. Precise Measurement of the $\\bar{p}p$ Total Cross-Section in the ISR Energy Range

    CERN Multimedia

    2002-01-01

    The major aim of this experiment is the precise measurement of the antiproton-proton total cross-section in the ISR energy range, using the total-rate method. The proton-proton total cross-section is remeasured with the same method and the same apparatus, and a precision of 0.5\\% is expected for both cross-sections. The total-rate method consists in the simultaneous measurement of the total interaction rate and the ISR luminosity. This is done with a set of scintillation-counter hodoscopes covering over 99.99\\% of the solid angle, which are sensitive to over 95\\% of all interactions. In addition to these detectors, small-angle drift-tube hodoscopes are used to measure the differential elastic cross-section as a function of the momentum transfert t. The total cross-section can be measured independently by extrapolating this differential cross-section to the forward direction and invoking the optical theorem. A study of the general features of charged-particle production is performed using finely divided scinti...

  4. Auroral radar measurements at 16-cm wavelength with high range and time resolution

    International Nuclear Information System (INIS)

    Schlegel, K.; Turunen, T.; Moorcroft, D.R.

    1990-01-01

    Auroral radar measurements performed with the EISCAT facility are presented. Backscatter cross sections of the irregularities produced by the two-stream (Farley-Buneman) or gradient drift plasma instabilities have been recorded with a range separation of 1.5 km, corresponding to a spacing of successive values in height of about 0.4 km. The apparent height profiles of the backscatter have a width of about 5-6 km and occur between 95 and 112 km altitude, with a mean at 104 km. Very often, fast motions of the backscatter layers are observed which can be explained as fast moving ionospheric structures controlled by magnetospheric convection. The maximal time resolution of the measurements is 12.5 ms. The statistics of the backscatter amplitudes at this time resolution is close to a Rice distribution with a Rice parameter a ∼ 3.7. The observed backscatter spectra do not change significantly in shape when the integration time is reduced from 5 s to 100 ms

  5. Gamma compensated pulsed ionization chamber wide range neutron/reactor power measurement system

    International Nuclear Information System (INIS)

    Ellis, W.H.

    1975-01-01

    An improved method and system of pulsed mode operation of ionization chambers is described in which a single sensor system with gamma compensation is provided by sampling, squaring, automatic gate selector, and differential amplifier circuit means, employed in relation to chambers sensitized to neutron plus gamma and gamma only to subtract out the gamma component, wherein squaring functions circuits, a supplemental high performance pulse rate system, and operational and display mode selection and sampling gate circuits are utilized to provide automatic wide range linear measurement capability for neutron flux and reactor power. Neon is employed as an additive in the ionization chambers to provide independence of ionized gas kinetics temperature effects, and the pulsed mode of operation provide independence of high temperature insulator leakage effects. (auth)

  6. Airborne Measurements of CO2 Column Concentration and Range Using a Pulsed Direct-Detection IPDA Lidar

    Science.gov (United States)

    Abshire, James B.; Ramanathan, Anand; Riris, Haris; Mao, Jianping; Allan, Graham R.; Hasselbrack, William E.; Weaver, Clark J.; Browell, Edward V.

    2013-01-01

    We have previously demonstrated a pulsed direct detection IPDA lidar to measure range and the column concentration of atmospheric CO2. The lidar measures the atmospheric backscatter profiles and samples the shape of the 1,572.33 nm CO2 absorption line. We participated in the ASCENDS science flights on the NASA DC-8 aircraft during August 2011 and report here lidar measurements made on four flights over a variety of surface and cloud conditions near the US. These included over a stratus cloud deck over the Pacific Ocean, to a dry lake bed surrounded by mountains in Nevada, to a desert area with a coal-fired power plant, and from the Rocky Mountains to Iowa, with segments with both cumulus and cirrus clouds. Most flights were to altitudes >12 km and had 5-6 altitude steps. Analyses show the retrievals of lidar range, CO2 column absorption, and CO2 mixing ratio worked well when measuring over topography with rapidly changing height and reflectivity, through thin clouds, between cumulus clouds, and to stratus cloud tops. The retrievals shows the decrease in column CO2 due to growing vegetation when flying over Iowa cropland as well as a sudden increase in CO2 concentration near a coal-fired power plant. For regions where the CO2 concentration was relatively constant, the measured CO2 absorption lineshape (averaged for 50 s) matched the predicted shapes to better than 1% RMS error. For 10 s averaging, the scatter in the retrievals was typically 2-3 ppm and was limited by the received signal photon count. Retrievals were made using atmospheric parameters from both an atmospheric model and from in situ temperature and pressure from the aircraft. The retrievals had no free parameters and did not use empirical adjustments, and >70% of the measurements passed screening and were used in analysis. The differences between the lidar-measured retrievals and in situ measured average CO2 column concentrations were 6 km.

  7. Absolute Hugoniot measurements for CH foams in the 2-9 Mbar range

    Science.gov (United States)

    Aglitskiy, Y.; Velikovich, A. L.; Karasik, M.; Schmitt, A. J.; Serlin, V.; Weaver, J. L.; Oh, J.; Obenschain, S. P.; Cochrane, K. R.

    2018-03-01

    Absolute Hugoniot measurements for empty plastic foams at ˜10% of solid polystyrene density and supporting rad-hydro simulation results are reported. Planar foam slabs, ˜400 μm thick and ˜500 μm wide, some of which were covered with a 10 μm solid plastic ablator, were directly driven by 4 ns long Nike krypton-fluoride 248 nm wavelength laser pulses that produced strong shock waves in the foam. The shock and mass velocities in our experiments were up to 104 km/s and 84 km/s, respectively, and the shock pressures up to ˜9 Mbar. The motion of the shock and ablation fronts was recorded using side-on monochromatic x-ray imaging radiography. The steadiness of the observed shock and ablation fronts within ˜1% has been verified. The Hugoniot data inferred from our velocity measurements agree with the predictions of the SESAME and CALEOS equation-of-state models near the highest pressure ˜9 Mbar and density compression ratio ˜5. In the lower pressure range 2-5 Mbar, a lower shock density compression is observed than that predicted by the models. Possible causes for this discrepancy are discussed.

