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Sample records for microextration spme fibers

  1. UPTAKE OF RADIONUCLIDE METALS BY SPME FIBERS

    SciTech Connect

    Duff, M; S Crump, S; Robert02 Ray, R; Keisha Martin, K; Donna Beals, D

    2006-08-28

    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 ({sup 239/240}Pu, {sup 238}U, {sup 237}Np, {sup 85}Sr, {sup 133}Ba, {sup 137}Cs, {sup 60}Co and {sup 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. Detection of Methyl Salicylate Transforted by Honeybees (Apis mellifera) Using Solid Phase Microextration (SPME) Fibers

    SciTech Connect

    BENDER, SUSAN FAE ANN; RODACY, PHILIP J.; BARNETT, JAMES L.; BENDER, GARY L.

    2001-12-01

    The ultimate goal of many environmental measurements is to determine the risk posed to humans or ecosystems by various contaminants. Conventional environmental monitoring typically requires extensive sampling grids covering several media including air, water, soil and vegetation. A far more efficient, innovative and inexpensive tactic has been found using honeybees as sampling mechanisms. Members from a single bee colony forage over large areas ({approx}2 x 10{sup 6} m{sup 2}), making tens of thousands of trips per day, and return to a fixed location where sampling can be conveniently conducted. The bees are in direct contact with the air, water, soil and vegetation where they encounter and collect any contaminants that are present in gaseous, liquid and particulate form. The monitoring of honeybees when they return to the hive provides a rapid method to assess chemical distributions and impacts (1). The primary goal of this technology is to evaluate the efficiency of the transport mechanism (honeybees) to the hive using preconcentrators to collect samples. Once the extent and nature of the contaminant exposure has been characterized, resources can be distributed and environmental monitoring designs efficiently directed to the most appropriate locations. Methyl salicylate, a chemical agent surrogate was used as the target compound in this study.

  3. Detection of organophosphorous pesticides in soil samples with multiwalled carbon nanotubes coating SPME fiber.

    PubMed

    Feng, Xilan; Li, Ying; Jing, Ruijun; Jiang, Xiaoying; Tian, Mengkui

    2014-12-01

    A headspace solid phase microextraction (HS-SPME) technique using stainless steel fiber coated with 20 μm multi-walled carbon nanotubes (MWCNTs) and gas chromatography with thermionic specific detector (GC-TSD) was developed to determine organophosphorous pesticides (OPPs) in soil. Parameters affecting the extraction efficiency such as extraction time and temperature, ionic strength, the volume of water added to the soil, sample solution volume to headspace volume ratio, desorption time, and desorption temperature were investigated and optimized. Compared to commercial polydimethylsiloxane (PDMS, 7 μm) fiber, the PDMS fiber was better to be corrected as phorate, whereas the MWCNTs fiber gave slightly better results for methyl parathion, chlorpyrifos and parathion. The optimized SPME method was applied to analyze OPPs in spiked soil samples. The limits of detection (LODs, S/N = 3) for the four pesticides were <0.216 ng g(-1), and their calibration curves were all linear (r (2) ≥ 0.9908) in the range from 1 to 200 ng g(-1). The precision (RSD, n = 6) for peak areas was 6.5 %-8.8 %. The recovery of the OPPs spiked real soil samples at 50 and 150 ng g(-1) ranged from 89.7 % to 102.9 % and 94.3 % to 118.1 %, respectively.

  4. Predicting the toxicity of permethrin to Daphnia magna in water using SPME fibers.

    PubMed

    Harwood, Amanda D; Bunch, Aubrey R; Flickinger, Dallas L; You, Jing; Lydy, Michael J

    2012-04-01

    Multiple factors can influence bioavailability, which can make predictions of toxicity in natural systems difficult. The current study examined the potential use of solid-phase microextraction fibers as a matrix-independent approach to predict the toxicity of permethrin to Daphnia magna across various water sources, including a laboratory reconstituted water, two natural waters, and a modified natural water. Water source strongly affected the toxicity of permethrin as well as the concentration-response relationships. Although permethrin concentrations in the water were predictive of toxicity to D. magna for individual water sources, there was no relationship between permethrin concentrations among water sources and mortality. This indicated that compositional differences among water sources can greatly influence toxicity, suggesting that benchmarks established using reconstituted water may be overly conservative for some natural waters. In addition, although permethrin tissue residues were predictive of mortality for individual waters, the correlation among waters was not as clear. Finally, both 48-h and equilibrium-based SPME fiber concentrations adequately predicted toxicity independent of water properties. This demonstrated that bioavailability-based estimates provided a more accurate prediction of toxicity than water concentrations and that SPME fibers could be used in environmental monitoring as a rapid and accurate means of predicting toxicity in natural waters.

  5. Using polyacrylate-coated SPME fibers to quantify sorption of polar and ionic organic contaminants to dissolved organic carbon.

    PubMed

    Haftka, Joris J-H; Scherpenisse, Peter; Jonker, Michiel T O; Hermens, Joop L M

    2013-05-07

    A passive sampling method using polyacrylate-coated solid-phase microextraction (SPME) fibers was applied to determine sorption of polar and ionic organic contaminants to dissolved organic carbon (DOC). The tested contaminants included pharmaceuticals, industrial chemicals, hormones, and pesticides and represented neutral, anionic, and cationic structures. Prior to the passive sampler application, sorption of the chemicals to the fibers was characterized. This was needed in order to accurately translate concentrations measured in fibers to freely dissolved aqueous concentrations during the sorption tests with DOC. Sorption isotherms of neutral compounds to the fiber were linear, whereas isotherms of basic chemicals covered a nonlinear and a linear range. Sorption of acidic and basic compounds to the fiber was pH-dependent and was dominated by sorption of the neutral sorbate species. Fiber- and DOC-water partition coefficients of neutral compounds were both linearly related to octanol-water partition coefficients (log Kow). The results of this study show that polyacrylate fibers can be used to quantify sorption to DOC of neutral and ionic contaminants, having multiple functional groups and spanning a wide hydrophobicity range (log Kow = 2.5-7.5).

  6. Assessment of thiol compounds from garlic by automated headspace derivatized in-needle-NTD-GC-MS and derivatized in-fiber-SPME-GC-MS.

    PubMed

    Warren, Jamie Marcus; Parkinson, Don-Roger; Pawliszyn, Janusz

    2013-01-23

    This study investigates the analysis of thiol compounds using a needle trap device (HS-NTD) and solid-phase microextraction (HS-SPME) derivatized headspace techniques coupled to GC-MS. Thiol compounds and their outgassed products are particularly difficult to monitor in foodstuffs. It was found that with in-needle and in-fiber derivatization, using the derivatization agent N-phenylmaleimide, it was possible to enhance the selectivity toward thiol, which allowed the quantitation of butanethiol, ethanethiol, methanethiol, and propanethiol compounds found in fresh garlic. A side-hole NTD was prepared and packed in house and utilized mixed DVB and Carboxen polymer extraction phases made of 60-80 mesh particles. NTD sampling was accomplished in the exhaustive sampling mode, where breakthrough was negligible. This work demonstrates a new application for a side-hole NTD sampling. A commercial mixed polymer phase of polydimethylsiloxane (PDMS) and divinylbenzene polymer (DVB) SPME fiber was used for SPME extractions. Under optimized derivatization, extraction, and analysis conditions for both NTD-GC-MS and SPME-GC-MS techniques, automated sampling methods were developed for quantitation. Both methods demonstrate a successful approach to thiol determination and provide a quantitative linear response between <0.1 and 10 mg L(-1) (R(2) = 0.9996), with limits of detection (LOD) in the low micrograms per liter range for the investigated thiols. Addition methods using known spiked quantities of thiol analytes in ground garlic facilitated method validation. Carry-over was also negligible for both SPME and NTD under optimized conditions.

  7. Remedy performance monitoring at contaminated sediment sites using profiling solid phase microextraction (SPME) polydimethylsiloxane (PDMS) fibers.

    PubMed

    Thomas, Courtney; Lampert, David; Reible, Danny

    2014-03-01

    Passive sampling using polydimethylsiloxane (PDMS) profilers was evaluated as a tool to assess the performance of in situ sediment remedies at three locations, Chattanooga Creek (Chattanooga, TN), Eagle Harbor (Bainbridge Island, WA) and Hunter's Point (San Francisco, CA). The remedy at the first two locations was capping over PAH contaminated sediments while at Hunter's Point, the assessment was part of an in situ treatment demonstration led by R. G. Luthy (Stanford University) using activated carbon mixed into PCB contaminated sediments. The implementation and results at these contaminated sediment sites were used to illustrate the utility and usefulness of the passive sampling approach. Two different approaches were employed to evaluate kinetics of uptake onto the sorbent fibers. At the capping sites, the passive sampling approach was employed to measure intermixing during cap placement, contamination migration into the cap post-placement and recontamination over time. At the in situ treatment demonstration site, reductions in porewater concentrations in treated versus untreated sediments were compared to measurements of bioaccumulation of PCBs in Neanthes arenaceodentata.

  8. Comparison between solid phase microextraction (SPME) and hollow fiber liquid phase microextraction (HFLPME) for determination of extractables from post-consumer recycled PET into food simulants.

    PubMed

    Oliveira, Éder Costa; Echegoyen, Yolanda; Cruz, Sandra Andrea; Nerin, Cristina

    2014-09-01

    Hollow fiber liquid phase microextraction (HFLPME) and solid phase microextraction (SPME) methods for pre-concentration of contaminants (toluene, benzophenone, tetracosane and chloroform) in food simulants were investigated. For HFLPME 1-heptanol, 2-octanone and dibutyl-ether were studied as extracting solvents. Analysis by gas chromatography coupled to mass spectrometry (GC-MS), flame ionization (GC-FID) and electron capture detectors (GC-ECD) were carried out. In addition, the methods were employed to evaluate the safety in use of a PET material after the recycling process (comprising washing, extrusion and solid state polymerization (SSP)) through extractability studies of the contaminants using 10% (v/v) ethanol in deionized water and 3% (w/v) acetic acid in deionized water as food simulants in different conditions: 10 days at 40°C and 2h at 70°C. The HFLPME preconcentration method provided increased sensitivity when compared to the SPME method and allowed to analyze concentration levels below 10 µg surrogate per kg food simulant. The results of the extractability studies showed considerable reductions after the extrusion and SSP processes and indicated the compliance with regulations for using recycled PET in contact with food.

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

    PubMed Central

    da Silva, Celia Eliane de Lara; da Costa, Willian Ferreira; Minguzzi, Sandro; da Silva, Rogério Cesar de Lara; Simionatto, Euclésio

    2013-01-01

    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. PMID:24371539

  10. Development and application of an SPME/GC method for the determination of trace phthalates in beer using a calix[6]arene fiber.

    PubMed

    Ye, Chang-Wen; Gao, Jie; Yang, Cai; Liu, Xiao-Jing; Li, Xiu-Juan; Pan, Si-Yi

    2009-05-08

    A simple, low-cost and sensitive method for the determination of phthalate acid esters (PAEs) in beer has been developed based on solid-phase microextraction (SPME) followed by gas chromatography using a novel sol-gel calixarene-contained fiber. Generally speaking, matrix interference is one of the most important problems that researchers have to face when quantifying trace compounds in the complicated beer samples. In order to reproduce the influence of the matrix, synthetic beer solutions were popularly used, while they could not represent the real beer matrix absolutely. Owing to the good selectivity and high sensitivity of this new calixarene fiber, matrix interference from the beer samples was effectively avoided and low limits of detection (LODs) could be achieved. As a result, the SPME was performed in real beer matrices. Five experimental parameters including extraction temperature, extraction time, stirring speed, salt concentration and ultrasonic time were evaluated and optimized by means of a Taguchi's L25 (5(6)) orthogonal array experimental design. Under the optimized conditions, LODs of 0.003-3.429 microg L(-1) were obtained and the relative standard deviation values were < or =13.51% for all of the eight PAEs. The method was validated using standard addition methodology and recovery values were between 86.3% and 109.3%. The survey of three bottled beer samples showed that dibutyl-phthalate ester and bis(2-ethylhexyl)-phthalate ester (DEHP) were the main PAEs found in beer. The concentration of DEHP was as high as 5.24 microg L(-1). In order to investigate the source of phthalates contamination in beer, the composition of phthalates in the plasticized polyvinyl chloride (PVC) gaskets of the lids was analyzed. Results revealed that the high content of DEHP incorporated in PVC gaskets could be a potential source of PAEs in bottled beers during transportation and storage.

  11. Study of the effect of different fiber coatings and extraction conditions on dry cured ham volatile compounds extracted by solid-phase microextraction (SPME).

    PubMed

    Garcia-Esteban, M; Ansorena, D; Astiasarán, I; Ruiz, J

    2004-10-08

    Extraction of dry cured ham volatile compounds by solid-phase microextraction (SPME) was optimized. Different fiber coatings (carboxen/polydimethylsiloxane (CAR/PDMS), divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS), polydimethylsiloxane (PDMS), polydimethylsiloxane/divinylbenzene (PDMS/DVB)), times of extraction (15, 30, 60min) and sample preparation (ground samples and homogenates with NaCl saturated solution) were assayed. CAR/PDMS and DVB/CAR/PDMS fiber coatings extracted more than 100 volatile compounds and showed the highest area counts for most volatile compounds. CAR/PDMS coating extracted better those compounds whose Kovats index (KI) was lower than 980 (on average) and DVB/CAR/PDMS those with higher KI. Fifteen minutes of extraction provided a volatile compound profile with lower area counts for most compounds and qualitatively different to that obtained with 30 and 60min of extraction. Homogenates gave a different profile compared to ground samples, with lower total counts for most compounds but higher proportion of aldehydes, and presence of several compounds not found in ground samples.

  12. 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.

    PubMed

    Hosseinzadeh, Reza; Moosavi Movahedi, Ali Akbar; Ghourchian, Hedayatollah

    2014-01-01

    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.

  13. 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

    PubMed Central

    Hosseinzadeh, Reza; Moosavi Movahedi, Ali Akbar; Ghourchian, Hedayatollah

    2014-01-01

    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. PMID:25068260

  14. Automated on-fiber derivatization with headspace SPME-GC-MS-MS for the determination of primary amines in sewage sludge using pressurized hot water extraction.

    PubMed

    Llop, Anna; Pocurull, Eva; Borrull, Francesc

    2011-07-01

    An automated, environmentally friendly, simple, selective, and sensitive method was developed for the determination of ten primary aliphatic amines in sewage sludge at μg/kg dry weight (d.w.). The procedure involves a pressurized hot water extraction (PHWE) of the analytes from the solid matrix, followed by a fully automated on-fiber derivatization with 2,3,4,5-pentafluorobenzaldehyde (PFBAY) and headspace solid-phase microextraction (HS-SPME) and subsequent gas chromatography ion-trap tandem mass spectrometry (GC-IT-MS-MS) analysis. The limits of detection (LODs) of the method were between 0.5 and 45 μg/kg (d.w.) for all compounds except for ethyl-, isopropyl-, and amylamine, whose LODs were 70, 109, and 116 μg/kg (d.w.), respectively. The limits of quantification (LOQs) were between 10 and 350 μg/kg (d.w.). Repeatability and intermediate precision, expressed as RSD(%) (n=3), were lower than 18 and 21%, respectively. The method developed enabled to determine primary aliphatic amines in sludge from various urban and industrial sewage treatment plants as well as from a potable treatment plant. Most of the primary aliphatic amines were found in the sewage sludge samples analyzed corresponding to the maximum concentrations to the samples from the urban plant: for instance, isobutylamine and methylamine were found at 7728 and 12 536 μg/kg (d.w.), respectively. Amylamine was detected only in few samples but always at concentrations lower than its LOQ.

  15. A two-component mass balance model for calibration of solid-phase microextraction fibers for pyrethroids in seawater.

    PubMed

    Lao, Wenjian; Maruya, Keith A; Tsukada, David

    2012-11-06

    Determination of the analyte-specific distribution coefficient between the aqueous and sorbing phases is required for estimation of the aqueous-phase concentration of the analyte of interest using polymeric materials. Poly(dimethylsiloxane)-coated solid-phase microextration (PDMS-SPME) fiber-water partition coefficient (K(f)) values for eight common-use pyrethroids were determined using a two-compartment mass balance model and parameters determined in experimental seawater microcosms. Mass balance, epimerization, and aqueous-phase degradation (i.e., hydrolysis) were characterized using gas chromatography-negative chemical ionization mass spectrometry to facilitate K(f) estimation. Of the eight pyrethroids, only bifenthrin exhibited increasing sorption on the SPME fiber over the entire time-series exposure, indicating that its K(f) value could be estimated through a stable-compound model. The remaining pyrethroids were found to be unstable (half-life of <22 days), underscoring the importance of accounting for degradation in estimating K(f). The two-compartment model explained the experimental time-series data for bifenthrin (R(2) > 0.98) and the remaining unstable pyrethroids (R(2) > 0.7), leading to estimated values of log K(f) between 5.7 and 6.4, after correcting for residual dissolved organic carbon (DOC) in the experimental seawater. These K(f) values can be used to determine freely dissolved pyrethroid concentrations in the pg/L range using PDMS-SPME in fresh or seawater matrices under equilibrium conditions in laboratory or field applications.

  16. Immersed sol-gel based amino-functionalized SPME fiber and HPLC combined with post-column photochemically induced fluorimetry derivatization and fluorescence detection of pyrethroid insecticides from water samples.

    PubMed

    Bagheri, Habib; Ghanbarnejad, Hadi; Khalilian, Faezeh

    2009-09-01

    A method based on direct immersion solid-phase microextraction (DI-SPME) coupled with high performance liquid chromatography combined with post-column photochemically induced fluorimetry derivatization and fluorescence detection (HPLC-PIF-FD) was developed to extract three pyrethroid insecticides, i.e. cyfluthrin, cypermethrin, and flumethrin from water samples. A sol-gel based coating fiber using 3-(trimethoxysilyl propyl) amine as precursor was prepared and used for the extraction of the pyrethroids from groundwater samples. A post-column photochemical reactor was designed and constructed for the derivatization of these environmentally important pollutants to increase their fluorescence sensitivity and determination in HPLC. The parameters affecting extraction process (extraction time and temperature, pH, salt addition, and co-solvent) and desorption step (solvent, desorption time, and temperature) of the analytes from the sol-gel-based fiber, along with photochemical reaction conditions were investigated. The developed method proved to be relatively rapid, simple, and easy and offers high sensitivity and reproducibility. Linear dynamic ranges (LDR) for these insecticides were ranged between 0.25 to 50 microg/L. The regression coefficients were satisfactory (R(2) > 0.984) for these pyrethroids. The limits of detection and limits of quantification varied between 0.09 and 0.35 microg/L and 0.25 and 1.00 microg/L, respectively. Relative standard deviation RSDs values varied between 4.41% and 6.20%. Relative recoveries obtained from analysis of Jajroud river water sample ranged between 94% and 104%.

  17. Solid-phase microextraction (SPME) of drugs and poisons from biological samples.

    PubMed

    Junting, L; Peng, C; Suzuki, O

    1998-11-09

    Solid-phase microextraction (SPME), a new solvent-free sample preparation technique, was invented by C. Arthur and J. Pawliszyn in 1990. This method mainly was applied for the extraction of volatile and semi-volatile organic pollutants in water samples. However, since 1995, SPME has been developed to various biological samples, such as whole blood, plasma, urine, hair and breath, in order to extract drugs and poisons in forensic field. The main advantages of SPME are: high sensitivity, solventless, small sample volume, simplicity and rapidity. We have reviewed the papers published in recent years about SPME in biological samples, and sorted out main experimental conditions, such as fibers, matrixes, the extraction approaches and time, as well as the acceleration method. We would expect SPME technique to have a promising future for toxicological analysis in forensic practice.

  18. Solid phase microextraction fiber cleaning and conditioning apparatus and method

    DOEpatents

    Alcaraz, Armando; Wiefel, Michael H.

    2006-05-23

    A SPME-fiber cleaning and conditioning apparatus and method having an elongated heating chamber with first and second opposite ends. The first end is capable of insertably receiving a SPME fiber portion of a SPME device, and the second end is a fluid outlet. A heater is provided for heating the chamber and heat-treating an inserted SPME fiber. Contaminants and other particles are agitated, desorbed and purged from the inserted SPME fiber by flowing a fluid through the chamber from the first end to the second end, away from the SPME device. Additionally, turbulence may be produced in the flow at a location adjacent the first end, to enhance agitation, desorption, and purging. A holder may also be provided extending from the first end for supporting the SPME device in a substantially horizontal orientation when the SPME fiber is positioned in the chamber.

  19. Some applications of solid phase micro extraction (SPME) in the analysis of pesticide residues in food.

    PubMed

    Volante, M; Cattaneo, M; Bianchi, M; Zoccola, G

    1998-05-01

    The Solid Phase Micro-Extraction (SPME) technique was applied to analyze chlorpropham in potatoes and amitraz in honey. The homogenized sample, suspended in water and stirred, was extracted with a 100 microns thick polidimetylsiloxane fiber and desorbed into the injection port of a gas chromatograph/mass-spectrometer (quadrupole) operating in single ion monitoring. Sensitivities down to 0.01 mg/Kg and linear responses in the range of 0.01-0.1 mg/Kg were obtained. The results of SPME pesticide residue analysis in potatoes corresponded to those obtained with a traditional multiresidue method.

  20. SPME technique for analyzing headspace volatiles in fish miso, a Japanese fish meat-based fermented product.

    PubMed

    Giri, Anupam; Osako, Kazufumi; Ohshima, Toshiaki

    2010-01-01

    The optimized conditions were evaluated for solid-phase microextraction (SPME) to investigate the headspace volatiles in fish miso, a Japanese fish meat-based fermented product. The influence on the efficiency for microextraction of such parameters as the sample size, isolation time and temperature, sensitivity and selectivity of several SPME fibers of different liquid phases as well as several extraction techniques was evaluated. Suitable reproducibility and sensitivity of SPME were achieved by combining carbowax/divenylbenzene of 65 µm thickness as the liquid phase of SPME, 3 g of fish miso, 40 °C of isolation temperature and 40 min of isolation time. The headspace volatiles of fish miso prepared from spotted mackerel were analyzed under the optimized conditions. Although several volatiles contributed to fish miso, certain volatile esters might have played the greatest role in imparting the sweet-fruity aroma to the product.

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

    PubMed

    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.

  2. HS-SPME determination of volatile carbonyl and carboxylic compounds in different matrices.

    PubMed

    Stashenko, Elena E; Mora, Amanda L; Cervantes, Martha E; Martínez, Jairo R

    2006-07-01

    Specific chromatographic methodologies are developed for the analysis of carboxylic acids (C(2)-C(6), benzoic) and aldehydes (C(2)-C(10)) of low molecular weight in diverse matrices, such as air, automotive exhaust gases, human breath, and aqueous matrices. For carboxylic acids, the method is based on their reaction with pentafluorobenzyl bromide in aqueous solution, followed by the separation and identification of the resultant pentafluorobenzyl esters by means of headspace (HS)-solid-phase microextraction (SPME) combined with gas chromatography (GC) and electron capture detection (ECD). Detection limits in the microg/m(3) range are reached, with relative standard deviation (RSD) less than 10% and linear response (R(2) > 0.99) over two orders of magnitude. The analytical methodology for aldehydes is based on SPME with simultaneous derivatization of the analytes on the fiber, by reaction with pentafluorophenylhydrazine. The derivatization reagent is previously deposited on the SPME fiber, which is then exposed to the gaseous matrix or the HS of the sample solution. The pentafluorophenyl hydrazones formed on the fiber are analyzed selectively by means of GC-ECD, with detection limits in the ng/m(3) range, RSD less than 10%, and linear response (R(2) > 0.99) over two orders of magnitude.

  3. GC-MS and GC-NPD Determination of Formaldehyde Dimethylhydrazone in Water Using SPME.

    PubMed

    Kenessov, Bulat; Sailaukhanuly, Yerbolat; Koziel, Jacek A; Carlsen, Lars; Nauryzbayev, Mikhail

    2011-01-01

    Formaldehyde dimethylhydrazone (FADMH) is one of the important transformation products of residual rocket fuel 1,1-dimethylhydrazine (1,1-DMH). Thus, recent studies show that FADMH toxicity is comparable to that of undecomposed 1,1-DMH. In this study, a new method for quantification of FADMH in water based on solid phase microextraction (SPME) in combination with gas chromatography (GC) with mass spectrometric (MS) and nitrogen-phosphorus detection (NPD) is presented. Effects of SPME fiber coating type, extraction and desorption temperatures, extraction time, and pH on analyte recovery were studied. The optimized method used 65 micron polydimethylsiloxane/divinylbenzene fiber coating for 1 min headspace extractions at 30 °C. Preferred pH and desorption temperature from the SPME fiber are >8.5 and 200 °C, respectively. Detection limits were estimated to be 1.5 and 0.5 μg L(-1) for MS and NPD, respectively. The method was applied to laboratory-scale experiments to quantify FADMH. Results indicate applicability for in situ sampling and analysis and possible first-time detection of free FADMH in water.

  4. GC–MS and GC–NPD Determination of Formaldehyde Dimethylhydrazone in Water Using SPME

    PubMed Central

    Sailaukhanuly, Yerbolat; Koziel, Jacek A.; Carlsen, Lars; Nauryzbayev, Mikhail

    2011-01-01

    Formaldehyde dimethylhydrazone (FADMH) is one of the important transformation products of residual rocket fuel 1,1-dimethylhydrazine (1,1-DMH). Thus, recent studies show that FADMH toxicity is comparable to that of undecomposed 1,1-DMH. In this study, a new method for quantification of FADMH in water based on solid phase microextraction (SPME) in combination with gas chromatography (GC) with mass spectrometric (MS) and nitrogen-phosphorus detection (NPD) is presented. Effects of SPME fiber coating type, extraction and desorption temperatures, extraction time, and pH on analyte recovery were studied. The optimized method used 65 micron polydimethylsiloxane/divinylbenzene fiber coating for 1 min headspace extractions at 30 °C. Preferred pH and desorption temperature from the SPME fiber are >8.5 and 200 °C, respectively. Detection limits were estimated to be 1.5 and 0.5 μg L−1 for MS and NPD, respectively. The method was applied to laboratory-scale experiments to quantify FADMH. Results indicate applicability for in situ sampling and analysis and possible first-time detection of free FADMH in water. PMID:21423319

  5. Electrospun polyamide-polyethylene glycol nanofibers for headspace solid-phase microextration.

    PubMed

    Bagheri, Habib; Najarzadekan, Hamid; Roostaie, Ali

    2014-07-01

    A solution of polyamide (PA) containing polyethylene glycol (PEG) as a side low-molecular-weight polymer was electrospun. After synthesizing the PA-PEG nanofibers, the constituent was subsequently removed (modified PA) and confirmed by Fourier transform infrared spectroscopy. The scanning electron microscopy images showed an average diameter of 640 and 148 nm for PA and PA-PEG coatings, respectively, while the latter coating structure was more homogeneous and porous. The extraction efficiencies of PA, PA-PEG, and the modified PA fiber coatings were assayed by headspace solid-phase microextraction of a number of chlorophenols from real water samples followed by their determination by gas chromatography with mass spectrometry. To prepare the most appropriate coatings, the amounts and the flow rate of the electrospinning solution were investigated. Various extraction parameters, such as the salt content, desorption condition, extraction temperature, and time were optimized. The limits of detection of the method were in the range of 0.8-25 ng/L, while the RSDs at two concentration levels of 200 and 80 ng/L were between 2.1 and 12.2%. The analysis of real water samples led to relative recoveries between 85 and 98% with a linearity of 8-1500 ng/L.

  6. Characterization of an urban landfill soil by using physicochemical analysis and solid phase microextraction (SPME)-GC/MS.

    PubMed

    Banar, Müfide; Ozkan, Aysun; Vardar, Ciğdem

    2007-04-01

    We have aimed at characterizing top soil samples taken in-situ from five different locations of the unregulated dumping site in Eskişehir/Turkey for a period of six months. The study is the first attempt in the city and in Turkey, regarding particularly the SPME (Solid Phase Microextraction Technique) analysis method utilized. A comprehensive research has been conducted to produce critical soil data to be used for indicating current risks as well as the urgency of rehabilitating the site and establishing a sanitary landfill in the site. Conventional physicochemical analytical methods and SPME technique were used to analyze the samples. Physicochemical analyses were performed for determining the pH, total dried matter, volatile matter, total nitrogen, phosphorus, macro elements and heavy metals. Meteorological data were also recorded for the same period. SPSS.10.0 statistical program was used to determine the correlation between meteorological data and physicochemical analysis results. Mean values were used in the correlation analyses. These data indicated that the air temperature and precipitation have significant effects on soil characteristics. SPME, coupled with GC/MS, was used to identify eighty six volatile and semi-volatile organic compounds contained in soil samples. The samples were extracted by headspace SPME with heating (DeltaHS-SPME). SPME analyses were conducted using a commercially available polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber having a film thickness of 65 microm (Supelco) as a capture medium. The experimentally optimized headspace sampling conditions were arranged (15 min. at 50 degrees C) before a 30 min. sampling period.

  7. Headspace solid-phase microextraction (HS-SPME) for the determination of benzene, toluene, ethylbenzene, and xylenes (BTEX) in foundry molding sand

    SciTech Connect

    Dungan, R.S.

    2005-07-01

    The use of headspace solid-phase microextraction (HS-SPME) to determine benzene, toluene, ethylbenzene, and xylenes (BTEX) in foundry molding sand, specifically a 'green sand' (clay-bonded sand) was investigated. The BTEX extraction was conducted using a 75 {mu} M carboxen-polydimethylsiloxane (CAR-PDMS) fiber, which was suspended above 10 g of sample. The SPME fiber was desorbed in a gas chromatograph injector port (280{sup o}C for 1 min) and the analytes were characterized by mass spectrometry. The effects of extraction time and temperature, water content, and clay and bituminous coal percentage on HS-SPME of BTEX were investigated. Because green sands contain bentonite clay and carbonaceous material such as crushed bituminous coal, a matrix effect was observed. The detection limits for BTEX were determined to be {lt}= 0.18 ng g{sup -1} of green sand.

  8. Fiber

    MedlinePlus

    ... it can help with weight control. Fiber aids digestion and helps prevent constipation . It is sometimes used ... fiber attracts water and turns to gel during digestion. This slows digestion. Soluble fiber is found in ...

  9. Analysis of trihalomethanes in drinking water using headspace-SPME technique with gas chromatography.

    PubMed

    Cho, Deok-Hee; Kong, Sung-Ho; Oh, Seong-Geun

    2003-01-01

    In many drinking water treatment plants, the chlorination process is one of the main techniques used for the disinfection of water. This disinfecting treatment leads to the formation of trihalomethanes (THMs) such as chloroform, dichlorobromomethane, chlorodibromomethane and bromoform. In this study, headspace-solid-phase microextraction (HS-SPME, 85 microm carboxen/polydimethylsiloxane fiber) technique was applied for the analysis of THMs in drinking water. The effects of experimental parameters such as kinds of SPME fiber, the volume ratio of sample to headspace, the addition of salts, magnetic stirring, extraction temperature, extraction time and desorption time on the analysis were investigated. Analytical parameters such as linearity, repeatability and limit of detection were also evaluated. The results of THMs from the survey of Seongnam (Korea) drinking water samples showed that the highest total trihalomethane and chloroform were 24.03 and 13.34 microg/l, which were well within the Korean drinking water quality standard of 100 and 80 microg/l, respectively.

  10. Transport of explosives II: use of headspace-SPME/GC μ-ECD and TEEM GC/MS for detection of TNT vapors from sand buried samples

    NASA Astrophysics Data System (ADS)

    Baez, Bibiana; Correa, Sandra N.; Hernandez-Rivera, Samuel P.

    2005-06-01

    The detection of hidden explosives using vapors emanating from explosives has been considered an area in explosives technology that requires high sensitivity and selectivity. In this work is reported the results of two methods for vapor explosive detection, GC-μECD and GC/MS coupled to a Tunable Electron Energy Monochromator (TEEM-GC/MS). Both used Solid Phase Microextraction (SPME) in Headspace (HS) mode to collect vapors above the samples. Optimum parameters for SPME were determined with the purpose of obtaining a high-quality extraction. The parameters were: type of SPME fiber, exposure time and desorption time at the injection port of the GC. Headspace SPME procedure was carried out in samples with crystals of TNT buried in soil. These samples were analyzed under important environmental conditions such as temperature and water content. Analyses at contact times after the TNT-soil mix preparation were carried out during 1 month. A comparison of results from both techniques was performed. Vapors of TNT and 2,4-DNT were found predominantly in the samples. HS-SPME coupled with GC-μ ECD and TEEM GC/MS exhibited excellent selectivity and sensitivity.

  11. Microcrystalline cellulose based matrix solid phase dispersion microextration for isomeric triterpenoid acids in loquat leaves by ultrahigh-performance liquid chromatography and quadrupole time-of-flight mass spectrometry.

    PubMed

    Cao, Jun; Peng, Li-Qing; Xu, Jing-Jing

    2016-11-11

    An analytical procedure based on matrix solid phase dispersion (MSPD) microextration and ultrahigh-performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry was developed for the determination of isomeric triterpenoid acids (maslinic acid, corosolic acid, oleanolic acid and ursolic acid) in loquat leaves. Microcrystalline cellulose was used for the first time as a solid sorbent in MSPD microextration. Compared with the traditional extraction methods, the proposed method possessed the advantages of shorter extraction time, and lower consumption of sample, sorbent and organic solvent. The MSPD parameters that influenced the extraction efficiency of isomeric analytes were investigated and optimized in detail. Under the optimized conditions, good linearity was obtained with correlation coefficients higher than 0.9990. The limits of detection and quantification were 19.6-51.6μg/kg and 65.3-171.8μg/kg, respectively. Meanwhile, the recoveries obtained for all the analytes were ranging from 90.1% to 107.5%. Finally, the optimized method was successfully applied for analyzing these isomeric acids in loquat leaves samples obtained from different cultivated areas.

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

    PubMed

    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.

  13. Syntactic Polysulfide Degradation Observed by SPME GC/MS

    SciTech Connect

    Vance, A L; Alviso, C; Harvey, C; Saab, A

    2005-03-09

    We have utilized SPME GC/MS to monitor the degradation of syntactic polysulfide in the presence of Viton A at elevated temperature. This approach allowed the identification of products from two distinct degradation mechanisms. Small-scale laboratory experiments of this type are directly applicable to gas sampling for enhanced surveillance.

  14. Recent Applications of SPME in Directed Stockpile Work (FY04)

    SciTech Connect

    Alviso, C; Harvey, C; Vance, A

    2004-11-08

    Solid Phase Microextraction (SPME) has been used to sample nonnuclear materials for analysis by gas chromatography-mass spectrometry (GC/MS). This report summarizes progress in the areas of individual materials' outgassing signatures, microcompatibility tests and analysis of polar analytes.

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

    PubMed

    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.

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

    PubMed

    Kenessov, Bulat N; Koziel, Jacek A; Grotenhuis, Tim; Carlsen, Lars

    2010-07-26

    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 parameters were studied to optimize analyte recovery. It was found that the 85 microm Carboxen/polydimethylsiloxane fiber coating provides the highest selectivity for selected UDMH transformation products. Optimal sampling/sample preparation parameters were determined to be 1-h soil headspace sampling time at 40 degrees C. The GC inlet temperature was optimized to 170 degrees C held for 0.1 min, then 1 degrees C s(-1) ramp to 250 degrees C where it was held for 40 min. Temperature programming resulted in a fast desorption along with minimal chemical transformation in the GC inlet. SPME was very effective extracting UDMH transformation products from soil samples contaminated with rocket fuel. The use of SPME resulted in high sensitivity, speed, small labor consumption due to an automation and simplicity of use. It was shown that water addition to soil leads to a significant decrease of recovery of almost all target transformation products of UDMH. The use of SPME for sampling and sample preparation resulted in detection of the total of 21 new compounds that are relevant to the UDMH transformation in soils. In addition, the number of confirmed transformation products of UDMH increased from 15 to 27. This sampling/sample preparation approach can be recommended for environmental assessment of soil samples from areas affected by space rocket activity.

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

    PubMed

    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.

  18. A passive sampler based on solid phase microextraction (SPME) for sediment-associated organic pollutants: Comparing freely-dissolved concentration with bioaccumulation.

    PubMed

    Maruya, Keith A; Lao, Wenjian; Tsukada, David; Diehl, Dario W

    2015-10-01

    The elevated occurrence of hydrophobic organic chemicals (HOCs) such as polycyclic aromatic hydrocarbons (PAH), polychlorinated biphenyls (PCBs) and legacy organchlorine pesticides (e.g. chlordane and DDT) in estuarine sediments continues to poses challenges for maintaining the health of aquatic ecosystems. Current efforts to develop and apply protective, science-based sediment quality regulations for impaired waterbodies are hampered by non-concordance between model predictions and measured bioaccumulation and toxicity. A passive sampler incorporating commercially available solid phase microextraction (SPME) fibers was employed in lab and field studies to measure the freely dissolved concentration of target HOCs (Cfree) and determine its suitability as a proxy for bioaccumulation. SPME deduced Cfree for organochlorines was highly correlated with tissue concentrations (Cb) of Macoma and Nereis spp. co-exposed in laboratory microcosms containing both spiked and naturally contaminated sediments. This positive association was also observed in situ for endemic bivalves, where SPME samplers were deployed for up to 1 month at an estuarine field site. The concordance between Cb and Cfree for PAH was more variable, in part due to likely biotransformation by model invertebrates. These results indicate that SPME passive samplers can serve as a proxy for bioaccumulation of sediment-associated organochlorines in both lab and field studies, reducing the uncertainty associated with model predictions that do not adequately account for differential bioavailability.

  19. Liquid-phase microextration combined with liquid chromatography-electrospray tandem mass spectrometry for detecting diuretics in urine.

    PubMed

    Tsai, Tzu-Feng; Lee, Maw-Rong

    2008-05-15

    Trace amounts of diuretics were determined in human urine by hollow fiber liquid-phase microextraction (LPME) combined with liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) in this study. Chromatography was performed on a C(8) reversed-phase column. A 25 microL n-octanol was used to extract analytes in urine. Extraction was optimized using a pH 2 solution spiked with 0.15 g/mL NaCl for 40 min at 40 degrees C with 1010 rpm stirring. The limits of detection of diuretics in urine were 0.3-6.8 ng/mL, and linearity range was 1-1000 ng/mL. Recoveries of spiked 50 ng/mL diuretics were 97.7-102.5%. The intra-day precision and inter-day precision were 3-18% and 4-21%, respectively. The diuretics concentration profiles in patient urine were also determined. The results of this study reveal the adequacy of LPME-LC-MS/MS method for analyzing diuretics in urine and quantification limits exceed World Anti-Doping Agency requirements.

  20. Preparation of polypyrrole composite solid-phase microextraction fiber coatings by sol-gel technique for the trace analysis of polar biological volatile organic compounds.

    PubMed

    Zhang, Zhuomin; Zhu, Li; Ma, Yunjian; Huang, Yichun; Li, Gongke

    2013-02-21

    Two novel polypyrrole (PPy) composite solid-phase microextraction (SPME) fiber coatings involving polypyrrole β-naphthalenesulfonic acid (PPy/β-NSA) and polypyrrole graphene (PPy/GR) composite SPME fiber coatings were prepared by a simple sol-gel technique for selectively sampling relatively polar biological volatile organic compounds (VOCs). Crucial preparation conditions of the PPy composite SPME fiber coatings were optimized and are discussed in detail. Physical tests suggested that the PPy composite SPME fiber coatings possessed a porous surface morphology, stable chemical and thermal properties. Due to the inducing polar functional groups in the PPy molecule, the PPy composite SPME fiber coatings achieved a higher extraction capacity and special selectivity for the polar biological VOCs with conjugate structures, compared with commercial SPME fiber coatings. Enrichment factors of most of the VOCs by the PPy/β-NSA and PPy/GR SPME fibers were much higher than those achieved by common commercially available SPME fiber coatings. Finally, the PPy/β-NSA and PPy/GR SPME fiber coatings were applied for the trace analysis of typical polar VOCs from ant and coriander samples coupled with gas chromatography/mass spectrometry (GC/MS) detection, respectively. It was satisfactory that the average contents of 4-heptanone, 4-heptanol, 4-nonanone and methyl 5-methylsalicylate from ant samples were actually found to be 28.0, 58.7, 3.0 and 0.6 μg g(-1), and the average contents of nonane, decanal, undecanal and dodecanal from coriander samples were actually found to be 0.79, 0.13, 0.06 and 0.21 μg g(-1). The results suggested that PPy composite SPME coatings will be a potentially excellent sampling technique for the trace analysis of polar biological VOCs.

  1. Solid Phase Micro-extraction (SPME) with In Situ Transesterification: An Easy Method for the Detection of Non-volatile Fatty Acid Derivatives on the Insect Cuticle.

    PubMed

    Kühbandner, Stephan; Ruther, Joachim

    2015-06-01

    Triacylglycerides (TAGs) and other non-volatile fatty acid derivatives (NFADs) occur in large amounts in the internal tissues of insects, but their presence on the insect cuticle is controversially discussed. Most studies investigating cuticular lipids of insects involve solvent extraction, which implies the risk of extracting lipids from internal tissues. Here, we present a new method that overcomes this problem. The method employs solid phase micro-extraction (SPME) to sample NFADs by rubbing the SPME fiber over the insect cuticle. Subsequently, the sampled NFADs are transesterified in situ with trimethyl sulfonium hydroxide (TMSH) into more volatile fatty acid methyl esters (FAMEs), which can be analyzed by standard GC/MS. We performed two types of control experiments to enable significant conclusions: (1) to rule out contamination of the GC/MS system with NFADs, and (2) to exclude the presence of free fatty acids on the insect cuticle, which would also furnish FAMEs after TMSH treatment, and thus might simulate the presence of NFADs. In combination with these two essential control experiments, the described SPME technique can be used to detect TAGs and/or other NFADs on the insect cuticle. We analyzed six insect species from four insect orders with our method and compared the results with conventional solvent extraction followed by ex situ transesterification. Several fatty acids typically found as constituents of TAGs were detected by the SPME method on the cuticle of all species analyzed. A comparison of the two methods revealed differences in the fatty acid compositions of the samples. Saturated fatty acids showed by trend higher relative abundances when sampled with the SPME method, while several minor FAMEs were detected only in the solvent extracts. Our study suggests that TAGs and maybe other NFADs are far more common on the insect cuticle than usually thought.

  2. Monolithic graphene fibers for solid-phase microextraction.

    PubMed

    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.

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

    PubMed

    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.

  4. Fiber-based solid phase microextraction using fused silica lined bottles to collect, store, and stabilize a multianalyte headspace gas sample for offline analyses.

    PubMed

    Harvey, Chris A; Carter, J Chance; Ertel, John R; Alviso, Cindy T; Chinn, Sarah C; Maxwell, Robert S

    2015-07-03

    We have developed a solid phase microextraction (SPME) sampling method using fused silica lined bottles (400 ml) to collect, store, and stabilize a headspace subsample from the source for subsequent offline, repetitive analyses of the gas using fiber-based SPME. The method enables long-term stability for repeated offline analysis of the organic species collected from the source headspace and retains all the advantages of fiber SPME sampling (e.g. rapid extraction, solvent free, simple and inexpensive) while providing additional advantages. Typically, the analytes collected on the SPME fiber must be desorbed and analyzed immediately to mitigate analyte loss or contamination. The new SPME sampling method, conducted offline using carboxen/polydimethylsiloxane (carboxen/PDMS - 85 μm) coated fibers, has been shown to be identical to in situ SPME sampling of a headspace acquired from an 80 component organic matrix with reproducibility demonstrated to be less than %RSD=7.0% for replicate samples measured over a 30-day period. In addition, repetitive samplings from one headspace aliquot are possible using one or more fibers and fiber types as well as quantitative options such as internal standard addition as demonstrated in a feasibility study using a benzene/toluene/xylene (BTX; 1 ppmv) certified gas standard, in which the SPME measurement precision (%RSD) was improved by a factor of 1.5-1.9 compared to the use of an external standard.

  5. Cold fiber solid-phase microextraction device based on thermoelectric cooling of metal fiber.

    PubMed

    Haddadi, Shokouh Hosseinzadeh; Pawliszyn, Janusz

    2009-04-03

    A new cold fiber solid-phase microextraction device was designed and constructed based on thermoelectric cooling. A three-stage thermoelectric cooler (TEC) was used for cooling a copper rod coated with a poly(dimethylsiloxane) (PDMS) hollow fiber, which served as the solid-phase microextraction (SPME) fiber. The copper rod was mounted on a commercial SPME plunger and exposed to the cold surface of the TEC, which was enclosed in a small aluminum box. A heat sink and a fan were used to dissipate the generated heat at the hot side of the TEC. By applying an appropriate dc voltage to the TEC, the upper part of the copper rod, which was in contact to the cold side of the TEC, was cooled and the hollow fiber reached a lower temperature through heat transfer. A thermocouple was embedded in the cold side of the TEC for indirect measurement of the fiber temperature. The device was applied in quantitative analysis of off-flavors in a rice sample. Hexanal, nonanal, and undecanal were chosen as three off-flavors in rice. They were identified according to their retention times and analyzed by GC-flame ionization detection instrument. Headspace extraction conditions (i.e., temperature and time) were optimized. Standard addition calibration graphs were obtained at the optimized conditions and the concentrations of the three analytes were calculated. The concentration of hexanal was also measured using a conventional solvent extraction method (697+/-143ng/g) which was comparable to that obtained from the cold fiber SPME method (644+/-8). Moreover, the cold fiber SPME resulted in better reproducibility and shorter analysis time. Cold fiber SPME with TEC device can also be used as a portable device for field sampling.

  6. Assessment of SPME Partitioning Coefficients: Implications for Passive Environmental Sampling of Hydrophobic Organic Compounds

    NASA Astrophysics Data System (ADS)

    Difilippo, E. L.; Eganhouse, R. P.

    2009-12-01

    Solid-phase microextraction (SPME) has shown potential as an in situ passive sampling technique in aqueous environments. The reliability of this method depends upon accurate determination of the partitioning coefficient between the fiber coating and water (Kf) for the compounds of interest. Kf values for poly(dimethylsiloxane) (PDMS) and water spanning 4 orders of magnitude have been reported for hydrophobic organic compounds (HOCs). However, most of the published data (86%) do not pass the criterion for negligible depletion (Vw > 100KfVf , where Vw is the sample volume [μl] and Vf is the fiber coating volume [μl]), resulting in erroneous Kf values. The range in reported Kf values is reduced to just over 2 orders of magnitude for some polychlorinated biphenyls (PCBs) when these erroneous values are removed. We conducted a two-tailed t-test comparing Kf values for the same compounds (polycyclic aromatic hydrocarbons (PAHs) and PCBs) measured with different fiber coating thicknesses and fiber manufacturers; the majority (85%) of these Kf values are not statistically different (p = 0.10). In addition to an accurate measurement of Kf, the impact of environmental factors on partitioning, such as temperature and ionic strength, are essential in applying laboratory-measured Kf values to field samples. To date, few studies have measured Kf at conditions other than at 25° C in distilled water. While the available data indicate slight differences in Kf at different temperatures and ionic strength, the data are too limited to make an accurate assessment of the impact of these factors on the accuracy of in situ concentration measurements. Because of the challenges in measuring Kf for HOCs, it may be useful to develop predictive models for calculating Kf using known or measured physico-chemical properties. A multi-parameter linear solvation energy relationship (LSER) was developed to estimate Kf in distilled water at 25° C for HOCs based on published physico

  7. Preparation of temperature sensitive molecularly imprinted polymer for solid-phase microextraction coatings on stainless steel fiber to measure ofloxacin.

    PubMed

    Zhao, Tong; Guan, Xiujuan; Tang, Wanjin; Ma, Ying; Zhang, Haixia

    2015-01-01

    A kind of new temperature sensitive molecularly imprinted polymer (MIP) with ofloxacin (OFL) as template was prepared for the coating of solid phase microextraction (SPME). Dopamine was self-polymerized on stainless steel fiber (SSF) as the SPME support followed by silanization. Then MIP was synthesized as SPME coating on the modified SSF in a capillary, with N-isopropyl acrylamide as temperature sensitive monomer and methacrylic acid as functional monomer. The synthesis could be well repeated with multiple capillaries putting in the same reaction solution. The obtained MIP fiber was evaluated in detail with different techniques and various adsorption experiments. At last the MIP fiber was used to extract the OFL in milk. Satisfied recoveries between 89.7 and 103.4% were obtained with the limit of quantification (LOQLC) of 0.04 μg mL(-1) by the method of SPME coupled with high performance of liquid chromatography (HPLC).

  8. Non-invasive characterization of the adipogenic differentiation of human bone marrow-derived mesenchymal stromal cells by HS-SPME/GC-MS

    PubMed Central

    Lee, Dong-Kyu; Yi, TacGhee; Park, Kyung-Eun; Lee, Hyun-Joo; Cho, Yun-Kyoung; Lee, Seul Ji; Lee, Jeongmi; Park, Jeong Hill; Lee, Mi-Young; Song, Sun U.; Kwon, Sung Won

    2014-01-01

    A non-invasive method to characterize human mesenchymal stromal cells during adipogenic differentiation was developed for the first time. Seven fatty acid methyl esters (FAMEs), including methyl laurate, methyl myristate, methyl palmitate, methyl linoleate, methyl oleate, methyl elaidate and methyl stearate, were used for characterizing adipogenic differentiation using headspace solid-phase microextraction (HS-SPME) which is a very simple and non-invasive method for the extraction of volatile compounds. Glassware was used for culturing mesenchymal stromal cells rather than the common plasticware to minimize contamination by volatile impurities. The optimal SPME fiber was selected by comparing diverse fibers containing two pure liquid polymers (PDMS and PA) and two porous solids (PDMS/DVB and CAR/PDMS). Using optimized procedures, we discovered that seven FAMEs were only detected in adipogenic differentiated mesenchymal stromal cells and not in the mesenchymal stromal cells before differentiation. These data could support the quality control of clinical mesenchymal stromal cell culture in the pharmaceutical industry in addition to the development of many clinical applications using mesenchymal stromal cells. PMID:25298091

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

    SciTech Connect

    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

  10. Preparation of novel alumina nanowire solid-phase microextraction fiber coating for ultra-selective determination of volatile esters and alcohols from complicated food samples.

    PubMed

    Zhang, Zhuomin; Ma, Yunjian; Wang, Qingtang; Chen, An; Pan, Zhuoyan; Li, Gongke

    2013-05-17

    A novel alumina nanowire (ANW) solid-phase microextraction (SPME) fiber coating was prepared by a simple and rapid anodization-chemical etching method for ultra-selective determination of volatile esters and alcohols from complicated food samples. Preparation conditions for ANW SPME fiber coating including corrosion solution concentration and corrosion time were optimized in detail for better surface morphology and higher surface area based on scanning electron microscope (SEM). Under the optimum conditions, homogeneous alumina nanowire structure of ANW SPME fiber coating was achieved with the average thickness of 20 μm around. Compared with most of commercial SPME fiber coatings, ANW SPME fiber coatings achieved the higher extraction capacity and special selectivity for volatile esters and alcohols. Finally, an efficient gas sampling technique based on ANW SPME fiber coating as the core was established and successfully applied for the ultra-selective determination of trace volatile esters and alcohols from complicated banana and fermented glutinous rice samples coupled with gas chromatography/mass spectrometry (GC/MS) detection. It was interesting that 25 esters and 2 alcohols among 30 banana volatile organic compounds (VOCs) identified and 4 esters and 7 alcohols among 13 identified VOCs of fermented glutinous rice were selectively sampled by ANW SPME fiber coatings. Furthermore, new analytical methods for the determination of some typical volatile esters and alcohols from banana and fermented glutinous rice samples at specific storage or brewing phases were developed and validated. Good recoveries for banana and fermented glutinous rice samples were achieved in range of 108-115% with relative standard deviations (RSDs) of 2.6-6.7% and 80.0-91.8% with RSDs of 0.3-1.3% (n=3), respectively. This work proposed a novel and efficient gas sampling technique of ANW SPME which was quite suitable for ultra-selectively sampling trace volatile esters and alcohols from

  11. Immersion mode SPME/μECD/GC and TEEM-GC/MS for analysis of explosives buried in sand

    NASA Astrophysics Data System (ADS)

    Correa, Sandra N.; Baez, Bibiana; de Jesus Echevarria, Maritza; Castro, Miguel E.; Briano, Julio; Hernandez-Rivera, Samuel P.

    2005-06-01

    The detection of trace amount of explosives is of utmost importance in many day-to-day military operations. Moreover, the detection of landmines is a complex and urgent worldwide problem, which needs specific, rapid and cost effective solutions. The most commonly used explosive in landmines is 2,4,6-trinitrotoluene (TNT). Almost 80% of the types of mines manufactured worldwide contain TNT. This contribution describes the use of Immersion Mode Solid-Phase Microextraction (I-SPME) for extraction of TNT and their degradation products from surface soil samples for subsequent analysis by either GC with 63Ni micro cell Electron Capture Detector or gas chromatograph-mass spectrometer coupled to a Tunable Electron Energy Monochromator. A pretreatment step was introduced for the soil samples which extracted the target compounds into an aqueous phase. The experimental results demonstrated the effects of controllable variables. Parameters studied include the chemical properties of the fiber coating, extraction and desorption times, fiber extraction and matrix effect. Surface soil samples containing TNT were evaluated to study the detection of the nitroaromatic explosives and its degradations products using different environmental conditions such as sample temperature, sample contact time and water content.

  12. Analysis of terpenes in white wines using SPE-SPME-GC/MS approach.

    PubMed

    Dziadas, Mariusz; Jeleń, Henryk H

    2010-09-10

    Terpenes contribute to some white wines aroma, especially these produced from Muscat grapes and others aromatic ones of high terpene contents (Gewürtztramminer, Traminer, Huxel, Sylvaner). Terpenes are present in wine in free and bound (in a form of glycosides) forms. Analyses of bound terpenes are usually performed using solid phase extraction after hydrolysis of glycosides. A new method for determination of terpenes from wine, focused on determination of terpenes released after acidic hydrolysis, based on solid phase extraction (SPE) followed by solid phase microextraction (SPME) was developed. Non-polar (free) and polar (bound terpenes) fractions were separated on 500 mg C18 cartridges. Bound terpenes were sampled using SPME immediately after acidic hydrolysis in non-equilibrium conditions. Application of combined SPE-SPME approach allowed quantification of selected terpenes in lower concentrations than in SPE approach and added a selectivity to the method, which enabled detection of compounds non-detectable in SPE extracts. Results obtained by SPE and SPE-SPME approach were correlated for free terpenes and those released after acid hydrolysis 20 white wines obtained from different grape varieties (R(2)=0.923). Although developed for wine terpenes analysis, SPE followed by SPME approach has a great potential in analysis of other bound wine flavor compounds, especially those potent odorants present in trace amounts.

  13. Determination of formaldehyde in Romanian cosmetic products using coupled GC/MS system after SPME extraction

    NASA Astrophysics Data System (ADS)

    Feher, I.; Schmutzer, G.; Voica, C.; Moldovan, Z.

    2013-11-01

    In this study we have made a quick review of some Romanian cosmetic products (shampoo, conditioner, face wash) in order to determine the formaldehyde content as well as other substances called "formaldehyde releasers". The process was performed based on solid-phase microextraction (SPME) followed by gas chromatography/mass spectrometry technique. Prior to SPME extraction we used a derivation step of formaldehyde using pentafluorophenyl hydrazine. The obtained product was adsorbed on SPME devices, then injected and desorbed into the GC/MS injection port. The concentration of formaldehyde (as derived compound) was calculated using calibration curve, having a regression coefficient of 0.9938. The performance parameters of the method were calculated using samples of standard concentration. The method proved to be sensitive, having a quantification limit (LOQ) of 0.15 μg/g.

  14. SPME-HPLC: a new approach to the analysis of explosives.

    PubMed

    Gaurav; Kaur, Varinder; Kumar, Ashwini; Malik, Ashok Kumar; Rai, P K

    2007-08-25

    Methods developed for the analysis of explosives by SPME coupled to HPLC are reviewed with special emphasis on determination and monitoring in environmental samples such as soil and water. Analysis of explosives by using SPME-HPLC as analytical technique is comparatively a new method on which a special attention is focused nowadays. It saves time, avoid use of hazardous extraction solvents, disposal costs and consequently improve the detection limits. The application of SPME is also widened for explosives by using modified 10-port interface and a C-8 refocusing unit combined with two pumps. Several parameters have been optimized to ensure quantitative results such as high concentration of salt and less acetonitrile:water ratio. CW/PDMS/DVB coatings were found to be superior over PA in terms of sensitivity.

  15. Odor active compounds content in spices and their microencapsulated powders measured by SPME.

    PubMed

    Wojtowicz, Elżbieta; Zawirska-Wojtasiak, Renata; Adamiec, Janusz; Wąsowicz, Erwin; Przygoński, Krzysztof; Remiszewski, Marian

    2010-10-01

    Within this study, main odorants of marjoram and thyme (linalool and thymol) were determined in spices and microencapsulated powders using solid-phase microextraction (SPME). Analyses were conducted on selected batches of spices before and after decontamination and on microencapsulated powders prepared for technological purposes (improvement of aroma in decontaminated spices). Conditions of SPME analyses were determined for individual compounds and matrices. Determination of total and surface contents of compounds and the percentage dependencies between encapsulated and surface aroma made it possible to identify the best powders in terms of their quality.

  16. Passive sampling of ambient ozone by solid phase microextraction with on-fiber derivatization.

    PubMed

    Lee, I-Su; Tsai, Shih-Wei

    2008-03-10

    The solid phase microextraction (SPME) device with the polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber was used as a passive sampler for ambient ozone. Both O-2,3,4,5,6-(pentafluorobenzyl)hydroxylamine hydrochloride (PFBHA) and 1,2-di-(4-pyridyl)ethylene (DPE) were loaded onto the fiber before sampling. The SPME fiber assembly was then inserted into a PTFE tubing as a passive sampler. Known concentrations of ozone around the ambient ground level were generated by a calibrated ozone generator. Laboratory validations of the SPME passive sampler with the direct-reading ozone monitor were performed side-by-side in an exposure chamber at 25 degrees C. After exposures, pyriden-4-aldehyde was formed due to the reaction between DPE and ozone. Further on-fiber derivatizations between pyriden-4-aldehyde and PFBHA were followed and the derivatives, oximes, were then determined by portable gas chromatography with electron capture detector. The experimental sampling rate of the SPME ozone passive sampler was found to be 1.10 x 10(-4) cm(3) s(-1) with detection limit of 58.8 microg m(-3) h(-1). Field validations with both SPME device and the direct-reading ozone monitor were also performed. The correlations between the results from both methods were found to be consistent with r=0.9837. Compared with other methods, the current designed sampler provides a convenient and sensitive tool for the exposure assessments of ozone.

  17. Development of a new SPME-HPLC-UV method for the analysis of nitro explosives on reverse phase amide column and application to analysis of aqueous samples.

    PubMed

    Gaurav; Malik, Ashok Kumar; Rai, P K

    2009-12-30

    A rapid, simple, sensitive and accurate quantitative method has been developed for the determination of eleven nitroaromatic components by solid phase microextraction (SPME) coupled to high performance liquid chromatography (HPLC) with UV detection from aqueous samples. PDMS/DVB resin fiber (60 microm) was used for concurrent extraction of all the analytes from aqueous matrix. Static desorption was carried out in the desorption chamber of SPME-HPLC interface containing mobile phase; methanol:water 43:57 (v/v) with subsequent liquid chromatographic analysis at isocratic flow rate of 1.3 mL/min and detection at 254 nm. A reverse phase amide column (5 microm) was used as a separation medium. The limit of detection (S/N=3) for TNT and Tetryl was found to be 0.35 and 0.54 ng/mL, respectively. Developed method has been applied successfully to the analysis of aqueous samples obtained from environmental and industrial sources like river water, ground water, drinking water and industrial waste water.

