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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. Validation of an SPME method, using PDMS, PA, PDMS-DVB, and CW-DVB SPME fiber coatings, for analysis of organophosphorus insecticides in natural waters.

    PubMed

    Lambropoulou, D A; Sakkas, V A; Albanis, T A

    2002-11-01

    Solid-phase microextraction (SPME) has been optimized and applied to the determination of the organophosphorus insecticides diazinon, dichlofenthion, parathion methyl, malathion, fenitrothion, fenthion, parathion ethyl, bromophos methyl, bromophos ethyl, and ethion in natural waters. Four types of SPME fiber coated with different stationary phases (PDMS, PA, PDMS-DVB, and CW-DVB) were used to examine their extraction efficiencies for the compounds tested. Conditions that might affect the SPME procedure, such as extraction time and salt content, were investigated to determine the analytical performance of these fiber coatings for organophosphorus insecticides. The optimized procedure was applied to natural waters - tap, sea, river, and lake water - spiked in the concentration range 0.5 to 50 micro g L(-1) to obtain the analytical characteristics. Recoveries were relatively high - >80% for all types of aqueous sample matrix - and the calibration plots were reproducible and linear (R(2)>0.982) for all analytes with all the fibers tested. The limits of detection ranged from 2 to 90 ng L(-1), depending on the detector and the compound investigated, with relative standard deviations in the range 3-15% at all the concentration levels tested. The SPME partition coefficients (K(f)) of the organophosphorus insecticides were calculated experimentally for all the polymer coatings. The effect of organic matter such as humic acids on extraction efficiency was also studied. The analytical performance of the SPME procedure using all the fibers in the tested natural waters proved effective for the compounds.

  4. 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.

  5. Fibers with polypyrrole and polythiophene phases for isolation and determination of adrenolytic drugs from human plasma by SPME-HPLC.

    PubMed

    Olszowy, Pawel; Szultka, Malgorzata; Ligor, Tomasz; Nowaczyk, Jacek; Buszewski, Boguslaw

    2010-08-15

    In this study, polypyrrole (PPy) and polythiophene (PTh) SPME coatings and their ability to extract selected adrenolytic drugs with different physico-chemical properties from standard solutions and human plasma samples were evaluated. In measurements metoprolol, oxprenolol, mexiletine, propranolol, and propaphenon were investigated. The main parameters such as extraction time, desorption conditions and pH influence were examined. Inter-day precisions were in range 0.1-2.0%, 1.1-2.9%, 1.3-2.6%, 0.1-2.6% and 0.3-2.1% for metoprolol, oxprenolol, mexiletine, propranolol and propaphenon, respectively. Accuracies were less than 15%, which was evaluated by analyzing preparation samples of five replicates. The method was successfully applied to human plasma samples spiked with selected adrenolytic drugs. The method was linear in the concentration range from 1 to 10microg/ml for all of studied adrenolytic drugs using human plasma samples. The PTh-SPME coating displayed higher extraction efficiency towards the target analytes in comparison to PPy-SPME. The reproducibility of the extraction using polypyrrole and polythiophene fibers was confirmed by variation coefficients lower than 8% and 3%, respectively. PMID:20643589

  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. PMID:23259687

  7. Influence of the type of fiber coating and extraction time on foal dry-cured loin volatile compounds extracted by solid-phase microextraction (SPME).

    PubMed

    Lorenzo, José M

    2014-01-01

    Extraction of dry-cured loin volatile compounds by solid-phase microextraction (SPME) was optimized. Two different fiber coatings: carboxen/polydimethylsiloxane (CAR/PDMS) and divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS), and three extraction times (15, 30 and 45 min) were assayed. Between the fibers tested, CAR/PDMS coated fibers extracted between two and three times more total amount of volatile compounds than the DVD/CAR/PDMS coating (1314×10(6) vs. 526×10(6) area units). Fifty five compounds were extracted by the CAR/PDMS fiber, while only 48 of these were found with the DVB/CAR/PDMS fiber. On the other hand, 6 additional volatile compounds were extracted by the CAR/PDMS coating, all of them being of low molecular weight. Three of the major compounds extracted, hexanoic acid, methyl ester; butanoic acid, 3-methyl-, methyl ester and hexanal, were found in high proportion in both fiber coatings. The effect of exposure time was more marked for the DVD/CAR/PDMS fiber than for the CAR/PDMS coating. Fifteen minutes of extraction provided a volatile compounds profile with lower area counts for most compounds and significantly different to that obtained with 30 and 45 min of extraction. The extraction yields of dry-cured loin volatile compounds varied according to the fiber coating used and the time of exposure. Therefore, extraction conditions should be selected depending on the objective of the study. Finally, it can be concluded that both porous fibers tested, CAR/PDMS and DVB/CAR/PDMS, provide a similar volatile compounds profile for dry-cured foal loin.

  8. 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

  9. Development of SPME-HPLC methodology for detection of nitroexplosives

    NASA Astrophysics Data System (ADS)

    Peña-Luengas, Sandra L.; Jerez-Rozo, Jackeline I.; Correa, Sandra N.; Peña, Nelson E.; Hernández-Rivera, Samuel P.

    2007-04-01

    Solid phase microextraction (SPME) has been coupled with liquid chromatography to widen its range of application to nonvolatile and thermally unstable compounds, generally limited for SPME-GC. A method for analysis of nitroaromatic explosives and its degradations products was developed by coupling SPME and high performance liquid chromatography with ultraviolet detection (HPLC/UV), introducing a modified interface that ensure accuracy, precision, repeatability, high efficiency, unique selectivity and high sensitive to detection and quantification of explosives from surface soil samples and increased chromatographic efficiency. A pretreatment step was introduced for the soil samples which extracted the target compounds into an aqueous phase. Several parameters that affect the microextraction were evaluated, such as: fiber coating, adsorption and desorption time and stirring rate. The effect of salting out (NaCl) on analyte extraction and the role of various solvents on SPME fiber were also evaluated. Carbowax-templated resin (CW/TPR) and Polydimethilsiloxane-divinilbenzene (PDMS-DVB) fibers were used to extract the analytes from the aqueous samples. Explosives were detected at low μg/mL concentrations. This study demonstrates that SPME-HPLC is a very promising method of analysis of explosives from aqueous samples and has been successfully applied to the determination of nitroaromatic compounds, such as TNT.

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

    PubMed

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

    2009-02-01

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

  11. Determination of methyltin compounds in urine of occupationally exposed and general population by in situ ethylation and headspace SPME coupled with GC-FPD.

    PubMed

    Cui, Zongyan; Zhang, Kegang; Zhou, Qunfang; Liu, Jiyan; Jiang, Guibin

    2011-08-15

    A method for the determination of methyltin compounds in human urine samples was developed using headspace solid-phase microextration (HS-SPME) coupled with gas chromatographic separation and flame photometric detection. Three methyltin compounds, monomethyltin (MMT), dimethyltin (DMT), and trimethyltin (TMT) were in situ ethylated by sodium tetraethylborate (NaBEt(4)) for SPME and GC-FPD analysis. Under the optimized condition, the detection limits of MMT, DMT, and TMT were 8.1, 2.5 and 5.6 ng Sn L(-1), and the relative standard deviations were 11.0%, 7.3% and 4.0%, respectively. Methyltin compounds in thirteen urine samples from occupationally exposed population and two from general population were analyzed by the proposed method. The concentrations of total methyltin in the tested urine samples of occupationally exposed population ranged from 26.0 to 7892 ng Sn L(-1), and the average level is higher than those of the two non-occupationally exposed individuals. The methyltins in urine were adjusted by osmolality in order to enhance the comparability of different urine samples and the feasibility of this correction method was validated. PMID:21726734

  12. [Solid phase microextraction (SPME) of sample preparation during of a complex biological matrix in biotransformation studies].

    PubMed

    Kroll, C; Borchert, H H

    1998-03-01

    Within the scope of the investigation of drug metabolism in keratinocytes solid phase microextraction (SPME) was investigated as a suitable method for sample preparation. The application of SPME is based on the fact, that a amount of analyte is absorbed by the polymer fiber at equilibrium, and the fiber is localized on a tip of a GC-syringe. The stable nitroxyl radical TEMPO (2,2,6,6-tetramthylpiperidine-1-oxyl) and its apolar metabolite 2,2,6,6-tetramethylpiperidine were analyzed by SPME and subsequent GC using thymol as internal standard. By means of the headspace-technique and an apolar fiber the recovery rate of TEMPO and the metabolite was nearly 100% and the precision was high. However, the results of the direct SPME were unsatisfactory. In comparison with conventional liquid/liquid extraction and solid phase extraction SPE the SPME proved the best results with regard to recovery rate and precision. Furthermore, the main advantages of SPME are the renunciation of organic solvents, the saving of time, the possibility to reuse the fiber about 100-150 times and the option for a complete automatisation of the extraction procedure. PMID:9547519

  13. Analysis of the volatile compounds in Ligusticum chuanxiong Hort. using HS-SPME-GC-MS.

    PubMed

    Zhang, Cong; Qi, Meiling; Shao, Qinglong; Zhou, Shan; Fu, Ruonong

    2007-06-28

    A headspace solid-phase microextraction (HS-SPME) method followed by gas chromatography-mass spectrometry (GC-MS) is described for the analysis of volatile compounds in the dry rhizome of Ligusticum chuanxiong Hort. Three types of SPME fibers including PDMS, PDMS-DVB and DVB-CAR-PDMS were investigated and the best extraction was achieved with the mixed fiber DVB-CAR-PDMS. Parameters for HS-SPME in terms of temperature and time, sample amount and particle size, and desorption time were also investigated. A polar capillary column was used for the chromatographic separation. As a result, 73 compounds were determined and identified by the HS-SPME-GC-MS method with at least 20 more compounds than those in the methods available. Comparison was made between HS-SPME-GC-MS and steam distillation (SD)-GC-MS methods. Using much less sample amount, shorter extraction time and simpler procedure, HS-SPME method can achieve similar results with those by SD. In conclusion, the present method is simple, rapid and effective and can be used for the analysis of volatile compounds in medicinal plants. PMID:17306492

  14. 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.

  15. Phytoscreening with SPME: Variability Analysis.

    PubMed

    Limmer, Matt A; Burken, Joel G

    2015-01-01

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

  16. Headspace single-drop microextration for the detection of organotin compounds.

    PubMed

    Colombini, Vanessa; Bancon-Montigny, Chrystelle; Yang, Lu; Maxwell, Paulette; Sturgeon, Ralph E; Mester, Zoltán

    2004-06-17

    The performance of single-drop microextraction (SDME), coupled with gas chromatography/mass spectrometry, was assessed for the determination of tributyltin compounds in water and solid samples. Experimental parameters impacting the performance of SDME, such as microextraction solvent and sampling and stirring time, were investigated. Analytical results obtained by SDME were compared with those generated by conventional solid phase microextraction (SPME) and liquid-liquid extraction (LLE) for the determination of TBT in PACS-2 sediment certified reference material (CRM). PMID:18969468

  17. New device for direct extraction of volatiles in solid samples using SPME.

    PubMed

    Ruiz, J; Ventanas, J; Cava, R

    2001-11-01

    A new device that allows extraction of volatiles from solid materials by SPME, avoiding preparation of the sample, was designed and tested in two different food products. Volatiles from dry-cured ham and canned liver sausage were analyzed by headspace SPME (HS SPME) and by using a new device that protects the SPME fiber in the core of the solid material. Volatile profiles generated by using both methods of extraction were very similar in both products. Compounds that have been previously highlighted as quality markers, such as products from oxidative degradation of lipids, products from Strecker degradation of amino acids, or terpenes, were satisfactorily extracted by SPME coupled to the device for direct extraction. In addition, by using this method no laboratory contaminants were extracted, whereas some major laboratory solvents were presented in the chromatogram using the HS SPME method. However, coefficients of variation were higher when performing the direct sampling procedure. This new device appears to have potential as a simple method for extracting volatiles in solid materials while at the same time avoiding taking samples.

  18. A simple analysis of 5 thinner components in human body fluids by headspace solid-phase microextraction (SPME).

    PubMed

    Lee, X P; Kumazawa, T; Sato, K

    1995-01-01

    A simple method for the extraction of 5 thinner components from human whole blood and urine, using the headspace solid-phase microextraction (SPME) method is presented. After heating a vial containing the samples with 5 compounds (toluene, benzene, n-butyl acetate, n-butanol and n-isoamyl acetate) at 80 degrees C, a polydimethylsiloxane-coated SPME fiber was exposed to the headspace of the vial to allow adsorption of the compounds. The fiber needle was then injected into a capillary gas chromatography (GC) port. The headspace SPME-GC gave intense peaks for each compound and a low level of background noise was seen only for whole blood. Recovery rates of the 5 compounds by use of the headspace SPME-GC were 50-70%. Reproducibility for headspace SPME-GC data were excellent for both body fluids. The calibration curves showed linearity in the range 2-100 ng/0.5 ml whole blood or urine. The detection limits of each compound were 1.1-2.4 ng/0.5 ml sample. The present results on the analysis of 5 thinner components by headspace SPME-GC suggest its applicability to a number of other volatile compounds in forensic toxicology.

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

    PubMed

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

    2016-01-01

    The main limitation in the standard application of head space analysis employing solid phase microextraction (HS-SPME) for the evaluation of plants as sources of essential oils (EOs) are different quantitative relations of EO components from those obtained by direct analysis of EO which was got in the steam distillation (SD) process from the same plant (EO/SD). The results presented in the paper for thyme, mint, sage, basil, savory, and marjoram prove that the quantitative relations of EO components established by HS-SPME procedure and direct analysis of EO/SD are similar when the plant material in the HS-SPME process is replaced by its suspension in oil of the same physicochemical character as that of SPME fiber coating. The observed differences in the thyme EO composition estimated by both procedures are insignificant (F(exp)SPME procedure proposed in this paper substantially shortens the evaluation time of plant material quality and thus may improve the efficiency of analytical laboratories. PMID:26695252

  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. 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

  3. 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.

  4. 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. PMID:21423319

  5. A new simultaneous derivatization and microextration method for the determination of memantine hydrochloride in human plasma.

    PubMed

    Jing, Shao-Jun; Li, Qing-Lian; Jiang, Ye

    2016-01-01

    A simple and sensitive method for simultaneous derivatization and hollow fiber liquid phase microextraction (HF-LPME) followed by high performance liquid chromatography-fluorescence detection (HPLC-FL) to determine memantine hydrochloride (MT) in human plasma was developed. The derivatization and microextraction was combined to a single step to ensure the precision. What is more, the derivatization reaction accelerated the mass transfer during the process of microextraction. The hollow fiber was filled with cyclohexane and dansyl chloride (derivatization agent) as acceptor phase and submersed in the alkalinized plasma sample. The system was submitted to stirring at 800rpm for 50min at 40°C. Different experimental parameters were systematically evaluated by response surface methodology. Under the optimized conditions, the calibration curve was linear in the range of 1-100ng/mL (r=0.9991) with a limit of detection of 0.1ng/mL (S/N=3). The precision estimated as the relative standard deviation (RSD) was less than 4.5% and the accuracy was 94.3-100.7%. The present method was successfully applied to determine MT in human plasma samples.

  6. Measurement of Drinking Water Contaminants by Solid Phase Microextraction (SPME) Initially Quantified in Source Water Samples by the USGS

    PubMed Central

    Stiles, Robert; Yang, Ill; Lippincott, Robert Lee; Murphy, Eileen; Buckley, Brian

    2014-01-01

    Two adsorbent solid phase microextraction (SPME) fibers, 70 μm Carbowax divinylbenzene (CW/DVB) and 65 μm polydimethylsiloxane divinylbenzene (PDMS/DVB), were selected for the analysis of several target analytes (phenols, phosphates, phthalates, polycyclic aromatic hydrocarbons (PAHs) and chlorinated pesticides) identified by the USGS in surface waters. Detection limits for standards ranged from 0.1 to 1 ng/mL for the CW/DVB fiber and 0.1 to 2 ng/mL for the PDMS/DVB fiber for twenty of the analytes. The remaining analytes were not extracted because their polarity precluded their partition to the solid phase of the SPME fiber. Groundwater and treated water samples collected from wells in Northern New Jersey were then sampled for the USGS analytes by the SPME method as well as a modified version of EPA 525.5 using C-18 bonded solid phase extraction (SPE) columns. Nine of the USGS analytes - bisphenol A, bis (2-ethylhexyl) phthalate, butylated hydroxytoluene, butlyated hydroxyanisole, diethyltoulamide, diethyl phthalate, bis (2-ethylhexyl) adipate, 1,4-dichlorobenzene and triphenyl phosphate - were detected in ground water samples using the CW/DVB fiber. PMID:18497153

  7. Focused microwave assistance for extracting some pesticide residues from strawberries into water before their determination by SPME/HPLC/DAD.

    PubMed

    Falqui-Cao, C; Wang, Z; Urruty, L; Pommier, J J; Montury, M

    2001-11-01

    A novel and simple method for the determination of some pesticide residues in strawberries using both focused microwave-assisted extraction (FMAE) and solid-phase micro extraction (SPME), coupled with high-performance liquid chromatography (HPLC), has been developed. The pesticides were first extracted from strawberries with water and the assistance of focused microwaves at 30 W for 7 min. Then, an aliquot of the resulting aqueous extract was subjected to SPME with a 60-microm thick poly(dimethylsiloxane)/divinylbenzene (PDMS/DVB) fiber for 45 min at room temperature, with the solution being stirred at 1000 rpm. The extracted pesticides on the SPME fiber were desorbed into the SPME/HPLC interface for quantitative analysis with a diode array detector (DAD). The whole sample pretreatment procedure before chromatographic analysis did not use any organic solvents or involve any blending or centrifugation steps. The five compounds (carbendazim, diethofencarb, azoxystrobine, napropamide, and bupirimate) were chosen because they cannot be analyzed easily by GC. The efficiency of this relatively fast procedure was comparable to that of previously reported methods, with detection limits at low microg/kg levels and linear responses in the range from 0.05 to 1 mg/kg of pesticide in strawberries, with RSDs between 3 and 7.3%, depending on the analyte. In all but one case results obtained by this method for field-incurred samples were comparable to those obtained with traditional methods. PMID:11714287

  8. SPME and GC-MS analysis of triethylene glycol dimethacrylate released from dental composite.

    PubMed

    Djozan, Djavanshir; Jozan, Saeed; Aminian, Roya; Baheri, Tahmineh

    2010-02-01

    A solid-phase microextraction (SPME) coupled with gas chromatography followed by mass spectrometry was developed for the determination of triethylene glycol dimethacrylate (TEGDMA) in aqueous media originated from cured dental composite. Cylindrical specimens of a common dental composite were cured and immersed for 48 h in 3 mL portions of human saliva and also some non-biologic media e.g., pure water and Ringer's solution. The extraction was carried out by direct SPME for 15 min. The efficiency and reliability of some commercially available and modified pencil lead fibers were evaluated for the extraction of interest compound from aqueous media. Some effective and experimental parameters of SPME and gas chromatography procedures were examined and optimized. The obtained results reveal that the direct SPME using the modified pencil lead is very effective and can extract TEGDMA with a good selectivety from among various compounds such as 2,6-di-tert-butyl-4-methyl phenol (buylated hydroxy toluene) (BHT), 2-propenoic acid, 2-methyl-oxybis (2,1-ethanediyl oxy-2,1-ethanediyl) ester (TEEGDMA), 3,5-di-t-butyl-4-hydroxy benzaldehyde, benzoic acid 4 (dimethyl-amino)-ethyl ester (DMA BEE), 2-propenoic acid, 2-methyl-dodecyl ester (methacrylic acid, dodecyl ester), 2-ethoxy ethyl methacrylate, and drometrizole (TINP). The results obtained also prove that the studied composite releases 11.0, 13.4, and 28.3 microg/mL TEGDMA into distilled water, Ringer's solution, and saliva, respectively, at 48 h of the exposition. PMID:20109291

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

    PubMed

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

    2016-07-01

    Benzene, toluene, ethylbenzene and xylenes (BTEX) comprise one of the most ubiquitous and hazardous groups of ambient air pollutants of concern. Application of standard analytical methods for quantification of BTEX is limited by the complexity of sampling and sample preparation equipment, and budget requirements. Methods based on SPME represent simpler alternative, but still require complex calibration procedures. The objective of this research was to develop a simpler, low-budget, and accurate method for quantification of BTEX in ambient air based on SPME and GC-MS. Standard 20-mL headspace vials were used for field air sampling and calibration. To avoid challenges with obtaining and working with 'zero' air, slope factors of external standard calibration were determined using standard addition and inherently polluted lab air. For polydimethylsiloxane (PDMS) fiber, differences between the slope factors of calibration plots obtained using lab and outdoor air were below 14%. PDMS fiber provided higher precision during calibration while the use of Carboxen/PDMS fiber resulted in lower detection limits for benzene and toluene. To provide sufficient accuracy, the use of 20mL vials requires triplicate sampling and analysis. The method was successfully applied for analysis of 108 ambient air samples from Almaty, Kazakhstan. Average concentrations of benzene, toluene, ethylbenzene and o-xylene were 53, 57, 11 and 14µgm(-3), respectively. The developed method can be modified for further quantification of a wider range of volatile organic compounds in air. In addition, the new method is amenable to automation. PMID:27154647

  10. 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 ...

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

    PubMed

    Haftka, Joris J-H; Scherpenisse, Peter; Oetter, Günter; Hodges, Geoff; Eadsforth, Charles V; Kotthoff, Matthias; Hermens, Joop L M

    2016-09-01

    The amphiphilic nature of surfactants drives the formation of micelles at the critical micelle concentration (CMC). Solid-phase microextraction (SPME) fibers were used in the present study to measure CMC values of 12 nonionic, anionic, cationic, and zwitterionic surfactants. The SPME-derived CMC values were compared to values determined using a traditional surface tension method. At the CMC of a surfactant, a break in the relationship between the concentration in SPME fibers and the concentration in water is observed. The CMC values determined with SPME fibers deviated by less than a factor of 3 from values determined with a surface tension method for 7 out of 12 compounds. In addition, the fiber-water sorption isotherms gave information about the sorption mechanism to polyacrylate-coated SPME fibers. A limitation of the SPME method is that CMCs for very hydrophobic cationic surfactants cannot be determined when the cation exchange capacity of the SPME fibers is lower than the CMC value. The advantage of the SPME method over other methods is that CMC values of individual compounds in a mixture can be determined with this method. However, CMC values may be affected by the presence of compounds with other chain lengths in the mixture because of possible mixed micelle formation. Environ Toxicol Chem 2016;35:2173-2181. © 2016 SETAC. PMID:26873883

  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

    2016-09-01

    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. PMID:27543021

  13. A validated SPME-GC-MS method for simultaneous quantification of club drugs in human urine.

    PubMed

    Brown, Stacy D; Rhodes, Daniel J; Pritchard, Boyd J

    2007-09-13

    A solid-phase microextraction-gas chromatographic-mass spectrometric (SPME-GC-MS) method has been developed and validated for measuring four club drugs in human urine. These drugs include gamma-hydroxybutyrate (GHB), ketamine (KET), methamphetamine (MAMP), and methylenedioxymethamphetamine (MDMA). These drugs are referred to as 'club drugs' because of their prevalence at parties and raves. Deuterium labeled internal standards for each of the four drugs was included in the assay to aid in quantitation. The drugs were spiked into human urine and derivatized using pyridine and hexylchloroformate to make them suitable for GC-MS analysis. The SPME conditions of extraction time/temperature and desorption time/temperature were optimized to yield the highest peak area for each of the four drugs. The final SPME parameters included a 90 degrees C extraction for 20min with a 1min desorption in the GC injector at 225 degrees C using a splitless injection. All SPME work was done using a 100microm PDMS fiber by Supelco. The ratio of pyridine to hexylchloroformate for derivatization was also optimized. The GC separation was carried out on a VF-5ht column by Varian (30m, 0.25mm i.d., 0.10microm film thickness) using a temperature program of 150-270 degrees C at 10 degrees C/min. The instrument used was a ThermoFinnigan Trace GC-Polaris Q interfaced with a LEAP CombiPal autosampler. The data was collected by using extracted ion chromatograms of marker m/z values for each drug from the total ion chromatograms (TIC) (full scan mode). Calibration curves with R(2)>0.99 were generated each day using the peak area ratios (peak area drug/peak area internal standard) versus concentration. The validated method resulted in intra-day and inter-day precision (% R.S.D.) of less than 15% and a % error of less than 15% for four concentrations in the range of 0.05-20microg/mL (MAMP) and 0.10-20microg/mL (GHB, KET, and MDMA). This method has the advantage of an easy sample preparation with

  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. Fiber

    MedlinePlus

    ... broccoli, spinach, and artichokes legumes (split peas, soy, lentils, etc.) almonds Look for the fiber content of ... salsa, taco sauce, and cheese for dinner. Add lentils or whole-grain barley to your favorite soups. ...