  8. Electrophoretic deposition of graphene oxide onto carbon fibers for in-tube solid-phase microextraction.

    Science.gov (United States)

    Feng, Juanjuan; Wang, Xiuqin; Tian, Yu; Bu, Yanan; Luo, Chuannan; Sun, Min

    2017-09-29

    Carbon fibers (CFs) were functionalized with graphene oxide (GO) by an electrophoretic deposition (EPD) method for in-tube solid-phase microextraction (SPME). GO-CFs were filled into a poly(ether ether ketone) (PEEK) tube to obtain a fibers-in-tube SPME device, which was connected with high performance liquid chromatography (HPLC) equipment to build online SPME-HPLC system. Compared with CFs, GO-CFs presented obviously better extraction performance, due to excellent adsorption property and large surface area of GO. Using ten polycyclic aromatic hydrocarbons (PAHs) as model analytes, the important extraction conditions were optimized, such as sample flow rate, extraction time, organic solvent content and desorption time. An online analysis method was established with wide linear range (0.01-50μgL -1 ) and low detection limits (0.001-0.004μgL -1 ). Good sensitivity resulted from high enrichment factors (1133-3840) of GO-CFs in-tube device towards PAHs. The analysis method was used to online determination of PAHs in wastewater samples. Some target analytes were detected and relative recoveries were in the range of 90.2-112%. It is obvious that the proposed GO-CFs in-tube device was an efficient extraction device, and EPD could be used to develop nanomaterials functionalized sorbents for sample preparation. Copyright © 2017 Elsevier B.V. All rights reserved.

  9. Metal-organic aerogel as a coating for solid-phase microextraction

    Energy Technology Data Exchange (ETDEWEB)

    Saraji, Mohammad, E-mail: saraji@cc.iut.ac.ir; Shahvar, Ali

    2017-06-22

    An iron-based metal-organic aerogel was synthesized using metal-organic framework nanoparticles and applied as a fiber coating for solid-phase microextraction (SPME). Chemical, thermal and morphological characteristics of the material were investigated. Headspace SPME followed by gas chromatography-electron capture detection was used for the determination of chlorobenzenes in the environmental samples. The key experimental factors affecting the extraction efficiency of the analytes, such as ionic strength, extraction and desorption temperature, and extraction time were investigated and optimized. The applicability of the coating for the extraction of chlorobenzenes from the environmental samples including river and tap water, sludge, and coastal soil was evaluated. The detection limits were in the range of 0.1–60 ng L{sup −1}. The relative standard deviations were between 2.0 and 5.0%. The extraction recovery of the analytes was in the range of 88–100%. Compared to the commercial PDMS fiber, the present fiber showed better extraction efficiency. - Highlights: • Metal-organic aerogel was synthesized and used as a novel fiber coating for SPME. • The new coating material showed high surface area and good thermal stability. • GC-ECD was used for determination of chlorobenzenes in environmental samples. • The method showed fast extraction and better efficiency than PDMS commercial fiber.

  10. Graphene-supported zinc oxide solid-phase microextraction coating with enhanced selectivity and sensitivity for the determination of sulfur volatiles in Allium species.

    Science.gov (United States)

    Zhang, Suling; Du, Zhuo; Li, Gongke

    2012-10-19

    A graphene-supported zinc oxide (ZnO) solid-phase microextraction (SPME) fiber was prepared via a sol-gel approach. Graphite oxide (GO), with rich oxygen-containing groups, was selected as the starting material to anchor ZnO on its nucleation center. After being deoxidized by hydrazine, the Zn(OH)2/GO coating was dehydrated at high temperature to give the ZnO/graphene coating. Sol-gel technology could efficiently incorporate ZnO/graphene composites into the sol-gel network and provided strong chemical bonding between sol-gel polymeric SPME coating and silica fiber surface, which enhanced the durability of the fiber and allowed more than 200 replicate extractions. Results indicated that pure ZnO coated fiber did not show adsorption selectivity toward sulfur compounds, which might because the ZnO nanoparticles were enwrapped in the sol-gel network, and the strong coordination action between Zn ion and S ion was therefore blocked. The incorporation of graphene into ZnO based sol-gel network greatly enlarged the BET surface area from 1.2 m2/g to 169.4 m2/g and further increased the adsorption sites. Combining the superior properties of extraordinary surface area of graphene and the strong coordination action of ZnO to sulfur compounds, the ZnO/graphene SPME fiber showed much higher adsorption affinity to 1-octanethiol (enrichment factor, EF, 1087) than other aliphatic compounds without sulfur-containing groups (EFsPDMS) and polydimethylsiloxane/divinylbenzene (PDMS/DVB) SPME fibers. Several most abundant sulfur volatiles in Chinese chive and garlic sprout were analyzed using the ZnO/graphene SPME fiber in combination with gas chromatography-mass spectrometry (GC-MS). Their limits of detection were 0.1-0.7 μg/L. The relative standard deviation (RSD) using one fiber ranged from 3.6% to 9.1%. The fiber-to-fiber reproducibility for three parallel prepared fibers was 4.8-10.8%. The contents were in the range of 1.0-46.4 μg/g with recoveries of 80.1-91.6% for four main

  11. Absolute distance measurement with extension of nonambiguity range using the frequency comb of a femtosecond laser

    Science.gov (United States)

    Jang, Yoon-Soo; Lee, Keunwoo; Han, Seongheum; Lee, Joohyung; Kim, Young-Jin; Kim, Seung-Woo

    2014-12-01

    We revisit the method of synthetic wavelength interferometry (SWI) for absolute measurement of long distances using the radio-frequency harmonics of the pulse repetition rate of a mode-locked femtosecond laser. Our intention here is to extend the nonambiguity range (NAR) of the SWI method using a coarse virtual wavelength synthesized by shifting the pulse repetition rate. The proposed concept of NAR extension is experimentally verified by measuring a ˜13-m distance with repeatability of 9.5 μm (root-mean-square). The measurement precision is estimated to be 31.2 μm in comparison with an incremental He-Ne laser interferometer. This extended SWI method is found to be well suited for long-distance measurements demanded in the fields of large-scale precision engineering, geodetic survey, and future space missions.