  18. Discrimination of smokeless powders by headspace SPME-GC-MS and SPME-GC-ECD, and the potential implications upon training canine detection of explosives

    NASA Astrophysics Data System (ADS)

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

    2005-05-01

    This presentation will provide an odour analysis of a variety of smokeless powders & communicate the rapid SPME-GC-ECD method utilized. This paper will also discuss the implications of the headspace analysis of Smokeless Powders upon the choice of training aids for Explosives Detection Canines. Canine detection of explosives relies upon the dogs" ability to equate finding a given explosive odour with a reward, usually in the form of praise or play. The selection of explosives upon which the dogs are trained thus determines which explosives the canines can and potentially cannot find. Commonly, the training is focussed towards high explosives such as TNT and Composition 4, and the low explosives such as Black and Smokeless Powders are added often only for completeness. Powder explosives constitute a major component of explosive incidents throughout the US, and canines trained to detect explosives must be trained across the entire range of powder products. Given the variability in the manufacture and product make-up many smokeless powders do not share common odour chemicals, giving rise to concerns over the extensiveness of canine training. Headspace analysis of a selection of Smokeless Powders by Solid Phase Microextraction Gas Chromatography using Mass Spectrometry (SPME-GC-MS) and Electron Capture Detectors (SPME-GC-ECD) has highlighted significant differences in the chemical composition of the odour available from different brands. This suggests that greater attention should be paid towards the choice of Powder Explosives when assigning canine training aids.

  19. Magnetron sputtering Si interlayer: a protocol to prepare solid phase microextraction coatings on metal-based fiber.

    PubMed

    Liu, Hongmei; Ji, Li; Li, Jubai; Liu, Shujuan; Liu, Xia; Jiang, Shengxiang

    2011-05-20

    Use of metal fibers in solid phase microextraction (SPME) can overcome the fragility drawback of conventional fused-silica ones. However, the surface modification of metal substrates is rather difficult, which largely prevents many mature traditional techniques, such as sol-gel and chemical bonding, being used in fabrication of SPME coating on metal-based fibers. This study demonstrates a protocol to resolve this problem by magnetron sputtering a firm Si interlayer on stainless steel fiber. The Si interlayer was easily modified active group, and attached with a multiwalled carbon nanotubes (MWCNTs) coating using the reported approach. The as-prepared MWCNTs/Si/stainless steel wire fiber not only preserved the excellent SPME behaviors of MWCNTs coatings, but also exhibited a number of advantages including high rigidity, long service life, and good stability at high temperature, in acid and alkali solutions. This new surface modification technique might provide a versatile approach to prepare sorbent coatings on unconfined substrates using traditional methods.

  20. Characterization of Human Skin Emanations by Solid Phase Microextraction (SPME) Extraction of Volatiles and Subsequent Analysis by Gas Chromatography-Mass Spectrometry (GC-MS)

    DTIC Science & Technology

    2007-11-02

    1 Characterization of Human Skin Emanations by Solid Phase Microextraction (SPME) Extraction of Volatiles and Subsequent Analysis by Gas...DATES COVERED - 4. TITLE AND SUBTITLE Characterization of Human Skin Emanations by Solid Phase Microextraction (SPME) Extraction of Volatiles...3 Characterization of Human Skin Emanations by Solid Phase Microextraction (SPME) Extraction of Volatiles and Subsequent Analysis by Gas

  1. Headspace analysis of polar organic compounds in biological matrixes using solid phase microextraction (SPME)

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Analysis of biological fluids and waste material is difficult and tedious given the sample matrix. A rapid automated method for the determination of volatile fatty acids and phenolic and indole compounds was developed using a multipurpose sampler (MPS) with solid phase microextraction (SPME) and GC-...

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

    PubMed

    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.

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

    PubMed

    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.

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

    PubMed

    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.

  5. Determination of urinary ortho- and meta-cresol in humans by headspace SPME gas chromatography/mass spectrometry.

    PubMed

    Fustinoni, Silvia; Mercadante, Rosa; Campo, Laura; Scibetta, Licia; Valla, Carla; Foà, Vito

    2005-03-25

    ortho-Cresol (o-C) and meta-cresol (m-C) are minor urinary metabolites of toluene, a widely used chemical with neurotoxicological properties. A new assay for their determination in human urine is here proposed. Urinary cresol sulphates and glucuronates are submitted to acid hydrolysis, urine is neutralized, added with o-cresols-d8, and analytes are sampled in the headspace of urine by SPME using a polydimethylsiloxane fiber. Analysis is performed by GC/MS using, for separation, either a SupelcoWax10 (for o-C) or a chiral CP Cresol (for o-C and m-C) column. The method is very specific, with a range of linearity 0-5.0 mg/l, within- and between-run precision, as coefficient of variation, <15% and <19%, limit of detection of 0.006 mg/l for o-C and 0.007 mg/l for m-C. The procedure is applied to the quantification of cresols in urine from workers exposed to toluene and from subjects belonging to the general population.

  6. Graphenized pencil lead fiber: facile preparation and application in solid-phase microextraction.

    PubMed

    Liu, Qian; Cheng, Mengting; Long, Yanmin; Yu, Miao; Wang, Thanh; Jiang, Guibin

    2014-01-17

    Graphenized pencil lead fiber was facilely prepared by in situ chemical exfoliation of graphite in pencil lead fiber to few-layered graphene sheets via a one-pot, one-step pressurized oxidation reaction for the first time. This new fiber was characterized and demonstrated to be a highly efficient but low-cost solid-phase microextraction (SPME) fiber. The extraction performance of the fiber was evaluated with four bisphenol analogs [bisphenol A (BPA), bisphenol S (BPS), bisphenol AF (BPAF), and tetrabromobisphenol A (TBBPA)] as model analytes in direct SPME mode. Unlike commercially available fibers, the graphenized pencil lead fiber showed an excellent chemical stability in highly saline, acidic, alkaline and organic conditions due to its coating-free configuration. The fiber also showed a very long lifespan. Furthermore, high extraction efficiency and good selectivity for the analytes with a wide polarity range could be obtained due to the exceptional properties of graphene. The detection limits (LODs) for the analytes were in the range of 1.1-25ng/L. The fiber was successfully applied in the analysis of tap water and effluent samples from a waste water treatment plant with spike recoveries ranging from 68.5 to 105.1%. Therefore, the graphenized pencil lead fiber provides a high performance, cheap, robust, and reliable tool for SPME.

  7. Preparation and application of solid-phase microextraction fiber based on molecularly imprinted polymer for determination of anabolic steroids in complicated samples.

    PubMed

    Qiu, Lijun; Liu, Wei; Huang, Min; Zhang, Lan

    2010-11-26

    A relatively selective, chemically and physically robust SPME fiber was developed in a simple way with testosterone-imprinted polymer, and then directly coupled with gas chromatography-mass spectrometry (GC-MS) for selective extraction and analysis of anabolic steroids. The factors influencing polymerization (i.e., cross-linker, polymerization solvent, polymerization time) were optimized in detail and the polymer was characterized by scanning electron microscope, infrared spectrometer and thermogravimetric analyzer. Furthermore, the extraction performance of the MIP-coated SPME fibers such as extraction ability and selectivity was evaluated. Moreover, the interaction mode between target analytes and fiber coating was deducted. Finally, the method for extraction and determination of androsterone, stanolone, androstenedione and methyltestosterone by the homemade MIP-coated SPME fibers with GC-MS was obtained. It was applied to the simultaneous analysis of four anabolic steroids in the spiked human urine with the satisfactory recoveries.

  8. Molecularly imprinted calixarene fiber for solid-phase microextraction of four organophosphorous pesticides in fruits.

    PubMed

    Li, Jing-Wen; Wang, Yu-Long; Yan, Shan; Li, Xiu-Juan; Pan, Si-Yi

    2016-02-01

    Calixarene was used as a functional monomer to fabricate a molecularly imprinted polymer (MIP) by sol-gel technique for solid-phase microextraction (SPME) of parathion-methyl and its structural analogs. The MIP-coated fiber possessed excellent thermal and chemical stability as well as high extraction capacity. Its selectivity and possible recognition mechanism were investigated. The similarities in molecular shape and functional group play a key role in the selective recognition of the imprinted material. Any changes to the structure of the template would decrease the imprinting factor. A comparison of MIP-SPME was made with liquid-liquid extraction coupled with gas chromatography for the determination of organophosphorus pesticides (OPPs) in fruits. Much lower limits of detection and better recoveries were achieved by SPME in spiked apple and pineapple samples. The experiment demonstrates that the proposed method using the calixarene MIP fiber was more suitable for selective determination of trace OPPs in those fruit samples.

  9. A new polyethylene glycol fiber prepared by coating porous zinc electrodeposited onto silver for solid-phase microextraction of styrene.

    PubMed

    Sungkaew, Sakchaibordee; Thammakhet, Chongdee; Thavarungkul, Panote; Kanatharana, Proespichaya

    2010-04-01

    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 microm carboxen/polydimethylsiloxane (CAR/PDMS) and 100 microm 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).

  10. Prediction of partition coefficients of organic compounds between SPME/PDMS and aqueous solution.

    PubMed

    Chao, Keh-Ping; Lu, Yu-Ting; Yang, Hsiu-Wen

    2014-02-14

    Polydimethylsiloxane (PDMS) is commonly used as the coated polymer in the solid phase microextraction (SPME) technique. In this study, the partition coefficients of organic compounds between SPME/PDMS and the aqueous solution were compiled from the literature sources. The correlation analysis for partition coefficients was conducted to interpret the effect of their physicochemical properties and descriptors on the partitioning process. The PDMS-water partition coefficients were significantly correlated to the polarizability of organic compounds (r = 0.977, p < 0.05). An empirical model, consisting of the polarizability, the molecular connectivity index, and an indicator variable, was developed to appropriately predict the partition coefficients of 61 organic compounds for the training set. The predictive ability of the empirical model was demonstrated by using it on a test set of 26 chemicals not included in the training set. The empirical model, applying the straightforward calculated molecular descriptors, for estimating the PDMS-water partition coefficient will contribute to the practical applications of the SPME technique.

  11. Analysis of haloacetic acids in water and air (aerosols) from indoor swimming pools using HS-SPME/GC/ECD.

    PubMed

    Sá, Christopher S A; Boaventura, Rui A R; Pereira, Isabel B

    2012-01-01

    A solid phase microextraction method was used for the analysis of nine haloacetic acids (HAAs) in water and air (aerosols) from indoor swimming pools (ISPs). The analysis is characterized by derivatization of HAAs to their methyl-esters with dimethyl sulphate, headspace solid phase microextraction (HS-SPME) with a Carboxen-polydimethylsiloxane (CAR-PDMS) fiber and gas chromatography - electron capture detector (GC/ECD). High correlation coefficients were obtained for esters mixture calibration lines and detection limits were found to be at the low ppb level. Repeatability was assessed and coefficients of variation varied from 10 to 20%. Reproducibility was also evaluated and coefficients of variation from 15 to 25% were obtained. Analytical results from four Portuguese ISPs showed that the mean concentration of total HAAs (THAAs) in water ranged from 10 ± 2 to 183 ± 28 μg/L in which 55 ± 20% corresponded to trichloroacetic and dichloroacetic acids (TCAA and DCAA). THAAs highest concentrations were directly related to higher ISPs' water organic matter content. In the lack of European specific regulation for water from ISPs and taking into consideration that ingestion is a form of exposure, THAAs concentration values were compared with drinking water maximum contamination level (MCL) of 60 μg/L proposed by the US EPA for the sum of five HAAs. In 35% of water sampling campaigns the sum of MBAA (monobromoacetic acid), MCAA (monochloroacetic acid), DCAA and TCAA exceeded that MCL value. The concentrations obtained for THAAs in the ISPs' atmosphere ranged from 5 ± 1 to 64 ± 10 μg/m(3) (T = 28°C at 5 cm above the water surface) and were proportional to the aerosols' quantity, which was deeply related to indoor air ventilation system.

  12. Preparation of solid-phase microextraction fiber coated with single-walled carbon nanotubes by electrophoretic deposition and its application in extracting phenols from aqueous samples.

    PubMed

    Li, Quanlong; Wang, Xuefeng; Yuan, Dongxing

    2009-02-27

    A novel solid-phase microextraction (SPME) Pt fiber coated with single-walled carbon nanotubes (SWCNTs) was prepared by electrophoretic deposition (EPD) and applied to the determination of phenols in aqueous samples by direct immersion (DI)-SPME-HPLC-UV. The results revealed that EPD was a simple and reproducible technique for the preparation of SPME fibers coated with SWCNTs without the use of adhesive. The obtained SWCNT coating did not swell in organic solvents nor strip off from substrate, and possessed high mechanical strength due to the strong Van der Waals attractions between the surfaces of the SWCNTs. The prepared SPME fiber was conductive since both SWCNT coating and Pt wire were conductive. Using Pt wire as substrate, the fiber was unbreakable. Owing to the presence of oxygenated groups on SWCNTs and the high surface area of SWCNTs, the SWCNT fiber was similar to or superior to commercial PA fiber in extracting the studied phenols from aqueous sample. A durability of more than 80 analyses was achieved for one unique fiber. Under optimized conditions, the detection limits for the phenols varied between 0.9 and 3.8 ng/mL, the precisions were in the range of 0.7-3.2% (n=3), and linear ranges were within 10 and 300 ng/mL. The method was successfully applied to the analysis of spiked seawater and tap water samples with the recoveries from 87.5 to 102.0%.

  13. Development of the HS-SPME-GC-MS/MS method for analysis of chemical warfare agent and their degradation products in environmental samples.

    PubMed

    Nawała, Jakub; Czupryński, Krzysztof; Popiel, Stanisław; Dziedzic, Daniel; Bełdowski, Jacek

    2016-08-24

    After World War II approximately 50,000 tons of chemical weapons were dumped in the Baltic Sea by the Soviet Union under the provisions of the Potsdam Conference on Disarmament. These dumped chemical warfare agents still possess a major threat to the marine environment and to human life. Therefore, continue monitoring of these munitions is essential. In this work, we present the application of new solid phase microextraction fibers in analysis of chemical warfare agents and their degradation products. It can be concluded that the best fiber for analysis of sulfur mustard and its degradation products is butyl acrylate (BA), whereas for analysis of organoarsenic compounds and chloroacetophenone, the best fiber is a co-polymer of methyl acrylate and methyl methacrylate (MA/MMA). In order to achieve the lowest LOD and LOQ the samples should be divided into two subsamples. One of them should be analyzed using a BA fiber, and the second one using a MA/MMA fiber. When the fast analysis is required, the microextraction should be performed by use of a butyl acrylate fiber because the extraction efficiency of organoarsenic compounds for this fiber is acceptable. Next, we have elaborated of the HS-SPME-GC-MS/MS method for analysis of CWA degradation products in environmental samples using laboratory obtained fibers The analytical method for analysis of organosulfur and organoarsenic compounds was optimized and validated. The LOD's for all target chemicals were between 0.03 and 0.65 ppb. Then, the analytical method developed by us, was used for the analysis of sediment and pore water samples from the Baltic Sea. During these studies, 80 samples were analyzed. It was found that 25 sediments and 5 pore water samples contained CWA degradation products such as 1,4-dithiane, 1,4-oxathiane or triphenylarsine, the latter being a component of arsine oil. The obtained data is evidence that the CWAs present in the Baltic Sea have leaked into the general marine environment.

  14. On-fiber furan formation from volatile precursors: a critical example of artefact formation during Solid-Phase Microextraction.

    PubMed

    Adams, An; Van Lancker, Fien; De Meulenaer, Bruno; Owczarek-Fendor, Agnieszka; De Kimpe, Norbert

    2012-05-15

    For the analysis of furan, a possible carcinogen formed during thermal treatment of food, Solid-Phase Microextraction (SPME) is a preferred and validated sampling method. However, when volatile furan precursors are adsorbed on the carboxen/PDMS fiber, additional amounts of furan can be formed on the fiber during thermal desorption, as shown here for 2-butenal and furfural. No significant increase in furan amounts was found upon heating the furan precursor 2-butenal, indicating that the furan amounts formed during precursor heating experiments are negligible as compared to the additional amounts of furan formed during fiber desorption. This artefactual furan formation increased with increasing desorption time, but especially with increasing desorption temperature. Although this effect was most pronounced on the Carboxen/PDMS SPME-fiber, it was also noted on two other SPME-fibers tested (PDMS and DVB/Carboxen/PDMS). The general impact on furan data from food and model systems in literature will depend on the amounts of volatile precursors present, but will probably remain limited. However, considering the importance of this worldwide food contaminant, special care has to be taken during SPME-analysis of furan. Especially when performing precursor studies, static headspace sampling should preferably be applied for furan analysis.

  15. Determination of different recreational drugs in hair by HS-SPME and GC/MS.

    PubMed

    Merola, Gustavo; Gentili, Stefano; Tagliaro, Franco; Macchia, Teodora

    2010-08-01

    A simple procedure combining headspace solid-phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC/MS) to detect and quantify amphetamines, ketamine, methadone, cocaine, cocaethylene and Delta(9)-tetrahydrocannabinol (THC) in hair is described. This procedure allows, in a single sample, even scant, analysis of drugs requiring different analytical conditions. A hair sample (10 mg) is washed and subjected to acidic hydrolysis. Then the HS-SPME is carried out (10 min at 90 degrees C) for amphetamines, ketamine, methadone, cocaine and cocaethylene. For derivatization of analytes, the fibre is introduced into the headspace of another closed vial containing acetic anhydride. After a chromatographic run, an alkaline hydrolysis for THC analysis is carried out in the same vial containing the hair sample previously used. For adsorption, the solid-phase microextraction needle is inserted into the headspace of the vial and the fibre is exposed for 30 min at 150 degrees C. For derivatization of analytes, the fibre is introduced into the headspace of another closed vial containing N-methyl-N-(trimethylsilyl)trifluoroacetamide. The GC/MS parameters were the same for both chromatographic runs. The linearity was proved to be between 0.01 and 10.00 ng/mg. The repeatability (intra- and interday precision) was below 10% as the coefficient of variation for all compounds. The accuracy, as the relative recovery, was 96.2-103.5% (spiked samples) and 88.6-101.7% (quality control sample). The limit of detection ranged from 0.01 to 0.12 ng/mg, and the limit of quantification ranged from 0.02 to 0.37 ng/mg. Application of the procedure to real hair samples is described. To the best of our knowledge, the proposed procedure combining HS-SPME and GC/MS is the first one be to successfully applied to the simultaneous determination of most of the common recreational drugs, including THC, in a single hair sample.

  16. Analysis of BTEX and other substituted benzenes in water using headspace SPME-GC-FID: method validation.

    PubMed

    Almeida, Cristina M M; Boas, Luís Vilas

    2004-01-01

    The analysis of BTEX and other substituted benzenes in water samples using solid phase microextraction (SPME) and quantification by gas chromatography with flame ionization detection (GC-FID) was validated. The best analytical conditions were obtained using PDMS/DVB/CAR fibre using headspace extraction (HS-SPME) at 50 [degree]C for 20 min without stirring. The linear range for each compound by HS-SPME with GC/FID was defined. The detection limits for these compounds obtained with PDMS/DVB/CAR fibre and GC/FID were: benzene (15 ng L(-1)), toluene (160 ng L(-1)), monochlorobenzene (54 ng L(-1)), ethylbenzene (32 ng L(-1)), m-xylene (56 ng L(-1)), p-xylene (69 ng L(-1)), styrene (35 ng L(-1)), o-xylene (42 ng L(-1)), m-dichlorobenzene (180 ng L(-1)), p-dichlorobenzene (230 ng L(-1)), o-dichlorobenzene (250 ng L(-1)) and trichlorobenzene (260 ng L(-1)). This headspace SPME-GC-FID method was compared with a previously validated method of analysis using closed-loop-stripping analysis (CLSA). The headspace SPME-GC-FID method is suitable for monitoring the production and distribution of potable water and was used, in field trials, for the analysis of samples from main intakes of water (surface or underground) and from the water supply system of a large area (Lisbon and neighbouring municipalities).

  17. In situ hydrothermal growth of metal-organic framework 199 films on stainless steel fibers for solid-phase microextraction of gaseous benzene homologues.

    PubMed

    Cui, Xiao-Yan; Gu, Zhi-Yuan; Jiang, Dong-Qing; Li, Yan; Wang, He-Fang; Yan, Xiu-Ping

    2009-12-01

    Metal-organic frameworks (MOFs) have received great attention due to their fascinating structures and intriguing potential applications in various fields. Herein, we report the first example of the utilization of MOFs for solid-phase microextraction (SPME). MOF-199 with unique pores and open metal sites (Lewis acid sites) was employed as the coating for SPME fiber to extract volatile and harmful benzene homologues. The SPME fiber was fabricated by in situ hydrothermal growth of thin MOF-199 films on etched stainless steel wire. The MOF-199-coated fiber not only offered large enhancement factors from 19,613 (benzene) to 110,860 (p-xylene), but also exhibited wide linearity with 3 orders of magnitude for the tested benzene homologues. The limits of detection for the benzene homologues were 8.3-23.3 ng L(-1). The relative standard deviation (RSD) for six replicate extractions using one SPME fiber ranged from 2.0% to 7.7%. The fiber-to-fiber reproducibility for three parallel prepared fibers was 3.5%-9.4% (RSD). Indoor air samples were analyzed for the benzene homologues using the SPME with the MOF-199-coated fiber in combination with gas chromatography-flame ionization detection. The recoveries for the spiked benzene homologues in the collected indoor air samples were in the range of 87%-106%. The high affinity of the MOF-199-coated fiber to benzene homologues resulted from the combined effects of the large surface area and the unique porous structure of the MOF-199, the pi-pi interactions of the aromatic rings of the analytes with the framework 1,3,5-benzenetricarboxylic acid molecules, and the pi-complexation of the electron-rich analytes to the Lewis acid sites in the pores of MOF-199.

  18. Sulfonated nanoparticles doped electrospun fibers with bioinspired polynorepinephrine sheath for in vivo solid-phase microextraction of pharmaceuticals in fish and vegetable.

    PubMed

    Qiu, Junlang; Chen, Guosheng; Zhu, Fang; Ouyang, Gangfeng

    2016-07-15

    In this study, the biocompatible copolymer Poly(lactic acid-co-caprolactone) (PLCL) doped with sulfonated γ-Al2O3 nanoparticles was used for electrospun on stainless wires. The electrospun fibers were further sheathed by the self-polymerization of norepinephrine, a catecholamine found both in neurotransmitters and mussel adhesive proteins, to improve the surface hydrophilicity and provide a smooth bio-interface. The modified electrospun fibers on stainless wires were developed as novel custom-made solid-phase microextraction (SPME) fibers. These fibers exhibited much higher extraction efficiency compared to the polydimethylsiloxane (PDMS) fibers, especially to the sulfonamides. The custom-made SPME fibers also showed excellent stability with the relative standard deviations (RSDs) of intra-fiber ranged from 1.98% to 9.86% and RSDs of inter-fiber ranged from 4.36% to 15.6%. Moreover, these fibers were also demonstrated to be anti-biofouling and suitable for in vivo sampling. The custom-made SPME fibers were successfully applied to determine the Pharmaceutical concentrations in living fishes and vegetables. The accuracies were verified by the comparison with liquid extraction and the sensitivities were demonstrated to be satisfying with the limits of detection (LODs) ranged from 0.16ng/g to 5.35ng/g in fish muscle and 0.02ng/g to 8.02ng/g in vegetable stem.

  19. Identification of volatile components in yak butter using SAFE, SDE and HS-SPME-GC/MS.

    PubMed

    Li, Ning; Sun, Bao-Guo; Zheng, Fu-Ping; Chen, Hai-Tao; Liu, Si-Yuan; Gu, Chen; Song, Zhen-Yang

    2012-01-01

    The volatile components of yak butter were isolated by solvent-assisted flavour evaporation (SAFE), simultaneous distillation extraction (SDE; dichloromethane and diethyl ether as solvent, respectively) and headspace solid-phase microextraction (HS-SPME; CAR/PDMS, PDMS/DVB and DVB/CAR/PDMS fibre extraction, respectively) and were analysed by GC/MS. A total of 83 volatile components were identified under six different conditions, including 28 acids, 12 esters, 11 ketones, 10 lactones, 10 alcohols, 4 other compounds, 2 aldehydes, 2 unsaturated aldehydes, 1 furan, 1 sulphur-containing compound, 1 unsaturated alcohol and 1 unsatruated ketone. Among them, 51 were identified by SAFE, 58 by SDE (45 with dichloromethane as solvent and 41 with diethyl ether as solvent) and 40 by HS-SPME (26 with CAR/PDMS; 26 with PDMS/DVB and 32 with DVB/CAR/PDMS). Three pretreatment methods were compared to show that the volatile components obtained using different methods varied greatly, both in terms of categories and in content. Therefore, a multi-pretreatment method should be adopted, together with GC/MS. A total of 25 aroma-active compounds were detected by gas chromatography-olfactometry, among which 20 aroma-active compounds were found by SDE (14 with dichloromethane as solvent and 14 with diethyl ether as solvent) and 17 by SAFE.

  20. Determination of trace levels of aquaculture chemotherapeutants in seawater samples by SPME-GC-MS/MS.

    PubMed

    García-Rodríguez, Diego; Carro, Antonia M; Lorenzo, Rosa A; Fernández, Fátima; Cela, Rafael

    2008-08-01

    A sensitive and efficient solid-phase microextraction (SPME) method for the determination of organophosphorous (OPPs) and pyrethroid pesticides (Pyrs) in aquaculture-seawater samples by using GC with MS/MS (GC-MS/MS) was developed. Dichlorvos and chlorpyrifos (OPPs); permethrin, alpha-cypermethrin and deltamethrin (Pyrs) were selected according to their use as chemotherapeutants in the aquaculture industry. Different parameters affecting extraction efficiency such as fibre coating, agitation, pH and extraction time profiles were investigated. An experimental central composite design (alpha = 1) and desirability functions were used for the simultaneous optimization of extraction temperature and sample volume. Finally, a method based on direct SPME in 40 min at 75 degrees C using 100-microm-thick poly(dimethyl)siloxane (PDMS) fibre and 20 mL of sample volume is proposed. The method was validated, exhibiting good linearity, precision and accuracy parameters with picogram per millilitre LODs. The proposed methodology was applied to determine the ultratrace levels of OPPs and Pyrs in aquaculture-seawater samples by the standard addition approach, which proved to be reliable and sensitive, in addition to requiring only small amounts of sample.

  1. MQ NMR and SPME analysis of nonlinearity in the degradation of a filled silicone elastomer

    SciTech Connect

    Chinn, S C; Alviso, C T; Berman, E S; Harvey, C A; Maxwell, R S; Wilson, T S; Cohenour, R; Saalwachter, K; Chasse, W

    2008-10-10

    Radiation induced degradation of polymeric materials occurs via numerous, simultaneous, competing chemical reactions. Though degradation is typically found to be linear in adsorbed dose, some silicone materials exhibit non-linear dose dependence due to dose dependent dominant degradation pathways. We have characterized the effects of radiative and thermal degradation on a model filled-PDMS system, Sylgard 184 (commonly used as an electronic encapsulant and in biomedical applications), using traditional mechanical testing, NMR spectroscopy, and sample headspace analysis using Solid Phase Micro-Extraction (SPME) followed by Gas Chromatography/Mass Spectrometry (GC/MS). The mechanical data and {sup 1}H spin-echo NMR indicated that radiation exposure leads to predominantly crosslinking over the cumulative dose range studies (0 to 250 kGray) with a rate roughly linear with dose. {sup 1}H Multiple Quantum NMR detected a bimodal distribution in the network structure, as expected by the proposed structure of Sylgard 184. The MQ-NMR further indicated that the radiation induced structural changes were not linear in adsorbed dose and competing chain scission mechanisms contribute more largely to the overall degradation process in the range of 50 -100 kGray (though crosslinking still dominates). The SPME-GC/MS data were analyzed using Principal Component Analysis (PCA), which identified subtle changes in the distributions of degradation products (the cyclic siloxanes and other components of the material) as a function of age that provide insight into the dominant degradation pathways at low and high adsorbed dose.

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

    PubMed

    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.

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

    PubMed

    Benhabib, Karim; Town, Raewyn M; van Leeuwen, Herman P

    2009-04-09

    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 coupled diffusion of free and particle-bound atrazine toward the solid/sample solution interface. In the eventual equilibrium the total atrazine concentration in the solid phase is dictated by the solid phase/water partition coefficient (K(sw)) and the concentration of the free atrazine in the sample solution. These observations demonstrate that the nanoparticles do not enter the solid phase. The experimental data show that the rate of release of sorbed atrazine from the latex particles is fast on the effective time scale of the microextraction process. A lability criterion is derived to quantitatively describe the relative rates of these two processes. All together, the results indicate that SPME has a strong potential for dynamic speciation analysis of organic compounds in media containing sorbing nanoparticles.

  4. Comparison of characteristic flavor and aroma volatiles in melons and standards using solid phase microextraction (SPME) and Stir Bar Sorptive Extraction (SBSE) with GC-MS.

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Stir bar sorptive extraction (SBSE) is a technique for extraction and analysis of organic compounds in aqueous matrices, similar in theory to solid phase microextraction (SPME). SBSE has been successfully used to analyze several organic compounds, including food matrices. When compared with SPME, ...

  5. A headspace solid-phase microextraction gas-chromatographic mass-spectrometric method (HS-SPME-GC/MS) to quantify hexanal in butter during storage as marker of lipid oxidation.

    PubMed

    Panseri, Sara; Soncin, Silvia; Chiesa, Luca Maria; Biondi, Pier Antonio

    2011-07-15

    A method using headspace solid-phase microextraction (HS-SPME) combined with gas chromatography-mass spectrometry (GC/MS) was developed and validated for the extraction and quantification of hexanal content in butter (at ngg(-1) level) during storage at 4°C. The variability of hexanal content among seasons of production and the influence of high extraction temperature on ex-novo formation of hexanal were also evaluated. The HS-SPME conditions were optimised and analytical parameters of the method (linearity, accuracy, and precision) demonstrate its usefulness. The reproducibility and accuracy of the quantitative analysis was assured by the use of D(12)-hexanal as internal standard. For the applications, the headspace was extracted using CAR/PDMS fiber for 180min at 4°C. Hexanal contents in samples during all storage period (shelf-life) and from butters produced in different seasons were analysed. Butter samples at the end of shelf-life and samples produced in August showed highest values of hexanal, confirming that the temperature both in storage and distribution phases represents a critical factor to maintain the quality of butter.

  6. Preparation and characterization of porous carbon material-coated solid-phase microextraction metal fibers.

    PubMed

    Zhu, Fang; Guo, Jiaming; Zeng, Feng; Fu, Ruowen; Wu, Dingcai; Luan, Tiangang; Tong, Yexiang; Lu, Tongbu; Ouyang, Gangfeng

    2010-12-10

    Two kinds of porous carbon materials, including carbon aerogels (CAs), wormhole-like mesoporous carbons (WMCs), were synthesized and used as the coatings of solid-phase microextraction (SPME) fibers. By using stainless steel wire as the supporting core, six types of fibers were prepared with sol-gel method, direct coating method and direct coating plus sol-gel method. Headspace SPME experiments indicated that the extraction efficiencies of the CA fibers are better than those of the WMC fibers, although the surface area of WMCs is much higher than that of CAs. The sol-gel-CA fiber (CA-A) exhibited excellent extraction properties for non-polar compounds (BTEX, benzene, toluene, ethylbenzene, o-xylene), while direct-coated CA fiber (CA-B) presented the best performance in extracting polar compounds (phenols). The two CA fibers showed wide linear ranges, low detection limits (0.008-0.047μgL(-1) for BTEX, 0.15-5.7μgL(-1) for phenols) and good repeatabilities (RSDs less than 4.6% for BTEX, and less than 9.5% for phenols) and satisfying reproducibilities between fibers (RSDs less than 5.2% for BTEX, and less than 9.9% for phenols). These fibers were successfully used for the analysis of water samples from the Pearl River, which demonstrated the applicability of the home-made CA fibers.

  7. Polypyrrole/sol-gel composite as a solid-phase microextraction fiber coating for the determination of organophosphorus pesticides in water and vegetable samples.

    PubMed

    Saraji, Mohammad; Rezaei, Behzad; Boroujeni, Malihe Khalili; Bidgoli, Ali Akbar Hajialiakbari

    2013-03-01

    A novel solid-phase microextraction (SPME) fiber coated with polypyrrole/sol-gel composite was prepared through electrochemical deposition. The composite polymer coating was prepared using a three-electrode electrochemical system and directly deposited on a stainless steel wire by applying a constant potential (1.2V for 1000 s). The coating has porous surface structure, stable performance in high temperature, and good coating preparation reproducibility. The SPME composite coating was evaluated by analyzing some organophosphorus pesticides (OPPs) in water and vegetable samples followed by gas chromatography and nitrogen phosphorus detection. Different SPME parameters influencing the extraction efficiency such as coating thickness, salt concentration, stirring rate, extraction time and temperature, desorption time and desorption temperature were investigated. Under the optimized conditions, the coating showed better extraction efficiency than polypyrrole and commercial SPME fibers. The detection limits were 1.5-10 ng L(-1). Relative standard deviations for intra- and inter-day precision for a single fiber were in the range of 1.1-2.9% and 2.2-4.2%, respectively. Fiber to fiber reproducibility was in the range of 6.0-10.1% (n=3). The calibration curves were linear in the concentration range from 5 to 2000 ng L(-1) (r(2)>0.9953). Finally, the developed method was applied for the analysis of cucumber, lettuce, tap and well water samples and the relative recovery was found to be in the range of 80-109%, at the optimum conditions.

  8. Extraction with SPME and synthesis of 2-methyl-6-vinylpyrazine by a 'one pot' reaction using microwaves.

    PubMed

    Robledo, Norma; Escalante, Jaime; Arzuffi, René

    2009-06-15

    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).

  9. Graphene oxide based sol-gel stainless steel fiber for the headspace solid-phase microextraction of organophosphate ester flame retardants in water samples.

    PubMed

    Jin, Tingting; Cheng, Jing; Cai, Cuicui; Cheng, Min; Wu, Shiju; Zhou, Hongbin

    2016-07-29

    In this paper, graphene oxide was coated onto a stainless steel wire through sol-gel technique and it was used as a solid phase microextraction (SPME) fiber. The prepared fiber was characterized by scanning electron microscopy (SEM), which displayed that the fiber had crinkled surface and porous structure The application of the fiber was evaluated through the headspace SPME of nine organophosphate ester flame retardants (OPFRs) with different characteristics in water samples followed by gas chromatography and nitrogen-phosphorous detector (GC/NPD). The major factors influencing the extraction efficiency, including the extraction and desorption conditions, were studied and optimized. Under the optimum conditions, the proposed method was evaluated, and applied to the analysis of organophosphate ester flame retardants in real environmental water samples. The results demonstrated the HS-SPME method based on GO sol-gel fiber had good linearity (R>0.9928), and limits of detection (1.4-135.6ngL(-1)), high repeatability (RSD<9.8%) and good recovery (76.4-112.4%). The GO based sol-gel fiber displayed bigger extraction capability than the commercial PDMS fiber and the pure sol-gel fiber for both polar and apolar organophosphate esters, especially for the OPFRs containing benzene rings.

  10. CMK-3 nanoporous carbon as a new fiber coating for solid-phase microextraction coupled to gas chromatography-mass spectrometry.

    PubMed

    Rahimi, Akram; Hashemi, Payman; Badiei, Alireza; Arab, Pezhman; Ghiasvand, Ali Reza

    2011-06-10

    CMK-3 nanoporous carbon was prepared and characterized as a highly porous fiber coating, with a highly ordered carbon framework, for solid-phase microextraction (SPME). The nanomaterial was immobilized onto platinum, stainless steel and copper metal wires for preparation of new SPME fibers. The copper-CMK-3 fiber showed superior properties and therefore was applied for extraction of some phenolic compounds in combination with GC-MS. For optimization of the extraction conditions, a simplex optimization method was used. The selected conditions were: sample volume 13 ml, extraction temperature 56°C, extraction time 7 min, ultrasonic time 5.5 min, pH 5 and salt concentration 8.9%. The selected fiber showed some selectivity towards the polar phenolic compounds and its extraction efficiency was better than a commercial PDMS fiber. Linear calibration curves with correlation coefficients better than 0.99 and detection limits in the range from 0.002 to 0.068 μg mL(-1) were obtained for the fiber. No significant change was observed in the extraction efficiency of the new SPME fiber over at least 40 extractions. The fiber was successfully used for the determination of phenolic compounds in natural water samples.

  11. 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.

    PubMed

    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.

  12. Solid-phase microextraction of phthalate esters from aqueous media by electrophoretically deposited TiO₂ nanoparticles on a stainless steel fiber.

    PubMed

    Banitaba, Mohammad Hossein; Davarani, Saied Saeed Hosseiny; Pourahadi, Ahmad

    2013-03-29

    A novel SPME fiber was prepared by electrophoretic deposition of titanium dioxide nanoparticles (nano-TiO2) on a stainless steel wire. It was used in the direct immersion solid-phase microextraction (DI-SPME) of four phthalate esters from aqueous samples prior to gas chromatographic (GC) analysis. The effects of various parameters on the efficiency of the SPME process such as the mode of extraction, extraction temperature, film thickness of the SPME fiber, salt content, extraction time and stirring rate were investigated. The comparison of the fiber with another homemade poly(3,4-ethylenedioxythiophene)-TiO2 (PEDOT-TiO2) nanocomposite fiber and a commercial polydimethylsiloxane (PDMS) fiber showed the better extraction efficiency of the nano-TiO2 fiber for phthalate esters. Under optimized conditions, the limit of detection (LOD) for the phthalate esters varied between 0.05 and 0.12μgL(-1). The inter-day and intra-day relative standard deviations for various phthalate esters at 10μgL(-1) concentration level (n=6) using a single fiber were 6.6-7.5% and 8.3-11.1%, respectively. The fiber to fiber repeatabilities (n=4), expressed as relative standard deviation (RSD%), were between 8.9% and 10.2% at 10μgL(-1) concentration level. The linear ranges varied between 0.5 and 1000μgL(-1). The method was successfully applied to the analysis of the bottled mineral water sample with recoveries from 86 to 107%.

  13. Polythiophene/hexagonally ordered silica nanocomposite coating as a solid-phase microextraction fiber for the determination of polycyclic aromatic hydrocarbons in water.

    PubMed

    Abolghasemi, Mir Mahdi; Yousefi, Vahid

    2014-01-01

    A highly porous fiber coated with polythiophene/hexagonally ordered silica nanocomposite was prepared for solid-phase microextraction (SPME). The prepared nanomaterial was immobilized onto a stainless-steel wire for the fabrication of the SPME fiber. Polythiophene/hexagonally ordered silica nanocomposite fibers were used for the extraction of some polycyclic aromatic hydrocarbons from water samples. The extracted analytes were transferred to the injection port of a gas chromatograph using a laboratory-designed SPME device. The results obtained prove the ability of the polythiophene/hexagonally ordered silica material as a new fiber for the sampling of organic compounds from water samples. This behavior is due most probably to the increased surface area of the polythiophene/hexagonally ordered silica nanocomposite. A one-at-a-time optimization strategy was applied for optimizing the important extraction parameters such as extraction temperature, extraction time, ionic strength, stirring rate, and desorption temperature and time. Under the optimum conditions, the LOD of the proposed method is 0.1-3 pg/mL for analysis of polycyclic aromatic hydrocarbons from aqueous samples, and the calibration graphs were linear in a concentration range of 0.001-20 ng/mL (R(2) > 0.990) for most of the polycyclic aromatic hydrocarbons. The single fiber repeatability and fiber-to-fiber reproducibility were less than 8.6 and 19.1% (n = 5), respectively.

  14. Determination of chlorophenols in water by headspace solid phase microextraction ion mobility spectrometry (HS-SPME-IMS).

    PubMed

    Holopainen, Sanna; Luukkonen, Ville; Nousiainen, Marjaana; Sillanpää, Mika

    2013-09-30

    Chlorophenols (CPs) as persistent toxic compounds are of worldwide environmental concern. Usage of chlorinated phenols, especially pentachlorophenol (PCP), has been restricted or widely banned in many countries due to their possible adverse health effects even at low concentrations. Ion mobility spectrometry (IMS) has received increasing interest in environmental applications due to its unique characteristics, such as portability and speed of analysis. A range of sample introduction methods combined with IMS enable analysis from different environmental matrices. This study utilised headspace solid phase microextraction IMS (HS-SPME-IMS) in the determination of CPs from water samples. The extraction conditions were examined and the method was applied to real water samples. The developed method is suitable to detect CPs at milligram per liter level in water. Based on the results, SPME-IMS setup is feasible as an early warning system for water monitoring of pollutants present in drinking or surface water in case of environmental accidents or leakages.

  15. Analytical comparison and sensory representativity of SAFE, SPME, and Purge and Trap extracts of volatile compounds from pea flour.

    PubMed

    Murat, Chloe; Gourrat, Karine; Jerosch, Heike; Cayot, Nathalie

    2012-12-01

    Pisum sativum is of great economic and nutritional interest due to its protein content. Nevertheless, pea products are underused as a protein source in human food because of their strong beany flavour. Therefore, the objective of this study was to select an efficient and representative method to extract volatile molecules of pea flour. In the first step, three extraction methods were chosen: solid phase micro extraction (SPME); Purge and Trap extraction and solvent assisted flavour evaporation (SAFE). The corresponding extracts were analysed by gas chromatography coupled with mass spectrometry. In the second step, the sensory representativity of the extracts was assessed either by direct gas chromatography-olfactometry for SPME and for Purge and Trap extracts, or by sniffing for the aqueous SAFE extract. It appeared that SAFE extraction was the most suitable method because of its good extraction capacities and its high sensory representativity of the global odour of pea flour.

  16. Preparation of durable graphene-bonded titanium fibers for efficient microextraction of phthalates from aqueous matrices and analysis with gas chromatography-mass spectrometry.

    PubMed

    Zhang, Bo-Tao; Li, Hai-Fang; Zheng, Xiaoxia; Teng, Yanguo; Liu, Yan; Lin, Jin-Ming

    2014-11-28

    A solid-phase microextraction fiber (SPME) was synthesized for pre-concentration of 15 phthalates from aqueous samples. Graphene oxide was immobilized on Ti wire with titanol groups using a cross-linking agent and subsequently reduced to yield a folded and wrinkled graphene coating. This graphene-Ti fiber demonstrated durable mechanical robustness and enhanced stability for more than 200 extraction cycles due to the Ti substrate and chemical bond. The extraction efficiencies reached highest when the graphene layers were four and their performances were superior to commercial SPME fibers. The prepared fiber was used for pre-concentration of phthalates from aqueous samples by direct immersion extraction and thermal desorption for gas chromatography-mass spectrometry analysis. The method was utilized for the simultaneous analysis of 15 phthalates with satisfactory recoveries in the range of 82.8-97.8% for bottled water and 73.3-102.0% for intravenous drips in plastic packaging.

  17. Development of a simple, accurate SPME-based method for assay of VOCs in column breakthrough experiments.

    PubMed

    Salaices Avila, Manuel Alejandro; Breiter, Roman; Mott, Henry

    2007-01-01

    Solid-phase microextraction (SPME) with gas chromatography is to be used for assay of effluent liquid samples from soil column experiments associated with VOC fate/transport studies. One goal of the fate/transport studies is to develop accurate, highly reproducible column breakthrough curves for 1,2-cis-dichloroethylene (cis-DCE) and trichloroethylene (TCE) to better understand interactions with selected natural solid phases. For SPME, the influences of the sample equilibration time, extraction temperature and the ratio of volume of sample bottle to that of the liquid sample (V(T)/V(w)) are the critical factors that could influence accuracy and precision of the measured results. Equilibrium between the gas phase and liquid phase was attained after 200 min of equilibration time. The temperature must be carefully controlled due to variation of both the Henry's constant (K(h)) and the fibre/gas phase distribution coefficient (K(fg)). K(h) decreases with decreasing temperature while K(fg) increases. Low V(T)/V(w) yields better sensitivity but results in analyte losses and negative bias of the resultant assay. High V(T)/V(w) ratio yields reduced sensitivity but analyte losses were found to be minimal, leading to better accuracy and reproducibility. A fast SPME method was achieved, 5 min for SPME extraction and 3.10 min for GC analysis. A linear calibration function in the gas phase was developed to analyse the breakthrough curve data, linear between a range of 0.9-236 microgl(-1), and a detection limit lower than 5 microgl(-1).

  18. Preparation and characterization of metal-organic framework MIL-101(Cr)-coated solid-phase microextraction fiber.

    PubMed

    Xie, Lijun; Liu, Shuqin; Han, Zhubing; Jiang, Ruifen; Liu, Hong; Zhu, Fang; Zeng, Feng; Su, Chengyong; Ouyang, Gangfeng

    2015-01-01

    Metal-organic frameworks (MOFs) have received great attention as novel sorbents due to their fascinating structures and intriguing potential applications in various fields. In this work, a MIL-101(Cr)-coated solid-phase microextraction (SPME) fiber was fabricated by a simple direct coating method and applied to the determination of volatile compounds (BTEX, benzene, toluene, ethylbenzene, m-xylene and o-xylene) and semi-volatile compounds (PAHs, polycyclic aromatic hydrocarbons) from water samples. The extraction and desorption conditions of headspace SPME (HS-SPME) were optimized. Under the optimized conditions, the established methods exhibited excellent extraction performance. Good precision (<7.7%) and low detection limits (0.32-1.7 ng L(-1) and 0.12-2.1 ng L(-1) for BTEX and PAHs, respectively) were achieved. In addition, the MIL-101(Cr)-coated fiber possessed good thermal stability, and the fiber can be reused over 150 times. The fiber was successfully applied to the analysis of BTEX and PAHs in river water by coupling with gas chromatography-mass spectrometry (GC-MS). The analytes at low concentrations (1.7 and 10 ng L(-1)) were detected, and the recoveries obtained with the spiked river water samples were in the range of 80.0-113% and 84.8-106% for BTEX and PAHs, respectively, which demonstrated the applicability of the self-made fiber.

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

    PubMed Central

    Kusano, Miyako; Iizuka, Yumiko; Kobayashi, Makoto; Fukushima, Atsushi; Saito, Kazuki

    2013-01-01

    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. PMID:24957989

  20. Optimization of headspace solid-phase Microextraction (SPME) for the odor analysis of surface-ripened cheese.

    PubMed

    Lecanu, Laurent; Ducruet, Violette; Jouquand, Céline; Gratadoux, Jean Jacques; Feigenbaum, Alexandre

    2002-06-19

    Fifty volatile compounds of surface smear-ripened cheese were detected and identified using headspace solid-phase microextraction (HS-SPME) and vacuum distillation coupled to gas chromatography-mass spectrometry. Changes in the headspace of aroma compounds were monitored over the whole packaging period (47 days) using the HS-SPME method. Initially, the concentration of methanethiol increased before reaching a plateau. This evolution could be linked to the growth of Brevibacterium linens. During the shelf life of cheese, levels of acetic acid and 3-methylbutanoic acid remained constant, whereas butane-2,3-dione, 3-hydroxybutan-2-one, and hydroxypropan-2-one levels gradually declined and acetone and 3-methylbutanol levels dropped sharply to a plateau. Changes in odor could be related to changes of the rind, which behaved as a barrier, strongly influencing the distribution of volatile compounds in the headspace. Using a gas chromatography-olfactometry technique without separation, it was shown that the SPME extract was representative of the cheese odor.

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

    PubMed

    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.

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

    NASA Astrophysics Data System (ADS)

    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.

  3. Determination of Volatile Organic Compounds in Snow Using Solid Phase Micro Extraction (SPME)

    NASA Astrophysics Data System (ADS)

    Kos, G.; Ariya, P. A.

    2004-12-01

    Volatile organic compounds (VOC) in snow-samples from different environments were determined. Samples were collected in Resolute, Nunavut in the high Arctic (latitude: 74.70° /longitude: - 94.91° ), the Gaspé Peninsula in Quebec (at Mont Albert near Ste-Anne-des Monts: 49.12° /- 66.49° ) and downtown Montreal, Quebec ( 45.54° /- 73.60° ) in order to reflect different degrees of anthropogenic influence. In order to assess the ability of compounds contained in the sample to perform photochemistry, samples were irradiated with UV-light in the 300-400 nm range. Filtering through a 0.2 μ m-filter provided information about compounds primarily associated with the liquid phase. A solid phase micro extraction (SPME) procedure was developed for sample preparation and VOC were identified using gas chromatography with mass spectrometric detection (GC-MS). We will present our results at several urban and remote sites, and the implication of the result to atmospheric chemistry will be discussed.

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

    PubMed Central

    Ding, Zhen; Peng, Shifu; Xia, Weiwen; Zheng, Hao; Chen, Xiaodong; Yin, Lihong

    2014-01-01

    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. PMID:24527037

  5. Method development by GC-ECD and HS-SPME-GC-MS for beer volatile analysis.

    PubMed

    da Silva, Gisele C; da Silva, Abner A S; da Silva, Larissa S N; Godoy, Ronoel Luiz de O; Nogueira, Luciana C; Quitério, Simone L; Raices, Renata S L

    2015-01-15

    Two methods for the extraction, identification and quantification of the highest occurrence and lowest perception threshold off-flavours in fifteen different samples of Brazilian Pilsner beers were developed. For this purpose, headspace solid phase microextraction in combination with a gas chromatography coupled to a mass spectrometric detection (HS-SPME-GC-MS) as well as headspace extraction in combination with a gas chromatography coupled to electron capture detection (HS-GC-ECD) were evaluated. The first and the second methods were used for esters and vicinal diketones analysis, respectively. All data were comprehended below the taster's threshold detection limit: ethyl acetate 39.48 ng mL(-1) (RSD mean value 4.2%), isoamyl acetate 3.88 ng mL(-1) (RSD mean value 3.4%), ethyl hexanoate 0.61 ng mL(-1) (RSD mean value 3.1%) and 2,3-butanedione 0.10 ng mL(-1) (RSD mean value 2.9%). The validated method demonstrated to be useful for the analysis of highest incidence beer off-flavours.

  6. Selective solid-phase microextraction of explosives using fibers coated with the La (III) complex of p-di (4,4,5,5,6,6,6-hepafluoro-1,3-hexanediony) benzene

    SciTech Connect

    Harvey, Scott D.

    2008-12-12

    This research demonstrates enhanced capture of explosives on polydimethylsiloxane (PDMS) solid-phase microextraction (SPME) fibers coated with a metal beta-diketonate polymer, [La(III) complex of p-di(4,4,5,5,6,6,6-heptafluoro-1,3-hexanedionyl)benzene, La(dihed)], compared to PDMS control fibers. SPME sampling was performed in an explosives bunker where the concentration of 2,4,6-trinitrotoluene (TNT) was estimated at less than 3 parts-per-trillion (v/v). Analysis by gas chromatography/mass spectrometry showed an approximate ten-fold enhancement in the quantity of 2,4-dinitrotoluene captured on La(dihed) over the control fiber. La(dihed) sampling also resulted in a strong signal for TNT, whereas this explosive was well below the detection limit (1 pg on fiber) on the control fiber.

  7. [Solid-phase microextraction coupled with capillary electrophoresis for doping analysis of propranolol enantiomers in urine using a sol-gel derived calix [4] arene fiber].

    PubMed

    Zhou, Xingwang; Li, Xiujuan; Zeng, Zhaorui

    2006-01-01

    A new type fiber coated with diglycidyloxy calix [4] arene/hydroxy-terminated silicone oil (diglycidyloxy-C [4] arene/OH-TSO) made by sol-gel method was prepared for capillary electrophoresis (CE) sample pretreatment. By using headspace solid-phase microextraction (HS-SPME) combined with a novel back-extraction facility coupled off-line to capillary zone electrophoresis (CZE), the determination of propranolol enantiomers in urine was achieved with combination of ultrasonic back-extraction and field amplified sample injection (FASI) technologies. Extraction and back-extraction parameters were optimized. The clean-up effect and preconcentration effect were realized without derivatization during the SPME process in terms of this strongly polar and thermally stable compound. Preconcentration of the sample by calix [4] arene fiber increased the sensitivity, yielding a limit of detection (LOD) of 0.01 mg/L by CZE-diode array detection (DAD). Method repeatability (relative standard deviations (RSD) < 6.5%) and fiber reusability (> 150 extraction procedures) were observed over a wide linear range of propranolol (0.05 - 10 mg/L) in urine samples. Compared with commercial SPME stationary phases, the new coating showed higher extraction efficiency and this SPME-CZE-DAD procedures could meet the demand of minimum required performance limits (MRPL) set by the World Anti-Doping Agency (WADA) for the detection of propranolol in urine samples.

  8. Field Analysis of Polychlorinated Biphenyls (PCBs) in Soil Using Solid-Phase Microextraction (SPME) and a Portable Gas Chromatography-Mass Spectrometry System.

    PubMed

    Zhang, Mengliang; Kruse, Natalie A; Bowman, Jennifer R; Jackson, Glen P

    2016-05-01

    An expedited field analysis method was developed for the determination of polychlorinated biphenyls (PCBs) in soil matrices using a portable gas chromatography-mass spectrometry (GC-MS) instrument. Soil samples of approximately 0.5 g were measured with a portable scale and PCBs were extracted by headspace solid-phase microextraction (SPME) with a 100 µm polydimethylsiloxane (PDMS) fiber. Two milliliters of 0.2 M potassium permanganate and 0.5 mL of 6 M sulfuric acid solution were added to the soil matrices to facilitate the extraction of PCBs. The extraction was performed for 30 min at 100 ℃ in a portable heating block that was powered by a portable generator. The portable GC-MS instrument took less than 6 min per analysis and ran off an internal battery and helium cylinder. Six commercial PCB mixtures, Aroclor 1016, 1221, 1232, 1242, 1248, 1254, and 1260, could be classified based on the GC chromatograms and mass spectra. The detection limit of this method for Aroclor 1260 in soil matrices is approximately 10 ppm, which is sufficient for guiding remediation efforts in contaminated sites. This method was applicable to the on-site analysis of PCBs with a total analysis time of 37 min per sample. However, the total analysis time could be improved to less than 7 min per sample by conducting the rate-limiting extraction step for different samples in parallel.

  9. Isotope dilution SPME GC/MS for the determination of methylmercury in tuna fish samples.

    PubMed

    Centineo, Giuseppe; Blanco González, Elisa; García Alonso, J Ignacio; Sanz-Medel, Alfredo

    2006-01-01

    The development of a rapid, precise and accurate analytical method for the determination of methylmercury in tuna fish samples is described. The method is based on the use of isotope dilution GC/MS with electron impact ionization, a widespread technique in routine testing laboratories. A certified spike containing (202)Hg-enriched methylmercury was used for the isotope dilution of the samples. After extraction of the methylmercury from the sample, methylmercury was propylated using sodium tetrapropyl borate in SPME vials and the analytes were sampled from the headspace for 15 min. For isotope measurements, the molecular ion (MePrHg(+)) was used in the SIM mode. Five molecular ions were monitored, corresponding to the (198)Hg, (199)Hg, (200)Hg, (201)Hg and (202)Hg isotopes. The detection at masses corresponding to (198)Hg was used to correct for m + 1 contributions of (13)C from the organic groups attached to the mercury atom on the (199)Hg, (200)Hg, (201)Hg and (202)Hg masses with simple mathematical equations, and the concentration of methylmercury was calculated on the basis of the corrected (200)Hg/(202)Hg isotope ratio. The (202)Hg-enriched methylmercury spike was applied, with satisfactory results, to the determination of methylmercury in the certified reference material BCR 464. The method was successfully applied to the determination of methylmercury in tuna fish samples, and the obtained results were included in the CCQM-P39 interlaboratory exercise, organized by the Institute for Reference Materials and Measurements (IRMM, Geel, Belgium) with excellent agreement between our results and the average obtained by the other participants.

  10. An automated solid-phase microextraction method based on magnetic molecularly imprinted polymer as fiber coating for detection of trace estrogens in milk powder.

    PubMed

    Lan, Hangzhen; Gan, Ning; Pan, Daodong; Hu, Futao; Li, Tianhua; Long, Nengbing; Qiao, Li

    2014-02-28

    A new automated solid-phase micro extraction (SPME) sampling method was developed for quantitative enrichment of estrogens (ES) from milk powder, using magnetic molecularly imprinted polymer (MMIP) as fiber coating. The method (MMIP-SPME) was built with several electromagnetic stainless steel fibers, placed in parallel for simultaneously extraction. The MMIP was synthesized using core-shell Fe3O4@SiO2 nanoparticles (NPs) as magnetic support. Estradiol (E2) was employed as the template molecule, acrylamide (AA) as functional monomer, and ethylene glycol dimethacrylate (EGDMA) as cross-linker. MMIP can be easily absorbed or desorbed from fibers when the current is turned on or off, creating magnetism. Compared to traditional MIP-SPME, the prepared procedure of MMIP-SPME is time-saving and organic solvent-free. The proposed device significantly improved the efficiency of separation and enrichment of estrogens from complex matrices thereby and facilitating the pretreatment steps by electromagnetically controlled extraction fibers to achieve full automation. Several experimental parameters were studied, including extraction and desorption kinetics, solution pH, desorption solution, ratio, and shuttle rate. The newly developed MMIP-SPME showed good sensitivity and high binding capacity, fast adsorption kinetics and desorption kinetics for estrone (E1), estradiol (E2), estriol (E3) and diethylstilbestrol (DES) under optimized conditions. The detection limits for the four estrogens were 1.5-5.5ngg(-1) with excellent reproducibility (RSD values less than 7.1%) when milk powder samples spiked with analytes at 20, 100 and 250ngg(-1) were studied.

  11. Recovery of phosphonate surface contaminants from glass using a simple vacuum extractor with a solid-phase microextraction fiber

    SciTech Connect

    Gary S. Groenewold; Jill R. Scott; Cathy Rae

    2011-07-01

    Recovery of chemical contaminants from fixed surfaces for analysis can be challenging particularly if it is not possible to acquire a solid sample. A simple device is described that collects semivolatile organic compounds from fixed surfaces by creating an enclosed volume over the surface, then generating a modest vacuum. A solid-phase microextraction 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 vacuum speeds partitioning of the semivolatile 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 (deltaTvac) resulted in fractional recovery efficiencies ranged from 10(-3) to > 10(-1), and in absolute terms collection of low nanograms was demonstrated. Fractional recovery values were correlated to the vapor pressure of the compounds being sampled. Fractional recovery increased with increasing deltaTvac, and displayed a roughly logarithmic profile indicating that an operational equilibrium is being approached. Fractional recovery decreased with increasing time between exposure and sampling, however recordable quantities of the phosphonates could be collected three weeks after exposure.

  12. Analysis of ammonium nitrate headspace by on-fiber solid phase microextraction derivatization with gas chromatography mass spectrometry.

    PubMed

    Lubrano, Adam L; Andrews, Benjamin; Hammond, Mark; Collins, Greg E; Rose-Pehrsson, Susan

    2016-01-15

    A novel analytical method has been developed for the quantitation of trace levels of ammonia in the headspace of ammonium nitrate (AN) using derivatized solid phase microextraction (SPME) fibers with gas chromatography mass spectrometry (GC-MS). Ammonia is difficult to detect via direct injection into a GC-MS because of its low molecular weight and extreme polarity. To circumvent this issue, ammonia was derivatized directly onto a SPME fiber by the reaction of butyl chloroformate coated fibers with the ammonia to form butyl carbamate. A derivatized externally sampled internal standard (dESIS) method based upon the reactivity of diethylamine with unreacted butyl chloroformate on the SPME fiber to form butyl diethylcarbamate was established for the reproducible quantification of ammonia concentration. Both of these compounds are easily detectable and separable via GC-MS. The optimized method was then used to quantitate the vapor concentration of ammonia in the headspace of two commonly used improvised explosive device (IED) materials, ammonium nitrate fuel oil (ANFO) and ammonium nitrate aluminum powder (Ammonal), as well as identify the presence of additional fuel components within the headspace.

  13. Determination of low level methyl tert-butyl ether, ethyl tert-butyl ether and methyl tert-amyl ether in human urine by HS-SPME gas chromatography/mass spectrometry.