  16. 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. PMID:23158309

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

    PubMed

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

    2010-07-26

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

  18. Assessment of strawberry aroma through SPME/GC and ANN methods. Classification and discrimination of varieties.

    PubMed

    Urruty, Louise; Giraudel, Jean-Luc; Lek, Sovan; Roudeillac, Philippe; Montury, Michel

    2002-05-22

    To provide an efficient and running analytical tool to strawberry plant breeders who have to characterize and compare the aromatic properties of new cultivars to those already known, a HS-SPME/GC-MS analysis method has been coupled with a statistical treatment method issued from the current development of artificial neuron networks (ANN), and more specifically, the unsupervised learning systems called Kohonen self-organizing maps (SOMs). So, 70 strawberry samples harvested at CIREF from 17 known varieties have been extracted by using a DVB/Carboxen/PDMS SPME fiber according to the headspace procedure, and then chromatographed. A panel of 23 characteristic aromatic constituents has been selected according to published results relative to strawberry aroma. The complex resulting matrix, collecting the relative abundance of the 23 selected constituents for each sample, has been input into the SOM software adapted and optimized from the Kohonen approach described by one of the authors. After a period of training, the self-organized system affords a map of virtual strawberries to which real samples are compared and plotted in the best matching unit (BMU) of the map. The efficiency for discriminating the real samples according to their variety is dependent on the number of units selected to define the map. In this case, a 24-unit map allowed the complete discrimination of the 17 selected varieties. Moreover, to test the validity of this approach, two additional samples were blind-analyzed and the results were computed according to the same procedure. At the end of this treatment, both samples were plotted into the same unit as those of the same variety used for training the map.

  19. Determination of geosmin, 2-methylisoborneol, and a musty-earthy odor in wheat grain by SPME-GC-MS, profiling volatiles, and sensory analysis.

    PubMed

    Jeleń, Henryk H; Majcher, Małgorzata; Zawirska-Wojtasiak, Renata; Wiewiórowska, Małgorzata; Wasowicz, Erwin

    2003-11-19

    Geosmin and 2-methylisoborneol-compounds responsible for the musty-earthy off-odor of wheat grain, were isolated by SPME and analyzed by GC-MS. Carboxen/PDMS/DVB fiber coating was selected because of its highest extraction efficiency. Concentrations of geosmin and 2-methylisoborneol as low as 0.001 microg/kg were detected in SIM mode using ion trap mass spectrometer. Apart from GC-MS determination of geosmin and 2-methylisoborneol, various methods for evaluating the musty-earthy off-odor caused by these compounds in wheat grain are presented. Sensory profile analysis differentiated wheat grain into sound and off-flavored, but the method was tedious. Similar groupings, however, were obtained using more rapid methods such as comparison of volatile profiles using SPME-fast GC with PCA projection of data and metal oxide (MOS) based electronic nose. PMID:14611175

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

    PubMed

    Haddadi, Shokouh Hosseinzadeh; Pawliszyn, Janusz

    2009-04-01

    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.

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

    PubMed

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

    2016-01-01

    The rapid detection of pesticide residues in wheat has become a top food security priority. A solvent-free headspace solid-phase microextraction (HS-SPME) has been evaluated for rapid screening of organophosphorus pesticide (OPP) residues in wheat with high sensitivity. Individual wheat samples (1.7 g), spiked with 10 OPPs, were placed in a 4 mL sealed amber glass vial and heated at 60°C for 45 min. During this time, the OPP residues were extracted with a 50 μm/30 μm divinylbenzene (DVB)/carboxen (CAR)/plasma desorption mass spectroscopy polydimethylsiloxane (PDMS) fiber from the headspace above the sample. The fiber was then removed and injected into the GC injection port at 250°C for desorption of the extracted chemicals. The multiple residues were identified by a GC mass spectrometer detector (GC-MSD) and quantified with a GC flame photometric detector (GC-FPD). Seven spiked levels of 10 OPPs on wheat were analyzed. The GC responses for a 50 μm/30 μm DVB/CAR/PDMS fiber increased with increasing spiking levels, yielding significant (R(2) > 0.98) linear regressions. The lowest LODs of the multiple pesticide standards were evaluated under the conditions of the validation study in a range of levels from 0 (control) to 100 ng of pesticide residue per g of wheat that separated on a low-polar GC capillary column (Agilent DB-35UI). The results of the HS-SPME method were compared with the QuEChERS AOAC 2007.01 method and they showed several advantages over the latter. These included improved sensitivity, selectivity, and simplicity. PMID:26964527

  2. 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.

  3. 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

    2015-07-01

    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.

  4. Development of an SPME-GC-MS/MS procedure for the monitoring of 2-phenoxyethanol in anaesthetised fish.

    PubMed

    Klimánková, Eva; Riddellová, Katerina; Hajslová, Jana; Poustka, Jan; Kolárová, Jitka; Kocourek, Vladimír

    2008-05-30

    2-Phenoxyethanol (ethylene glycol monophenyl ether, C(8)H(10)O(2)) is a promising anaesthetic agent used in fisheries and aquaculture. The aim of this study was to develop a fast and easy method to determine 2-phenoxyethanol residue levels in fish tissue and blood plasma, and, subsequently, to use the method to monitor the dynamics of 2-phenoxyethanol residues in fish treated with anaesthetic. We developed a new procedure that employs solid phase microextraction (SPME) of the target analyte from the sample headspace followed by gas chromatography-mass spectrometry (GC-MS). Both sample handling, aimed at maximum transfer of 2-phenoxyethanol into the headspace, and SPME-GC-MS conditions were carefully optimised. Using a divinylbenzene/Carboxen/polydimethylsiloxane (PDMS/CAR/DVB) fiber for 60 min sampling at 30 degrees C and an ion trap detector operated in MS/MS mode, we obtained detection (LOD) and quantification (LOQ) limits of 0.03 and 0.1 mg kg(-1) of sample, respectively. The method was linear in a range of 0.1-250 mg kg(-1) and, depending on the sample matrix and spiking level, a repeatability (expressed as relative standard deviation, R.S.D.) of between 3% and 11% was obtained.

  5. Transient Method for Determining Indoor Chemical Concentrations Based on SPME: Model Development and Calibration.

    PubMed

    Cao, Jianping; Xiong, Jianyin; Wang, Lixin; Xu, Ying; Zhang, Yinping

    2016-09-01

    Solid-phase microextraction (SPME) is regarded as a nonexhaustive sampling technique with a smaller extraction volume and a shorter extraction time than traditional sampling techniques and is hence widely used. The SPME sampling process is affected by the convection or diffusion effect along the coating surface, but this factor has seldom been studied. This paper derives an analytical model to characterize SPME sampling for semivolatile organic compounds (SVOCs) as well as for volatile organic compounds (VOCs) by considering the surface mass transfer process. Using this model, the chemical concentrations in a sample matrix can be conveniently calculated. In addition, the model can be used to determine the characteristic parameters (partition coefficient and diffusion coefficient) for typical SPME chemical samplings (SPME calibration). Experiments using SPME samplings of two typical SVOCs, dibutyl phthalate (DBP) in sealed chamber and di(2-ethylhexyl) phthalate (DEHP) in ventilated chamber, were performed to measure the two characteristic parameters. The experimental results demonstrated the effectiveness of the model and calibration method. Experimental data from the literature (VOCs sampled by SPME) were used to further validate the model. This study should prove useful for relatively rapid quantification of concentrations of different chemicals in various circumstances with SPME. PMID:27476381

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

    PubMed

    Bravo, Manuel; Lespes, Gaëtane; De Gregori, Ida; Pinochet, Hugo; Gautier, Martine Potin

    2005-12-01

    A method based on Headspace solid-phase microextraction (HS-SPME, with a 100 mum PDMS-fiber) in combination with gas-chromatography and pulsed flame-photometric detection (GC-PFPD) has been investigated for simultaneous determination of eight organotin compounds. Monobutyltin (MBT), dibutyltin (DBT), tributyltin (TBT), monophenyltin (MPhT), and the semi-volatile diphenyltin (DPhT), triphenyltin (TPhT), monooctyltin (MOcT), and dioctyltin (DOcT) were determined after derivatization with sodium tetraethylborate. The conditions used for the extraction and preconcentration step were optimised by experimental design methodology. Tripropyltin (TPrT) and diheptyltin (DHepT) were used as internal standards for quantification of volatile and semi-volatile organotin compounds, respectively. The analytical precision (RSD) for ten successive injections of a standard mixture containing all the organic tin compounds ranged between 2 and 11%. The limits of detection for all the organotin compounds were sub ng (Sn) L(-1) in water and close to ng (Sn) kg(-1) in sediments. The accuracy of the method was evaluated by analysis of two certified reference material (CRM) sediment samples. The HS-SPME-GC-PFPD was then applied to the analysis of three harbour sediment samples. The results showed that headspace SPME is an attractive tool for analysis of organotin compounds in solid environmental matrices. PMID:16328254

  7. Au-coated ZnO nanorods on stainless steel fiber for self-cleaning solid phase microextraction-surface enhanced Raman spectroscopy.

    PubMed

    Li, Bo; Shi, Yu-E; Cui, Jingcheng; Liu, Zhen; Zhang, Xiaoli; Zhan, Jinhua

    2016-06-01

    Solid phase microextraction-surface enhanced Raman spectroscopy (SPME-SERS), combining the pretreatment and determination functions, has been successfully used in environmental analysis. In this work, Au-coated ZnO nanorods were fabricated on stainless steel fiber as a self-cleaning SERS-active SPME fiber. The ZnO nanorods grown on stainless steel fiber were prepared via a simple hydrothermal approach. Then the obtained nanostructures were decorated with Au nanoparticles through ion-sputtering at room temperature. The obtained SERS-active SPME fiber is a reproducible sensitivity sensor. Taking p-aminothiophenol as the probe molecule, the RSD value of the SERS-active SPME fiber was 8.9%, indicating the fiber owned good uniformity. The qualitative and quantitative detection of crystal violet and malachite green was also achieved. The log-log plot of SERS intensity to crystal violet and malachite green concentration showed a good linear relationship. Meanwhile, this SERS-active SPME fiber can achieve self-cleaning owning to the excellent photocatalytic performance of ZnO nanorods. Crystal violet was still successfully detected even after five cycles, which indicated the high reproducibility of this SERS-active SPME fiber.

  8. Au-coated ZnO nanorods on stainless steel fiber for self-cleaning solid phase microextraction-surface enhanced Raman spectroscopy.

    PubMed

    Li, Bo; Shi, Yu-E; Cui, Jingcheng; Liu, Zhen; Zhang, Xiaoli; Zhan, Jinhua

    2016-06-01

    Solid phase microextraction-surface enhanced Raman spectroscopy (SPME-SERS), combining the pretreatment and determination functions, has been successfully used in environmental analysis. In this work, Au-coated ZnO nanorods were fabricated on stainless steel fiber as a self-cleaning SERS-active SPME fiber. The ZnO nanorods grown on stainless steel fiber were prepared via a simple hydrothermal approach. Then the obtained nanostructures were decorated with Au nanoparticles through ion-sputtering at room temperature. The obtained SERS-active SPME fiber is a reproducible sensitivity sensor. Taking p-aminothiophenol as the probe molecule, the RSD value of the SERS-active SPME fiber was 8.9%, indicating the fiber owned good uniformity. The qualitative and quantitative detection of crystal violet and malachite green was also achieved. The log-log plot of SERS intensity to crystal violet and malachite green concentration showed a good linear relationship. Meanwhile, this SERS-active SPME fiber can achieve self-cleaning owning to the excellent photocatalytic performance of ZnO nanorods. Crystal violet was still successfully detected even after five cycles, which indicated the high reproducibility of this SERS-active SPME fiber. PMID:27155303

  9. Surface characterization of commercial fibers for solid-phase microextraction and related problems in their application.

    PubMed

    Haberhauer-Troyer, C; Crnoja, M; Rosenberg, E; Grasserbauer, M

    2000-02-01

    The surfaces of commercially available polydimethylsiloxane (PDMS) and Carboxen-PDMS fibers for solid-phase microextraction (SPME) were investigated by optical and electron microscopy. Damage to the coating as well as contamination of new fibers and a highly variable number of pores in Carboxen-PDMS coatings were observed. Together with the contamination of the fibers during their use with metallic particles originating from the SPME fiber holder they are possible explanations for the problems encountered in the analysis of organolead, organotin and organosulfur compounds, such as artifact formation and low repeatability. PMID:11220312

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

    PubMed

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

    2011-03-01

    Solid-phase microextraction (SPME) coupled to gas chromatography/isotope ratio mass spectrometry (GC/IRMS) was used to elucidate the effects of N-atom protonation on the analysis of N and C isotope signatures of selected aromatic amines. Precise and accurate isotope ratios were measured using polydimethylsiloxane/divinylbenzene (PDMS/DVB) as the SPME fiber material at solution pH-values that exceeded the pK(a) of the substituted aniline's conjugate acid by two pH-units. Deviations of δ(15)N and δ(13)C-values from reference measurements by elemental analyzer IRMS were small (<0.9‰) and within the typical uncertainties of isotope ratio measurements by SPME-GC/IRMS. Under these conditions, the detection limits for accurate isotope ratio measurements were between 0.64 and 2.1 mg L(-1) for δ(15)N and between 0.13 and 0.54 mg L(-1) for δ(13)C, respectively. Substantial inverse N isotope fractionation was observed by SPME-GC/IRMS as the fraction of protonated species increased with decreasing pH leading to deviations of -20‰ while the corresponding δ(13)C-values were largely invariant. From isotope ratio analysis at different solution pHs and theoretical calculations by density functional theory, we derived equilibrium isotope effects, EIEs, pertinent to aromatic amine protonation of 0.980 and 1.001 for N and C, respectively, which were very similar for all compounds investigated. Our work shows that N-atom protonation can compromise accurate compound-specific N isotope analysis of aromatic amines.

  11. 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).

  12. 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

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

    PubMed

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

    2016-12-15

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

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

    PubMed

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

    2016-12-15

    Among methods to detect wine adulteration, profiling volatiles is one with a great potential regarding robustness, analysis time and abundance of information for subsequent data treatment. Volatile fraction fingerprinting by solid-phase microextraction with direct analysis by mass spectrometry without compounds separation (SPME-MS) was used for differentiation of white as well as red wines. The aim was to differentiate between varieties used for wine production and to also differentiate wines by country of origin. The results obtained were compared to SPME-GC/MS analysis in which compounds were resolved by gas chromatography. For both approaches the same type of statistical procedure was used to compare samples: principal component analysis (PCA) followed by linear discriminant analysis (LDA). White wines (38) and red wines (41) representing different grape varieties and various regions of origin were analysed. SPME-MS proved to be advantageous in use due to better discrimination and higher sample throughput. PMID:27451239

  15. SPME-GC-EC of chlorinated paraffins in water

    SciTech Connect

    Webster, G.R.B.; Sarna, L.P.; Thomas, D.A.

    1995-12-31

    Contamination of aquatic ecosystems with chlorinated organic contaminants is an increasing toxicological problem. Chlorinated paraffins (CPs) are a class of compounds which are used as fire retardants in paints and as high pressure lubricants and are classified as Priority Toxic Substances under the Canadian Environmental Protection Act (CEPA). As the largest group of high molecular weight chlorinated hydrocarbons produced in Western Europe and North America, CPs have recently come under increased regulatory scrutiny in Canada, the USA, and Europe, because of concerns about their environmental persistence, possible adverse effects on terrestrial and aquatic organisms, and potential carcinogenicity to humans. In both the monitoring of such contamination and the determination of the success of remediation methods, straightforward and inexpensive analytical methodology increases the ease of environmental assessment and facilitates regulatory enforcement. CPs have been considered to be incapable of being analyzed by GC. The authors report the solid phase microextraction (SPME) based analysis of CPs by GC using electron capture (EC) detection. Both synthetic C{sub 10} standards and fractionated commercially derived material have been analyzed by this method in water.

  16. 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

  17. Cryotrap/SPME/GC/MS method for profiling of monoterpenes in cheese and their clustering according to geographic origin.

    PubMed

    Tompa, Gorazd; Susič, Robert; Rogelj, Irena; Pompe, Matevž

    2013-01-01

    A variant of purge/cryotrap/thaw/static headspace Solid Phase Microextraction (SPME) was developed as a means for preconcentrating Volatile Organic Compounds (VOC) in cheese. An originally designed cryotrap partially filled with glass beads was employed that facilitated efficient flow-through of purging gas and trapping of the volatiles. In stopped-flow mode, thawing was allowed, and the same vessel was used for the exposure of the appropriate SPME fiber, effectively achieving double preconcentration. Gas chromatography/mass spectrometry (GC/MS) was subsequently employed to identify components and assess their relative chromatographic peak areas. Monoterpenes were chosen as a model group of substances, and their relative concentration profiles were evaluated as potential markers for the respective geographic origin. The procedure was tested on samples of five traditional Slovenian cheeses featuring Protected Designation of Origin (PDO): Tolminc, Mohant, Nanoški cheese, together with Bovški cheese and Karst Ewe's cheese. The dataset of the peak areas of nine prominent monoterpenes (α-pinene, camphene, α-phellandrene, β-pinene, 3-carene, 2-carene, limonene, tricyclene, and γ-terpinene) in cheese samples showed clustering that relates the cheeses to the area of production. According to the silhouette metrics, four clusters were identified by partitioning around medoids (PAM) method. The latter packed data for Tolminc and Bovški cheese into a single cluster, closely reflecting the vicinity of their geographic origin, but classified correctly the rest of the data into separate clusters for all other cheeses. PMID:24169714

  18. Nondestructive, minimal-disturbance, direct-burial solid-phase microextraction fiber technique for measuring TNT in sediment.

    PubMed

    Conder, Jason M; La Point, Thomas W; Lotufo, Guilherme R; Steevens, Jeffery A

    2003-04-15

    We explored a novel technique to deploy solid-phase microextraction (SPME) fibers to nondestructively measure the explosive compound 2,4,6-trinitrotoluene (TNT) and its nitroaromatic (NA) degradation products in laboratory sediment toxicity tests and field sediments in situ. SPME fibers within steel mesh envelopes were exposed statically via direct burial within sediment. Six fiber types (polymer coatings) were tested. Polyacrylate (PA) SPME fiber was sufficiently durable for this application, yielded the lowest detection limits, and exhibited a linear uptake relationship across toxicologically relevant sediment NA concentrations (100-2000 nmol/g dw (20-500 microg/g dw)). Temperature greatly influenced SPME absorption kinetics. Via evaluation of absorption at different temperatures, recommended sampling times needed to achieve steady-state equilibrium were 48 h for room temperatures (23-25 degrees C) and up to 7 d for cold (5 degrees C) temperatures. Although a comparison of TNT residues by SPMEs and TNT bioavailability and toxicity in sediments has not been completed, differences in SPME availability of TNT and its degradation products were found between two different TNT-spiked sediments. Our disposable SPME technique was slightly less expensive and as precise as the conventional extraction for total NAs and may prove to be a powerful exposure evaluation tool for assessing the ecological risk of these compounds.

  19. 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

  20. Optimization of the HS-SPME-GC-IT/MS method using a central composite design for volatile carbonyl compounds determination in beers.

    PubMed

    Moreira, Nathalie; Meireles, Sónia; Brandão, Tiago; de Pinho, Paula Guedes

    2013-12-15

    An automated headspace solid-phase microextraction (HS-SPME) combined with gas chromatography and ion trap mass spectrometry detection (GC-IT/MS) was developed in order to quantify a large number of carbonyl compounds in beers. Carbonyl compounds were previously derivatized with O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine hydrochloride (PFBHA). Volatile carbonyl compounds associated with staling beer aroma includes alkanals, alkenals, alkadienals, dicarbonyl compounds, Strecker aldehydes, ketones and furans. The HS-SPME was performed using a polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber. The procedures were optimized for HS-SPME pre-incubation temperature and time, extraction temperature and time, and PFBHA addition. A central composite design was used in the optimization of extraction conditions and PFBHA addition. The volatile compounds showed optimal extraction incubating 5 ml of beer with 700 mg l(-1) of PFBHA for 7 min and extracted for more 20 min at 45 °C. The method was validated with regard to the linearity, repeatability, inter and intra-day precision and accuracy. The method achieved detection limits ranging from 0.003 to 0.510 µg l(-1), except for furans (1.54-3.44 µg l(-1)). The quantification limits varied from 0.010 to 1.55 µg l(-1), except for 2-furfural (4.68 µg l(-1)), 5-methyl-2-furfural (5.82 µg l(-1)) and 5-hyfroxymethylfurfural (10.4 µg l(-1)). Repeatability values of all compounds were lower than 17%. The method accuracy was satisfactory with recoveries ranging from 88% to 114%. The validated method showed to be suitable for a fast and reliable determination of main carbonyl compounds in beers.

  1. 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.

  2. 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.

  3. 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. PMID:21535518

  4. 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.

  5. 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.