  12. Applications of compound-specific carbon isotope ratios in organic contaminant studies

    International Nuclear Information System (INIS)

    Aravena, R.; Hunkeler, D.; Bloom, Y.; Frape, S.K.; Butler, B.; Edwards, E.; Cox, E.

    1999-01-01

    In this paper results are presented on the application of compound-specific isotope ratios measurements to assess biodegradation of chlorinated solvents, in particularly on microbial dechlorination of tetrachloroethene (PCE) and trichloroethene (TCE). Analytical aspects and isotope data from laboratory and field studies are discussed. The analytical tests showed that both headspace and SPME techniques provide accurate δ 13 C values with a similar precision for a wide range of chlorinated solvents. However, the SPME method is generally more sensitive. The microcosm experiments show that a significant isotopic fractionation occurs during dechlorination of PCE and TCE to ethene. The largest fractionation factors are observed in the steps DCE-VC and VC-Ethene. In general, the δ 13 C of each dechlorination product was always more negative than the δ 13 C of the corresponding precursor. In addition, the δ 13 C values of each compound increased with time. A similar pattern was observed for dechlorination of PCE at a field site. These results show that compound-specific carbon isotope ratios technology is a very sensitive tool for evaluation of natural attenuation of chlorinated solvents in groundwater. (author)

  13. Long-range weight functions in fundamental measure theory of the non-uniform hard-sphere fluid

    International Nuclear Information System (INIS)

    Hansen-Goos, Hendrik

    2016-01-01

    We introduce long-range weight functions to the framework of fundamental measure theory (FMT) of the non-uniform, single-component hard-sphere fluid. While the range of the usual weight functions is equal to the hard-sphere radius R , the modified weight functions have range 3 R . Based on the augmented FMT, we calculate the radial distribution function g (r) up to second order in the density within Percus’ test particle theory. Consistency of the compressibility and virial routes on this level allows us to determine the free parameter γ of the theory. As a side result, we obtain a value for the fourth virial coefficient B 4 which deviates by only 0.01% from the exact result. The augmented FMT is tested for the dense fluid by comparing results for g (r) calculated via the test particle route to existing results from molecular dynamics simulations. The agreement at large distances (r   >  6 R) is significantly improved when the FMT with long-range weight functions is used. In order to improve agreement close to contact (r   =  2 R) we construct a free energy which is based on the accurate Carnahan–Starling equation of state, rather than the Percus–Yevick compressibility equation underlying standard FMT. (paper)

  14. 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

  15. 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

  16. Non-destructive profiling of volatile organic compounds using HS-SPME/GC-MS and its application for the geographical discrimination of white rice.

    Science.gov (United States)

    Lim, Dong Kyu; Mo, Changyeun; Lee, Dong-Kyu; Long, Nguyen Phuoc; Lim, Jongguk; Kwon, Sung Won

    2018-01-01

    The authenticity determination of white rice is crucial to prevent deceptive origin labeling and dishonest trading. However, a non-destructive and comprehensive method for rapidly discriminating the geographical origins of white rice between countries is still lacking. In the current study, we developed a volatile organic compound based geographical discrimination method using headspace solid-phase microextraction coupled to gas chromatography-mass spectrometry (HS-SPME/GC-MS) to discriminate rice samples from Korea and China. A partial least squares discriminant analysis (PLS-DA) model exhibited a good classification of white rice between Korea and China (accuracy = 0.958, goodness of fit = 0.937, goodness of prediction = 0.831, and permutation test p-value = 0.043). Combining the PLS-DA based feature selection with the differentially expressed features from the unpaired t-test and significance analysis of microarrays, 12 discriminatory biomarkers were found. Among them, hexanal and 1-hexanol have been previously known to be associated with the cultivation environment and storage conditions. Other hydrocarbon biomarkers are novel, and their impact on rice production and storage remains to be elucidated. In conclusion, our findings highlight the ability to rapidly discriminate white rice from Korea and China. The developed method maybe useful for the authenticity and quality control of white rice. Copyright © 2017. Published by Elsevier B.V.

  17. Aroma volatiles obtained at harvest by HS-SPME/GC-MS and INDEX/MS-E-nose fingerprint discriminate climacteric behaviour in melon fruit.

    Science.gov (United States)

    Chaparro-Torres, Libia A; Bueso, María C; Fernández-Trujillo, Juan P

    2016-05-01

    Melon aroma volatiles were extracted at harvest from juice of a climacteric near-isogenic line (NIL) SC3-5-1 with two quantitative trait loci (QTLs) introgressed which produced climacteric behaviour and its non-climacteric parental (PS) using two methodologies of analysis: static headspace solid phase micro-extraction (HS-SPME) by gas chromatography-mass spectrometry (GC-MS) and inside needle dynamic extraction (INDEX) by MS-based electronic nose (MS-E-nose). Of the 137 volatiles compounds identified, most were found at significantly higher concentrations in SC3-5-1 than in PS in both seasons. These volatiles were mostly esters, alcohols, sulfur-derived esters and even some aldehydes and others. The number of variables with high correlation values was reduced by using correlation network analysis. Partial least squares-discriminant analysis (PLS-DA) achieved the correct classification of PS and SC3-5-1. The ions m/z 74, 91, 104, 105, 106 and 108, mainly volatile derivatives precursor phenylalanine, were the most discriminant in SC3-5-1 and PS. As many as 104 QTLs were mapped in season 1 and at least 78 QTLs in each season with an effect above the PS mean. GC-MS gave better discrimination than E-nose. Most of the QTLs that mapped in both seasons enhanced aroma volatiles associated with climacteric behaviour. © 2015 Society of Chemical Industry.