    PubMed

    Scibetta, Licia; Campo, Laura; Mercadante, Rosa; Foà, Vito; Fustinoni, Silvia

    2007-01-02

    Methyl tert-butyl ether (MTBE), ethyl tert-butyl ether (ETBE) and tert-amyl methyl ether (TAME) are oxygenated compounds added to gasoline to enhance octane rating and to improve combustion. They may be found as pollutants of living and working environments. In this work a robotized method for the quantification of low level MTBE, ETBE and TAME in human urine was developed and validated. The analytes were sampled in the headspace of urine by SPME in the presence of MTBE-d12 as internal standard. Different fibers were compared for their linearity and extraction efficiency: carboxen/polydimethylsiloxane, polydimethylsiloxane/divinylbenzene, and polydimethylsiloxane. The first, although highly efficient, was discarded due to deviation of linearity for competitive displacement, and the polydimethylsiloxane/divinylbenzene fiber was chosen instead. The analysis was performed by GC/MS operating in the electron impact mode. The method is very specific, with range of linearity 30-4600 ng L(-1), within- and between-run precision, as coefficient of variation, <22 and <16%, accuracy within 20% the theoretical level, and limit of detection of 6 ng L(-1) for all the analytes. The influence of the matrix on the quantification of these ethers was evaluated analysing the specimens of seven traffic policemen exposed to autovehicular emissions: using the calibration curve and the method of standard additions comparable levels of MTBE (68-528 ng L(-1)), ETBE (<6 ng L(-1)), and TAME (<6 ng L(-1)) were obtained.

  14. Evaluation of the solid-phase microextraction fiber coated with single walled carbon nanotubes for the determination of benzene, toluene, ethylbenzene, xylenes in aqueous samples.

    PubMed

    Li, Quanlong; Ma, Xiaoxia; Yuan, Dongxing; Chen, Jinsheng

    2010-04-09

    A solid-phase microextraction (SPME) fiber coated with single walled carbon nanotubes (SWCNTs) was prepared by electrophoretic deposition and treated at 500 degrees C in H(2) stream. In order to evaluate the characteristics of the obtained fiber, it was applied in the headspace solid-phase microextraction (HS-SPME) of benzene, toluene, ethylbenzene and xylenes (BTEX) from water sample and quantification by gas chromatography with flame ionization detection (GC-FID). The results indicated that the thermal treatment with H(2) enhanced the extraction of the SWCNTs fiber for BTEX significantly. Thermal stability and durability of the fiber were also investigated, showing excellent stability up to 350 degrees C and life time over 120 times. In the comparison with the commercial CAR-PDMS fiber, the SWCNTs fiber showed similar and higher extraction efficiencies for BTEX. Under the optimized conditions, the linearity, LODs (S/N=3) and LOQs (S/N=10) of the method based on the SWCNTs fiber were 0.5-50.0, 0.005-0.026 and 0.017-0.088 microg/L, respectively. Repeatability for one fiber (n=3) was in the range of 1.5-5.6% and fiber-to-fiber reproducibility (n=3) was in the range of 4.2-8.3%. The proposed method was successfully applied in the analysis of BTEX compounds in seawater, tap water and wastewater from a paint plant.

  15. HS-SPME-GC×GC-qMS volatile metabolite profiling of Chrysolina herbacea frass and Mentha spp. leaves.

    PubMed

    Cordero, Chiara; Zebelo, Simon Atsbaha; Gnavi, Giorgio; Griglione, Alessandra; Bicchi, Carlo; Maffei, Massimo E; Rubiolo, Patrizia

    2012-02-01

    Headspace solid-phase microextraction (HS-SPME) comprehensive two-dimensional (2D) gas chromatography combined with quadrupole-mass spectrometry (GC×GC-qMS) with dedicated comparative data elaboration was applied to separate chemical patterns arising from the interaction between some Mentha species and the herbivore Chrysolina herbacea, also known as the mint bug. Upon feeding on different Mentha species (Mentha spicata L., Mentha × piperita L. and Mentha longifolia L.), C. herbacea produced frass (faeces) which were characterized by a typical volatile fraction. HS-SPME GC×GC-qMS analysis of the complex volatile fraction of both mint leaf and C. herbacea frass was submitted to advanced fingerprinting analysis of 2D chromatographic data. 1,8-Cineole, found in the leaves of all the Mentha species examined, was oxidized, and C. herbacea frass yielded high rates of several hydroxy-1,8-cineoles, including 2α-hydroxy-, 3α-hydroxy-, 3β-hydroxy- and 9-hydroxy-1,8-cineole. Upon insect feeding, several unknown oxidized monoterpenes, a p-menthane diol and three unknown phenylpropanoids were also detected in the frass volatiles. In M. longifolia, the occurrence of the monoterpene piperitenone oxide was found to be toxic and associated with insect death. The results of this work show that high throughput techniques such as HS-SPME and GC×GC-qMS fingerprint analysis are ideal tools to analyze complex volatile matrices, and provide a sensitive method for the direct comparison and chemical visualization of plant and insect emitted volatile components.

  16. In situ solvothermal synthesis of metal-organic framework coated fiber for highly sensitive solid-phase microextraction of polycyclic aromatic hydrocarbons.

    PubMed

    Gao, Jia; Huang, Chuanhui; Lin, Yifen; Tong, Ping; Zhang, Lan

    2016-03-04

    The present work reported a facile and simple in situ solvothermal growth method for immobilization of metal-organic framework UiO-66 via covalent bonding on amino functional silica fiber for highly sensitive solid-phase microextraction (SPME) of ten polycyclic aromatic hydrocarbons (PAHs) by coupling with gas chromatography-mass spectrometry (GC-MS) analysis. The developed SPME coated fiber has been characterized through SEM, TGA and XRD, confirmed the coating thickness of ∼25μm with high thermal and chemical stability. Under optimized conditions, the obtained method exhibited satisfactory linearity in range of 1.0-5000.0ngL(-1) for all the PAHs. The low detection limits were from 0.28ngL(-1) to 0.60ngL(-1) (S/N=3). The UiO-66 coated fibers showed good repeatability (RSDs less than 8.2%, n=5) and satisfying reproducibility between fiber to fiber (RSDs less than 8.9%, n=5). This method was successfully used for simultaneous determination of ten PAHs from Minjiang water and soil samples with satisfactory recoveries of 87.0-113.6% and 83.8-116.7%, respectively. Experimental results shows that the chemical bonding approach has dramatically improve the stability and lifetime of pure MOFs coating for SPME in sample pretreatment.

  17. A novel silver-coated solid-phase microextraction metal fiber based on electroless plating technique.

    PubMed

    Feng, Juanjuan; Sun, Min; Li, Jubai; Liu, Xia; Jiang, Shengxiang

    2011-09-09

    A novel silver-coated solid-phase microextraction fiber was prepared based on electroless plating technique. Good extraction performance of the fiber for model compounds including phthalate esters (dibutyl phthalate, dioctyl phthalate, dicyclohexyl phthalate and diallyl phthalate) and polycyclic aromatic hydrocarbons (naphthalene, fluorene, phenanthrene, fluoranthene) in aqueous solution was obtained. Under the optimized conditions (extraction temperature, extraction time, ionic strength and desorption temperature), the proposed SPME-GC method showed wide linear ranges with correlation coefficients (R(2)) ranging from 0.9745 to 0.9984. The limits of detection were at the range of 0.02 to 0.1 μg L(-1). Single fiber repeatability and fiber-to-fiber reproducibility as well as stability to acid, alkali and high temperature were studied and the results were all satisfactory. The method was applied successfully to the aqueous extracts of disposable paper cup and instant noodle barrel. Several kinds of analytes were detected and quantified.

  18. Multiple headspace solid-phase microextraction using a new fiber for avoiding matrix interferences in the quantitative determination of ethyl carbamate in pickles.

    PubMed

    Lei, Fen-Fen; Zhang, Xue-Na; Gao, Yuan-Li; Han, Ya-Hong; Li, Xiu-Juan; Pan, Si-Yi

    2012-05-01

    Multiple headspace solid-phase microextraction (HS-SPME) using a novel fiber coated with anilino-methyl triethoxy silicane-methacrylic acid/terminated silicone oil has been introduced as a useful pretreatment technique coupled to gas chromatography-flame ionization detector for the detection of ethyl carbamate in pickles. Anilino-methyl triethoxy silicane and methacrylic acid are put into use simultaneously with the aim to increase the hydrogen interaction strength between ethyl carbamate and the coating. In addition, the new fiber exhibits high thermal stability, good reproducibility, and long lifetime. Extraction temperature, extraction time, amount of desiccant, and amount of sample were well optimized to guarantee the suitability of multiple HS-SPME. Significant matrix interference was observed among various types of pickles and the multiple HS-SPME procedure was proved to be effective in avoiding the matrix effect by a complete recovery of the analyte. The method showed satisfactory linearity (0.1-100 mg kg(-1)), precision (4.25%, n = 5), and detection limit (0.038 mg kg(-1)). The accuracy of the method was evaluated by comparison with standard addition method and the results were statistically equivalent. The study indicates that the multiple HS-SPME procedure is simple, convenient, accurate, and low-cost, and most of all, can be used for quantitative analysis in complex matrix without matrix effect.

  19. Fiber biology

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Cotton fiber cells arising from seed epidermis is the most important agricultural textile commodity in the world. To produce fully mature fibers, approximately two months of fiber developmental process are required. The timing of four distinctive fiber development stages consisting of initiation, ...

  20. Characterization of Aronia melanocarpa volatiles by headspace-solid-phase microextraction (HS-SPME), simultaneous distillation/extraction (SDE), and gas chromatography-olfactometry (GC-O) methods.

    PubMed

    Kraujalytė, Vilma; Leitner, Erich; Venskutonis, Petras Rimantas

    2013-05-22

    The profiles of volatile constituents of berry fruit of two Aronia melanocarpa genotypes were evaluated by headspace-solid-phase microextraction (HS-SPME), simultaneous distillation and extraction (SDE), and gas chromatography-olfactometry (GC-O). In total, 74 volatile compounds were identified in chokeberry juice, 3-penten-2-one, 3,9-epoxy-p-menth-1-ene, and benzaldehyde being the most abundant constituents; however, their percentage concentrations were remarkably different in the HS-SPME and SDE profiles. Twenty two aroma-active compounds were detected and characterized by the trained panelists in HS-SPME using GC-O detection frequency analysis. Olfactometry revealed that ethyl-2-methyl butanoate, ethyl-3-methyl butanoate, ethyl decanoate ("fruity" aroma notes), nonanal ("green" notes), unidentified compound possessing "moldy" odor, and some other volatiles may be very important constituents in formation of chokeberry aroma of both analyzed plant cultivars.

  1. Volatile profile analysis and quality prediction of Longjing tea (Camellia sinensis) by HS-SPME/GC-MS

    PubMed Central

    Lin, Jie; Dai, Yi; Guo, Ya-nan; Xu, Hai-rong; Wang, Xiao-chang

    2012-01-01

    This study aimed to analyze the volatile chemical profile of Longjing tea, and further develop a prediction model for aroma quality of Longjing tea based on potent odorants. A total of 21 Longjing samples were analyzed by headspace solid phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC-MS). Pearson’s linear correlation analysis and partial least square (PLS) regression were applied to investigate the relationship between sensory aroma scores and the volatile compounds. Results showed that 60 volatile compounds could be commonly detected in this famous green tea. Terpenes and esters were two major groups characterized, representing 33.89% and 15.53% of the total peak area respectively. Ten compounds were determined to contribute significantly to the perceived aroma quality of Longjing tea, especially linalool (0.701), nonanal (0.738), (Z)-3-hexenyl hexanoate (−0.785), and β-ionone (−0.763). On the basis of these 10 compounds, a model (correlation coefficient of 89.4% and cross-validated correlation coefficient of 80.4%) was constructed to predict the aroma quality of Longjing tea. Summarily, this study has provided a novel option for quality prediction of green tea based on HS-SPME/GC-MS technique. PMID:23225852

  2. Analysis of the chloroacetanilide herbicides in water using SPME with CAR/PDMS and GC/ECD.

    PubMed

    Hwang, Ying-Ming; Wong, Yih-Gang; Ho, Wu-Hsiung

    2005-01-01

    The solid-phase microextraction (SPME) technique using a 75 mm film of carboxen/polydimethylsiloxane was applied to the analysis of chloroacetanilide herbicides (acetochlor, alachlor, butachlor, metolachlor, and propachlor) residues. The feasibility of SPME with gas chromatography electron capture detection analysis has been evaluated. The effects of experimental parameters such as magnetic stirring, salt addition, humic acid addition, pH value, and extraction time, as well as desorption temperature and time, were investigated. Analytical parameters such as linearity, repeatability and limit of detection were also evaluated. The inhibition of humic acid to the extraction of chloroacetanilide herbicides was observed. A standard addition method for calibration was recommended to reduce deviations caused by matrix interferences. The proposed method provided a simple and rapid analytical procedure for chloroacetanilide herbicides in water with limits of detection 0.002-0.065 microg/L for deionized water, and 0.005-0.22 microg/L for farm water. The relative standard deviations (n = 5) for analyses of farm water were 7-20% for 5 [corrected] microg/L chloroacetanilide herbicides. This application was illustrated by the analysis of sample collected from farm water in the Chung-hwa area, Taiwan.

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

    PubMed

    Caupos, Emilie; Touffet, Arnaud; Mazellier, Patrick; Croue, Jean-Philippe

    2015-03-01

    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 DOM varied from 4.3 to 5.8, depending on the nature of the organic material. A good correlation was established between log K DOM and 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.

  4. Selective extraction and enrichment of glycoproteins based on boronate affinity SPME and determination by CIEF-WCID.

    PubMed

    Li, Lixian; Xia, Zhining; Pawliszyn, Janusz

    2015-07-30

    In this study, a new thin-film boronic acid coating was developed for solid-phase microextraction (SPME) followed by capillary isoelectric focusing with whole-column imaging detection (CIEF-WCID). Boronate functionalized particles of phenylboronic acid (PBA) and 3-aminophenylboronic acid (3-aPBA) were utilized as boronate affinity solid phase coating on thin-film stainless steel blades for selective extraction and enrichment of glycoproteins. The process of extraction and elution could be easily controlled by adjusting pH. To test specificity, asialofetuin and lactoferrin were selected as glycoproteins test molecules, while BSA and myoglobin were used as control non-glycoproteins in this study. The boronate affinity coating was characterized. The effect of buffer, pH, extraction profiles and elution profiles were investigated. The developed method was successfully applied to extract glycoproteins from standard buffer, PBS, human plasma and 10-fold diluted human blood using two kinds of boronate affinity blades. Boronate affinity SPME could be a promising tool for selective extraction and enrichment of low-abundance glycoproteins in real biological samples.

  5. Investigation of cuticular hydrocarbons from Bagrada hilaris genders by SPME/GC-MS.

    PubMed

    De Pasquale, C; Guarino, S; Peri, E; Alonzo, G; Colazza, S

    2007-10-01

    The cuticular hydrocarbons of male and female Bagrada hilaris Burmeister (Heteroptera: Pentatomidae) were investigated, by headspace solid-phase microextraction followed by gas chromatography-mass spectrometry. Measurements were done with fiber coatings of different polarity after optimization of headspace volumes and extraction temperatures. This resulted in the use of polyacrylate fiber, 22-ml vial as the sample holder, and an extraction temperature of 150 degrees C. The analytical procedures allowed identification of 13 peaks, corresponding to a homologous series of n-alkanes (nC(17)-nC(29)). The hydrocarbon profiles of male and female B. hilaris were qualitatively equal, but marked sex-specific quantitative differences were observed for some of the linear alkanes.

  6. SPME-GC determination of methanol as a hydrate inhibitor in crude oil.

    PubMed

    Mokhtari, Bahram; Pourabdollah, Kobra

    2011-12-15

    This work focused on the quantitation of methanol as a hydrate inhibitor in the crude oil. The novelty is microextraction of a polar compound from a complex non-polar matrix and selection of proper fiber with maximum selectivity, loading percent, and lifetime. This approach not only does not require specific instrumentation, such as multiple columns, and selective detectors, but also has eliminated the use of organic solvent and avoids the insertion of water inside the GC columns. The objective is optimization of extraction conditions, GC adjustments and data processing. Experiments were conducted on the real sample of Iranian offshore crude oil by a carboxen/PDMS fiber via a GC equipped with a cross-linked polyethylene glycol column and FID. The results revealed that this fiber adsorbed the alcohols among other light non-polar compounds of crude oil. Moreover, the interference effects of ethanol were solved by proper selection of thermal program. The LOD, LOQ and linear range of this approach were determined to be 3.9, 12.9 and 14-229 mg L(-1) for methanol, respectively. Moreover, the sensitivity was 30 area-counts per mg L(-1). Using the standard calibration and the standard addition methods, the relative errors of 1.6-7.2 and 5.3-14.0% were determined, respectively.

  7. Facile and efficient poly(ethylene terephthalate) fibers-in-tube for online solid-phase microextraction towards polycyclic aromatic hydrocarbons.

    PubMed

    Bu, Yanan; Feng, Juanjuan; Sun, Min; Zhou, Changli; Luo, Chuannan

    2016-07-01

    Poly(ethylene terephthalate) (polyester) fibers as solid-phase microextraction (SPME) adsorbent were directly filled in a poly(ether ether ketone) (PEEK) tube, for online analysis of polycyclic aromatic hydrocarbons (PAHs) in environmental water samples, coupled with high-performance liquid chromatography. The facile, economic, and environmental polyester fibers-in-tube SPME device exhibited high extraction efficiency, good selectivity for PAHs, and satisfactory durability. Under optimum conditions, the polyester fibers provided satisfactory enhancement factors in the range of 307-1646, and low detection limits ranging from 0.01 to 0.03 μg L(-1). The linearity was in the range of 0.03-80 μg L(-1) with correlation coefficients (r) ranging from 0.9978 to 0.9997. Limit of quantification was defined as a concentration of the analytes with a ten-time signal-to-noise ratio (S/N = 10) and was in the range of 0.03-0.1 μg L(-1). The intra-day and inter-day precisions for quantitative analysis were investigated and the relative standard deviation (RSD) was lower than 5.8 and 6.9 %, respectively. Extraction repeatability was also investigated and its RSD was in the range of 3.8-7.8 %. Finally, the fiber-in-tube SPME device was successfully applied to analyze PAHs in water samples. Graphical abstract Schematic diagrams of polyester fibers-in-tube device and the automated in-tube SPME-HPLC system.

  8. Solid-phase microextraction-gas chromatography-time-of-flight mass spectrometry utilized for the evaluation of the new-generation super elastic fiber assemblies.

    PubMed

    Setkova, Lucie; Risticevic, Sanja; Linton, Christopher M; Ouyang, Gangfeng; Bragg, Leslie M; Pawliszyn, Janusz

    2007-01-09

    The aim of this study was to evaluate the performance characteristics of the recently developed super elastic solid-phase microextraction (SPME) fibers. The fiber needle, plunger and fiber core are manufactured with a special type of flexible alloy that exhibits excellent shape memory and tensile strength. This material makes the assemblies more robust, permitting several hundreds of analyses in a sequence, which is one of the ways to improve the robustness and sample throughput of automated SPME methods. The design and size of the needle utilized in the new fiber assemblies is discussed here, as well as the use of a septum-free injector replacement and a low-volume direct injection glass liner placed in the GC inlet. Deionized water and pump oil samples spiked with target volatile compounds (McReynold's probes and toluene) were used for the purposes of the presented study. A fully automated SPME sample preparation technique was combined with the GC-TOFMS system for the chromatographic separation and identification/quantification of the target analytes.

  9. Fiber introduction mass spectrometry: determination of pesticides in herbal infusions using a novel sol-gel PDMS/PVA fiber for solid-phase microextraction.

    PubMed

    da Silva, Rogério Cesar; Zuin, Vânia Gomes; Yariwake, Janete Harumi; Eberlin, Marcos Nogueira; Augusto, Fabio

    2007-06-01

    An application of the direct coupling of solid-phase microextraction (SPME) with mass spectrometry (MS), a technique known as fiber introduction mass spectrometry (FIMS), is described to determine organochlorine (OCP) and organophosphorus (OPP) pesticides in herbal infusions of Passiflora L. A new fiber coated with a composite of poly(dimethylsiloxane) and poly(vinyl alcohol) (PDMS/PVA) was used. Sensitive, selective, simple and simultaneous quantification of several OCP and OPP was achieved by monitoring diagnostic fragment ions of m/z 266 (chlorothalonil), m/z 195 (alpha-endosulfan), m/z 278 (fenthion), m/z 263 (methyl parathion) and m/z 173 (malathion). Simple headspace SPME extraction (25 min) and fast FIMS detection (less than 40 s) of OCP and OPP from a highly complex herbal matrix provided good linearity with correlation coefficients of 0.991-0.999 for concentrations ranging from 10 to 140 ng ml(-1) of each compound. Good accuracy (80 to 110%), precision (0.6-14.9%) and low limits of detection (0.3-3.9 ng ml(-1)) were also obtained. Even after 400 desorption cycles inside the ionization source of the mass spectrometer, no visible degradation of the novel PDMS/PVA fiber was detected, confirming its suitability for FIMS. Fast (ca 20 s) pesticide desorption occurs for the PDMS/PVA fiber owing to the small thickness of the film and its reduced water sorption.

  10. Fiber introduction mass spectrometry: determination of pesticides in herbal infusions using a novel sol-gel PDMS/PVA fiber for solid-phase microextraction.

    PubMed

    da Silva, Rogério Cesar; Zuin, Vânia Gomes; Yariwake, Janete Harumi; Eberlin, Marcos Nogueira; Augusto, Fabio

    2007-10-01

    An application of the direct coupling of solid-phase microextraction (SPME) with mass spectrometry (MS), a technique known as fiber introduction mass spectrometry (FIMS), is described to determine organochlorine (OCP) and organophosphorus (OPP) pesticides in herbal infusions of Passiflora L. A new fiber coated with a composite of poly(dimethylsiloxane) and poly(vinyl alcohol) (PDMS/PVA) was used. Sensitive, selective, simple and simultaneous quantification of several OCP and OPP was achieved by monitoring diagnostic fragment ions of m/z 266 (chlorothalonil), m/z 195 (alpha-endosulfan), m/z 278 (fenthion), m/z 263 (methyl parathion) and m/z 173 (malathion). Simple headspace SPME extraction (25 min) and fast FIMS detection (less than 40 s) of OCP and OPP from a highly complex herbal matrix provided good linearity with correlation coefficients of 0.991-0.999 for concentrations ranging from 10 to 140 ng ml(-1) of each compound. Good accuracy (80 to 110%), precision (0.6-14.9%) and low limits of detection (0.3-3.9 ng ml(-1)) were also obtained. Even after 400 desorption cycles inside the ionization source of the mass spectrometer, no visible degradation of the novel PDMS/PVA fiber was detected, confirming its suitability for FIMS. Fast (ca 20 s) pesticide desorption occurs for the PDMS/PVA fiber owing to the small thickness of the film and its reduced water sorption.

  11. Anti-malarial activity and HS-SPME-GC-MS chemical profiling of Plinia cerrocampanensis leaf essential oil

    PubMed Central

    2014-01-01

    Background Plinia cerrocampanensis is an endemic plant of Panama. The leaf essential oil of this plant has shown antibacterial activity. However, anti-malarial activity and chemical profiling by HS-SPME-GC-MS of this essential oil have not been reported before. Methods Anti-malarial activity of the essential oil (EO) was evaluated in vitro against chloroquine-sensitive HB3 and chloroquine-resistant W2 strains of Plasmodium falciparum. Synergistic effect of chloroquine and the EO on parasite growth was evaluated by calculating the combination index. A methodology involving headspace solid phase microextraction and gas chromatography-mass spectrometry (HS-SPME-GC-MS) was developed to investigate the composition of Plinia cerrocampanensis EO. Results Plinia cerrocampanensis EO showed a high anti-malarial activity and a synergistic interaction with chloroquine. The Plinia cerrocampanensis EO inhibited P. falciparum growth in vitro at an IC50 of 7.3 μg/mL. Chloroquine together with the EO decreased the IC50 of chloroquine from 0.1 μg/mL to 0.05 μg/mL, and of the EO from 7.3 μg/mL to 1.1 μg/mL. The measured combination index was 0.58, which clearly indicates that the EO acts synergistically with chloroquine. Since the EO maintained its inhibitory activity on the chloroquine-sensitive strain of the parasite, it could be acting by a different mechanism of action than chloroquine. The best HS-SPME-GC-MS analytical conditions were obtained when the temperature of extraction was 49°C, incubation time 14 min, and the time of extraction 10 min. This method allowed for the identification of 53 volatile constituents in the EO, including new compounds not reported earlier. Conclusions The anti-malarial activity exhibited by the Plinia cerrocampanensis EO may lend support for its possible use as an alternative for anti-malarial therapy. PMID:24410874

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

    ERIC Educational Resources Information Center

    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…

  13. Fiber Techniques

    ERIC Educational Resources Information Center

    Nalle, Leona

    1976-01-01

    Describes a course in fiber techniques, which covers design methods involving fibers and fabric, that students in the Art Department at Sleeping Giant Junior High School had the opportunity to learn. (Author/RK)

  14. Analyzing freely dissolved concentrations of cationic surfactant utilizing ion-exchange capability of polyacrylate coated solid-phase microextraction fibers.

    PubMed

    Chen, Yi; Droge, Steven T J; Hermens, Joop L M

    2012-08-24

    A 7-μm polyacrylate (PA) coated fiber was successfully employed to determine freely dissolved concentrations of cationic surfactants by solid-phase microextraction (SPME) and utilizing the capability of the PA-coating to sorb organic cations via ion-exchange at carboxylic groups. Measured fiber-water partitioning coefficients (K(fw)) were constant below a fiber loading of 2mmol per liter polyacrylate, allowing for simple and accurate analysis in a concentration range that is relevant from a risk assessment point of view. Ion-exchange was confirmed to be the main sorption mechanism because of a decreasing K(fw) with either higher CaCl(2) concentrations or lower pH, and maximum fiber uptake at the polyacrylate cation-exchange capacity (CEC, at 30mmol/L PA). Fiber-water sorption isotherms were established in various aqueous media in toxicological relevant concentrations. The developed SPME method has a high potential for application in ecotoxicological studies, as demonstrated in sorption studies with humic acid in different electrolyte solutions at aqueous concentrations down to the sub nM range. Cationic surfactant sorption affinities for humic acid also depend on medium composition but are orders of magnitude higher than to the PA fiber on a sorbent weight basis.

  15. Sampling gaseous compounds from essential oils evaporation by solid phase microextraction devices

    NASA Astrophysics Data System (ADS)

    Cheng, Wen-Hsi; Lai, Chin-Hsing

    2014-12-01

    Needle trap samplers (NTS) are packed with 80-100 mesh divinylbenzene (DVB) particles to extract indoor volatile organic compounds (VOCs). This study compared extraction efficiency between an NTS and a commercially available 100 μm polydimethylsiloxane-solid phase microextration (PDMS-SPME) fiber sampler used to sample gaseous products in heated tea tree essential oil in different evaporation modes, which were evaporated respectively by free convection inside a glass evaporation dish at 27 °C, by evaporation diffuser at 60 °C, and by thermal ceramic wicks at 100 °C. The experimental results indicated that the NTS performed better than the SPME fiber samplers and that the NTS primarily adsorbed 5.7 ng ethylbenzene, 5.8 ng m/p-xylenes, 11.1 ng 1,2,3-trimethylbenzene, 12.4 ng 1,2,4-trimethylbenzene and 9.99 ng 1,4-diethylbenzene when thermal ceramic wicks were used to evaporate the tea tree essential oil during a 1-hr evaporation period. The experiment also indicated that the temperature used to heat the essential oils should be as low as possible to minimize irritant VOC by-products. If the evaporation temperature does not exceed 100 °C, the concentrations of main by-products trimethylbenzene and diethylbenzene are much lower than the threshold limit values recommended by the National Institute for Occupational Safety and Health (NIOSH).

  16. Characterization and aging study of currency ink and currency canine training aids using headspace SPME/GC-MS.

    PubMed

    Vu, Doan-Trang T

    2003-07-01

    Solid-phase microextraction/gas chromatography-mass spectrometry (SPME/GC-MS) was used to characterize the volatile components associated with U.S. currency, U.S. currency inks, and Canadian currency. Compounds that can be attributed to the ink-curing process include series of straight-chain aldehydes, alkenals, acids, alcohols, and ketones and a series of lactones and 2-alkyl furans. Solvent compounds include naphthenic and paraffinic hydrocarbons with a profile typical of petroleum products, alkyl cyclohexanes, various ethylene glycol alkyl ethers, and traces of chlorinated solvents. Trace levels of 2-phenoxyethanol, a solvent often used in ink formulations, were also detected. Environmental contaminants, those compounds found in circulating currency but not in currency ink, include 2,2'-diethyl-1,1'-biphenyl, methyl benzoate and salicylate, menthol, limonene, dimethyl and diethyl phthalate, and ionol. Not including simple hydrocarbons, over 100 compounds were identified in the headspace of currency-related samples.

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

    PubMed

    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.

  18. Dietary Fiber

    MedlinePlus

    Fiber is a substance in plants. Dietary fiber is the kind you eat. It's a type of carbohydrate. You may also see it listed on a food label as soluble ... types have important health benefits. Good sources of dietary fiber include Whole grains Nuts and seeds Fruit and ...

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

    USGS Publications Warehouse

    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.

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

    PubMed

    Limmer, Matt A; Balouet, Jean-Christophe; Karg, Frank; Vroblesky, Don A; Burken, Joel G

    2011-10-01

    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.

  1. Critical evaluation of fiber coatings for organotin determination by using solid phase microextraction in headspace mode.

    PubMed

    Bravo, Manuel M; Valenzuela, Aníbal S; Fuentes, Edwar P; Quiroz, Waldo V

    2012-02-03

    In the present work three different SPME fibers have been investigated for simultaneous determination of methyl-, butyl- and phenyltins by using gas chromatography-pulsed flame photometer detection (GC-PFPD). The optimal experimental conditions for each fiber were determined and the respective figures of merit were evaluated. All fiber evaluated presented similar limit of detection (sub ng L⁻¹) and requires two internal standards to reach an acceptable repeatability. However, the CAR-PDMS fiber offers the best compromise between selectivity and sensibility for determination of organotins selected. The developed method was validated for analysis of certified reference material and spiked samples, obtaining satisfactory results. Finally, some contaminated samples were analyzed demonstrating the applicability of developed method for determination of organotin compounds in the environment and for monitoring their biochemical cycle.

  2. High scalable implementation of SPME using parallel spherical cutoff three-dimensional FFT on the six-dimensional torus QCDOC supercomputer

    NASA Astrophysics Data System (ADS)

    Fang, Bin

    In order to model complex heterogeneous biophysical systems with non-trivial charge distributions such as globular proteins in water, it is important to evaluate the long range forces present in these systems accurately and efficiently. The Smooth Particle Mesh Ewald summation technique (SPME) is commonly employed to determine the long range part of electrostatic energy in large scale molecular simulations. While the SPME technique does not give rise to a performance bottleneck in a single processor or scalar computation, current implementations of SPME on massively parallel supercomputers become problematic at large processor numbers, limiting the time and length scales that can be reached. Here, two accomplishments have been made in this dissertation to give rise to both improved accuracy and efficiency on massively parallel computing platforms. First of all, a well designed parallel framework of 3D complex-to-complex FFT and 3D real-to-complex FFT for the novel QCDOC supercomputer with its 6D-torus architecture is given. The efficiency of this framework was tested on up to 4096 processors. Secondly, a new modification of the SPME technique is exploited, which was inspired by the non-linear growth of the approximation error of Euler Exponential Spline interpolation function. This fine grained parallel implementation of SPME has been embedded into MDoC package. Numerical tests of package performance on up to 1024-processor QCDOC supercomputer residing at Brookhaven National Lab are presented for two systems of interest, beta-hairpin solvated in explicit water, a system which consists of 1112 water molecules and a 20 residue protein for a total of 3579 atoms, and HIV-1 protease solvated in explicit water, a system which consists of 8793 water molecules and a 198 residue protein for a total of 29508 atoms.

  3. A metal organic framework-polyaniline nanocomposite as a fiber coating for solid phase microextraction.

    PubMed

    Bagheri, Habib; Javanmardi, Hasan; Abbasi, Alireza; Banihashemi, Solmaz

    2016-01-29

    A metal organic framework-polyaniline (MOF/PANI) nanocomposite was electrodeposited on a stainless steel wire and used as a solid phase microextraction (SPME) fiber coating. The electropolymerization process was carried out under a constant deposition potential and applied to the corresponding aqueous electrolyte containing aniline and MOF particles. The employment of MOFs with their large and small cages and 3-D structures in synthesizing a nanocomposite was assumed to be efficient constitutes to induce more non-smooth and porous structures, approved by scanning electron microscopy (SEM) images. Three different MOFs were incorporated to synthesize the desired nanocomposites and the preliminary experiments showed that all of them, particularly the one containing MOF2, have higher extraction performances in compared with PANI. The applicability of the new fiber coating was examined by headspace-solid phase microextraction (HS-SPME) of some chlorobenzenes (CBs) from aqueous samples. Influencing parameters on the synthesize and extraction processes including the electrodeposition voltage and its duration time, the weight ratio of PANI and MOF, the ionic strength, desorption temperature and time, and extraction time and temperature were optimized. The developed method was validated by analyzing the spiked distilled water and gas chromatography-mass spectrometry (GC-MS). Under optimum condition, the relative standard deviation (RSD%) values for a double distilled water spiked with the selected CBs at 20ngL(-1) were 5-8% (n=3) and the detection limits were below 0.2ngL(-1). The linear dynamic range (LDR) of the method was in the concentration range of 0.5-1000ngL(-1) (R(2)>0.9994). The fiber-to-fiber reproducibility was found to be in the range of 4-7%. Eventually, various real-water samples were analyzed by the MOF/PANI-based HS-SPME and GC-MS and the relative recovery values were found to be in the range of 92-98%.

  4. Graphene-coated fiber for solid-phase microextraction of triazine herbicides in water samples.

    PubMed

    Wu, Qiuhua; Feng, Cheng; Zhao, Guangying; Wang, Chun; Wang, Zhi

    2012-01-01

    Graphene is a novel and interesting carbon material that could be used for the separation and purification of some chemical compounds. In this investigation, graphene was used as a novel fiber-coating material for the solid-phase microextraction (SPME) of four triazine herbicides (atrazine, prometon, ametryn and prometryn) in water samples. The main parameters that affect the extraction and desorption efficiencies, such as the extraction time, stirring rate, salt addition, desorption solvent and desorption time, were investigated and optimized. The optimized SPME by graphene-coated fiber coupled with high-performance liquid chromatography-diode array detection (HPLC-DAD) was successfully applied for the determination of the four triazine herbicides in water samples. The linearity of the method was in the range from 0.5 to 200 ng/mL, with the correlation coefficients (r) ranging from 0.9989 to 0.9998. The limits of detection of the method were 0.05-0.2 ng/mL. The relative standard deviations varied from 3.5 to 4.9% (n=5). The recoveries of the triazine herbicides from water samples at spiking levels of 20.0 and 50.0  ng/mL were in the range between 86.0 and 94.6%. Compared with two commercial fibers (CW/TPR, 50 μm; PDMS/DVB, 60 μm), the graphene-coated fiber showed higher extraction efficiency.

  5. Preparation and characterization of polydimethylsiloxane/poly(vinylalcohol) coated solid phase microextraction fibers using sol-gel technology.

    PubMed

    Lopes, Alexandre Leite; Augusto, Fabio

    2004-11-12

    The applicability of a composite composed of polydimethylsiloxane (PDMS) and poly(vinyl alcohol) (PDMS/PVA) as coating sorbent for SPME fibers is demonstrated here. Fused silica (FS) fibers were coated with PDMS/PVA composite through a sol-gel process, using methyltrimethoxysilane as reticulating agent. The chemical and physical properties of the sol-gel PDMS/PVA composite were determined by infrared spectroscopy and thermogravimetric analysis. Electron scanning microscopy of the prepared fibers, showed that the coating obtained was highly microporous, having a thickness of approximately 5 microm. The fibers were tested for the headspace extraction of several organic compounds (o-xylene, naphthalene, ethyl caprate, p-chlorotoluene and PCB) prior to gas chromatographic analysis. The extractive capacity of the PDMS/PVA coating was found to be superior to that of pure conventional PDMS fibers.

  6. Contact solid-phase microextraction with uncoated glass and polydimethylsiloxane-coated fibers versus solvent sampling for the determination of hydrocarbons in adhesion secretions of Madagascar hissing cockroaches Gromphadorrhina portentosa (Blattodea) by gas chromatography-mass spectrometry.

    PubMed

    Gerhardt, Heike; Schmitt, Christian; Betz, Oliver; Albert, Klaus; Lämmerhofer, Michael

    2015-04-03

    Molecular profiles of adhesion secretions of Gromphadorrhina portentosa (Madagascar hissing cockroach, Blattodea) were investigated by gas chromatography mass spectrometry with particular focus on a comprehensive analysis of linear and branched hydrocarbons. For this purpose, secretions from the tarsi (feet), possibly contributing to adhesion on smooth surfaces, and control samples taken from the tibiae (lower legs), which contain general cuticular hydrocarbons that are supposed to be not involved in the biological adhesion function, were analyzed and their molecular fingerprints compared. A major analytical difficulty in such a study constitutes the representative, spatially controlled, precise and reproducible sampling from a living insect as well as the minute quantities of insect secretions on both tarsi and tibiae. Thus, three different in vivo sampling methods were compared in terms of sampling reproducibility and extraction efficiency by replicate measurement of samples from tarsi and tibiae. While contact solid-phase microextraction (SPME) with a polydimethylsiloxane (PDMS) fiber showed higher peak intensities, a self-made uncoated glass fiber had the best repeatability in contact-SPME sampling. Chromatographic profiles of these two contact-SPME sampling methods were statistically not significantly different. Inter-individual variances were larger than potentially existing minor differences in molecular patterns of distinct sampling methods. Sampling by solvent extraction was time consuming, showed lower sensitivities and was less reproducible. In general, sampling by contact-SPME with a cheap glass fiber turned out to be a viable alternative to PDMS-SPME sampling. Hydrocarbon patterns of the tarsal adhesion secretions were qualitatively similar to those of epicuticular hydrocarbon profiles of the tibiae. However, hydrocarbons were in general less abundant in tarsal secretions than secretions from tibiae.

  7. Solid-phase microextraction of methadone in urine samples by electrochemically co-deposited sol-gel/Cu nanocomposite fiber.

    PubMed

    Mohammadiazar, Sirwan; Hasanli, Fateme; Maham, Mehdi; Payami Samarin, Somayeh

    2016-12-30

    Electrochemically co-deposited sol-gel/Cu nanocomposites have been introduced as a novel, simple and single-step technique for preparation of solid-phase microextraction (SPME) coating to extract methadone (MDN) (a synthetic opioid) in urine samples. The porous surface structure of the sol-gel/Cu nanocomposite coating was revealed by scanning electron microscopy. Direct immersion SPME followed by HPLC-UV determination was employed. The factors influencing the SPME procedure, such as the salt content, desorption solvent type, pH and equilibration time, were optimized. The best conditions were obtained with no salt content, acetonitrile as desorption solvent type, pH 9 and 10 min equilibration time. The calibration graphs for urine samples showed good linearity. The detection limit was about 0.2 ng mL(-1) . Also, the novel method for preparation of nanocomposite fiber was compared with previously reported techniques for MDN determination. The results show that the novel nanocomposite fiber has relatively high extraction efficiency.

  8. Development of solid-phase microextraction fibers based on multi-walled carbon nanotubes for pre-concentration and analysis of alkanes in human breath.

    PubMed

    Tang, Zhentao; Liu, Yong; Duan, Yixiang

    2015-12-18

    In this work, a laboratory preparation method based on sol-gel technology was proposed to develop a new kind of SPME (solid phase microextraction) fibers. Multi-walled carbon nanotubes (MWCNT) were selected as sol-gel active organic component. Stainless steel wires were used as the substrate of the fibers. Instead of traditional modification methods, microwave induced plasma was used to modify the stainless steel wire surface, resulting in a significant improvement in chemical adhesion of the fiber substrate and coating. The MWCNT coating exhibited several good properties. Acceptable fiber-to-fiber reproducibility (RSD≤13%) and repeatability (RSD<7%) were obtained. End-tidal breath of 10 normal humans were collected by Bio-VOC(®) sampler and assayed by the optimized SPME-GC-MS method. The calibration curves were all linear (R(2)≥0.994) in the range from 0.03 to 403.3ppbv for five alkanes. Detection limits (down to 0.001ppbv) were about one order of magnitude better than those of commercial PDMS fibers. The recovery of the spiked alkanes in real breath sample at 1ppbv ranged from 89.71 to 101.08% and the relative standard deviations were less than 8%. These results demonstrated the feasibility and practicality of the proposed preparation procedure. Applications of the in-house fabricated fibers for human breath analysis were successfully verified.

  9. Polydimethylsiloxane/metal-organic frameworks coated fiber for solid-phase microextraction of polycyclic aromatic hydrocarbons in river and lake water samples.

    PubMed

    Zhang, Guijiang; Zang, Xiaohuan; Li, Zhi; Wang, Chun; Wang, Zhi

    2014-11-01

    In this study, polydimethylsiloxane/metal-organic frameworks (PDMS/MOFs), including PDMS/MIL-101 and PDMS/MOF-199, were immobilized onto a stainless steel wire through sol-gel technique as solid-phase microextraction (SPME) fiber coating. The prepared fibers were used for the extraction of some polycyclic aromatic hydrocarbons (PAHs) from water samples prior to gas chromatography-mass spectrometry (GC-MS) analysis. Under the optimized experiment conditions, the PDMS/MIL-101 coated fiber exhibited higher extraction efficiency towards PAHs than that of PDMS/MOF-199. Several parameters affecting the extraction of PAHs by SPME with PDMS/MIL-101 fiber, including the extraction temperature, extraction time, sample volume, salt addition and desorption conditions, were investigated. The limits of detection (LODs) were less than 4.0 ng L(-1) and the linearity was observed in the range from 0.01 to 2.0 µg L(-1) with the correlation coefficients (r) ranging from 0.9940 to 0.9986. The recoveries of the method for the PAHs from water samples at spiking levels of 0.05 and 0.2 µg L(-1) ranged from 78.2% to 110.3%. Single fiber repeatability and fiber-to-fiber reproducibility were less than 9.3% and 13.8%, respectively.

  10. Highly sensitive copper fiber-in-tube solid-phase microextraction for online selective analysis of polycyclic aromatic hydrocarbons coupled with high performance liquid chromatography.

    PubMed

    Sun, Min; Feng, Juanjuan; Bu, Yanan; Luo, Chuannan

    2015-08-21

    A fiber-in-tube solid-phase microextraction (SPME) device was developed with copper wire and copper tube, which was served as both the substrate and sorbent with high physical strength and good flexibility. Its morphology and surface properties were characterized by scanning electron microscopy and energy dispersive X-ray spectrometry. It was coupled with high performance liquid chromatography (HPLC) equipment by replacing the sample loop of six-port injection valve, building the online SPME-HPLC system conveniently. Using ten polycyclic aromatic hydrocarbons (PAHs) as model analytes, extraction conditions including sampling rate, extraction time, organic content and desorption time were investigated and optimized. The copper fiber-in-tube exhibits excellent extraction efficiency toward PAHs, with enrichment factors from 268 to 2497. The established online SPME-HPLC method provides good linearity (0.05-100μgL(-1)) and low detection limits (0.001-0.01μgL(-1)) for PAHs. It has been used to determine PAHs in water samples, with recoveries in the range of 86.2-115%. Repeatability on the same extraction tube is in the range of 0.6-3.6%, and repeatability among three tubes is in the range of 5.6-20.1%. Compared with phthalates, anilines and phenols, the copper fiber-in-tube possesses good extraction selectivity for PAHs. The extraction mechanism is probably related to hydrophobic interaction and π-electron-metal interaction.

  11. Preparation of ionic liquid based solid-phase microextraction fiber and its application to forensic determination of methamphetamine and amphetamine in human urine.

    PubMed

    He, Yi; Pohl, Jeremy; Engel, Robert; Rothman, Leah; Thomas, Marie

    2009-06-12

    A new solid-phase microextraction (SPME) procedure using an ionic liquid (IL) has been developed. Reusable IL-based SPME fiber was prepared for the first time by fixing IL through cross-linkage of IL impregnated silicone elastomer on the surface of a fused silica fiber. 1-Ethoxyethyl-3-methylimidazloium bis(trifluoromethane) sulfonylimide ([EeMim][NTf(2)]) ionic liquid was employed as a demonstration and the prepared fiber was applied to the forensic headspace determination of methamphetamine (MAP) and amphetamine (AP) in human urine samples. Important extraction parameters including the concentration of salt and base in sample matrix, extraction temperature and extraction time were investigated and optimized. Combined with gas chromatography/mass spectrometry (GC/MS) working in selected ion monitoring (SIM) mode, the new method showed good linearity in the range of 20-1500 microg L(-1), good repeatability (RSD<7.5% for MAP, and <11.5% for AP, n=6), and low detection limits (0.1 microg L(-1) for MAP and 0.5 microg L(-1) for AP). Feasibility of the method was evaluated by analyzing human urine samples. Although IL-based SPME is still at the beginning of its development stage, the results obtained by this work showed that it is a promising simple, fast and sensitive sample preparation method.

  12. Preparation and evaluation of amino modified graphene solid-phase microextraction fiber and its application to the determination of synthetic musks in water samples.

    PubMed

    Li, Siyan; Zhu, Fang; Jiang, Ruifen; Ouyang, Gangfeng

    2016-01-15

    In the current study, amino modified (NH2-modified) graphene was developed as a solid-phase microextraction (SPME) coating for the first time. The structure of the NH2-modified graphene was characterized by X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM). The fiber was fabricated using xylene-diluted silicone sealant as an adhesion agent. The performance and feasibility of the NH2-modified graphene fiber was evaluated through autosampler-assisted direct immersion (DI) SPME followed by gas chromatography-mass spectrometry (GC/MS) for the analysis of five synthetic musks (muscone, galaxolide, musk-xylene, tonalide and musk-ketone) in aqueous samples. The results showed that the prepared fiber had good thermal stability, excellent solvent resistance and a long service lifetime (more than 200 replicate extraction cycles). The proposed autosampler-assisted DI-SPME-GC/MS method showed low limits of detection (0.46-5.96 ng L(-1)), wide linear ranges (5-500 ng L(-1)), and acceptable reproducibility (relative standard deviation, RSD<12%). Finally, the method was successfully applied to the analysis of synthetic musks in environmental water samples with good recoveries (82.3-112%) and satisfactory precisions (RSD<9.9%). These results indicated that the NH2-modified graphene provided a promising alternative in sample pretreatment.

  13. Development of a cheap and accessible carbon fibers-in-poly(ether ether ketone) tube with high stability for online in-tube solid-phase microextraction.

    PubMed

    Feng, Juanjuan; Sun, Min; Bu, Yanan; Luo, Chuannan

    2016-02-01

    Carbon fibers (CFs) are one kind of important industrial materials that can be obtained commercially at low price. Based on the high extraction efficiency of carbon sorbents, a cheap and accessible carbon fibers-in-poly(ether ether ketone) (PEEK) tube was developed for online in-tube solid-phase microextraction (SPME) method. Coupled to high performance liquid chromatography (HPLC), the CFs-in-tube SPME was applied to analyze eight polycyclic aromatic hydrocarbons (PAHs) in environmental aqueous samples. Extraction conditions (sampling rate, extraction time, methanol content) and desorption time were investigated for optimization of conditions. Under the optimum conditions, the CFs-in-tube SPME-HPLC method provided high extraction efficiency with enrichment factors up to 1748. Good linearity (0.05-50 μg L(-1), 0.5-50 μg L(-1)) and low detection limits (0.01-0.1 μg L(-1)) were also obtained. The online analysis method was finally applied to determine several model PAHs analytes in real environmental aqueous samples. Some target analytes were detected and relative recoveries were in the range of 92.3-111%. Due to natural chemical stability of carbon fibers and PEEK tube, the CFs-in-tube device exhibited high resistance to organic solvent, acid and alkaline conditions.

  14. Hydrothermally grown and self-assembled modified titanium and nickel oxide composite nanosheets on Nitinol-based fibers for efficient solid phase microextraction.

    PubMed

    Wang, Huiju; Song, Wenlan; Zhang, Min; Zhen, Qi; Guo, Mei; Zhang, Yida; Du, Xinzhen

    2016-10-14

    A novel titanium and nickel oxide composite nanosheets (TiO2/NiOCNSs) coating was in situ grown on a Nitinol (NiTi) wire by direct hydrothermal treatment and modified by self-assembly of trichlorophenylsilane for solid phase microextraction (SPME). TiO2/NiOCNSs were radially oriented and chemically bonded to the NiTi substrate with double-faced open access sites. Moreover the phenyl modified TiO2/NiOCNSs (TiO2/NiOCNSs-Ph) coating exhibited original surface supporting framework favorable for effective SPME. The extraction performance of TiO2/NiOCNSs-Ph coated NiTi (NiTi-TiO2/NiOCNSs-Ph) fiber was investigated for the concentration and detection of ultraviolet (UV) filters, polycyclic aromatic hydrocarbons (PAHs), phthalate acid esters and polychlorinated biphenyls coupled to HPLC with UV detection. The novel fiber exhibited better selectivity for UV filters and PAHs and presented greater extraction capability compared to commercial polydimethylsiloxane and polyacrylate fibers. Under the optimized conditions for SPME of UV filters, the proposed method presented linear ranges from 0.1 to 300μg/L with correlation coefficients of higher than 0.999 and limits of detection from 0.030μg/L to 0.064μg/L. Relative standard deviations (RSDs) were below 7.16% and 8.42% for intra-day and inter-day measurements with the single fiber, respectively. Furthermore RSDs for fiber-to-fiber reproducibility from 6.57% to 8.93% were achieved. The NiTi-TiO2/NiOCNSs-Ph fiber can be used up to 200 times. The proposed method was successfully applied to the preconcentration and determination of trace target UV filters in different environmental water samples. The relative recoveries from 87.3% to 104% were obtained with RSDs less than 8.7%.

  15. Liquid-liquid-solid microextraction based on membrane-protected molecularly imprinted polymer fiber for trace analysis of triazines in complex aqueous samples.

    PubMed

    Hu, Yuling; Wang, Yangyang; Hu, Yufei; Li, Gongke

    2009-11-20

    A novel liquid-liquid-solid microextraction (LLSME) technique based on porous membrane-protected molecularly imprinted polymer (MIP)-coated silica fiber has been developed. In this technique, a MIP-coated silica fiber was protected with a length of porous polypropylene hollow fiber membrane which was filled with water-immiscible organic phase. Subsequently the whole device was immersed into aqueous sample for extraction. The LLSME technique was a three-phase microextraction approach. The target analytes were firstly extracted from the aqueous sample through a few microliters of organic phase residing in the pores and lumen of the membrane, and were then finally extracted onto the MIP fiber. A terbutylazine MIP-coated silica fiber was adopted as an example to demonstrate the feasibility of the novel LLSME method. The extraction parameters such as the organic solvent, extraction and desorption time were investigated. Comparison of the LLSME technique was made with molecularly imprinted polymer based solid-phase microextraction (MIP-SPME) and hollow fiber membrane-based liquid-phase microextraction (HF-LPME), respectively. The LLSME, integrating the advantages of high selectivity of MIP-SPME and enrichment and sample cleanup capability of the HF-LPME into a single device, is a promising sample preparation method for complex samples. Moreover, the new technique overcomes the problem of disturbance from water when the MIP-SPME fiber was exposed directly to aqueous samples. Applications to analysis of triazine herbicides in sludge water, watermelon, milk and urine samples were evaluated to access the real sample application of the LLSME method by coupling with high-performance liquid chromatography (HPLC). Low limits of detection (0.006-0.02 microg L(-1)), satisfactory recoveries and good repeatability for real sample (RSD 1.2-9.6%, n = 5) were obtained. The method was demonstrated to be a fast, selective and sensitive pretreatment method for trace analysis of triazines

  16. Ionic liquid coated copper wires and tubes for fiber-in-tube solid-phase microextraction.

    PubMed

    Sun, Min; Feng, Juanjuan; Bu, Yanan; Luo, Chuannan

    2016-08-05

    A fiber-in-tube solid-phase microextraction (SPME) device was developed by filling eleven copper wires into a copper tube, and all of those were functionalized with ionic liquids. Its morphology and surface properties were characterized by scanning electron microscopy. It was connected into high performance liquid chromatography (HPLC) equipment by replacing the sample loop of six-port injection valve, building the online SPME-HPLC system. In the optimization of extraction conditions, sampling rate, sample volume, pH of sample and desorption time were investigated with five estrogens as model analytes. Under the optimum conditions, an online SPME-HPLC analysis method was achieved, showing enrichment efficiency from 611 to 1661 and a good linearity of 0.06-60μgL(-1) with low detection limits of 0.02-0.05μgL(-1). It was applied to detect estrogens analytes in two water samples, with recoveries in the range of 85-114%. Relative standard deviation (n=3) of extraction repeatability is in the range of 1.9-3.0%. Relative standard deviation of extraction tubes (n=3) is in the range of 12-19%. The extraction mechanism is probably related to hydrophobic, π-π and dipole-dipole interactions between ionic liquids coating and estrogens analytes.

  17. Development and application of a new solid-phase microextraction fiber by sol-gel technology on titanium wire.

    PubMed

    Es-haghi, Ali; Hosseini, Seyed Maryam; Khoshhesab, Zahra Monsef

    2012-09-12

    Novel solid-phase microextraction fibers were prepared based on sol-gel technique. Commonly used fused silica substrate was replaced by titanium wire which provided high strength and longer fiber life cycle. Titanium isopropoxide was employed as the precursor which provides a sol solution containing Ti-OH groups and shows more tendencies to the molecularly similar group on the substrate. Three different polymers, poly (dimethylsiloxane) (PDMS), poly(ethylenepropyleneglycol)-monobutyl ether (Ucon) and polyethylene glycol (PEG) were employed as coating polymer in preparing three different fibers. The applicability of these fibers was assessed for the headspace SPME (HS-SPME) of benzene, toluene, ethylbenzene and xylenes (BTEX) from water sample followed by gas chromatography-mass spectrometry (GC-MS). Effects of different parameters such as fiber coating type, extraction condition, desorption condition were investigated and optimized. Under the optimized conditions, LODs and LOQs of 0.75-10 μg L(-1) (S/N=3) and 1-20 μg L(-1) (S/N=10) were respectively obtained. The method showed linearity in the range of 10-25,000 μg L(-1) with correlation coefficient of >0.99. The relative standard deviation was less than 8%.

  18. Application of β-cyclodextrin-modified, carbon nanotube-reinforced hollow fiber to solid-phase microextraction of plant hormones.

    PubMed

    Song, Xin-Yue; Ha, Wei; Chen, Juan; Shi, Yan-Ping

    2014-12-29

    A new, efficient, and environmental friendly solid-phase microextraction (SPME) medium based on β-cyclodextrin (β-CD)-modified carbon nanotubes (CNTs) and a hollow fiber (HF) was prepared. Functionalized β-CD was covalently linked to the surface of the carboxylic CNTs and then the obtained nanocomposite was immobilized into the wall pores of HFs under ultrasonic-assisted effect. The scanning electron microscope was used to inspect surface characteristics of fibers, demonstrating the presence of nanocomposites in their wall pores. The reinforced HF was employed in SPME, and its extraction performance was evaluated by analyzing 1-naphthaleneacetic acid (NAA) and 2-naphthoxyacetic acid (2-NOA) in vegetables. Without any tedious clean-up procedure, analytes were extracted from the sample to the adsorbent and organic solvent immobilized in HFs and then desorbed in acetonitrile prior to chromatographic analysis. Under the optimized extraction conditions, the method provided 275- and 283-fold enrichment factors of NAA and 2-NOA, low limits of detection and quantification (at an ngg(-1) level), satisfactory spiked recoveries, good inter-fiber repeatability, and batch-to-batch reproducibility. The selectivity of the developed fiber was investigated to three structurally similar compounds and two reference compounds with recognition coefficients up to 3.18. The obtained results indicate that the newly developed fiber is a feasible, selective, green, and cost-effective microextraction medium and could be successfully applied for extraction and determination of naphthalene-derived plant hormones in complex matrices.

  19. Facile modification of multi-walled carbon nanotubes-polymeric ionic liquids-coated solid-phase microextraction fibers by on-fiber anion exchange.

    PubMed

    Feng, Juanjuan; Sun, Min; Bu, Yanan; Luo, Chuannan

    2015-05-08

    In situ anion exchange has been proved to be an efficient method for facile modification of polymeric ionic liquids (PILs)-based stationary phases. In this work, an on-fiber anion exchange process was utilized to tune the extraction performance of a multi-walled carbon nanotubes (MWCNTs)-poly(1-vinyl-3-octylimidazolium bromide) (poly(VOIm(+)Br(-)))-coated solid-phase microextraction (SPME) fiber. MWCNTs were first coated onto the stainless steel wire through a layer-by-layer fabrication method and then the PILs were coated onto the MWCNTs physically. Anion of the MWCNTs-poly(VOIm(+)Br(-)) fiber was changed into bis(triflroromethanesulfonyl)imide (NTf2(-)) and 2-naphthalene-sulfonate (NapSO3(-)) by on-fiber anion exchange. Coupled to gas chromatography, the MWCNTs-poly(VOIm(+)Br(-)) fiber showed acceptable extraction efficiency for hydrophilic and hydrogen-bonding-donating alcohols, with limits of detection (LODs) in the range of 0.005-0.05μgmL(-1); after the anion exchange with NTf2(-), the obtained MWCNTs-poly(VOIm(+)NTf2(-)) fiber brought wide linear ranges for hydrophobic n-alkanes with correlation coefficient (R) ranging from 0.994 to 0.997; aromatic property of the fiber was enhanced by aromatic NapSO3(-) anions to get sufficient extraction capacity for phthalate esters and halogenated aromatic hydrocarbons. The MWCNTs-poly(VOIm(+)NapSO3(-)) fiber was finally applied to determine several halogenated aromatic hydrocarbons in groundwater of industrial park.

  20. Enantiomeric and non-enantiomeric monoterpenes of Juniperus communis L. and Juniperus oxycedrus needles and berries determined by HS-SPME and enantioselective GC/MS.

    PubMed

    Foudil-Cherif, Yazid; Yassaa, Noureddine

    2012-12-01

    For the first time, enantiomeric and non-enantiomeric distribution of monoterpenes in the headspace of Juniperus communis L. and Juniperus oxycedrus needles and berries has been determined using HS-SPME combined with enantioselective GC/MS. The essential oils from needles and berries of both Juniperus species obtained by hydrodistillation were also performed. HS-SPME has shown good potential to reproduce the same results as the commonly used hydrodistillation extraction technique. While needles and berries of J. communis showed high contents of sabinene, α-pinene and β-myrcene with 19-30%, 12-24% and 9-20%, respectively, J. oxycedrus was strongly dominated by α-pinene with 85-92% in both needles and berries. Large variations in chiral distribution of monoterpenes within the same plant species and between the two junipers were observed. Interestingly, similar enantiomeric preferences of monoterpenes were obtained between needles and berries of the two junipers.

  1. Application of solid phase-microextraction (SPME) and electronic nose techniques to differentiate volatiles of sesame oils prepared with diverse roasting conditions.

    PubMed

    Park, Min Hee; Jeong, Min Kyu; Yeo, JuDong; Son, Hee-Jin; Lim, Chae-Lan; Hong, Eun Jeung; Noh, Bong-Soo; Lee, JaeHwan

    2011-01-01

    Headspace volatiles of sesame oil (SO) from sesame seeds roasted at 9 different conditions were analyzed by a combination of solid phase microextraction (SPME)-gas chromatography/mass spectrometry (GC/MS), electronic nose/metal oxide sensors (MOS), and electronic nose/MS. As roasting temperature increased from 213 to 247 °C, total headspace volatiles and pyrazines increased significantly (P < 0.05). Pyrazines were major volatiles in SO and furans, thiazoles, aldehydes, and alcohols were also detected. Roasting temperature was more discrimination factor than roasting time for the volatiles in SO through the principal component analysis (PCA) of SPME-GC/MS, electronic nose/MOS, and electronic nose/MS. Electronic nose/MS showed that ion fragment 52, 76, 53, and 51 amu played important roles in discriminating volatiles in SO from roasted sesame seeds, which are the major ion fragments from pyrazines, furans, and furfurals. SO roasted at 213, 230, and 247 °C were clearly differentiated from each other on the base of volatile distribution by SPME-GC/MS, electronic nose/MOS, and electronic nose/MS analyses. Practical Application: The results of this study are ready to apply for the discriminating samples using a combinational analysis of volatiles. Not only vegetable oils prepared from roasting process but also any food sample possessing volatiles could be targets for the SPME-GC/MS and electronic nose assays. Contents and types of pyrazines in sesame seed oil could be used as markers to track down the degree of roasting and oxidation during oil preparation.