  6. 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. PMID:27664623

  7. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2016-08-01

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

  9. Improvement of measurement precision of SPME-GC/MS determination of tributyltin using isotope dilution calibration.

    PubMed

    Bancon-Montigny, Chrystelle; Maxwell, Paulette; Yang, Lu; Mester, Zoltán; Sturgeon, Ralph E

    2002-11-01

    A unique approach was developed to improve the precision of quantification of tributyltin (TBT) in sedimentsby solid phase microextraction (SPME) using isotope dilution GC/MS. The precision of the analytical technique was initially evaluated using standard calibration solutions. In selective ion monitoring (SIM) mode, the relative standard deviation (RSD) obtained for TBT based on peak area response was 18% (n = 11). When an internal standard, tripropyltin (TPrT), was used, the RSD decreased to 12%. A significant improvement in the precision using SPME was noted when a 117Sn-enriched TBT spike was employed; the RSD decreased 4-fold to 3%. Detection limits of 0.2 and 20 ng(Sn) L(-1) were achieved with SPME sampling and liquid-liquid extraction, respectively. Six analyses were performed for determination of TBT in PACS-2 sediment Certified Reference Material using both standard additions and isotope dilution procedures. For the latter, a 117Sn-enriched TBT spike was used. A concentration of 0.88 +/- 0.03 microg g(-1) (RSD 3.4%) obtained using standard additions was in good agreement with the certified value of 0.98 +/- 0.13 microg g(-1) as tin. Concentrations found using isotope dilution were 0.895 +/- 0.015 microg g(-1) (RSD 1.73%) as tin and 0.874 +/- 0.014 microg g(-1) (RSD 1.66%) as tin using a liquid-liquid extraction and SPME sampling, respectively. A 2-fold improvement in the precision of TBT concentration measurement using isotope dilution was clearly achieved, demonstrating its superiority in providing more accurate and precise results as compared to the method of standard additions. The isotope dilution technique eliminated the problem of poor reproducibility, which typically plagues SPME. PMID:12433095

  10. 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.

  11. 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.

  12. 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. PMID:26304345

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

    PubMed

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

    2016-05-12

    The main quest for the implementation of direct SPME to complex matrices has been the development of matrix compatible coatings that provide sufficient sensitivity towards the target analytes. In this context, we present here a thorough evaluation of PDMS-overcoated fibers suitable for simultaneous extraction of different polarities analytes, while maintaining adequate matrix compatibility. For this, eleven analytes were selected, from various application classes (pesticides, industrial chemicals and pharmaceuticals) and with a wide range of log P values (ranging from 1.43 to 6). The model matrix chosen was commercial Concord grape juice, which is rich in pigments such as anthocyanins, and contains approximately 20% of sugar (w/w). Two types of PDMS, as well as other intrinsic factors associated with the PDMS-overcoated fiber fabrication are studied. The evaluation showed that the PDMS-overcoated fibers considerably slowed down the coating fouling process during direct immersion in complex matrices of high sugar content. Longevity differences could be seen between the two types of PDMS tested, with a proprietary Sylgard(®) giving superior performance because of lesser amount of reactive groups and enhanced hydrophobicity. Conversely, the thickness of the outer layer did not seem to have a significant effect on the fiber lifetime. We also demonstrate that the uniformity of the overcoated PDMS layer is paramount to the achievement of reliable data and extended fiber lifetime. Employing the optimum overcoated fiber, limits of detection (LOD) in the range of 0.2-1.3 ng/g could be achieved. Additional improvement is attainable by introducing washing of the coatings after desorption, so that any carbon build-up (fouling) left on the coating surface after thermal desorption can be removed. PMID:27114223

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

    PubMed

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

    2016-05-12

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

  15. Determination of the acaricide fenbutatin oxide in water samples by automated headspace-SPME-GC/MS.

    PubMed

    Devos, Christophe; Moens, Luc; Sandra, Pat

    2005-05-01

    The analysis of the acaricide fenbutatin oxide (FBTO) having a molecular weight of 1052.66 g mol(-1) in water samples by capillary GC/MS after in-situ derivatization with sodium tetraethylborate (NaBEt4) and headspace-SPME enrichment is described. Automated SPME is performed at 80 degrees C for 30 min. Detection is carried out in the ion monitoring mode with deuterated triphenyltin (TPhTd15) as internal standard. Good linearity (R2 = 0.9993) was obtained in the dynamic range 20 to 1000 ng L(-1) with a limit of detection of 16 ng L(1) (LOD at 3 S/N) and a limit of quantitation of 50 ng L(-1) (LOQ at 10 S/N). Intra-day RSD% for n=6 was 8.9 at the LOQ level. PMID:15912737

  16. Development of SPME method for concomitant sample preparation of rocuronium bromide and tranexamic acid in plasma.

    PubMed

    Gorynski, Krzysztof; Bojko, Barbara; Kluger, Michael; Jerath, Angela; Wąsowicz, Marcin; Pawliszyn, Janusz

    2014-04-01

    A high-throughput method using solid-phase microextraction coupled to liquid chromatography-tandem mass spectrometry (SPME-LC-MS/MS) for determination of tranexamic acid and rocuronium bromide in human plasma was developed and validated. Standard analytical approaches employ acidification of the sample due to the instability of rocuronium bromide in collected plasma samples. However, acidification affects the binding equilibrium of the drug and consequently no information on the free/bound concentration can be obtained. Contrary to these protocols, the proposed method requires minimum sample handling and no ion pairing and/or derivatization procedure. A weak cation exchange coating was chosen as the best extracting phase for selected drugs, guaranteed a good recovery, minimum carry-over, reusability and reproducibility. SPME procedure met all Food and Drug Administration acceptance criteria for bioanalytical assays at three concentration levels, for both selected drugs. Post-extraction addition experiments showed that matrix effect was less than ±3%. Here, a weak cation exchange thin-film solid-phase microextraction (WCX TF-SPME) approach is presented, offering effective cleanup procedure and full quantitation of the drugs in plasma, undoubtedly one the most challenging matrices with regards to its complexity. In addition, the 96-well plate format of WCX TF-SPME system provides considerable advantages, such as high throughput analysis for up to 96 samples in 35min (22s/sample), requirement of small amounts of plasma samples (0.8mL), and a simple sample preparation protocol, all of which shows a promise for possible on-site application in hospitals to monitor concentrations of the drugs in close to real time. PMID:24525565

  17. Evaluation of polycaprolactone as a new sorbent coating for determination of polar organic compounds in water samples using membrane-SPME.

    PubMed

    Marcinkowski, Łukasz; Kloskowski, Adam; Spietelun, Agata; Namieśnik, Jacek

    2015-02-01

    Commercially available solid-phase microextraction fibers used for isolation of polar analytes are based on the adsorption phenomenon. In consequence, typical limitations bonded with analytes displacement and matrix effects are very frequent. In the present study, alternative solution is described. Polycaprolactone (PCL) was used for the first time as sorbent to isolate polar organic compounds from water samples using the membrane-solid-phase microextraction (M-SPME) technique. In this technique, due to protective role of the mechanically and thermally stable polydimethylsiloxane (PDMS) membrane, internal polar coating might be melted during extraction and desorption of analytes. In consequence sorbents with low melting points like a PCL might be utilized. Based on chromatographic retention data, triazines were selected as a model compounds for evaluation of the sorptive properties of the polycaprolactone. Applying the screening plan and central composite design, statistically significant parameters influencing extraction efficiency were determined and optimized. The analysis of variance confirmed the significant influence of temperature, salt content, and pH of samples on the extraction efficiency. Besides the new PCL/PDMS fiber, a commercial fiber coated with divinylbenzene/polydimethylsiloxane (DVB/PDMS) was used for comparative studies. The results obtained showed that PCL is an interesting sorbent which can be successfully applied for isolation of polar organics from aqueous matrices at a broad range of analytes concentration. The determined detection limits of procedure based on the novel fiber enable its application at the concentration levels of triazines recommended by the US EPA standards. The practical applicability of the developed fiber has been confirmed by the results based on the analysis of real samples.

  18. 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. PMID

  19. 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.

  20. Investigation of a Quantitative Method for the Analysis of Chiral Monoterpenes in White Wine by HS-SPME-MDGC-MS of Different Wine Matrices.

    PubMed

    Song, Mei; Xia, Ying; Tomasino, Elizabeth

    2015-01-01

    A valid quantitative method for the analysis of chiral monoterpenes in white wine using head-space solid phase micro-extraction-MDGC-MS (HS-SPME-MDGC-MS) with stable isotope dilution analysis was established. Fifteen compounds: (S)-(-)-limonene, (R)-(+)-limonene, (+)-(2R,4S)-cis-rose oxide, (-)-(2S,4R)-cis-rose oxide, (-)-(2R,4R)-trans-rose oxide, (+)-(2S,4S)-cis-rose oxide, furanoid (+)-trans-linalool oxide, furanoid (-)-cis-linalool oxide, furanoid (-)-trans-linalool oxide, furanoid (+)-cis-linalool oxide, (-)-linalool, (+)-linalool, (-)-α-terpineol, (+)-α-terpineol and (R)-(+)-β-citronellol were quantified. Two calibration curves were plotted for different wine bases, with varying residual sugar content, and three calibration curves for each wine base were investigated during a single fiber's lifetime. This was needed as both sugar content and fiber life impacted the quantification of the chiral terpenes. The chiral monoterpene content of six Pinot Gris wines and six Riesling wines was then analyzed using the verified method. ANOVA with Tukey multiple comparisons showed significant differences for each of the detected chiral compounds in all 12 wines. PCA score plots showed a clear separation between the Riesling and Pinot Gris wines. Riesling wines had greater number of chiral terpenes in comparison to Pinot Gris wines. Beyond total terpene content it is possible that the differences in chiral terpene content may be driving the aromatic differences in white wines.

  1. Determination of parabens in cosmetic products by solid-phase microextraction of poly(ethylene glycol) diacrylate thin film on fibers and ultra high-speed liquid chromatography with diode array detector.

    PubMed

    Fei, Ting; Li, Haifang; Ding, Mingyu; Ito, Masahito; Lin, Jin-Ming

    2011-07-01

    The fabrication of a solid-phase microextraction (SPME) fiber through UV-induced polymerization of poly(ethylene glycol) diacrylate (PEG-DA) for determination of parabens in cosmetic products is presented in this work. The PEG-DA polymer coating was covalently attached to the fiber by introducing a surface modification with 3-(trichlorosilyl)propyl methacrylate (TPM). The PEG-DA polymer thin film coated on the fiber was homogeneous and wrinkled, which led to an increase of the surface area and high extraction efficiency. The extraction performances of the prepared SPME fibers were assessed by preconcentration of parabens including methylparaben, ethylparaben, propylparaben and benzylparaben from cosmetic products. The analysis was performed on an ultra high-speed liquid chromatography with diode array detector. The prepared SPME fibers exhibited good repeatability (for one fiber) and reproducibility (fiber-to-fiber) with RSDs of 5.4 and 6.9%, respectively. The optimized SPME method supported a wide linear range of 0.50-160 μg/mL and the detection limits for parabens were in the range of 0.12-0.15 μg/mL (S/N=3). The developed method was successfully applied for determination of parabens in cosmetic products with different natures.

  2. 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).

  3. 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.

  4. Characterisation of absorptive sampling with SPME fibres in the EUPHORE photoreactor.

    PubMed

    Gómez Alvarez, E

    2007-07-31

    The implementation of an experimental set-up for sampling, and characterisation of parameters related to absorptive sampling solid phase microextraction (SPME) in the EUPHORE photoreactor is described. Toluene was taken as probe compound. Optimisation of the sampling and calibration curves are presented. Equilibrium was achieved in just 30s due to the good agitation in the chambers and the LOD was 0.24 ppbV. The precision was +/-0.02 expressed as relative standard deviation (n=9). The inter-fibre reproducibility was +/-0.03 expressed as relative standard deviation. The effect of the temperature and the sun radiation on absorption in the fibre is also studied using a relative method to calculate the ratio K/K(0) (ratio of absorption constants at two different times during the experiment at which temperature and radiation conditions experimented important variations) calculated through known parameters, avoiding in this way the need for external calibrations in the calculation of K. The results showed a difficult to predict dependence of absorption over the combination of temperature and sun radiation and the need to develop sampling systems with absorptive SPME in which sun radiation has no influence. The stability in different conditions of compounds absorbed in the fibre was also subject to study. At room temperature half of the compound absorbed is expected to desorb in 1.21 h. Conversely, when fibres were kept at low temperatures (-86 degrees C) after 21 days, desorption was negligible.

  5. 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. PMID:21074162

  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. 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. PMID:20582406

  8. 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. PMID:27371020

  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. CNT-TiO2 coating bonded onto stainless steel wire as a novel solid-phase microextraction fiber.

    PubMed

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

    2013-09-30

    A novel solid-phase microextraction (SPME) fiber based on carbon nanotubes-titanium oxide (CNT-TiO2) composite coating bonded onto stainless steel wire was prepared via electroless plating and sol-gel techniques. The SPME coating was characterized by scanning electron microscopy and Raman microscopy. Coupled to gas chromatography (GC), the fiber was investigated with seven polycyclic aromatic hydrocarbons (PAHs) in direct-immersion mode. The SPME-GC analytical method was evaluated under optimized extraction conditions. Compared with other reports, higher sensitivity (LODs, 0.002-0.004 μg L(-1)) and better linear range (0.01-100 and 0.01-200 μg L(-1)) were obtained by the proposed method. The fiber exhibited high thermal stability to 300 °C and excellent durability in HCl and NaOH solutions. The as-established SPME-GC method was used to analyze the real water samples and satisfactory results were obtained.

  11. Analysis of trace levels of pesticides in rainwater by SPME and GC-tandem mass spectrometry after derivatisation with PFBBr.

    PubMed

    Scheyer, Anne; Briand, Olivier; Morville, Stéphane; Mirabel, Philippe; Millet, Maurice

    2007-01-01

    Solid-phase microextraction (SPME) was used for the analysis of some pesticides (bromoxynil, chlorotoluron, diuron, isoproturon, 2,4-MCPA, MCPP and 2,4-D) in rainwater after derivatisation with PFBBr and gas chromatography-ion trap mass spectrometry. The derivatisation procedure was optimized by testing different methods: direct derivatisation in the aqueous phase followed by SPME extraction, on-fibre derivatisation and derivatisation in the injector. The best result was obtained by headspace coating the PDMS/DVB fibre with PFBBr for 10 min followed by direct SPME extraction for 60 min at 68 degrees C (pH 2 and 75% NaCl). Good detection limits were obtained for all the compounds: these ranged between 10 and 1,000 ng L-1 with a relatively high uncertainty due to the combination of derivatisation and SPME extraction steps. The optimized procedure was applied to the analysis of pesticides in rainwater and results obtained shows that this method is a fast and simple technique to assess the spatial and temporal variations of concentrations of pesticides in rainwater.

  12. Zeolitic imidazole framework templated synthesis of nanoporous carbon as a novel fiber coating for solid-phase microextraction.

    PubMed

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

    2016-02-01

    A new solid-phase microextraction (SPME) fiber coating material, a zeolitic imidazole framework-67 (ZIF-67) templated nanoporous carbon, Co-NPC, was fabricated by one-step direct carbonization of ZIF-67 without using any other carbon precursors. The prepared Co-NPC was then coated onto a functionalized stainless steel wire by a simple physical coating method to prepare SPME fibers. By coupling the Co-NPC coated fiber based SPME with gas chromatography/micro-electron capture detection (GC/μECD), the developed method exhibited low limits of detection (0.07-0.45 ng g(-1)) and a wide linearity (0.30-50 ng g(-1)) for the determination of five organochlorine pesticides (OCPs) in vegetable samples. The method was applied to the analysis of cabbage, cucumber and celery cabbage samples, and the recoveries of the analytes were in the range of 87.9-103.9% with the relative standard deviations (RSDs) ranging from 5.1% to 10.4% (n = 5). Single fiber repeatability and fiber-to-fiber reproducibility values expressed as RSDs were in the range of 4.9-9.6% and 5.8-11.0%, respectively. The method was simple, convenient and feasible for the determination of OCPs in real samples. PMID:26699844

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

    PubMed Central

    Griffith, Robert T.; Jayachandran, Krishnaswamy; Shetty, Kateel G.; Whitstine, William; Furton, Kenneth G.

    2007-01-01

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

  14. A SPME-GC procedure for monitoring peppermint flavor in tablets.

    PubMed

    Yeung, David Yong-Hoi; Lee, Tony; Grant, Gail; Ma, Minhui; Kwong, Elizabeth

    2003-01-01

    A method was developed using solid-phase microextraction (SPME) and gas chromatography to monitor the peppermint flavor loss in a taste-masked tablet formulation. This was accomplished by headspace sampling of two major components of peppermint: menthone and menthol. It was found that the excipients from the tablet produced an important matrix effect and that standard addition analysis was necessary for improved accuracy of the determination. The method was shown to be specific and precise. Furthermore, the method produced acceptable results with adequate quantitation limits to determine peppermint flavors in taste-masked tablets. The optimized extraction procedure was successfully used to monitor the stability of peppermint flavor in an oral solid formulation. The accelerated stability studies of the tablet showed that the menthone and menthol was lost in an exponential manner and levels off after several days of heat exposure.

  15. Quantification of jasmonic acid by SPME in tomato plants stressed by ozone.

    PubMed

    Zadra, Claudia; Borgogni, Andrea; Marucchini, Cesare

    2006-12-13

    Jasmonates are signalling molecules induced in plants as a response to various biotic and/or abiotic stresses. As ozone is known to activate defense responses in plants, we have monitored the concentration of jasmonic acid in tomato leaves during and after an acute exposure to this abiotic elicitor. In this experiment, we observed that the maximum induction of jasmonic acid in O3-fumigated plants occurred 9 h after the end of treatment and the concentration of jasmonic acid in stressed plants increased 13-fold. However, the level of endogenous methyl-jasmonate was constant during the observed period. The extraction and quantification of jasmonic acid as its methyl ester was performed by headspace-solid-phase microextraction (or HS-SPME) in combination with GC-FID and GC-MS. The sensitivity (LOD = 2 ng/g) of this method permitted the detection and quantification of jasmonic acid present in plant tissues at very low concentrations. PMID:17147413

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

    PubMed

    Chinn, Sarah C; Alviso, Cynthia T; Berman, Elena S F; Harvey, Christopher A; Maxwell, Robert S; Wilson, Thomas S; Cohenour, Rebecca; Saalwächter, Kay; Chassé, Walter

    2010-08-01

    Radiation-induced degradation of polymeric materials occurs through numerous, simultaneous, competing chemical reactions. Although degradation is typically found to be linear in adsorbed dose, some silicone materials exhibit nonlinear 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 in electronic encapsulation and in biomedical applications), using traditional mechanical testing, NMR spectroscopy, and sample headspace analysis using solid-phase microextraction (SPME) followed by gas chromatography/mass spectrometry (GC/MS). The mechanical data and (1)H spin-echo NMR spectra indicated that radiation exposure leads to predominantly cross-linking over the cumulative dose range studied (0-250 kGy) with a rate roughly linear with dose. (1)H multiple-quantum NMR spectroscopy detected a bimodal distribution in the network structure, as expected from the proposed structure of Sylgard 184. The MQ NMR spectra further indicated that the radiation-induced structural changes were not linear in adsorbed dose and that competing chain scission mechanisms made a greater contribution to the overall degradation process in the range of 50-100 kGy (although cross-linking still dominated). 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.

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

    PubMed

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

    2009-05-30

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

  18. 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. PMID:26775020

  19. 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%.

  20. 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.

  1. 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.

  2. 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.

  3. 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

  4. SPME-GC method as a tool to differentiate VOC profiles in Saccharomyces cerevisiae wine yeasts.

    PubMed

    Mauriello, Giacomo; Capece, Angela; D'Auria, Maurizio; Garde-Cerdán, Teresa; Romano, Patrizia

    2009-05-01

    The aim of this work was to study the variability of 36 Saccharomyces cerevisiae wild strains isolated from different grape varieties and from two very distant zones, located in Northern and Southern Italy. The strains were differentiated on the basis of parameters of technological interest, such as resistance to antimicrobial compounds frequently present in wine, and the production of volatile aromatic compounds (VOC), determined by SPME procedure in the experimental wines obtained by inoculated fermentations. The VOC profile allowed to differentiate the yeasts in function of isolation area: S. cerevisiae isolated from Southern Italy grapes were able to produce more volatile compounds than those from Northern Italy. The compounds synthesized by all the yeasts, besides the ethanol, were 3-methyl-1-butanol and ethyl acetate. The production of acids during the alcoholic fermentation was a characteristic of Southern yeast strains. The screening of S. cerevisiae strains for technological parameters, such as sulphur dioxide, copper and ethanol resistance or hydrogen sulphide production, revealed similar behaviour for sulphur dioxide resistance among Northern and Southern S. cerevisiae strains. Copper resistance and sulphur dioxide production were correlated to isolation area: S. cerevisiae "Northern" strains showed higher copper resistance and lowest hydrogen sulphide production than that exhibited from "Southern" strains. PMID:19269564

  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. PMID:25148961

  6. Evaluation of vapor profiles of explosives over time using ATASS (Automated Training Aid Simulation using SPME).

    PubMed

    Moore, Stephanie; Maccrehan, William; Schantz, Michele

    2011-10-10

    Despite numerous instrumental achievements, canines are still considered the most effective field method for explosive detection. However, due to strict explosive regulations and safety requirements, it can be a challenge for agencies with "bomb dogs" to train using neat explosive materials. This establishes a need for non-explosive canine training aids with the same volatile component profiles as the explosives that they represent. In order to compare mimic materials to their explosive counterparts, a technique must be established that not only allows for identification of volatile compounds but also can monitor changes in the headspace profile over time with respect to time and temperature. The Automated Training Aid Simulation using SPME (or ATASS) was developed for that purpose. As described, ATASS was used to observe changes in the volatile profile of three explosives (Composition C-4, 2,4-dinitrotoluene (DNT), and triacetone triperoxide (TATP)) and respective prototype training materials (0.1% by mass C-4, 1% by mass 2,4-DNT, and 1% by mass TATP). Samples were prepared in vials and metal tins within a gallon (≈ 3785 mL) paint can to simulate common field techniques for canine training. Monitoring these materials in real time provides a better understanding of the major volatile components present and how the relative abundances of these components can change over time. The results presented indicate that ATASS successfully allows for a sufficient comparison between explosive and non-explosive training materials. PMID:21696900

  7. 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.

  8. 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.

  9. 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. PMID:27247764

  10. Evaluation of vapor profiles of explosives over time using ATASS (Automated Training Aid Simulation using SPME).

    PubMed

    Moore, Stephanie; Maccrehan, William; Schantz, Michele

    2011-10-10

    Despite numerous instrumental achievements, canines are still considered the most effective field method for explosive detection. However, due to strict explosive regulations and safety requirements, it can be a challenge for agencies with "bomb dogs" to train using neat explosive materials. This establishes a need for non-explosive canine training aids with the same volatile component profiles as the explosives that they represent. In order to compare mimic materials to their explosive counterparts, a technique must be established that not only allows for identification of volatile compounds but also can monitor changes in the headspace profile over time with respect to time and temperature. The Automated Training Aid Simulation using SPME (or ATASS) was developed for that purpose. As described, ATASS was used to observe changes in the volatile profile of three explosives (Composition C-4, 2,4-dinitrotoluene (DNT), and triacetone triperoxide (TATP)) and respective prototype training materials (0.1% by mass C-4, 1% by mass 2,4-DNT, and 1% by mass TATP). Samples were prepared in vials and metal tins within a gallon (≈ 3785 mL) paint can to simulate common field techniques for canine training. Monitoring these materials in real time provides a better understanding of the major volatile components present and how the relative abundances of these components can change over time. The results presented indicate that ATASS successfully allows for a sufficient comparison between explosive and non-explosive training materials.