  18. Non-destructive profiling of volatile organic compounds using HS-SPME/GC–MS and its application for the geographical discrimination of white rice

    Directory of Open Access Journals (Sweden)

    Dong Kyu Lim

    2018-01-01

    Full Text Available The authenticity determination of white rice is crucial to prevent deceptive origin labeling and dishonest trading. However, a non-destructive and comprehensive method for rapidly discriminating the geographical origins of white rice between countries is still lacking. In the current study, we developed a volatile organic compound based geographical discrimination method using headspace solid-phase microextraction coupled to gas chromatography–mass spectrometry (HS-SPME/GC–MS to discriminate rice samples from Korea and China. A partial least squares discriminant analysis (PLS-DA model exhibited a good classification of white rice between Korea and China (accuracy = 0.958, goodness of fit = 0.937, goodness of prediction = 0.831, and permutation test p-value = 0.043. Combining the PLS-DA based feature selection with the differentially expressed features from the unpaired t-test and significance analysis of microarrays, 12 discriminatory biomarkers were found. Among them, hexanal and 1-hexanol have been previously known to be associated with the cultivation environment and storage conditions. Other hydrocarbon biomarkers are novel, and their impact on rice production and storage remains to be elucidated. In conclusion, our findings highlight the ability to rapidly discriminate white rice from Korea and China. The developed method maybe useful for the authenticity and quality control of white rice.

  19. Use of boron nitride for neutron spectrum characterization and cross-section validation in the epithermal range through integral activation measurements

    Science.gov (United States)

    Radulović, Vladimir; Trkov, Andrej; Jaćimović, Radojko; Gregoire, Gilles; Destouches, Christophe

    2016-12-01

    A recent experimental irradiation and measurement campaign using containers made from boron nitride (BN) at the Jožef Stefan Institute (JSI) TRIGA Mark II reactor in Ljubljana, Slovenia, has shown the applicability of BN for neutron spectrum characterization and cross-section validation in the epithermal range through integral activation measurements. The first part of the paper focuses on the determination of the transmission function of a BN container through Monte Carlo calculations and experimental measurements. The second part presents the process of tayloring the sensitivity of integral activation measurements to specific needs and a selection of suitable radiative capture reactions for neutron spectrum characterization in the epithermal range. A BN container used in our experiments and its qualitative effect on the neutron spectrum in the irradiation position employed is displayed in the Graphical abstract.

  20. A wide-frequency range AC magnetometer to measure the specific absorption rate in nanoparticles for magnetic hyperthermia

    International Nuclear Information System (INIS)

    Garaio, E.; Collantes, J.M.; Garcia, J.A.; Plazaola, F.; Mornet, S.; Couillaud, F.; Sandre, O.

    2014-01-01

    Measurement of specific absorption rate (SAR) of magnetic nanoparticles is crucial to assert their potential for magnetic hyperthermia. To perform this task, calorimetric methods are widely used. However, those methods are not very accurate and are difficult to standardize. In this paper, we present AC magnetometry results performed with a lab-made magnetometer that is able to obtain dynamic hysteresis-loops in the AC magnetic field frequency range from 50 kHz to 1 MHz and intensities up to 24 kA m −1 . In this work, SAR values of maghemite nanoparticles dispersed in water are measured by AC magnetometry. The so-obtained values are compared with the SAR measured by calorimetric methods. Both measurements, by calorimetry and magnetometry, are in good agreement. Therefore, the presented AC magnetometer is a suitable way to obtain SAR values of magnetic nanoparticles. - Highlights: • We propose AC magnetometry as a method to measure the specific absorption rate (SAR) of magnetic nanoparticles suitable for magnetic hyperthermia therapy. • We have built a lab-made AC magnetometer, which is able to measure magnetic dynamic hysteresis-loops of nanoparticle dispersions. • The device works with AC magnetic field intensities up to 24 kA m −1 in a frequency range from 75 kHz to 1 MHz. • The SAR values of maghemite nanoparticles around 12 nm in magnetic diameter dispersed in water are measured by the lab-made magnetometer and different calorimetric methods. • Although all methods are in good agreement, several factors (probe location, thermal inertia, losses, etc.) make calorimetric method less accurate than AC magnetometry

  1. Determination of imidazole derivatives by micellar electrokinetic chromatography combined with solid-phase microextraction using activated carbon-polymer monolith as adsorbent.

    Science.gov (United States)

    Shih, Yung-Han; Lirio, Stephen; Li, Chih-Keng; Liu, Wan-Ling; Huang, Hsi-Ya

    2016-01-08

    In this study, an effective method for the separation of imidazole derivatives 2-methylimidazole (2-MEI), 4- methylimidazole (4-MEI) and 2-acetyl-4-tetrahydroxybutylimidazole (THI) in caramel colors using cation-selective exhaustive injection and sweeping micellar electrokinetic chromatography (CSEI-sweeping-MEKC) was developed. The limits of detection (LOD) and quantitation (LOQ) for the CSEI-sweeping-MEKC method were in the range of 4.3-80μgL(-1) and 14-270μgL(-1), respectively. Meanwhile, a rapid fabrication activated carbon-polymer (AC-polymer) monolithic column as adsorbent for solid-phase microextraction (SPME) of imidazole colors was developed. Under the optimized SPME condition, the extraction recoveries for intra-day, inter-day and column-to-column were in the range of 84.5-95.1% (<6.3% RSDs), 85.6-96.1% (<4.9% RSDs), and 81.3-96.1% (<7.1% RSDs), respectively. The LODs and LOQs of AC-polymer monolithic column combined with CSEI-sweeping-MEKC method were in the range of 33.4-60.4μgL(-1) and 111.7-201.2μgL(-1), respectively. The use of AC-polymer as SPME adsorbent demonstrated the reduction of matrix effect in food samples such as soft drink and alcoholic beverage thereby benefiting successful determination of trace-level caramel colors residues using CSEI-sweeping-MEKC method. The developed AC-polymer monolithic column can be reused for more than 30 times without any significant loss in the extraction recovery for imidazole derivatives. Copyright © 2015 Elsevier B.V. All rights reserved.