  2. Development of novel molecularly imprinted solid-phase microextraction fiber and its application for the determination of triazines in complicated samples coupled with high-performance liquid chromatography.

    PubMed

    Hu, Xiaogang; Hu, Yuling; Li, Gongke

    2007-04-13

    A novel molecularly imprinted polymer (MIP) coated solid-phase microextraction (SPME) fiber that could be coupled directly to high-performance liquid chromatography (HPLC) was prepared with prometryn as the template molecule. The characteristics and application of this fiber were investigated. Electron microscope photographs indicated that the MIP coating with average thickness of 25.0 microm was homogeneous and porous. The extraction yield of prometryn with the MIP-coated fibers was 10 times as much as that with the non-imprinted polymer (NIP) coated fibers. And special selectivity to other triazines which have similar structure to prometryn was discovered with the MIP-coated fibers. A method for the determination of triazines by the MIP-coated SPME coupled with HPLC was developed. The optimized extraction conditions were studied. Detection limits for the triazines studied were within the range of 0.012-0.090 microg/L. The method was applied to five triazines determination in the spiked soybean, corn, lettuce, and soil samples with the recoveries of 78.0-103.5%, 82.4-113.4%, 75.5-83.4%, and 81.0-106.1%, respectively. The MIP-coated fibers are suitable for the selective extraction of trace triazines in complicated samples.

  3. A new poly(phthalazine ether sulfone ketone)-coated fiber for solid-phase microextraction to determine nitroaromatic explosives in aqueous samples.

    PubMed

    Guan, Wenna; Xu, Feng; Liu, Wenmin; Zhao, Jinghong; Guan, Yafeng

    2007-04-13

    A novel polar solid-phase microextraction (SPME) fiber coated with poly(phthalazine ether sulfone ketone) (PPESK) was prepared by immersion precipitation technique. The microstructure of the coating exhibits a sponge-like sublayer supporting a dense cracking shaped top layer (about 1 microm in thickness). This coating shows long lifetime (up to 100 times) and is stable at desorption temperature up to 290 degrees C due to the rigid aromatic rings in chemical structure. We evaluated the extraction-desorption properties of the PPESK fiber for nitroaromatic explosives in aqueous samples. The parameters affecting the extraction were optimized, including extraction temperature and time, salt addition, desorption temperature and time. Limits of detection (LOD), precisions and linear dynamic range for the analysis of explosives by SPME-GC/TSD or ECD were evaluated. Limits of detection of the new fiber was three orders of magnitude lower than those with carbowax/divinylbenzene (CW/DVB), and the relative standard deviation (RSD) of single fiber and fiber-to-fiber were less than 9.3 and 10.4%, respectively. The results demonstrated that the PPESK coating exhibited high extraction efficiency for nitroaromatic compounds due to the pi-pi interaction, dipole-dipole interactions and interactions by polar functional groups. The method was applied to the analysis of nitroaromatic explosives in real aqueous samples including seawater and groundwater samples, with relative recoveries better than 90.7%.

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

    PubMed

    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 (p<0.05). Benzaldehyde decreased from 2934.6±272.5 ng/g (raw almonds) 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.

  5. HS-SPME-GC-FID method for detection and quantification of Bacillus cereus ATCC 10702 mediated 2-acetyl-1-pyrroline.

    PubMed

    Deshmukh, Yogita; Khare, Puja; Patra, D D; Nadaf, Altafhusain B

    2014-01-01

    A rapid micro-scale solid-phase micro-extraction (SPME) procedure coupled with gas-chromatography with flame ionized detector (GC-FID) was used to extract parts per billion levels of a principle basmati aroma compound "2-acetyl-1-pyrroline" (2-AP) from bacterial samples. In present investigation, optimization parameters of bacterial incubation period, sample weight, pre-incubation time, adsorption time, and temperature, precursors and their concentrations has been studied. In the optimized conditions, detection of 2-AP produced by Bacillus cereus ATCC10702 using only 0.5 g of sample volume was 85 μg/kg. Along with 2-AP, 15 other compounds produced by B. cereus were also reported out of which 14 were reported for the first time consisting mainly of (E)-2-hexenal, pentadecanal, 4-hydroxy-2-butanone, n-hexanal, 2-6-nonadienal, 3-methoxy-2(5H) furanone and 2-acetyl-1-pyridine and octanal. High recovery of 2-AP (87 %) from very less amount of B. cereus samples was observed. The method is reproducible fast and can be used for detection of 2-AP production by B. cereus.

  6. Evaluation of Residual Diazinon and Chlorpiryfos in Children Herbal Medicines by Headspace-SPME and GC-FID.

    PubMed

    Mosaddegh, Mohammad Hossein; Emami, Fakhrossadat; Asghari, Gholamreza

    2014-01-01

    The oldest method for the managing of the illness is the use of medicinal plants. The use of herbal products as the first choice in self-treatment of minor conditions continues to expand rapidly across Iran. This makes the safety of herbal products an important public health issue. Pesticides are used widely in agriculture to increase the production by controlling the harmful insects and disease vectors, however it has some hazards on biological system of human especially children. The present study was designed to examine the residual amount of organophosphorus pesticides (Diazinon and Chlorpyrifos) in children herbal medicines available in the Iranian market. Five children herbal medicine liquid dosage forms were purchased from pharmacy store. They were extracted with SPME (Solid Phase Microextraction) using the PDMS-DVB fibre. Then the extracts were injected into a GC. The gas chromatograph was Younglin model YL 6100 equipped with a flame ionization detector. The column was Technokroma 60 m length, 0.53 mm internal diameter and 1.25 µm film coated. The presence and quantity of Diazinon and Chlorpyrifos were evaluated using their standard curves. Trace amounts of chlorpyrifos and diazinon were detected in a few herbal medicines. Based on European pharmacopeia, threshold limits of chlorpyrifos and diazinon residues for medicinal plant materials are 0.2 and 0.5 mg/Kg, respectively. Our analysis results showed that residue limits of these two pesticides in five children herbal medicines are ignorable.

  7. Identification of volatile components in Chinese Sinkiang fermented camel milk using SAFE, SDE, and HS-SPME-GC/MS.

    PubMed

    Ning, Li; Fu-Ping, Zheng; Hai-Tao, Chen; Si-Yuan, Liu; Chen, Gu; Zhen-Yang, Song; Bao-Guo, Sun

    2011-12-01

    The volatile components of Chinese Sinkiang fermented camel milk were isolated by solvent assisted flavour evaporation (SAFE), simultaneous distillation extraction (SDE, dichloromethane and diethyl ether as solvent, respectively) and headspace solid-phase microextraction (HS-SPME, CAR/PDMS, PDMS/DVB and DVB/CAR/PDMS fibre extraction, respectively) and analysed by GC/MS. A total of 133 volatile components were identified under 6 different conditions, including 30 esters, 20 acids, 18 saturated alcohols, 15 unsaturated aliphatic alcohols, 8 saturated ketones, 9 saturated aldehydes, 8 unsaturated aliphatic aldehydes, 6 furans, 5 sulphur-containing compounds, 5 ethers, 5 lactones, 3 other compounds, and 1 unsaturated aliphatic ketone. Three pretreatment methods were compared, assisted by principal component analysis (PCA). The results indicated that the volatile components obtained using different methods varied greatly both in categories and in content, and therefore, a multi-pretreatment method should be adopted together with GC/MS. A total of 71 aroma-active compounds were detected by gas chromatography-olfactometry (GC-O), among which 66 aroma-active compounds were found by SDE (60, dichloromethane as solvent; 24, diethyl ether as solvent), 26 by SAFE.

  8. Formation of the aroma of a raw goat milk cheese during maturation analysed by SPME-GC-MS.

    PubMed

    Delgado, Francisco José; González-Crespo, José; Cava, Ramón; Ramírez, Rosario

    2011-12-01

    The volatile profile of the Spanish goat raw milk cheese of the protected designation of origin (PDO) "Queso Ibores" was studied at four stages of maturation (day 1, 30, 60, and 90) by the method of solid-phase micro-extraction-gas chromatography-mass spectrometry (SPME-GC-MS) to determinate the characteristic volatile compounds of this cheese and to know the changes in the volatile profile of this cheese during maturation. According to the PDO, Ibores cheese aroma varies between sweet and mild and it has a strong taste, slightly tart. A total of 64 compounds were detected: 14 acids, 18 alcohols, 13 esters, 6 ketones and 13 compounds which could not be classified in these groups. Carboxylic acids were the most abundant volatile compounds in the headspace of Ibores cheese. Content of volatile compounds was significantly modified (P<0.05) during ripening. The relative total amounts of acids, esters and ketones increased during the first 60days of maturation. The most characteristic compounds of Ibores cheese aroma were butanoic, hexanoic and octanoic acids, some alcohols (2-butanol and 2-heptanol), ethyl esters of hexanoic and butanoic acids, some methyl ketones (2-butanone, 2-pentanone and 2-heptanone) and δ-decalactone.

  9. Statistical analysis for improving data precision in the SPME GC-MS analysis of blackberry (Rubus ulmifolius Schott) volatiles.

    PubMed

    D'Agostino, M F; Sanz, J; Martínez-Castro, I; Giuffrè, A M; Sicari, V; Soria, A C

    2014-07-01

    Statistical analysis has been used for the first time to evaluate the dispersion of quantitative data in the solid-phase microextraction (SPME) followed by gas chromatography-mass spectrometry (GC-MS) analysis of blackberry (Rubus ulmifolius Schott) volatiles with the aim of improving their precision. Experimental and randomly simulated data were compared using different statistical parameters (correlation coefficients, Principal Component Analysis loadings and eigenvalues). Non-random factors were shown to significantly contribute to total dispersion; groups of volatile compounds could be associated with these factors. A significant improvement of precision was achieved when considering percent concentration ratios, rather than percent values, among those blackberry volatiles with a similar dispersion behavior. As novelty over previous references, and to complement this main objective, the presence of non-random dispersion trends in data from simple blackberry model systems was evidenced. Although the influence of the type of matrix on data precision was proved, the possibility of a better understanding of the dispersion patterns in real samples was not possible from model systems. The approach here used was validated for the first time through the multicomponent characterization of Italian blackberries from different harvest years.

  10. Identification of volatile components of liverwort (Porella cordaeana) extracts using GC/MS-SPME and their antimicrobial activity.

    PubMed

    Bukvicki, Danka; Gottardi, Davide; Veljic, Milan; Marin, Petar D; Vannini, Lucia; Guerzoni, Maria Elisabetta

    2012-06-06

    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.

  11. Metal-organic framework UiO-66 coated stainless steel fiber for solid-phase microextraction of phenols in water samples.

    PubMed

    Shang, Hai-Bo; Yang, Cheng-Xiong; Yan, Xiu-Ping

    2014-08-29

    Effective solid-phase microextraction (SPME) of polar phenols from water samples is usually difficult due to the strong interaction between polar phenols and aqueous matrix. Here, we report the fabrication of a metal-organic framework UiO-66 coated stainless steel fiber via physical adhesion for the SPME of polar phenols (phenol, o-cresol, p-cresol, 2,6-dimethylphenol, 2,4-dichlorophenol and 2,6-dichlorophenol) in water samples before gas chromatographic separation with flame ionic detection. Headspace SPME of 10mL sample solution with the fabricated UiO-66 coated fiber gave the enhancement factors of 160 (phenol) - 3769 (2,4-dichlorophenol), and the linear ranges of 1-1000μgL(-1) (2,6-dimethylphenol, 2,4-dichlorophenol and 2,6-dichlorophenol), 1-500μgL(-1) (o-cresol and p-cresol) and 5-500μgL(-1) (phenol). The detection limits ranged from 0.11μgL(-1) (2,6-dimethylphenol) to 1.23μgL(-1) (phenol). The precision (relative standard deviations, RSDs) for six replicate determinations of the analytes at 100μgL(-1) using a single UiO-66 coated fiber ranged from 2.8% to 6.2%. The fiber-to-fiber reproducibility (RSDs) for three parallel UiO-66 coated fibers varied from 5.9% to 10%. The recoveries obtained by spiking 5μgL(-1) of the phenols in the water samples ranged from 80% to 115%.

  12. Development of a solid-phase microextraction fiber by chemical binding of polymeric ionic liquid on a silica coated stainless steel wire.

    PubMed

    Pang, Long; Liu, Jing-Fu

    2012-03-23

    A novel approach was developed for the fabrication of solid-phase microextraction (SPME) fiber by coating stainless steel fiber with a polymeric ionic liquid (PIL) through covalent bond. The stainless steel fiber was sequentially coated with a gold film by replacement reaction between Fe and Au when immerged in chloroauric acid, assembled with a monolayer of 3-(mercaptopropyl) triethoxysilane on the gold layer through the Au-S bond, and coated with a silica layer by the hydrolysis and polycondensation reaction of the surface-bonded siloxane moieties and the active silicate solution. Then, 1-vinyl-3-(3-triethoxysilylpropyl)-4,5-dihydroimidazolium chloride ionic liquid was anchored on the silica layer by covalent bond, and the PIL film was further formed by free radical copolymerization between 1-vinyl-3-(3-triethoxysilylpropyl)-4,5-dihydroimidazdium and vinyl-substituted imidazolium with azobisisobutyronitrile (AIBN) as initiator. Parameters influencing the preparation of PIL fiber were optimized, and the developed SPME fiber has a coating thickness of ~20 μm with good thermal stability and long lifetime. The performance of the PIL fiber was evaluated by analysis of polycyclic aromatic hydrocarbons (PAHs) in water samples. The developed PIL fiber showed good linearity between 0.5 and 20 μg l(-1) with regression coefficient in the range of 0.963-0.999, detection limit ranging from 0.05 to 0.25 μg l(-1), and relative standard deviation of 9.2-29% (n=7). This developed PIL fiber exhibited comparable analytical performance to commercial 7 μm thickness PDMS fiber in the extraction of PAHs. The spiked recoveries for three real water samples at 0.5-5 μg l(-1) levels were 49.6-111% for the PIL fiber and 40.8-103% for the commercial PDMS fiber.

  13. Two Fiber Optical Fiber Thermometry

    NASA Technical Reports Server (NTRS)

    Jones, Mathew R.; Farmer, Jeffery T.; Breeding, Shawn P.

    2000-01-01

    An optical fiber thermometer consists of an optical fiber whose sensing tip is given a metallic coating. The sensing tip of the fiber is essentially an isothermal cavity, so the emission from this cavity will be approximately equal to the emission from a blackbody. Temperature readings are obtained by measuring the spectral radiative heat flux at the end of the fiber at two wavelengths. The ratio of these measurements and Planck's Law are used to infer the temperature at the sensing tip. Optical fiber thermometers have high accuracy, excellent long-term stability and are immune to electromagnetic interference. In addition, they can be operated for extended periods without requiring re-calibration. For these reasons. it is desirable to use optical fiber thermometers in environments such as the International Space Station. However, it has recently been shown that temperature readings are corrupted by emission from the fiber when extended portions of the probe are exposed to elevated temperatures. This paper will describe several ways in which the reading from a second fiber can be used to correct the corrupted temperature measurements. The accuracy and sensitivity to measurement uncertainty will be presented for each method.

  14. Disposable Polydimethylsiloxane (PDMS)-Coated Fused Silica Optical Fibers for Sampling Pheromones of Moths

    PubMed Central

    Lievers, Rik; Groot, Astrid T.

    2016-01-01

    In the past decades, the sex pheromone composition in female moths has been analyzed by different methods, ranging from volatile collections to gland extractions, which all have some disadvantage: volatile collections can generally only be conducted on (small) groups of females to detect the minor pheromone compounds, whereas gland extractions are destructive. Direct-contact SPME overcomes some of these disadvantages, but is expensive, the SPME fiber coating can be damaged due to repeated usage, and samples need to be analyzed relatively quickly after sampling. In this study, we assessed the suitability of cheap and disposable fused silica optical fibers coated with 100 μm polydimethylsiloxane (PDMS) by sampling the pheromone of two noctuid moths, Heliothis virescens and Heliothis subflexa. By rubbing the disposable PDMS fibers over the pheromone glands of females that had called for at least 15 minutes and subsequently extracting the PDMS fibers in hexane, we collected all known pheromone compounds, and we found a strong positive correlation for most pheromone compounds between the disposable PDMS fiber rubs and the corresponding gland extracts of the same females. When comparing this method to volatile collections and the corresponding gland extracts, we generally found comparable percentages between the three techniques, with some differences that likely stem from the chemical properties of the individual pheromone compounds. Hexane extraction of cheap, disposable, PDMS coated fused silica optical fibers allows for sampling large quantities of individual females in a short time, eliminates the need for immediate sample analysis, and enables to use the same sample for multiple chemical analyses. PMID:27533064

  15. Preparation of solid-phase microextraction fibers by in-mold coating strategy for derivatization analysis of 24-epibrassinolide in pollen samples.

    PubMed

    Pan, Jialiang; Hu, Yuling; Liang, Tingan; Li, Gongke

    2012-11-02

    A novel and simple in-mold coating strategy was proposed for the preparation of uniform solid-phase microextraction (SPME) coatings. Such a strategy is based on the direct synthesis of the polymer coating on the surface of a solid fiber using a glass capillary as the mold. The capillary was removed and the polymer with well-controlled thickness could be coated on the silica fiber reproductively. Following the strategy, a new poly(acrylamide-co-ethylene glycol dimethacrylate) (poly(AM-co-EGDMA)) coating was prepared for the preconcentration of 24-epibrassinolide (24-epiBL) from plant matrix. The coating had the enrichment factor of 32 folds, and the extraction efficiency per unit thickness was 5 times higher than that of the commercial polydimethylsiloxane/divinylbenzene (PDMS/DVB) coating. A novel method based on SPME coupled with derivatization and large volume injection-high performance liquid chromatography (LVI-HPLC) was developed for the analysis of 24-epiBL. The linear range was 0.500-20.0 μg/L with the detection limit of 0.13 μg/L. The amounts of endogenous 24-epiBL in rape and sunflower breaking-wall pollens samples were determined with satisfactory recovery (77.8-104%) and reproducibility (3.9-7.9%). The SPME-DE/LVI-HPLC method is rapid, reliable, convenient and applicable for complicated plant samples.

  16. Fireblocking Fibers

    NASA Technical Reports Server (NTRS)

    1986-01-01

    PBI was originally developed for space suits. In 1980, the need for an alternative to asbestos and stricter government anti-pollution standards led to commercialization of the fire blocking fiber. PBI is used for auto racing driver suits and aircraft seat covers. The fiber does not burn in air, is durable and easily maintained. It has been specified by a number of airliners and is manufactured by Hoechst-Celanese Corporation.

  17. Dietary fiber.

    PubMed

    Madar, Z; Thorne, R

    1987-01-01

    Studies done on dietary fiber (DF) over the past five years are presented in this Review. The involvement of dietary fiber in the control of plasma glucose and lipid levels is now established. Two dietary fiber sources (soybean and fenugreek) were studied in our laboratory and are discussed herein. These sources were found to be potentially beneficial in the reduction of plasma glucose in non-insulin dependent diabetes mellitus subjects. They are shown to be acceptable by human subjects and are easy to use either in a mixture of milk products and in cooking. The mechanism by which dietary fiber alters the nutrient absorption is also discussed. The effect of DF on gastric emptying, transit time, adsorption and glucose transport may contribute to reducing plasma glucose and lipid levels. DF was found to be effective in controlling blood glucose and lipid levels of pregnant diabetic women. Dietary fiber may also be potentially beneficial in the reduction of exogenous insulin requirements in these subjects. However, increased consumption of DF may cause adverse side effects; the binding capabilities of fiber may affect nutrient availability, particularly that of minerals and prolonged and high DF dosage supplementation must be regarded cautiously. This is particularly true when recommending such a diet for pregnant or lactating women, children or subjects with nutritional disorders. Physiological effects of DF appear to depend heavily on the source and composition of fiber. Using a combination of DF from a variety of sources may reduce the actual mass of fiber required to obtain the desired metabolic effects and will result in a more palatable diet. Previously observed problems, such as excess flatus, diarrhea and mineral malabsorption would also be minimized.

  18. Nanocomposite Fibers

    DTIC Science & Technology

    2003-01-01

    attempts to prepare carbon nanotube , CNT, containing fiber material. Modulus and tenacity tests on experimentally prepared nanosilica filled PET...individual entities of nanofibers, such as carbon nanotubes and SiC whiskers, silica and clay, into polymers with the goal of producing new forms of...if carbon nanotube (CNT) particle implanted fibers are used, one would expect a great increase in the electrical conductivity of the so-reinforced

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

    NASA Astrophysics Data System (ADS)

    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. Validation of SPME-GCMS method for the analysis of virgin olive oil volatiles responsible for sensory defects.

    PubMed

    Romero, I; García-González, D L; Aparicio-Ruiz, R; Morales, M T

    2015-03-01

    Volatile compounds are responsible for the aroma of virgin olive oil and also for its quality. The high number and different nature of volatile compounds drive to the need of a reliable analytical method that allows their proper quantification to explain the standard method of panel test. Although there are some analytical solutions available, they have not been validated and the regulatory bodies are reluctant to adopt them since they can be subjected to unknown errors. In this regards, the European Union has encouraged the validation of these analytical tools through the research program Horizon2020, which involves gaining knowledge from the analytical properties of the chemical methods for sensory assessment. This work is focused on the analytical validation of the methodology used to determine the actual concentration of volatiles in virgin olive oils when applying SPME-GCMS. The validation process includes the calibration curves for 29 volatile compounds responsible for the most common sensory perceptions in virgin olive oils, the determination of their working ranges with linear response, the detection and quantification limits, the sensitivity, the accuracy estimated as trueness and precision and the selectivity. Sixty-seven percent of the compounds presented a relative standard deviation in repeatability lower than 10%, and this percentage rises to 95% in lampante virgin olive oils. The accuracy was established in 97% of the studied volatile compounds. Finally, an empirical example of the ability of the method to discriminate virgin olive oils of different categories (extra virgin, virgin, ordinary and lampante) by the quantification of their volatiles is provided.

  1. A solid-phase microextraction fiber with carbon nanoparticles as sorbent material prepared by a simple flame-based preparation process.

    PubMed

    Sun, Min; Feng, Juanjuan; Qiu, Huamin; Fan, Lulu; Li, Leilei; Luo, Chuannan

    2013-07-26

    A novel carbon nanoparticles-coated solid-phase microextraction (SPME) fiber was prepared via a simple and low-cost flame-based preparation process, with stainless steel wire as support. Surface characteristic of the fiber was studied with scanning electron microscope. A nano-scaled brushy structure was observed. Coupled to gas chromatography (GC), the fiber was used to extract phthalate esters (PAEs) and polycyclic aromatic hydrocarbons (PAHs) in aqueous samples. Analytical performances of the proposed method were investigated under the optimum extraction conditions (extraction temperature, 40°C; content of KCl, 30% (w/v); extraction time, 50min for PAEs and 40min for PAHs) and compared with other reports for the same analytes. Calibration ranges were 0.06-500μgL(-1) for di-n-butyl phthalate (DBP), and 0.1-300μgL(-1) for di-cyclohexyl phthalate (DCHP) and di-(2-ethyl-hexyl) phthalate (DEHP). For the eight PAHs, good linearity was obtained ranging from 0.01 to 150μgL(-1). Limits of detection were 0.005μgL(-1) for three PAEs and 0.001-0.003μgL(-1) for eight PAHs. The fiber exhibited excellent stability. It can be used for 100 times with RSDs of extraction efficiency less than 22.4%. The as-established SPME-GC method was applied to determine PAEs in food-wrap and PAHs in cigarette ash and snow water, and satisfactory results were obtained. The carbon nanoparticles-coated SPME fiber was efficient for sampling of organic compounds from aqueous samples.

  2. Hollow fiber membrane-coated functionalized polymeric ionic liquid capsules for direct analysis of estrogens in milk samples.

    PubMed

    Feng, Juanjuan; Sun, Min; Bu, Yanan; Luo, Chuannan

    2016-02-01

    Protein removal process is always time-consuming for the analysis of milk samples. In this work, hollow fiber membrane-coated functionalized polymeric ionic liquid (HF-PIL) capsules were synthesized and used as solid-phase microextraction (SPME) sorbent for direct analysis of estrogens in milk samples. The functionalized PIL monolith sorbent was obtained by copolymerization between 1-(3-aminopropyl)-3-(4-vinylbenzyl)imidazolium 4-styrenesulfonate IL monomer and 1,6-di(3-vinylimidazolium) hexane bishexafluorophosphate IL-crosslinking agent. A group of four capsules were installed as SPME device, to determine four kinds of estrogens (estrone, diethylstilbestrol, hexestrol, and 17α-ethynylestradiol) in milk samples, coupled to high performance liquid chromatography. Extraction and desorption conditions were optimized to get satisfactory extraction efficiency. Good linearity was obtained in the range of 5-200 μg L(-1). The limits of detection were 1 μg L(-1) for diethylstilbestrol and 2 μg L(-1) for 17α-ethynylestradiol, estrone, and hexestrol. The present method was applied to analyze the model analytes in different milk samples. Relative recoveries were in the range of 85.5-112%. The HF-PIL SPME capsules showed satisfactory extraction efficiency and high resistance to sample matrix interference.

  3. Mechanisms of Neutral and Anionic Surfactant Sorption to Solid-Phase Microextraction Fibers.

    PubMed

    Haftka, Joris J-H; Hammer, Jort; Hermens, Joop L M

    2015-09-15

    Octanol-water partitioning (Kow) is considered a key parameter for hydrophobicity and is often applied in the prediction of the environmental fate and exposure of neutral organic compounds. However, surfactants can create difficulties in the determination of Kow because of emulsification of both water and octanol phases. Moreover, not only is sorption behavior of ionic surfactants related to hydrophobicity, but also other interactions are relevant in sorption processes. A different approach to develop parameters that can be applied in predictive modeling of the fate of surfactants in the environment is therefore required. Distribution between solid-phase microextraction (SPME) fibers and water was used in this study to measure the affinity of surfactants to a hydrophobic phase. Fiber-water sorption coefficients of alcohol ethoxylates, alkyl carboxylates, alkyl sulfates, and alkyl sulfonates were determined at pH 7 by equilibration of the test analytes between fiber and water. Distribution between fiber and water of anionic compounds with pKa ∼ 5 (i.e., alkyl carboxylates) was dominated by the neutral fraction. Anionic surfactants with pKa ≤ 2 (i.e., alkyl sulfates and alkyl sulfonates) showed strong nonlinear distribution to the fiber. The fiber-water sorption coefficients for alcohol ethoxylates and alkyl sulfates showed a linear trend with bioconcentration factors from the literature. Fiber-water sorption coefficients are promising as a parameter to study the effects of hydrophobicity and other potential interactions on sorption behavior of neutral and anionic surfactants.

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

    SciTech Connect

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

    2009-05-23

    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{sup 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{sup -1} to 0.05 {mu}g L{sup -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{sup -1}. to 0.022 ng L{sup -1}. This methodology is applicable for in vivo determination of odor-causing chemicals associated with emissions of volatiles from insects.

  5. The evolution of volatile compounds profile of "Toscano" dry-cured ham during ripening as revealed by SPME-GC-MS approach.

    PubMed

    Pugliese, C; Sirtori, F; Calamai, L; Franci, O

    2010-09-01

    The volatile compounds profile is an important feature for the characterization of dry-cured hams. Some minor typical Italian products, such as 'Toscano' ham, have been poorly studied in regards to their composition of volatile compounds. In this article, we studied the evolution of the aromatic profile of 'Toscano' dry-cured ham by solid-phase microextraction-gas chromatographic-mass spectrometry (SPME-GC-MS) with ripening. Ten right thighs were cured according to the 'Toscano' PDO protocol, sampled at 0, 1, 3, 6 and 12 months and submitted to volatile compounds analysis by SPME with a Divinylbenzene (DVB)/Carboxen/Polydimethylsiloxane (PDMS) 75-µ Stable Flex fibre. An Agilent 5975C mass selective detector (MSD) spectrometer with electron ionization (EI) source operating in scan mode within the m/z 29-350 range was used for data collection. Seven internal standards, either deuterium labeled or absent in the specimens and chosen to represent low or high boiling esters, alcohols, acids or phenols, were added to the homogenized samples and used to normalize the SPME fibre response to account for response changes upon wearing. Linear calibrations were obtained in this way for selected representative compounds. Over 60 compounds belonging to esters, aldehydes, organic acids, ketones and alcohols were identified by comparison with spectral libraries and Kovats indices. Aldehydes were the most represented chemical family, followed by organic acids, alcohols, ketones and esters. The aldehydes and ketones increased during the first 3 months, when the larger formation of volatiles occurred. For other families, the evolution over time was less evident. The principal component and discriminant analyses of the aromatic profile were effective in classifying the hams at 0, 6 or 12 months of ripening while for 1 and 3 months' samples a partial overlapping was shown. These results represent the first characterization of 'Toscano' ham and may constitute the basis to identify the

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

    NASA Astrophysics Data System (ADS)

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

    2009-05-01

    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 (R2>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.

  7. Photovoltaic fibers

    NASA Astrophysics Data System (ADS)

    Gaudiana, Russell; Eckert, Robert; Cardone, John; Ryan, James; Montello, Alan

    2006-08-01

    It was realized early in the history of Konarka that the ability to produce fibers that generate power from solar energy could be applied to a wide variety of applications where fabrics are utilized currently. These applications include personal items such as jackets, shirts and hats, to architectural uses such as awnings, tents, large covers for cars, trucks and even doomed stadiums, to indoor furnishings such as window blinds, shades and drapes. They may also be used as small fabric patches or fiber bundles for powering or recharging batteries in small sensors. Power generating fabrics for clothing is of particular interest to the military where they would be used in uniforms and body armor where portable power is vital to field operations. In strong sunlight these power generating fabrics could be used as a primary source of energy, or they can be used in either direct sunlight or low light conditions to recharge batteries. Early in 2002, Konarka performed a series of proof-of-concept experiments to demonstrate the feasibility of building a photovoltaic cell using dye-sensitized titania and electrolyte on a metal wire core. The approach taken was based on the sequential coating processes used in making fiber optics, namely, a fiber core, e.g., a metal wire serving as the primary electrode, is passed through a series of vertically aligned coating cups. Each of the cups contains a coating fluid that has a specific function in the photocell. A second wire, used as the counter electrode, is brought into the process prior to entering the final coating cup. The latter contains a photopolymerizable, transparent cladding which hardens when passed through a UV chamber. Upon exiting the UV chamber, the finished PV fiber is spooled. Two hundred of foot lengths of PV fiber have been made using this process. When the fiber is exposed to visible radiation, it generates electrical power. The best efficiency exhibited by these fibers is 6% with an average value in the 4

  8. Analytical Determination of KDOC-Values of Polycyclic Musk Compounds with HS-SPME and GC/MS/MS

    NASA Astrophysics Data System (ADS)

    Böhm, L.; Düring, R.-A.

    2009-04-01

    Polycyclic musk compounds, used as fragrances in cosmetics and detergents, get into rivers via domestic wastewater and sewage treatment plants and with sewage sludge as fertilizer into soils. Because of their persistence and lipophilic character they accumulate in biota, so they are pollutants with environmental relevance. The coefficient KDOC is used to quantify the distribution of substances between aqueous phase and dissolved organic matter (DOM) which is quantified by the determination of dissolved organic carbon (DOC). DOM is of specific relevance for the transport and fate of persistent and lipophilic compounds in the environment. The affinity to DOM increases, the more lipophilic a substance is. So the environmental mobility is enhanced with increasing binding on DOM. For that reason, measured KDOC-values are important to predict the fate and behaviour of chemicals in the environment and should be used for environmental fate modelling purposes. LITZ ET AL. (2007) state that, to carry out a risk-assessment for polycyclic musk compounds, further research on their sorption-behaviour is necessary. For the determination of KDOC-values, different concentrations of humic acid were spiked with a multi-component stock solution. The samples were analysed with headspace solid-phase microextraction in combination with gas chromatography coupled with mass spectrometry (HS-SPME GC/MS/MS). The KDOC-values were calculated according to YABUTA ET AL. (2004). The method was validated with single substance stock solutions and with polycyclic aromatic hydrocarbons (PAHs). The results show that the method is applicable, repeatable and suitable to get KDOC-values for many substances very fast, cheap and solvent-free. With our results KDOC-values for polycyclic musk compounds were determined for the first time. Literature LITZ, N. TH., MüLLER, J. AND BöHMER, W. (2007): Occurrence of Polycyclic Musks in Sewage Sludge and their Behaviour in Soils and Plants. Part 2: Investigation

  9. Preliminary construction of integral analysis for characteristic components in complex matrices by in-house fabricated solid-phase microextraction fibers combined with gas chromatography-mass spectrometry.

    PubMed

    Tang, Zhentao; Hou, Wenqian; Liu, Xiuming; Wang, Mingfeng; Duan, Yixiang

    2016-08-26

    Integral analysis plays an important role in study and quality control of substances with complex matrices in our daily life. As the preliminary construction of integral analysis of substances with complex matrices, developing a relatively comprehensive and sensitive methodology might offer more informative and reliable characteristic components. Flavoring mixtures belonging to the representatives of substances with complex matrices have now been widely used in various fields. To better study and control the quality of flavoring mixtures as additives in food industry, an in-house fabricated solid-phase microextraction (SPME) fiber was prepared based on sol-gel technology in this work. The active organic component of the fiber coating was multi-walled carbon nanotubes (MWCNTs) functionalized with hydroxyl-terminated polydimethyldiphenylsiloxane, which integrate the non-polar and polar chains of both materials. In this way, more sensitive extraction capability for a wider range of compounds can be obtained in comparison with commercial SPME fibers. Preliminarily integral analysis of three similar types of samples were realized by the optimized SPME-GC-MS method. With the obtained GC-MS data, a valid and well-fit model was established by partial least square discriminant analysis (PLS-DA) for classification of these samples (R2X=0.661, R2Y=0.996, Q2=0.986). The validity of the model (R2=0.266, Q2=-0.465) has also approved the potential to predict the "belongingness" of new samples. With the PLS-DA and SPSS method, further screening out the markers among three similar batches of samples may be helpful for monitoring and controlling the quality of the flavoring mixtures as additives in food industry. Conversely, the reliability and effectiveness of the GC-MS data has verified the comprehensive and efficient extraction performance of the in-house fabricated fiber.

  10. Monolithic molecular imprinted polymer fiber for recognition and solid phase microextraction of ephedrine and pseudoephedrine in biological samples prior to capillary electrophoresis analysis.

    PubMed

    Deng, Dong-Li; Zhang, Ji-You; Chen, Chen; Hou, Xiao-Ling; Su, Ying-Ying; Wu, Lan

    2012-01-06

    A novel capillary electrophoresis (CE) method coupled with monolithic molecular imprinted polymer (MIP) fiber based solid phase microextraction (SPME) was developed for selective and sensitive determination of ephedrine (E) and pseudoephedrine (PE). With in situ polymerization in a silica capillary mold and E as template, the MIP fibers could be produced in batch reproducibly and each fiber was available for 50 extraction cycles without significant decrease in extraction ability. Using the MIP fiber under optimized extraction conditions, CE detection limits of E and PE were greatly lowered from 0.20 to 0.00096 μg/mL and 0.12 to 0.0011 μg/mL, respectively. Analysis of urine and serum samples by the MIP-SPME-CE method was also performed, with results indicating that E and PE could be selectively extracted. The recoveries and relative standard deviations (RSDs) for sample analysis were found in the range of 91-104% and 3.8-9.1%, respectively.

  11. The dynamics of the HS/SPME-GC/MS as a tool to assess the spoilage of minced beef stored under different packaging and temperature conditions.

    PubMed

    Argyri, Anthoula A; Mallouchos, Athanasios; Panagou, Efstathios Z; Nychas, George-John E

    2015-01-16

    The aim of the current study was to assess meat spoilage through the evolution of volatile compounds using chemometrics. Microbiological and sensory assessment, pH measurement and headspace solid phase microextraction gas chromatography/mass spectroscopy (headspace SPME-GC/MS) analysis were carried out in minced beef stored aerobically and under modified atmosphere packaging (MAP) at 0, 5, 10, and 15 °C. It was shown that the HS/SPME-GC/MS analysis provided useful information about a great number of volatile metabolic compounds detected during meat storage. Many of the identified and semi-quantified compounds were correlated with the sensory scores through the use of chemometrics, depicting possible spoilage indicators such as 2-pentanone, 2-nonanone, 2-methyl-1-butanol, 3-methyl-1-butanol, ethyl hexanoate, ethyl propanoate, ethyl lactate, ethyl acetate, ethanol, 2-heptanone, 3-octanone, diacetyl, and acetoin. Finally, the applied GC/MS global models were able to estimate the microbial counts of the different microorganisms and the sensory scores of a meat sample regardless of storage conditions (i.e. packaging and temperature).

  12. Re-exploring the high-throughput potential of microextraction techniques, SPME and MEPS, as powerful strategies for medical diagnostic purposes. Innovative approaches, recent applications and future trends.

    PubMed

    Pereira, Jorge; Silva, Catarina Luís; Perestrelo, Rosa; Gonçalves, João; Alves, Vera; Câmara, José S

    2014-03-01

    The human population continues to grow exponentially in the fast developing and most populated countries, whereas in Western Europe it is getting older and older each year. This inevitably raises the demand for better and more efficient medical services without increasing the economic burden in the same proportion. To meet these requirements, improvement of medical diagnosis is certainly a key aspect to consider. Therefore, we need powerful analytical methodologies able to go deeper and further in the characterization of human metabolism and identification of disease biomarkers and endogenous molecules in body fluids and tissues. The ultimate goal is to have a reliable and early medical diagnosis, mitigating the disease complications as much as possible. Microextraction techniques (METs) represent a key step in these analytical methodologies by providing samples in the suitable volumes and purification levels necessary for the characterization of the target analytes. In this aspect, solid-phase microextraction (SPME) and, more recently, microextraction by packed sorbent (MEPS), are powerful sample preparation techniques, characterized by their reduced time of analysis, low solvent consumption, and broad application. Moreover, as miniaturized techniques, they can be easily automatized to have a high-throughput performance in the clinical environment. In this review, we explore some of the most interesting MEPS and SPME applications, focusing on recent trends and applications to medical diagnostic, particularly the in vivo and near real time applications.

  13. Investigation of volatiles evolution during the alcoholic fermentation of grape must using free and immobilized cells with the help of solid phase microextraction (SPME) headspace sampling.

    PubMed

    Mallouchos, Athanasios; Komaitis, Michael; Koutinas, Athanasios; Kanellaki, Maria

    2002-06-19

    A biocatalyst was prepared by immobilization of Saccharomyces cerevisiae strain AXAZ-1 on delignified cellulosic material (DCM). Repeated batch fermentations were conducted using these biocatalysts and free cells, separately, at temperatures of 20, 15, and 10 degrees C. Solid phase microextraction (SPME) was used in monitoring the formation of volatile alcohols, acetate esters, and ethyl esters of fatty acids. The kinetics of volatile production were similar for free and immobilized cells. In all cases immobilized cells showed a better rate of volatile production, which was directly connected to sugar consumption. The main difference observed was in propanol production, which increased with temperature decrease for the immobilized cells, whereas it remained constant for the free ones. In the case of immobilized cells significant amounts of esters were also produced. It is well-known that esters contribute to the fruity aroma of wine. It was also established that SPME is a very sensitive, accurate, and reliable technique and can be used without any reservation in the characterization of volatile constituents of wine.

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

    PubMed Central

    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

    2015-01-01

    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 (sapt) reference data. Various neutral molecular dimers have been tested as results on charged systems (metal cation complexes) are 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 complexe bio- or bioinorganic systems in periodic boundary conditions. PMID:26814845

  15. Metal-organic framework-199/graphite oxide hybrid composites coated solid-phase microextraction fibers coupled with gas chromatography for determination of organochlorine pesticides from complicated samples.

    PubMed

    Zhang, Suling; Du, Zhuo; Li, Gongke

    2013-10-15

    The hybrid material of a copper-based metal-organic framework (MOF-199) and graphite oxide (GO) was explored as the solid-phase microextraction (SPME) coating for the first time. This fiber was fabricated by using 3-amino-propyltriethoxysilane (APTES) as the cross-linking agent, which enhanced its durability and allowed more than 140 replicate extractions. With the incorporation of GO, the MOF-199/GO fibers with GO contents ranging from 5 to 15 wt% exhibited enhanced adsorption affinity to organochlorine pesticides (OCPs) compared to MOF or GO individually. This improvement was linked to the enhanced dispersive forces (increased volume of small pores) that provided by the dense carbon layers of GO. Combining the superior properties of high porosity of MOFs and the unique layered character of GO, the MOF-199/GO (10 wt%) fiber exhibited higher adsorption affinity to some OCPs than commercial polydimethylsiloxane (PDMS) and polydimethylsiloxane/divinylbenzene (PDMS/DVB) fibers. This new fiber was developed for headspace (HS) SPME of eight OCPs followed by GC/ECD analysis. The limits of detection were 2.3-6.9 ng/L. The relative standard deviation (RSD) for five replicate extractions using one fiber ranged from 5.3% to 8.8%. The fiber-to-fiber reproducibility was 5.2-12.8%. This method was successfully used for simultaneous determination of eight OCPs from river water, soil, water convolvulus and longan with satisfactory recoveries of 90.6-104.4%, 82.7-96.8%, 72.2-107.7% and 82.8-94.3%, respectively. These results indicated the MOF-199/GO composite provided a promising alternative in sample pretreatment.

  16. A smooth particle-mesh Ewald algorithm for Stokes suspension simulations: The sedimentation of fibers

    NASA Astrophysics Data System (ADS)

    Saintillan, David; Darve, Eric; Shaqfeh, Eric S. G.

    2005-03-01

    Large-scale simulations of non-Brownian rigid fibers sedimenting under gravity at zero Reynolds number have been performed using a fast algorithm. The mathematical formulation follows the previous simulations by Butler and Shaqfeh ["Dynamic simulations of the inhomogeneous sedimentation of rigid fibres," J. Fluid Mech. 468, 205 (2002)]. The motion of the fibers is described using slender-body theory, and the line distribution of point forces along their lengths is approximated by a Legendre polynomial in which only the total force, torque, and particle stresslet are retained. Periodic boundary conditions are used to simulate an infinite suspension, and both far-field hydrodynamic interactions and short-range lubrication forces are considered in all simulations. The calculation of the hydrodynamic interactions, which is typically the bottleneck for large systems with periodic boundary conditions, is accelerated using a smooth particle-mesh Ewald (SPME) algorithm previously used in molecular dynamics simulations. In SPME the slowly decaying Green's function is split into two fast-converging sums: the first involves the distribution of point forces and accounts for the singular short-range part of the interactions, while the second is expressed in terms of the Fourier transform of the force distribution and accounts for the smooth and long-range part. Because of its smoothness, the second sum can be computed efficiently on an underlying grid using the fast Fourier transform algorithm, resulting in a significant speed-up of the calculations. Systems of up to 512 fibers were simulated on a single-processor workstation, providing a different insight into the formation, structure, and dynamics of the inhomogeneities that occur in sedimenting fiber suspensions.

  17. Polyimide Fibers

    NASA Technical Reports Server (NTRS)

    St.Clair, Terry L. (Inventor); Fay, Catharine C. (Inventor); Working, Dennis C. (Inventor)

    1997-01-01

    A polyimide fiber having textile physical property characteristics and the process of melt extruding same from a polyimide powder. Polyimide powder formed as the reaction product of the monomers 3.4'-ODA and ODPA, and endcapped with phthalic anhydride to control the molecular weight thereof, is melt extruded in the temperature range of 340? C. to 360? C. and at heights of 100.5 inches, 209 inches and 364.5 inches. The fibers obtained have a diameter in the range of 0.0068 inch to 0.0147 inch; a mean tensile strength in the range of 15.6 to 23.1 ksi; a mean modulus of 406 to 465 ksi; and a mean elongation in the range of 14 to 103%.

  18. Polyimide Fibers

    NASA Technical Reports Server (NTRS)

    St.Clair, Terry L. (Inventor); Fay, Catharine C. (Inventor); Working, Dennis C. (Inventor)

    1998-01-01

    A polyimide fiber having textile physical property characteristics and the process of melt extruding same from a polyimide powder. Polyimide powder formed as the reaction product of the monomers 3.4'-ODA and ODPA, and end- capped with phthalic anhydride to control the molecular weight thereof, is melt extruded in the temperature range of 340 C. to 360 C. and at heights of 100.5 inches. 209 inches and 364.5 inches. The fibers obtained have a diameter in the range of 0.0068 inch to 0.0147 inch; a mean tensile strength in the range of 15.6 to 23.1 ksi; a mean modulus of 406 to 465 ksi, and a mean elongation in the range of 14 to 103%.

  19. Preparation, characterization, and applications of a novel solid-phase microextraction fiber by sol-gel technology on the surface of stainless steel wire for determination of poly cyclic aromatic hydrocarbons in aquatic environmental samples.

    PubMed

    Es-haghi, Ali; Hosseininasab, Valiallah; Bagheri, Habib

    2014-02-27

    A novel solid-phase microextraction(SPME) fiber was prepared using sol-gel technology with ethoxylated nonylphenol as a fiber coating material. The fiber was employed to develop a headspace SPME-GC-MS method suitable for quantification of 13 polycyclic aromatic hydrocarbons (PAHs) in water samples. Surface characteristics of the fibers were inspected by energy dispersive X-ray (EDX) spectroscopy as well as by scanning electron microscopy (SEM). The SEM measurements showed the presence of highly porous nano-sized particles in the coating. Important parameters affecting the extraction efficiency such as extraction temperature and time, desorption conditions as well as ionic strength have been evaluated and optimized. In the next step, the validation of the new method have been performed, finding it to be specific in the trace analysis of PAHs, with the limit of detection (LOD) ranging from 0.01 to 0.5 μg L(-1) and the linear range from the respective LOD to 200 μg L(-1) with RSD amounting to less than 8%. The thermal stability of the fibers was investigated as well and they were found to be durable at 280°C for 345 min. Furthermore, the proposed method was successfully applied for quantification of PAHs in real water samples.

  20. Fabrication of a polymeric ionic liquid-based adsorbent for multiple monolithic fiber solid-phase microextraction of endocrine disrupting chemicals in complicated samples.

    PubMed

    Pei, Miao; Zhang, Zirui; Huang, Xiaojia; Wu, Yuanfei

    2017-04-01

    A multiple monolithic fiber solid-phase microextraction (MMF-SPME) utilizing polymeric ionic liquid-based adsorbent was prepared. The adsorbent was obtained by in situ copolymerization of an ionic liquid, 1-trimethyl-(4-vinylbenzyl) aminium chloride and dual cross-linkers (divinylbenzene and ethylenedimethacrylate). The effect of preparation conditions including the content of ionic liquid and porogen in the polymerization mixture on extraction performance was studied in detail. Infrared spectroscopy, elemental analysis, scanning electron microscopy and mercury intrusion porosimetry were used to inspect the physicochemical properties of the new adsorbent. The applicability of the new MMF-SPME was demonstrated by the extraction of trace endocrine disrupting chemicals (EDCs). Results indicated that the prepared MMF-SPME could extract EDCs effectively through multi-interactions such as ion-exchange, π-π and hydrophobic interactions. After optimization of extraction parameters, a method of MMF-SPME coupled to high performance liquid chromatography/diode array detection was conducted to detect trace EDCs in complicated samples including environmental water and human urine. The limits of detection (S/N=3) and quantification (S/N=10) for targeted compounds were 0.011-0.065μg/L and 0.036-0.21μg/L, respectively. Satisfactory precision was also achieved by evaluating the repeatability and intermediate precision with relative standard deviations (RSDs) of less than 9% and 10%, respectively. At the same time, the proposed method was successfully applied for the determination of EDCs in water and human urine with spiking recoveries ranged from 70.6% to 119%.

  1. Novel molecularly-imprinted solid-phase microextraction fiber coupled with gas chromatography for analysis of furan.

    PubMed

    Hashemi-Moghaddam, Hamid; Ahmadifard, Mojtaba

    2016-04-01

    This study combined a molecularly-imprinted polymer with headspace solid-phase microextraction (HS-SPME). Preparation of molecularly-imprinted polymer is not effective for volatile compounds. To overcome this limitation, pyrrole was chosen as a template for the preparation of the furan-imprinted polymer. The holes in the synthesized polymer were suitable for furan adsorption because the chemical structure of pyrrole is similar to that of furan. The extraction properties of the fiber to furan were examined using an HS-SPME device coupled with gas chromatography-flame ionization detection (GC-FID) and gas chromatography-mass spectrometry (GC-MS). The effects of the extraction parameters of exposure time, sampling temperature, and salt concentration on extraction efficiency were studied. Satisfactory reproducibility was obtained for extractions from spiked water samples at RSD<7.5% (n=5). The calibration graphs were linear at 0.5-100 ng ml(-1) and the detection limit for furan was 0.042 ng ml(-1). The fabricated fiber was successfully applied for headspace extraction of furan from tap water and canned tuna as shown by GC-MS analysis.

  2. Assessment of solid phase microfiber extraction fibers for the monitoring of volatile organoarsinicals emitted from a plant-soil system.

    PubMed

    Ruppert, L; Lin, Z-Q; Dixon, R P; Johnson, K A

    2013-11-15

    Phytoremediation, the use of plants and microbes to clean up inorganic and organic pollutants, has shown great promise as an inexpensive and feasible form of remediation. More recently, studies have shown that some plants have an amazing capacity to volatilize contaminants and can be an effective remediation strategy if the chemicals released are non-toxic. Arsenic contamination and remediation has drawn great attention in the scientific community. However, its toxicity also varies depending on its form. We evaluated, optimized, and then utilized a solid phase microfiber extraction (SPME) head space sampling technique to characterize the organoarsinical emissions from rabbitfoot grass (Polypogon monspeliensis) in arsenic treated soils to determine if the potentially more toxic organic forms of arsenic (AsH3, AsH2CH3, AsH(CH3)2, and As(CH3)3) were being emitted from the plant-soil system. The SPME fiber that proved best fitted for this application was the DVB/CAR/PDMS fiber with a 45 min sampling period. We did detect and confirm the emissions of dimethylchloroarsine (AsCl(CH3)2) and pentamethylarsine (As(CH3)5). However, it was determined that the more toxic organic forms of arsenic were not released during phytovolatilization.

  3. Assay of aroma active components of virgin olive oils from southern Italian regions by SPME-GC/ion trap mass spectrometry.

    PubMed

    Benincasa, Cinzia; De Nino, Antonio; Lombardo, Nicola; Perri, Enzo; Sindona, Giovanni; Tagarelli, Antonio

    2003-01-29

    An SPME-GC/ion trap method was exploited to determine the chromatogram of volatile compounds of organic olive oils of southern Italian regions. The method is based on the assay of the terminal species of the "lipoxygenase pathway", which are present in the volatile fraction of the sampled compounds. Ethyl isobutanoate was used as internal standard in either the EI or CI ionization mode. The absolute concentration values of each analyte were evaluated through good-to-excellent calibration curves. Case studies on oils obtained from different cultivars or harvesting times are presented. The quantitative data for each compound were subjected to principal component analysis to characterize the different cultivars of this work.

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

    PubMed Central

    Silva, Catarina; Cavaco, Carina; Perestrelo, Rosa; Pereira, Jorge; Câmara, José S.

    2014-01-01

    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. PMID:24958388

  5. Discrimination of oolong tea (Camellia sinensis) varieties based on feature extraction and selection from aromatic profiles analysed by HS-SPME/GC-MS.

    PubMed

    Lin, Jie; Zhang, Pan; Pan, Zhiqiang; Xu, Hairong; Luo, Yaoping; Wang, Xiaochang

    2013-11-01

    This study aimed to develop an objective and accurate analytical method to discriminate oolong tea varieties that easily causing adulteration by potential volatile compounds. A total of 75 oolong tea samples of five similar varieties (Tieguanyin, Benshan, Maoxie, Huangjingui and Jinguanyin) were analysed by headspace solid phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC-MS). The relative content of 26 major volatile compounds varied significantly according to variety, combined with the results of hierarchical cluster analysis (HCA), indicating that the varietal differences of aromatic profile remain significant for tea cultivars with very close origin. Principal component analysis (PCA) of the aromatic profiles showed that the feature of variety dominated over the other features (like producing region and quality). By stepwise linear discriminant analysis (S-LDA), 18 volatiles with the best discriminating capacity were selected, and 4 discriminant functions (DFs) enabled simultaneously discrimination of the five oolong varieties with 100% correct rate.

  6. 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.

    PubMed

    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.

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

    NASA Astrophysics Data System (ADS)

    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.

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

    PubMed

    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.

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

    NASA Astrophysics Data System (ADS)

    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

  10. Carbon-fiber technology

    NASA Technical Reports Server (NTRS)

    Hansen, C. F.; Parker, J. A.

    1980-01-01

    The state of the art of PAN based carbon fiber manufacture and the science of fiber behavior is surveyed. A review is given of the stabilization by oxidation and the subsequent carbonization of fibers, of the apparent structure of fibers deduced from scanning electron microscopy, from X-ray scattering, and from similarities with soft carbons, and of the known relations between fiber properties and heat treatment temperature. A simplified model is invoked to explain the electrical properties of fibers and recent quantum chemical calculations on atomic clusters are used to elucidate some aspects of fiber conductivity. Some effects of intercalation and oxidative modification of finished fibers are summarized.

  11. Rapid determination of 54 pharmaceutical and personal care products in fish samples using microwave-assisted extraction-Hollow fiber-Liquid/solid phase microextraction.

    PubMed

    Zhang, Yi; Guo, Wen; Yue, Zhenfeng; Lin, Li; Zhao, Fengjuan; Chen, Peijin; Wu, Weidong; Zhu, Hong; Yang, Bo; Kuang, Yanyun; Wang, Jiong

    2017-04-15

    In this paper, a simple, rapid, solvent-less and environmental friendliness microextraction method, microwave-assisted extraction-hollow fiber-liquid/solid phase microextraction (MAE-HF-L/SME), was developed for simultaneous extraction and enrichment of 54 trace hydrophilic/lipophilic pharmaceutical and personal care products (PPCPs) from fish samples. A solid-phase extraction material, solid-phase microextraction (SPME) fiber, was synthesized. The SPME fiber had a homogeneous, loose structure and good mechanical properties, and they exhibited a good adsorption capacity for most PPCPs selected. The material formed the basis for the method of MAE-HF-L/SME. A method of liquid chromatography-high resolution mass spectroscopy (LC-HRMS) for analysis of 54 PPCPs. Under optimal synthesis and extraction conditions, the limits of detection (LODs, n=3) and the limits of quantitation (LOQs, n=10) for the 54 PPCPs were between 0.01-0.50μg·kg(-1) and 0.052.00μg·kg(-1), respectively. Percent recoveries and the relative standard deviations (RSDs) in spiked fish samples (n=6) were between 56.3%-119.9% and 0.3%-17.1%, respectively. The microextraction process of 54 PPCPs in MAE-HF-L/SME took approximately 12min. The method has a low matrix interference and high enrichment factor and may be applicable for determination of 54 different PPCPs in fish samples.

  12. Determination of phthalate esters in drinking water and edible vegetable oil samples by headspace solid phase microextraction using graphene/polyvinylchloride nanocomposite coated fiber coupled to gas chromatography-flame ionization detector.

    PubMed

    Amanzadeh, Hatam; Yamini, Yadollah; Moradi, Morteza; Asl, Yousef Abdossalmi

    2016-09-23

    In the current study, a graphene/polyvinylchloride nanocomposite was successfully coated on a stainless steel substrate by a simple dip coating process and used as a novel headspace solid phase microextraction (HS-SPME) fiber for the extraction of phthalate esters (PEs) from drinking water and edible vegetable oil samples. The prepared SPME fibers exhibited high extractability for PEs (due to the dominant role of π-π stacking interactions and hydrophobic effects) yielding good sensitivity and precision when followed by a gas chromatograph with a flame ionization detector (GC-FID). The optimization strategy of the extraction process was carried out using the response surface method based on a central composite design. The developed method gave a low limit of detection (0.06-0.08μgL(-1)) and good linearity (0.2-100μgL(-1)) for the determination of the PEs under the optimized conditions (extraction temperature, 70±1°C; extraction time, 35min; salt concentration, 30% w/v; stirring rate, 900rpm; desorption temperature, 230°C; and desorption time, 4min) whereas the repeatability and fiber-to-fiber reproducibility were in the range 6.1-7.8% and 8.9-10.2%, respectively. Finally, the proposed method was successfully applied to the analysis of PEs in drinking water and edible oil samples with good recoveries (87-112%) and satisfactory precisions (RSDs<8.3%), indicating the absence of matrix effects in the proposed HS-SPME method.

  13. Hollow fiber liquid-liquid-liquid microextraction followed by solid-phase microextraction and in situ derivatization for the determination of chlorophenols by gas chromatography-electron capture detection.

    PubMed

    Saraji, Mohammad; Ghani, Milad

    2015-10-30

    A method based on the combination of hollow fiber liquid-liquid-liquid microextraction and solid-phase microextraction (SPME) followed by gas chromatography-electron capture detection was developed for the determination of chlorophenols in water and wastewater samples. Silica microstructures fabricated on the surface of a stainless steel wire were coated by an organic solvent and used as a SPME fiber. The analytes were extracted through a hollow fiber membrane containing n-decane from sample solution to an alkaline aqueous acceptor phase. They were then extracted and in situ derivatized on the SPME fiber using acetic anhydride. Experimental parameters such as the type of extraction solvent, acceptor phase NaOH concentration, donor phase HCl concentration, the amount of derivatizing reagent, salt concentration, stirring rate and extraction time were investigated and optimized. The precision of the method for the analytes at 0.02-30μgL(-1) concentration level ranged from 7.1 to 10.2% (as intra-day relative standard deviation) and 6.4 to 9.8% (as inter-day relative standard deviation). The linear dynamic ranges were in the interval of 5-500μgL(-1), 0.05-5μgL(-1), 0.02-1μgL(-1) and 0.001-0.5μgL(-1) for 2-chlorophenol, 2,4-dichlorophenol, 2,4,6-trichlorophenol and pentachlorophenol, respectively. The enrichment factors were between 432 and 785. The limits of detection were in the range of 0.0004-1.2μgL(-1). Tap water, well water and wastewater samples were also analyzed to evaluate the method capability for real sample analysis.

  14. Evaluation of simulant migration of volatile nitrosamines from latex gloves and balloons by HS-SPME-GC-MS.

    PubMed

    Feng, Di; Liu, Luo; Zhao, Liyuan; Zhou, Qingfeng; Tan, Tianwei

    2012-09-01

    Nitrosamines are a group of carcinogens that have been found in various latex products. Methods have been developed for extraction, concentration and detection of simulant migration of volatile nitrosamines from latex gloves and balloons. After glove samples or balloon samples were treated with artificial sweat and artificial saliva, headspace solid-phase microextraction and gas chromatography with mass spectrometer detection were performed. Eight volatile nitrosamines were extracted by a fused silica fiber coated with carboxen-polydimethylsioxane, and solid-phase microextraction conditions were optimized. The developed method was successfully used to analyze simulant migration of volatile nitrosamines from latex gloves and balloons. The described methods are rapid and simple, with adequate sensitivity and without organic solvent.

  15. Single-walled carbon nanotubes coated fibers for solid-phase microextraction and gas chromatography-mass spectrometric determination of pesticides in Tea samples.