  11. 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

  12. Transport and fate of dieldrin in poplar and willow trees analyzed by SPME.

    PubMed

    Skaates, Serena V; Ramaswami, Anu; Anderson, Larry G

    2005-09-01

    Dieldrin is a hydrophobic organochlorine insecticide that is persistent in the environment. The fate and transport of dieldrin in trees is important both in the context of potential remediation, as well as food chain impacts through dieldrin transport to shoots and leaves. Experiments were conducted to measure the degree of dieldrin partitioning to plant tissue and the potential for biodegradation of dieldrin in the microbe rich tree rhizosphere. Dieldrin was analyzed in water and plant tissue using headspace solid-phase microextraction (SPME) coupled with gas chromatography. Poplar and willow saplings planted in soil and watered with 10 microgl(-1) dieldrin for up to 9 months showed no adverse effects due to dieldrin exposure and no dieldrin was observed in plant shoots with a method detection limit (MDL) of 7 ngg(-1). One-week hydroponic tests of poplar saplings exposed to aqueous dieldrin also showed no detection of dieldrin in shoots, with an average of 66% of the dieldrin partitioned to the plant roots and an overall mass balance recovery of 76% in the plant-water system. The root concentration factor (RCF) was found to be 30+/-3 ml water g(-1) root. Biodegradation of dieldrin was not observed in an aqueous batch bioreactor containing 8 microgl(-1) dieldrin, nutrients and bacteria from the root zone of a poplar sapling that had been exposed to dieldrin for 9 months. These results show that planting trees is likely to be safe and potentially useful at sites containing low-levels of dieldrin in groundwater.

  13. 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.

  14. 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. PMID:26718189

  15. 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.

  16. A water resistant solid-phase microextraction fiber with high selectivity prepared by a metal organic framework with perfluorinated pores.

    PubMed

    Niu, Jiajia; Li, Zhongyue; Yang, Huijuan; Ye, Changwen; Chen, Chen; Li, Dong; Xu, Jun; Fan, Li

    2016-04-01

    A novel solid-phase microextraction (SPME) fiber was fabricated by the construction of fluorous metal organic frameworks (FMOF) and a polyimide (PI) composite strategy. As an auxiliary material, PI was expected to help FMOF particles form well-knit film on the surface of stainless steel wire and reinforce the coating, and FMOF was expected to afford a special structure to absorb, extract and enrich. Furthermore, it was explored for the headspace SPME (HS-SPME) of six volatile aromatic compounds (VACs) from water samples followed by gas chromatographic (GC) separation with flame ionization detection. Under the optimized conditions, the fiber afforded wide linear ranges (1-1000 μgL(-1)), low detection limits (0.15-0.9 μgL(-1)) and acceptable repeatability (<4.6%) and reproducibility (<7.3%). The FMOF@PI coated fiber not only offered large enhancement factors for benzene (1227) but also exhibited high extraction selectivity for benzene to other benzene homologues, hydrocarbons and phenols; for example, the extraction ratio of benzene to toluene, n-hexane and phenol could be as high as 10.2, 64.1 and 32.3, respectively. Moreover, the FMOF@PI-coated fiber afforded good thermal, water and organic solvent stabilities, and a long lifetime (over 200 times). The developed method was successfully applied to the determination of VACs in wastewater samples. PMID:26949215

  17. Headspace-solid phase microextraction-gas chromatography-tandem mass spectrometry (HS-SPME-GC-MS2) method for the determination of pyrazines in perilla seed oils: impact of roasting on the pyrazines in perilla seed oils.

    PubMed

    Kwon, Tae Young; Park, Ji Su; Jung, Mun Yhung

    2013-09-11

    A new headspace (HS)-solid phase microextraction (SPME)-gas chromatography-tandem quadrupole mass spectrometry (GC-MS(2)) was established for the simultaneous characterization and quantitation of pyrazines in perilla seed oils. HS-SPME conditions such as fiber choice, extraction temperature, and adsorption times were tested. The established GC-MS(2) showed low detection limit (LOD) and high specificity, recovery, and precision for analysis of pyrazines in perilla seed oils. The LODs for the pyrazines were in the range of 0.07-22.22 ng/g oil. The relative standard deviations (RSDs) for the intra- and interday repeated analyses of pyrazines were less than 9.49 and 9.76%, respectively. The mean recoveries for spiked pyrazines in perilla seed oil were in the range of 94.6-107.92%. Perilla seed oils were obtained by mechanical pressing from perilla seeds roasted to different degrees of roasting (mild, medium, medium dark, and dark roasting). Fourteen pyrazine compounds in perilla seed oils were isolated, identified, and quantitated. Among them, 2-methyl-3-propylpyrazine, tetramethylpyrazine, and 2,3-diethyl-5-methylpyrazine were the first identified in perilla seed oils. Degree of roasting influenced greatly the composition and contents of pyrazines in perilla seed oils. In light-roasted perilla seed oil, 2,5-dimethylpyrazine was the most predominant pyrazine. However, in dark-roasted perilla seed oil, 2-methylpyrazine was the most abundant pyrazine in the oil, representing 38.3% of its total pyrazine content. Dark-roasted perilla seed oil contains 16.78 times higher quantity of pyrazines than light-roasted perilla seed oil. This represents the first report on the quantity of pyrazines in perilla seed oils.

  18. 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. PMID:27170778

  19. 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.

  20. Simple preparation of solid-phase microextraction fiber with cation exchange capacities using poly(butadiene-maleic acid).

    PubMed

    Zhu, Yingli; Shen, Guobin; Zhang, Feifang; Yang, Bingcheng

    2013-01-01

    A simply way was proposed to prepare solid-phase microextraction (SPME) fiber with cation-exchange functional groups by the thermally initiated radical polymerization of poly(butadiene-maleic acid) (PBMA) copolymer onto a silica capillary. The capacity of the fiber coating could be easily controlled by fabricating successive layers of PBMA. The performance of the fiber combined with ion chromatography was evaluated by choosing Mg(2+) and Ca(2+) as model analytes; ∼13 and ∼51-fold enrichment factors for Mg(2+) and Ca(2+) were obtained, respectively. PMID:24107568

  1. A sol-gel based solid phase microextraction fiber for analysis of aromatic hydrocarbons.

    PubMed

    Farhadi, Khalil; Mamaghanian, Maliheh; Maleki, Ramin

    2008-04-01

    A sol-gel based solid phase microextraction fiber for headspace sampling (HP-SPME) and GC determination of benzene, toluene, ethylbenzene and xylenes (BTEX) is introduced. The influences of fiber composition, microextraction conditions such as temperature and time on the fiber performance and desorption temperature and time were investigated. Under optimal conditions, the use of proposed fiber was thermally stable up to 250 degrees C and demonstrated high sensitive and fast sampling of BTEX from gaseous phase. Depending on the analysed substance, the linear range for a selected fiber and the applied GC-FID technique was from 4 to 80 ng mL(-1)with limit of detection (LOD) 0.2-0.7 ng mL(-1) and 100-1000 ng mL(-1) with LOD 8-20 ng mL(-1) for gaseous and soil samples, respectively. HP-SPME-GC analysis was highly reproducible-relative standard deviations (R.S.D.) were between 5.0 and 7.9%. The proposed fiber was successfully used for BTEX sampling from indoor air and headspace of soil samples. PMID:17804156

  2. 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).

  3. 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

    2007-01-01

    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.

  4. 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

    2016-03-01

    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.

  5. 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, ...

  6. 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.

  7. 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.

  8. 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. PMID:17902108

  9. 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. PMID:25277710

  10. 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.

  11. Preconcentration and determination of Sn- and Pb-organic species in environmental samples by SPME and GC-AED.

    PubMed

    Tutschku, S; Mothes, S; Wennrich, R

    1996-03-01

    A new sample preparation and preconcentration technique - solid phase microextraction (SPME) - is reported for the application of several tinorganic compounds and tetrabutyllead in aqueous samples. The solvent-free procedure is rapid in comparison with liquid-liquid extraction or SFE but also sensitive. Analytical variables of the extraction such as adsorption and desorption time, stirring rate and temperature has been investigated. The determination has been performed by GC coupled with atomic emission detection (AED). After optimization of the conditions of SPME a calibration was realized on the basis of a multicomponent standard solution, prepared by ethylation of organotin salts directly in the sample using sodium tetraethylborate (NaBEt(4)) without prior separation of the analytes from the matrix. The method permits preconcentration. Values of about 10 can be reached. A detection limit of 0.09 pg Sn and 0.08 pg Pb can be achieved under optimized conditions. The proposed procedure has been successfully applied to the analysis of organotin compounds in various slurry samples. PMID:15067450

  12. 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

  13. Discrimination of teas with different degrees of fermentation by SPME-GC analysis of the characteristic volatile flavour compounds.

    PubMed

    Wang, Li-Fei; Lee, Joo-Yeon; Chung, Jin-Oh; Baik, Joo-Hyun; So, Sung; Park, Seung-Kook

    2008-07-01

    As tea is traded all over the world, it is necessary for both customs officers and business investigators to develop an easy and reliable method to discriminate teas from each other. A total of 56 kinds of various green, Oolong, and black teas were collected from different countries and markets, and their catechin contents and volatile flavour compounds (VFC) were compared by analyses, using HPLC and solid-phase microextraction-gas chromatograph (SPME-GC). It was found that neither total catechin nor individual catechin contents in green and Oolong teas were significantly different among the samples investigated, but the fermentation processes altered the profiles of tea VFC. Because many of the individual VFC did not change in response to the fermentation levels, several VFC in combination might be more reliable than a single compound to identify broader ranges of teas. A total concentration of five VFC, trans-2-hexenal, benzaldehyde, methyl-5-hepten-2-one, methyl salicylate, and indole, was shown to be able to discriminate clearly unfermented and fermented teas, while that of trans-2-hexenal and methyl salicylate together supplied an index to differentiate semi- and fully-fermented teas. In addition, the SPME-GC analysis was also able to distinguish real jasmine teas from fake jasmine teas based on the disappearance of some grassy/green odorants.

  14. 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. PMID:22099658

  15. 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

    2012-02-01

    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.

  16. 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

    2012-02-01

    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. PMID:22209358

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

    PubMed

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

    2014-01-17

    A novel nanocomposite coating made of poly(3,4-ethylenedioxythiophene) (PEDOT) and graphene oxide was electrochemically prepared on gold wire. The prepared fiber was applied to the solid-phase microextraction (SPME) and gas chromatographic analysis of six polycyclic aromatic hydrocarbons (PAHs). Three modes of extraction i.e. direct immersion (DI), headspace (HS) and headspace cold fiber (HS-CF) in SPME were investigated. The results were compared under optimized conditions of each mode, considering the effects of the three most important parameters which are extraction temperature, extraction time and ionic strength. The comparison showed that HS-CF-SPME results in the best outcome for the extraction of PAHs from water samples. Under the optimized conditions of this mode, the calibration curves were linear within the range of 0.4-600μgL(-1) and the detection limits were between 0.05 and 0.13μgL(-1). The intra-day and inter-day relative standard deviations obtained at 10μgL(-1) (n=5), using a single fiber, were 4.1-6.8% and 4.8-8.4%, respectively. The fiber-to-fiber repeatabilities (n=4), expressed as the relative standard deviations (RSD%), were between 6.5% and 10.7% at a 10μgL(-1) concentration level. The method was successfully applied to the analysis of PAHs in seawater samples showing recoveries from 85% to 107%. PMID:24373534

  18. 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%.

  19. 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

  20. 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.

  1. Preparation and application of poly(dimethylsiloxane)/beta-cyclodextrin solid-phase microextraction fibers.

    PubMed

    Fu, Yue-Li; Hu, Yu-Ling; Zheng, Yan-Jie; Li, Gong-Ke

    2006-11-01

    A novel poly(dimethylsiloxane)/beta-cyclodextrin (PDMS/beta-CD) coating was prepared for solid-phase microextraction (SPME). The PDMS/beta-CD coating proved to have a porous structure, providing high surface areas and allowing for high extraction efficiency. The coating had a high thermal stability (340 degrees C) and a long lifetime due to its chemical binding to the fiber surface. Polar phenols and amines were used to evaluate the character of the coating fiber by headspace (HS) extraction and thermal desorption, followed by GC-FID analysis. Parameters that affected the extraction process were investigated; these include extraction time and temperature, desorption time, pH, and ionic strength of the solution. For phenols, the range of linearity of the method was 4-500 microg/L and the LOD was 1.3-2.1 microg/L. For amines, the range of linearity was 1-1000 microg/L and the LOD was 1.2-2.8 microg/L. The presence of beta-CD not only increases the thermal stability of the fiber coating, but also enhances its selectivity. Compared with commercially available SPME fibers, the new phases show better selectivity and sensitivity towards polar compounds. PMID:17313110

  2. 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…

  3. 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.

  4. 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.

  5. Qualitative analysis of the smoke-stream of different kinds of incense by SPME/GC-MS.

    PubMed

    Lombardozzi, Antonietta; Strano, Morela; Cortese, Manuela; Ricciutelli, Massimo; Vittori, Sauro; Maggi, Filippo

    2010-08-01

    Seventeen different kinds of incenses were analyzed for the volatile components emitted during burning using a HS-SPME method coupled with GC-MS, in order to check their conformity to IFRA (International Fragrance Association) guidelines and 67/548/CEE Directive rules. A total of 51 volatiles were identified in the smoke of the incenses. They were represented mainly by aromatic compounds (17) and oxygenated monoterpenes (10), with esters (5) and aldehydes (4) being the most widespread volatiles in the former, and alcohols (4) and esters (4) in the latter. The aromatic ester benzyl benzoate and the oxygenated sesquiterpene patchouli alcohol were the most frequent volatile compounds, occurring in the smokes emitted from 10 and 8 kinds of incenses, respectively.

  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

    2015-04-01

    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. 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. PMID:26614173

  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. 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.

  11. 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.

  12. Determination of benzimidazole anthelmintics in milk and honey by monolithic fiber-based solid-phase microextraction combined with high-performance liquid chromatography-diode array detection.

    PubMed

    Zhang, Yong; Huang, Xiaojia; Yuan, Dongxing

    2015-01-01

    A porous poly(methacrylic acid-co-ethylene dimethacrylate) monolithic fiber (MEMF) for solid-phase microextraction (SPME) of five benzimidazole anthelmintics was prepared by in-situ polymerization. The effect of polymerization conditions on SPME of the target analytes was studied thoroughly. The physicochemical properties of the monolith were characterized by infrared spectroscopy, elemental analysis, scanning electron microscopy, and mercury intrusion porosimetry. Several conditions affecting the extraction efficiency were investigated and, under the optimized conditions, a simple and sensitive method for the determination of trace benzimidazoles residues in milk and honey was established by coupling MEMF-SPME with high-performance liquid chromatography-diode array detection (MEMF-SPME-HPLC-DAD). Under the optimum experimental conditions, the limits of detection (S/N = 3) of the method were 0.11-0.30 μg L(-1) for milk and 0.086-0.28 μg L(-1) for honey. Evaluation of intra-day and inter-day precision showed reproducibility was satisfactory-relative standard deviations (RSD) for both were <10 %. Finally, the method was successfully used for determination of benzimidazole residues in milk and honey. Recoveries obtained for determination of benzimidazole anthelmintics in spiked samples ranged from 72.3 to 121 %, with RSD always <11 %.

  13. Sensitive and selective determination of polycyclic aromatic hydrocarbons in mainstream cigarette smoke using a graphene-coated solid-phase microextraction fiber prior to GC/MS.

    PubMed

    Wang, Xiaoyu; Wang, Yuan; Qin, Yaqiong; Ding, Li; Chen, Yi; Xie, Fuwei

    2015-08-01

    A simple method has been developed for the simultaneous determination of 16 polycyclic aromatic hydrocarbons (PAHs) in mainstream cigarette smoke. The procedure is based on employing a homemade graphene-coated solid-phase microextraction (SPME) fiber for extraction prior to GC/MS. In comparison to commercial 100-μm poly(dimethyl siloxane) (PDMS) fiber, the graphene-coated SPME fiber exhibits advantageous cleanup and preconcentration efficiencies. By collecting the particulate phase 5 cigarettes, the LODs and LOQs of 16 target PAHs were 0.02-0.07 and 0.07-0.22 ng/cigarette, respectively, and all of the linear correlation efficiencies were larger than 0.995. The validation results also indicate that the method has good repeatability (RSD between 4.2% and 9.5%) and accuracy (spiked recoveries between 80% and 110%). The developed method was applied to analyze two Kentucky reference cigarettes (1R5F and 3R4F) and six Chinese brands of cigarettes. In addition, the PAH concentrations in the particulate phase of the smoke from the 1R5F Kentucky cigarettes were in good agreement with recently reported results. Due to easy operation and good validation results, this SPME-GC/MS method may be an excellent alternative for trace analysis of PAHs in cigarette smoke.

  14. 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.

  15. 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. PMID:26653455

  16. 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.

  17. Development, validation and application of a methodology based on solid-phase micro extraction followed by gas chromatography coupled to mass spectrometry (SPME/GC-MS) for the determination of pesticide residues in mangoes.

    PubMed

    Menezes Filho, Adalberto; dos Santos, Fábio Neves; Pereira, Pedro Afonso de Paula

    2010-04-15

    A method was developed for the simultaneous analysis of 14 pesticide residues (clofentezine, carbofuran, diazinon, methyl parathion, malathion, fenthion, thiabendazole, imazalil, bifenthrin, permethrin, prochloraz, pyraclostrobin, difenoconazole and azoxystrobin) in mango fruit, based on solid-phase micro extraction (SPME) coupled to gas chromatography-mass spectrometry (GC-MS). Different parameters of the method were evaluated, such as fiber type, extraction mode (direct immersion and headspace), temperature, extraction and desorption times, stirring velocities and ionic strength. The best results were obtained using polyacrylate fiber and direct immersion mode at 50 degrees C for 30 min, along with stirring at 250 rpm and desorption for 5 min at 280 degrees C. The method was validated using mango samples spiked with pesticides at concentration levels ranging from 33.3 to 333.3 microg kg(-1). The average recoveries (n=3) for the lowest concentration level ranged from 71.6 to 117.5%, with relative standard deviations between 3.1 and 12.3%, respectively. Detection and quantification limits ranged from 1.0 to 3.3 microg kg(-1) and from 3.33 to 33.33 microg kg(-1), respectively. The optimized method was then applied to 16 locally purchased mango samples, all of them containing the pesticides bifenthrin and azoxystrobin in concentrations of 18.3-57.4 and 12.7-55.8 microg kg(-1), respectively, although these values were below the MRL established by Brazilian legislation. The method proved to be selective, sensitive, and with good precision and recovery rates, presenting LOQ below the MRL admitted by Brazilian legislation. PMID:20188930

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

    PubMed

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

    2016-08-01

    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.

  19. Determination of Polycyclic Aromatic Hydrocarbons in Sediment by Pressure-Balanced Cold Fiber Solid Phase Microextraction.

    PubMed

    Xu, Shengrui; Shuai, Qin; Pawliszyn, Janusz

    2016-09-20

    An improved performance of the cold fiber solid phase microextraction (CF-SPME) technique was accomplished with the use of the pressure-balanced procedure. In order to obtain a pressure-balanced state during extraction at 200 °C, 7 mL of air volume was withdrawn from 10 mL commercial vials, while 15 mL was withdrawn from vials where 5 μL of diethylamine was added as a modifier/displacer. The benefits of the balanced system were demonstrated for determination of polycyclic aromatic hydrocarbons (PAHs) from solid matrixes, including sand and certified sediment samples. Results showed the pressure-balanced procedure enhanced the extraction efficiency of the method, especially for high volatility compounds, as the leakage of analytes was mitigated under sample temperature conditions of 200 °C. Analytical precision was also improved, with relative standard deviations (RSDs) ranging from 4% to 8% for all analytes under study. For the determination of PAHs in certified sediment samples, pressure-balanced CF-SPME yielded more accurate results in comparison to nonpressure-balanced CF-SPME. The proposed methodology provided the additional benefit of improved recoveries at lower pressures. PMID:27562230

  20. 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

    2015-05-01

    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.

  1. Graphene coating bonded onto stainless steel wire as a solid-phase microextraction fiber.

    PubMed

    Sun, Min; Feng, Juanjuan; Bu, Yanan; Wang, Xiaojiao; Duan, Huimin; Luo, Chuannan

    2015-03-01

    A graphene coating bonded onto stainless steel wire was fabricated and investigated as a solid-phase microextraction fiber. The coating was characterized by scanning electron microscopy and energy-dispersive X-ray spectrometer. The coating with rough and crinkled structure was about 1 μm. These characteristics were helpful for promoting extraction. Using five n-alkanes (n-undecane, n-dodecane, n-tridecane, n-tetradecane and n-hexadecane) as analytes, the fiber was evaluated in direct-immersion mode by coupling with gas chromatography (GC). Through optimizing extraction and desorption conditions, a sensitive SPME-GC analytical method was established. SPME-GC method provided wide linearity range (0.2-150 μg L(-1)) and low limits of determination (0.05-0.5 μg L(-1)). It was applied to analyze rain water and a soil sample, and analytes were quantified in the range of 0.85-1.96 μg L(-1) and 0.09-3.34 μg g(-1), respectively. The recoveries of samples spiked at 10 μg L(-1) were in the range of 90.1-120% and 80.6-94.2%, respectively. The fiber also exhibited high thermal and chemical stability, due to the covalent bonds between graphene coating and wire, and the natural resistance of graphene for thermal, acid and basic conditions. PMID:25618658

  2. Graphene coating bonded onto stainless steel wire as a solid-phase microextraction fiber.

    PubMed

    Sun, Min; Feng, Juanjuan; Bu, Yanan; Wang, Xiaojiao; Duan, Huimin; Luo, Chuannan

    2015-03-01

    A graphene coating bonded onto stainless steel wire was fabricated and investigated as a solid-phase microextraction fiber. The coating was characterized by scanning electron microscopy and energy-dispersive X-ray spectrometer. The coating with rough and crinkled structure was about 1 μm. These characteristics were helpful for promoting extraction. Using five n-alkanes (n-undecane, n-dodecane, n-tridecane, n-tetradecane and n-hexadecane) as analytes, the fiber was evaluated in direct-immersion mode by coupling with gas chromatography (GC). Through optimizing extraction and desorption conditions, a sensitive SPME-GC analytical method was established. SPME-GC method provided wide linearity range (0.2-150 μg L(-1)) and low limits of determination (0.05-0.5 μg L(-1)). It was applied to analyze rain water and a soil sample, and analytes were quantified in the range of 0.85-1.96 μg L(-1) and 0.09-3.34 μg g(-1), respectively. The recoveries of samples spiked at 10 μg L(-1) were in the range of 90.1-120% and 80.6-94.2%, respectively. The fiber also exhibited high thermal and chemical stability, due to the covalent bonds between graphene coating and wire, and the natural resistance of graphene for thermal, acid and basic conditions.

  3. Characterisation of odorants emissions from landfills by SPME and GC/MS.

    PubMed

    Davoli, E; Gangai, M L; Morselli, L; Tonelli, D

    2003-05-01

    Odorous compounds from a landfill have been characterised by gas-chromatography-mass-spectrometry, identifying about 100 volatile organic compounds. Air samples from different landfill sites and from the environment have been analysed after a solid-phase microextraction on a three-phase fiber, DVB/Carboxen/PDMS, which allowed a preconcentration and the chromatographic data obtained from the most significant emission sources have been submitted to chemometric analysis in order to better establish specific markers of olfactory pollution. For example limonene was a typical tracer of fresh wastes, while p-cymene was characteristic of leachate and biogas. By the developed analytical procedure it has been evaluated the efficiency of a scrubber plant utilised in the landfill in order to remove malodour compounds. The average removal efficiency was not very high (about 23.5%) due to scarce ability in removing low polarity compounds. Furthermore, it has been demonstrated the suitability of a microgas chromatograph for the continuous on-site monitoring of air pollution in order to rapidly individuate emission sources of olfactive nuisances. PMID:12598001

  4. 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.