  2. A system for using the air radioactivity measurements in a long range model to forecast cloud evolution

    Energy Technology Data Exchange (ETDEWEB)

    Galmarini, S.; Graziani, G. (Commission of the European Communities, Ispra (Italy). Joint Research Centre); Grippa, G.; De Cort, M. (Maind srl, Milan (Italy))

    1993-01-01

    A procedure was developed in the past to reduce uncertainties in long range transport model predictions mainly due to inputing windfield data to atmospheric transport models which are the result of the forecasts of global or regional circulation models. Measurements available in real-time of the air concentrations from national monitoring grids have been used to reduce the uncertainties. The system is based on a long range transport model which can run using a limited amount of meteorological information, and an interpolation routine which generates a new area source from the air measurements, available in real-time, at ground level. The procedure has now been fully automated and is available on a PC, with graphical output, to ease its use in emergency situations. The system requires a connection to the ECMWF network for meteorological input data and to a radiological data bank (ECURIE) or national monitoring networks for monitoring data. (author).

  3. Oxidative degradation and non-enzymatic browning due to the interaction between oxidised lipids and primary amine groups in different marine PL emulsions

    DEFF Research Database (Denmark)

    Lu, Henna Fung Sieng; Nielsen, Nina Skall; Baron, Caroline P.

    2012-01-01

    investigated through the measurement of secondary volatile compounds by solid-phase microextraction (SPME) and dynamic headspace (DHS) connected to gas chromatography (GC–MS). Non-enzymatic browning reactions were investigated through the measurement of Strecker derived volatiles, colour changes and pyrrole...

  4. A compact design for monochromatic OSL measurements in the wavelength range 380-1020 NM

    DEFF Research Database (Denmark)

    Bøtter-Jensen, L.; Poolton, N.R.J.; Willumsen, F.

    1994-01-01

    automated Riso TL/OSL dating apparatus, thus allowing for either routine scanning or more detailed thermo-optical investigations. The high throughput efficiency of the unit means that the existing 75 W tungsten-halogen lamp can be directly used for such measurements on both quartz and feldspar samples......The development and performance of a compact module is described that allows for the monochromatic illumination of samples in the wavelength range 380-1020 nm, enabling the measurement of energy-resolved optically stimulated luminescence. The unit is designed to couple directly to the existing....... The design allows for rapid spectral scanning with a choice of resolution of anywhere between 10 and 80 nm: stray light levels are less than 0.01%. The unit can equally be used for recording wavelength-resolved emission spectra, whether photo-excited or thermally stimulated; the capabilities of the system...

  5. Raman spectroscopy, electronic microscopy and SPME-GC-MS to elucidate the mode of action of a new antimicrobial food packaging material.

    Science.gov (United States)

    Clemente, Isabel; Aznar, Margarita; Salafranca, Jesús; Nerín, Cristina

    2017-02-01

    One critical challenge when developing a new antimicrobial packaging material is to demonstrate the mode of action of the antimicrobials incorporated into the packaging. For this task, several analytical techniques as well as microbiology are required. In this work, the antimicrobial properties of benzyl isothiocyanate, allyl isothiocyanate and essential oils of cinnamon and oregano against several moulds and bacteria have been evaluated. Benzyl isothiocyanate showed the highest antimicrobial activity and it was selected for developing the new active packaging material. Scanning electron microscopy and Raman spectroscopy were successfully used to demonstrate the mode of action of benzyl isothiocyanate on Escherichia coli. Bacteria exhibited external modifications such as oval shape and the presence of septum surface, but they did not show any disruption or membrane damage. To provide data on the in vitro action of benzyl isothiocyanate and the presence of inhibition halos, the transfer mechanism to the cells was assessed using solid-phase microextraction-gas chromatography-mass spectrometry. Based on the transfer system, action mechanism and its stronger antimicrobial activity, benzyl isothiocyanate was incorporated to two kinds of antimicrobial labels. The labels were stable and active for 140 days against two mould producers of ochratoxin A; Penicillium verrucosum is more sensitive than Aspergillus ochraceus. Details about the analytical techniques and the results obtained are shown and discussed. Graphical Abstract Antimicrobial evaluation of pure compounds, incorporation in the packaging and study for mode of action on S. coli by Raman, SEM and SPME-GC-MS.

  6. Monolithic graphene fibers for solid-phase microextraction.

    Science.gov (United States)

    Fan, Jing; Dong, Zelin; Qi, Meiling; Fu, Ruonong; Qu, Liangti

    2013-12-13

    Monolithic graphene fibers for solid-phase microextraction (SPME) were fabricated through a dimensionally confined hydrothermal strategy and their extraction performance was evaluated. For the fiber fabrication, a glass pipeline was innovatively used as a hydrothermal reactor instead of a Teflon-lined autoclave. Compared with conventional methods for SPME fibers, the proposed strategy can fabricate a uniform graphene fiber as long as several meters or more at a time. Coupled to capillary gas chromatography (GC), the monolithic graphene fibers in a direct-immersion (DI) mode achieved higher extraction efficiencies for aromatics than those for n-alkanes, especially for polycyclic aromatic hydrocarbons (PAHs), thanks to π-π stacking interaction and hydrophobic effect. Additionally, the fibers exhibited excellent durability and can be repetitively used more than 160 times without significant loss of extraction performance. As a result, an optimum extraction condition of 40°C for 50min with 20% NaCl (w/w) was finally used for SPME of PAHs in aqueous samples. For the determination of PAHs in water samples, the proposed DI-SPME-GC method exhibited linear range of 0.05-200μg/L, limits of detection (LOD) of 4.0-50ng/L, relative standard deviation (RSD) less than 9.4% and 12.1% for one fiber and different fibers, respectively, and recoveries of 78.9-115.9%. The proposed method can be used for analysis of PAHs in environmental water samples. Copyright © 2013 Elsevier B.V. All rights reserved.