    PubMed

    Wu, Fang; Lu, Wanping; Chen, Jinghua; Liu, Wei; Zhang, Lan

    2010-08-15

    Using a single-walled carbon nanotubes (SWCNTs) as stationary phase of solid-phase microextraction (SPME) fibers, a simple, low cost and environmentally friendly method for extraction of 13 pesticides in Tea samples has been developed following gas chromatography-mass spectrometric determination. Potential factors affecting the extraction efficiency were investigated and optimized, including extraction and desorption time, extraction temperature, stirring rate, solution pH and ionic strength. Under optimized conditions, the linearity of the developed method was in the range of 0.125-25 ng/mL with correlation coefficients greater than 0.9928 and the limits of detections (LODs) were 0.027-0.23 ng/mL (S/N=3). Meanwhile, the relative standard deviations (RSDs) for five successive measurements with single fiber, fiber-to-fiber, day-to-day were 2.3-13.0, 8.2-14.6 and 4.1-12.5%, respectively, indicating good reproducibility of the proposed method. The fiber had high extraction efficiency for studied pesticides in comparison with commercial poly(dimethylsiloxane) (PDMS) and polyacrylate (PA) fibers and could be used for more than 70 times without decrease of efficiency. The developed method was successfully applied for the analysis of real samples including green Tea, oolong Tea, white Tea, and flower Tea, and the recoveries of the pesticides spiked in these samples ranged from 75.1 to 118.4%. Chlorfenapyr and lambda-cyhalothrin were found in the Tea samples bought randomly from local market. The results demonstrated that the developed SWCNTs-SPME method was a simple, efficient pretreatment and enrichment procedure for pesticides in complex matrices.

  16. Covalent Bonding of Metal-Organic Framework-5/Graphene Oxide Hybrid Composite to Stainless Steel Fiber for Solid-Phase Microextraction of Triazole Fungicides from Fruit and Vegetable Samples.

    PubMed

    Zhang, Shuaihua; Yang, Qian; Wang, Wenchang; Wang, Chun; Wang, Zhi

    2016-04-06

    A hybrid material of the zinc-based metal-organic framework-5 and graphene oxide (metal-organic framework-5/graphene oxide) was prepared as a novel fiber coating material for solid-phase microextraction (SPME). The SPME fibers were fabricated by covalent bonding via chemical cross-linking between the coating material metal-organic framework-5/graphene oxide and stainless steel wire. The prepared fiber was used for the extraction of five triazole fungicides from fruit and vegetable samples. Gas chromatography coupled with microelectron capture detector (GC-μECD) was used for quantification. The developed method gave a low limit of detection (0.05-1.58 ng g(-1)) and good linearity (0.17-100 ng g(-1)) for the determination of the triazole fungicides in fruit and vegetable samples. The relative standard deviations (RSDs) for five replicate extractions of the triazole fungicides ranged from 3.7 to 8.9%. The method recoveries for spiked fungicides (5, 20, and 50 ng g(-1)) in grape, apple, cucumber, celery cabbage, pear, cabbage, and tomato samples were in the range of 85.6-105.8% with the RSDs ranging from 3.6 to 11.4%, respectively, depending on both the analytes and samples. The metal-organic framework-5/graphene oxide coated fiber was stable enough for 120 extraction cycles without a significant loss of extraction efficiency. The method was suitable for the determination of triazole fungicides in fruit and vegetable samples.

  17. Composite Fiber Hazards

    DTIC Science & Technology

    1990-12-01

    34L boton Ion a tungsten boride core, and appear more like fine wires ,tin fibers. The fibers are combined with an epoxy matrix to form a prepreg j i...a 8-hour TWA Recommended Exposure Limit (REL) for fibrous glass of 3 fibers/cm3 for fibers with length >10 Jim and diameter ɛ.5 pm, and total

  18. Fiber optic connector

    DOEpatents

    Rajic, Slobodan; Muhs, Jeffrey D.

    1996-01-01

    A fiber optic connector and method for connecting composite materials within which optical fibers are imbedded. The fiber optic connector includes a capillary tube for receiving optical fibers at opposing ends. The method involves inserting a first optical fiber into the capillary tube and imbedding the unit in the end of a softened composite material. The capillary tube is injected with a coupling medium which subsequently solidifies. The composite material is machined to a desired configuration. An external optical fiber is then inserted into the capillary tube after fluidizing the coupling medium, whereby the optical fibers are coupled.

  19. Fiber optic temperature sensor

    NASA Technical Reports Server (NTRS)

    Sawatari, Takeo (Inventor); Gaubis, Philip A. (Inventor)

    2000-01-01

    A fiber optic temperature sensor uses a light source which transmits light through an optical fiber to a sensor head at the opposite end of the optical fiber from the light source. The sensor head has a housing coupled to the end of the optical fiber. A metallic reflective surface is coupled to the housing adjacent the end of the optical fiber to form a gap having a predetermined length between the reflective surface and the optical fiber. A detection system is also coupled to the optical fiber which determines the temperature at the sensor head from an interference pattern of light which is reflected from the reflective surface.

  20. Fiber optic temperature sensor

    NASA Technical Reports Server (NTRS)

    Sawatari, Takeo (Inventor); Gaubis, Philip A. (Inventor); Mattes, Brenton L. (Inventor); Charnetski, Clark J. (Inventor)

    1999-01-01

    A fiber optic temperature sensor uses a light source which transmits light through an optical fiber to a sensor head at the opposite end of the optical fiber from the light source. The sensor head has a housing coupled to the end of the optical fiber. A metallic reflective surface is coupled to the housing adjacent the end of the optical fiber to form a gap having a predetermined length between the reflective surface and the optical fiber. A detection system is also coupled to the optical fiber which determines the temperature at the sensor head from an interference pattern of light which is reflected from the reflective surface.

  1. Fiber optic connector

    DOEpatents

    Rajic, S.; Muhs, J.D.

    1996-10-22

    A fiber optic connector and method for connecting composite materials within which optical fibers are imbedded are disclosed. The fiber optic connector includes a capillary tube for receiving optical fibers at opposing ends. The method involves inserting a first optical fiber into the capillary tube and imbedding the unit in the end of a softened composite material. The capillary tube is injected with a coupling medium which subsequently solidifies. The composite material is machined to a desired configuration. An external optical fiber is then inserted into the capillary tube after fluidizing the coupling medium, whereby the optical fibers are coupled. 3 figs.

  2. Coatings for graphite fibers

    NASA Technical Reports Server (NTRS)

    Galasso, F. S.; Scola, D. A.; Veltri, R. D.

    1980-01-01

    Graphite fibers released from composites during burning or an explosion caused shorting of electrical and electronic equipment. Silicon carbide, silica, silicon nitride and boron nitride were coated on graphite fibers to increase their electrical resistances. Resistances as high as three orders of magnitude higher than uncoated fiber were attained without any significant degradation of the substrate fiber. An organo-silicone approach to produce coated fibers with high electrical resistance was also used. Celion 6000 graphite fibers were coated with an organo-silicone compound, followed by hydrolysis and pyrolysis of the coating to a silica-like material. The shear and flexural strengths of composites made from high electrically resistant fibers were considerably lower than the shear and flexural strengths of composites made from the lower electrically resistant fibers. The lower shear strengths of the composites indicated that the coatings on these fibers were weaker than the coating on the fibers which were pyrolyzed at higher temperature.

  3. Alumina fiber strength improvement

    NASA Technical Reports Server (NTRS)

    Pepper, R. T.; Nelson, D. C.

    1982-01-01

    The effective fiber strength of alumina fibers in an aluminum composite was increased to 173,000 psi. A high temperature heat treatment, combined with a glassy carbon surface coating, was used to prevent degradation and improve fiber tensile strength. Attempts to achieve chemical strengthening of the alumina fiber by chromium oxide and boron oxide coatings proved unsuccessful. A major problem encountered on the program was the low and inconsistent strength of the Dupont Fiber FP used for the investigation.

  4. Fiber optic monitoring device

    DOEpatents

    Samborsky, James K.

    1993-01-01

    A device for the purpose of monitoring light transmissions in optical fibers comprises a fiber optic tap that optically diverts a fraction of a transmitted optical signal without disrupting the integrity of the signal. The diverted signal is carried, preferably by the fiber optic tap, to a lens or lens system that disperses the light over a solid angle that facilitates viewing. The dispersed light indicates whether or not the monitored optical fiber or system of optical fibers is currently transmitting optical information.

  5. Photonic Crystal Fibers

    DTIC Science & Technology

    2005-12-01

    passive and active versions of each fiber designed under this task. Crystal Fibre shall provide characteristics of the fiber fabricated to include core...passive version of multicore fiber iteration 2. 15. SUBJECT TERMS EOARD, Laser physics, Fibre Lasers, Photonic Crystal, Multicore, Fiber Laser 16...9 00* 0 " CRYSTAL FIBRE INT ODUCTION This report describes the photonic crystal fibers developed under agreement No FA8655-o5-a- 3046. All

  6. Antimicrobial Acrylic Fiber

    DTIC Science & Technology

    2006-08-01

    hydantoin). The fibers were extruded from a single solvent, dimenthyl acetamide. The fibers could be chlorinated to produce halamines and thus... chlorine adsorption was shown to be proportional to the specific surface area of the fibers, as might be expected for hydrophobic materials which can react...hydantoin). The fibers were extruded from a single solvent, dimethyl acetamide. The fibers could be chlorinated to produce halamines and thus rendered

  7. Volatile profile of cashew apple juice fibers from different production steps.

    PubMed

    Nobre, Ana Carolina de Oliveira; de Almeida, Áfia Suely Santos da Silva; Lemos, Ana Paula Dajtenko; Magalhães, Hilton César Rodrigues; Garruti, Deborah dos Santos

    2015-05-27

    This study aimed to determine the volatile profile of cashew apple fibers to verify which compounds are still present after successive washings and thus might be responsible for the undesirable remaining cashew-like aroma present in this co-product, which is used to formulate food products like vegetarian burgers and cereal bars. Fibers were obtained from cashew apple juice processing and washed five times in an expeller press. Compounds were analyzed by the headspace solid-phase micro extraction technique (HS-SPME) and gas chromatography-mass spectrometry (GC-MS), using a DB-5 column. Sensory analysis was also performed to compare the intensity of the cashew-like aroma of the fibers with the original juice. Altogether, 80 compounds were detected, being esters and terpenes the major chemical classes. Among the identified substances, 14 were classified as odoriferous in the literature, constituting the matrix used in the Principal Component Analysis (PCA). Odoriferous esters were substantially reduced, but many compounds were extracted by the strength used in the expeller press and remained until the last wash. Among them are the odoriferous compounds ethyl octanoate, γ-dodecalactone, (E)-2-decenal, copaene, and caryophyllene that may contribute for the mild but still perceptible cashew apple aroma in the fibers that have been pressed and washed five times. Development of a deodorization process should include reduction of pressing force and stop at the second wash, to save water and energy, thus reducing operational costs and contributing to process sustainability.

  8. Study of the volatile compounds and odor-active compounds of dry-cured Iberian ham extracted by SPME.

    PubMed

    del Pulgar, José Sánchez; García, Carmen; Reina, Raquel; Carrapiso, Ana I

    2013-06-01

    The volatile compounds and the most odor-active compounds of dry-cured Iberian ham were investigated by extracting them using a solid phase microextraction technique with a 2 cm Carboxen/PDMS/DVB fiber. The detection frequency method was applied to estimate the potential contribution of each compound to the odor of hams. Twenty-one volatile compounds were tentatively identified for the first time in dry-cured ham by gas chromatography-mass spectrometry, and eight in dry-cured Iberian ham. Gas chromatography-olfactometry allowed the identification for the first time of six compounds not previously reported as odorants of Iberian ham, and also two odorants were newly identified in dry-cured ham. According to the detection frequency method, the most odor active compounds found were 3-methylbutanoic acid (dirty sock-like smelling), hexanal (cut grass-like odor), 3-methylbutanal (sweaty and bitter almond-like odor), 2-methyl-3-furanthiol (toasted nuts-like odor) and 1-octen-3-one (mushroom-like odor).

  9. 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

    NASA Astrophysics Data System (ADS)

    Nomngongo, Philiswa N.; Ngila, J. Catherine

    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- 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.

  10. Bis(trifluoromethanesulfonyl)imide-based ionic liquids grafted on graphene oxide-coated solid-phase microextraction fiber for extraction and enrichment of polycyclic aromatic hydrocarbons in potatoes and phthalate esters in food-wrap.

    PubMed

    Hou, Xiudan; Guo, Yong; Liang, Xiaojing; Wang, Xusheng; Wang, Lei; Wang, Licheng; Liu, Xia

    2016-06-01

    A class of novel, environmental friendly ionic liquids (ILs) were synthesized by on-fiber preparation strategy and modified on graphene oxide (GO)-coated stainless steel wire, which was used as a solid-phase microextraction (SPME) fiber for efficient enrichment of polycyclic aromatic hydrocarbons (PAHs) and phthalate esters (PAEs). Surface characteristic of the ILs and polymeric-ILs (PILs) fibers with the wave-structure were inspected by scanning electron microscope. The successfully synthesis of bis(trifluoromethanesulfonyl)imide (NTf2(-))-based ILs were also characterized by energy dispersive spectrometer analysis. Through the chromatograms of the proposed two ILs (1-aminoethyl-3-methylimidazolium bromide (C2NH2MIm(+)Br(-)), C2NH2MIm(+)NTf2(-)) and two PILs (polymeric 1-vinyl-3-hexylimidazolium bromide (poly(VHIm(+)Br(-))), poly(VHIm(+)NTf2(-)))-GO-coated fibers for the extraction of analytes, NTf2(-)-based PIL demonstrated higher extraction capacity for hydrophobic compounds than other as-prepared ILs. Analytical performances of the proposed fibers were investigated under the optimized extraction and desorption conditions coupled with gas chromatography (GC). Compared with the poly(VHIm(+)Br(-))-GO fiber, the poly(VHIm(+)NTf2(-))-GO SPME fiber brought wider linear ranges for analytes with correlation coefficient in the range of 0.9852-0.9989 and lower limits of detection ranging from 0.015-0.025μgL(-1). The obtained results indicated that the newly prepared PILs-GO coating was a feasible, selective and green microextraction medium, which could be suitable for extraction and determination of PAHs and PAEs in potatoes and food-wrap sample, respectively.

  11. Monitoring the emission of volatile organic compounds from flowers of Jasminum sambac using solid-phase micro-extraction fibers and gas chromatography with mass spectrometry detection.

    PubMed

    Pragadheesh, Vppalayam Shanmugam; Yadav, Anju; Chanotiya, Chandan Singh; Rout, Prasanta Kumar; Uniyal, Girish Chandra

    2011-09-01

    Solid-phase micro-extraction (SPME) was studied as a solvent free alternative method for the extraction and characterization of volatile compounds in intact and plucked flowers of Jasminum sambac at different day time intervals using gas chromatography (GC-FID) and gas chromatography-quadrupole mass spectrometry. The analytes identified included alcohols, esters, phenolic compounds, and terpenoids. The main constituents identified in the flower aroma using different fibers were cis-3-hexenyl acetate, (E)-beta-ocimene, linalool, benzyl acetate, and (E,E)-alpha-farnesene. The benzyl acetate proportion decreased from morning to afternoon and then increased in evening collections. PDMS fiber showed a high proportion of (E,E)-alpha-farnesene in jasmine floral aroma. Among other constituents identified, cis-3-hexenyl acetate, linalool, and benzyl acetate were major aroma contributors in plucked and living flowers extracts using PDMS/DVB, Carboxen/PDMS, and DVB/Carboxen/PDMS fibers. PDMS/DVB recorded the highest emission for benzyl acetate while the (E)-beta-ocimene proportion was highest in DVB/Carboxen/PDMS when compared with the rest. The highest linalool content, with increasing proportion from morning to noon, was found using mixed coating fibers. Almost negligible volatile adsorption was recorded for the polyacrylate fiber for intact flower aroma, whereas it was most effective for benzyl acetate, followed by indole under plucked conditions. Moreover, the highest amounts extracted, evaluated from the sum of peak areas, were achieved using Carboxen/PDMS, and DVB/Carboxen/PDMS. Introduction of a rapid, and solvent free SPME method for the analysis of multicomponent volatiles can be successfully employed to monitor the extraction and characterization of flower aroma constituents.

  12. Solid phase microextraction procedure for the determination of alkylphenols in water by on-fiber derivatization with N-tert-butyl-dimethylsilyl-N-methyltrifluoroacetamide.

    PubMed

    Pan, Yi-Ping; Tsai, Shih-Wei

    2008-08-29

    The solid phase microextraction (SPME) technique with on-fiber derivatization was evaluated for the analysis of alkylphenols (APs), including 4-tert-octylphenol (4-t-OP), technical nonylphenol isomers (t-NPs) and 4-nonylphenol (4-NP), in water. The 85 microm polyacrylate (PA) fiber was used and a two-step sample preparation procedure was established. In the first step, water sample of 2 mL was placed in a 4 mL PTFE-capped glass vial. Headspace extraction of APs in water was then performed under 65 degrees C for 30 min with 800 rpm magnetic stirring and the addition of 5% of sodium chloride. In the second step, the SPME fiber was placed in another 4 mL vial, which contained 100 microL of N-tert-butyl-dimethylsilyl-N-methyltrifluoroacetamide (MTBSTFA) with 1% tert-butyl-dimethylchlorosilane (TBDMCS). Headspace extraction of MTBSTFA and on-fiber derivatization with APs were performed at 45 degrees C for 10 min. Gas chromatography/mass spectrometry (GC/MS) was used for the analysis of derivatives formed on-fiber. The adsorption-time profiles were also examined. The precision, accuracy and method detection limits (MDLs) for the analysis of all the APs were evaluated with spiked water samples, including detergent water, chlorinated tap water, and lake water. The relative standard deviations were all less than 10% and the accuracies were 100+/-15%. With 2 mL of water sample, MDLs were in the range of 1.58-3.85 ng L(-1). Compared with other techniques, the study described here provided a simple, fast and reliable method for the analysis of APs in water.

  13. Electrospun modified silica-polyamide nanocomposite as a novel fiber coating.

    PubMed

    Bagheri, Habib; Roostaie, Ali

    2014-01-10

    In the present work, a new solid phase microextraction (SPME) fiber coating based on modified silica-polyamide (PA) nanocomposite was electrospun on a stainless steel wire. Four modified silica-PA nanocomposites together with PA were fabricated by dispersing several typical modified silica nanoparticles in PA polymer solution prior to electrospinning. The surface characteristic of PA nanofibers and modified silica-PA nanocomposites was investigated using scanning electron microscopy (SEM). The homogeneity and the porous surface structure of the modified silica-PA nanocomposites were confirmed by SEM, showing nanofibers diameters lower than 170 nm. The applicability of the new fiber coating was examined by headspace SPME of some selected chlorobenzenes (CBs), as model compounds, from aqueous samples. Subsequently, the extracted analytes were transferred into a gas chromatography (GC) by thermal desorption. Influencing parameters on the morphology of nanocomposites such as type of modified silica nanoparticles and the weight ratio of components were optimized. In addition, effects of different parameters influencing the extraction efficiency including extraction temperature, extraction time, ionic strength, desorption temperature, and desorption time were investigated and optimized. Eventually, the developed method was validated by gas chromatography-mass spectrometry (GC-MS). At the optimum conditions, the relative standard deviation values for a double distilled water spiked with the selected CBs at 100 ng L(-1) were 4-12% (n=3) and the limit of detection for the studied compounds was between 5 and 30 ng L(-1). The calibration curves of analytes were investigated in the range of 50-1000 ng L(-1) and correlation coefficients (R(2)) between 0.9897 and 0.9992 were obtained.

  14. 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.

    PubMed

    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.

  15. Hollow fiber-stir bar sorptive extraction and microwave assisted derivatization of amino acids in biological matrices.

    PubMed

    Li, Jia; Qi, Huan-Yang; Wang, Yan-Bin; Su, Qiong; Wu, Shang; Wu, Lan

    2016-11-25

    A kind of solid phase microextraction configuration combining the principles of hollow fiber solid phase microextraction (HF-SPME) and stir bar sorptive extraction (SBSE) is presented. The main feature of HF-SBSE is the use of microporous hollow fiber acting as the carrier and filter, while a thin stainless steel wire and silica microspheres in the lumen of hollow fiber respectively acting as the magnetic stirrer and the dispersed sorbents for the collection and extraction of the target analytes, thus affording extraction process like SBSE. Moreover, the prepared hollow fiber stir bar was applied to direct microextraction and microwave assisted derivatization with N,O-Bis(trimethylsilyl)trifluroacetamide (BSTFA) of four amino acids in rats' urine and cerebrospinal fluid followed by gas chromatography mass spectrometric analysis. The limits of detection for four amino acids were found to be in the range of 0.0003-0.017μgmL(-1), and all the analytes did not exhibit any lack of fit. The extraction recoveries using HF-SBSE techniques ranged from 71.8% to 102.3%. The results indicated that hollow fiber stir bar sorptive extraction was a promising technique for the enrichment and direct derivatization of analytes extracted from biological matrices without sample clean-up.

  16. Analysis of perfluorooctane sulfonate and perfluorooctanoic acid with a mixed-mode coating-based solid-phase microextraction fiber.

    PubMed

    Chen, Chunyan; Wang, Jianping; Yang, Shaolei; Yan, Zhihong; Cai, Qingyun; Yao, Shouzhuo

    2013-09-30

    A novel mixed-mode coating-based solid-phase microextraction (SPME) fiber was prepared by chemical bonding dimethyloctadecyl [3-(trimethoxysilyl) propyl] ammonium chloride and 3-(trimethoxysilyl)-1-propanamine, the sol-gel precursors, on an anodized Ti wire, aiming to effectively adsorb perfluorooctane sulfonate (PFOS) and perfluorooctanoic acid (PFOA). The anodized Ti wire with uniform TiO2 nanotube arrays provides high mechanical strength and strong adhesion to the mixed-mode coating. The prepared fiber shows excellent organic solvent stability due to the covalent bonding between the coating and the fiber, and significantly higher extraction efficiency than the commercial fibers, 100 μm polydimethylsiloxane and 85 μm polyacrylate fiber, due to the synergistic extraction effects of the coating functional groups. Good linearity (R(2)=0.9994 for PFOS, R(2)=0.9992 for PFOA) was obtained with detection limits of 2.5 and 7.5 pg mL(-1) for PFOS and PFOA, respectively. Recoveries were in the range of 88%-102%. The proposed method was successfully applied in the analysis of PFOS and PFOA in a local river with the results of 0.05 and 0.06 ng mL(-1), respectively.

  17. Ceramic fiber reinforced filter

    DOEpatents

    Stinton, David P.; McLaughlin, Jerry C.; Lowden, Richard A.

    1991-01-01

    A filter for removing particulate matter from high temperature flowing fluids, and in particular gases, that is reinforced with ceramic fibers. The filter has a ceramic base fiber material in the form of a fabric, felt, paper of the like, with the refractory fibers thereof coated with a thin layer of a protective and bonding refractory applied by chemical vapor deposition techniques. This coating causes each fiber to be physically joined to adjoining fibers so as to prevent movement of the fibers during use and to increase the strength and toughness of the composite filter. Further, the coating can be selected to minimize any reactions between the constituents of the fluids and the fibers. A description is given of the formation of a composite filter using a felt preform of commercial silicon carbide fibers together with the coating of these fibers with pure silicon carbide. Filter efficiency approaching 100% has been demonstrated with these filters. The fiber base material is alternately made from aluminosilicate fibers, zirconia fibers and alumina fibers. Coating with Al.sub.2 O.sub.3 is also described. Advanced configurations for the composite filter are suggested.

  18. Volatile profiles of Italian monovarietal extra virgin olive oils via HS-SPME-GC-MS: newly identified compounds, flavors molecular markers, and terpenic profile.

    PubMed

    Cecchi, Teresa; Alfei, Barbara

    2013-12-01

    This study aims to contribute to the knowledge of the commercial, sensory, and analytical characteristics of extra virgin olive oil (EVOO) from Italy (Marche region), renowned since ancient times. Headspace solid-phase micro-extraction (HS-SPME) was applied for the very first time to the sampling of volatile compounds of eleven typical Italian monocultivar EVOOs. Forty-eight compounds were characterised by GC-MS, some of them were only occasionally found in other EVOOs and some other were never detected before in any EVOO. Compounds belonging mainly to alcohols, esters, aldehydes, ketones and hydrocarbons chemical classes characterised the volatile profiles. The main volatile compounds detected in the EVOOs were the C6 compounds derived from polyunsaturated fatty acids, through the lipoxygenase pathway, in different proportion according to the specific cultivar. The results suggest that genetic factors strongly influence volatile formation and terpene hydrocarbons are claimed to be suitable markers of the geographic origin and genotype of the EVOO. Correlations among sensory attributes evaluated by a panel test and the presence of specific volatile compounds were highlighted for the very first time. The significance of the presence of some newly identified volatile compounds was discussed.

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

    PubMed

    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.

  20. 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.

    PubMed

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

    2014-04-11

    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).

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

    PubMed

    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.

  2. Quantification of furanic compounds in coated deep-fried products simulating normal preparation and consumption: optimisation of HS-SPME analytical conditions by response surface methodology.

    PubMed

    Pérez-Palacios, T; Petisca, C; Melo, A; Ferreira, I M P L V O

    2012-12-01

    The validation of a method for the simultaneous quantification of furanic compounds in coated deep-fried samples processed and handled as usually consumed is presented. The deep-fried food was grinded using a device that simulates the mastication, and immediately analysed by headspace solid phase microextraction coupled to gas chromatography-mass spectrometry. Parameters affecting the efficiency of HS-SPME procedure were selected by response surface methodology, using a 2(3) full-factorial central composite design. Optimal conditions were achieved using 2g of sample, 3g of NaCl and 40min of absorption time at 37°C. Consistency between predicted and experimented values was observed and quality parameters of the method were established. As a result, furan, 2-furfural, furfuryl alcohol and 2-pentylfuran were, for the first time, simultaneously detected and quantified (5.59, 0.27, 10.48 and 1.77μgg(-1) sample, respectively) in coated deep-fried fish, contributing to a better understanding of the amounts of these compounds in food.

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

    PubMed

    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.

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

    PubMed

    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.

  5. Polyparameter linear free energy models for polyacrylate fiber-water partition coefficients to evaluate the efficiency of solid-phase microextraction.

    PubMed

    Endo, Satoshi; Droge, Steven T J; Goss, Kai-Uwe

    2011-02-15

    The fiber-water partition coefficient, K(fw), is decisive for performance of solid-phase microextraction (SPME) techniques in organic chemical analyses. In this study, polyacrylate (PA)-coated fiber was evaluated for its K(fw) values toward diverse neutral organic compounds. Literature K(fw) data were thoroughly evaluated, and additional K(fw) values for 69 compounds were measured in phosphate-buffered saline (PBS) solution at 37 °C. These K(fw) data, spanning over 6 orders of magnitude, were used to construct polyparameter linear free energy relationship (PP-LFER) models. The PP-LFER models fit well to the data with a standard deviation of 0.15-0.23 log units. Additional experiments indicated that the differences in temperature (25 vs 37 °C), electrolyte concentrations (pure water vs PBS), and conditioning methods (heat vs methanol) had only minor influences (<0.3 log units) on K(fw). Using the established PP-LFERs, the SPME extraction efficiency of PA coating toward compounds of differing polarity was evaluated in comparison to poly(dimethylsiloxane) (PDMS) coating. PA exhibited higher extraction capacities for H-bond donor compounds (e.g., phenols, anilines, amides, and many drugs and pesticides) with the estimated K(fw) values being 1-4 log units higher than those of PDMS. Also, PA was shown to be more efficient than PDMS for hydrophobic aromatic compounds.

  6. New nanostructure of polydimethylsiloxane coating as a solid-phase microextraction fiber: Application to analysis of BTEX in aquatic environmental samples.

    PubMed

    Zali, Sara; Jalali, Fahimeh; Es-Haghi, Ali; Shamsipur, Mojtaba

    2016-10-15

    Electrospinning technique was used to convert polydimethyl siloxane (PDMS) sol-gel solution to a new nanostructure on a stainless steel wire. The surface morphology of the fiber was observed by scanning electron microscopy (SEM). It showed a diameter range of 30-60nm for PDMS nanoparticles with a homogeneous and porous surface structure. The applicability of this coating was assessed for the headspace SPME (HS-SPME) of benzene, toluene, ethylbenzene and xylenes (BTEX) from water samples followed by gas chromatography-mass spectrometry. The important parameters affecting extraction efficiency such as extraction time and temperature, desorption conditions, agitation rate and ionic strength were investigated and optimized. Under the optimized conditions, LODs and LOQs of 0.3-5μgL(-1) and 1-10μgL(-1) were obtained, respectively. The method showed linearity in the broad range of 1-5000μgL(-1) with correlation coefficient of >0.99. Inter-day and intra-day precisions of the developed method ranged from 2.43% to 6.54% and from 5.24% to 13.73%, respectively. The thermal stability of the fiber was investigated on stainless steel wire. It was found to be durable at 260°C for more than 360min. Furthermore, the proposed method was successfully applied for quantification of BTEX in real water samples.

  7. Sources of fiber (image)

    MedlinePlus

    ... to avoid constipation. Vegetables, fresh fruits (especially dried fruits) and whole wheat, bran, or oatmeal cereals are excellent sources of fiber. To reap the benefits of fiber, it is very important to drink ...

  8. Fiber Optics Instrumentation Development

    NASA Technical Reports Server (NTRS)

    Chan, Patrick Hon Man; Parker, Allen R., Jr.; Richards, W. Lance

    2010-01-01

    This is a general presentation of fiber optics instrumentation development work being conducted at NASA Dryden for the past 10 years and recent achievements in the field of fiber optics strain sensors.

  9. Fiber Optics Technology.

    ERIC Educational Resources Information Center

    Burns, William E.

    1986-01-01

    Discusses various applications of fiber optics technology: information systems, industrial robots, medicine, television, transportation, and training. Types of jobs that will be available with fiber optics training (such as electricians and telephone cable installers and splicers) are examined. (CT)

  10. Soluble vs. insoluble fiber

    MedlinePlus

    ... soluble and insoluble. Both are important for health, digestion, and preventing diseases. Soluble fiber attracts water and turns to gel during digestion. This slows digestion. Soluble fiber is found in ...

  11. Omnidirectional fiber optic tiltmeter

    DOEpatents

    Benjamin, B.C.; Miller, H.M.

    1983-06-30

    A tiltmeter is provided which is useful in detecting very small movements such as earth tides. The device comprises a single optical fiber, and an associated weight affixed thereto, suspended from a support to form a pendulum. A light source, e.g., a light emitting diode, mounted on the support transmits light through the optical fiber to a group of further optical fibers located adjacent to but spaced from the free end of the single optical fiber so that displacement of the single optical fiber with respect to the group will result in a change in the amount of light received by the individual optical fibers of the group. Photodetectors individually connectd to the fibers produce corresponding electrical outputs which are differentially compared and processed to produce a resultant continuous analog output representative of the amount and direction of displacement of the single optical fiber.

  12. Fiber length distributions and fiber quality

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Cotton (Gossypium hirsutum L.) is grown in Georgia on ~1 million acres by producers as a raw material input for textile mills. Georgia cotton fiber qualities continue to improve through crop management, genetic, and ginning improvements. Competition from synthetic fibers, mill modernization, and g...

  13. Graphite Fibers from Pitch

    DTIC Science & Technology

    1975-07-01

    carbon fibers derived from pitch (Type-P fibers). But even if such perfect mesophase pitch fibers could be obtained, the subsequent carbonization... mesophase pitch filaments with diameters below lOfim was demonstrated in the preceding contract period. Further effort was aimed at reproducibly...Isotropie pitch fibers. ’ It seemed prudent for us to establish whether some of these agents could be used to advantage with the mesophase pitch

  14. Helical Fiber Amplifier

    DOEpatents

    Koplow, Jeffrey P.; Kliner, Dahy; Goldberg, Lew

    2002-12-17

    A multi-mode gain fiber is provided which affords substantial improvements in the maximum pulse energy, peak power handling capabilities, average output power, and/or pumping efficiency of fiber amplifier and laser sources while maintaining good beam quality (comparable to that of a conventional single-mode fiber source). These benefits are realized by coiling the multimode gain fiber to induce significant bend loss for all but the lowest-order mode(s).

  15. Graphite Fibers from Pitch

    DTIC Science & Technology

    1976-09-01

    yarn filaments may cause early fiber failure, particularly when the crack follows a tight spiral along the fiber axis, as it was observed in isolated...ray Results 4. Mechanical Properties 5. Conclusions V. STRUCTURE OF FILAMENTS IN TYPE P YARN 1. Fiber Structure Terminology 2. Correlation of...Fiber Structure with Single Filament Properties 3. Optical Microscopy of Filaments with Variable Structure 4. SEM Studies of Yarn Samples with

  16. Diode Pumped Fiber Laser

    DTIC Science & Technology

    1983-07-01

    acousto - optic beam deflector for greater absolute accuracy. The detection system was also upgraded to a response time of • 1 usec. The... 2 C. SUMMARY OF RESULTS.., 3 D . GENERAL PLAN 5 II. Nd:YAG FIBER PREPARATION 7 A. FIBER GROWTH 7 B. PHYSICAL PROPERTIES OF Nd:YAG...A. INTRODUCTION 25 B. GENERAL FORMALISM 26 C. FREE-SPACE LASERS 35 D . FIBER LASERS 43 1. Fiber Laser Configuration 43 2 . F

  17. Fiber optic coupled optical sensor

    DOEpatents

    Fleming, Kevin J.

    2001-01-01

    A displacement sensor includes a first optical fiber for radiating light to a target, and a second optical fiber for receiving light from the target. The end of the first fiber is adjacent and not axially aligned with the second fiber end. A lens focuses light from the first fiber onto the target and light from the target onto the second fiber.

  18. Mineral Fiber Toxicology

    EPA Science Inventory

    The chemical and physical properties of different forms of mineral fibers impact biopersistence and pathology in the lung. Fiber chemistry, length, aspect ratio, surface area and dose are critical factors determining mineral fiber-associated health effects including cancer and as...

  19. The Fiber Optic Connection.

    ERIC Educational Resources Information Center

    Reese, Susan

    2003-01-01

    Describes the fiber optics programs at the Career and Technical Center in Berlin, Pennsylvania and the Charles S. Monroe Technology Center in Loudoun County, Virginia. Discusses the involvement of the Fiber Optic Association with education, research and development, manufacturing, sales, distribution, installation, and maintenance of fiber optic…

  20. Advanced Engineering Fibers.

    ERIC Educational Resources Information Center

    Edie, Dan D.; Dunham, Michael G.

    1987-01-01

    Describes Clemson University's Advanced Engineered Fibers Laboratory, which was established to provide national leadership and expertise in developing the processing equipment and advance fibers necessary for the chemical, fiber, and textile industries to enter the composite materials market. Discusses some of the laboratory's activities in…

  1. SYNTHETIC FIBERS, 1965,

    DTIC Science & Technology

    The following groups of fibers are each briefly discussed: Glass and other inorganic fibers, viscose rayon, cuprammonium rayon, saponified acetate rayon, alginate rayon, regenerated protein fibers, cellulose nitrate, cellulose acetate rayon, cellulose triacetate, polyamides, acrylics, modacrylics, polyvinyls, polyvinylidenes, polyesters, polyolefins, polyurethanes, fluorocarbons.

  2. Oxynitride glass fibers

    NASA Technical Reports Server (NTRS)

    Patel, Parimal J.; Messier, Donald R.; Rich, R. E.

    1991-01-01

    Research at the Army Materials Technology Laboratory (AMTL) and elsewhere has shown that many glass properties including elastic modulus, hardness, and corrosion resistance are improved markedly by the substitution of nitrogen for oxygen in the glass structure. Oxynitride glasses, therefore, offer exciting opportunities for making high modulus, high strength fibers. Processes for making oxynitride glasses and fibers of glass compositions similar to commercial oxide glasses, but with considerable enhanced properties, are discussed. We have made glasses with elastic moduli as high as 140 GPa and fibers with moduli of 120 GPa and tensile strengths up to 2900 MPa. AMTL holds a U.S. patent on oxynitride glass fibers, and this presentation discusses a unique process for drawing small diameter oxynitride glass fibers at high drawing rates. Fibers are drawn through a nozzle from molten glass in a molybdenum crucible at 1550 C. The crucible is situated in a furnace chamber in flowing nitrogen, and the fiber is wound in air outside of the chamber, making the process straightforward and commercially feasible. Strengths were considerably improved by improving glass quality to minimize internal defects. Though the fiber strengths were comparable with oxide fibers, work is currently in progress to further improve the elastic modulus and strength of fibers. The high elastic modulus of oxynitride glasses indicate their potential for making fibers with tensile strengths surpassing any oxide glass fibers, and we hope to realize that potential in the near future.

  3. Three dimensionally honeycomb layered double hydroxides framework as a novel fiber coating for headspace solid-phase microextraction of phenolic compounds.

    PubMed

    Abolghasemi, Mir Mahdi; Yousefi, Vahid

    2014-06-06

    A new solid phase microextraction (SPME) fiber based on high-temperature three dimensionally honeycomb layered double hydroxide (TDH-LDH) material is presented. The fiber coating can be prepared easily, it is mechanically stable and exhibits relatively high thermal stability. This study shows that three dimensionally honeycomb layered double hydroxide generated porous morphology. The TDH-LDH material was tested for the extraction of some phenolic and polycyclic aromatic hydrocarbon compounds from aqueous sample solutions in combination with gas chromatography-mass spectrometry (GC-MS). The TDH-LDH fiber contains polar groups and its efficiency for non-polar polycyclic aromatic hydrocarbon compounds was lower than phenolic compounds. On the other hand, a high tendency towards the adsorption of polar phenolic compounds was observed for the proposed fiber. The effects of the extraction and desorption parameters including extraction temperature, extraction time, ionic strength, stirring rate, pH and desorption temperature and time have been studied. In optimum conditions, the repeatability for one fiber (n=5), expressed as relative standard deviation (R.S.D. %), was between 2.8% and 7.1% for the phenolic compounds. The detection limits for the studied phenolic compounds were between 0.02 and 5.8 ng mL(-1). The developed method offers the advantage of being simple to use, with shorter analysis time, lower cost of equipment, thermal stability of fiber and high relative recovery in comparison to conventional methods of analysis.

  4. Fiber coating method

    DOEpatents

    Corman, Gregory Scot

    2001-01-01

    A coating is applied to reinforcing fibers arranged into a tow by coaxially aligning the tow with an adjacent separation layer and winding or wrapping the tow and separation layer onto a support structure in an interleaved manner so that the separation layer separates a wrap of the tow from an adjacent wrap of the tow. A coating can then be uniformly applied to the reinforcing fibers without defects caused by fiber tow to fiber tow contact. The separation layer can be a carbon fiber veil.

  5. Hybrid matrix fiber composites

    DOEpatents

    Deteresa, Steven J.; Lyon, Richard E.; Groves, Scott E.

    2003-07-15

    Hybrid matrix fiber composites having enhanced compressive performance as well as enhanced stiffness, toughness and durability suitable for compression-critical applications. The methods for producing the fiber composites using matrix hybridization. The hybrid matrix fiber composites include two chemically or physically bonded matrix materials, whereas the first matrix materials are used to impregnate multi-filament fibers formed into ribbons and the second matrix material is placed around and between the fiber ribbons that are impregnated with the first matrix material and both matrix materials are cured and solidified.

  6. Fiber optic monitoring device

    DOEpatents

    Samborsky, J.K.

    1993-10-05

    A device for the purpose of monitoring light transmissions in optical fibers comprises a fiber optic tap that optically diverts a fraction of a transmitted optical signal without disrupting the integrity of the signal. The diverted signal is carried, preferably by the fiber optic tap, to a lens or lens system that disperses the light over a solid angle that facilitates viewing. The dispersed light indicates whether or not the monitored optical fiber or system of optical fibers is currently transmitting optical information. 4 figures.

  7. Fiber optic laser rod

    DOEpatents

    Erickson, G.F.

    1988-04-13

    A laser rod is formed from a plurality of optical fibers, each forming an individual laser. Synchronization of the individual fiber lasers is obtained by evanescent wave coupling between adjacent optical fiber cores. The fiber cores are dye-doped and spaced at a distance appropriate for evanescent wave coupling at the wavelength of the selected dye. An interstitial material having an index of refraction lower than that of the fiber core provides the optical isolation for effective lasing action while maintaining the cores at the appropriate coupling distance. 2 figs.

  8. Fiber optic sensors

    NASA Technical Reports Server (NTRS)

    Hesse, J.; Sohler, W.

    1984-01-01

    A survey of the developments in the field of fiber optics sensor technology is presented along with a discussion of the advantages of optical measuring instruments as compared with electronic sensors. The two primary types of fiber optics sensors, specifically those with multiwave fibers and those with monowave fibers, are described. Examples of each major sensor type are presented and discussed. Multiwave detectors include external and internal fiber optics sensors. Among the monowave detectors are Mach-Zender interferometers, Michelson interferometers, Sagnac interferometers (optical gyroscopes), waveguide resonators, and polarimeter sensors. Integrated optical sensors and their application in spectroscopy are briefly discussed.

  9. Fiber coating method

    DOEpatents

    Corman, Gregory Scot

    2003-04-15

    A coating is applied to reinforcing fibers arranged into a tow by coaxially aligning the tow with an adjacent separation layer and winding or wrapping the tow and separation layer onto a support structure in an interleaved manner so that the separation layer separates a wrap of the tow from an adjacent wrap of the tow. A coating can then be uniformly applied to the reinforcing fibers without defects caused by fiber tow to fiber tow contact. The separation layer can be a carbon fiber veil.

  10. Preparation and characterization of microporous fibers for sample preparation and LC-MS determination of drugs.

    PubMed

    Buszewski, Boguslaw; Nowaczyk, Jacek; Ligor, Tomasz; Olszowy, Pawel; Ligor, Magdalena; Wasiniak, Bartlomiej; Miekisch, Wolfram; Schubert, Jochen K; Amann, Anton

    2009-07-01

    The aim of this study was the preparation of polypyrrole (PPy) fibers for solid phase microextraction (SPME). PPy coatings were obtained during the electrochemical polymerization process. The utility of various metal wires (Fe, Cu, Ag, Cu/Ag, kanthal and medical stainless steel) as a support for polymers was compared. Various experimental conditions of the synthesis process such as scan rate, voltage limits and number of scans and deposition time were applied. The average polymer thickness was in the range of 7-125 microm and its weight was in the scope of 0.65-5.6 mg. Different techniques, mainly elemental analysis, Fourier transform infrared spectroscopy, microscopy, and chromatography were performed for the characterization of obtained fibers with microporous structure. The extraction efficiency of cardiovascular drugs (metoprolol, propranolol, oxprenolol, propafenone and mexiletine) by means of fibers was tested. The concentration of mentioned compounds in standard solution was in the span of 10-150 ng/mL. LC-MS was employed for determination of drugs in desorption solution. LODs varied from 0.013 to 1.51 ng/mL for metoprolol and mexiletine respectively. The repeatability of extraction was obtained with the RSD values lower than 10%.

  11. Kinetics of fiber solidification

    PubMed Central

    Mercader, C.; Lucas, A.; Derré, A.; Zakri, C.; Moisan, S.; Maugey, M.; Poulin, P.

    2010-01-01

    Many synthetic or natural fibers are produced via the transformation of a liquid solution into a solid filament, which allows the wet processing of high molecular weight polymers, proteins, or inorganic particles. Synthetic wet-spun fibers are used in our everyday life from clothing to composite reinforcement applications. Spun fibers are also common in nature. Silk solidification results from the coagulation of protein solutions. The chemical phenomena involved in the formation of all these classes of fibers can be quite different but they all share the same fundamental transformation from a liquid to a solid state. The solidification process is critical because it governs the production rate and the strength that fibers can sustain to be drawn and wound. An approach is proposed in this work to investigate the kinetics of fiber solidification. This approach consists in circulating solidifying fibers in the extensional flow of a surrounding liquid. Such as polymers in extensional flows, the fibers break if resultant drag forces exceed the fiber tensile strength. The solidification kinetics of nanotube composite fibers serves as a validation example of this approach. The method could be extended to other systems and advance thereby the science and technology of fiber and textile materials. It is also a way to directly visualize the scission of chain-like systems in extensional flows. PMID:20937910

  12. Splicing of aged fibers

    NASA Astrophysics Data System (ADS)

    Volotinen, Tarja T.; Yuce, Hakan H.; Bonanno, Nicholas; Frantz, Rolf A.; Duffy, Sean

    1993-11-01

    The deployment of fiber in the subscriber loop will require that an optical fiber network maintain the highest possible level of reliability over time, despite being subjected to extremes of temperature, humidity, and other environmental and mechanical stresses imposed on the outside plant. At the same time, both the initial cost and the ongoing maintenance expenses for loop equipment must be kept low. Fiber in the Loop (FITL) applications will entail increased fiber handling. Cable lengths will be shorter, and fiber counts higher, than has been the case so far in long-distance applications. There will also be more cable sheath openings per unit length of cable and/or fiber, as well as more splicing and connectorization. It may become a common practice that a customer is connected to a cable installed many years earlier. In subscriber loops, cables and fibers will be installed in harsher and more varying environments. Fibers will be exposed to higher humidity and temperature, particularly in splice boxes mounted on building walls, in pedestal cabinets, and in other similar enclosures. Corrosive gases and/or liquids may also be present at some locations and will adversely affect the fibers. The combination of increased handling, greater exposure, and more stressful environments may give rise to a need for new, more stringent requirements for fiber mechanical reliability. These can include increaSed fiber strength, increased aging resistance, and increased fatigue resistance.

  13. Fiber optic vibration sensor

    DOEpatents

    Dooley, J.B.; Muhs, J.D.; Tobin, K.W.

    1995-01-10

    A fiber optic vibration sensor utilizes two single mode optical fibers supported by a housing with one optical fiber fixedly secured to the housing and providing a reference signal and the other optical fiber having a free span length subject to vibrational displacement thereof with respect to the housing and the first optical fiber for providing a signal indicative of a measurement of any perturbation of the sensor. Damping or tailoring of the sensor to be responsive to selected levels of perturbation is provided by altering the diameter of optical fibers or by immersing at least a portion of the free span length of the vibration sensing optical fiber into a liquid of a selected viscosity. 2 figures.

  14. Fiber optic vibration sensor

    DOEpatents

    Dooley, Joseph B.; Muhs, Jeffrey D.; Tobin, Kenneth W.

    1995-01-01

    A fiber optic vibration sensor utilizes two single mode optical fibers supported by a housing with one optical fiber fixedly secured to the housing and providing a reference signal and the other optical fiber having a free span length subject to vibrational displacement thereof with respect to the housing and the first optical fiber for providing a signal indicative of a measurement of any perturbation of the sensor. Damping or tailoring of the sensor to be responsive to selected levels of perturbation is provided by altering the diameter of optical fibers or by immersing at least a portion of the free span length of the vibration sensing optical fiber into a liquid of a selected viscosity.

  15. Fiber optic moisture sensor

    DOEpatents

    Kirkham, R.R.

    1984-08-03

    A method and apparatus for sensing moisture changes by utilizing optical fiber technology. One embodiment uses a reflective target at the end of an optical fiber. The reflectance of the target varies with its moisture content and can be detected by a remote unit at the opposite end of the fiber. A second embodiment utilizes changes in light loss along the fiber length. This can be attributed to changes in reflectance of cladding material as a function of its moisture content. It can also be affected by holes or inserts interposed in the cladding material and/or fiber. Changing light levels can also be coupled from one fiber to another in an assembly of fibers as a function of varying moisture content in their overlapping lengths of cladding material.

  16. Fiber Accelerating Structures

    SciTech Connect

    Hammond, Andrew P.; /Reed Coll. /SLAC

    2010-08-25

    One of the options for future particle accelerators are photonic band gap (PBG) fiber accelerators. PBG fibers are specially designed optical fibers that use lasers to excite an electric field that is used to accelerate electrons. To improve PBG accelerators, the basic parameters of the fiber were tested to maximize defect size and acceleration. Using the program CUDOS, several accelerating modes were found that maximized these parameters for several wavelengths. The design of multiple defects, similar to having closely bound fibers, was studied to find possible coupling or the change of modes. The amount of coupling was found to be dependent on distance separated. For certain distances accelerating coupled modes were found and examined. In addition, several non-periodic fiber structures were examined using CUDOS. The non-periodic fibers produced several interesting results and promised more modes given time to study them in more detail.

  17. Indium fluoride glass fibers

    NASA Astrophysics Data System (ADS)

    Saad, Mohammed

    2012-03-01

    Fluoride glasses are the only material that transmit light from ultraviolet to mid-infrared and can be drawn into industrial optical fibers. The mechanical and optical properties of new indium fluoride glass fibers have been investigated. Multimode fiber 190 microns, has very high mechanical strength greater than 100 kpsi and optical loss as low as 45 dB/km between 2 and 4 microns. Unlike chalcogenide glass fibers, indium fluoride fiber has a wide transmission window from 0.3 to 5.5 microns without any absorption peak. Indium fluoride glass fibers are the technology of choice for all application requiring transmission up to 5 micron such as infrared contour measure (IRCM) and chemical sensing. Furthermore, Indium fluoride glasses have low phonon energy and can be heavily doped and co-doped whit rare-earth elements. Therefore they are very promising candidates for infrared fiber lasers.

  18. SPME-GCMS study of the natural attenuation of aviation diesel spilled on the perennial ice cover of Lake Fryxell, Antarctica.

    PubMed

    Jaraula, Caroline M B; Kenig, Fabien; Doran, Peter T; Priscu, John C; Welch, Kathleen A

    2008-12-15

    In January 2003, a helicopter crashed on the 5 m thick perennial ice cover of Lake Fryxell (McMurdo Dry Valleys, East Antarctica), spilling approximately 730 l of aviation diesel fuel (JP5-AN8 mixture). The molecular composition of the initial fuel was analyzed by solid phase microextraction (SPME) gas chromatography-mass spectrometry (GC-MS), then compared to the composition of the contaminated ice, water, and sediments collected a year after the spill. Evaporation is the major agent of diesel weathering in meltpool waters and in the ice. This process is facilitated by the light non-aqueous phase liquid properties of the aviation diesel and by the net upward movement of the ice as a result of ablation. In contrast, in sediment-bearing ice, biodegradation by both alkane- and aromatic-degraders was the prominent attenuation mechanism. The composition of the diesel contaminant in the ice was also affected by the differential solubility of its constituents, some ice containing water-washed diesel and some ice containing exclusively relatively soluble low molecular weight aromatic hydrocarbons such as alkylbenzene and naphthalene homologues. The extent of evaporation, water washing and biodegradation between sites and at different depths in the ice are evaluated on the basis of molecular ratios and the results of JP5-AN8 diesel evaporation experiment at 4 degrees C. Immediate spread of the aviation diesel was enhanced where the presence of aeolian sediments induced formations of meltpools. However, in absence of melt pools, slow spreading of the diesel is possible through the porous ice and the ice cover aquifer.

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

    PubMed

    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.

  20. Application of the experimental design of experiments (DoE) for the determination of organotin compounds in water samples using HS-SPME and GC-MS/MS.

    PubMed

    Coscollà, Clara; Navarro-Olivares, Santiago; Martí, Pedro; Yusà, Vicent

    2014-02-01

    When attempting to discover the important factors and then optimise a response by tuning these factors, experimental design (design of experiments, DoE) gives a powerful suite of statistical methodology. DoE identify significant factors and then optimise a response with respect to them in method development. In this work, a headspace-solid-phase micro-extraction (HS-SPME) combined with gas chromatography tandem mass spectrometry (GC-MS/MS) methodology for the simultaneous determination of six important organotin compounds namely monobutyltin (MBT), dibutyltin (DBT), tributyltin (TBT), monophenyltin (MPhT), diphenyltin (DPhT), triphenyltin (TPhT) has been optimized using a statistical design of experiments (DOE). The analytical method is based on the ethylation with NaBEt4 and simultaneous headspace-solid-phase micro-extraction of the derivative compounds followed by GC-MS/MS analysis. The main experimental parameters influencing the extraction efficiency selected for optimization were pre-incubation time, incubation temperature, agitator speed, extraction time, desorption temperature, buffer (pH, concentration and volume), headspace volume, sample salinity, preparation of standards, ultrasonic time and desorption time in the injector. The main factors (excitation voltage, excitation time, ion source temperature, isolation time and electron energy) affecting the GC-IT-MS/MS response were also optimized using the same statistical design of experiments. The proposed method presented good linearity (coefficient of determination R(2)>0.99) and repeatibilty (1-25%) for all the compounds under study. The accuracy of the method measured as the average percentage recovery of the compounds in spiked surface and marine waters was higher than 70% for all compounds studied. Finally, the optimized methodology was applied to real aqueous samples enabled the simultaneous determination of all compounds under study in surface and marine water samples obtained from Valencia region

  1. Volatile Compound Profiling by HS-SPME/GC-MS-FID of a Core Olive Cultivar Collection as a Tool for Aroma Improvement of Virgin Olive Oil.

    PubMed

    García-Vico, Lourdes; Belaj, Angjelina; Sánchez-Ortiz, Araceli; Martínez-Rivas, José M; Pérez, Ana G; Sanz, Carlos

    2017-01-14

    Virgin olive oil (VOO) is the only food product requiring official sensory analysis to be classified in commercial categories, in which the evaluation of the aroma plays a very important role. The selection of parents, with the aim of obtaining new cultivars with improved oil aroma, is of paramount importance in olive breeding programs. We have assessed the volatile fraction by headspace-solid-phase microextraction/gas chromatography-mass spectrometry-flame ionization detection (HS-SPME/GC-MS-FID) and the deduced aroma properties of VOO from a core set of olive cultivars (Core-36) which possesses most of the genetic diversity found in the World Olive Germplasm Collection (IFAPA Alameda del Obispo) located in Cordoba, Spain. The VOO volatile fractions of Core-36 cultivars display a high level of variability. It is mostly made of compounds produced from polyunsaturated fatty acids through the lipoxygenase pathway, which confirms to be a general characteristic of the olive species (Olea europaea L.). The main group of volatile compounds in the oils was six straight-chain carbon compounds derived from linolenic acid, some of them being the main contributors to the aroma of the olive oils according to their odor activity values (OAV). The high level of variability found for the volatile fraction of the oils from Core-36 and, therefore, for the aroma odor notes, suggest that this core set may be a very useful tool for the choice of optimal parents in olive breeding programs in order to raise new cultivars with improved VOO aroma.

  2. Tequila authenticity assessment by headspace SPME-HRGC-IRMS analysis of 13C/12C and 18O/16O ratios of ethanol.

    PubMed

    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.

  3. The Study of Fingerprint Characteristics of Dayi Pu-Erh Tea Using a Fully Automatic HS-SPME/GC–MS and Combined Chemometrics Method

    PubMed Central

    Lv, Shidong; Wu, Yuanshuang; Zhou, Jiangsheng; Lian, Ming; Li, Changwen; Xu, Yongquan; Liu, Shunhang; Wang, Chao; Meng, Qingxiong

    2014-01-01

    The quality of tea is presently evaluated by the sensory assessment of professional tea tasters, however, this approach is both inconsistent and inaccurate. A more standardized and efficient method is urgently needed to objectively evaluate tea quality. In this study, the chemical fingerprint of 7 different Dayi Pu-erh tea brands and 3 different Ya'an tea brands on the market were analyzed using fully automatic headspace solid-phase microextraction (HS-SPME) combined with gas chromatography-mass spectrometry (GC–MS). A total of 78 volatiles were separated, among 75 volatiles were identified by GC–MS in seven Dayi Pu-erh teas, and the major chemical components included methoxyphenolic compounds, hydrocarbons, and alcohol compounds, such as 1,2,3-trimethoxybenzene, 1,2,4-trimethoxybenzene, 2,6,10,14-tetramethyl-pentadecane, linalool and its oxides, α-terpineol, and phytol. The overlapping ratio of peaks (ORP) of the chromatogram in the seven Dayi Pu-erh tea samples was greater than 89.55%, whereas the ORP of Ya'an tea samples was less than 79.10%. The similarity and differences of the Dayi Pu-erh tea samples were also characterized using correlation coefficient similarity and principal component analysis (PCA). The results showed that the correlation coefficient of similarity of the seven Dayi Pu-erh tea samples was greater than 0.820 and was gathered in a specific area, which showed that samples from different brands were basically the same, despite have some slightly differences of chemical indexes was found. These results showed that the GC-MS fingerprint combined with the PCA approach can be used as an effective tool for the quality assessment and control of Pu-erh tea. PMID:25551231

  4. Determination of volatile organic compounds (VOCs) from wrapping films and wrapped PDO Italian cheeses by using HS-SPME and GC/MS.

    PubMed

    Panseri, Sara; Chiesa, Luca Maria; Zecconi, Alfonso; Soncini, Gabriella; De Noni, Ivano

    2014-06-25

    Nowadays food wrapping assures attractive presentation and simplifies self-service shopping. Polyvinylchloride (PVC)- and polyethylene (PE)-based cling-films are widely used worldwide for wrapping cheeses. For this purpose, films used in retail possess suitable technical properties such as clinginess and unrolling capacity, that are achieved by using specific plasticizers during their manufacturing process. In the present study, the main VOCs of three cling-films (either PVC-based or PE-based) for retail use were characterized by means of Solid-Phase Micro-Extraction and GC/MS. In addition, the effects of cling film type and contact time on the migration of VOCs from the films to four different PDO Italian cheeses during cold storage under light or dark were also investigated. Among the VOCs isolated from cling-films, PVC released 2-ethylhexanol and triacetin. These compounds can likely be considered as a "non-intentionally added substance". These same compounds were also detected in cheeses wrapped in PVC films with the highest concentration found after 20 days storage. The PE cling-film was shown to possess a simpler VOC profile, lacking some molecules peculiar to PVC films. The same conclusions can be drawn for cheeses wrapped in the PE cling-film. Other VOCs found in wrapped cheeses were likely to have been released either by direct transfer from the materials used for the manufacture of cling-films or from contamination of the films. Overall, HS-SPME is shown to be a rapid and solvent free technique to screen the VOCs profile of cling-films, and to detect VOCs migration from cling-films to cheese under real retail storage conditions.

  5. Highly porous nanostructured copper foam fiber impregnated with an organic solvent for headspace liquid-phase microextraction.

    PubMed

    Saraji, Mohammad; Ghani, Milad; Rezaei, Behzad; Mokhtarianpour, Maryam

    2016-10-21

    A new headspace liquid-phase microextraction technique based on using a copper foam nanostructure substrate followed by gas chromatography-flame ionization detection was developed for the determination of volatile organic compounds in water and wastewater samples. The copper foam with highly porous nanostructured walls was fabricated on the surface of a copper wire by a rapid and facile electrochemical process and used as the extractant solvent holder. Propyl benzoate was immobilized in the pores of the copper foam coating and used for the microextraction of benzene, toluene, ethylbenzene and xylenes. The experimental parameters such as the type of organic solvent, desorption temperature, desorption time, salt concentration, sample temperature, equilibrium time and extraction time, were investigated and optimized. Under the optimum conditions, the method detection limit was between 0.06 and 0.25μgL(-1). The relative standard deviation of the method for the analytes at 4-8μgL(-1) concentration level ranged from 7.9 to 11%. The fiber-to-fiber reproducibility for three fibers prepared under the same condition was 9.3-12%. The enrichment factor was in the range of 615-744. Different water samples were analyzed for the evaluation of the method in real sample analysis. Relative recoveries for spiked tap, river and wastewater samples were in the range of 85-94%. Finally, the extraction efficiency of the method was compared with those of headspace single drop microextraction and headspace SPME with the commercial fibers.

  6. Coatings for Graphite Fibers

    NASA Technical Reports Server (NTRS)

    Galasso, F. S.; Scola, D. A.; Veltri, R. D.