  5. 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%.

  6. Fabrication and application of zinc-zinc oxide nanosheets coating on an etched stainless steel wire as a selective solid-phase microextraction fiber.

    PubMed

    Song, Wenlan; Guo, Mei; Zhang, Yida; Zhang, Min; Wang, Xuemei; Du, Xinzhen

    2015-03-01

    A novel zinc-zinc oxide (Zn-ZnO) nanosheets coating was directly fabricated on an etched stainless steel wire substrate as solid-phase microextraction (SPME) fiber via previous electrodeposition of robust Zn coating. The scanning electron micrograph of the Zn-ZnO nanosheets coated fiber exhibits a flower-like nanostructure with high surface area. The SPME performance of as-fabricated fiber was investigated for the concentration and determination of polycyclic aromatic hydrocarbons, phthalates and ultraviolet (UV) filters coupled to high performance liquid chromatography with UV detection (HPLC-UV). It was found that the Zn-ZnO nanosheets coating exhibited high extraction capability, good selectivity and rapid mass transfer for some UV filters. The main parameters affecting extraction performance were investigated and optimized. Under the optimized conditions, the calibration graphs were linear over the range of 0.1-200μgL(-1). The limits of detection of the proposed method were 0.052-0.084μgL(-1) (S/N=3). The single fiber repeatability varied from 5.18% to 7.56% and the fiber-to-fiber reproducibility ranged from 6.74% to 8.83% for the extraction of spiked water with 50μgL(-1) UV filters (n=5). The established SPME-HPLC-UV method was successfully applied to the selective concentration and sensitive determination of target UV filters from real environmental water samples with recoveries from 85.8% to 105% at the spiking level of 10μgL(-1) and 30μgL(-1). The relative standard deviations were below 9.7%.

  7. Optical Fibers

    NASA Astrophysics Data System (ADS)

    Ghatak, Ajoy; Thyagarajan, K.

    With the development of extremely low-loss optical fibers and their application to communication systems, a revolution has taken fiber glass place during the last 40 years. In 2001, using glass fibers as the transmission medium and lightwaves as carrier wave waves, information was transmitted at a rate more than 1 Tbit/s (which is roughly equivalent to transmission of about 15 million simultaneous telephone conversations) through one hair thin optical fiber. Experimental demonstration of transmission at the rate of 14 Tbit/s over a 160 km long single fiber was demonstrated in 2006, which is equivalent to sending 140 digital high definition movies in 1 s. Very recently record transmission of more than 100 Tbit/s over 165 km single mode fiber has been reported. These can be considered as extremely important technological achievements. In this chapter we will discuss the propagation characteristics of optical fibers with special applications to optical communication systems and also present some of the noncommunication applications such as sensing.

  8. Preparation and characteristics of sol-gel-coated calix[4]arene fiber for solid-phase microextraction.

    PubMed

    Li, Xiujuan; Zeng, Zhaorui; Gao, Shengzhe; Li, Haibing

    2004-01-01

    5,11,17,23-Tetra-tert-butyl-25,27-diethoxy-26,28-dihydroxycalix[4]arene/hydroxy-terminated silicone oil coated fiber was first prepared and applied for solid-phase microextraction (SPME) with sol-gel technology. The possible sol-gel mechanism was discussed and confirmed by IR spectra. It showed wonderful selectivity and sensitivity to polar (aromatic amines), nonpolar (benzene derivatives, polycyclic aromatic hydrocarbons) and high boiling point compounds (phthalates) and the extraction equilibria were reached quite fast. The coating has high thermal stability (380 degrees C) and solvent stability (organic and inorganic), thus its lifetime is longer than conventional fibers. In addition, it has surprising fiber-to-fiber and batch-to-batch reproducibility. The detection limits were quite low and the linear ranges were pretty broad for all analytes.

  9. Application of Twisselmann extraction, SPME, and GC-MS to assess input sources for organophosphate esters into soil.

    PubMed

    Mihajlović, Ivana; Miloradov, Mirjana Vojinović; Fries, Elke

    2011-03-15

    Although the ubiquitous distribution of organophosphate esters (OPEs) in the environment has been documented very thoroughly, data on their occurrence in soil is so far sparse. In this study, an analytical method was developed to determine six OPEs in soil. The method consists of a combination of Twisselmann extraction and solid-phase microextraction (SPME), followed by gas chromatography-mass spectrometry (GC-MS). To develop the method, spiked soil was extracted using a Twisselmann extractor after freeze-drying. The extract was evaporated to dryness, redissolved, and filtered. A volume of 7 mL was then analyzed by SPME, followed by GC-MS. The effects of different parameters on analyte recoveries during sample preparation, e.g., solvent for Twisselmann extraction, solvent for redissolving the extract, addition of copper, and filtration of the extract, were systematically investigated. Under optimum conditions, 10 g soil samples were extracted using toluene, and the extract was redissolved in methanol/water (1:14) and filtered. It was not necessary to add copper. For TnBP, TBEP, TCPP, and TCEP, recoveries ranged from 77.0% to 89.6%. Those for TPP and TDCP were much lower, at 31.5% and 42.0%, respectively (addition level 22.9-45.8 ng g(-1)). The variability of recoveries under these conditions was between 0.3 and 16.2% (n = 3). Limits of detection (LOD) were 0.002-3 ng g(-1). When ultrasonication was used in place of Twisselmann extraction in the developed method, recoveries were three to four times lower (27.4% to 30.6%), but the variability of recoveries was below 3% (n = 3). The method was applied to quantify OPEs in soil collected from the university campus in Osnabrueck (Germany). Average concentrations (n = 6) in soil samples ranged from 1.23 ng g(-1) to 4.96 ng g(-1) (dry weight) for TCPP, TPP, and TCEP. The results demonstrate for the first time that atmospheric deposition leads to soil contamination by OPEs.

  10. Direct synthesis of nitrogen-doped graphene on platinum wire as a new fiber coating method for the solid-phase microextraction of BXes in water samples: Comparison of headspace and cold-fiber headspace modes.

    PubMed

    Memarian, Elham; Hosseiny Davarani, Saied Saeed; Nojavan, Saeed; Movahed, Siyavash Kazemi

    2016-09-01

    In this work, a new solid-phase microextraction fiber was prepared based on nitrogen-doped graphene (N-doped G). Moreover, a new strategy was proposed to solve problems dealt in direct coating of N-doped G. For this purpose, first, Graphene oxide (GO) was coated on Pt wire by electrophoretic deposition method. Then, chemical reduction of coated GO to N-doped G was accomplished by hydrazine and NH3. The prepared fiber showed good mechanical and thermal stabilities. The obtained fiber was used in two different modes (conventional headspace solid-phase microextraction and cold-fiber headspace solid-phase microextraction (CF-HS-SPME)). Both modes were optimized and applied for the extraction of benzene and xylenes from different aqueous samples. All effective parameters including extraction time, salt content, stirring rate, and desorption time were optimized. The optimized CF-HS-SPME combined with GC-FID showed good limit of detections (LODs) (0.3-2.3 μg/L), limit of quantifications (LOQs) (1.0-7.0 μg/L) and linear ranges (1.0-5000 μg/L). The developed method was applied for the analysis of benzene and xylenes in rainwater and some wastewater samples.

  11. Direct synthesis of nitrogen-doped graphene on platinum wire as a new fiber coating method for the solid-phase microextraction of BXes in water samples: Comparison of headspace and cold-fiber headspace modes.

    PubMed

    Memarian, Elham; Hosseiny Davarani, Saied Saeed; Nojavan, Saeed; Movahed, Siyavash Kazemi

    2016-09-01

    In this work, a new solid-phase microextraction fiber was prepared based on nitrogen-doped graphene (N-doped G). Moreover, a new strategy was proposed to solve problems dealt in direct coating of N-doped G. For this purpose, first, Graphene oxide (GO) was coated on Pt wire by electrophoretic deposition method. Then, chemical reduction of coated GO to N-doped G was accomplished by hydrazine and NH3. The prepared fiber showed good mechanical and thermal stabilities. The obtained fiber was used in two different modes (conventional headspace solid-phase microextraction and cold-fiber headspace solid-phase microextraction (CF-HS-SPME)). Both modes were optimized and applied for the extraction of benzene and xylenes from different aqueous samples. All effective parameters including extraction time, salt content, stirring rate, and desorption time were optimized. The optimized CF-HS-SPME combined with GC-FID showed good limit of detections (LODs) (0.3-2.3 μg/L), limit of quantifications (LOQs) (1.0-7.0 μg/L) and linear ranges (1.0-5000 μg/L). The developed method was applied for the analysis of benzene and xylenes in rainwater and some wastewater samples. PMID:27543024

  12. Determination of non-steroidal anti-inflammatory drugs in urine by hollow-fiber liquid membrane-protected solid-phase microextraction based on sol-gel fiber coating.

    PubMed

    Sarafraz-Yazdi, Ali; Amiri, Amirhassan; Rounaghi, Gholamhossein; Eshtiagh-Hosseini, Hossein

    2012-11-01

    A new rapid, simple and effective cleanup procedure is demonstrated for the determination of ibuprofen, naproxen and diclofenac in urine samples by using hollow-fiber liquid membrane-protected solid-phase microextraction (HFLM-SPME) based on sol-gel technique and gas chromatography-flame ionization detector (GC-FID). In this technique, a sol-gel coated 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 urine sample for extraction. Poly(ethylene glycol) (PEG) grafted onto multi-walled carbon nanotubes (PEG-g-MWCNTs) was used as extraction phase to prepare the sol-gel SPME fiber. Important parameters influencing the extraction efficiency such as desorption temperature and time, organic solvent, extraction temperature and time, pH, stirring speed and salt effect were investigated and optimized. Under the optimal conditions, the method detection limits (S/N=3) were in the range of 0.03-0.07ngmL(-1) and the limits of quantification (S/N=10) between 0.08 and 0.15ngmL(-1). Relative standard deviations for intra-day and inter-day precisions were 4.8-9.0% and 4.9-8.1%, respectively. Subsequently, the method was successfully applied to human urine fractions after administration of ibuprofen, naproxen and diclofenac.

  13. 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.

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

    PubMed

    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

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

    PubMed

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

    2014-12-01

    The confirmation of Δ9-tetrahydrocannabinol (THC) in oral fluid (OF) is an important issue for assessing Driving Under the Influence of Drugs (DUID). The aim of this research was to develop a highly sensitive method with minimal sample pre-treatment suitable for the analysis of small OF volumes (100 μL) for the confirmation of cannabinoids in DUID cases. Two methods were compared for the confirmation of THC in residual OF samples, obtained from a preliminary on-site screening with commercial devices. An ultra high performance LC-MS (UHPLC-MS/MS) method and an SPME-GC/MS method were hence developed. 100 μL of the residual mixture OF/preservative buffer or neat OF was simply added to 10 μL of THC-D3 (1 μg/mL) and submitted to the two different analyses: A - direct injection of 10 μL in UHPLC-MS/MS in positive electrospray ionisation (ESI) mode and B - sampling for 30 min with SPME (100 μm polydimethylsiloxane or PDMS fibre) and direct injection by desorption of the fibre in the GC injection port. The lowest limit of detection (LLOD) of THC was 2 ng/mL in UHPLC-MS/MS and 0.5 ng/mL in SPME-GC/MS. In addition, cannabidiol (CBD) and cannabinol (CBN) could be detected in GC/MS equipment at 2 ng/mL, whilst in UHPLC-MS/MS the LLOD was 20 ng/mL. Both methods were applied to 70 samples coming from roadside tests. By SPME-GC/MS analysis, THC was confirmed in 42 samples, whilst CBD was detected in 21 of them, along with CBN in 14 samples. THC concentrations ranged from traces below the lowest limit of quantification or LLOQ (2 ng/mL) up to 690 ng/mL. PMID:25498928

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

    PubMed

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

    2016-08-17

    A new molecularly imprinted polymer modified with restricted access material (a hydrophilic external layer), (MIP-RAM) was synthesized via polymerization in situ in an open fused silica capillary. This stationary phase was used as sorbent for in-tube solid phase microextraction (in-tube SPME) to determine parabens in breast milk samples by ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Scanning electron micrographs (SEM) illustrate MIP surface modification after glycerol dimethacrylate (hydrophilic monomer) incorporation. The interaction between parabens and MIP-RAM was investigated by Fourier-transform infrared (FTIR) spectroscopy. The Scatchard plot for MIP-RAM presented two linear parts with different slopes, illustrating binding sites with high- and low-affinity. Endogenous compounds exclusion from the MIP-RAM capillary was demonstrated by in-tube SPME/LC-UV assays carried out with blank milk samples. The in-tube SPME/UHPLC-MS/MS method presented linear range from 10 ng mL(-1) (LLOQ) to 400 ng mL(-1) with coefficients of determination higher than 0.99, inter-assay precision with coefficient of variation (CV) values ranging from 2 to 15%, and inter-assay accuracy with relative standard deviation (RSD) values ranging from -1% to 19%. Analytical validation parameters attested that in-tube SPME/UHPLC-MS/MS is an appropriate method to determine parabens in human milk samples to assess human exposure to these compounds. Analysis of breast milk samples from lactating women demonstrated that the proposed method is effective. PMID:27286769

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

    PubMed

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

    2016-08-17

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

  19. Determination of different recreational drugs in sweat by headspace solid-phase microextraction gas chromatography mass spectrometry (HS-SPME GC/MS): Application to drugged drivers.

    PubMed

    Gentili, Stefano; Mortali, Claudia; Mastrobattista, Luisa; Berretta, Paolo; Zaami, Simona

    2016-09-10

    A procedure based on headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography/mass spectrometry (GC/MS) has been developed for the determination of most commonly used drugs of abuse in sweat of drivers stopped during roadside controls. DrugWipe 5A sweat screening device was used to collect sweat by a specific pad rubbed gently over forehead skin surface. The procedure involved an acid hydrolysis, a HS-SPME extraction for drugs of abuse but Δ(9)-tetrahydrocannabinol, which was directly extracted in alkaline medium HS-SPME conditions, a GC separation of analytes by a capillary column and MS detection by electron impact ionisation. The method was linear from the limit of quantification (LOQ) to 50ng drug per pad (r(2)≥0.99), with an intra- and inter-assay precision and accuracy always less than 15% and an analytical recovery between 95.1% and 102.8%, depending on the considered analyte. Using the validated method, sweat from 60 apparently intoxicated drivers were found positive to one or more drugs of abuse, showing sweat patches testing as a viable economic and simple alternative to conventional (blood and/or urine) and non conventional (oral fluid) testing of drugs of abuse in drugged drivers. PMID:27442890

  20. Determination of organophosphorus fire retardants and plasticizers in wastewater samples using MAE-SPME with GC-ICPMS and GC-TOFMS detection.

    PubMed

    Ellis, Jenny; Shah, Monika; Kubachka, Kevin M; Caruso, Joseph A

    2007-12-01

    Determination of organophosphorus fire retardants and plasticizers at trace levels in wastewater is described. In this work, microwave assisted extraction (MAE) and solid-phase microextraction (SPME) are used for sample preparation to extract and preconcentrate the analytes, followed by analysis by gas chromatography coupled to inductively coupled plasma mass spectrometry (GC-ICP-MS) for phosphorus-specific detection. Gas chromatography coupled to time of flight mass spectrometry (GC-TOF-MS) was used to confirm the organphosphorus fire retardants in wastewater. The detection limits of organophosphorus fire retardants (OPFRs) were 29 ng L(-1) for tri-n-butyl phosphate (TnBP), 45 ng for L(-1) for tris(2-butoxyethyl)phosphate (TBEP), and 50 ng L(-1) for tris(2-ethylhexyl)phosphate (TEHP). Optimized extraction conditions were performed at 65 degrees C for 30 min and with 10% NaCl. Application of MAE during the sample preparation prior to the SPME allowed the detection of tris(2-ethylhexyl) phosphate, which has been difficult to determine in previous work. Application of the method to wastewater samples resulted in detecting 3.1 microg L(-1) P from TnBP, 5.0 microg L(-1) P from TBEP, and 4.0 microg L(-1) P from TEHP. The presence of these compounds were also confirmed by SPME-GC-TOF-MS.

  1. Differentiation of manuka honey from kanuka honey and from jelly bush honey using HS-SPME-GC/MS and UHPLC-PDA-MS/MS.

    PubMed

    Beitlich, Nicole; Koelling-Speer, Isabelle; Oelschlaegel, Stefanie; Speer, Karl

    2014-07-01

    In the present study, pollen-identical pure manuka and kanuka honeys and an Australian jelly bush honey were analyzed for the nonvolatiles by UHPLC-PDA-MS/MS and for the volatiles by HS-SPME-GC/MS. A chromatographic profile matchup by means of characteristic marker compounds achieved a clear discrimination between manuka, kanuka, and jelly bush honey. UHPLC-PDA profiles of manuka honey show leptosin, acetyl-2-hydroxy-4-(2-methoxyphenyl)-4-oxobutanate, 3-hydroxy-1-(2-methoxyphenyl)-penta-1,4-dione, kojic acid, 5-methyl-3-furancarboxylic acid, and two unknown compounds as prominent, kanuka honey was characterized by 4-methoxyphenyllactic acid, methyl syringate, p-anisic acid, and lumichrome. 2-Methylbenzofuran, 2'-hydroxyacetophenone, and 2'-methoxyacetophenone were markant volatiles for manuka honey, whereas kanuka honey was characterized by 2,6,6-trimethyl-2-cyclohexene-1,4-dione, phenethyl alcohol, p-anisaldehyde, and an unknown compound in HS-SPME-GC/MS. The jelly bush honey differed from the manuka honey by higher contents of 2-methoxybenzoic acid and an individual unknown substance in the PDA profile and by lower intensities of 2'-methoxyacetophenone, higher concentrations of cis-linalool oxide, and 3,4,5-trimethylphenol in the HS-SPME-GC/MS profile.

  2. Differentiation of manuka honey from kanuka honey and from jelly bush honey using HS-SPME-GC/MS and UHPLC-PDA-MS/MS.

    PubMed

    Beitlich, Nicole; Koelling-Speer, Isabelle; Oelschlaegel, Stefanie; Speer, Karl

    2014-07-01

    In the present study, pollen-identical pure manuka and kanuka honeys and an Australian jelly bush honey were analyzed for the nonvolatiles by UHPLC-PDA-MS/MS and for the volatiles by HS-SPME-GC/MS. A chromatographic profile matchup by means of characteristic marker compounds achieved a clear discrimination between manuka, kanuka, and jelly bush honey. UHPLC-PDA profiles of manuka honey show leptosin, acetyl-2-hydroxy-4-(2-methoxyphenyl)-4-oxobutanate, 3-hydroxy-1-(2-methoxyphenyl)-penta-1,4-dione, kojic acid, 5-methyl-3-furancarboxylic acid, and two unknown compounds as prominent, kanuka honey was characterized by 4-methoxyphenyllactic acid, methyl syringate, p-anisic acid, and lumichrome. 2-Methylbenzofuran, 2'-hydroxyacetophenone, and 2'-methoxyacetophenone were markant volatiles for manuka honey, whereas kanuka honey was characterized by 2,6,6-trimethyl-2-cyclohexene-1,4-dione, phenethyl alcohol, p-anisaldehyde, and an unknown compound in HS-SPME-GC/MS. The jelly bush honey differed from the manuka honey by higher contents of 2-methoxybenzoic acid and an individual unknown substance in the PDA profile and by lower intensities of 2'-methoxyacetophenone, higher concentrations of cis-linalool oxide, and 3,4,5-trimethylphenol in the HS-SPME-GC/MS profile. PMID:24941132

  3. 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.

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

    PubMed

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

    2016-09-01

    The investigation of explosive events requires appropriate evidential protocols to recover and preserve residues from the scene. In this study, a central composite design was used to determine statistically validated optimum recovery parameters for double-base smokeless powder residues on steel, analysed using total vaporisation (TV) SPME/GC-MS. It was found that maximum recovery was obtained using isopropanol-wetted swabs stored under refrigerated conditions, then extracted for 15min into acetone on the same day as sample collection. These parameters were applied to the recovery of post-blast residues deposited on steel witness surfaces following a PVC pipe bomb detonation, resulting in detection of all target components across the majority of samples. Higher overall recoveries were obtained from plates facing the sides of the device, consistent with the point of first failure occurring in the pipe body as observed in previous studies. The methodology employed here may be readily applied to a variety of other explosive compounds, and thus assist in establishing 'best practice' procedures for explosive investigations. PMID:27343617

  5. 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.

  6. 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.

  7. Analysis of volatile compounds of Iberian dry-cured loins with different intramuscular fat contents using SPME-DED.

    PubMed

    Ventanas, Sonia; Estevez, Mario; Andrés, Ana I; Ruiz, Jorge

    2008-05-01

    In order to study the effect of both, ripening time and IMF content on the volatile profile of Iberian dry-cured loin, volatile compounds from the headspace of 10 Iberian dry-cured loins with different intramuscular fat contents (IMF), low (average IMF content of 2.3%) and high (average IMF content of 6.7%), at days 40 and 55 of the ripening process were analysed using SPME coupled to a direct extraction device (DED) and subsequent gas chromatography/mass spectrometry (GC/MS). Chromatographic areas of the main chemical families detected (hydrocarbons, aldehydes, alcohols, ketones and acids) increased with ripening time. A higher total chromatographic area was detected in the headspace of high IMF loins compared to low IMF ones. Several volatile compounds derived from lipid oxidative reactions, such as hexanol, octanal, (E,E)-2,4-heptadienal or (E)-2-decenal, and others from the degradation of certain amino acids, such as dimethylsulfide, 3-methylbutanal or phenylacetaldehyde, showed higher chromatographic areas in the headspace of high IMF loins than in low IMF ones. Thus, IMF content could influence both the generation of volatile compounds and the transfer of such compounds from the product matrix to the headspace.

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

    PubMed Central

    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. PMID:25237349

  9. 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

    2012-11-01

    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.

  10. 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. PMID:26753984

  11. 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.

  12. 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.

  13. 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

  14. 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.

  15. Simple fabrication of solid phase microextraction fiber employing nitrogen-doped ordered mesoporous polymer by in situ polymerization.

    PubMed

    Zheng, Juan; Liang, Yeru; Liu, Shuqin; Jiang, Ruifen; Zhu, Fang; Wu, Dingcai; Ouyang, Gangfeng

    2016-01-01

    A combination of nitrogen-doped ordered mesoporous polymer (NOMP) and stainless steel wires led to highly sensitive, selective, and stable solid phase microextraction (SPME) fibers by in situ polymerization for the first time. The ordered structure of synthesized NOMP coating was illustrated by transmission electron microscopy (TEM) and X-ray diffraction (XRD), and microscopy analysis by scanning electron microscopy (SEM) confirmed a homogenous morphology of the NOMP-coated fiber. The NOMP-coated fiber was further applied for the extraction of organochlorine pesticides (OCPs) with direct-immersion solid-phase microextraction (DI-SPME) method followed by gas chromatography-mass spectrometry (GC-MS) quantification. Under the optimized conditions, low detection limits (0.023-0.77 ng L(-1)), a wide linear range (9-1500 ng L(-1)), good repeatability (3.5-8.1%, n=6) and excellent reproducibility (1.5-8.3%, n=3) were achieved. Moreover, the practical feasibility of the proposed method was evaluated by determining OCPs in environmental water samples with satisfactory recoveries. PMID:26702590

  16. 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. PMID:27457562

  17. 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.