  7. Attenuation on an Earth-space path measured in the wavelength range of 8 to 14 micrometers.

    Science.gov (United States)

    Wilson, R W

    1970-06-19

    A telescope operating over the wavelength range of 8 to 14 micrometers has been added to the Crawford Hill sun tracker for the purpose of measuring attenuation in that atmospheric window. Over a 9-month period the attenuation (typically from clouds) exceeded 10, 20, and 30 decibels for 48, 43, and 34 percent of the time.

  8. Photopolarimetric properties of leaf and vegetation covers over a wide range of measurement directions

    Science.gov (United States)

    Sun, Zhongqiu; Peng, Zhiyan; Wu, Di; Lv, Yunfeng

    2018-02-01

    The optical scattering property of the target is the essential signal for passive remote sensing applications. To deepen our understanding of the light reflected from vegetation, we present results of photopolarimetric laboratory measurements from single leaf and two vegetation covers (planophile and erectophile) over a wide range of viewing directions. The bidirectional polarized reflectance factor (BPRF) was used to characterize the polarization property of our samples. We observed positive and negative polarization (-BPRFQ) of all samples in the forward scattering and backward scattering directions, respectively. Based on the comparison of the BPRF among single leaf, planophile vegetation and erectophile vegetation, our measurements demonstrate that the orientation of the leaf is a key factor in describing the amount of polarization in the forward scattering direction. Our measurements also validated certain model results stating that (1) specular reflection generates a portion of polarization in the forward scattering direction and diffuses scattering of polarized light in all hemisphere directions, (2) BPRFU is anti-symmetric in the principal plane from a recent study in which the authors simulated the polarized reflectance of vegetation cover using the vector radiative transfer theory. These photopolarimetric measurement results, which can be completely explained by the theoretical results, are useful in remote sensing applications to vegetation.

  9. Long-range active retroreflector to measure the rotational orientation in conjunction with a laser tracker

    Science.gov (United States)

    Hofherr, O.; Wachten, Christian; Müller, C.; Reinecke, H.

    2014-11-01

    High precision optical non-contact position measurement is a key technology in modern engineering. Laser trackers (LT) accurately determine x-y-z coordinates of passive retroreflectors. Next-generation systems answer the need to measure an object`s rotational orientation (pitch, yaw, roll). So far, these devices are based either on photogrammetry or on enhanced retroreflectors. Here we present a new method to measure all six degrees of freedom in conjunction with a LT. The basic principle is to analyze the orientation to the LT's beam path by coupling-out laser radiation. The optical design is inspired by a cat's eye retroreflector equipped with an integrated beam splitter layer. The optical spherical aberration is compensated, which reduces the divergence angle for the reflected beam by one order of magnitude compared to an uncompensated standard system of the same size. The wave front distortion is reduced to less than 0.1 λ @ 633 nm for beam diameters up to 8 mm. Our active retroreflector is suitable for long-range measurements for a distance > 10 m.

  10. Dual sightline measurements of MeV range deuterons with neutron and gamma-ray spectroscopy at JET

    DEFF Research Database (Denmark)

    Eriksson, J.; Nocente, M.; Binda, F.

    2015-01-01

    Observations made in a JET experiment aimed at accelerating deuterons to the MeV range by third harmonic radio-frequency (RF) heating coupled into a deuterium beam are reported. Measurements are based on a set of advanced neutron and gamma-ray spectrometers that, for the first time, observe......-ray spectroscopy based on a one-dimensional model and by a consistency check among the individual measurement techniques. A systematic difference is seen between the two lines of sight and is interpreted to originate from the sensitivity of the oblique detectors to the pitch-angle structure of the distribution...

  11. Performance of passive samplers for monitoring estuarine water column concentrations: 2. Emerging contaminants.

    Science.gov (United States)

    Perron, Monique M; Burgess, Robert M; Suuberg, Eric M; Cantwell, Mark G; Pennell, Kelly G

    2013-10-01

    Measuring dissolved concentrations of emerging contaminants, such as polybrominated diphenyl ethers (PBDEs) and triclosan, can be challenging due to their physicochemical properties resulting in low aqueous solubilities and association with particles. Passive sampling methods have been applied to assess dissolved concentrations in water and sediments primarily for legacy contaminants. Although the technology is applicable to some emerging contaminants, the use of passive samplers with emerging contaminants is limited. In the present study, the performance of 3 common passive samplers was evaluated for sampling PBDEs and triclosan. Passive sampling polymers included low-density polyethylene (PE) and polyoxymethylene (POM) sheets, and polydimethylsiloxane (PDMS)-coated solid-phase microextraction (SPME) fibers. Dissolved concentrations were calculated using measured sampler concentrations and laboratory-derived partition coefficients. Dissolved tri-, tetra-, and pentabrominated PBDE congeners were detected at several of the study sites at very low pg/L concentrations using PE and POM. Calculated dissolved water concentrations of triclosan ranged from 1.7 ng/L to 18 ng/L for POM and 8.8 ng/L to 13 ng/L for PE using performance reference compound equilibrium adjustments. Concentrations in SPME were not reported due to lack of detectable chemical in the PDMS polymer deployed. Although both PE and POM were found to effectively accumulate emerging contaminants from the water column, further research is needed to determine their utility as passive sampling devices for emerging contaminants. © 2013 SETAC.

  12. Extending the range of turbidity measurement using polarimetry

    Science.gov (United States)

    Baba, Justin S.

    2017-11-21

    Turbidity measurements are obtained by directing a polarized optical beam to a scattering sample. Scattered portions of the beam are measured in orthogonal polarization states to determine a scattering minimum and a scattering maximum. These values are used to determine a degree of polarization of the scattered portions of the beam, and concentrations of scattering materials or turbidity can be estimated using the degree of polarization. Typically, linear polarizations are used, and scattering is measured along an axis that orthogonal to the direction of propagation of the polarized optical beam.