    1980-01-01

    Several approaches for applying high resistance coatings continuously to graphite yarn were investigated. Two of the most promising approaches involved (1) chemically vapor depositing (CVD) SiC coatings on the surface of the fiber followed by oxidation, and (2) drawing the graphite yarn through an organo-silicone solution followed by heat treatments. In both methods, coated fibers were obtained which exhibited increased electrical resistances over untreated fibers and which were not degraded. This work was conducted in a previous program. In this program, the continuous CVD SiC coating process used on HTS fiber was extended to the coating of HMS, Celion 6000, Celion 12000 and T-300 graphite fiber. Electrical resistances three order of magnitude greater than the uncoated fiber were measured with no significant degradation of the fiber strength. Graphite fibers coated with CVD Si3N4 and BN had resistances greater than 10(exp 6) ohm/cm. Lower pyrolysis temperatures were used in preparing the silica-like coatings also resulting in resistances as high as three orders of magnitude higher than the uncoated fiber. The epoxy matrix composites prepared using these coated fibers had low shear strengths indicating that the coatings were weak.

  7. Raman fiber lasers

    NASA Astrophysics Data System (ADS)

    Supradeepa, V. R.; Feng, Yan; Nicholson, Jeffrey W.

    2017-02-01

    High-power fiber lasers have seen tremendous development in the last decade, with output powers exceeding multiple kilowatts from a single fiber. Ytterbium has been at the forefront as the primary rare-earth-doped gain medium owing to its inherent material advantages. However, for this reason, the lasers are largely confined to the narrow emission wavelength region of ytterbium. Power scaling at other wavelength regions has lagged significantly, and a large number of applications rely upon the diversity of emission wavelengths. Currently, Raman fiber lasers are the only known wavelength agile, scalable, high-power fiber laser technology that can span the wavelength spectrum. In this review, we address the technology of Raman fiber lasers, specifically focused on the most recent developments. We will also discuss several applications of Raman fiber lasers in laser pumping, frequency conversion, optical communications and biology.

  8. Solid phase microextraction of diclofenac using molecularly imprinted polymer sorbent in hollow fiber combined with fiber optic-linear array spectrophotometry

    NASA Astrophysics Data System (ADS)

    Pebdani, Arezou Amiri; Shabani, Ali Mohammad Haji; Dadfarnia, Shayessteh; Khodadoust, Saeid

    2015-08-01

    A simple solid phase microextraction method based on molecularly imprinted polymer sorbent in the hollow fiber (MIP-HF-SPME) combined with fiber optic-linear array spectrophotometer has been applied for the extraction and determination of diclofenac in environmental and biological samples. The effects of different parameters such as pH, times of extraction, type and volume of the organic solvent, stirring rate and donor phase volume on the extraction efficiency of the diclofenac were investigated and optimized. Under the optimal conditions, the calibration graph was linear (r2 = 0.998) in the range of 3.0-85.0 μg L-1 with a detection limit of 0.7 μg L-1 for preconcentration of 25.0 mL of the sample and the relative standard deviation (n = 6) less than 5%. This method was applied successfully for the extraction and determination of diclofenac in different matrices (water, urine and plasma) and accuracy was examined through the recovery experiments.

  9. Solid phase microextraction of diclofenac using molecularly imprinted polymer sorbent in hollow fiber combined with fiber optic-linear array spectrophotometry.

    PubMed

    Pebdani, Arezou Amiri; Shabani, Ali Mohammad Haji; Dadfarnia, Shayessteh; Khodadoust, Saeid

    2015-08-05

    A simple solid phase microextraction method based on molecularly imprinted polymer sorbent in the hollow fiber (MIP-HF-SPME) combined with fiber optic-linear array spectrophotometer has been applied for the extraction and determination of diclofenac in environmental and biological samples. The effects of different parameters such as pH, times of extraction, type and volume of the organic solvent, stirring rate and donor phase volume on the extraction efficiency of the diclofenac were investigated and optimized. Under the optimal conditions, the calibration graph was linear (r(2)=0.998) in the range of 3.0-85.0 μg L(-1) with a detection limit of 0.7 μg L(-1) for preconcentration of 25.0 mL of the sample and the relative standard deviation (n=6) less than 5%. This method was applied successfully for the extraction and determination of diclofenac in different matrices (water, urine and plasma) and accuracy was examined through the recovery experiments.

  10. Nanotailored Carbon Fibers

    DTIC Science & Technology

    2012-04-27

    precursor fiber and also utilize bi- component spinning along with gel spinning, to obtain small diameter fibers. Various processing parameters during...shape of the fiber. In this regard, we have also conducted single component gel spinning using different gelation bath temperatures (100% methanol). SEM...domestic dishwashing detergent, Palmolive antibacterial , 3 wt% detergent and 97% water) for about a week and retested. *** For 5th trial, tungsten

  11. Fiber Optic Feed

    DTIC Science & Technology

    1990-11-06

    Naval Research Laboratory IIK Washington, DC,20375 5000 NRL Memorandum Report 6741 0 N Fiber Optic Feed DENZIL STILWELL, MARK PARENT AND LEw GOLDBERG...SUBTITLE S. FUNDING NUMBERS Fiber Optic Feed 53-0611-A0 6. AUTHOR(S) P. D. Stilwell, M. G. Parent, L. Goldberg 7. PERFORMING ORGANIZATION NAME(S) AND...DISTRIBUTION CODE Approved for public release; distribution unlimited. 13. ABSTRACT (Maximum 200 words) This report details a Fiber Optic Feeding

  12. Continuous Fiber Ceramic Composites

    SciTech Connect

    2002-09-01

    Fiber-reinforced ceramic composites demonstrate the high-temperature stability of ceramics--with an increased fracture toughness resulting from the fiber reinforcement of the composite. The material optimization performed under the continuous fiber ceramic composites (CFCC) included a series of systematic optimizations. The overall goals were to define the processing window, to increase the robustinous of the process, to increase process yield while reducing costs, and to define the complexity of parts that could be fabricated.

  13. Fiber composite flywheel rim

    DOEpatents

    Davis, Donald E.; Ingham, Kenneth T.

    1987-01-01

    A flywheel 2 comprising a hub 4 having at least one radially projecting disc 6, an annular rim 14 secured to said disc and providing a surface circumferential to said hub, a first plurality of resin-impregnated fibers 22 wound about said rim congruent to said surface, and a shell 26 enclosing said first plurality of fibers and formed by a second plurality of resin-impregnated fibers wound about said rim tangentially to said surface.

  14. Fiber composite flywheel rim

    DOEpatents

    Davis, D.E.; Ingham, K.T.

    1987-04-28

    A flywheel comprising a hub having at least one radially projecting disc, an annular rim secured to said disc and providing a surface circumferential to said hub, a first plurality of resin-impregnated fibers wound about said rim congruent to said surface, and a shell enclosing said first plurality of fibers and formed by a second plurality of resin-impregnated fibers wound about said rim tangentially to said surface. 2 figs.

  15. Fiber optic micro accelerometer

    DOEpatents

    Swierkowski, Steve P.

    2005-07-26

    An accelerometer includes a wafer, a proof mass integrated into the wafer, at least one spring member connected to the proof mass, and an optical fiber. A Fabry-Perot cavity is formed by a partially reflective surface on the proof mass and a partially reflective surface on the end of the optical fiber. The two partially reflective surfaces are used to detect movement of the proof mass through the optical fiber, using an optical detection system.

  16. High Power Fiber Lasers

    DTIC Science & Technology

    2012-08-02

    mode, purity of polarization state, minimization of nonlinear effects, compatibility with all-fiber pumps, and high temperature buffer coatings. Over...nonlinear effects, compatibility with all-fiber pumps, and high temperature buffer coatings. Over the duration of this program the most significant...minimization of nonlinear effects, compatibility with all-fiber pumps, and high temperature buffer coatings. Over the duration of this program the most

  17. Improved Graphite Fiber Adhesion.

    DTIC Science & Technology

    1981-09-01

    determined from a variety of surface analysis techniques , the oxygen-containing functional groups on commercial AS-i graphite fiber are predominantly...heterogenity within the fiber itself or experimental errors within the technique . In the limited time devoted to this work we did not devise a procedure...samples. Drzal optically measured the diameter of each fiber tested. Figure 6 shows the linear regression analysis plot used to determine the polar and

  18. Insulated Fiber Brush.

    DTIC Science & Technology

    An insulated-strand fiber brush is provided for a DC motor /generator. The brush is comprised of a plurality of fiber segments which are insulated from one another near the contact surface of a rotor bar. In one embodiment, insulating spacers are fixed to a brush assembly and wear with the fibers, and in another embodiment insulation is provided by a separate shell. (Author)

  19. Innovative fabrication of the flower-like nanocomposite coating on a nitinol fiber through Fenton's oxidation for selective and sensitive solid-phase microextraction.

    PubMed

    Zhang, Min; Zhen, Qi; Wang, Huiju; Guo, Mei; Zhou, Shanshan; Wang, Xuemei; Du, Xinzhen

    2016-09-01

    A novel flower-like nanostructure was successfully in situ fabricated on the surface of nitinol wire through Fenton's oxidation for the first time. It was found that the densely immobilized coating on the surface of the nitinol fiber was composed of nickel and titanium oxide nanocomposite (NiO/TiO2NC). The NiO/TiO2NC coated fiber was used to extract aromatic compounds coupled with high performance liquid chromatography (HPLC) with UV detection and exhibited excellent extraction efficiency for polycyclic aromatic hydrocarbons (PAHs) with larger delocalized π-system among the studied analytes. Important factors affecting extraction efficiency of PAHs were examined. Under the optimized conditions, the calibration curves were linear in the range from 0.05 to 500μgL(-1) with correlation coefficients of R(2)≥0.999, and the lowest limit of detection of 0.006μgL(-1) was achieved for benzo[a]pyrene. Furthermore, the intra-day and inter-day precisions for the single fiber varied from 4.69% to 5.97% and from 5.28% to 6.32% for five replicates of PAHs at the spiking level of 50μgL(-1), respectively. The fiber-to-fiber precision for five fibers prepared in different batches ranged from 6.19% to 8.35%. The developed method was successfully applied to concentration and determination of target PAHs from real environmental water samples. Moreover, this novel nitinol-based fiber exhibited long lifespan. Therefore, the proposed fiber can be used as a promising candidate for a conventional fused silica-based fiber in SPME.

  20. Solid-phase microextraction (SPME) for the determination of pyrethroids in cucumber and watermelon using liquid chromatography combined with post-column photochemically induced fluorimetry derivatization and fluorescence detection.

    PubMed

    Vázquez, P Parrilla; Mughari, Ahmed R; Galera, M Martínez

    2008-01-21

    A sensitive and efficient solid-phase microextraction (SPME) method for the determination of seven pyrethroid insecticides including fenpropathrin, lambda-cyhalothrin, deltamethrin, fenvalerate, permethrin, tau-fluvalinate and bifenthrin in cucumber and watermelon samples using high performance liquid chromatography combined with post-column photochemically induced fluorimetry derivatization and fluorescence detection (SPME-HPLC-PIF-FD) was developed and validated. The optimum SPME conditions were used for the extraction of samples of both matrices (extraction time 30 min, stirring rate 1100 rpm, extraction temperature 65 degrees C, sample pH 3, soaking time 7 min, desorption time 5 min, ACN content 25%, desorption and soaking solvent was the mobile phase and in static mode). The method was validated in terms of limits of detection (LODs) and the limits of quantification (LOQs) in both IUPAC and EURACHEM criteria. LODs and LOQs were achieved in values lower than the maximum residue levels (MRLs) established in the Spanish regulations for all pesticides in this study (MRLs range between 0.01 and 0.1 mg kg(-1) for all pyrethroid insecticides in both matrices). LOQs according to the second criterion were between 1.5 and 5 microg kg(-1) for cucumber; and between 1.3 and 5 microg kg(-1) for watermelon samples. Precision and recovery studies were evaluated at two concentration levels for each matrix. Good precision was obtained and relative standard deviation values were less than 10% in all cases. Recovery values were calculated at 0.05 and 0.5 mg kg(-1) levels (n=6) and they ranged between 93% and 108% for cucumber and between 91% and 110% for watermelon samples. Applicability of the method to pyrethroids in cucumber and watermelon of commercial samples was demonstrated.

  1. Apparatus Impregnates Weak Fibers

    NASA Technical Reports Server (NTRS)

    Stanfield, Clarence E.; Wilson, Maywood L.

    1989-01-01

    Low-cost apparatus developed for use in conventional drum winding machine to impregnate fibrous materials having very low tensile strengths. Fiber fitted onto freely-spinning unwinding creel. Unwinds from creel between two tension bars onto guide spools, aligns fiber so properly enters sealed reservoir of resin. Stainless-steel metering die at entrance to reservoir aligns fiber and seals reservoir. Beneficial results obtained by use of reservoir made of polyethylene. Composite material made from resin matrices reinforced by fibers have great potential for solving challenging and often critical problems in design of spacecraft, space structures, and terrestrial structures.

  2. Microstructured polarizing fiber

    NASA Astrophysics Data System (ADS)

    Mergo, Pawel; Wójcik, Jan; Czyzewska, Lidia; Walewski, Aleksander

    2005-09-01

    Introduction of metal elements into the optical fiber's structure creates new possibilities of waveguides' parameters' modification especially permit to obtain polarizing fibers. A known solution is introducing of molten metal into a hole situated along a single-mode fibre's core. The alternative manner is deposition of metal layers on the internal surface of those holes. In our laboratory we manufactured new kind of optical fibers named side metal pipe (SMP) optical fiber. Its structure is similar to that of the side-hole optical fiber but the internal surface of the two open holes placed on the both sides of the core is covered with silver. The silver layers were deposited with elaborated in our laboratory static method deposition from liquid phase. The measured polarizing efficiency of this fiber of 1 m length was equal to 25% for 633nm wavelength. In the last time we manufactured the high birefringent single mode SMP fiber with elliptical core (SMK HB). Paper presents the basis of technology of SMK HB optical fiber, description of the static method of preparation of silver layers by liquid phase deposition and geometrical and optical parameters of the SMK HB optical fiber.

  3. Molecularly imprinted polymer coated solid-phase microextraction fibers for determination of Sudan I-IV dyes in hot chili powder and poultry feed samples.

    PubMed

    Hu, Xiaogang; Cai, Quanlin; Fan, Yanan; Ye, Tingting; Cao, Yujuan; Guo, Changjuan

    2012-01-06

    In this research, a novel strategy was developed to prepare molecularly imprinted polymer (MIP) coated solid-phase microextraction fibers on a large scale with Sudan I as template and stainless steel fibers as substrate. More than 20 fibers could be obtained in one glass tube, and the efficiency and coating repeatability were enhanced remarkably in contrast with the yield of only one fiber in our previous works. The obtained MIP-coated stainless steel fibers were characterized by homogeneous and highly cross-linked coating, good chemical and thermal stabilities, high extraction capacities, and specific selectivities to Sudan I-IV dyes. Based on the systemic optimization of extraction conditions, a simple and cost-effective method based on the coupling of MIP-coated SPME with high-performance liquid chromatography was developed for the fast and selective determination of trace Sudan I-IV dyes in hot chili powder and poultry feed samples. The limits of detection of Sudan I-IV dyes were within 2.5-4.6 ng g(-1), and the spiked recoveries were in the range of 86.3-96.3% for hot chili powder sample and 84.6-97.4% for poultry feed sample.

  4. Exploration of metal-organic framework MOF-177 coated fibers for headspace solid-phase microextraction of polychlorinated biphenyls and polycyclic aromatic hydrocarbons.

    PubMed

    Wang, Guanhua; Lei, Yongqian; Song, Huacan

    2015-11-01

    Metal-organic frameworks (MOFs) have received much attention in analytical science for their large langmuir surface and high thermostability. Herein MOF-177-coated solid-phase micro-extraction (SPME) fibers were fabricated on etched stainless steel by an adhensive method, and applied to the enrichment of polychlorinated biphenyls (PCB01, PCB05, PCB29, PCB47, PCB98, PCB154, PCB171, PCB201) and polycyclic aromatic hydrocarbons (ANY, ANA, FLU, PHE, ANT, FLT, PYR) from environmental water samples. Several parameters affecting the extraction efficiency were optimized prior to the gas chromatography-mass spectrometry analysis, including extraction temperature and time, desorption time, stirring rate and salt addition. The results indicated that the coated fiber gave low detection limits (0.69-4.42 ng L(-1)) and good repeatability with the RSD ranging from 1.47% to 8.67% for PCBs and PAHs. The recoveries were between 81.8% and 113% with the spiked level of 10 ng L(-1) for the real water samples. Besides, the MOF-177 coated fiber was stable enough over 100 extraction cycles and the RSD for fiber-to- fiber reproducibility was less than 9.82% during the experiment.

  5. Fabrication of metal-organic framework MIL-88B films on stainless steel fibers for solid-phase microextraction of polychlorinated biphenyls.

    PubMed

    Wu, Ye-Yu; Yang, Cheng-Xiong; Yan, Xiu-Ping

    2014-03-21

    Metal-organic frameworks (MOFs) have received considerable attention as novel sorbents for sample preparation due to their fascinating structures and functionalities such as large surface area, good thermal stability, and uniform structured nanoscale cavities. Here, we report the application of a thermal and solvent stable MOF MIL-88B with nanosized bipyramidal cages and large surface area for solid-phase microextraction (SPME) of polychlorinated biphenyls (PCBs). Novel MIL-88B coated fiber was fabricated via an in situ hydrothermal growth of MIL-88B film on etched stainless steel fiber. The MIL-88B coated fiber gave large enhancement factors (757-2243), low detection limits (0.45-1.32ngL(-1)), and good linearity (5-200ngL(-1)) for PCBs. The relative standard deviation (RSD) for six replicate extractions of PCBs at 100ngL(-1) on MIL-88B coated fiber ranged from 4.2% to 8.7%. The recoveries for spiked PCBs (10ngL(-1)) in water and soil samples were in the range of 79.7-103.2%. Besides, the MIL-88B coated fiber was stable enough for 150 extraction cycles without significant loss of extraction efficiency. The developed method was successfully applied to the determination of PCBs in water samples and soil samples.

  6. Ultrafine PBI fibers and yarns

    NASA Technical Reports Server (NTRS)

    Leal, J. R.; Tan, M.

    1979-01-01

    Gentle precisely controlled process is used to draw polybenzimidazole (PBI) fibers to denier as low as 0.17 per fiber. Yarns of lightweight fibers could be useful in applications where lightweight textiles must withstand high temperatures, corrosion, or radiation.

  7. Soluble and insoluble fiber (image)

    MedlinePlus

    Dietary fiber is the part of food that is not affected by the digestive process in the body. ... of the stool. There are two types of dietary fiber, soluble and insoluble. Soluble fiber retains water and ...

  8. Preconcentration and determination of polybrominated diphenyl ethers in environmental water samples by solid-phase microextraction with Fe3O4-coated bamboo charcoal fibers prior to gas chromatography-mass spectrometry.

    PubMed

    Zhao, Ru-Song; Liu, Yan-Long; Chen, Xiang-Feng; Yuan, Jin-Peng; Bai, Ai-Ying; Zhou, Jia-Bin

    2013-03-26

    In this paper, bamboo charcoals were modified using Fe3O4 nanosheets for the first time. The composites, as a novel solid-phase microextraction (SPME) fiber coating, were used for the extraction of seven polybrominated diphenyl ethers (PBDEs) in environmental water samples. The extraction factors (stirring rate, extraction time, and ionic strength) and desorption factors (desorption time and desorption temperature) of the fibers were systematically investigated and optimized. Under optimum conditions, the linear range was 1-1000 ng L(-1). Based on the ratio of chromatographic signal to base line noise (SN(-1)=3), the limits of detection (LODs) can reach 0.25-0.62 ng L(-1). The novel method was successful in the analysis of PBDEs in real environmental water samples. The results indicate that bamboo charcoal/Fe3O4 as an SPME coating material coupled with gas chromatography-negative chemical ionization-mass spectrometry is an excellent method for the routine analysis of PBDEs at trace levels in environmental water samples.

  9. Optimization of a novel method for determination of benzene, toluene, ethylbenzene, and xylenes in hair and waste water samples by carbon nanotubes reinforced sol-gel based hollow fiber solid phase microextraction and gas chromatography using factorial experimental design.

    PubMed

    Es'haghi, Zarrin; Ebrahimi, Mahmoud; Hosseini, Mohammad-Saeid

    2011-05-27

    A novel design of solid phase microextraction fiber containing carbon nanotube reinforced sol-gel which was protected by polypropylene hollow fiber (HF-SPME) was developed for pre-concentration and determination of BTEX in environmental waste water and human hair samples. The method validation was included and satisfying results with high pre-concentration factors were obtained. In the present study orthogonal array experimental design (OAD) procedure with OA(16) (4(4)) matrix was applied to study the effect of four factors influencing the HF-SPME method efficiency: stirring speed, volume of adsorption organic solvent, extraction and desorption time of the sample solution, by which the effect of each factor was estimated using individual contributions as response functions in the screening process. Analysis of variance (ANOVA) was employed for estimating the main significant factors and their percentage contributions in extraction. Calibration curves were plotted using ten spiking levels of BTEX in the concentration ranges of 0.02-30,000ng/mL with correlation coefficients (r) 0.989-0.9991 for analytes. Under the optimized extraction conditions, the method showed good linearity (0.3-20,000ng/L), repeatability, low limits of detections (0.49-0.7ng/L) and excellent pre-concentration factors (185-1872). The best conditions which were estimated then applied for the analysis of BTEX compounds in the real samples.

  10. Method of carbonizing polyacrylonitrile fibers

    NASA Technical Reports Server (NTRS)

    Cagliostro, D. E.; Lerner, N. R. (Inventor)

    1983-01-01

    This invention relates to a method of carbonizing polyacrylonitrile fibers by exposing the fibers at an elevated temperature to an oxidizing atmosphere; then exposing the oxidized fibers to an atmosphere of an inert gas such as nitrogen containing a carbonaceous material such as acetylene. The fibers are preferably treated with an organic compound, for example benzoic acid, before the exposure to an oxidizing atmosphere. The invention also relates to the resulting fibers. The treated fibers have enhanced tensile strength.

  11. Low dielectric polyimide fibers

    NASA Technical Reports Server (NTRS)

    Dorogy, William E., Jr. (Inventor); St.clair, Anne K. (Inventor)

    1994-01-01

    A high temperature resistant polyimide fiber that has a dielectric constant of less than 3 is presented. The fiber was prepared by first reacting 2,2-bis (4-(4aminophenoxy)phenyl) hexafluoropropane with 2,2-bis (3,4-dicarboxyphenyl) hexafluoropropane dianhydride in an aprotic solvent to form a polyamic acid resin solution. The polyamic acid resin solution is then extruded into a coagulation medium to form polyamic acid fibers. The fibers are thermally cured to their polyimide form. Alternatively, 2,2-bis(4-(4-aminophenoxy)phenyl) hexafluoropropane is reacted with 2,2-bis(3,4-dicarboxyphenyl) hexafluoropropane dianhydride to form a polyamic acid, and the polyamic acid is chemically converted to its polyimide form. The polyimide is then dissolved in a solvent to form a polyimide resin solution, and the polyimide resin is extruded into a coagulation medium to form a polyimide wet gel filament. In order to obtain polyimide fibers of increased tensile properties, the polyimide wet gel filaments are stretched at elevated temperatures. The tensile properties of the fibers were measured and found to be in the range of standard textile fibers. Polyimide fibers obtained by either method will have a dielectric constant similar to that of the corresponding polymer, viz., less than 3 at 10 GHz.

  12. Diamond fiber field emitters

    DOEpatents

    Blanchet-Fincher, Graciela B.; Coates, Don M.; Devlin, David J.; Eaton, David F.; Silzars, Aris K.; Valone, Steven M.

    1996-01-01

    A field emission electron emitter comprising an electrode formed of at least one diamond, diamond-like carbon or glassy carbon composite fiber, said composite fiber having a non-diamond core and a diamond, diamond-like carbon or glassy carbon coating on said non-diamond core, and electronic devices employing such a field emission electron emitter.

  13. Multimode optical fiber

    SciTech Connect

    Bigot-Astruc, Marianne; Molin, Denis; Sillard, Pierre

    2014-11-04

    A depressed graded-index multimode optical fiber includes a central core, an inner depressed cladding, a depressed trench, an outer depressed cladding, and an outer cladding. The central core has an alpha-index profile. The depressed claddings limit the impact of leaky modes on optical-fiber performance characteristics (e.g., bandwidth, core size, and/or numerical aperture).

  14. Fiber Laser Array

    DTIC Science & Technology

    2004-01-01

    telecommunications market and do not emphasize high powers. Because high power applications are of significant interest to the Air Force, we were interested in fiber...available from NTIC . 9. T.B. Simpson, A. Gavrielides and P. Peterson, “Extraction Characteristics of a Dual Fiber Compound Cavity,” Optics Express 10

  15. Fiber Sensor Technology Today

    NASA Astrophysics Data System (ADS)

    Hotate, Kazuo

    2006-08-01

    Fiber sensor technologies are overviewed. Since the early 1970s, this field has been developed, on the basis of the same devices and photonic principles as fiber communication technologies. Besides simple configurations, in which the fiber acts only as a data transmission line, sophisticated configurations have also been developed, in which the fiber is used as a device to realize unique sensing mechanisms. The fiber optic gyroscope (FOG) is a good example, and has been developed as an absolute rotation sensor used, for example, for navigation and/or attitude control applications. Compared with traditional spinning-mass gyroscopes, the FOG has advantages, such as a short warming-up time, a light weight, and easy handling. A Japanese satellite, which was launched in August 2005 with a mission to observe the aurora, is controlled with a FOG. The FOG has also been used in consumer applications, such as the camera stabilizer, radio-controlled (RC) helicopter navigation, and the control of humanoid robots. Recently, distributed and multiplexed sensing schemes, in particular, have been studied and developed, in which a long fiber acts like a “nerve” for feeling the strain and/or the temperature distribution along the fiber. Performances of artificial nerve systems have markedly improved within the last couple of years, in spatial resolution and measurement speed. By embedding the “fiber-optic nerve system” in aircraft wings, bridges and tall buildings, these materials and structures can sense damage to prevent disasters.

  16. ROLE OF FIBER MODIFICATION IN NATURAL FIBER COMPOSITE PROCESSING

    SciTech Connect

    Fifield, Leonard S.; Denslow, Kayte M.; Gutowska, Anna; Simmons, Kevin L.; Holbery, Jim

    2005-11-03

    The prediction and characterization of the adhesion between fiber, surface treatment, and polymer is critical to the success of large-scale natural fiber based polymer composites in automotive semi-structural application. The two primary factors limiting the use of natural fiber in polymer composites are fiber moisture uptake and fiber degradation during high-temperature processing. In this study, we have developed several fiber surface modification techniques and analyzed the fiber-polymer adhesion of modified fibers to more clearly understand the critical parameters controlling moisture uptake, swelling, and fiber degradation due to interfacial structure. We will present a overview of surface modification techniques we have applied to date for hemp fiber sources, and illustrate a path to characterize surface modification effects on natural fiber adhesion in thermoplastic composites.

  17. Solid Phase Microextraction (SPME) as a Method to Defect the Presence of Escherichia Coli in Waster by Headspace Sampling and Gas Chromatography/Mass Spectrometry Analysis

    DTIC Science & Technology

    2002-01-01

    to penetrate the septum of the sample vial. In the extraction step, the fiber is lowered from the needle into the sample by depressing the plunger...GPO, 1999. 4. Macfarlane, GT and Macfarlane, S. “Human Colonic Microbiota : Ecology, Physiology and Metabolic Potential of Intestinal

  18. Ion-exchange hollow fibers

    NASA Technical Reports Server (NTRS)

    Rembaum, Alan (Inventor); Yen, Shiao-Ping S. (Inventor); Klein, Elias (Inventor)

    1977-01-01

    An ion-exchange hollow fiber is prepared by introducing into the wall of the fiber polymerizable liquid monomers, and polymerizing the monomers therein to form solid, insoluble, cross-linked, ion-exchange resin particles which embed in the wall of the fiber. Excess particles blocking the central passage or bore of the fiber are removed by forcing liquid through the fiber. The fibers have high ion-exchange capacity, a practical wall permeability and good mechanical strength even with very thin wall dimensions. Experimental investigation of bundles of ion-exchange hollow fibers attached to a header assembly have shown the fiber to be very efficient in removing counterions from solution.

  19. Ion-exchange hollow fibers

    NASA Technical Reports Server (NTRS)

    Rembaum, Alan (Inventor); Yen, Shiao-Ping S. (Inventor); Klein, Elias (Inventor)

    1980-01-01

    An ion-exchange hollow fiber is prepared by introducing into the wall of the fiber polymerizable liquid monomers, and polymerizing the monomers therein to form solid, insoluble, cross-linked, ion-exchange resin particles which embed in the wall of the fiber. Excess particles blocking the central passage or bore of the fiber are removed by forcing liquid through the fiber. The fibers have high ion-exchange capacity, a practical wall permeability and good mechanical strength even with very thin wall dimensions. Experimental investigation of bundles of ion-exchange hollow fibers attached to a header assembly have shown the fiber to be very efficient in removing counterions from solution.

  20. Ion-exchange hollow fibers

    NASA Technical Reports Server (NTRS)

    Rembaum, A.; Yen, S. P. S.; Klein, E. (Inventor)

    1976-01-01

    An ion-exchange hollow fiber is prepared by introducing into the wall of the fiber polymerizable liquid monomers, and polymerizing the monomers therein to form solid, insoluble, crosslinked, ion-exchange resin particles which embed in the wall of the fiber. Excess particles blocking the central passage or bore of the fiber are removed by forcing liquid through the fiber. The fibers have high ion-exchange capacity, a practical wall permeability and good mechanical strength even with very thin wall dimensions. Experimental investigation of bundles of ion-exchange hollow fibers attached to a header assembly have shown the fiber to be very efficient in removing counterions from solution.

  1. Fiber optic hydrophone

    DOEpatents

    Kuzmenko, P.J.; Davis, D.T.

    1994-05-10

    A miniature fiber optic hydrophone based on the principles of a Fabry-Perot interferometer is disclosed. The hydrophone, in one embodiment, includes a body having a shaped flexible bladder at one end which defines a volume containing air or suitable gas, and including a membrane disposed adjacent a vent. An optical fiber extends into the body with one end terminating in spaced relation to the membrane. Acoustic waves in the water that impinge on the bladder cause the pressure of the volume therein to vary causing the membrane to deflect and modulate the reflectivity of the Fabry-Perot cavity formed by the membrane surface and the cleaved end of the optical fiber disposed adjacent to the membrane. When the light is transmitted down the optical fiber, the reflected signal is amplitude modulated by the incident acoustic wave. Another embodiment utilizes a fluid filled volume within which the fiber optic extends. 2 figures.

  2. Fiber optic hydrophone

    DOEpatents

    Kuzmenko, Paul J.; Davis, Donald T.

    1994-01-01

    A miniature fiber optic hydrophone based on the principles of a Fabry-Perot interferometer. The hydrophone, in one embodiment, includes a body having a shaped flexible bladder at one end which defines a volume containing air or suitable gas, and including a membrane disposed adjacent a vent. An optic fiber extends into the body with one end terminating in spaced relation to the membrane. Acoustic waves in the water that impinge on the bladder cause the pressure of the volume therein to vary causing the membrane to deflect and modulate the reflectivity of the Fabry-Perot cavity formed by the membrane surface and the cleaved end of the optical fiber disposed adjacent to the membrane. When the light is transmitted down the optical fiber, the reflected signal is amplitude modulated by the incident acoustic wave. Another embodiment utilizes a fluid filled volume within which the fiber optic extends.

  3. Woven fiber optics.

    PubMed

    Schmidt, A C; Courtney-Pratt, J S; Ross, E A

    1975-02-01

    In this paper we describe how the art of weaving can be applied to fiber optics in order to produce precisely controlled reproducible image guides and image dissectors. As examples of the types of device for which woven fiber optics are applicable, we describe a 3:1 interleaver for use with a cathode-ray tube to produce color images, and a high speed alpha numeric output device. The techniques of weaving fiber optics are discussed in sufficient detail in order to allow for further work. Although, in principle, one might be able to weave glass optical fibers, all the work described here made use of plastic optical fibers 0.25 mm in diameter.

  4. Splicing plastic optical fibers

    NASA Astrophysics Data System (ADS)

    Carson, Susan D.; Salazar, Roberto A.

    1991-12-01

    Polymethylmethacrylate (PMMA) plastic optical fiber (500 micrometers diameter, fluoropolymer cladding) has been spliced using a fused silica sleeve and a variety of solvent/PMMA solutions as adhesives. Mechanical splicing using index matching fluid has also been investigated. To ensure good bonding and minimize scattering, fiber ends are polished prior to application of adhesive. Using an LED ((lambda) max approximately 640 nm), losses are routinely less than 1.0 dB/splice, and some adhesive formulations have exhibited losses as low as 0.2 dB/splice. Five-meter fibers with as many as ten splices/fiber have been monitored over a period of several months. No fiber has exhibited an increase in optical loss with time.

  5. Fluorescent fiber diagnostics

    DOEpatents

    Toeppen, John S.

    1994-10-04

    A fluorescent fiber (13) having a doped core (16) is pumped (11) by light (18) of a relatively short wavelength to produce fluorescence at a longer wavelength that is detected by detector (24). The level of fluorescence is monitored (26) and evaluated to provide information as to the excitation of the fiber (13) or the environment thereof. In particular, the level of intensity of the detected fluorescence may be used to measure the intensity of a light beam (18) passing axially through an optical fiber system (12) (FIG. 1 ), or the intensity of a light beam (46) passing radially through a fluorescent fiber (13) (FIG. 2 ), or the level of a fluid (32) in a tank (31) (FIG. 3 ), or a scintillation event (37) in a fluorescent fiber (13) pumped to produce amplification of the scintillation event (FIG. 4 ).

  6. Fluorescent fiber diagnostics

    DOEpatents

    Toeppen, John S.

    1994-01-01

    A fluorescent fiber (13) having a doped core (16) is pumped (11) by light (18) of a relatively short wavelength to produce fluorescence at a longer wavelength that is detected by detector (24). The level of fluorescence is monitored (26) and evaluated to provide information as to the excitation of the fiber (13) or the environment thereof. In particular, the level of intensity of the detected fluorescence may be used to measure the intensity of a light beam (18) passing axially through an optical fiber system (12) (FIG. 1 ), or the intensity of a light beam (46) passing radially through a fluorescent fiber (13) (FIG. 2 ), or the level of a fluid (32) in a tank (31) (FIG. 3 ), or a scintillation event (37) in a fluorescent fiber (13) pumped to produce amplification of the scintillation event (FIG. 4 ).

  7. Remote optical fiber dosimetry

    NASA Astrophysics Data System (ADS)

    Huston, A. L.; Justus, B. L.; Falkenstein, P. L.; Miller, R. W.; Ning, H.; Altemus, R.

    2001-09-01

    Optical fibers offer a unique capability for remote monitoring of radiation in difficult-to-access and/or hazardous locations. Optical fiber sensors can be located in radiation hazardous areas and optically interrogated from a safe distance. A variety of remote optical fiber radiation dosimetry methods have been developed. All of the methods take advantage of some form of radiation-induced change in the optical properties of materials such as: radiation-induced darkening due to defect formation in glasses, luminescence from native defects or radiation-induced defects, or population of metastable charge trapping centers. Optical attenuation techniques are used to measure radiation-induced darkening in fibers. Luminescence techniques include the direct measurement of scintillation or optical excitation of radiation-induced luminescent defects. Optical fiber radiation dosimeters have also been constructed using charge trapping materials that exhibit thermoluminescence or optically stimulated luminescence (OSL).

  8. Python fiber optic seal

    SciTech Connect

    Ystesund, K.; Bartberger, J.; Brusseau, C.; Fleming, P.; Insch, K.; Tolk, K.

    1993-08-01

    Sandia National Laboratories has developed a high security fiber optic seal that incorporates tamper resistance features that are not available in commercial fiber optic seals. The Python Seal is a passive fiber optic loop seal designed to give indication of unauthorized entry. The seal includes a fingerprint feature that provides seal identity information in addition to the unique fiber optic pattern created when the seal is installed. The fiber optic cable used for the seal loop is produced with tamper resistant features that increase the difficulty of attacking that component of a seal. A Seal Reader has been developed that will record the seal signature and the fingerprint feature of the seal. A Correlator software program then compares seal images to establish a match or mismatch. SNL is also developing a Polaroid reader to permit hard copies of the seal patterns to be obtained directly from the seal.

  9. Method for the preparation of carbon fiber from polyolefin fiber precursor, and carbon fibers made thereby

    DOEpatents

    Naskar, Amit Kumar; Hunt, Marcus Andrew; Saito, Tomonori

    2015-08-04

    Methods for the preparation of carbon fiber from polyolefin fiber precursor, wherein the polyolefin fiber precursor is partially sulfonated and then carbonized to produce carbon fiber. Methods for producing hollow carbon fibers, wherein the hollow core is circular- or complex-shaped, are also described. Methods for producing carbon fibers possessing a circular- or complex-shaped outer surface, which may be solid or hollow, are also described.

  10. 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

    NASA Astrophysics Data System (ADS)

    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.

  11. Chemical differences in volatiles between Melittis melissophyllum L. subsp. melissophyllum and subsp. albida (Guss) P. W. Ball (Lamiaceae) determined by solid-phase microextraction (SPME) coupled with GC/FID and GC/MS.

    PubMed

    Maggi, Filippo; Conti, Fabio; Cristalli, Gloria; Giuliani, Claudia; Papa, Fabrizio; Sagratini, Gianni; Vittori, Sauro

    2011-02-01

    Melittis melissophyllum (Lamiaceae) is a perennial herb, typical of woody places, occurring in Italy with two subspecies, i.e., melissophyllum and albida. So far, the classification of these two taxa was only based on morphology, i.e., the presence of glandular trichomes, the dimension of the leaves, and the number of teeth on each side as the main discriminant characters. To find marker compounds to chemically discriminate the subsp. melissophyllum with respect to the subsp. albida, a solid-phase microextraction SPME analysis coupled with GC/FID (=flame ionization detector) and GC/MS was carried out. SPME proved to be a chemotaxonomically useful technique that permitted a clearly differentiation of the two subspecies at headspace level. The subsp. melissophyllum was characterized by high amount of the mushroom alcohol oct-1-en-3-ol and the phenolic coumarin, whilst the subsp. albida exhibited a high content in monoterpenes and sesquiterpenes, α-pinene, sabinene, and (E)-caryophyllene being the major compounds. Multivariate chemometric techniques, such as cluster analysis (CA) and principal-component analysis (PCA), were used to support chemical data and characterize the population according to the taxonomy. In addition, the micromorphology and distribution of glandular trichomes of both subspecies were studied by scanning electron microscopy (SEM).

  12. Fiber Pulling Apparatus

    NASA Technical Reports Server (NTRS)

    Workman, Gary L.; Smith, Guy A.; OBrien, Sue; Adcock, Leonard

    1998-01-01

    The fiber optics industry has grown into a multi-billion marketplace that will continue to grow into the 21st century. Optical fiber communications is currently dominated by silica glass technology. Successful efforts to improve upon the low loss transmission characteristics of silica fibers have propelled the technology into the forefront of the communications industry. However, reaching the theoretical transmission capability of silica fiber through improved processing has still left a few application areas in which other fiber systems can provide an influential role due to specific characteristics of high theoretical transmission in the 2 - 3 micron wavelength region. One of the other major materials used for optical fibers is the systems based upon Heavy Metal Fluoride Glass (HMFG). Commercial interest is driven primarily by the potential for low loss repeaterless infrared fibers. An example of the major communications marketplace which would benefit from the long distance repeaterless capability of infrared fibers is the submarine cables which link the continents. When considering commercial interests, optical fiber systems provide a healthy industrial position which continues to expand. Major investments in the systems used for optical fiber communications have continued to increase each year and are predicted to continue well into the next century. Estimates of 8.5% compounded annually are predicted through 1999 for the North American market and 1 1 % worldwide. The growth for the optical fiber cable itself is expected to continue between 44 and 50 per cent of the optical fiber communications budget through 1999. The total budget in 1999 world-wide is expected to be in the neighborhood of $9 billion. Another survey predicts that long haul telecommunications represents 15% of a world-wide fiber optics market in 1998. The actual amount allotted to cable was not specified. However, another market research had predicted that the cable costs alone represents more

  13. Fiber optic hydrogen sensor

    DOEpatents

    Buchanan, B.R.; Prather, W.S.

    1991-01-01

    Apparatus and method for detecting a chemical substance by exposing an optic fiber having a core and a cladding to the chemical substance so that the chemical substance can be adsorbed onto the surface of the cladding. The optic fiber is coiled inside a container having a pair of valves for controlling the entrance and exit of the substance. Light from a light source is received by one end of the optic fiber, preferably external to the container, and carried by the core of the fiber. Adsorbed substance changes the transmissivity of the fiber as measured by a spectrophotometer at the other end, also preferably external to the container. Hydrogen is detected by the absorption of infrared light carried by an optic fiber with a silica cladding. Since the adsorption is reversible, a sensor according to the present invention can be used repeatedly. Multiple positions in a process system can be monitored using a single container that can be connected to each location to be monitored so that a sample can be obtained for measurement, or, alternatively, containers can be placed near each position and the optic fibers carrying the partially-absorbed light can be multiplexed for rapid sequential reading, by a single spectrophotometer.

  14. Fiber optic hydrogen sensor

    DOEpatents

    Buchanan, B.R.; Prather, W.S.

    1992-10-06

    An apparatus and method are described for detecting a chemical substance by exposing an optic fiber having a core and a cladding to the chemical substance so that the chemical substance can be adsorbed onto the surface of the cladding. The optic fiber is coiled inside a container having a pair of valves for controlling the entrance and exit of the substance. Light from a light source is received by one end of the optic fiber, preferably external to the container, and carried by the core of the fiber. Adsorbed substance changes the transmissivity of the fiber as measured by a spectrophotometer at the other end, also preferably external to the container. Hydrogen is detected by the absorption of infrared light carried by an optic fiber with a silica cladding. Since the adsorption is reversible, a sensor according to the present invention can be used repeatedly. Multiple positions in a process system can be monitored using a single container that can be connected to each location to be monitored so that a sample can be obtained for measurement, or, alternatively, containers can be placed near each position and the optic fibers carrying the partially-absorbed light can be multiplexed for rapid sequential reading by a single spectrophotometer. 4 figs.

  15. Fiber optic hydrogen sensor

    DOEpatents

    Buchanan, Bruce R.; Prather, William S.

    1992-01-01

    An apparatus and method for detecting a chemical substance by exposing an optic fiber having a core and a cladding to the chemical substance so that the chemical substance can be adsorbed onto the surface of the cladding. The optic fiber is coiled inside a container having a pair of valves for controlling the entrance and exit of the substance. Light from a light source is received by one end of the optic fiber, preferably external to the container, and carried by the core of the fiber. Adsorbed substance changes the transmissivity of the fiber as measured by a spectrophotometer at the other end, also preferably external to the container. Hydrogen is detected by the absorption of infrared light carried by an optic fiber with a silica cladding. Since the adsorption is reversible, a sensor according to the present invention can be used repeatedly. Multiple positions in a process system can be monitored using a single container that can be connected to each location to be monitored so that a sample can be obtained for measurement, or, alternatively, containers can be placed near each position and the optic fibers carrying the partially-absorbed light can be multiplexed for rapid sequential reading by a single spectrophotometer.

  16. Chiral fiber sensors

    NASA Astrophysics Data System (ADS)

    Kopp, Victor I.; Churikov, Victor M.; Singer, Jonathan; Neugroschl, Daniel; Genack, Azriel Z.

    2010-04-01

    We have fabricated a variety of chiral fiber sensors by twisting one or more standard or custom optical fibers with noncircular or nonconcentric core as they pass though a miniature oven. The resulting structures are as stable as the glass material and can be produced with helical pitch ranging from microns to hundreds of microns. The polarization selectivity of the chiral gratings is determined by the geometry of the fiber cross section. Single helix structures are polarization insensitive, while double helix gratings interact only with a single optical polarization component. Both single and double helix gratings may function as a fiber long period grating, coupling core and cladding modes or as a diffraction grating scattering light from the fiber core out of the fiber. The resulting dips in the transmission spectrum are sensitive to fiber elongation, twist and temperature, and (in the case of the long period gratings) to the refractive index of the surrounding medium. The suitability of chiral gratings for sensing temperature, elongation, twist and liquid levels will be discussed. Gratings made of radiation sensitive glass can be used to measure the cumulative radiation dose, while gratings made of radiation-hardened glass are suitable for stable sensing of the environment in nuclear power plants. Excellent temperature stability up to 900°C is found in pure silica chiral diffraction grating sensors.

  17. Fiber Optic Microphone

    NASA Technical Reports Server (NTRS)

    Cho, Y. C.; George, Thomas; Norvig, Peter (Technical Monitor)

    1999-01-01

    Research into advanced pressure sensors using fiber-optic technology is aimed at developing compact size microphones. Fiber optic sensors are inherently immune to electromagnetic noise, and are very sensitive, light weight, and highly flexible. In FY 98, NASA researchers successfully designed and assembled a prototype fiber-optic microphone. The sensing technique employed was fiber optic Fabry-Perot interferometry. The sensing head is composed of an optical fiber terminated in a miniature ferrule with a thin, silicon-microfabricated diaphragm mounted on it. The optical fiber is a single mode fiber with a core diameter of 8 micron, with the cleaved end positioned 50 micron from the diaphragm surface. The diaphragm is made up of a 0.2 micron thick silicon nitride membrane whose inner surface is metallized with layers of 30 nm titanium, 30 nm platinum, and 0.2 micron gold for efficient reflection. The active sensing area is approximately 1.5 mm in diameter. The measured differential pressure tolerance of this diaphragm is more than 1 bar, yielding a dynamic range of more than 100 dB.

  18. Kinetics of stress fibers

    NASA Astrophysics Data System (ADS)

    Stachowiak, Matthew R.; O'Shaughnessy, Ben

    2008-02-01

    Stress fibers are contractile cytoskeletal structures, tensile actomyosin bundles which allow sensing and production of force, provide cells with adjustable rigidity and participate in various processes such as wound healing. The stress fiber is possibly the best characterized and most accessible multiprotein cellular contractile machine. Here we develop a quantitative model of the structure and relaxation kinetics of stress fibers. The principal experimentally known features are incorporated. The fiber has a periodic sarcomeric structure similar to muscle fibers with myosin motor proteins exerting contractile force by pulling on actin filaments. In addition the fiber contains the giant spring-like protein titin. Actin is continuously renewed by exchange with the cytosol leading to a turnover time of several minutes. In order that steady state be possible, turnover must be regulated. Our model invokes simple turnover and regulation mechanisms: actin association and dissociation occur at filament ends, while actin filament overlap above a certain threshold in the myosin-containing regions augments depolymerization rates. We use the model to study stress fiber relaxation kinetics after stimulation, as observed in a recent experimental study where some fiber regions were contractile and others expansive. We find that two distinct episodes ensue after stimulation: the turnover-overlap system relaxes rapidly in seconds, followed by the slow relaxation of sarcomere lengths in minutes. For parameter values as they have been characterized experimentally, we find the long time relaxation of sarcomere length is set by the rate at which actin filaments can grow or shrink in response to the forces exerted by the elastic and contractile elements. Consequently, the stress fiber relaxation time scales inversely with both titin spring constant and the intrinsic actin turnover rate. The model's predicted sarcomere velocities and contraction-expansion kinetics are in good

  19. Infrared Fiber Optics.

    DTIC Science & Technology

    1979-12-01

    This unit is thca placed in a larger plastic tube which mates with the fiber connectors. Commercial AMP connectors are used that allow the fiber cable...AD-A082 450 HUSHES RESEARCH LABS MALIBU CA pie 20/6 INFRARED FIBER OPTICS.(U) DEC 79 J A HARRINSTON, R TURK, M HENDERSON F1962-R78-C-0109...Laboratories AE.WR r z7 3011 Malibu Canyon Road t 2 Hanscom AFB MA 01731 E I NUBROPAS I5s. OECLASSIFI ATION/DOWNGRADING SN/ A SCHEDULE 16. DISTRI13UTION

  20. Optical fiber metamagnetics.

    PubMed

    Wang, Xi; Venugopal, Gayatri; Zeng, Jinwei; Chen, Yinnan; Lee, Dong Ho; Litchinitser, Natalia M; Cartwright, Alexander N

    2011-10-10

    To date, magnetic and negative-index metamaterials at optical frequencies were realized on bulk substrates in the form of thin films with thicknesses on the order of, or less than, optical wavelengths. In this work, we design and experimentally demonstrate, for the first time, fiber-coupled magnetic metamaterials integrated on the transverse cross-section of an optical fiber. Such fiber-metamaterials integration may provide fundamentally new solutions for photonic-on-a-chip systems for sensing, subwavelength imaging, image processing, and biomedical applications.

  1. QUARTZ FIBER ELECTROSCOPES

    DOEpatents

    Henderson, R.P.

    1957-09-17

    An instrument carried unobtrusively about the person such as in a finger ring to indicate when that person has been exposed to an unusual radiation hazard is described. A metallized quartz fiber is electrically charged to indicate a full scale reading on an etched glass background. The quartz fiber and the scale may be viewed through a magnifying lens for ease of reading. Incident radiation will ionize gaseous particles in the sealed structure thereby allowing the charge to leak off the quartz fiber with its resulting movement across the scale proportionally indicating the radiation exposure.

  2. Optical fiber phase discriminator.

    PubMed

    Danielson, B L

    1978-11-15

    Phase discriminators are devices widely used at rf and microwave frequencies to convert phase, or frequency, changes to amplitude changes. They find widespread use in generating audio feedback signals for frequency stabilization of oscillators and in angle demodulation applications. This paper demonstrates that similar devices, with similar functions, can be constructed in the visible region using optical fibers as delay-line elements. The operating principles of an optical-fiber delay-line phase discriminator are discussed. The sensitivity is shown to be proportional to the fiber propagation-delay time. A device working at 0.6328 microm is described and compared with predictions.

  3. Photochromic glass optical fiber

    NASA Astrophysics Data System (ADS)

    Alvi, Bilal A.; Israr, Amber; Asif, Muhammad; Aamir, Muhammad; Rehan, Muhammad

    2016-02-01

    This paper describes the fabrication and analysis of novel twin cored fiber which contains a transparent and silver halide doped photochromic core in same cladding. The Photochromic core fibers were fabricated in twin cored structure by rode and tube method. The diameter of photochromic core and transparent core is around 15 m. The distance between two cores is 1.5m. The transparent core was used to guide the probe beam and photochromic core was excited by UV source. The interaction of the probe beam with the excited photochromic core showed the photochromic behavior of the fiber.

  4. Nanotailored Carbon Fibers

    DTIC Science & Technology

    2009-06-07

    Chae, Han Gi, Ph.D. Nano Engineered Materials Corporation 2349 Lake Forest Trail Lawrenceville, GA 30043 Air Force Office of Scientific...0065, AF08‐T028  Nanotailored Carbon Fibers  Nano  Engineered Materials Corp    Nanotailored Carbon Fibers (STTR Phase I final technical report...14   FA9550‐08‐C‐0065, AF08‐T028  Nanotailored Carbon Fibers  Nano

  5. Analysis of Volatile Components of Cape Gooseberry (Physalis peruviana L.) Grown in Turkey by HS-SPME and GC-MS

    PubMed Central

    2014-01-01

    Volatile components in cape gooseberry fruit at ripe stage were collected using headspace-solid phase microextraction, and analyzed by gas chromatography-mass spectrometry. Three solid phase microextraction fiber coatings (DVB/CAR/PDMS, CAR/PDMS, and PDMS/DVB) were tested for evaluation of volatile compounds. DVB/CAR/PDMS fiber showed a strong extraction capacity for volatile compounds and produced the best result in case of total peak areas. A total of 133 volatile compounds were identified in fruit pulp; among them 1-hexanol (6.86%), eucalyptol (6.66%), ethyl butanoate (6.47%), ethyl octanoate (4.01%), ethyl decanoate (3.39%), 4-terpineol (3.27%), and 2-methyl-1-butanol (3.10%) were the major components in the sample extracts. PMID:24741358

  6. Fabrication of ciprofloxacin molecular imprinted polymer coating on a stainless steel wire as a selective solid-phase microextraction fiber for sensitive determination of fluoroquinolones in biological fluids and tablet formulation using HPLC-UV detection.

    PubMed

    Mirzajani, Roya; Kardani, Fatemeh

    2016-04-15

    A molecularly imprinted polymer (MIP) fiber on stainless steel wire using ciprofloxacin template with a mild template removal condition was synthetized and evaluated for fiber solid phase microextraction (SPME) of fluoroquinolones (FQs) from biological fluids and pharmaceutical samples, followed by high performance liquid chromatography analysis with UV detection (HPLC-UV). The developed MIP fiber exhibited high selectivity for the analytes in complex matrices. The coating of the fibers were inspected using fourier transform infrared spectrophotometry, thermogaravimetric analysis, energy dispersive X-ray (EDX) spectroscopy as well as by scanning electron microscopy (SEM). The fiber shows high thermal stability (up to 300°C), good reproducibility and long lifetime. The composite coating did not swell in organic solvents nor did it strip off from the substrate. It was also highly stable and extremely adherent to the surface of the stainless steel fiber. The fabricated fiber exclusively exhibited excellent extraction efficiency and selectivity for some FQs. The effective parameters influencing the microextraction efficiency such as pH, extraction time, desorption condition, and stirring rate were investigated. Under optimized conditions, the limits of detection of the four FQs ranged from 0.023-0.033 μg L(-1) (S/N=5) and the calibration graphs were linear in the concentration range from 0.1-40 μg L(-1), the inter-day and intraday relative standard deviations (RSD) for various FQs at three different concentration level (n=5) using a single fiber were 1.1-4.4% and the fiber to fiber RSD% (n=5) was 4.3-6.7% at 5 μg L(-1) of each anlyetes. The method was successfully applied for quantification of FQs in real samples including serum, plasma and tablet formulation with the recoveries between 97 to 102%.

  7. Reduced Gravity Zblan Optical Fiber

    NASA Technical Reports Server (NTRS)

    Tucker, Dennis S.; Workman, Gary L.; Smith, Guy A.

    2000-01-01

    Two optical fiber pullers have been designed for pulling ZBLAN optical fiber in reduced gravity. One fiber puller was designed, built and flown on board NASA's KC135 reduced gravity aircraft. A second fiber puller has been designed for use on board the International Space Station.

  8. Muscle Fiber Types and Training.

    ERIC Educational Resources Information Center

    Karp, Jason R.

    2001-01-01

    The specific types of fibers that make up individual muscles greatly influence how people will adapt to their training programs. This paper explains the complexities of skeletal muscles, focusing on types of muscle fibers (slow-twitch and fast-twitch), recruitment of muscle fibers to perform a motor task, and determining fiber type. Implications…

  9. Carbon Fiber Risk Analysis. [conference

    NASA Technical Reports Server (NTRS)

    1979-01-01

    The scope and status of the effort to assess the risks associated with the accidental release of carbon/graphite fibers from civil aircraft is presented. Vulnerability of electrical and electronic equipment to carbon fibers, dispersal of carbon fibers, effectiveness of filtering systems, impact of fiber induced failures, and risk methodology are among the topics covered.

  10. Fiber optics: A research paper

    NASA Technical Reports Server (NTRS)

    Drone, Melinda M.

    1987-01-01

    Some basic aspects concerning fiber optics are examined. Some history leading up to the development of optical fibers which are now used in the transmission of data in many areas of the world is discussed. Basic theory of the operation of fiber optics is discussed along with methods for improving performance of the optical fiber through much research and design. Splices and connectors are compared and short haul and long haul fiber optic networks are discussed. Fiber optics plays many roles in the commercial world. The use of fiber optics for communication applications is emphasized.

  11. Fiber optics: A research paper

    NASA Astrophysics Data System (ADS)

    Drone, Melinda M.

    1987-08-01

    Some basic aspects concerning fiber optics are examined. Some history leading up to the development of optical fibers which are now used in the transmission of data in many areas of the world is discussed. Basic theory of the operation of fiber optics is discussed along with methods for improving performance of the optical fiber through much research and design. Splices and connectors are compared and short haul and long haul fiber optic networks are discussed. Fiber optics plays many roles in the commercial world. The use of fiber optics for communication applications is emphasized.

  12. Fiber bundle phase conjugate mirror

    DOEpatents

    Ward, Benjamin G.

    2012-05-01

    An improved method and apparatus for passively conjugating the phases of a distorted wavefronts resulting from optical phase mismatch between elements of a fiber laser array are disclosed. A method for passively conjugating a distorted wavefront comprises the steps of: multiplexing a plurality of probe fibers and a bundle pump fiber in a fiber bundle array; passing the multiplexed output from the fiber bundle array through a collimating lens and into one portion of a non-linear medium; passing the output from a pump collection fiber through a focusing lens and into another portion of the non-linear medium so that the output from the pump collection fiber mixes with the multiplexed output from the fiber bundle; adjusting one or more degrees of freedom of one or more of the fiber bundle array, the collimating lens, the focusing lens, the non-linear medium, or the pump collection fiber to produce a standing wave in the non-linear medium.

  13. High-fiber foods

    MedlinePlus

    ... potatoes with skin Broccoli, artichokes, squashes, and string beans You can also get more fiber by eating: Legumes, such as lentils, black beans, split peas, kidney beans, lima beans, and chickpeas ...

  14. Fiber Optics: No Illusion.

    ERIC Educational Resources Information Center

    American School and University, 1983

    1983-01-01

    A campus computer center at Hofstra University (New York) that holds 70 terminals for student use was first a gymnasium, then a language laboratory. Strands of fiber optics are used for the necessary wiring. (MLF)

  15. Cerenkov fiber sampling calorimeters

    SciTech Connect

    Arrington, K.; Kefford, D.; Kennedy, J.; Pisani, R.; Sanzeni, C.; Segall, K.; Wall, D.; Winn, D.R. ); Carey, R.; Dye, S.; Miller, J.; Sulak, L.; Worstell, W. ); Efremenko, Y.; Kamyshkov, Y.; Savin, A.; Shmakov, K.; Tarkovsky, E. )

    1994-08-01

    Clear optical fibers were used as a Cerenkov sampling media in Pb (electromagnetic) and Cu (hadron) absorbers in spaghetti calorimeters, for high rate and high radiation dose experiments, such as the forward region of high energy colliders. The fiber axes were aligned close to the direction of the incident particles (1[degree]--7[degree]). The 7 [lambda] deep hadron tower contained 2.8% by volume 1.5 mm diameter core clear plastic fibers. The 27 radiation length deep electromagnetic towers had packing fractions of 6.8% and 7.2% of 1 mm diameter core quartz fibers as the active Cerenkov sampling medium. The energy resolution on electrons and pions, energy response, pulse shapes and angular studies are presented.

  16. Fiber-Scanned Microdisplays

    NASA Technical Reports Server (NTRS)

    Crossman-Bosworth, Janet; Seibel, Eric

    2010-01-01

    Helmet- and head-mounted display systems, denoted fiber-scanned microdisplays, have been proposed to provide information in an "augmented reality" format (meaning that the information would be optically overlaid on the user's field of view).

  17. Fiber and Your Child

    MedlinePlus

    ... fiber sources are: whole-grain breads and cereals apples oranges bananas berries prunes pears green peas legumes ( ... grams) of almonds (3.5 grams) 1 small apple with skin (3.6 grams) ¼ cup (59 ...

  18. Simulating Optical Fibers.

    ERIC Educational Resources Information Center

    Edgar, Dale

    1988-01-01

    Described is a demonstration of Snell's law using a laser beam and an optical fiber. Provided are the set-up method of the demonstration apparatus and some practical suggestions including "index matching" technique using vaseline. (YP)

  19. Fiber optic gas sensor

    NASA Technical Reports Server (NTRS)

    Chen, Peng (Inventor); Buric, Michael P. (Inventor); Swinehart, Philip R. (Inventor); Maklad, Mokhtar S. (Inventor)

    2010-01-01

    A gas sensor includes an in-fiber resonant wavelength device provided in a fiber core at a first location. The fiber propagates a sensing light and a power light. A layer of a material is attached to the fiber at the first location. The material is able to absorb the gas at a temperature dependent gas absorption rate. The power light is used to heat the material and increases the gas absorption rate, thereby increasing sensor performance, especially at low temperatures. Further, a method is described of flash heating the gas sensor to absorb more of the gas, allowing the sensor to cool, thereby locking in the gas content of the sensor material, and taking the difference between the starting and ending resonant wavelengths as an indication of the concentration of the gas in the ambient atmosphere.