  18. 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.

  19. 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.

  20. Polypyrrole nanowire as an excellent solid phase microextraction fiber for bisphenol A analysis in food samples followed by ion mobility spectrometry.

    PubMed

    Kamalabadi, Mahdie; Mohammadi, Abdorreza; Alizadeh, Naader

    2016-08-15

    A polypyrrole nanowire coated fiber was prepared and used in head-space solid phase microextraction coupled with ion mobility spectrometry (HS-SPME-IMS) to the analysis of bisphenol A (BPA) in canned food samples, for the first time. This fiber was synthesized by electrochemical oxidation of the monomer in aqueous solution. The fiber characterization by scanning electron microscopy (SEM) revealed that the new fiber exhibited two-dimensional structures with a nanowire morphology. The effects of important extraction parameters on the efficiency of HS-SPME were investigated and optimized. Under the optimum conditions, the linearity of 10-150ngg(-1) and limit of detection (based on S/N=3) of 1ngg(-1) were obtained in BPA analysis. The repeatability (n=5) expressed as the relative standard deviation (RSD%) was 5.8%. At the end, the proposed method was successfully applied to determine BPA in various canned food samples (peas, corns, beans). Relative recoveries were obtained 93-96%. Method validation was conducted by comparing our results with those obtained through HPLC with fluorescence detection (FLD). Compatible results indicate that the proposed method can be successfully used in BPA analysis. This method is simple and cheaper than chromatographic methods, with no need of extra organic solvent consumption and derivatization prior to sample introduction. PMID:27260447

  1. 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

    2012-01-01

    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.

  2. 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. PMID:24054558

  3. 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.

  4. 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

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

    PubMed

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

    2016-02-15

    We propose a general coupling of the Smooth Particle Mesh Ewald SPME approach for distributed multipoles to a short-range charge penetration correction modifying the charge-charge, charge-dipole and charge-quadrupole energies. Such an approach significantly improves electrostatics when compared to ab initio values and has been calibrated on Symmetry-Adapted Perturbation Theory reference data. Various neutral molecular dimers have been tested and results on the complexes of mono- and divalent cations with a water ligand are also provided. Transferability of the correction is adressed in the context of the implementation of the AMOEBA and SIBFA polarizable force fields in the TINKER-HP software. As the choices of the multipolar distribution are discussed, conclusions are drawn for the future penetration-corrected polarizable force fields highlighting the mandatory need of non-spurious procedures for the obtention of well balanced and physically meaningful distributed moments. Finally, scalability and parallelism of the short-range corrected SPME approach are addressed, demonstrating that the damping function is computationally affordable and accurate for molecular dynamics simulations of complex bio- or bioinorganic systems in periodic boundary conditions. PMID:26814845

  6. Determination of a wide range of volatile and semivolatile organic compounds in snow by use of solid-phase micro-extraction (SPME).

    PubMed

    Kos, Gregor; Ariya, Parisa A

    2006-05-01

    Quantification and transformation of organic compounds are pivotal in understanding atmospheric processes, because such compounds contribute to the oxidative capacity of the atmosphere and drive climate change. It has recently been recognized that chemical reactions in snow play a role in the production or destruction of photolabile volatile organic compounds (VOC). We present an environmentally friendly method for determination of VOC and semi-VOC in snow collected at three sites-remote, urban, and (sub-)arctic. A solid-phase micro-extraction (SPME) procedure was developed and (semi-)VOC were identified by gas chromatography with mass spectrometric detection (GC-MS). A broad spectrum of (semi-)VOC was found in snow samples, including aldehydes, and aromatic and halogenated compounds. Quantification was performed for 12 aromatic and/or oxygenated compounds frequently observed in snow by use of neat standard solutions. The concentrations detected were between 0.12 (styrene and ethylbenzene) and 316 microg L(-1) (toluene) and limits of detection varied between 0.11 (styrene) and 1.93 microg L(-1) (benzaldehyde). These results indicate that the SPME technique presented is a broad but selective, versatile, solvent-free, ecological, economical, and facile method of analysis for (semi-)VOC in natural snow samples.

  7. Screening of volatile compounds in honey using a new sampling strategy combining multiple extraction temperatures in a single assay by HS-SPME-GC-MS.

    PubMed

    Bianchin, Joyce Nunes; Nardini, Giuliana; Merib, Josias; Dias, Adriana Neves; Martendal, Edmar; Carasek, Eduardo

    2014-02-15

    This paper proposes a new optimization strategy for the extraction of volatile compounds from honey samples using headspace solid-phase microextraction (HS-SPME) and separation/detection by gas chromatography-mass spectrometry (GC-MS). The new optimization strategy was based on the use of three different extraction temperatures in a single assay, aiming at extracting a high number of compounds with wide range of volatilities. As an analytical tool, experimental designs were used for the optimization. The variables extraction time (10-80 min), extraction temperature (0-60 °C), water volume (0.5-5 mL) and percentage of sodium chloride saturation in water (0-100%) were optimised using a five-level fractional central composite design with CAR/DVB/PDMS fibre. The final optimised combination of extraction times at each temperature was 60 min with the sample temperature being held at 60 °C for 36 min, 40 °C for 18 min and 0 °C for 6 min. The proposed method was compared to conventional methods which employ one or two extraction temperatures. It was found that the proposed method presented better results considering the response in terms of the arithmetic means of the peak areas. The use of multiple extraction temperatures for the HS-SPME procedure proved to be an excellent alternative for the screening of compounds present in honey with a wide range of volatilities. PMID:24128584

  8. Frog volatile compounds: application of in vivo SPME for the characterization of the odorous secretions from two species of Hypsiboas treefrogs.

    PubMed

    Brunetti, Andrés E; Merib, Josias; Carasek, Eduardo; Caramão, Elina B; Barbará, Janaina; Zini, Claudia A; Faivovich, Julián

    2015-04-01

    A novel in vivo design was used in combination with solid-phase microextraction (SPME) and gas chromatography/mass spectrometry (GC/MS) to characterize the volatile compounds from the skin secretion of two species of tree frogs. Conventional SPME-GC/MS also was used for the analysis of volatiles present in skin samples and for the analysis of volatiles present in the diet and terraria. In total, 40 and 37 compounds were identified in the secretion of Hypsiboas pulchellus and H. riojanus, respectively, of which, 35 were common to both species. Aliphatic aldehydes, a low molecular weight alkadiene, an aromatic alcohol, and other aromatics, ketones, a methoxy pyrazine, sulfur containing compounds, and hemiterpenes are reported here for the first time in anurans. Most of the aliphatic compounds seem to be biosynthesized by the frogs following different metabolic pathways, whereas aromatics and monoterpenes are most likely sequestered from environmental sources. The characteristic smell of the secretion of H. pulchellus described by herpetologists as skunk-like or herbaceous is explained by a complex blend of different odoriferous components. The possible role of the volatiles found in H. pulchellus and H. riojanus is discussed in the context of previous hypotheses about the biological function of volatile secretions in frogs (e.g., sex pheromones, defense secretions against predators, mosquito repellents). PMID:25912225

  9. 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).

  10. Frog volatile compounds: application of in vivo SPME for the characterization of the odorous secretions from two species of Hypsiboas treefrogs.

    PubMed

    Brunetti, Andrés E; Merib, Josias; Carasek, Eduardo; Caramão, Elina B; Barbará, Janaina; Zini, Claudia A; Faivovich, Julián

    2015-04-01

    A novel in vivo design was used in combination with solid-phase microextraction (SPME) and gas chromatography/mass spectrometry (GC/MS) to characterize the volatile compounds from the skin secretion of two species of tree frogs. Conventional SPME-GC/MS also was used for the analysis of volatiles present in skin samples and for the analysis of volatiles present in the diet and terraria. In total, 40 and 37 compounds were identified in the secretion of Hypsiboas pulchellus and H. riojanus, respectively, of which, 35 were common to both species. Aliphatic aldehydes, a low molecular weight alkadiene, an aromatic alcohol, and other aromatics, ketones, a methoxy pyrazine, sulfur containing compounds, and hemiterpenes are reported here for the first time in anurans. Most of the aliphatic compounds seem to be biosynthesized by the frogs following different metabolic pathways, whereas aromatics and monoterpenes are most likely sequestered from environmental sources. The characteristic smell of the secretion of H. pulchellus described by herpetologists as skunk-like or herbaceous is explained by a complex blend of different odoriferous components. The possible role of the volatiles found in H. pulchellus and H. riojanus is discussed in the context of previous hypotheses about the biological function of volatile secretions in frogs (e.g., sex pheromones, defense secretions against predators, mosquito repellents).

  11. Automated SPME-GC-MS monitoring of headspace metabolomic responses of E. coli to biologically active components extracted by the coating.

    PubMed

    Hossain, S M Zakir; Bojko, Barbara; Pawliszyn, Janusz

    2013-05-01

    Monitoring extracellular metabolites of bacteria is very useful for not only metabolomics research but also for assessment of the effects of various chemicals, including antimicrobial agents and drugs. Herein, we describe the automated headspace solid-phase microextraction (HS-SPME) method coupled with gas chromatography-mass spectrometry (GC-MS) for the qualitative as well as semi-quantitative determination of metabolic responses of Escherichia coli to an antimicrobial agent, cinnamaldehyde. The minimum inhibitory concentration of cinnamaldehyde was calculated to be 2 g L(-1). We found that cinnamaldehyde was an important factor influencing the metabolic profile and growth process. A higher number of metabolites were observed during the mid-logarithmic growth phase. The metabolite variations (types and concentrations) induced by cinnamaldehyde were dependent on both cell density and the dose of cinnamaldehyde. Simultaneously, 25 different metabolites were separated and detected (e.g., indole, alkane, alcohol, organic acids, esters, etc.) in headspace of complex biological samples due to intermittent addition of high dose of cinnamaldehyde. The study was done using an automated system, thereby minimizing manual workup and indicating the potential of the method for high-throughput analysis. These findings enhanced the understanding of the metabolic responses of E. coli to cinnamaldehyde shock effect and demonstrated the effectiveness of the SPME-GC-MS based metabolomics approach to study such a complex biological system. PMID:23601279

  12. 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.

  13. Determination of furfural and hydroxymethylfurfural from baby formula using headspace solid phase microextraction based on nanostructured polypyrrole fiber coupled with ion mobility spectrometry.

    PubMed

    Kamalabadi, Mahdie; Ghaemi, Elham; Mohammadi, Abdorreza; Alizadeh, Naader

    2015-08-15

    Furfural (Fu) and hydroxymethylfurfural (HMFu) are extracted using a dodecylbenzenesulfonate-doped polypyrrole coating as a fiber for headspace solid phase microextraction (HS-SPME) method in baby formula samples and detected using ion mobility spectrometry (IMS). Sample pH, salt effect, extraction time and temperature were investigated and optimized as effective parameters in HS-SPME. The calibration curves were linear in the range of 20-300 ng g(-1) (R(2)>0.99). Limits of detection for Fu and HMFu were 6 ng g(-1) and 5 ng g(-1), respectively. The RSD% of Fu and HMFu for five analyses was 4.4 and 4.9, respectively. The proposed method was successfully applied to determine of Fu and HMFu in the different baby formula samples with satisfactory result. The results were in agreement with those obtained using HPLC analysis. The HS-SPME-IMS is precise, selective and sensitive analytical method for determination of Fu and HMFu in baby formula samples, without any derivatization process.

  14. Solid phase microextraction using new sol-gel hybrid polydimethylsiloxane-2-hydroxymethyl-18-crown-6-coated fiber for determination of organophosphorous pesticides.

    PubMed

    Wan Ibrahim, Wan Aini; Farhani, Hadijah; Sanagi, Mohd Marsin; Aboul-Enein, Hassan Y

    2010-07-23

    A new sol-gel hybrid coating, polydimethylsiloxane-2-hydroxymethyl-18-crown-6 (PDMS-2OHMe18C6) was prepared in-house for use in solid phase microextraction (SPME). The three compositions produced were assessed for its extraction efficiency towards three selected organophosphorus pesticides (OPPs) based on peak area extracted obtained from gas chromatography with electron capture detection. All three compositions showed superior extraction efficiencies compared to commercial 100 microm PDMS fiber. The composition showing best extraction performance was used to obtain optimized SPME conditions: 75 degrees C extraction temperature, 10 min extraction time, 120 rpm stirring rate, desorption time 5 min, desorption temperature 250 degrees C and 1.5% (w/v) of NaCl salt addition. The method detection limits (S/N=3) of the OPPs with the new sol-gel hybrid material ranged from 4.5 to 4.8 ng g(-1), which is well below the maximum residue limit set by Codex Alimentarius Commission and European Commission. Percentage recovery of OPPs from strawberry, green apple and grape samples with the new hybrid sol-gel SPME material ranged from 65 to 125% with good precision of the method (%RSD) ranging from 0.3 to 7.4%.

  15. Highly porous solid-phase microextraction fiber coating based on poly(ethylene glycol)-modified ormosils synthesized by sol-gel technology.

    PubMed

    da Costa Silva, Raquel Gomes; Augusto, Fabio

    2005-04-22

    The preparation and characteristics of solid-phase microextraction (SPME) fibers coated with Carbowax 20M ormosil (organically modified silica) are described here. Raw fused silica fibers were coated with Carbowax 20M-modified silica using sol-gel process. Scanning electron micrographs of fibers revealed a highly porous, sponge-like coating with an average thickness of (8 +/- 1) microm. The sol-gel Carbowax fibers were compared to commercial fibers coated with 100 microm polydimethylsiloxane (PDMS) and 65 microm Carbowax-divinylbenzene (DVB). Shorter equilibrium times were possible with the sol-gel Carbowax fiber: for headspace extraction of the test analytes, they ranged from less than 3 min for benzene to 15 min for o-xylene. Extraction efficiencies of the sol-gel Carbowax fiber were superior to those of conventional fibers: for o-xylene, the extracted masses were 230 and 540% of that obtained with 100 microm PDMS and 65 microm Carbowax-DVB fibers, respectively. PMID:15881453

  16. Low-fiber diet

    MedlinePlus

    ... restricted diet; Crohn disease - low fiber diet; Ulcerative colitis - low fiber diet; Surgery - low fiber diet ... of: Irritable bowel syndrome Diverticulitis Crohn disease Ulcerative colitis Sometimes people are put on this diet after ...

  17. Fiber distributed feedback laser

    NASA Technical Reports Server (NTRS)

    Elachi, C.; Evans, G. A.; Yeh, C. (Inventor)

    1976-01-01

    Utilizing round optical fibers as communication channels in optical communication networks presents the problem of obtaining a high efficiency coupling between the optical fiber and the laser. A laser is made an integral part of the optical fiber channel by either diffusing active material into the optical fiber or surrounding the optical fiber with the active material. Oscillation within the active medium to produce lasing action is established by grating the optical fiber so that distributed feedback occurs.

  18. Strong fibers

    SciTech Connect

    Li, Che-Yu.

    1991-03-01

    This program was directed to a new and generic approach to the development of new materials with novel and interesting properties, and to the precision fabrication of these materials in one and two-dimensional forms. Advanced deposition processes and microfabrication technology were used to produce fibers and grids of metals, semiconductors, ceramics, and mixtures of controlled composition and structure, and with new and interesting mechanical and physical properties. Deposition processes included electron beam evaporation, co-deposition of mixtures by dual electron beam evaporation, thermal evaporation, sputtering of a single element or compound, sputtering of a single element in a gaseous atmosphere to produce compounds, plasma enhanced chemical vapor deposition (PECVD), low pressure chemical vapor deposition (LPCVD), and selective tungsten chemical vapor deposition (W-CVD). The approach was to use the deposition processes in coordination with patterns generated by optical lithography to produce fibers with transverse dimensions in the micron range, and lengths from less than a millimeter to several centimeters. The approach is also applicable to the production of two-dimensional grids and particulates of controlled sizes and geometries.

  19. 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.

  20. 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. PMID:26838393

  1. Determination of polycyclic aromatic hydrocarbons from ambient air particulate matter using a cold fiber solid phase microextraction gas chromatography-mass spectrometry method.

    PubMed

    Menezes, Helvécio Costa; de Lourdes Cardeal, Zenilda

    2011-05-27

    Polycyclic aromatic hydrocarbons (PAH) from ambient air particulate matter (PM) were analyzed by a new method that utilized direct immersion (DI) and cold fiber (CF) SPME-GC/MS. Experimental design was used to optimize the conditions of extraction by DI-CF-SPME with a 100μm polydimethylsiloxane (PDMS) fiber. The optimal conditions included a 5min equilibration at 70°C time in an ultrasonic bath with an extraction time of 60min. The optimized method was validated by the analysis of a NIST standard reference material (SRM), 1649b urban dust. The results obtained were in good agreement with certified values. PAH recoveries for reference materials were between 88 and 98%, with a relative standard deviation ranging from 5 to 17%. Detection limits (LOD) varied from 0.02 to 1.16ng and the quantification limits (LOQ) varied from 0.05 to 3.86ng. The optimized and validated method was applied to the determination of PAH from real particulate matter (PM10) and total suspended particulate (TPS) samples collected on quartz fiber filters with high volume samplers.

  2. Headspace solid-phase microextraction with on-fiber derivatization for the determination of aldehydes in algae by gas chromatography-mass spectrometry.

    PubMed

    Ma, Jiping; Xiao, Ronghui; Li, Jinhua; Li, Jie; Shi, Benzhang; Liang, Yanjuan; Lu, Wenhui; Chen, Lingxin

    2011-06-01

    A simple, fast, sensitive and cost-effective method based on headspace solid-phase microextraction (HS-SPME) with on-fiber derivatization coupled with gas chromatography-mass spectrometry was developed for the determination of six typical aldehydes, 2E-hexenal, heptanal, 2E-heptenal, 2E,4E-heptadienal, 2E-decenal and 2E,4E-decadienal in laboratory algae cultures. As derivatization reagent, O-2,3,4,5,6-(pentafluorobenzyl) hydroxylamine hydrochloride, was loaded onto the poly(dimethylsiloxane)/divinylbenzene fiber for aldehydes on-fiber derivatization prior to HS-SPME. Various influence factors of extraction efficiency were systematically investigated. Under optimized extraction conditions, excellent method performances for all the six aldehydes were attained, such as satisfactory extraction recoveries ranging from 67.1 to 117%, with the precision (relative standard deviation) within 5.3-11.1%, and low detection limits in the range of 0.026-0.044 μg/L. The validated method was successfully applied for the analysis of the aldehydes in two diatoms (Skeletonema costatum and Chaetoceros muelleri), two pyrrophytas (Prorocentrum micans and Scrippsiella trochoidea) and Calanus sinicus eggs (feeding on the two diatoms above). PMID:21567947

  3. [Preparation of a solid-phase microextraction fiber coated with gamma-Al2O3 and determination of volatile organic compounds in aqueous and gaseous samples].

    PubMed

    Wei, Liming; Li, Jubai; Wang, Guojun; Ou, Qingyu

    2004-07-01

    A method for the preparation of a novel gamma-Al2O3 coated layer on fibers for solid-phase microextraction (SPME) was developed. The adsorption and desorption properties of the coated fibers were studied by the extraction of some volatile organic compounds such as benzene, toluene, ethylbenzene and xylene isomers (BTEXs) from aqueous samples. The calibration graphs were linear in the range 0.01 mg/L to 3 mg/L and the detection limits for BTEX compounds were between 1 microg/L and 10 microg/L. Also the gamma-Al2O3 coated fibers exhibited a good thermal stability (to 350 degrees C ) and reproducibility with relative standard deviation of 8.3%. It can be used to determine organic compounds in the real gaseous samples.

  4. 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. PMID:27592610

  5. 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.

  6. 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.

  7. Coupling of SPME with MCC/UV-IMS as a tool for rapid on-site detection of groundwater and surface water contamination.

    PubMed

    Walendzik, G; Baumbach, J I; Klockow, D

    2005-08-01

    The combination of headspace solid phase microextraction (HS-SPME) [1] with fast chromatographic pre-separation by means of multi-capillary columns (MCC) coupled to an ion mobility spectrometer equipped with a 10.6 eV photoionisation source was applied to rapid on-site monitoring of ground and surface water contaminations. Under field conditions, water contaminants were directly detectable down to the upper microg/L range. The potential of the developed method is illustrated by measurements of BTEX, naphthalene, chlorinated alkenes and chlorinated benzenes in water. Practical results from investigations of contaminated groundwater at a former gasworks site and groundwater from the site of a metal processing plant, focusing on the key substances benzene, naphthalene and tetrachloroethene, demonstrate the feasibility of the system for field studies. PMID:16059675

  8. Coupling of SPME with MCC/UV-IMS as a tool for rapid on-site detection of groundwater and surface water contamination.

    PubMed

    Walendzik, G; Baumbach, J I; Klockow, D

    2005-08-01

    The combination of headspace solid phase microextraction (HS-SPME) [1] with fast chromatographic pre-separation by means of multi-capillary columns (MCC) coupled to an ion mobility spectrometer equipped with a 10.6 eV photoionisation source was applied to rapid on-site monitoring of ground and surface water contaminations. Under field conditions, water contaminants were directly detectable down to the upper microg/L range. The potential of the developed method is illustrated by measurements of BTEX, naphthalene, chlorinated alkenes and chlorinated benzenes in water. Practical results from investigations of contaminated groundwater at a former gasworks site and groundwater from the site of a metal processing plant, focusing on the key substances benzene, naphthalene and tetrachloroethene, demonstrate the feasibility of the system for field studies.

  9. Review: DNA oxidation, its consequences and efficacy of GC-MS and SPME-GC-MS for In Vitro quantification of DNA oxidative products

    NASA Astrophysics Data System (ADS)

    Singh, Himansha; Udawat, Abhishek; Franklin, Tony; Sarathi, Sai Partha

    2012-10-01

    DNA oxidation could be one of the main factors contributing to DNA damage, eventually leading to carcinogenesis, mutations or non-carcinogenic diseases such as Parkinsonís and Alzheimerís. Only recently has the focus turned towards identifying oxidative products of DNA and their consequences. Metabolism activities in vitro produce reactive radicals, which can break DNA strands to cause lesions. These lesions could also act as biomarkers for diagnostic purposes. This review provides an insight of the DNA oxidation mechanism, its harmful consequences and the advantages/disadvantages of available techniques to quantify such DNA oxidative products, focussing mainly on the use GC-MS along with derivatization reaction. In addition, the review also discusses the use of Solid Phase Micro Extraction (SPME) before conducting GC-MS as a potential assay to overcome the discrepancies involved in using GC-MS alone for the identification of DNA oxidative products.

  10. 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.

  11. Sol-gel/nanoclay composite as a solid-phase microextraction fiber coating for the determination of organophosphorus pesticides in water samples.