  13. Measurement of Shoulder Range of Motion in Patients with Adhesive Capsulitis Using a Kinect.

    Directory of Open Access Journals (Sweden)

    Seung Hak Lee

    Full Text Available Range of motion (ROM measurements are essential for the evaluation for and diagnosis of adhesive capsulitis of the shoulder (AC. However, taking these measurements using a goniometer is inconvenient and sometimes unreliable. The Kinect (Microsoft, Seattle, WA, USA is gaining attention as a new motion detecting device that is nonintrusive and easy to implement. This study aimed to apply Kinect to measure shoulder ROM in AC; we evaluated its validity by calculating the agreement of the measurements obtained using Kinect with those obtained using goniometer and assessed its utility for the diagnosis of AC. Both shoulders of 15 healthy volunteers and affected shoulders of 12 patients with AC were included in the study. The passive and active ROM of each were measured with a goniometer for flexion, abduction, and external rotation. Their active shoulder motions for each direction were again captured using Kinect and the ROM values were calculated. The agreement between the two measurements was tested with the intraclass correlation coefficient (ICC. Diagnostic performance using the Kinect ROM was evaluated with Cohen's kappa value. The cutoff values of the limited ROM were determined in the following ways: the same as passive ROM values, reflecting the mean difference, and based on receiver operating characteristic curves. The ICC for flexion/abduction/external rotation between goniometric passive ROM and the Kinect ROM were 0.906/0.942/0.911, while those between active ROMs and the Kinect ROMs were 0.864/0.932/0.925. Cohen's kappa values were 0.88, 0.88, and 1.0 with the cutoff values in the order above. Measurements of the shoulder ROM using Kinect show excellent agreement with those taken using a goniometer. These results indicate that the Kinect can be used to measure shoulder ROM and to diagnose AC as an alternative to goniometer.

  14. α-Tocopherol/chitosan-based nanoparticles: characterization and preliminary investigations for emulsion systems application

    Science.gov (United States)

    Aresta, Antonella; Calvano, Cosima Damiana; Trapani, Adriana; Zambonin, Carlo Giorgio; De Giglio, Elvira

    2014-02-01

    The processes of lipids oxidation represent a great concern for the consumer health because they are one of the major causes of quality deterioration in fat-containing products. One of the most effective methods of delaying lipid oxidation consists in incorporating antioxidants. The present investigation describes the formulation of chitosan and novel glycol chitosan nanoparticles (NPs) loaded with α-Tocopherol (αToc-NPs). The obtained NPs were characterized by various techniques, such as particle size (showing mean diameters in the range 335-503 nm) and zeta potential measurements, X-ray photoelectron spectroscopy and Fourier transform infrared spectroscopy. The NPs were, then, added in the preparation of oil-in-water simple emulsion both to make the lipophilic αToc available in an aqueous medium and to prevent emulsion oxidation. For this purpose, a new highly sensitive, simple and solvent-free method based on a solid phase microextraction (SPME) coupled to gas chromatography mass spectrometry was developed for the determination of αToc in aqueous medium. All the parameters influencing SPME, including fiber coating, time and temperature extraction, pH, ionic strength and desorption conditions, have been carefully screened. The method was successfully applied to the determination of vitamin in the αToc-NPs and its release from NPs-enriched simple emulsion formulations. SPME provided high recovery yields and the limits of detection and of quantification in emulsion were 0.1 and 0.5 μg/mg, respectively. The precision of the method has been also estimated. The delay of the lipid oxidation by the proposed formulations has been evaluated exploiting the Kreis test on αToc-NPs-enriched emulsions.

  15. A pressurized ion chamber monitoring system for environmental radiation measurements utilizing a wide-range temperature-compensated electrometer

    International Nuclear Information System (INIS)

    Stevenick, W. Van

    1994-01-01

    The performance of a complete pressurized ion chamber (PIC) radiation monitoring system is described. The design incorporates an improved temperature-compensated electrometer which is stable to ±3 · 10 -16 A over the environmental range of temperature (-40 to +40 C). Using a single 10 11 Ω feed-back resistor, the electrometer accurately measures currents over a range from 3 · 10 -15 A to 3 · 10 -11 A. While retaining the sensitivity of the original PIC system (the instrument responds readily to small background fluctuations on the order of 0.1 μR h -1 ), the new system measures radiation levels up to the point where the collection efficiency of the ion chamber begins to drop off, typically ∼27 pA at 1 mR h -1 . A data recorder and system controller was designed using the Tattletale trademark Model 4A computer. Digital data is stored on removable solid-state, credit-card style memory cards

  16. Feasibility of RACT for 3D dose measurement and range verification in a water phantom.

    Science.gov (United States)

    Alsanea, Fahed; Moskvin, Vadim; Stantz, Keith M

    2015-02-01

    The objective of this study is to establish the feasibility of using radiation-induced acoustics to measure the range and Bragg peak dose from a pulsed proton beam. Simulation studies implementing a prototype scanner design based on computed tomographic methods were performed to investigate the sensitivity to proton range and integral dose. Derived from thermodynamic wave equation, the pressure signals generated from the dose deposited from a pulsed proton beam with a 1 cm lateral beam width and a range of 16, 20, and 27 cm in water using Monte Carlo methods were simulated. The resulting dosimetric images were reconstructed implementing a 3D filtered backprojection algorithm and the pressure signals acquired from a 71-transducer array with a cylindrical geometry (30 × 40 cm) rotated over 2π about its central axis. Dependencies on the detector bandwidth and proton beam pulse width were performed, after which, different noise levels were added to the detector signals (using 1 μs pulse width and a 0.5 MHz cutoff frequency/hydrophone) to investigate the statistical and systematic errors in the proton range (at 20 cm) and Bragg peak dose (of 1 cGy). The reconstructed radioacoustic computed tomographic image intensity was shown to be linearly correlated to the dose within the Bragg peak. And, based on noise dependent studies, a detector sensitivity of 38 mPa was necessary to determine the proton range to within 1.0 mm (full-width at half-maximum) (systematic error ionizing radiation-induced acoustics can be used to verify dose distribution and proton range with centi-Gray sensitivity. Realizing this technology into the clinic has the potential to significantly impact beam commissioning, treatment verification during particle beam therapy and image guided techniques.