  20. Hollow-Fiber Clinostat

    NASA Technical Reports Server (NTRS)

    Rhodes, Percy H.; Miller, Teresa Y.; Snyder, Robert S.

    1990-01-01

    Hollow-fiber clinostat, is bioreactor used to study growth and other behavior of cells in simulated microgravity. Cells under study contained in porous hollow fiber immersed in culture medium inside vessel. Bores in hollow fiber allow exchange of gases, nutrients, and metabolic waste products between living cells and external culture media. Hollow fiber lies on axis of vessel, rotated by motor equipped with torque and speed controls. Desired temperature maintained by operating clinostat in standard tissue-culture incubator. Axis of rotation made horizontal or vertical. Designed for use with conventional methods of sterilization and sanitation to prevent contamination of specimen. Also designed for asepsis in assembly, injection of specimen, and exchange of medium.

  1. Fiber alignment apparatus and method

    DOEpatents

    Kravitz, S.H.; Warren, M.E.; Snipes, M.B. Jr.; Armendariz, M.G.; Word, J.C. V

    1997-08-19

    A fiber alignment apparatus includes a micro-machined nickel spring that captures and locks arrays of single mode fibers into position. The design consists of a movable nickel leaf shaped spring and a fixed pocket where fibers are held. The fiber is slid between the spring and a fixed block, which tensions the spring. When the fiber reaches the pocket, it automatically falls into the pocket and is held by the pressure of the leaf spring. 8 figs.

  2. Fiber alignment apparatus and method

    DOEpatents

    Kravitz, Stanley H.; Warren, Mial Evans; Snipes, Jr., Morris Burton; Armendariz, Marcelino Guadalupe; Word, V., James Cole

    1997-01-01

    A fiber alignment apparatus includes a micro-machined nickel spring that captures and locks arrays of single mode fibers into position. The design consists of a movable nickel leaf shaped spring and a fixed pocket where fibers are held. The fiber is slid between the spring and a fixed block, which tensions the spring. When the fiber reaches the pocket, it automatically falls into the pocket and is held by the pressure of the leaf spring.

  3. Fiber optics welder

    DOEpatents

    Higgins, R.W.; Robichaud, R.E.

    A system is described for welding fiber optic waveguides together. The ends of the two fibers to be joined together are accurately, collinearly aligned in a vertical orientation and subjected to a controlled, diffuse arc to effect welding and thermal conditioning. A front-surfaced mirror mounted at a 45/sup 0/ angle to the optical axis of a stereomicroscope mounted for viewing the junction of the ends provides two orthogonal views of the interface during the alignment operation.

  4. Infrared fiber optic materials

    NASA Technical Reports Server (NTRS)

    Feigelson, Robert S.

    1987-01-01

    The development of IR fiber optics for use in astronomical and other space applications is summarized. Candidate materials were sought for use in the 1 to 200 micron and the 200 to 1000 micron wavelength range. Synthesis and optical characterization were carried out on several of these materials in bulk form. And the fabrication of a few materials in single crystal fiber optic form were studied.

  5. Fiber optic detector

    NASA Astrophysics Data System (ADS)

    Partin, Judy K.; Ward, Thomas E.; Grey, Alan E.

    1990-04-01

    This invention is comprised of a portable fiber optic detector that senses the presence of specific target chemicals by exchanging the target chemical for a fluorescently-tagged antigen that is bound to an antibody which is in turn attached to an optical fiber. Replacing the fluorescently-tagged antigen reduces the fluorescence so that a photon sensing detector records the reduced light level and activates an appropriate alarm or indicator.

  6. Fiber optic detector

    SciTech Connect

    Partin, J.K.; Ward, T.E.; Grey, A.E.

    1990-12-31

    This invention is comprised of a portable fiber optic detector that senses the presence of specific target chemicals by exchanging the target chemical for a fluorescently-tagged antigen that is bound to an antibody which is in turn attached to an optical fiber. Replacing the fluorescently-tagged antigen reduces the fluorescence so that a photon sensing detector records the reduced light level and activates an appropriate alarm or indicator.

  7. Production of mullite fibers

    NASA Technical Reports Server (NTRS)

    Tucker, Dennis S. (Inventor); Sparks, J. Scott (Inventor)

    1991-01-01

    Disclosed here is a process for making mullite fibers wherein a hydrolizable silicon compound and an aluminum compound in the form of a difunctional aluminum chelate are hydrolized to form sols using water and an alcohol with a catalytic amount of hydrochloric acid. The sols are mixed in a molar ratio of aluminum to silicon of 3 to 1 and, under polycondensation conditions, a fibrous gel is formed. From this gel the mullite fibers can be produced.

  8. Determination of organophosphorus pesticides in ecological textiles by solid-phase microextraction with a siloxane-modified polyurethane acrylic resin fiber.

    PubMed

    Hu, Xianlei; Zhang, Mingqiu; Ruan, Wenhong; Zhu, Fang; Ouyang, Gangfeng

    2012-07-29

    A novel solid-phase microextraction (SPME) fiber coating was prepared with siloxane-modified polyurethane acrylic resin by photo-cured technology. The ratio of two monomers was investigated to obtain good microphase separation structure and better extraction performance. The self-made fiber was then applied to organophosphorus pesticides (OPPs) analysis and several factors, such as extraction/desorption time, extraction temperature, salinity, and pH, were studied. The optimized conditions were: 15 min extraction at 25 °C, 5% Na(2)SO(4) content, pH 7.0 and 4 min desorption in GC inlet. The self-made fiber coating exhibited better extraction efficiency for OPPs, compared with three commercial fiber coatings. Under the optimized conditions, the detection limits of 11 OPPs were from 0.03 μg L(-1) to 0.5 μg L(-1). Good recoveries and repeatabilities were obtained when the method was used to determine OPPs in ecological textile.

  9. Fiber optics for controls

    NASA Technical Reports Server (NTRS)

    Seng, Gary T.

    1987-01-01

    The challenge of those involved in control-system hardware development is to accommodate an ever-increasing complexity in aircraft control, while limiting the size and weight of the components and improving system reliability. A technology that displays promise towards this end is the area of fiber optics for controls. The primary advantages of employing optical fibers, passive optical sensors, and optically controlled actuators are weight and volume reduction, immunity from electromagnetic effects, superior bandwidth capabilities, and freedom from short circuits and sparking contacts. Since 1975, NASA Lewis has performed in-house, contract, and grant research in fiber optic sensors, high-temperature electro-optic switches, and fly-by-light control-system architecture. Passive optical sensor development is an essential yet challenging area of work and has therefore received much attention during this period. A major effort to develop fly-by-light control-system technology, known as the Fiber-Optic Control System Integration (FOCSI) program, was initiated in 1985 as a cooperative effort between NASA and DOD. Phase 1 of FOCSI, completed in 1986, was aimed at the design of a fiber-optic integrated propulsion/flight control system. Phase 2, yet to be initiated, will provide subcomponent and system development, and a system engine test. In addition to a summary of the benefits of fiber optics, the FOCSI program, sensor advances, and future directions in the NASA Lewis program will be discussed.

  10. Electrospun Amplified Fiber Optics

    PubMed Central

    2015-01-01

    All-optical signal processing is the focus of much research aiming to obtain effective alternatives to existing data transmission platforms. Amplification of light in fiber optics, such as in Erbium-doped fiber amplifiers, is especially important for efficient signal transmission. However, the complex fabrication methods involving high-temperature processes performed in a highly pure environment slow the fabrication process and make amplified components expensive with respect to an ideal, high-throughput, room temperature production. Here, we report on near-infrared polymer fiber amplifiers working over a band of ∼20 nm. The fibers are cheap, spun with a process entirely carried out at room temperature, and shown to have amplified spontaneous emission with good gain coefficients and low levels of optical losses (a few cm–1). The amplification process is favored by high fiber quality and low self-absorption. The found performance metrics appear to be suitable for short-distance operations, and the large variety of commercially available doping dyes might allow for effective multiwavelength operations by electrospun amplified fiber optics. PMID:25710188

  11. Electrospun amplified fiber optics.

    PubMed

    Morello, Giovanni; Camposeo, Andrea; Moffa, Maria; Pisignano, Dario

    2015-03-11

    All-optical signal processing is the focus of much research aiming to obtain effective alternatives to existing data transmission platforms. Amplification of light in fiber optics, such as in Erbium-doped fiber amplifiers, is especially important for efficient signal transmission. However, the complex fabrication methods involving high-temperature processes performed in a highly pure environment slow the fabrication process and make amplified components expensive with respect to an ideal, high-throughput, room temperature production. Here, we report on near-infrared polymer fiber amplifiers working over a band of ∼20 nm. The fibers are cheap, spun with a process entirely carried out at room temperature, and shown to have amplified spontaneous emission with good gain coefficients and low levels of optical losses (a few cm(-1)). The amplification process is favored by high fiber quality and low self-absorption. The found performance metrics appear to be suitable for short-distance operations, and the large variety of commercially available doping dyes might allow for effective multiwavelength operations by electrospun amplified fiber optics.

  12. Cladded single crystal fibers for high power fiber lasers

    NASA Astrophysics Data System (ADS)

    Kim, W.; Shaw, B.; Bayya, S.; Askins, C.; Peele, J.; Rhonehouse, D.; Meyers, J.; Thapa, R.; Gibson, D.; Sanghera, J.

    2016-09-01

    We report on the recent progress in the development of cladded single crystal fibers for high power single frequency lasers. Various rare earth doped single crystal YAG fibers with diameters down to 17 μm with length > 1 m have been successfully drawn using a state-of-the-art Laser Heated Pedestal Growth system. Single and double cladding on rare earth doped YAG fibers have been developed using glasses where optical and physical properties were precisely matched to doped YAG core single crystal fiber. The double clad Yb:YAG fiber structures have dimensions analogous to large mode area (LMA) silica fiber. We also report successful fabrications of all crystalline core/clad fibers where thermal and optical properties are superior over glass cladded YAG fibers. Various fabrication methods, optical characterization and gain measurements on these cladded YAG fibers are reported.

  13. Fiber-matrix interfacial adhesion in natural fiber composites

    NASA Astrophysics Data System (ADS)

    Tran, L. Q. N.; Yuan, X. W.; Bhattacharyya, D.; Fuentes, C.; van Vuure, A. W.; Verpoest, I.

    2015-04-01

    The interface between natural fibers and thermoplastic matrices is studied, in which fiber-matrix wetting analysis and interfacial adhesion are investigated to obtain a systematic understanding of the interface. In wetting analysis, the surface energies of the fibers and the matrices are estimated using their contact angles in test liquids. Work of adhesion is calculated for each composite system. For the interface tests, transverse three point bending tests (3PBT) on unidirectional (UD) composites are performed to measure interfacial strength. X-ray photoelectron spectroscopy (XPS) characterization on the fibers is also carried out to obtain more information about the surface chemistry of the fibers. UD composites are examined to explore the correlation between the fiber-matrix interface and the final properties of the composites. The results suggest that the higher interfacial adhesion of the treated fiber composites compared to untreated fiber composites can be attributed to higher fiber-matrix physico-chemical interaction corresponding with the work of adhesion.

  14. Evaluation of the flexural strength of carbon fiber-, quartz fiber-, and glass fiber-based posts.

    PubMed

    Galhano, Graziela Avila; Valandro, Luiz Felipe; de Melo, Renata Marques; Scotti, Roberto; Bottino, Marco Antonio

    2005-03-01

    This study investigated the flexural strength of eight fiber posts (one carbon fiber, one carbon/quartz fiber, one opaque quartz fiber, two translucent quartz fiber, and three glass fiber posts). Eighty fiber posts were used and divided into eight groups (n = 10): G1: C-POST (Bisco); G2: AESTHETI-POST (Bisco); G3: AESTHETI-PLUS (Bisco); G4: LIGHT-POST (Bisco); G5: D.T. LIGHT-POST (Bisco); G6: PARAPOST WHITE (Coltene); G7: FIBERKOR (Pentron); G8: REFORPOST (Angelus). All of the samples were tested using the three-point bending test. The averages obtained were submitted to the ANOVA and to Tukey's test (p < 0.05). The mean values (MPa) of the groups AESTHETI-POST-carbon/quartz fiber post (Bisco) and AESTHETI-PLUS-quartz fiber post (Bisco) were statistically similar and higher than the mean values of the other groups. The mean values of the groups C-POST-carbon fiber post (Bisco), LIGHT-POST-translucent quartz fiber post (Bisco), D.T. LIGHT-POST-double tapered translucent quartz fiber post (Bisco), PARAPOST WHITE-glass fiber post (Coltene) and FIBREKOR--glass fiber post (Pentron) were similar and higher than the group REFORPOST-glass fiber post (Angelus).

  15. The optimal fiber volume fraction and fiber-matrix property compatibility in fiber reinforced composites

    NASA Technical Reports Server (NTRS)

    Pan, Ning

    1992-01-01

    Although the question of minimum or critical fiber volume fraction beyond which a composite can then be strengthened due to addition of fibers has been dealt with by several investigators for both continuous and short fiber composites, a study of maximum or optimal fiber volume fraction at which the composite reaches its highest strength has not been reported yet. The present analysis has investigated this issue for short fiber case based on the well-known shear lag (the elastic stress transfer) theory as the first step. Using the relationships obtained, the minimum spacing between fibers is determined upon which the maximum fiber volume fraction can be calculated, depending on the fiber packing forms within the composites. The effects on the value of this maximum fiber volume fraction due to such factors as fiber and matrix properties, fiber aspect ratio and fiber packing forms are discussed. Furthermore, combined with the previous analysis on the minimum fiber volume fraction, this maximum fiber volume fraction can be used to examine the property compatibility of fiber and matrix in forming a composite. This is deemed to be useful for composite design. Finally some examples are provided to illustrate the results.

  16. Electrospun cross linked rosin fibers

    NASA Astrophysics Data System (ADS)

    Baek, Woo-il; Nirmala, R.; Barakat, Nasser A. M.; El-Newehy, Mohamed H.; Al-Deyab, Salem S.; Kim, Hak Yong

    2011-12-01

    In this study, we describe the first reported preparation of rosin in fiber form through use of an electrospinning technique utilizing various solvent systems. The polymer concentration of the formed fiber was studied by using various solvents such as chloroform, ethanol, N-N dimethylformamide (DMF), tetrahydrofuran (THF), acetone, and methylene chloride (MC). An electrospray of the solution resulted in the beaded form of the rosin. By varying the polymer concentration with MC, we were then able to obtain uniform fibers. However, the fibers exhibited large diameter. We believe that it is possible to reduce the diameter of the rosin fibers through appropriate selection of electrospinning parameters. In addition, the morphological transitions from beads, to beaded fiber, to fiber were studied at different polymer concentrations. We propose a possible physical cross linking mechanism for the formation of rosin fibers during the electrospinning process. Our results demonstrate the feasibility of producing fiber nanostructures of rosin by using an electrospinning technique.

  17. Toward high performance graphene fibers.

    PubMed

    Chen, Li; He, Yuling; Chai, Songgang; Qiang, Hong; Chen, Feng; Fu, Qiang

    2013-07-07

    Two-dimensional graphene and graphene-based materials have attracted tremendous interest, hence much attention has been drawn to exploring and applying their exceptional characteristics and properties. Integration of graphene sheets into macroscopic fibers is a very important way for their application and has received increasing interest. In this study, neat and macroscopic graphene fibers were continuously spun from graphene oxide (GO) suspensions followed by chemical reduction. By varying wet-spinning conditions, a series of graphene fibers were prepared, then, the structural features, mechanical and electrical performances of the fibers were investigated. We found the orientation of graphene sheets, the interaction between inter-fiber graphene sheets and the defects in the fibers have a pronounced effect on the properties of the fibers. Graphene fibers with excellent mechanical and electrical properties will yield great advances in high-tech applications. These findings provide guidance for the future production of high performance graphene fibers.

  18. Optical fiber stripper positioning apparatus

    DOEpatents

    Fyfe, Richard W.; Sanchez, Jr., Amadeo

    1990-01-01

    An optical fiber positioning apparatus for an optical fiber stripping device is disclosed which is capable of providing precise axial alignment between an optical fiber to be stripped of its outer jacket and the cutting blades of a stripping device. The apparatus includes a first bore having a width approximately equal to the diameter of an unstripped optical fiber and a counter bore axially aligned with the first bore and dimensioned to precisely receive a portion of the stripping device in axial alignment with notched cutting blades within the stripping device to thereby axially align the notched cutting blades of the stripping device with the axis of the optical fiber to permit the notched cutting blades to sever the jacket on the optical fiber without damaging the cladding on the optical fiber. In a preferred embodiment, the apparatus further includes a fiber stop which permits determination of the length of jacket to be removed from the optical fiber.

  19. Effects of fiber manipulation methods on optical fiber properties

    NASA Astrophysics Data System (ADS)

    Reynolds, Robert O.; Bechter, Andrew; Crass, Jonathan

    2016-07-01

    Optical fibers are routinely used to couple high-resolution spectrographs to modern telescopes, enabling important advantages in areas such as the search for extrasolar planets using spectroscopic radial velocity measurements of candidate stars. Optical fibers partially scramble the input illumination, and this feature enables a fiber feed to provide more uniform illumination to the spectrograph optics, thereby reducing systematic errors in radial velocity measurements. However fibers suffer from focal ratio degradation (FRD), a spreading of the beam at the output of the fiber with respect to that at the fiber input, which results in losses in throughput and resolution. Modal noise, a measurement uncertainty caused by inherent fiber properties and evident as a varying spatial intensity at the fiber exit plane, reduces the signal to noise ratio in the data. Devices such as double scramblers are often used to improve scrambling, and better fiber end preparation can mitigate FRD. Many instruments agitate the fiber during an observation to reduce modal noise, and stretching the fiber during use has been shown to offer a greater reduction in that noise. But effects of agitation and stretching on fiber parameters such as total transmission and focal ratio degradation have not been adequately studied. In this paper we present measurements of transmission loss and focal ratio degradation for both agitated and stretched fibers.

  20. Fiber-optic technology review

    SciTech Connect

    Lyons, P.B.

    1980-01-01

    A history of fiber technology is presented. The advantages of fiber optics are discussed (bandwidth, cost, weight and size, nonmetallic construction and isolation). Some aspects of the disadvantages of fiber systems briefly discussed are fiber and cable availability, fiber components, radiation effects, receivers and transmitters, and material dispersion. Particular emphasis over the next several years will involve development of fibers and systems optimized for use at wavelengths near 1.3 ..mu..m and development of wavelengths multiplexers for simultaneous system operation at several wavelengths.

  1. Enhanced radiation resistant fiber optics

    DOEpatents

    Lyons, Peter B.; Looney, Larry D.

    1993-01-01

    A process for producing an optical fiber having enhanced radiation resitance is provided, the process including maintaining an optical fiber within a hydrogen-containing atmosphere for sufficient time to yield a hydrogen-permeated optical fiber having an elevated internal hydrogen concentration, and irradiating the hydrogen-permeated optical fiber at a time while the optical fiber has an elevated internal hydrogen concentration with a source of ionizing radiation. The radiation source is typically a cobalt-60 source and the fiber is pre-irradiated with a dose level up to about 1000 kilorads of radiation.

  2. Enhanced radiation resistant fiber optics

    DOEpatents

    Lyons, P.B.; Looney, L.D.

    1993-11-30

    A process for producing an optical fiber having enhanced radiation resistance is provided, the process including maintaining an optical fiber within a hydrogen-containing atmosphere for sufficient time to yield a hydrogen-permeated optical fiber having an elevated internal hydrogen concentration, and irradiating the hydrogen-permeated optical fiber at a time while the optical fiber has an elevated internal hydrogen concentration with a source of ionizing radiation. The radiation source is typically a cobalt-60 source and the fiber is pre-irradiated with a dose level up to about 1000 kilorads of radiation. 4 figures.

  3. Natural Fiber Composites: A Review

    SciTech Connect

    Westman, Matthew P.; Fifield, Leonard S.; Simmons, Kevin L.; Laddha, Sachin; Kafentzis, Tyler A.

    2010-03-07

    The need for renewable fiber reinforced composites has never been as prevalent as it currently is. Natural fibers offer both cost savings and a reduction in density when compared to glass fibers. Though the strength of natural fibers is not as great as glass, the specific properties are comparable. Currently natural fiber composites have two issues that need to be addressed: resin compatibility and water absorption. The following preliminary research has investigated the use of Kenaf, Hibiscus cannabinus, as a possible glass replacement in fiber reinforced composites.

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

    PubMed

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

    2016-03-24

    In the present study, a molecularly imprinted solid-phase microextraction fiber (MIP-SPMEf) 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 (Qmax) was determined by Langmuir- Freundlich model and was 149 mg/g for MIP-SPMEf. 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.

  5. Rapid analysis of amphetamine, methamphetamine, MDA, and MDMA in urine using solid-phase microextraction, direct on-fiber derivatization, and analysis by GC-MS.

    PubMed

    Jurado, C; Giménez, M P; Soriano, T; Menéndez, M; Repetto, M

    2000-01-01

    A rapid, sensitive, and solvent-free procedure for the simultaneous determination of amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine (MDA), and 3,4-methylenedioxymethamphetamine (MDMA) in urine was developed using solid-phase microextraction (SPME) and gas chromatography-mass spectrometry (GC-MS) in the selected ion monitoring mode. A headspace vial containing the urine sample, NaOH, NaCl, and amphetamine-d3 as the internal standard was heated at 100 degrees C for 20 min. A polydimethylsiloxane fiber was maintained in the vial headspace for 10 min in order to adsorb the amphetaminic compounds, which were subsequently derivatized by exposing the fiber to trifluoroacetic anhydride for 20 min in the headspace of another vial maintained at 60 degrees C for 20 min. The trifluoroacetyl derivatives were desorbed in the GC injection port for 5 min. Several parameters were considered during the method optimization process. These included a comparison of SPME with or without headspace, the required derivatization procedure, and the influence of temperature on the headspace extraction and derivatization methods. The optimized method was validated for the four compounds tested. Calibration curves showed linearity in the range 50-1000 ng/mL (r = 0.9946-0.9999). Recovery data were 71.89-103.24%. The quantitation limits were 10 ng/mL for amphetamine and methamphetamine and 20 ng/mL for MDA and MDMA. All of these data recommend the applicability of the method for use in the analytical routine of a forensic laboratory.

  6. Full automation of solid-phase microextraction/on-fiber derivatization for simultaneous determination of endocrine-disrupting chemicals and steroid hormones by gas chromatography-mass spectrometry.

    PubMed

    Yang, Lihua; Lan, Chongyu; Liu, Hongtao; Dong, Jun; Luan, Tiangang

    2006-09-01

    A fully automated method using direct immersion solid-phase microextraction (DI-SPME) and headspace on-fiber silylation for simultaneous determinations of exogenous endocrine-disrupting chemicals (EDCs) and endogenous steroid hormones in environmental aqueous and biological samples by gas chromatography-mass spectrometry (GC-MS) was developed and compared to a previously reported manual method. Three EDCs and five endocrine steroid hormones were selected to evaluate this method. The extraction and derivatization time, ion strength, pH, incubation temperature, sample volume, and extraction solvent were optimized. Satisfactory results in pure water were obtained in terms of linearity of calibration curve (R2=0.9932-1.0000), dynamic range (3 orders of magnitude), precision (4-9% RSD), as well as LOD (0.001-0.124 microg L(-1)) and LOQ (0.004-0.413 microg L(-1)), respectively. These results were similar to those obtained using a manual method, and moreover, the precision was improved. This new automated method has been applied to the determinations of target compounds in real samples used in our previous study on a manual SPME method. Exogenous octylphenol (OP), technical grade nonylphenol (t-NP), and diethylstilbestrol (DES) were at 0.13, 5.03, and 0.02 microg L(-1) in river water and 3.76, 13.25, and 0.10 microg L(-1) in fish serum, respectively. Natural steroid hormones estrone (E1), 17beta-estradiol (E2), and testosterone (T) were at 0.19, 0.11, and 6.22 microg L(-1) in river water; and in female fish serum E1, E2, and pregnenolone (PREG) were at 1.37, 1.95, and 6.25 microg L(-1), respectively. These results were confirmed by the manual method. The developed fully automated SPME and on-fiber silylation procedures showed satisfactory applications in environmental analysis and the performances show improved precision and a reduced analysis time compared to the manual method.

  7. Continuous fiber thermoplastic prepreg

    NASA Technical Reports Server (NTRS)

    Wilson, Maywood L. (Inventor); Johnson, Gary S. (Inventor)

    1993-01-01

    A pultrusion machine employing a corrugated impregnator vessel to immerse multiple, continuous strand, fiber tow in an impregnating material, and an adjustable metered exit orifice for the impregnator vessel to control the quantity of impregnating material retained by the impregnated fibers, is provided. An adjustable height insert retains transverse rod elements within each depression of the corrugated vessel to maintain the individual fiber tows spread and in contact with the vessel bottom. A series of elongated heating dies, transversely disposed on the pultrusion machine and having flat heating surfaces with radiused edges, ensure adequate temperature exposed dwell time and exert adequate pressure on the impregnated fiber tows, to provide the desired thickness and fiber/resin ratio in the prepreg formed. The prepreg passing through the pulling mechanism is wound on a suitable take-up spool for subsequent use. A formula is derived for determining the cross sectional area opening of the metering device. A modification in the heating die system employs a heated nip roller in lieu of one of the pressure applying flat dies.

  8. In situ hydrothermal growth of ZnO/g-C3N4 nanoflowers coated solid-phase microextraction fibers coupled with GC-MS for determination of pesticides residues.

    PubMed

    Zhang, Ning; Gao, Jia; Huang, Chuanhui; Liu, Wei; Tong, Ping; Zhang, Lan

    2016-08-31

    In this paper, Zinc oxide (ZnO) hybridized with graphite-like C3N4 (ZnO/g-C3N4) nanoflowers based solid phase microextraction (SPME) coating was prepared on fiber using in situ hydrothermal growth method for gas chromatographic -mass spectrum (GC- MS) separation and analysis target analytes in complex matrixes for the first time. The proposed hybrid ZnO/g-C3N4 fiber exhibited wide linearity for the pesticide residues in range of 0.003-5.0 ng mL(-1). The limits of detection (LOD) were 0.001-0.0025 ng mL(-1). The relative standard deviation (RSD) for three replicate extractions using one fiber was ranged from 2.3% to 7.6%. The fiber to fiber RSD was 5.3-11.3% (n = 3). This method was successfully used for simultaneous determination of nine pesticide residues in cucumber, pear, Green tea and Minjiang water with satisfactory recoveries of 79.1-103.5%. These results indicated that the ZnO/g-C3N4 composite provided a promising alternative in sample pretreatment and analysis.

  9. Determination of 1-chloro-4-[2,2,2-trichloro-1-(4-chlorophenyl)ethyl]benzene and related compounds in marine pore water by automated thermal desorption-gas chromatography/mass spectrometry using disposable optical fiber

    USGS Publications Warehouse

    Eganhouse, Robert P.; DiFilippo, Erica L

    2015-01-01

    A method is described for determination of ten DDT-related compounds in marine pore water based on equilibrium solid-phase microextraction (SPME) using commercial polydimethylsiloxane-coated optical fiber with analysis by automated thermal desorption-gas chromatography/mass spectrometry (TD-GC/MS). Thermally cleaned fiber was directly exposed to sediments and allowed to reach equilibrium under static conditions at the in situ field temperature. Following removal, fibers were rinsed, dried and cut into appropriate lengths for storage in leak-tight containers at -20°C. Analysis by TD-GC/MS under full scan (FS) and selected ion monitoring (SIM) modes was then performed. Pore-water method detection limits in FS and SIM modes were estimated at 0.05-2.4ng/L and 0.7-16pg/L, respectively. Precision of the method, including contributions from fiber handling, was less than 10%. Analysis of independently prepared solutions containing eight DDT compounds yielded concentrations that were within 6.9±5.5% and 0.1±14% of the actual concentrations in FS and SIM modes, respectively. The use of optical fiber with automated analysis allows for studies at high temporal and/or spatial resolution as well as for monitoring programs over large spatial and/or long temporal scales with adequate sample replication. This greatly enhances the flexibility of the technique and improves the ability to meet quality control objectives at significantly lower cost.

  10. Measurement of fiber orientation in short-fiber composites

    SciTech Connect

    Gonzalez, L.M.; Cumbrera, F.L.; Sanchez-Bajo, F.; Pajares, A. . Dept. de Fisica)

    1994-03-01

    The degree of fiber orientation in short-fiber composites plays an important role in determining many properties of these materials. In order to predict the toughening of a composite by using fiber reinforcements, the authors must consider the orientation of fibers as described probabilistically by the distribution function f([psi]), where [psi] is the angle which each fiber makes with the normal to the crack face. Here, a method for the characterization of the fiber orientation is built up in successive steps. In a first step the measurements of a planar array of fibers is afforded by extracting the important statistical information contained in a calculated Fraunhofer diffraction pattern of the fiber distribution. Subsequently, a method is proposed allowing us to derive the relevant f([psi]) distribution from the two-dimensional characterization of two orthogonal plane sections of the composite.

  11. Optical fiber switch

    DOEpatents

    Early, James W.; Lester, Charles S.

    2002-01-01

    Optical fiber switches operated by electrical activation of at least one laser light modulator through which laser light is directed into at least one polarizer are used for the sequential transport of laser light from a single laser into a plurality of optical fibers. In one embodiment of the invention, laser light from a single excitation laser is sequentially transported to a plurality of optical fibers which in turn transport the laser light to separate individual remotely located laser fuel ignitors. The invention can be operated electro-optically with no need for any mechanical or moving parts, or, alternatively, can be operated electro-mechanically. The invention can be used to switch either pulsed or continuous wave laser light.

  12. Probabilistic Fiber Composite Micromechanics

    NASA Technical Reports Server (NTRS)

    Stock, Thomas A.

    1996-01-01

    Probabilistic composite micromechanics methods are developed that simulate expected uncertainties in unidirectional fiber composite properties. These methods are in the form of computational procedures using Monte Carlo simulation. The variables in which uncertainties are accounted for include constituent and void volume ratios, constituent elastic properties and strengths, and fiber misalignment. A graphite/epoxy unidirectional composite (ply) is studied to demonstrate fiber composite material property variations induced by random changes expected at the material micro level. Regression results are presented to show the relative correlation between predictor and response variables in the study. These computational procedures make possible a formal description of anticipated random processes at the intra-ply level, and the related effects of these on composite properties.

  13. Containerless glass fiber processing

    NASA Technical Reports Server (NTRS)

    Ethridge, E. C.; Naumann, R. J.

    1986-01-01

    An acoustic levitation furnace system is described that was developed for testing the feasibility of containerless fiber pulling experiments. It is possible to levitate very dense materials such as platinum at room temperature. Levitation at elevated temperatures is much more difficult. Samples of dense heavy metal fluoride glass were levitated at 300 C. It is therefore possible that containerless fiber pulling experiments could be performed. Fiber pulling from the melt at 650 C is not possible at unit gravity but could be possible at reduced gravities. The Acoustic Levitation Furnace is described, including engineering parameters and processing information. It is illustrated that a shaped reflector greatly increases the levitation force aiding the levitation of more dense materials.

  14. Carbon Fiber Composites

    NASA Technical Reports Server (NTRS)

    1997-01-01

    HyComp(R), Inc. development a line of high temperature carbon fiber composite products to solve wear problems in the harsh environment of steel and aluminum mills. WearComp(R), self-lubricating composite wear liners and bushings, combines carbon graphite fibers with a polyimide binder. The binder, in conjunction with the fibers, provides the slippery surface, one that demands no lubrication, yet wears at a very slow rate. WearComp(R) typically lasts six to ten times longer than aluminum bronze. Unlike bronze, WearComp polishes the same surface and imparts a self-lube film for years of service. It is designed for continuous operation at temperatures of 550 degrees Fahrenheit and can operate under high compressive loads.

  15. Determination of atmospheric amines by on-fiber derivatization solid-phase microextraction with 2,3,4,5,6-pentafluorobenzyl chloroformate and 9-fluorenylmethoxycarbonyl chloride.

    PubMed

    Parshintsev, Jevgeni; Rönkkö, Tuukka; Helin, Aku; Hartonen, Kari; Riekkola, Marja-Liisa

    2015-01-09

    Alkylamines play an important role in atmospheric chemistry and are of concern for human health. Determining them from the vapor phase is challenging owing to their high polarity and volatility, water solubility, low concentrations, and poor chromatographic properties. We propose on-fiber derivatization solid-phase microextraction (SPME) to increase sensitivity and selectivity for the determination of alkylamines in air samples. SPME fibers coated in head-space with 2,3,4,5,6-pentafluorobenzyl chloroformate (PFBCF, 10min) or 9-fluorenylmethoxycarbonyl (FMOC) chloride (5min) were exposed to the sample for 5-120min, after which the derivatized alkylamines were thermally desorbed in the GC injection port and analyzed by GC-MS. The specific focus of the research was dimethylamine (DMA) but, as well as secondary amines, both coating agents readily react with primary and tertiary amines and with ammonia at ambient temperatures. The fiber coating procedures, sampling times, and analytical conditions were optimized, and methods were tested with natural samples. PFBCF was more selective and almost an order of magnitude more sensitive than FMOC chloride. Both reagents are applicable, however, depending on the requirements. With scan mode and use of molecular ion for quantification, the limit of quantification for DMA was 0.17μgL(-1) when derivatized with PFBCF and 3.4μgL(-1) when derivatized with FMOC chloride. When selected ion monitoring was used with the most abundant ion, the limit of quantification for DMA was 2.8ngL(-1). Intermediate reproducibility expressed as relative standard deviation was around 30% with PFBCF and less than 20% with FMOC chloride. Fibers coated with PFBCF could be used at least up to 24h when stored at 4°C and for 5 to 7h when stored at room temperature. After sampling/derivatization, storage time before analysis should not exceed 48h at 4°C or 24h at room temperature. At maximum, the PFBCF-coated fiber can be used in 100 coating

  16. Tunable random fiber laser

    SciTech Connect

    Babin, S. A.; Podivilov, E. V.; El-Taher, A. E.; Harper, P.; Turitsyn, S. K.

    2011-08-15

    An optical fiber is treated as a natural one-dimensional random system where lasing is possible due to a combination of Rayleigh scattering by refractive index inhomogeneities and distributed amplification through the Raman effect. We present such a random fiber laser that is tunable over a broad wavelength range with uniquely flat output power and high efficiency, which outperforms traditional lasers of the same category. Outstanding characteristics defined by deep underlying physics and the simplicity of the scheme make the demonstrated laser a very attractive light source both for fundamental science and practical applications.

  17. Geophysical Fiber Interferometer Gyroscope.

    DTIC Science & Technology

    1979-12-31

    gravitational antenna. Basically, their device was a Twyman -Green laser interferometer that was allegedly well-isolated from its thermal and...r ~AD-AO92 913 UTAH UNIV RESEARCH INST SALT LAKE CITY GEOSPACE SCIE-EYC F/B 20/6 GEOPHYSICAL FIBER INTERFEROMETER GYROSCOPE(U) .S DEC 79 L 0 WEAVER...ACCESSION no: S, 111CIPIENT’S CATALOG NUMBER AF6ii M_ __ _ __I_ _ 4. TItLIL (eovm4jk"IU .TYEo nPaTawn.ocoet GEOPHYSICAL FIBER INTERFEROMETER GYROSCOPE. / 9

  18. QUARTZ FIBER ELECTROSCOPES

    DOEpatents

    Henderson, R.P.

    1956-04-17

    This patent pertains to quartz fiber electroscopes of small size for use by personnel to monitor nuclear radiation. The invention resides tn a novel way of charging the electroscope whereby the charging of the electroscope whereby the charging of the electroscope is carried out without obtaining contact with the fiber system or its support and the electroscope can therefore be constructed without a protective cap to prevent wrongful discharge. The electroscope is charged by placing a voltage between an electrode located in close proximity to the element to be charged and the electroscope me metallic case. ABSTRACTS

  19. Automated fiber pigtailing machine

    DOEpatents

    Strand, Oliver T.; Lowry, Mark E.

    1999-01-01

    The Automated Fiber Pigtailing Machine (AFPM) aligns and attaches optical fibers to optoelectonic (OE) devices such as laser diodes, photodiodes, and waveguide devices without operator intervention. The so-called pigtailing process is completed with sub-micron accuracies in less than 3 minutes. The AFPM operates unattended for one hour, is modular in design and is compatible with a mass production manufacturing environment. This machine can be used to build components which are used in military aircraft navigation systems, computer systems, communications systems and in the construction of diagnostics and experimental systems.

  20. Automated fiber pigtailing machine

    DOEpatents

    Strand, O.T.; Lowry, M.E.

    1999-01-05

    The Automated Fiber Pigtailing Machine (AFPM) aligns and attaches optical fibers to optoelectronic (OE) devices such as laser diodes, photodiodes, and waveguide devices without operator intervention. The so-called pigtailing process is completed with sub-micron accuracies in less than 3 minutes. The AFPM operates unattended for one hour, is modular in design and is compatible with a mass production manufacturing environment. This machine can be used to build components which are used in military aircraft navigation systems, computer systems, communications systems and in the construction of diagnostics and experimental systems. 26 figs.

  1. Silicon fiber optic sensors

    DOEpatents

    Pocha, Michael D.; Swierkowski, Steve P.; Wood, Billy E.

    2007-10-02

    A Fabry-Perot cavity is formed by a partially or wholly reflective surface on the free end of an integrated elongate channel or an integrated bounding wall of a chip of a wafer and a partially reflective surface on the end of the optical fiber. Such a constructed device can be utilized to detect one or more physical parameters, such as, for example, strain, through the optical fiber using an optical detection system to provide measuring accuracies of less than aboutb0.1%.

  2. Fiber-Optic Sensing Technology

    SciTech Connect

    Milnes, M.; Baylor, L.C.; Bave, S.

    1996-10-24

    This article offers a basic review of fiber-optic sensing technology, or more specifically, fiber-optic sensing technology as applied to the qualitative or quantitative identification of a chemical sample, and how it works,

  3. Ionic Liquid-Mediated Multi-Walled Carbon Nanotube-Polydimethylsiloxane Fiber for Headspace Solid-Phase Microextraction of Phenolic Compounds in Aqueous Samples by Gas Chromatography Coupled to Flame Ionization Detector.

    PubMed

    Sadri, Minoo; Vatani, Hossein

    2017-02-01

    An ionic liquid-mediated multi-walled carbon nanotube (MWCNT)-polydimethylsiloxane (PDMS) sorbent was developed for headspace solid-phase microextraction (HS-SPME) of phenolic compounds from human urine samples. Sol-gel method was used to prepare this sorbent. For this purpose, MWCNTs were functionalized covalently and were attached chemically to the hydroxyl-terminated PDMS. Prepared fiber showed high thermal stability (over than 320°C) and good lifespan (>210 times). These good performances can be attributed to the performance of carbon nanotubes and sol-gel method. Affecting parameters on the efficiency of HS-SPME were investigated and optimized. Under the optimal conditions, linear dynamic ranges were observed over a range of 0.002-200 ng mL(-1) with limits of detection from 0.0005 to 0.005 ng mL(-1) and limits of quantitation between 0.002 and 0.02 ng mL(-1) The relative standard deviations for one fiber (repeatability) (n = 5) at three different concentrations (0.05, 2 and 100 ng mL(-1)) were obtained from 4.6 up to 6.7% and between fibers or batch to batch (n = 3) (reproducibility) in the range of 5.7-7.8%. Urine samples were used as real samples. All real samples were spiked at 0.5 ng mL(-1) of understudy analytes and the relative recovery percentages obtained from 90.7 to 102.1%.

  4. Optical Fibers for Nonlinear Optics.

    DTIC Science & Technology

    1986-10-01

    wavelength, showing structure due to water absorption bands .............................. 21 11 Schematic diagram of the experimental apparatus for phase...Figure 10. (b) Spectrum of PK3 fiber attenuation versus wavelength, showing structure due to water absorption bands. -L -L1 D C- LCL 0 (0 o o wj 0 00zzo...crystal fibers (ADP). 1984 Development of traveling zone method converting polycrystalline extruded fiber to single-crystal fiber (AgCl, AgBr, CuCl

  5. Low-Loss Fiber Waveguides.

    DTIC Science & Technology

    1980-10-01

    low- loss fibers requires producing fiber from unconventional, non-oxide materials such as the metal halides or some special fluoride glasses...hot rolling over extrusion is that there is less friction between the fiber and forming surface (roller or die) and smaller reductions per pass. At...quality was poor, exhibiting a fish- scale appearance that resulted from friction between the die and the surface of the fiber. We have to conclude

  6. Boron nitride converted carbon fiber

    SciTech Connect

    Rousseas, Michael; Mickelson, William; Zettl, Alexander K.

    2016-04-05

    This disclosure provides systems, methods, and apparatus related to boron nitride converted carbon fiber. In one aspect, a method may include the operations of providing boron oxide and carbon fiber, heating the boron oxide to melt the boron oxide and heating the carbon fiber, mixing a nitrogen-containing gas with boron oxide vapor from molten boron oxide, and converting at least a portion of the carbon fiber to boron nitride.

  7. Fluoride Glass Fiber Sources: Problems and Prospects

    DTIC Science & Technology

    2010-09-01

    earths for mid IR emission High power and supercontinuum Fiber must withstand large pump power Reliability of resonator, splicing and end faces...conversion ZBLAN fiber lasers: Mid IR Supercontinuum Significant achievements with ZBLAN fibers Various parameters: fiber length, attenuation, pump power...pump frequency, pump wavelength, N.A., dispersion, fiber geometry… Laboratory results Available systems Supercontinuum using short fibers From

  8. In-fiber integrated Michelson interferometer

    NASA Astrophysics Data System (ADS)

    Yuan, Libo; Yang, Jun; Liu, Zhihai; Sun, Jiaxing

    2006-09-01

    A novel fiber-optic in-fiber integrated Michelson interferometer has been proposed and demonstrated. It consists of a segment of two-core fiber with a mirrored fiber end. The sensing characteristics based on the two-core fiber bending, corresponding to the shift of the phase of the two-core in-fiber integrated Michelson interferometer, are investigated.

  9. In-fiber integrated Michelson interferometer.

    PubMed

    Yuan, Libo; Yang, Jun; Liu, Zhihai; Sun, Jiaxing

    2006-09-15

    A novel fiber-optic in-fiber integrated Michelson interferometer has been proposed and demonstrated. It consists of a segment of two-core fiber with a mirrored fiber end. The sensing characteristics based on the two-core fiber bending, corresponding to the shift of the phase of the two-core in-fiber integrated Michelson interferometer, are investigated.

  10. Development of nitrogen-enriched carbonaceous material coated titania nanotubes array as a fiber coating for solid-phase microextraction of ultraviolet filters in environmental water.

    PubMed

    Ma, Mingguang; Wang, Huiju; Zhen, Qi; Zhang, Min; Du, Xinzhen

    2017-05-15

    A novel solid-phase microextraction (SPME) fiber was fabricated by direct electrodeposition of polyaniline (PANI) coated the titania nanotube arrays in situ grown on the titanium wire followed by carbonization at 500°C under nitrogen atmosphere. The resulting titanium-based fiber with nitrogen-enriched carbonaceous material coated titania nanotubes (N-C/TiO2NTs/Ti) showed better extraction performance for ultraviolet (UV) filters among model aromatic compounds compared with common PANI as well as commercial polydimethylsiloxane and polyacrylate coatings. The influence of various experimental parameters on the extraction efficiency of UV filters were investigated and optimized. The calibration curves were linear from 0.2 to 200μgL(-1) for each analyte with correlation coefficients above 0.9980. Limits of detection (LODs) and limits of quantitation (LOQs) ranged from 0.03 to 0.05μgL(-1) and from 0.11 to 0.18μgL(-1) for UV filters, respectively. Relative standard deviations (RSDs) for single fiber repeatability ranged from 3.3% to 4.1% (n=5) and RSDs for fiber-to-fiber reproducibility (n=3) varied from 5.7% to 7.7%. The proposed method was successfully applied to the preconcentration and determination of target UV filters in river water and wastewater samples with good recoveries from 86.2% to 113%. Moreover this novel Ti-based fiber is mechanically and chemically stable, and can be easily prepared in a highly reproducible manner.

  11. Fabrication of Optical Fiber Devices

    NASA Astrophysics Data System (ADS)

    Andres, Miguel V.

    In this paper we present the main research activities of the Laboratorio de Fibras Opticas del Instituto de Ciencia de los Materiales de la Universidad de Valencia. We show some of the main results obtained for devices based on tapered fibers, fiber Bragg gratings, acousto-optic effects and photonic crystal fibers.

  12. Buying Fiber-Optic Networks.

    ERIC Educational Resources Information Center

    Fickes, Michael

    2003-01-01

    Describes consortia formed by college and university administrators to buy, manage, and maintain their own fiber-optic networks with the goals of cutting costs of leasing fiber-optic cable and planning for the future. Growth capacity is the real advantage of owning fiber-optic systems. (SLD)

  13. Large core fiber optic cleaver

    DOEpatents

    Halpin, John M.

    1996-01-01

    The present invention relates to a device and method for cleaving optical fibers which yields cleaved optical fiber ends possessing high damage threshold surfaces. The device can be used to cleave optical fibers with core diameters greater than 400 .mu.m.

  14. Fiber Optics and Library Technology.

    ERIC Educational Resources Information Center

    Koenig, Michael

    1984-01-01

    This article examines fiber optic technology, explains some of the key terminology, and speculates about the way fiber optics will change our world. Applications of fiber optics to library systems in three major areas--linkage of a number of mainframe computers, local area networks, and main trunk communications--are highlighted. (EJS)

  15. Shedding Light on Fiber Optics.

    ERIC Educational Resources Information Center

    Bunch, Robert M.

    1994-01-01

    Explains the principles of fiber optics as a medium for light-wave communication. Current uses of fiber systems on college campuses include voice, video, and local area network applications. A group of seven school districts in Minnesota are linked via fiber-optic cables. Other uses are discussed. (MLF)

  16. Advanced Optical Fiber Communication Systems

    DTIC Science & Technology

    1992-08-01

    Optical Network with Physical Star Topology," Advanced Fiber Communications Technologies , Leonid G. Kazovsky... advances in the performance and capabilities of optical fiber communication systems. While some of these technologies are interrelated (for example...multi gigabit per second hybrid circuit/packet switched lightwave network ," Proc. SPIE Advanced Fiber Communications Technologies , Boston 󈨟, Sept.

  17. Large core fiber optic cleaver

    DOEpatents

    Halpin, J.M.

    1996-03-26

    The present invention relates to a device and method for cleaving optical fibers which yields cleaved optical fiber ends possessing high damage threshold surfaces. The device can be used to cleave optical fibers with core diameters greater than 400 {micro}m. 30 figs.

  18. Aerogel-clad optical fiber

    DOEpatents

    Sprehn, Gregory A.; Hrubesh, Lawrence W.; Poco, John F.; Sandler, Pamela H.

    1997-01-01

    An optical fiber is surrounded by an aerogel cladding. For a low density aerogel, the index of refraction of the aerogel is close to that of air, which provides a high numerical aperture to the optical fiber. Due to the high numerical aperture, the aerogel clad optical fiber has improved light collection efficiency.

  19. Aerogel-clad optical fiber

    DOEpatents

    Sprehn, G.A.; Hrubesh, L.W.; Poco, J.F.; Sandler, P.H.

    1997-11-04

    An optical fiber is surrounded by an aerogel cladding. For a low density aerogel, the index of refraction of the aerogel is close to that of air, which provides a high numerical aperture to the optical fiber. Due to the high numerical aperture, the aerogel clad optical fiber has improved light collection efficiency. 4 figs.

  20. Procedure for dispersing fiber bundles

    NASA Technical Reports Server (NTRS)

    Padilla, D.

    1974-01-01

    Fiber bundles are dispersed and fibers are cleaned within enclosed container; therefore, safety clothing, masks, and eye protection are not required. Procedure also could be used wherever materials, such as fiberglass or insulation, require dispersion, fluffing, or cleaning. Process could be automated into continuous operation for handling large quantities of fiber.

  1. Development of fiber-to-fiber connectors for scintillating tile/fiber calorimeters

    NASA Astrophysics Data System (ADS)

    Aota, S.; Bossert, R. C.; Fukuda, S.; Hara, K.; Kawamoto, H.; Kim, S.; Kondo, K.; Mishina, M.; Nakada, H.; Sato, H.; Seiya, Y.; Takikawa, K.

    1995-02-01

    We have developed fiber-to-fiber connectors for plastic fibers of 0.83, 0.90, and 1.00 mm in diameter. Such a connector is essential for detectors that use a large number of optical fibers, scintillating or clear. Typical applicators are unscintillating tile/fiber calorimetry and scintillating fiber tracking. We describe the design and performance of two types of small 10-fiber connectors which were developed for the CDF endplug tile/fiber calorimeter. The connectors showed a light transmission of 85-90% with a uniformity of 2.5-3.1%, and a reproducibility of 1%. Use of optical matching material at the joints could further improve the transmission and uniformity but showed instability after heat cycles.

  2. Infrared Fibers for Sensors

    DTIC Science & Technology

    2010-06-01

    they can be used to demonstrate broadband supercontinuum sources in the infrared (figure 3) when pumped with suitable lasers. They can also be used for...doped chalcogenide glasses. Figure 3. The supercontinuum emission from preliminary IR fibers. Figure 4. Chalcogenide glass based photonic

  3. Optical Fiber Protection

    NASA Technical Reports Server (NTRS)

    1999-01-01

    F&S Inc. developed and commercialized fiber optic and microelectromechanical systems- (MEMS) based instrumentation for harsh environments encountered in the aerospace industry. The NASA SBIR programs have provided F&S the funds and the technology to develop ruggedized coatings and coating techniques that are applied during the optical fiber draw process. The F&S optical fiber fabrication facility and developed coating methods enable F&S to manufacture specialty optical fiber with custom designed refractive index profiles and protective or active coatings. F&S has demonstrated sputtered coatings using metals and ceramics and combinations of each, and has also developed techniques to apply thin coatings of specialized polyimides formulated at NASA Langley Research Center. With these capabilities, F&S has produced cost-effective, reliable instrumentation and sensors capable of withstanding temperatures up to 800? C and continues building commercial sales with corporate partners and private funding. More recently, F&S has adapted the same sensing platforms to provide the rapid detection and identification of chemical and biological agents

  4. Fiber optics for controls

    NASA Technical Reports Server (NTRS)

    Seng, Gary T.

    1990-01-01

    The design, development, and testing of a fiber optic integrated propulsion/flight control system for an advanced supersonic dash aircraft (flies at supersonic speeds for short periods of time) is the goal of the joint NASA/DOD Fiber Optic Control System Integration (FOCSI) program. Phase 1 provided a comparison of electronic and optical control systems, identified the status of current optical sensor technology, defined the aircraft sensor/actuator environment, proposed architectures for fully optical control systems, and provided schedules for development. Overall, it was determined that there are sufficient continued efforts to develop such a system. It was also determined that it is feasible to build a fiber optic control system for the development of a data base for this technology, but that further work is necessary in sensors, actuators, and components to develop an optimum design, fully fiber optic integrated control system compatible with advanced aircraft environments. Phase 2 is to design, construct, and ground test a fly by light control system. Its first task is to provide a detailed design of the electro-optic architecture.

  5. Interferometric Fiber Optic Sensors

    PubMed Central

    Lee, Byeong Ha; Kim, Young Ho; Park, Kwan Seob; Eom, Joo Beom; Kim, Myoung Jin; Rho, Byung Sup; Choi, Hae Young

    2012-01-01

    Fiber optic interferometers to sense various physical parameters including temperature, strain, pressure, and refractive index have been widely investigated. They can be categorized into four types: Fabry-Perot, Mach-Zehnder, Michelson, and Sagnac. In this paper, each type of interferometric sensor is reviewed in terms of operating principles, fabrication methods, and application fields. Some specific examples of recently reported interferometeric sensor technologies are presented in detail to show their large potential in practical applications. Some of the simple to fabricate but exceedingly effective Fabry-Perot interferometers, implemented in both extrinsic and intrinsic structures, are discussed. Also, a wide variety of Mach-Zehnder and Michelson interferometric sensors based on photonic crystal fibers are introduced along with their remarkable sensing performances. Finally, the simultaneous multi-parameter sensing capability of a pair of long period fiber grating (LPG) is presented in two types of structures; one is the Mach-Zehnder interferometer formed in a double cladding fiber and the other is the highly sensitive Sagnac interferometer cascaded with an LPG pair. PMID:22736961

  6. Carbon fiber study

    NASA Technical Reports Server (NTRS)

    1977-01-01

    A coordinated Federal Government action plan for dealing with the potential problems arising from the increasing use of graphite fiber reinforced composite materials in both military and civilian applications is presented. The required dissemination of declassified information and an outline of government actions to minimize the social and economic consequences of proliferated composite materials applications were included.

  7. Infrared Fiber Optic Sensors

    NASA Technical Reports Server (NTRS)

    1997-01-01

    Successive years of Small Business Innovation Research (SBIR) contracts from Langley Research Center to Sensiv Inc., a joint venture between Foster-Miller Inc. and Isorad, Ltd., assisted in the creation of remote fiber optic sensing systems. NASA's SBIR interest in infrared, fiber optic sensor technology was geared to monitoring the curing cycles of advanced composite materials. These funds helped in the fabrication of an infrared, fiber optic sensor to track the molecular vibrational characteristics of a composite part while it is being cured. Foster-Miller ingenuity allowed infrared transmitting optical fibers to combine with Fourier Transform Infrared spectroscopy to enable remote sensing. Sensiv probes operate in the mid-infrared range of the spectrum, although modifications to the instrument also permits its use in the near-infrared region. The Sensiv needle-probe is built to be placed in a liquid or powder and analyze the chemicals in the mixture. Other applications of the probe system include food processing control; combustion control in furnaces; and maintenance problem solving.

  8. Drying of fiber webs

    DOEpatents

    Warren, David W.

    1997-01-01

    A process and an apparatus for high-intensity drying of fiber webs or sheets, such as newsprint, printing and writing papers, packaging paper, and paperboard or linerboard, as they are formed on a paper machine. The invention uses direct contact between the wet fiber web or sheet and various molten heat transfer fluids, such as liquified eutectic metal alloys, to impart heat at high rates over prolonged durations, in order to achieve ambient boiling of moisture contained within the web. The molten fluid contact process causes steam vapor to emanate from the web surface, without dilution by ambient air; and it is differentiated from the evaporative drying techniques of the prior industrial art, which depend on the uses of steam-heated cylinders to supply heat to the paper web surface, and ambient air to carry away moisture, which is evaporated from the web surface. Contact between the wet fiber web and the molten fluid can be accomplished either by submersing the web within a molten bath or by coating the surface of the web with the molten media. Because of the high interfacial surface tension between the molten media and the cellulose fiber comprising the paper web, the molten media does not appreciately stick to the paper after it is dried. Steam generated from the paper web is collected and condensed without dilution by ambient air to allow heat recovery at significantly higher temperature levels than attainable in evaporative dryers.

  9. Drying of fiber webs

    DOEpatents

    Warren, D.W.

    1997-04-15

    A process and an apparatus are disclosed for high-intensity drying of fiber webs or sheets, such as newsprint, printing and writing papers, packaging paper, and paperboard or linerboard, as they are formed on a paper machine. The invention uses direct contact between the wet fiber web or sheet and various molten heat transfer fluids, such as liquefied eutectic metal alloys, to impart heat at high rates over prolonged durations, in order to achieve ambient boiling of moisture contained within the web. The molten fluid contact process causes steam vapor to emanate from the web surface, without dilution by ambient air; and it is differentiated from the evaporative drying techniques of the prior industrial art, which depend on the uses of steam-heated cylinders to supply heat to the paper web surface, and ambient air to carry away moisture, which is evaporated from the web surface. Contact between the wet fiber web and the molten fluid can be accomplished either by submersing the web within a molten bath or by coating the surface of the web with the molten media. Because of the high interfacial surface tension between the molten media and the cellulose fiber comprising the paper web, the molten media does not appreciatively stick to the paper after it is dried. Steam generated from the paper web is collected and condensed without dilution by ambient air to allow heat recovery at significantly higher temperature levels than attainable in evaporative dryers. 6 figs.

  10. Bluebonnet Fiber Collages

    ERIC Educational Resources Information Center

    Sterling, Joan

    2009-01-01

    This article presents a lesson that uses stitching and applique techniques to create a fiber collage in which every child is successful with high-quality work. This lesson was inspired by Tomie dePaola's "The Legend of the Bluebonnet." The back cover had a lovely illustration of the bluebonnet flower the author thought would translate easily to a…

  11. Fiber optic temperature sensor

    NASA Technical Reports Server (NTRS)

    Quick, William H. (Inventor); August, Rudolf R. (Inventor); James, Kenneth A. (Inventor); Strahan, Jr., Virgil H. (Inventor); Nichols, Donald K. (Inventor)

    1980-01-01

    An inexpensive, lightweight fiber optic micro-sensor that is suitable for applications which may require remote temperature sensing. The disclosed temperature sensor includes a phosphor material that, after receiving incident light stimulation, is adapted to emit phosphorescent radiation output signals, the amplitude decay rate and wavelength of which are functions of the sensed temperature.

  12. Optical Fiber Spectroscopy

    NASA Technical Reports Server (NTRS)

    Buoncristiani, A. M.

    1999-01-01

    This is the final report of work done on NASA Grant NAG-1-443. The work covers the period from July 1, 1992 to December 1, 1998. During this period several distinct but related research studies and work tasks were undertaken. These different subjects are enumerated below with a description of the work done on each of them. The focus of the research was the development of optical fibers for use as distributed temperature and stress sensors. The initial concept was to utilize the utilize the temperature and stress dependence of emission from rare earth and transition metal ions substitutionally doped into crystalline or glass fibers. During the course of investigating this it became clear that fiber Bragg gratings provided a alternative for making the desired measurements and there was a shift of research focus on to include the photo-refractive properties of germano-silicate glasses used for most gratings and to the possibility of developing fiber laser sources for an integrated optical sensor in the research effort. During the course of this work several students from Christopher Newport University and other universities participated in this effort. Their names are listed below. Their participation was an important part of their education.

  13. Refractory ceramic fibers

    Integrated Risk Information System (IRIS)

    Refractory ceramic fibers ; CASRN Not found Human health assessment information on a chemical substance is included in the IRIS database only after a comprehensive review of toxicity data , as outlined in the IRIS assessment development process . Sections I ( Health Hazard Assessments for Noncarcino

  14. Interferometric fiber optic sensors.

    PubMed

    Lee, Byeong Ha; Kim, Young Ho; Park, Kwan Seob; Eom, Joo Beom; Kim, Myoung Jin; Rho, Byung Sup; Choi, Hae Young

    2012-01-01

    Fiber optic interferometers to sense various physical parameters including temperature, strain, pressure, and refractive index have been widely investigated. They can be categorized into four types: Fabry-Perot, Mach-Zehnder, Michelson, and Sagnac. In this paper, each type of interferometric sensor is reviewed in terms of operating principles, fabrication methods, and application fields. Some specific examples of recently reported interferometeric sensor technologies are presented in detail to show their large potential in practical applications. Some of the simple to fabricate but exceedingly effective Fabry-Perot interferometers, implemented in both extrinsic and intrinsic structures, are discussed. Also, a wide variety of Mach-Zehnder and Michelson interferometric sensors based on photonic crystal fibers are introduced along with their remarkable sensing performances. Finally, the simultaneous multi-parameter sensing capability of a pair of long period fiber grating (LPG) is presented in two types of structures; one is the Mach-Zehnder interferometer formed in a double cladding fiber and the other is the highly sensitive Sagnac interferometer cascaded with an LPG pair.