    PubMed

    Saraji, Mohammad; Jafari, Mohammad Taghi; Sherafatmand, Hossein

    2015-02-01

    A novel solid-phase microextraction (SPME) fiber coated with a sol-gel/nanoclay composite was prepared by the sol-gel technique involving the hydrolysis reaction of alkoxysilanes and the subsequent condensation reaction with hydroxyl groups of the nanoclay on a stainless steel wire. A method based on direct immersion SPME and gas chromatography-corona discharge ion mobility spectrometry was developed for the determination of four organophosphorus pesticides in aqueous samples. The effect of different experimental parameters on the extraction efficiency of the method was investigated. The sol-gel/nanoclay fiber showed higher extraction performance for the organophosphorus pesticides compared with Ppy/nanoclay, sol-gel coating, and three commercial fibers (polydimethylsiloxane (PDMS), PDMS/divinylbenzene (DVB), and polyacrylate (PA)). Limits of detection (LOD) and quantitation (LOQ) of the method were in the range of 0.003-0.012 and 0.01-0.02 μg L(-1), respectively. The calibration curves were linear in a concentration range from 0.01 to 2.0 μg L(-1) (r (2)  > 0.995). The relative standard deviations for intra- and inter-day precision were 3.3-5.6 and 6.4-8.4 %, respectively. Fiber-to-fiber reproducibility for three prepared fibers was 7.4-10.2 %. Finally, the method was successfully applied for the extraction of the studied compounds from water samples. The relative recovery obtained for the spiked real-water samples were 86-104 %. PMID:25471290

  12. 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.

  13. 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.

  14. 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

    2016-04-01

    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. PMID:26998567

  15. 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

    2016-04-01

    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.

  16. 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

  17. Analysis of volatiles in porcine liver pâtés with added sage and rosemary essential oils by using SPME-GC-MS.

    PubMed

    Estévez, Mario; Ventanas, Sonia; Ramírez, Rosario; Cava, Ramón

    2004-08-11

    The effect of the addition of two natural antioxidant extracts (sage and rosemary essential oils) and one synthetic (BHT) on the generation of volatile compounds in liver pâtés from Iberian and white pigs was analyzed using SPME-GC-MS. Lipid-derived volatiles such as aldehydes [hexanal, octanal, nonanal, hept-(Z)-4-enal, oct-(E)-2-enal, non-(Z)-2-enal, dec-(E)-2-enal, deca-(E,Z)-2,4-dienal] and alcohols (pentan-1-ol, hexan-1-ol, oct-1-en-3-ol) were the most abundant compounds in the headspace of porcine liver pâtés. Pâtés from different pig breeds presented different volatiles profiles due to their different oxidation susceptibilities as a probable result of their fatty acid profiles and vitamin E content. Regardless of the origin of the pâtés, the addition of BHT successfully reduced the amount of volatiles derived from PUFA oxidation. Added essential oils showed a different effect on the generation of volatiles whether they were added in pâtés from Iberian or white pigs because they inhibited lipid oxidation in the former and enhanced oxidative instability in the latter. SPME successfully allowed the isolation and analysis of 41 volatile terpenes from pâtés with added sage and rosemary essential oils including alpha-pinene, beta-myrcene, 1-limonene, (E)-caryophyllene, linalool, camphor, and 1,8-cineole, which might contribute to the aroma characteristics of liver pâtés.

  18. 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.

  19. 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.

  20. 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.

  1. Ultrathin phenyl-functionalized solid phase microextraction fiber coating developed by sol-gel deposition.

    PubMed

    Azenha, Manuel; Malheiro, Catarina; Silva, A Fernando

    2005-04-01

    A new sol-gel application for the development of SPME fibers is described. Phenyltrimethoxysilane (PTMOS) and methyltrimethoxysilane (MTMOS) were the sol-gel precursors used at different proportions, together with different water contents, catalyst and reaction time. It was observed that obtaining a good film quality was determinant for a good extracting fiber performance. The film thickness ranged 0.2-1 microm and could not be increased by multi-coating processes. Apparently, a dense, non-porous microstructure was obtained. These coatings exhibited a strong hydrophobic character, as shown by the capability of extraction of long chain and apolar aromatic compounds, which, was comparable to that of the 100 microm polydimethylsiloxane (PDMS) and 65 microm carbowax-divinylbenzene (CW-DVB). The developed fiber has shown high thermal (350 degrees C) and organic solvent stability (ethanol, toluene and dichloromethane), thus bearing adequate characteristics to be associated to GC and potentialities that may also envisage suitability for HPLC. The new fibers may be useful for the microextraction of non-polar compounds, although at trace levels and in simple matrixes only, due to the susceptibility to competition.

  2. 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

    2015-01-01

    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. PMID:26023940

  3. Specialty optical fibers: revisited

    NASA Astrophysics Data System (ADS)

    Romaniuk, Ryszard S.

    2011-10-01

    The paper contains description of chosen aspects of analysis and design of tailored optical fibers. By specialty optical fibers we understand here the fibers which have complex construction and which serve for the functional processing of optical signal rather than long distance transmission. Thus, they are called also instrumentation optical fibers. The following issues are considered: transmission properties, transformation of optical signal, fiber characteristics, fiber susceptibility to external reactions. The technology of tailored optical fibers offers a wider choice of the design tools for the fiber itself, and then various devices made from these fiber, than classical technology of communication optical fibers. The consequence is different fiber properties, nonstandard dimensions and different metrological problems. The price to be paid for wider design possibilities are bigger optical losses of these fibers and weaker mechanical properties, and worse chemical stability. These fibers find their applications outside the field of telecommunications. The applications of instrumentation optical fibers combine other techniques apart from the photonics ones like: electronic, chemical and mechatronic.

  4. Determination of trace Cd, Cu, Fe, Pb and Zn in diesel and gasoline by inductively coupled plasma mass spectrometry after sample clean up with hollow fiber solid phase microextraction system

    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.

  5. Composite Random Fiber Networks

    NASA Astrophysics Data System (ADS)

    Picu, Catalin; Shahsavari, Ali

    2013-03-01

    Systems made from fibers are common in the biological and engineering worlds. In many instances, as for example in skin, where elastin and collagen fibers are present, the fiber network is composite, in the sense that it contains fibers of very different properties. The relationship between microstructural parameters and the elastic moduli of random fiber networks containing a single type of fiber is understood. In this work we address a similar target for the composite networks. We show that linear superposition of the contributions to stiffness of individual sub-networks does not apply and interesting non-linear effects are observed. A physical basis of these effects is proposed.

  6. 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. PMID:27130133

  7. 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.

  8. 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.

  9. 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.

  10. 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)

  11. 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 ...

  12. 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.

  13. 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. PMID:27595648

  14. Fiber pulling apparatus modification

    NASA Technical Reports Server (NTRS)

    Smith, Guy A.; Workman, Gary L.

    1992-01-01

    A reduced gravity fiber pulling apparatus (FPA) was constructed in order to study the effects of gravity on glass fiber formation. The apparatus was specifically designed and built for use on NASA's KC-135 aircraft. Four flights have been completed to date during which E-glass fiber was successfully produced in simulated zero, high, and lunar gravity environments. In addition simulated lunar soil samples were tested for their fiber producing properties using the FPA.

  15. 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).

  16. 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.

  17. 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…

  18. 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.

  19. 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...

  20. Linearly polarized fiber amplifier

    SciTech Connect

    Kliner, Dahv A.; Koplow, Jeffery P.

    2004-11-30

    Optically pumped rare-earth-doped polarizing fibers exhibit significantly higher gain for one linear polarization state than for the orthogonal state. Such a fiber can be used to construct a single-polarization fiber laser, amplifier, or amplified-spontaneous-emission (ASE) source without the need for additional optical components to obtain stable, linearly polarized operation.

  1. 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…

  2. Polypyrrole/montmorillonite nanocomposite as a new solid phase microextraction fiber combined with gas chromatography-corona discharge ion mobility spectrometry for the simultaneous determination of diazinon and fenthion organophosphorus pesticides.

    PubMed

    Jafari, Mohammad T; Saraji, Mohammad; Sherafatmand, Hossein

    2014-03-01

    A novel solid phase microextraction (SPME) fiber was prepared and coupled with gas chromatography corona discharge ion mobility spectrometry (GC-CD-IMS) based on polypyrrole/montmorillonite nanocomposites for the simultaneous determination of diazinon and fenthion. The nanocomposite polymer was coated using a three-electrode electrochemical system and directly deposited on a Ni-Cr wire by applying a constant potential. The scanning electron microscopy images revealed that the new fiber exhibited a rather porous and homogenous surface. The thermal stability of the fabricated fiber was investigated by thermogravimetric analysis. The effects of different parameters influencing the extraction efficiency such as extraction temperature and time, salt addition, stirring rate, the amount of nanoclay, and desorption temperature were investigated and optimized. The method was exhaustively evaluated in terms of sensitivity, recovery, and reproducibility. The linearity ranges of 0.05-10 and 0.08-10 μg L(-1), and the detection limits of 0.020 and 0.035 μg L(-1) were obtained for diazinon and fenthion, respectively. The relative standard deviation values were calculated to be lower than 5% and 8% for intra-day and inter-day, respectively. Finally, the developed method was applied to determine the diazinon and fenthion (as model compounds) in cucumber, lettuce, apple, tap and river water samples. The satisfactory recoveries revealed the capability of the two-dimensional separation technique (retention time in GC and drift time in IMS) for the analysis of complex matrices extracted by SPME. PMID:24528846

  3. Detection of total microcystin in fish tissues based on lemieux oxidation, and recovery of 2-methyl-3-methoxy-4-phenylbutanoic acid (MMPB) by solid-phase microextraction gas chromatography-mass spectrometry (SPME-GC/MS)

    PubMed Central

    Suchy, Patricia; Berry, John

    2012-01-01

    Microcystins (MCs) are widespread cyanobacterial toxins in freshwater systems, and have been linked to both acute and chronic health effects. A growing number of studies suggest that MC can bioaccumulate in food webs. Although, several methods (i.e. ELISA, LC-MS) have been developed for analysis of MC in water, extraction (for subsequent analysis) of the toxin from biological matrices (i.e. animal tissues) is impeded owing to covalent binding of toxins and active sites of their cellular targets, i.e. protein phosphatases. As an alternative approach, chromatographic methods for analysis of a unique marker, 2-methyl-3-methoxy-4-phenylbutanoic acid (MMPB), the product of the Lemieux oxidation of MCs, have been previously developed, and shown to measure total (bound and unbound) MC. Application, however, has been limited by poor recovery of the analyte. An improved recovery method is proposed – specifically the use of solidphase microextraction (SPME). The MMPB analogue, 4-phenylbutanoic acid (4PB), and oxidized MC, were used to develop methods, and we specifically investigated several SPME fibres, and post-oxidation steps. Specifically, a method employing post-oxidation methyl esterification, followed by headspace SPME recovery of MMPB, was developed, and subsequently applied to analysis of environmental samples (i.e. fish tissues) previously shown to contain MCs. The method shows high linearity for both water and tissues spiked with MC, and an improved limit of quantitation of approximately 140 ng g−1. Evaluation of field samples by SPME-GC/MS detected considerably higher levels of MC, than detected by conventional methods (i.e. ELISA), and it is proposed that this technique reveals MC (particularly in the bound form) that is not detected by these methods. These results indicate that the developed method provides improved detection capability for MC in biological matrices, and will enhance our ability to understand bioaccumulation in freshwater food webs, as well

  4. 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.

  5. Multimaterial Acoustic Fibers

    NASA Astrophysics Data System (ADS)

    Chocat, Noemie

    The emergence of multimaterial fibers that combine a multiplicity of solid materials with disparate electrical, optical, and mechanical properties into a single fiber presents new opportunities for extending fiber applications well beyond optical transmission. Fiber reflectors, thermal detectors, photodetectors, chemical sensors, surface-emitting fiber lasers, fiber diodes, and other functional fiber devices have been demonstrated with this approach. Yet, throughout this development and indeed the development of fibers in general, a key premise has remained unchanged : that fibers are essentially static devices incapable of controllably changing their properties at high frequencies. Unique opportunities would arise if a rapid, electrically-driven mechanism for changing fiber properties existed. A wide spectrum of hitherto passive fiber devices could at once become active with applications spanning electronics, mechanics, acoustics, and optics, with the benefits of large surface-area, structural robustness, and mechanical flexibility. This thesis addresses the challenges and opportunities associated with the realization of electromechanical transduction in fibers through the integration of internal piezoelectric and electrostrictive domains. The fundamental challenges related to the fabrication of piezoelectric devices in fiber form are analyzed from a materials perspective, and candidate materials and geometries are selected that are compatible with the thermal drawing process. The first realization of a thermally drawn piezoelectric fiber device is reported and its piezoelectric response is established over a wide range of frequencies. The acoustic properties of piezoelectric fiber devices are characterized and related to their mechanical and geometric properties. Collective effects in multi-fiber constructs are discussed and demonstrated by the realization of a linear phased array of piezoelectric fibers capable of acoustic beam steering. High strain actuation

  6. 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.

  7. 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.

  8. 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.

  9. 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.

  10. 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.

  11. Determination of butyl- and phenyltin compounds in human urine by HS-SPME after derivatization with tetraethylborate and subsequent determination by capillary GC with microwave-induced plasma atomic emission and mass spectrometric detection.

    PubMed

    Zachariadis, G A; Rosenberg, E

    2009-04-30

    A headspace solid-phase micro-extraction (HS-SPME) method was developed and optimized for gas chromatographic separation and determination of commonly found organotin compounds in human urine after potential exposure. Butyl- and phenyltin compounds were in situ derivatized to ethylated derivatives by sodium tetraethylborate (NaBEt(4)) directly in the urine matrix. The relevant parameters affecting the yield of the SPME procedure were examined using tetrabutyltin as internal standard. The method was optimized for direct use in the analysis of undiluted human urine samples and mono-, di- and tri-substituted butyl- and phenyltin compounds could be determined after a 15-min headspace extraction time at room temperature. The selectivity of the microwave-induced plasma atomic emission detector (MIP-AED) as an element specific detector in combination with the relatively selective sample preparation technique of HS-SPME allowed the interference-free detection of the organotin compounds in all cases. A quadrupole mass spectrometer was used in parallel experiments as a detector for the confirmation of the identity molecular structure of the eluted compounds. The performance characteristics of the developed method are given for the determination of mixtures of these compounds. Finally the proposed method was applied to the analysis of several human urine samples. PMID:19203626

  12. Comparison of volatile components in Chinese traditional pickled peppers using HS-SPME-GC-MS, GC-O and multivariate analysis.

    PubMed

    Xiao, Z B; Zhu, J C; Feng, T; Tian, H X; Yu, H Y; Niu, Y W; Zhang, X M

    2010-12-01

    Volatile compounds of Chinese traditional pickled peppers (CTPPs) were extracted by solid-phase micro-extraction (SPME) and analysed by gas chromatography-mass spectrometry (GC-MS) and gas chromatography-olfactometry (GC-O) to visually compare their volatile compositions by applying principal component analysis (PCA). A total of 67 volatile components were identified by GC-MS, including 7 acids, 6 alkanes, 14 alcohols, 9 esters, 11 terpenes, 3 aldehydes, 5 ketones, 7 phenols and 5 miscellaneous compounds, tentatively identified or identified by comparing with mass spectra and retention indices of the standards or from literature. Of 45 volatile compounds detected in the sniffing port of GC-O, the majority of odour-active components included acetic acid, 2-ethyl phenol, L-linalool, tridecane, butyl butanoate, δ-3-carene. The individual concentrations of the volatile compounds such as acetic acid, ethanol, 1-propanol, L-linalool, hexyl 2-methyl butyrate and hexyl pentanoate corresponded well to the intensities of related attributes in the correlation analysis. Due to their high concentration level and low threshold value, these compounds played an important role in the final aromatic profile of the pickled peppers. The differences in flavours were observed by applying PCA to GC-MS data sets. From the PCA results, samples were primarily separated along the first principal component.

  13. 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.

  14. A fast and effective routine method based on HS-SPME-GC-MS/MS for the analysis of organotin compounds in biota samples.

    PubMed

    Noventa, Seta; Barbaro, Jvan; Formalewicz, Malgorzata; Gion, Claudia; Rampazzo, Federico; Brusà, Rossella Boscolo; Gabellini, Massimo; Berto, Daniela

    2015-02-01

    This work validated an automated, fast, and low solvent- consuming methodology suited for routine analysis of tributyltin (TBT) and degradation products (dibutyltin, DBT; monobutyltin, MBT) in biota samples. The method was based on the headspace solid-phase microextraction methodology (HS-SPME), coupled with gas chromatographic separation and tandem mass-spectrometry (GC-MS/MS). The effectiveness of the matrix-matched signal ratio external calibration was tested for quantification purposes. The exclusion of matrix influences in the calibration curves proved the suitability of this versatile quantification method. The method detection limits obtained were of 3 ng Sn g(-1) dw for all the analytes. The analysis of references materials showed satisfying accuracy under optimum calibration conditions (% recovery between 87-111%; |Z-scores|<2). The repeatability RSD% and intra-laboratory reproducibility RSD% were lower than 9.6% and 12.6%, respectively. The work proved the remarkable analytical performances of the method and its high potential for routine application in monitoring organotin compounds (OTC). PMID:25597804

  15. 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).

  16. 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.

  17. HS-SPME comparative analysis of genotypic diversity in the volatile fraction and aroma-contributing compounds of Capsicum fruits from the annuum-chinense-frutescens complex.

    PubMed

    Rodríguez-Burruezo, Adrián; Kollmannsberger, Hubert; González-Mas, M Carmen; Nitz, Siegfried; Fernando, Nuez

    2010-04-14

    Volatile constituents of ripe fruits of 16 Capsicum accessions from the annuum-chinense-frutescens complex, with different aroma impressions and geographical origins, were isolated by headspace-solid phase microextraction (HS-SPME) and analyzed by gas chromatography-olfactometry-mass spectrometry (GC-sniffing port-MS). More than 300 individual compounds could be detected in the studied genotypes; most of them could be identified by comparing mass spectra and retention times with authentic reference substances or literature data. Esters and terpenoids were the main groups, although other minor compounds, such as nitrogen and sulfur compounds, phenol derivatives, norcarotenoids, lipoxygenase derivatives, carbonyls, alcohols, and other hydrocarbons, were also identified. The sniffing test revealed that the diversity of aromas found among the studied cultivars is due to qualitative and quantitative differences of, at least, 23 odor-contributing volatiles (OCVs). C. chinense, and C. frutescens accessions, with fruity/exotic aromas, were characterized by a high contribution of several esters and ionones and a low or nil contribution of green/vegetable OCVs. Different combinations of fruity/exotic and green/vegetable OCVs would explain the range of aroma impressions found among C. annuum accessions. Implications of these findings for breeding and phylogeny studies in Capsicum are also discussed.

  18. 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). PMID:24745744

  19. Effect of radial directional dependences and rainwater influence on CVOC concentrations in tree core and birch sap samples taken for phytoscreening using HS-SPME-GC/MS.

    PubMed

    Holm, Olaf; Rotard, Wolfgang

    2011-11-15

    Phytoscreening for chlorinated volatile organic compounds (CVOC) in tree core samples is influenced by many factors. For instance, greater fluctuations are observed for CVOC concentrations in samples taken around the trunk at a fixed height compared to samples taken directly next to each other. To avoid false negatives and inaccurate interpretation of the results, we investigated this radial directional dependence as well as the influence of rainwater on measured concentrations. CVOC analysis was performed by gas chromatography/mass spectrometry (GC/MS) following Solid-Phase-Microextraction (SPME). Phytoscreening was successfully carried out at three sites using this method. In addition, sap samples were taken from white birches during their budding period as a novel phytoscreening approach. Birch sap sampling is shown to be a suitable means of characterizing contaminant distribution within the soil subsurface. Radial directional dependence of CVOC concentrations varies by almost 80% for tree core samples and 50% for birch sap samples. Variations in concentrations measured around the trunk do not, however, provide information on the inflow direction of contaminated groundwater. The weather conditions were shown to have a greater influence so that CVOC concentrations measured from samples taken during colder, rainier weather were, on average, a factor of 100 lower than those taken during a warm and dry period. Nevertheless phytoscreening is adequate for CVOC characterization in the soil subsurface if the campaign is carried out during a dry weather period, the results then can be taken as being semiquantitative.

  20. 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.

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

    PubMed

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

    2016-04-01

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

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

    PubMed

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

    2016-08-01

    A HS-SPME method coupled with GC-MS analysis has been developed for simultaneously measuring the concentration of 10 volatile organic compounds (VOCs) (benzene, toluene, ethylbenzene, o-, m-, and p-xylene, methyl tert-butyl ether, ethyl tert-butyl ether, 2-methyl-2-butyl methyl ether, and diisopropyl ether) in urine matrix as a biomonitoring tool for populations at low levels of exposure to such VOCs. These compounds, potentially toxic for human health, are common contaminants of both outdoor and indoor air, as they are released by autovehicular traffic; some of them are also present in environmental tobacco smoke (ETS). Thus, the exposure to these pollutants cannot be neglected and should be assessed. The low limits of detection and quantification (LODs and LOQs <6.5 and 7.5 ng L(-1), respectively) and the high reproducibility (CVs <4 %) make the developed method suited for biomonitoring populations exposed at low levels such as children. Further, the method is cost-effective and low in time-consumption; therefore, it is useful for investigating large populations. It has been applied to children exposed to traffic pollution and/or ETS; the relevant results are reported, and the relevant implications are discussed. PMID:27311952

  3. Digestion of kiwifruit fiber.

    PubMed

    Henare, Sharon J; Rutherfurd, Shane M

    2013-01-01

    Dietary fiber affects the digestion and absorption of nutrients in the gastrointestinal tract. Moreover, it is generally believed that fiber largely escapes digestion in the human small intestine and is therefore mainly a substrate for microbial fermentation in the hindgut. Kiwifruit is a food naturally high in dietary fiber, yet the impact of dietary kiwifruit on nutrient availability has not been reported. The digestion of kiwifruit has been investigated but only in in vitro digestion studies. With its naturally high nonstarch polysaccharide content, it would be expected that kiwifruit would possess the characteristics of a good source of fiber for nutrition and health. Kiwifruit contains soluble and nonsoluble fiber components, both of which would be expected to affect the physical attributes of digesta as it transits the gastrointestinal tract. This chapter summarizes fiber digestion in general and current knowledge of kiwifruit fiber digestion in the gastrointestinal tract.

  4. 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.

  5. 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.

  6. 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.

  7. 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%. PMID:19569094

  8. 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.

  9. Fiber optic temperature sensor

    NASA Technical Reports Server (NTRS)

    Morey, W. W.; Glenn, W. H.; Snitzer, E.

    1983-01-01

    A temperature sensor has been developed that utilizes the temperature dependent absorption of a rare earth doped optical fiber. The temperature measurement is localized at a remote position by splicing a short section of the rare earth fiber into a loop of commercial data communication fiber that sends and returns an optical probe signal to the temperature sensitive section of fiber. The optical probe signal is generated from two different wavelength filtered LED sources. A four port fiber optic coupler combines the two separate wavelength signals into the fiber sensing loop. Time multiplexing is used so that each signal wavelength is present at a different time. A reference signal level measurement is also made from the LED sources and a ratio taken with the sensor signal to produce a transmission measurement of the fiber loop. The transmission is affected differently at each wavelength by the rare earth temperature sensitive fiber. The temperature is determined from a ratio of the two transmission measurements. This method eliminates any ambiguity with respect to changes in signal level in the fiber loop such as mating and unmating optical connectors. The temperature range of the sensor is limited to about 800 C by the temperature limit fo the feed fibers.