  17. Alanine-EPR dosimetry for measurements of ionizing radiation absorbed doses in the range 0.5-10 kGy

    CERN Document Server

    Peimel-Stuglik, Z

    2001-01-01

    The usefulness of two, easy accessible alanine dosimeters (ALANPOL from IChTJ and foil dosimeter from Gamma Service, Radeberg, Germany) to radiation dose measurement in the range of 0.5-10 kGy, were investigated. In both cases, the result of the test was positive. The foil dosemeter from Gamma Service is recommended for dose distribution measurements in fantoms or products, ALANPOL - for routine measurements. The EPR-alanine method based on the described dosimeters can be successfully used, among others, in the technology of radiation protection of food.

  18. LHC MD2877: Beam-beam long range impact on coupling measurements

    CERN Document Server

    Wenninger, Jorg; Carlier, Felix Simon; Coello De Portugal - Martinez Vazquez, Jaime Maria; Fuchsberger, Kajetan; Hostettler, Michi; Persson, Tobias Hakan Bjorn; Tomas Garcia, Rogelio; Valuch, Daniel; Garcia-Tabares Valdivieso, Ana; CERN. Geneva. ATS Department

    2018-01-01

    The LHC is now operating with a tune separation of ∼0.004 in collision. This puts tight constraints on the allowed transverse coupling since a |C−| larger than a fraction of the fractional tune split may lead to beam instabilities. In the last years a new tool based on the ADT used in a similar way as an AC-dipole to excite the beam was developed. The ADT AC-dipole gives coherent oscillations without increasing the beam emittance. These oscillations are analyzed automatically to obtain the value of the coupling. A coupling measurement campaign was done in 2017 and while the correction converged and stayed rather constant over time it was observed that depending on the target bunch and filling scheme the results could vary by Δ|C−| ∼ 0.002. In this MD report we investigated 3 different bunches, one with Long Range Beam-Beam (LRBB) in IPs 1 and 5, one with LRBB in all IPs and one with no LRBB. The results indicate that there are differences in coupling between the bunches experiencing different LR...

  19. Fractional momentum transfer in incomplete fusion reaction: measurement of recoil range distributions in 20Ne + 159Tb system

    International Nuclear Information System (INIS)

    Ali, R.; Singh, D.; Pachouri, Dipti; Afzal Ansari, M.; Rashid, M.H.

    2007-01-01

    The recoil range distribution (RRD) of several residues have been measured for the system 20 Ne + 159 Tb at 165 MeV beam energy by collecting the recoiling residues in the Al-catcher foils of varying thickness

  20. Highly accurate nuclear and electronic stopping cross sections derived using Monte Carlo simulations to reproduce measured range data

    Science.gov (United States)

    Wittmaack, Klaus; Mutzke, Andreas

    2017-03-01

    We have examined and confirmed the previously unexplored concept of using Monte Carlo calculations in combination with measured projected ranges of ions implanted in solids to derive a quantitative description of nuclear interaction and electronic stopping. The study involved 98 ranges of 11B in Si between 1 keV and 8 MeV, contained in 12 sets of 10 different groups. Systematic errors by up to ±8% were removed to establish a refined data base with 93 ranges featuring only statistical uncertainties (±1.8%). The Monte Carlo calculations could be set up to reproduce the refined ranges with a mean ratio 1.002 ± 1.7%. The input parameters required for this very high level of agreement are as follows. Nuclear interaction is best described by the Kr-C potential, but in obligatory combination with the Lindhard-Scharff (LS) screening length. Up to 300 keV, the electronic stopping cross section is proportional to the projectile velocity, Se = kSe,LS, with k = 1.46 ± 0.01. At higher energies, Se falls progressively short of kSe,LS. Around the Bragg peak, i.e., between 0.8 and 10 MeV, Se is modeled by an adjustable function serving to tailor the peak shape properly. Calculated and measured isotope effects for ranges of 10B and 11B in Si agree within the experimental uncertainty (±0.25%). The range-based Se,R(E) reported here predicts the scarce experimental data derived from the energy loss in projectile transmission through thin Si foils to within 2% or better. By contrast, Se(E) data of available stopping power tables exhibit deviations from Se,R(E) between -40% and +14%.

  1. An absolute measurement of 252Cf prompt fission neutron spectrum at low energy range

    International Nuclear Information System (INIS)

    Lajtai, A.; Dyachenko, P.P.; Kutzaeva, L.S.; Kononov, V.N.; Androsenko, P.A.; Androsenko, A.A.

    1983-01-01

    Prompt neutron energy spectrum at low energies (25 keV 252 Cf spontaneous fission has been measured with a time-of-flight technique on a 30 cm flight-path. Ionization chamber and lithium-glass were used as fission fragment and neutron detectors, respectively. Lithium glasses of NE-912 (containing 6 Li) and of NE-913 (containing 7 Li) 45 mm in diameter and 9.5 mm in thickness have been employed alternatively, for the registration of fission neutrons and gammas. For the correct determination of the multiscattering effects - the main difficulty of the low energy neutron spectrum measurements - a special geometry for the neutron detector was used. Special attention was paid also to the determination of the absolute efficiency of the neutron detector. The real response function of the spectrometer was determined by a Monte-Carlo calculation. The scattering material content of the ionization chamber containing a 252 Cf source was minimized. As a result of this measurement a prompt fission neutron spectrum of Maxwell type with a T=1.42 MeV parameter was obtained at this low energy range. We did not find any neutron excess or irregularities over the Maxwellian. (author)

  2. Depth Dose Measurement using a Scintillating Fiber Optic Dosimeter for Proton Therapy Beam of the Passive-Scattering Mode Having Range Modulator Wheel

    Science.gov (United States)

    Hwang, Ui-Jung; Shin, Dongho; Lee, Se Byeong; Lim, Young Kyung; Jeong, Jong Hwi; Kim, Hak Soo; Kim, Ki Hwan

    2018-05-01

    To apply a scintillating fiber dosimetry system to measure</