  15. Multiwavelength fiber laser for the fiber link monitoring system

    NASA Astrophysics Data System (ADS)

    Peng, Peng-Chun; Lee, Wei-Yun; Wu, Shin-Shian; Hu, Hsuan-Lun

    2013-10-01

    This work proposes a novel fiber link monitoring system that uses a multiwavelength fiber laser for wavelength-division-multiplexed (WDM) passive optical network (PON). The multiwavelength fiber laser is based on an erbium-doped fiber amplifier (EDFA) and a semiconductor optical amplifier (SOA). Experimental results show the feasibility using the system to monitor a fiber link with a high and stable signal-to-noise ratio (SNR) of over 26 dB. The link quality of downstream signals as well as the fiber link on WDM channels can be monitored in real time. Favorable carrier-to-noise ratio (CNR), composite second-order (CSO), and composite triple beat (CTB) performance metrics were obtained for cable television (CATV) signals that were transported through 25 km of standard single-mode fiber (SMF).

  16. Saccharification of Okara fiber by plant dietary fiber hydrolases.

    PubMed

    Matsuo, Masako

    2004-08-01

    In this paper, the saccharification process of okara fiber with pectinase, xylanase and cellulase was investigated as a preliminary attempt to effectively utilize okara fiber. The solubilization of okara fiber was raised in proportion to the number of enzymes used; that is, by a single enzyme, two enzymes and three enzymes, in that order. The saccharification of okara fiber was much more completed by a combination of pectinase, xylanase and cellulase than by using individual preparations. This multi-enzyme system liberated sugars equivalent to 80% of the original okara fiber by weight. Moreover the structure of okara fiber gradually disintegrated by hydrolytic reactions with pectinase, xylanase and cellulase in turns. These results suggest that the saccharification of okara fiber progresses by the cooperative action of pectinase, xylanase and cellulase.

  17. Health Benefits of Fiber Fermentation.

    PubMed

    Dahl, Wendy J; Agro, Nicole C; Eliasson, Åsa M; Mialki, Kaley L; Olivera, Joseph D; Rusch, Carley T; Young, Carly N

    2017-02-01

    Although fiber is well recognized for its effect on laxation, increasing evidence supports the role of fiber in the prevention and treatment of chronic disease. The aim of this review is to provide an overview of the health benefits of fiber and its fermentation, and describe how the products of fermentation may influence disease risk and treatment. Higher fiber intakes are associated with decreased risk of cardiovascular disease, type 2 diabetes, and some forms of cancer. Fiber may also have a role in lowering blood pressure and in preventing obesity by limiting weight gain. Fiber is effective in managing blood glucose in type 2 diabetes, useful for weight loss, and may provide therapeutic adjunctive roles in kidney and liver disease. In addition, higher fiber diets are not contraindicated in inflammatory bowel disease or irritable bowel syndrome and may provide some benefit. Common to the associations with disease reduction is fermentation of fiber and its potential to modulate microbiota and its activities and inflammation, specifically the production of anti-inflammatory short chain fatty acids, primarily from saccharolytic fermentation, versus the deleterious products of proteolytic activity. Because fiber intake is inversely associated with all-cause mortality, mechanisms by which fiber may reduce chronic disease risk and provide therapeutic benefit to those with chronic disease need further elucidation and large, randomized controlled trials are needed to confirm causality.Teaching Points• Strong evidence supports the association between higher fiber diets and reduced risk of cardiovascular disease, type 2 diabetes, and some forms of cancer.• Higher fiber intakes are associated with lower body weight and body mass index, and some types of fiber may facilitate weight loss.• Fiber is recommended as an adjunctive medical nutritional therapy for type 2 diabetes, chronic kidney disease, and certain liver diseases.• Fermentation and the resulting shifts in

  18. Polymer-Derived Ceramic Fibers

    NASA Astrophysics Data System (ADS)

    Ichikawa, Hiroshi

    2016-07-01

    SiC-based ceramic fibers are derived from polycarbosilane or polymetallocarbosilane precursors and are classified into three groups according to their chemical composition, oxygen content, and C/Si atomic ratio. The first-generation fibers are Si-C-O (Nicalon) fibers and Si-Ti-C-O (Tyranno Lox M) fibers. Both fibers contain more than 10-wt% oxygen owing to oxidation during curing and lead to degradation in strength at temperatures exceeding 1,300°C. The maximum use temperature is 1,100°C. The second-generation fibers are SiC (Hi-Nicalon) fibers and Si-Zr-C-O (Tyranno ZMI) fibers. The oxygen content of these fibers is reduced to less than 1 wt% by electron beam irradiation curing in He. The thermal stability of these fibers is improved (they are stable up to 1,500°C), but their creep resistance is limited to a maximum of 1,150°C because their C/Si atomic ratio results in excess carbon. The third-generation fibers are stoichiometric SiC fibers, i.e., Hi-Nicalon Type S (hereafter Type S), Tyranno SA, and Sylramic™ fibers. They exhibit improved thermal stability and creep resistance up to 1,400°C. Stoichiometric SiC fibers meet many of the requirements for the use of ceramic matrix composites for high-temperature structural application. SiBN3C fibers derived from polyborosilazane also show promise for structural applications, remain in the amorphous state up to 1,800°C, and have good high-temperature creep resistance.

  19. Thulium Fiber Laser lithotripsy

    NASA Astrophysics Data System (ADS)

    Blackmon, Richard Leious, Jr.

    The Thulium Fiber Laser (TFL) has been studied as a potential alternative to the conventional Holmium:YAG laser (Ho:YAG) for the treatment of kidney stones. The TFL is more ideally suited for laser lithotripsy because of the higher absorption coefficient of the emitted wavelength in water, the superior Gaussian profile of the laser beam, and the ability to operate at arbitrary temporal pulse profiles. The higher absorption of the TFL by water helps translate into higher ablation of urinary stones using less energy. The Gaussian spatial beam profile allows the TFL to couple into fibers much smaller than those currently being used for Ho:YAG lithotripsy. Lastly, the ability of arbitrary pulse operation by the TFL allows energy to be delivered to the stone efficiently so as to avoid negative effects (such as burning or bouncing of the stone) while maximizing ablation. Along with these improvements, the unique properties of the TFL have led to more novel techniques that have currently not been used in the clinic, such as the ability to control the movement of stones based on the manner in which the laser energy is delivered. Lastly, the TFL has led to the development of novel fibers, such as the tapered fiber and removable tip fiber, to be used for lithotripsy which can lead to safer and less expensive treatment of urinary stones. Overall, the TFL has been demonstrated as a viable alternative to the conventional Ho:YAG laser and has the potential to advance methods and tools for treatment of kidney stones.

  20. Optical-Fiber Leak Detector

    NASA Technical Reports Server (NTRS)

    Workman, Gary L.; Kosten, Susan E.

    1994-01-01

    Proposed optical-fiber sensor detects small changes in pressure in elastomeric O-ring or similar pressure seal, which may indicate deterioration of seal and interpreted as indications of incipient failure. According to concept, length of optical fiber embedded in seal. Light-emitting diode illuminates one end of fiber; photodetector measures intensity of light emerging from other end. Pressure-induced changes in seal bend fiber slightly, altering microbending-induced loss of light from fiber and alter intensity of light at photodetector. Change in intensity approximately proportional to change in pressure.

  1. Improved Optical Fiber Chemical Sensors

    NASA Technical Reports Server (NTRS)

    Egalon, Claudio O.; Rogowski, Robert S.

    1994-01-01

    Calculations, based on exact theory of optical fiber, have shown how to increase optical efficiency sensitivity of active-core, step-index-profile optical-fiber fluorosensor. Calculations result of efforts to improve efficiency of optical-fiber chemical sensor of previous concept described in "Making Optical-Fiber Chemical Sensors More Sensitive" (LAR-14525). Optical fiber chemical detector of enhanced sensitivity made in several configurations. Portion of fluorescence or chemiluminescence generated in core, and launched directly into bound electromagnetic modes that propagate along core to photodetector.

  2. Fiber pad for pressure mapping

    NASA Astrophysics Data System (ADS)

    Purwanto, H.; Fitriani, U. R.; Dwijosutomo, A.; Marzuki, A.

    2016-11-01

    Optical fiber sandwiched pad designed as a pressure mapping sensor has been configured and characterized. Optical fiber sensor was aligned to form a web-like configuration (x- y matrix). Several fibers were positioned to form lines parallel to y-axis while others are in parallel to x-axis. When a mass with a particular surface contour was loaded on the fiber pad, we have shown the dependence of the magnitude of light attenuation on the mass surface contour. Combining these light attenuation results we have successfully constructed a three dimensional contours showing the pressure distribution given by the mass to the fiber pad.

  3. Determination of diethylstilbestrol in milk using carbon nanotube-reinforced hollow fiber solid-phase microextraction combined with high-performance liquid chromatography.

    PubMed

    Yang, Yang; Chen, Juan; Shi, Yan-Ping

    2012-08-15

    Carbon nanotube-reinforced hollow fiber solid-phase microextraction (CNTs-HF-SPME) combined with high-performance liquid chromatography (HPLC) was used to extract and determine diethylstilbestrol (DES) in milk products. Wall pores of the hollow fiber were filled with multi-walled carbon nanotubes (MWCNTs) using sol-gel technology. In the proposed method, DES was selectively extracted by MWCNTs, desorbed to methanol, and analyzed by HPLC. The parameters affecting the efficiency of CNTs-HFSPME, such as the length of the hollow fiber, extraction and desorption times, extraction temperature, stirring rate, pH of the sample solution, and the amount of organic solvent and salt in the sample solution, were investigated and optimized. Under the optimized extraction conditions, the method showed good linearity (24-960 μg L(-1)), a low method detection limit (MDL, 5.1 μg L(-1)), and good recoveries at four different concentrations. It was proven to be simple, rapid, sensitive, and solvent free for the analysis of DES in dairy products.

  4. [Analysis of phenolic compounds in aqueous samples by gas chromatography coupled with headspace solid-phase microextraction using poly (phthalazine ether sulfone ketone) coated fiber].

    PubMed

    Yao, Guiyan; Guan, Wenna; Xu, Feng; Wang, Hua; Guan, Yafeng

    2008-09-01

    The direct trace analysis of phenolic compounds in aqueous samples was performed by headspace solid-phase microextraction/gas chromatography (HS-SPME/GC). A laboratory made poly (phthalazine ether sulfone ketone) (PPESK, 30 microm) coated fiber was used to extract the phenols from aqueous samples. The parameters affecting the extraction efficiency, such as extraction temperature and time, pH value, and salt concentration, were optimized. The low pH value and high salt concentration can increase the extraction efficiency of phenols. The limits of detection (LODs) were from 0.003 to 0.041 microg/L, which were within the range of EPA Method 604. The relative standard deviations (RSDs) were less than 16%. Compared with commercial polyacrylate (PA) fiber (85 microm), the PPESK fiber shows high affinity toward phenolic compounds, and therefore, high absolute recoveries. The phenols were detected with the recoveries of 100.5%-111.8% for a tap water sample and 94.8%-117.3% for a seawater sample at the spiked level of 20 microg/L.

  5. Scintillating glass fiber neutron senors

    SciTech Connect

    Abel, K.H.; Arthur, R.J.; Bliss, M.

    1994-04-01

    Cerium-doped lithium-silicate glass fibers have been developed at Pacific Northwest Laboratory (PNL) for use as thermal neutron detectors. By using highly-enriched {sup 6} Li , these fibers efficiently capture thermal neutrons and produce scintillation light that can be detected at the ends of the fibers. Advantages of scintillating fibers over {sup 3}He or BF{sub 3} proportional tubes include flexibility in geometric configuration, ruggedness in high-vibration environments, and less detector weight for the same neutron sensitivity. This paper describes the performance of these scintillating fibers with regard to count rates, pulse height spectra, absolute efficiencies, and neutron/gamma discrimination. Fibers with light transmission lengths (1/e) of greater than 2 m have been produced at PNL. Neutron sensors in fiber form allow development of a variety of neutron detectors packaged in previously unavailable configurations. Brief descriptions of some of the devices already produced are included to illustrate these possibilities.

  6. Fiber-optic voltage sensor

    NASA Astrophysics Data System (ADS)

    Wood, C. B.

    1990-07-01

    A fiber-optic voltage sensor is described which includes a source of light, a reference fiber for receiving a known percentage of the light and an electrostrictive element having terminals across which is applied, and a voltage to be measured. The electrostrictive element is responsive to the applied voltage to assume an altered physical state. A measuring fiber also receives a known percentage of light from the light source and is secured about the electrostrictive element. The measuring fiber is provided with a cladding and exhibits an evanescent wave in the cladding. The measuring fiber has a known length which is altered when the electrostrictive element assumes its altered physical state. A differential sensor is provided which senses the intensity of light in both the reference fiber and the measuring fiber and provides an output indicative of the difference between the intensities.

  7. Fano resonances in kagome fibers

    NASA Astrophysics Data System (ADS)

    Vincetti, L.; Setti, V.; Zoboli, M.

    2012-06-01

    Confinement Loss of microstructured fibers whose cladding is composed by a triangular arrangement of tubes of various shapes is theoretically and numerically investigated. Kagome Fibers belong from this family of fibers with cladding tubes with hexagonal shape. The shape of the cladding tubes is proved to strongly affect the performance of the microstructured fiber. In order to understand the reasons for this behavior, the spectral properties of the tubes that constitute the cladding are investigated first. It is proved that also these tubes suffer from additional Fano Resonances when they are given a polygonal shape. It is proved that, by using the analytical model developed for the stand alone polygonal tubes, it is possible to predict the spectral position of Fano Resonances also in microstructured fibers. This is extremely important since it suggest new ways to reduce confinement loss in kagome fibers and microstructured fibers in general.

  8. Predicting bioavailability of PAHs and PCBs with porewater concentrations measured by solid-phase microextraction fibers.

    PubMed

    Lu, Xiaoxia; Skwarski, Alison; Drake, Brian; Reible, Danny D

    2011-05-01

    Bioaccumulation of polycyclic aromatic hydrocarbons (PAHs) and polychlorinated biphenyls (PCBs) was measured in the deposit-feeding oligochaete Ilyodrilus templetoni exposed for 28 d to Anacostia River sediment (Washington, DC, USA) and to an initially uncontaminated sediment from Brown Lake (Vicksburg, MS, USA) sequentially diluted with 3 to 25% contaminated New Bedford Harbor sediment (New Bedford, MA, USA). The Anacostia River sediment studies represented exposure to a historically contaminated sediment with limited availability, whereas exposure to the other sediment included both the historically contaminated New Bedford Harbor sediment and fresh redistribution of contaminants into the Brown Lake sediments. Organism tissue concentrations did not correlate with bulk sediment concentrations in the Anacostia River sediment but did correlate with the sequentially diluted sediment. Porewater concentrations measured via disposable solid-phase microextraction fiber (SPME) with polydimethylsiloxane (PDMS), however, correlated well with organism uptake in all sediments. Bioaccumulation was predicted well by a linear relationship with the product of porewater concentration and compound octanol-water partition coefficient (Anacostia, slope = 1.08, r² = 0.76; sequentially diluted sediments, slope = 1.24, r² = 0.76). The data demonstrate that the octanol-water partition coefficient is a good indicator of the lipid-water partition coefficient and that porewater concentrations provide a more reliable indicator of bioaccumulation in the organism than sediment concentrations, even when the route of uptake is expected to be via sediment ingestion.

  9. Thulium fiber laser lithotripsy using small spherical distal fiber tips

    NASA Astrophysics Data System (ADS)

    Wilson, Christopher R.; Hardy, Luke A.; Kennedy, Joshua D.; Irby, Pierce B.; Fried, Nathaniel M.

    2016-02-01

    This study tests a 100-μm-core fiber with 300-μm-diameter ball tip during Thulium fiber laser (TFL) lithotripsy. The TFL was operated at 1908 nm wavelength with 35-mJ pulse energy, 500-μs pulse duration, and 300-Hz pulse rate. Calcium oxalate/phosphate stone samples were weighed, laser procedure times measured, and ablation rates calculated for ball tip fibers, with comparison to bare tip fibers. Photographs of ball tips were taken before and after each procedure to observe ball tip degradation and determine number of procedures completed before need to replace fiber. Saline irrigation rates and ureteroscope deflection were measured with and without TFL fiber present. There was no statistical difference (P > 0.05) between stone ablation rates for single-use ball tip fiber (1.3 +/- 0.4 mg/s) (n=10), multiple-use ball tip fiber (1.3 +/- 0.5 mg/s) (n=44), and conventional single-use bare tip fibers (1.3 +/- 0.2 mg/s) (n=10). Ball tip durability varied widely, but fibers averaged > 4 stone procedures before decline in stone ablation rates due to mechanical damage at front surface of ball tip. The small fiber diameter did not impact ureteroscope deflection or saline flow rates. The miniature ball tip fiber may provide a cost-effective design for safe fiber insertion through the ureteroscope working channel and the ureter without risk of scope damage or tissue perforation, and without compromising stone ablation efficiency during TFL ablation of kidney stones.

  10. Fiberized fluorescent dye microtubes

    NASA Astrophysics Data System (ADS)

    Vladev, Veselin; Eftimov, Tinko

    2013-03-01

    In the present work we study the effect of the length of fluorescent dye-filled micro-capillaries on the fluorescence spectra. Two types of micro-capillaries have been studied: a 100 μm inner diameter fused silica capillary with a transparent coating and one of the holes of a fiber optic glass ferrule with 125 μm inner diameter. The tubes were filled with solutions of Rhodamine 6G dissolved in ethanol and then in glycerin. Experimental data show that the maximum fluorescence and the largest spectral widths are observed for a sample length of about 0.25 mm for the used concentration. This results show that miniature tunable fiberized dye lasers can be developed using available standard micro-and fibre-optic components.

  11. Fiber optic fluid detector

    DOEpatents

    Angel, S. Michael

    1989-01-01

    Particular gases or liquids are detected with a fiber optic element (11, 11a to 11j) having a cladding or coating of a material (23, 23a to 23j) which absorbs the fluid or fluids and which exhibits a change of an optical property, such as index of refraction, light transmissiveness or fluoresence emission, for example, in response to absorption of the fluid. The fluid is sensed by directing light into the fiber optic element and detecting changes in the light, such as exit angle changes for example, that result from the changed optical property of the coating material. The fluid detector (24, 24a to 24j) may be used for such purposes as sensing toxic or explosive gases in the atmosphere, measuring ground water contamination or monitoring fluid flows in industrial processes, among other uses.

  12. Fiber optic fluid detector

    DOEpatents

    Angel, S.M.

    1987-02-27

    Particular gases or liquids are detected with a fiber optic element having a cladding or coating of a material which absorbs the fluid or fluids and which exhibits a change of an optical property, such as index of refraction, light transmissiveness or fluoresence emission, for example, in response to absorption of the fluid. The fluid is sensed by directing light into the fiber optic element and detecting changes in the light, such as exit angle changes for example, that result from the changed optical property of the coating material. The fluid detector may be used for such purposes as sensing toxic or explosive gases in the atmosphere, measuring ground water contamination or monitoring fluid flows in industrial processes, among other uses. 10 figs.

  13. Fiber optic TV direct

    NASA Technical Reports Server (NTRS)

    Kassak, John E.

    1991-01-01

    The objective of the operational television (OTV) technology was to develop a multiple camera system (up to 256 cameras) for NASA Kennedy installations where camera video, synchronization, control, and status data are transmitted bidirectionally via a single fiber cable at distances in excess of five miles. It is shown that the benefits (such as improved video performance, immunity from electromagnetic interference and radio frequency interference, elimination of repeater stations, and more system configuration flexibility) can be realized if application of the proven fiber optic transmission concept is used. The control system will marry the lens, pan and tilt, and camera control functions into a modular based Local Area Network (LAN) control network. Such a system does not exist commercially at present since the Television Broadcast Industry's current practice is to divorce the positional controls from the camera control system. The application software developed for this system will have direct applicability to similar systems in industry using LAN based control systems.

  14. Fiber Optic Velocity Interferometry

    SciTech Connect

    Neyer, Barry T.

    1988-04-01

    This paper explores the use of a new velocity measurement technique that has several advantages over existing techniques. It uses an optical fiber to carry coherent light to and from a moving target. A Fabry-Perot interferometer, formed by a gradient index lens and the moving target, produces fringes with a frequency proportional to the target velocity. This technique can measure velocities up to 10 km/s, is accurate, portable, and completely noninvasive.

  15. Optical fiber laser

    SciTech Connect

    Hakimi, F.; Po, H.; Snitzer, E.

    1987-07-14

    An optical fiber laser is described comprising: a gain cavity including a single mode optical fiber of given length having a core with a given index of refraction and a cladding surrounding the core and having an index of refraction lower than that of the core. The core comprises a host glass having incorporated a laser gain material with a fluorescence spectrum having at least one broadband region in which there is at least one peak emission line; filter means optically coupled to one end of the gain cavity and reflective to radiation emitted from the gain material over a predetermined wavelength interval about the peak emission line to provide feedback in the gain cavity; an etalon filter section butt coupled to the remaining end of the gain cavity optical fiber, the etalon filter section comprising a pair of filters spaced apart in parallel by a predetermined length of material transparent to any radiation emitted from the gain cavity. The predetermined length of the transparent material is such that the etalon filter section is no longer than the distance over which the wave train energy from the fiber core remains substantially planar so that the etalon filter section is inside the divergent region to enhance feedback in the gain cavity; and means for pumping energy into the gain cavity to raise the interval energy level such that only a small part of the ion population, corresponding to a predetermined bandwidth about the peak emission line, is raised above laser threshold. The laser emits radiation only over narrow lines over a narrow wavelength interval centered about the peak emission line.

  16. Functional Polymer Matrix Fibers

    DTIC Science & Technology

    2007-11-02

    the carbon nanofibers led to the deterioration of the polymeric cellulose structure. Extensive research on the surface treatment of carbon nanofibers...1 November 2003 - 14-Mar-05 4. TITLE AND SUBTITLE 5a. CONTRACT NUMBER FA8655-03-1-3042 Functional Polymer Matrix Fibres 5b. GRANT NUMBER 5c. PROGRAM...MARYLABONE RD LONDON NWl 5TH PERFORMANCE REPORT Project title: Functional polymer matrix fibers Period of performance: 1 November 2003 - 31 October 2004

  17. Fiber optic geophysical sensors

    DOEpatents

    Homuth, Emil F.

    1991-01-01

    A fiber optic geophysical sensor in which laser light is passed through a sensor interferometer in contact with a geophysical event, and a reference interferometer not in contact with the geophysical event but in the same general environment as the sensor interferometer. In one embodiment, a single tunable laser provides the laser light. In another embodiment, separate tunable lasers are used for the sensor and reference interferometers. The invention can find such uses as monitoring for earthquakes, and the weighing of objects.

  18. Intercalated Graphite Fiber Conductor.

    DTIC Science & Technology

    1980-12-01

    Lightweight electrical conductors were developed from graphitic fibers inter- calated with highly electrophilic intercalants. Conductance increases of...intercalated with highly electrophilic molecules ("intercalants") to en- hance their electrical conductivity. Evaluation of the elec- trical resistance of two...corrosion resistant to fluorine containing chemicals. Since the moisture permeability of the TFE is much less than that of the FEP, attempts were made to

  19. Genetics of Fiber Initiation

    Technology Transfer Automated Retrieval System (TEKTRAN)

    To study the cellular mechanisms involved in fiber initiation, three fiberless lines were crossed with wildtype and fuzzless seed cotton and the F1, F2 and BC1 progeny ratios are presently being evaluated. The three fiberless lines included: MD17 (N1N1n2n2), SL1-7-1 (N1N1fl1fl1n3n3) and XZ142w. XZ...

  20. Diode Pumped Fiber Laser.

    DTIC Science & Technology

    1987-08-01

    mounting fixture beeame soft and gradually come out of the fixture. S)me chemical reaction was takin- place between the epoxy and the dye solvent , which...loose. The solvent apparenlly did no)t affect the bonding agent used to attach the fibers inside the capillarie,. \\lthmigh individual capillarv tubes...pure solvent . was added to the cavity laser oscillation ceased, and was onlv re, ,t()red after readjuisting the orientation of the output coupler, as

  1. A solid-phase microextraction platinized stainless steel fiber coated with a multiwalled carbon nanotube-polyaniline nanocomposite film for the extraction of thymol and carvacrol in medicinal plants and honey.

    PubMed

    Ghiasvand, Alireza; Dowlatshah, Samira; Nouraei, Nadia; Heidari, Nahid; Yazdankhah, Fatemeh

    2015-08-07

    A mechanically hard and cohesive porous fiber, with large surface area, for more strong attachment of the coating was provided by platinizing a stainless steel wire. Then, the platinized stainless steel fiber was coated with a multiwalled carbon nanotube/polyaniline (MWCNT/PANI) nanocomposite using electrophoretic deposition (EPD) method and applied for the extraction of thymol and carvacrol with direct-immersion solid-phase microextraction (DI-SPME) method followed by high-performance liquid chromatography-ultraviolet detection (HPLC-UV) quantification. To provide a larger coarse surface for the tightened attachment of coating on the fiber, a stainless steel wire was platinized using a suitable optimized EPD method. Different experimental parameters were studied and the optimal conditions were obtained as: pH of the sample solution: 2; extraction time: 60min; salt content in the sample solution: 1% w/v NaNO3; desorption time: 60min; type and volume of the desorption solvent: acetonitrile, 100μL. Under the optimized conditions, limits of detection (LODs) were 0.6 and 0.8μgmL(-1) for thymol and carvacrol, respectively. Linear dynamic range (LDR) for the calibration curves of both analytes were 1-80μgmL(-1). Relative standard deviation (RSD%, n=6) was 6.8 for thymol and 12.7 for carvacrol. The proposed fiber was successfully applied for the recovery and determination of thymol and carvacrol in thyme, savory, and honey samples.

  2. Cardiovascular benefits of dietary fiber.

    PubMed

    Satija, Ambika; Hu, Frank B

    2012-12-01

    The relationship between dietary fiber and risk of cardiovascular disease (CVD) has been extensively studied. There is considerable epidemiological evidence indicating an inverse association between dietary fiber intake and CVD risk. The association has been found to be stronger for cereal fiber than for fruit or vegetable fiber, and several studies have also found increased whole grain consumption to be associated with CVD risk reduction. In light of this evidence, recent US dietary guidelines have endorsed increased consumption of fiber rich whole grains. Regular consumption of dietary fiber, particularly fiber from cereal sources, may improve CVD health through multiple mechanisms including lipid reduction, body weight regulation, improved glucose metabolism, blood pressure control, and reduction of chronic inflammation. Future research should focus on various food sources of fiber, including different types of whole grains, legumes, fruits, vegetables, and nuts, as well as resistant starch in relation to CVD risk and weight control; explore the biological mechanisms underlying the cardioprotective effect of fiber-rich diets; and study different ethnic groups and populations with varying sources of dietary fiber.

  3. 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.

    PubMed

    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

  4. Nematic droplets on fibers

    NASA Astrophysics Data System (ADS)

    Batista, V. M. O.; Silvestre, N. M.; Telo da Gama, M. M.

    2015-12-01

    The emergence of new techniques for the fabrication of nematic droplets with nontrivial topology provides new routes for the assembly of responsive devices. Here we explore some of the properties of nematic droplets on fibers, which constitute the basic units of a type of device that is able to respond to external stimuli, including the detection of gases. We perform a numerical study of spherical nematic droplets on fibers. We analyze the equilibrium textures for homogeneous and hybrid boundary conditions and find that in some cases the nematic avoids the nucleation of topological defects, which would provide a different optical response. We consider in detail a homeotropic nematic droplet wrapped around a fiber with planar anchoring. We investigate the effect of an electric field on the texture of this droplet. In the presence of a dc field, the system undergoes an orientational transition above a given threshold Ec, for which a ring defect is transformed into a figure-eight defect. We also consider ac fields, at high and low frequencies, and find that the textures are similar to those observed for static fields, in contrast with recently reported experiments.

  5. Applications of electrospun fibers.

    PubMed

    Lu, Ping; Ding, Bin

    2008-01-01

    The simplicity of the electrospinning fabrication process, the diversity of electrospinnable materials, and the unique features associated with electrospun fibers make this technique and resultant structures attractive for various applications. The past few years witnessed the significant progresses in the application areas of electrospun fibers, which were demonstrated by the numbers of the recent published patents on electrospinning. It is very apparent that the current focus has been shifted from studying the modification of the electrospinning conditions and apparatus for obtaining fibers with different sizes, shapes, morphologies, structures, alignments before 2000 to looking for the possible applications of these resultant nanofibers with broad functionalities after 2001. The current paper presents a systematic review on the recent applications of electrospun nanofibers in a broad range of fields including biomedical applications such as drug delivery, tissue engineering, wound dressing and cosmetics, functional materials and devices such as composite reinforcement, filters, protective clothing and smart textiles, and energy and electronics such as batteries/cells and capacitors, sensors and catalysts. Although some of these applications may be still remained in the laboratory in the current stage, plenty of successful examples have proved that electrospun nanofibers have a bright future in a variety of industries.

  6. Fiber pixelated image database

    NASA Astrophysics Data System (ADS)

    Shinde, Anant; Perinchery, Sandeep Menon; Matham, Murukeshan Vadakke

    2016-08-01

    Imaging of physically inaccessible parts of the body such as the colon at micron-level resolution is highly important in diagnostic medical imaging. Though flexible endoscopes based on the imaging fiber bundle are used for such diagnostic procedures, their inherent honeycomb-like structure creates fiber pixelation effects. This impedes the observer from perceiving the information from an image captured and hinders the direct use of image processing and machine intelligence techniques on the recorded signal. Significant efforts have been made by researchers in the recent past in the development and implementation of pixelation removal techniques. However, researchers have often used their own set of images without making source data available which subdued their usage and adaptability universally. A database of pixelated images is the current requirement to meet the growing diagnostic needs in the healthcare arena. An innovative fiber pixelated image database is presented, which consists of pixelated images that are synthetically generated and experimentally acquired. Sample space encompasses test patterns of different scales, sizes, and shapes. It is envisaged that this proposed database will alleviate the current limitations associated with relevant research and development and would be of great help for researchers working on comb structure removal algorithms.

  7. Optical fiber networks for remote fiber optic sensors.

    PubMed

    Fernandez-Vallejo, Montserrat; Lopez-Amo, Manuel

    2012-01-01

    This paper presents an overview of optical fiber sensor networks for remote sensing. Firstly, the state of the art of remote fiber sensor systems has been considered. We have summarized the great evolution of these systems in recent years; this progress confirms that fiber-optic remote sensing is a promising technology with a wide field of practical applications. Afterwards, the most representative remote fiber-optic sensor systems are briefly explained, discussing their schemes, challenges, pros and cons. Finally, a synopsis of the main factors to take into consideration in the design of a remote sensor system is gathered.

  8. Optical Fiber Networks for Remote Fiber Optic Sensors

    PubMed Central

    Fernandez-Vallejo, Montserrat; Lopez-Amo, Manuel

    2012-01-01

    This paper presents an overview of optical fiber sensor networks for remote sensing. Firstly, the state of the art of remote fiber sensor systems has been considered. We have summarized the great evolution of these systems in recent years; this progress confirms that fiber-optic remote sensing is a promising technology with a wide field of practical applications. Afterwards, the most representative remote fiber-optic sensor systems are briefly explained, discussing their schemes, challenges, pros and cons. Finally, a synopsis of the main factors to take into consideration in the design of a remote sensor system is gathered. PMID:22666011

  9. FIBER ORIENTATION IN INJECTION MOLDED LONG CARBON FIBER THERMOPLASTIC COMPOSITES

    SciTech Connect

    Wang, Jin; Nguyen, Ba Nghiep; Mathur, Raj N.; Sharma, Bhisham; Sangid, Michael D.; Costa, Franco; Jin, Xiaoshi; Tucker III, Charles L.; Fifield, Leonard S.

    2015-03-23

    A set of edge-gated and center-gated plaques were injection molded with long carbon fiber-reinforced thermoplastic composites, and the fiber orientation was measured at different locations of the plaques. Autodesk Simulation Moldflow Insight (ASMI) software was used to simulate the injection molding of these plaques and to predict the fiber orientation, using the anisotropic rotary diffusion and the reduced strain closure models. The phenomenological parameters of the orientation models were carefully identified by fitting to the measured orientation data. The fiber orientation predictions show very good agreement with the experimental data.

  10. Preparation and evaluation of solid-phase microextraction fibers based on monolithic molecularly imprinted polymers for selective extraction of diacetylmorphine and analogous compounds.

    PubMed

    Djozan, Djavanshir; Baheri, Tahmineh

    2007-09-28

    All of the studies on solid-phase microextraction based on molecularly imprinted polymers up to now have been carried out on the synthesis of the polymer on the surface of the fiber which is brittle and the polymer coating strips during handling. The objective of this study was to develop a method for fabrication of a monolithic and robust solid-phase microextraction fiber on the basis of molecularly imprinted polymer for selective extraction of diacetylmorphine and its structural analogues followed by their GC or GC/MS analysis. A fiber was produced by copolymerization of methacrylic acid-ethylene glycol dimethacrylate imprinted with diacetylmorphine. The effective factors influencing the polymerization have been investigated and are detailed here. Also, the influences of pH, extraction time and temperature on the extraction efficiency of analytes were investigated. The prepared fiber was thermally stable up to 300 degrees C which has vital importance in SPME coupled with GC or GC/MS. The adsorption isotherm modeling was performed by fitting the data of studied compounds to bi-Langmuir isotherm model. The evaluated equilibrium constants for diacetylmorphine were 0.011 and 1824.72 microM(-1), and the number of binding sites was 170.37 and 4.64 nmolg(-1), respectively. This fiber was successfully used for extraction of template molecule from aqueous solution and further analysis with GC or GC/MS. The high extraction efficiency was obtained for diacetylmorphine, 6-monoacetylcodeine, and 6-monoacetylmorphine, yielding the detection limits of 300, 47, and 1 ngmL(-1), respectively.

  11. Optical fiber grating tuning device and application

    NASA Astrophysics Data System (ADS)

    Luo, Fei; Yeh, T.

    2008-12-01

    A new design for tuning optical fiber grating is proposed. The fiber grating is placed in the grooves between a pair of slides, in which one end of the fiber is bonded on the bottom slide, and the other end of the fiber is bonded on the top slide, the grating section of the fiber is confined in grooves, so that the fiber grating is remaining straight without buckling during axial compressive force applied to the fiber. An actuator is used for driving slide to apply force on fiber to axially compress or stretch the fiber grating. The wavelength of the fiber grating is tuned according to applied stress on the fiber. The applications of the device include tunable fiber laser, tunable fiber filter etc.

  12. Drop impact on a fiber

    NASA Astrophysics Data System (ADS)

    Kim, Sung-Gil; Kim, Wonjung

    2016-04-01

    We present the results of a combined experimental and theoretical investigation of drop impact on a thin fiber. Using high-speed videography, we analyze the dynamics of droplet collision with a fiber. Based on the systematic experiments, we identify three outcomes of collision: capturing, single drop falling, and splitting. The outcomes are presented in a regime map, where the regime boundaries are explained through a scale analysis of forces. We also measure the liquid retention on the fiber after the droplet impact. By considering a liquid film on the fiber, we develop a mechanical model that predicts the residual water mass. Our model reveals that the residual mass depends critically on the fiber thickness and less on the impact speed. Our study can be extended to predicting the remaining droplet, critical problems in air filtration, water collection, and fiber coating.

  13. Direct spinning of fiber supercapacitor

    NASA Astrophysics Data System (ADS)

    Xu, Tong; Ding, Xiaoteng; Liang, Yuan; Zhao, Yang; Chen, Nan; Qu, Liangti

    2016-06-01

    A direct wet spinning approach is demonstrated for facile and continuous fabrication of a whole fiber supercapacitor using a microfluidic spinneret. The resulting fiber supercapacitor shows good electrochemical properties and possesses high flexibility and mechanical stability. This strategy paves the way for large-scale continuous production of fiber supercapacitors for weavable electronics.A direct wet spinning approach is demonstrated for facile and continuous fabrication of a whole fiber supercapacitor using a microfluidic spinneret. The resulting fiber supercapacitor shows good electrochemical properties and possesses high flexibility and mechanical stability. This strategy paves the way for large-scale continuous production of fiber supercapacitors for weavable electronics. Electronic supplementary information (ESI) available: Design of the microfluidic spinneret and operation of the spinneret (movie). See DOI: 10.1039/c6nr03116a

  14. Impact resistance of fiber composites

    NASA Technical Reports Server (NTRS)

    Chamis, C. C.; Sinclair, J. H.

    1982-01-01

    Stress-strain curves are obtained for a variety of glass fiber and carbon fiber reinforced plastics in dynamic tension, over the stress-strain range of 0.00087-2070/sec. The test method is of the one-bar block-to-bar type, using a rotating disk or a pendulum as the loading apparatus and yielding accurate stress-strain curves up to the breaking strain. In the case of glass fiber reinforced plastic, the tensile strength, strain to peak impact stress, total strain and total absorbed energy all increase significantly as the strain rate increases. By contrast, carbon fiber reinforced plastics show lower rates of increase with strain rate. It is recommended that hybrid composites incorporating the high strength and rigidity of carbon fiber reinforced plastic with the high impact absorption of glass fiber reinforced plastics be developed for use in structures subjected to impact loading.

  15. Fiber Laser Development for LISA

    NASA Technical Reports Server (NTRS)

    Numata, Kenji; Chen, Jeffrey R.

    2009-01-01

    We have developed a linearly-polarized Ytterbium-doped fiber ring laser with single longitudinal-mode output at 1064nm for LISA and other space applications. Single longitudinal-mode selection was achieved by using a fiber Bragg grating (FBG) and a fiber Fabry-Perot (FFP). The FFP also serves as a frequency-reference within our ring laser. Our laser exhibits comparable low frequency and intensity noise to Non-Planar Ring Oscillator (NPRO). By using a fiber-coupled phase modulator as a frequency actuator, the laser frequency can be electro-optically tuned at a rate of 100kHz. It appears that our fiber ring laser is promising for space applications where robustness of fiber optics is desirable.

  16. Selenium semiconductor core optical fibers

    SciTech Connect

    Tang, G. W.; Qian, Q. Peng, K. L.; Wen, X.; Zhou, G. X.; Sun, M.; Chen, X. D.; Yang, Z. M.

    2015-02-15

    Phosphate glass-clad optical fibers containing selenium (Se) semiconductor core were fabricated using a molten core method. The cores were found to be amorphous as evidenced by X-ray diffraction and corroborated by Micro-Raman spectrum. Elemental analysis across the core/clad interface suggests that there is some diffusion of about 3 wt % oxygen in the core region. Phosphate glass-clad crystalline selenium core optical fibers were obtained by a postdrawing annealing process. A two-cm-long crystalline selenium semiconductor core optical fibers, electrically contacted to external circuitry through the fiber end facets, exhibit a three times change in conductivity between dark and illuminated states. Such crystalline selenium semiconductor core optical fibers have promising utility in optical switch and photoconductivity of optical fiber array.

  17. Fiber optic sensor and method for making

    DOEpatents

    Vartuli, James Scott; Bousman, Kenneth Sherwood; Deng, Kung-Li; McEvoy, Kevin Paul; Xia, Hua

    2010-05-18

    A fiber optic sensor including a fiber having a modified surface integral with the fiber wherein the modified surface includes an open pore network with optical agents dispersed within the open pores of the open pore network. Methods for preparing the fiber optic sensor are also provided. The fiber optic sensors can withstand high temperatures and harsh environments.

  18. Low-Bending-Loss Single-Mode Fibers for Fiber-to-the-Home

    NASA Astrophysics Data System (ADS)

    Himeno, Kuniharu; Matsuo, Shoichiro; Guan, Ning; Wada, Akira

    2005-11-01

    Recent progress on low-bending-loss single-mode optical fibers for fiber-to-the-home (FTTH) is reviewed. Designing and manufacturing for three types of fibers-a step-index-profile fiber, a trench-index-profile fiber, and a holey fiber-are discussed. The trench-index-profile fibers and the holey fibers are confirmed to be candidates for indoor wiring because of their low bending losses, as well as splice losses.

  19. System for testing optical fibers

    DOEpatents

    Golob, John E. [Olathe, KS; Looney, Larry D. [Los Alamos, NM; Lyons, Peter B. [Los Alamos, NM; Nelson, Melvin A. [Santa Barbara, CA; Davies, Terence J. [Santa Barbara, CA

    1980-07-15

    A system for measuring a combination of optical transmission properties of fiber optic waveguides. A polarized light pulse probe is injected into one end of the optical fiber. Reflections from discontinuities within the fiber are unpolarized whereas reflections of the probe pulse incident to its injection remain polarized. The polarized reflections are prevented from reaching a light detector whereas reflections from the discontinuities reaches the detector.

  20. System for testing optical fibers

    DOEpatents

    Golob, J.E.; Looney, L.D.; Lyons, P.B.; Nelson, M.A.; Davies, T.J.

    1980-07-15

    A system for measuring a combination of optical transmission properties of fiber optic waveguides. A polarized light pulse probe is injected into one end of the optical fiber. Reflections from discontinuities within the fiber are unpolarized whereas reflections of the probe pulse incident to its injection remain polarized. The polarized reflections are prevented from reaching a light detector whereas reflections from the discontinuities reaches the detector. 2 figs.

  1. Fiber-matrix interface failures

    NASA Technical Reports Server (NTRS)

    Rabenberg, Lew; Marcus, Harris L.; Park, Hun Sub; Zong, Gui Sheng; Brown, Lloyd D.

    1989-01-01

    Interface fractures of aluminum-graphite composites under transverse loading are expected to occur within the graphite fibers, but very near the interface. Residual stresses in aluminum, reinforced with the new high modulus pitch-based fibers, are much lower than would be expected based on simple elasticity calculations. The excess stress may be relaxed by shearing internal to the fibers or at the interface rather than by plastic flow of the matrix. The internal shearing also occurs during repeated thermal cycling of these composites; the fibers are repeatedly intruded, then extruded, during repeated temperature excursions.

  2. Electrospinning of semicrystalline polymer fibers

    NASA Astrophysics Data System (ADS)

    Liu, Ying; Chen, Shuang; Li, Chunhua; Dimasi, Elaine; Marom, Gad; Rafailovich, Miriam

    2009-03-01

    Electrospinning of polymeric fibers has been attracted increased interest in recent years. However, the research for ethylene-vinyl acetate (EVA) and linear polyethylene (PE) is still limited, due to their relatively poor solubility in conventional solvent systems at ambient temperature. In this study, EVA and PE fibers were electrospun with different fiber diameter when the electrospinning solution was kept at a temperature greater than that of the solidification temperature of the polymer solutions. The effects of the fiber physical dimension to its crystallization and mechanical properties were thus detected. The morphology of the fibers was measured by scanning electron microscope (SEM) and atomic force microscope (AFM). The shear modulation force microscopy technique (SMFM) was used to measure the melting point, Tm, which was found to increase with increased fiber diameter and crystallinity. AFM three-point bending test demonstrated that the Young's modulus of the fibers drastically increased as fiber diameter decreased.Grazing-incidence small angle x-ray scattering (GISAX) showed that, compared to the bulk material, the crystallinity of the electrospun fibers had been changed.

  3. Short-fiber-reinforced thermoplastics

    SciTech Connect

    Tekkanat, B.

    1987-01-01

    One of the objectives of this study was to explore the simplest predictive theories for composite stiffness and strength in injection-molded SFRTP materials which would be easy to use and would be accurate over a wide range of materials. The intention was also to try to understand the predicted dependence of stiffness and strength on fiber length for SFRTP's. The effects of matrix ductility on the mechanical properties and failure mechanisms of SFRTP's were investigated by controlling the matrix ductility via composition in PS-PPO system. In addition to matrix ductility, consideration was given to the following parameters: fiber-length distribution (FLD), fiber-orientation distribution (FOD), fiber-volume fraction, aspect ratio, and fiber-end configuration to understand the role they play on the mechanical properties, efficiency of reinforcement, and failure mechanisms of SFRTP's. Sub-surface analysis by transmission optical microscopy under polarized light was utilized along with fracture surface analysis and found to be a useful technique in determining the detailed microdeformation mechanisms of both matrix and short-fiber-reinforced systems. Fiber-reinforcement efficiency in terms of both stiffness and strength was found to be strongly dependent on the fiber length and fiber-volume fraction.

  4. Optical fiber dispersion characterization study

    NASA Technical Reports Server (NTRS)

    Geeslin, A.; Arriad, A.; Riad, S. M.; Padgett, M. E.

    1979-01-01

    The theory, design, and results of optical fiber pulse dispersion measurements are considered. Both the hardware and software required to perform this type of measurement are described. Hardware includes a thermoelectrically cooled injection laser diode source, an 800 GHz gain bandwidth produce avalanche photodiode and an input mode scrambler. Software for a HP 9825 computer includes fast Fourier transform, inverse Fourier transform, and optimal compensation deconvolution. Test set construction details are also included. Test results include data collected on a 1 Km fiber, a 4 Km fiber, a fused spliced, eight 600 meter length fibers concatenated to form 4.8 Km, and up to nine optical connectors.

  5. Health benefits of prebiotic fibers.

    PubMed

    Meyer, Diederick

    2015-01-01

    This chapter describes the various compounds that can act as prebiotic fibers: their structure, occurrence, production, and physiological effects (health effects) will be presented. The basis for the description is the latest definitions for dietary fibers and for prebiotics. Using as much as possible data from human studies, both the fiber and the prebiotic properties will be described of a variety of compounds. Based on the presented data the latest developments in the area of prebiotics, fibers and gut and immune health will be discussed in more detail as they show best what the potential impact of prebiotics on health of the human host might be.

  6. In-fiber integrated accelerometer.

    PubMed

    Peng, Feng; Yang, Jun; Li, Xingliang; Yuan, Yonggui; Wu, Bing; Zhou, Ai; Yuan, Libo

    2011-06-01

    A compact in-fiber integrated fiber-optic Michelson interferometer based accelerometer is proposed and investigated. In the system, the sensing element consists of a twin-core fiber acting as a bending simple supported beam. By demodulating the optical phase shift, we obtain that the acceleration is proportional to the force applied on the central position of the twin-core fiber. A simple model has been established to calculate the sensitivity and resonant frequency. The experimental results show that such an accelerometer has a sensitivity of 0.09 rad/g at the resonant frequency of 680 Hz.

  7. Compression Testing of Carbon Fibers

    DTIC Science & Technology

    1989-11-01

    ksi (2205 MPa) (17:217). The cross section texture of pitch fibers will vary depending on the spinning process. Some fibers exhibit a radial texture...while others exhibit onion skin or random textures. Radial TeAture Onion-Skin iexture Ranom Texiure Figure 3 Textures of Pitch Fibers Reprinted From (17...18 JUL 89 iST Fiber (tension to compresion ) 300 200 -00 200 T- ]-- r -F _ -1 OOE-02 -2 0OE-] ,nnE r -6 OOE-03 2 20E -0 1, ME 02 STRAIN Figure 50

  8. Capillary stretching of elastic fibers

    NASA Astrophysics Data System (ADS)

    Protiere, Suzie; Stone, Howard A.; Duprat, Camille

    2014-11-01

    Fibrous media consisting of constrained flexible fibers can be found in many engineered systems (membranes in filters, woven textile, matted paper). When such materials interact with a liquid, the presence of liquid/air interfaces induces capillary forces that deform the fibers. To model this interaction we study the behaviour of a finite volume of liquid deposited on two parallel flexible fibers clamped at both ends. A tension along the fibers is imposed and may be varied. We show that the system undergoes various morphological changes as the interfiber distance, the elasticity and the tension of the fibers are varied. For a certain range of parameters, the liquid spreads along the fibers and pulls them together, leading to the ``zipping'' of the fibers. This capillary adhesion can then be enhanced or reduced by changing the tension within the fibers. We will show that balancing stretching and capillary forces allows the prediction of this transition as well as the conditions for which detachment of the fibers occurs. These results may be used to prevent the clogging of fibrous membranes or to optimize the capture of liquids.

  9. Preparation of silicon carbide fibers

    DOEpatents

    Wei, G.C.

    1983-10-12

    Silicon carbide fibers suitable for use in the fabrication of dense, high-strength, high-toughness SiC composites or as thermal insulating materials in oxidizing environments are fabricated by a new, simplified method wherein a mixture of short-length rayon fibers and colloidal silica is homogenized in a water slurry. Water is removed from the mixture by drying in air at 120/sup 0/C and the fibers are carbonized by (pyrolysis) heating the mixture to 800 to 1000/sup 0/C in argon. The mixture is subsequently reacted at 1550 to 1900/sup 0/C in argon to yield pure ..beta..-SiC fibers.

  10. Surface-core fiber gratings

    NASA Astrophysics Data System (ADS)

    Osório, Jonas H.; Oliveira, Ricardo; Mosquera, L.; Franco, Marcos A. R.; Heidarialamdarloo, Jamshid; Bilro, Lúcia; Nogueira, Rogério N.; Cordeiro, Cristiano M. B.

    2015-09-01

    In this paper, we report, to our knowledge, the first demonstration of the induction of long-period and Bragg gratings on surface-core optical fibers. Surface-core fibers described herein were fabricated from commercial silica tubes and germanium-doped silica rods by employing a very simple procedure. Being the core on the fiber surface, it can be sensitive to refractive index variations in the environment in which the fiber is immersed. Thus, results concerning the sensitivity of these gratings to environmental refractive index variations are presented. Besides, simulation data are presented for comparison to the experimental behavior and for projecting future steps in this research.

  11. 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.

    PubMed

    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).

  12. Influence of harvest maturity and fruit logistics on pineapple (Ananas comosus [L.] Merr.) volatiles assessed by headspace solid phase microextraction and gas chromatography-mass spectrometry (HS-SPME-GC/MS).

    PubMed

    Steingass, Christof B; Grauwet, Tara; Carle, Reinhold

    2014-05-01

    Profiling of volatiles from pineapple fruits was performed at four ripening stages using headspace solid-phase microextraction and gas chromatography-mass spectrometry (HS-SPME-GC/MS). In total, 142 volatiles were detected, of which 132 were identified. Multivariate data analysis was carried out to assess the effect of post-harvest storage on volatiles composition of green-ripe sea-freighted pineapple in comparison to air-freighted fruits harvested at full maturity. The latter fruits were characterised by volatiles described as potent odorants in pineapples, such as δ-octalactone, γ-lactones, 1-(E,Z)-3,5-undecatriene and 1,3,5,8-undecatetraene, as well as various methyl esters. In contrast, post-harvest storage of green-ripe sea-freighted fruits resulted in an increased formation of ethyl esters, acetates, acetoxy esters and alcohols, thus allowing the authentication of sea- and air-freighted pineapples, respectively. Particularly, compounds presumably derived from methyl-branched amino acid catabolism were identified in the fruits at later post-harvest stages. In addition, physicochemical traits were determined to characterise the fruit maturity stages.

  13. Correlation between emitted and total amount of 2-cyclopentyl-cyclopentanone in polyamide 6.6 allows rapid assessment by HS and HS-SPME under non-equilibrium conditions.

    PubMed

    Gröning, Mikael; Hakkarainen, Minna

    2004-10-15

    A correlation was found between the emitted and total amount of 2-cyclopentyl-cyclopentanone in polyamide 6.6. The emitted amounts were measured by GC-MS after headspace (HS) or headspace solid-phase microextraction (HS-SPME) and the total content was determined after microwave-assisted extraction (MAE). The correlation was valid also under non-equilibrium conditions, which allows rapid assessment of 2-cyclopentyl-cyclopentanone content in polyamide 6.6 by headspace techniques. The incubation time needed for non-equilibrium headspace analysis could be reduced from 5 h to 45 min if the PA66 granules were milled to powder prior to extraction. However, to reach equilibrium between the analyte in the solid sample and the headspace still required 12 h of incubation at 80 degrees C. The long incubation time is explained by slow diffusion rate due to the strong hydrogen bonding between analyte and matrix and the relatively high crystallinity of polyamide 6.6. The headspace extraction profile showed several equilibrium-like patterns that are easily mistaken for the real equilibrium.

  14. Advanced fiber lasers and related all-fiber devices

    NASA Astrophysics Data System (ADS)

    Srinivasan, Balaji

    2000-11-01

    Fiber lasers based on rare-earth ions now play an important role in several applications ranging from communications and surgery to spectroscopic sensing because of their efficiency and compactness, and their intrinsic compatibility with single mode communication fibers. As such, there is a strong need to investigate key issues related to the design and fabrication of ``rugged'' state-of-the-art fiber lasers, and in particular to fabricate versatile high-performance fiber lasers based on ``all-fiber'' devices, i.e. using only in-fiber devices. This dissertation addresses some of these needs. One such issue is the polarization property of lasers and amplifiers based on polarization preserving fibers. A dedicated study of the polarization properties of amplifiers and lasers based on rare-earth doped elliptical core fibers has been performed. The results indicate a polarization dependent gain, with a larger gain at the polarization parallel to the major axis of the ellipse. This gain anisotropy is attributed to the differences in the confinement of the two orthogonally polarized fundamental modes of the fiber. Another issue that has been driven by several medical, sensing, and data storage applications is that of efficient laser transitions in the mid-infrared and visible spectral regions. Such lasers are difficult to achieve in conventional fibers based on silica glass hosts due to their relatively large phonon energies. A fluoride based glass host (ZBLAN) with low phonon energy was chosen to enable green and blue laser transitions using upconversion schemes in erbium and thulium respectively, and realize an efficient mid-infrared transition in erbium. Specifically, the following results have been demonstrated: (1)Green (544 nm) fiber laser with the highest combination of power (50 mW) and efficiency (37%) in Er:ZBLAN; (2)Novel Raman fiber laser-pumped 22 mW blue (490 nm) laser in Tm:ZBLAN; (3)Diode-pumped mid-infrared (2.7 μm) laser with 660 mW output in Er

  15. Graphene oxide-silica composite coating hollow fiber solid phase microextraction online coupled with inductively coupled plasma mass spectrometry for the determination of trace heavy metals in environmental water samples.

    PubMed

    Su, Shaowei; Chen, Beibei; He, Man; Hu, Bin

    2014-06-01

    In this work, a novel graphene oxide-silica (GO-silica) composite coating was prepared for hollow fiber solid phase microextraction (HF-SPME) of trace Mn, Co, Ni, Cu, Cd and Pb followed by on-line inductively coupled plasma mass spectrometry (ICP-MS) detection. The structure of the prepared graphene oxide and GO-silica composite was studied and elucidated by atomic force microscopy (AFM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR) and X-ray photoelectron spectroscopy (XPS). The GO-silica composite coated hollow fiber was characterized by scanning electron microscope (SEM), and the results show that the GO-silica composite coating possessed a homogeneous and wrinkled structure. Various experimental parameters affecting the extraction of the target metal ions by GO-silica composite coated HF-SPME have been investigated carefully. Under the optimum conditions, the limits of detection (LODs, 3σ) for Mn, Co, Ni, Cu, Cd and Pb were 7.5, 0.39, 20, 23, 6.7 and 28 ng L(-1) and the relative standard deviations (RSDs, c(Mn, Co, Cd)=0.05 μg L(-1), c(Ni, Cu, Pb)=0.2 μg L(-1), n=7) were 7.2, 7.0, 5.6, 7.3, 7.8 and 4.6%, respectively. The accuracy of the proposed method was validated by the analysis of Certified Reference Material of GSBZ 50009-88 environmental water and the determined values were in a good agreement with the certified values. The proposed method has been successfully applied for the determination of trace metals in real environmental water samples with recoveries ranging from 85 to 119%.

  16. Fiber sample presentation system for spectrophotometer cotton fiber color measurements

    Technology Transfer Automated Retrieval System (TEKTRAN)

    The Uster® High Volume Instrument (HVI) is used to class U.S. cotton for fiber color, yielding the industry accepted, cotton-specific color parameters Rd and +b. The HVI examines a 9 square inch fiber sample, and it is also used to test large AMS standard cotton “biscuits” or rectangles. Much inte...

  17. Experiments on room temperature optical fiber-fiber direct bonding

    NASA Astrophysics Data System (ADS)

    Hao, Jinping; Yan, Ping; Xiao, Qirong; Wang, Yaping; Gong, Mali

    2012-08-01

    High quality permanent connection between optical fibers is a significant issue in optics and communication. Studies on room temperature optical large diameter fiber-fiber direct bonding, which is essentially surface interactions of glass material, are presented here. Bonded fiber pairs are obtained for the first time through the bonding technics illustrated here. Two different kinds of bonding technics are provided-fresh surface (freshly grinded and polished) bonding and hydrophobic surface (activated by H2SO4 and HF) bonding. By means of fresh surface bonding, a bonded fiber pair with light transmitting efficiency of 98.1% and bond strength of 21.2 N is obtained. Besides, in the bonding process, chemical surface treatment of fibers' end surfaces is an important step. Therefore, various ways of surface treatment are analyzed and compared, based on atomic force microscopy force curves of differently disposed surfaces. According to the comparison, fresh surfaces are suggested as the prior choice in room temperature optical fiber-fiber bonding, owing to their larger adhesive force, attractive force, attractive distance, and adhesive range.

  18. Compact fiber optic immunosensor using tapered fibers and acoustic enhancement

    NASA Astrophysics Data System (ADS)

    Zhou, Chonghua; Pivarnik, Philip E.; Auger, Steven; Rand, Arthur G.; Letcher, Stephen V.

    1997-06-01

    A compact fiber-optic sensing system that features all-fiber optical design and semiconductor-laser excitation has been developed and tested. A 2X2 fiber coupler directs the input light to the SMA connected sensing fiber tip and the fluorescent signal back to a CCD fiber spectrophotometer. In this system, the fluorescent signal is confined in the fiber system so the signal-to-noise ratio is greatly improved and the system can be operate in ambient light conditions. The utilization of a red laser diode has reduced the background signal of non-essential biomolecules. The fluorescent dye used is Cy5, which has an excitation wavelength of 650 nm and a fluorescent center wavelength of 680 nm. To illustrate the biosensor's diagnostic capabilities, a sandwich immunoassay to detect Salmonella is presented. Tapered fiber tips with different shapes and treatments were studied and optimized. An enhancement system employing ultrasonic concentration of target particles has also been developed and applied to the detection of Salmonella. The immunoassay was conducted in a test chamber that also serves as an ultrasonic standing-wave cell and allows microspheres to be concentrated in a column along the fiber probe. The system demonstrates broad promise in future biomedical application.

  19. BN Bonded BN fiber article from boric oxide fiber

    DOEpatents

    Hamilton, Robert S.

    1978-12-19

    A boron nitride bonded boron nitride fiber article and the method for its manufacture which comprises forming a shaped article with a composition comprising boron oxide fibers and boric acid, heating the composition in an anhydrous gas to a temperature above the melting point of the boric acid and nitriding the resulting article in ammonia gas.

  20. Environmental and biological determination of acrolein using new cold fiber solid phase microextraction with gas chromatography mass spectrometry.

    PubMed

    Dias, Cláudia M; Menezes, Helvécio C; Cardeal, Zenilda L

    2017-04-01

    Acrolein is a pollutant released daily to the indoor environment from different sources. The present study reports the development of a simple and sensitive cold fiber solid phase microextraction sampling method for the determination of acrolein in exhaled air and indoor air by gas chromatography mass spectrometry. O-(2,3,4,5,6-pentafluorobenzyl) hydroxylamine was used as derivatizing agent supported on a 65-μm polydimethylsiloxane-divinylbenzene SPME fiber. An acrolein permeation tube at 326.25 ng min(-1) rate was used to generate gaseous standards. The method shows good results for main validation parameters. The limits of detection and quantification were 2.88 and 5.08 μg m(-3), respectively, for indoor analysis; and 2.40 and 3.79 μg m(-3), respectively, for exhaled air analysis. The precision showed standard deviation ranges from 6.00 to 8.00% for intra-assay analyses and from 8.00 to 10.00% for inter-assay analyses. After optimizing the conditions, analyses of real samples were performed on indoor environments contaminated by cigarette smoke, or heated oil, including pastry shops, restaurants, churros stands, and closed parking cars located in the city of Belo Horizonte, Brazil. Acrolein breaths of exposed people were also determined. A good Pearson correlation coefficient (r = 0.901) was observed between the concentration of acrolein in indoor air and exhaled air, allowing to propose acrolein breath as environmental exposure biomarker. Graphical Abstract Cold fiber solid phase microextraction gas chromatography/mass spectrometry.