  10. Novel fiber coated with amide bridged-calix[4]arene used for solid-phase microextraction of aliphatic amines.

    PubMed

    Li, Xiujuan; Zeng, Zhaorui; Zhou, Jingjing; Gong, Shuling; Wang, Wei; Chen, Yuanyin

    2004-07-01

    Solid-phase microextraction (SPME) using a novel fiber coated with 25,27-dihydroxy-26, 28-oxy(2',7'-dioxo-3',6'-diazaoctyl)oxy-p-tert-butylcalix[4]arene/hydroxy-terminated silicone oil has been introduced as a rapid and sensitive pretreatment technique coupled to gas chromatography-flame ionization detection (GC-FID) for the detection of aliphatic amines without derivatization. Due to the introduction of the polar amide bridge in calix[4]arene, the new fiber shows good selectivity and sensitivity to the polar aliphatic amines in addition to its high thermal stability (380 degrees C), solvent stability and good reproducibility between fibers. The extraction temperature, extraction time, pH, and ionic strength of the matrix sample were modified to allow for maximum sorption of the analytes onto the fiber. The method proposed in this study showed satisfactory linearity, precision and detection limits. Practical applicability was demonstrated through the determination of trimethylamine (TMA) in fish tissue. Mean recovery of 92.5% (n = 5) was obtained for the fish extracts and the relative standard deviation was 4.9% (n = 5). The results of fish freshness assay indicate the present method is a validated and simple procedure for the simultaneous determination of TMA in fish. PMID:15281248

  11. Capillary stretching of fibers

    NASA Astrophysics Data System (ADS)

    Duprat, C.; Protiere, S.

    2015-09-01

    We study the interaction of a finite volume of liquid with two parallel thin flexible fibers. A tension along the fibers is imposed and may be varied. We report two morphologies, i.e. two types of wet adhesion: a weak capillary adhesion, where a liquid drop bridges the fibers, and a strong elastocapillary adhesion where the liquid is spread between two collapsed fibers. We show that geometry, capillarity and stretching are the key parameters at play. We describe the collapse and detachment of the fibers as a function of two nondimensional parameters, arising from the geometry of the system and a balance between capillary and stretching energies. In addition, we show that the morphology, thus the capillary adhesion, can be controlled by changing the tension within the fibers.

  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, 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.

  14. 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.

  15. Fiber optic micro accelerometer

    SciTech Connect

    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. 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.

  17. 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

    2015-08-01

    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 (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.

  18. Graphitic carbon nitrides modified hollow fiber solid phase microextraction for extraction and determination of uric acid in urine and serum coupled with gas chromatography-mass spectrometry.

    PubMed

    Sun, Ying-pei; Chen, Juan; Qi, Huan-yang; Shi, Yan-ping

    2015-11-01

    An elevated uric acid (UA) in urine or serum can affect renal function and blood pressure, which is an indicator of gout, cardiovascular and renal diseases, hypertension, etc. In this work, a new type of mixed matrix membrane (MMM), based on graphitic carbon nitrides (g-CNs) and hollow fiber (HF), was prepared and combined with solid phase microextraction (SPME) mode to determine UA in urine and serum followed by gas chromatography-mass spectrometry (GC/MS). The porous g-CNs were dispersed in ammonia, and then the exfoliated g-CNs nanosheets were held in the pores of HF by capillary forces and sonification. The prepared g-CNs modified HF (g-CNs-HF) was immersed in biofluid directly to extract UA with SPME mode and the solvent-free mode is convenient for further derivatization and analysis. To achieve the highest extraction efficiency (EF), main extraction and derivatization parameters, such as g-CNs-HF immobilizing time, sonification power and time of extraction, derivatization and desorption time, were optimized. Under the optimum extraction conditions, a favorable linearity of UA was obtained in the range 0.1-200μgmL(-1) with correlation coefficients higher than 0.9990, and the average recoveries at three spiked levels of UA in urine and serum ranged from 80.7% to 121.6%, from 84.7% to 101.1%, respectively. The obtained results demonstrated the developed g-CNs-HF-SPME is a simple, rapid, cost-effective, solvent-free method for the analysis of UA in biofluid.

  19. Graphitic carbon nitrides modified hollow fiber solid phase microextraction for extraction and determination of uric acid in urine and serum coupled with gas chromatography-mass spectrometry.

    PubMed

    Sun, Ying-pei; Chen, Juan; Qi, Huan-yang; Shi, Yan-ping

    2015-11-01

    An elevated uric acid (UA) in urine or serum can affect renal function and blood pressure, which is an indicator of gout, cardiovascular and renal diseases, hypertension, etc. In this work, a new type of mixed matrix membrane (MMM), based on graphitic carbon nitrides (g-CNs) and hollow fiber (HF), was prepared and combined with solid phase microextraction (SPME) mode to determine UA in urine and serum followed by gas chromatography-mass spectrometry (GC/MS). The porous g-CNs were dispersed in ammonia, and then the exfoliated g-CNs nanosheets were held in the pores of HF by capillary forces and sonification. The prepared g-CNs modified HF (g-CNs-HF) was immersed in biofluid directly to extract UA with SPME mode and the solvent-free mode is convenient for further derivatization and analysis. To achieve the highest extraction efficiency (EF), main extraction and derivatization parameters, such as g-CNs-HF immobilizing time, sonification power and time of extraction, derivatization and desorption time, were optimized. Under the optimum extraction conditions, a favorable linearity of UA was obtained in the range 0.1-200μgmL(-1) with correlation coefficients higher than 0.9990, and the average recoveries at three spiked levels of UA in urine and serum ranged from 80.7% to 121.6%, from 84.7% to 101.1%, respectively. The obtained results demonstrated the developed g-CNs-HF-SPME is a simple, rapid, cost-effective, solvent-free method for the analysis of UA in biofluid. PMID:26444336

  20. 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.

  1. 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

  2. The study of fingerprint characteristics of Dayi Pu-Erh tea using a fully automatic HS-SPME/GC-MS and combined chemometrics method.

    PubMed

    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.

  3. 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.

  4. The study of fingerprint characteristics of Dayi Pu-Erh tea using a fully automatic HS-SPME/GC-MS and combined chemometrics method.

    PubMed

    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

  5. Evaluation of HS-SPME and ultrasonic solvent extraction for monitoring of plant flavours added by the bees to herbhoneys: traceability biomarkers.

    PubMed

    Kuś, Piotr Marek; Marijanović, Zvonimir; Jerković, Igor

    2015-01-01

    The volatile composition of 21 herbhoneys (HHs) of 7 different botanical origins was characterised for the first time. Ultrasound solvent extraction (USE) and headspace solid-phase microextraction (HS-SPME) followed by GC-FID/MS were successfully applied as complementary methods for monitoring the volatile plant flavours added by the bees. HHs showed significant compositional variability related to the botanical origin and compounds that could serve as traceability biomarkers were identified. The most important compounds with high abundance were (E,extract; H, headspace): caffeine (up to 68.7%, E) and trans-linalool oxide (up to 26.0%, H) in coffee HH, α-terpineol (up to 8.2%, E; 27.1%, H) and bornyl acetate (up to 3.1, E; 11.9%, H) in pine HH, thymol (up to 3.1%, E; 55.4%, H) in thyme HH. Hawthorn HH was characterised by the presence of herniarin (up to 13.4%, E) and lemon HH contained limonene (up to 1.6%, E; 33.2%, H). Other HHs (nettle and aloe) contained lower amounts of volatiles and their profiles were not specific. In all the HHs, methyl syringate was found and it was most abundant in thyme HH (up to 17.4%, E). The volatile fraction of HHs showed some substantial similarities and differences with the composition of herbs from which they derive. It confirms the selective bee-mediated transfer of phytochemicals, including known flavour-active volatiles into the final product, but also biotransformation of several compounds. Additionally, several similarities to the corresponding natural honeys were observed, but in general HHs exhibited less rich volatile profiles. PMID:26365314

  6. 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

  7. Evaluation of HS-SPME and ultrasonic solvent extraction for monitoring of plant flavours added by the bees to herbhoneys: traceability biomarkers.

    PubMed

    Kuś, Piotr Marek; Marijanović, Zvonimir; Jerković, Igor

    2015-01-01

    The volatile composition of 21 herbhoneys (HHs) of 7 different botanical origins was characterised for the first time. Ultrasound solvent extraction (USE) and headspace solid-phase microextraction (HS-SPME) followed by GC-FID/MS were successfully applied as complementary methods for monitoring the volatile plant flavours added by the bees. HHs showed significant compositional variability related to the botanical origin and compounds that could serve as traceability biomarkers were identified. The most important compounds with high abundance were (E,extract; H, headspace): caffeine (up to 68.7%, E) and trans-linalool oxide (up to 26.0%, H) in coffee HH, α-terpineol (up to 8.2%, E; 27.1%, H) and bornyl acetate (up to 3.1, E; 11.9%, H) in pine HH, thymol (up to 3.1%, E; 55.4%, H) in thyme HH. Hawthorn HH was characterised by the presence of herniarin (up to 13.4%, E) and lemon HH contained limonene (up to 1.6%, E; 33.2%, H). Other HHs (nettle and aloe) contained lower amounts of volatiles and their profiles were not specific. In all the HHs, methyl syringate was found and it was most abundant in thyme HH (up to 17.4%, E). The volatile fraction of HHs showed some substantial similarities and differences with the composition of herbs from which they derive. It confirms the selective bee-mediated transfer of phytochemicals, including known flavour-active volatiles into the final product, but also biotransformation of several compounds. Additionally, several similarities to the corresponding natural honeys were observed, but in general HHs exhibited less rich volatile profiles.

  8. 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.

  9. 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.

  10. 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. PMID:27343598

  11. Soluble and insoluble fiber (image)

    MedlinePlus

    ... stool. There are two types of dietary fiber, soluble and insoluble. Soluble fiber retains water and turns to gel during ... and nutrient absorption from the stomach and intestine. Soluble fiber is found in foods such as oat ...

  12. 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.

  13. 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.

  14. 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.

  15. Multimode optical fiber

    DOEpatents

    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).

  16. Super capacitor with fibers

    SciTech Connect

    Farmer, Joseph Collin; Kaschmitter, James

    2015-02-17

    An electrical cell apparatus includes a first current collector made of a multiplicity of fibers, a second current collector spaced from the first current collector; and a separator disposed between the first current collector and the second current collector. The fibers are contained in a foam.

  17. 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.

  18. 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.

  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, 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.

  1. 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.

  2. 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 ).

  3. 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 ).

  4. Fiber optic attenuator

    NASA Technical Reports Server (NTRS)

    Buzzetti, Mike F. (Inventor)

    1994-01-01

    A fiber optic attenuator of the invention is a mandrel structure through which a bundle of optical fibers is wrapped around in a complete circle. The mandrel structure includes a flexible cylindrical sheath through which the bundle passes. A set screw on the mandrel structure impacts one side of the sheath against two posts on the opposite side of the sheath. By rotating the screw, the sheath is deformed to extend partially between the two posts, bending the fiber optic bundle to a small radius controlled by rotating the set screw. Bending the fiber optic bundle to a small radius causes light in each optical fiber to be lost in the cladding, the amount depending upon the radius about which the bundle is bent.

  5. Fiber optic hydrophone

    SciTech Connect

    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.

  6. 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.

  7. 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.

  8. 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.

  9. 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

  10. 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.

  11. 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.

  12. 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.

  13. 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.

  14. Automated fiber pigtailing technology

    NASA Astrophysics Data System (ADS)

    Strand, O. T.; Lowry, M. E.; Lu, S. Y.; Nelson, D. C.; Nikkel, D. J.; Pocha, M. D.; Young, K. D.

    1994-02-01

    The high cost of optoelectronic (OE) devices is due mainly to the labor-intensive packaging process. Manually pigtailing such devices as single-mode laser diodes and modulators is very time consuming with poor quality control. The Photonics Program and the Engineering Research Division at LLNL are addressing several issues associated with automatically packaging OE devices. A furry automated system must include high-precision fiber alignment, fiber attachment techniques, in-situ quality control, and parts handling and feeding. This paper will present on-going work at LLNL in the areas of automated fiber alignment and fiber attachment. For the fiber alignment, we are building an automated fiber pigtailing machine (AFPM) which combines computer vision and object recognition algorithms with active feedback to perform sub-micron alignments of single-mode fibers to modulators and laser diodes. We expect to perform sub-micron alignments in less than five minutes with this technology. For fiber attachment, we are building various geometries of silicon microbenches which include on-board heaters to solder metal-coated fibers and other components in place; these designs are completely compatible with an automated process of OE packaging. We have manually attached a laser diode, a thermistor, and a thermo-electric heater to one of our microbenches in less than 15 minutes using the on-board heaters for solder reflow; an automated process could perform this same exercise in only a few minutes. Automated packaging techniques such as these will help lower the costs of OE devices.

  15. Nanotube composite carbon fibers

    NASA Astrophysics Data System (ADS)

    Andrews, R.; Jacques, D.; Rao, A. M.; Rantell, T.; Derbyshire, F.; Chen, Y.; Chen, J.; Haddon, R. C.

    1999-08-01

    Single walled carbon nanotubes (SWNTs) were dispersed in isotropic petroleum pitch matrices to form nanotube composite carbon fibers with enhanced mechanical and electrical properties. We find that the tensile strength, modulus, and electrical conductivity of a pitch composite fiber with 5 wt % loading of purified SWNTs are enhanced by ˜90%, ˜150%, and 340% respectively, as compared to the corresponding values in unmodified isotropic pitch fibers. These results serve to highlight the potential that exits for developing a spectrum of material properties through the selection of the matrix, nanotube dispersion, alignment, and interfacial bonding.

  16. 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.

  17. Fiber optic communication links

    SciTech Connect

    Meyer, R. H.

    1980-01-01

    Fiber optics is a new, emerging technology which offers relief from many of the problems which limited past communications links. Its inherent noise immunity and high bandwidth open the door for new designs with greater capabilities. Being a new technology, certain problems can be encountered in specifying and installing a fiber optic link. A general fiber optic system is discussed with emphasis on the advantages and disadvantages. It is not intended to be technical in nature, but a general discussion. Finally, a general purpose prototype Sandia communications link is presented.

  18. 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.

  19. 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.

  20. 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…

  1. Robust fiber clustering of cerebral fiber bundles in white matter

    NASA Astrophysics Data System (ADS)

    Yao, Xufeng; Wang, Yongxiong; Zhuang, Songlin

    2014-11-01

    Diffusion tensor imaging fiber tracking (DTI-FT) has been widely accepted in the diagnosis and treatment of brain diseases. During the rendering pipeline of specific fiber tracts, the image noise and low resolution of DTI would lead to false propagations. In this paper, we propose a robust fiber clustering (FC) approach to diminish false fibers from one fiber tract. Our algorithm consists of three steps. Firstly, the optimized fiber assignment continuous tracking (FACT) is implemented to reconstruct one fiber tract; and then each curved fiber in the fiber tract is mapped to a point by kernel principal component analysis (KPCA); finally, the point clouds of fiber tract are clustered by hierarchical clustering which could distinguish false fibers from true fibers in one tract. In our experiment, the corticospinal tract (CST) in one case of human data in vivo was used to validate our method. Our method showed reliable capability in decreasing the false fibers in one tract. In conclusion, our method could effectively optimize the visualization of fiber bundles and would help a lot in the field of fiber evaluation.

  2. 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.

  3. 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)

  4. Tapered GRIN fiber microsensor.

    PubMed

    Beltrán-Mejía, Felipe; Biazoli, Claudecir R; Cordeiro, Cristiano M B

    2014-12-15

    The sensitivity of an optical fiber microsensor based on inter-modal interference can be considerably improved by tapering a short extension of the multimode fiber. In the case of Graded Index fibers with a parabolic refractive index profile, a meridional ray exhibits a sinusoidal path. When these fibers are tapered, the period of the propagated beam decrease down-taper and increase up-taper. We take advantage of this modulation -along with the enhanced overlap between the evanescent field and the external medium- to substantially increase the sensitivity of these devices by tuning the sensor's maximum sensitivity wavelength. Moreover, the extension of this device is reduced by one order of magnitude, making it more propitious for reduced space applications. Numerical and experimental results demonstrate the success and feasibility of this approach. PMID:25606989

  5. Fiber based optofluidic biosensors

    NASA Astrophysics Data System (ADS)

    Lismont, M.; Vandewalle, N.; Joris, B.; Dreesen, L.

    2014-09-01

    Medicinal diagnosis requires the development of innovative devices allowing the detection of small amounts of biological species. Among the large variety of available biosensors, the ones based on fluorescence phenomenon are really promising. Here, we show a prototype of the basic unit of a multi-sensing biosensor combining optics and microfluidics benefits. This unit makes use of two crossed optical fibers: the first fiber is used to carry small probe molecules droplets and excite fluorescence, while the second one is devoted to target molecules droplets transport and fluorescence detection. Within this scheme, the interaction takes place in each fiber node. The main benefits of this detection setup are the absence of fibers functionalization, the use of microliter volumes of target and probe species, their separation before interaction, and a better detection limit compared to cuvettes setups.

  6. Fiber and Your Child

    MedlinePlus

    ... pears green peas legumes (dried beans, split peas, lentils, etc.) artichokes almonds A high-fiber food has ... salsa, taco sauce, and cheese for dinner. Add lentils or whole-grain barley to soups. Create mini- ...

  7. 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)

  8. 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).

  9. Optical fiber magnetometer

    NASA Astrophysics Data System (ADS)

    Scarzello, John F.; Finkel, Jack

    1991-08-01

    An optical fiber magnetometer having omnidirectional capability is disclosed herein for measuring a total magnetic field independent of its physical orientation or the direction of the field or fields. A relatively long optical fiber defining a sensing arm for exposure to a magnetic field is wound in the form of a spheroid (like rubber bands on a golf ball or yarn threads on a baseball) to provide optical lengths of substantially the same total length in every direction through the spheroid winding. The plane of polarization of light transmitted through the optical fiber winding is caused to rotate (Faraday effect) when the fiber or components thereof is exposed parallel to a magnetic field. The extent of plane rotation is determined, inter alia, by the total magnetic field passing through the spheroid winding.

  10. 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.

  11. Ways to Boost Fiber

    MedlinePlus

    ... and Reproduction Top Articles dad holding baby at apple orchard - Kidney Disease: High- and Moderate-Potassium Foods ... lower its fiber content. For example, one medium apple with the peel contains 4.4 grams of ...

  12. Fiber-optic gyroscope

    NASA Astrophysics Data System (ADS)

    Lefevre, Herve C.; Arditty, Herve J.

    1992-05-01

    This paper reviews the technological evolution of the interferometric fiber gyroscope over the last fifteen years. Today a psychological barrier has been passed, and it is now accepted that this new technology will find many applications during the 90's.

  13. High-fiber foods

    MedlinePlus

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

  14. 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.

  15. 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.

  16. 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.

  17. [Carbohydrates and fiber].

    PubMed

    Lajolo, F M; de Menezes, E W; Filisetti-Cozzi, T M

    1988-09-01

    Dietary carbohydrates comprise two fractions that may be classified as digestible, and which are useful as energy sources (simple and complex carbohydrates) and fiber, which is presumed to be of no use to the human body. There are insufficient epidemiologic data on the metabolic effects of simple carbohydrates and it is not advisable to make quantitative recommendations of intake. It is questionable to recommend in developing countries that a fixed proportion of dietary energy be derived from simple sugars, due to the high prevalence of deficient energy intake, cultural habits, and regional differences in food intake and physical activity. In relation to recommendations of complex carbohydrates, it should be considered that their absorption is influenced by many factors inherent to the individual and to the foods. Fiber is defined as a series of different substances derived from tissue structures, cellular residues and undigested chemical substances that may be partially utilized after intestinal bacteria have acted on them. There is not a clear definition of the chemical composition of fiber, but it consists mainly of polysaccharides (such as cellulose, hemicellulose and pectins), lignin and end products of the interactions of various food components. The effects of fiber, such as control of food intake, regulation of gastrointestinal transit, post-prandial blood concentrations of cholesterol, glucose and insulin, flatulence and alterations in nutrient bioavailability are due to various physical properties inherent to its chemical components. Impairment of nutrient absorption may be harmful, mainly among populations whose food intake is lower than their energy needs, and with a high fiber content. This may be particularly important in pregnant women, growing children and the elderly, and should be considered when making nutrient recommendations. A precise knowledge of fiber is also important to calculate the real energy value of foods, mainly for two reasons: 1

  18. 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.

  19. 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.

  20. 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.

  1. 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.

  2. 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.

  3. Wetting fibers with liposomes.

    PubMed

    Borghi, N; Alias, K; de Gennes, P-G; Brochard-Wyart, F

    2005-05-01

    Giant unilamellar vesicles (GUVs) are deposited on glass microfibers. The vesicles adopt the classical "onduloidal" shape of liquid droplets on fibers. They spread by two simultaneous mechanisms: envelopment and emission of a precursor film. This film spreads faster than on a uniform plane surface and eventually stops, signaling the presence of defects on the rod. This fast spreading tenses the vesicles; transient pores open on the GUVs and the internal liquid leaks out. This process leads to a new technique for fiber coating.

  4. Glass fiber insulation

    SciTech Connect

    Griffith, E.J.; Ngo, T.M.

    1993-06-29

    A composition for a glass fiber insulation is described comprising a loose mat of glass fibers having at least a portion of the surface coated with a water insoluble, non-hygroscopic, amorphous aluminum phosphate polymer having a molar ratio of Al[sub 2]O[sub 3] to P[sub 2]O[sub 5] of less than 1 and providing a substantial thermal resistance.

  5. The use of headspace solid-phase microextraction (HS-SPME) to assess the quality and stability of fruit products: an example using red mombin pulp (Spondias purpurea L.).

    PubMed

    Todisco, Katieli Martins; Castro-Alves, Victor Costa; Garruti, Deborah Dos Santos; Costa, José Maria Correia da; Clemente, Edmar

    2014-01-01

    The present study aimed to evaluate the volatiles profile of red mombin (Spondias purpurea) pulp and its powder produced by spray-drying (SD) as an example to show utility of headspace solid-phase microextraction (HS-SPME) in the analysis of parameters such as the quality and stability of fruit products. Volatiles profiles of the pulp were identified by gas chromatography-mass spectrometry (GC-MS), quantified by gas chromatography-flame ionization detector (GC-FID) and compared to the profile of the powder stored at 0, 60 and 120 days in plastic (PP) or laminated packages (LP). The results showed that the technique was able to identify 36 compounds in the red mombin pulp, 17 out of which have been described for the first time in this fruit, showing that red mombin fresh pulp appears to be unique in terms of volatiles composition. However, only 24 compounds were detected in the powder. This decrease is highly correlated (r2 = 0.99), at least for the majority of compounds, to the degree of volatility of compounds. Furthermore, the powder stored in PP or LP showed no statistical differences in the amounts of its components for a period of 120 days of storage. Finally, this work shows how HS-SPME analysis can be a valuable tool to assess the quality and stability of fruit products. PMID:25338176

  6. 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.

  7. The use of headspace solid-phase microextraction (HS-SPME) to assess the quality and stability of fruit products: an example using red mombin pulp (Spondias purpurea L.).

    PubMed

    Todisco, Katieli Martins; Castro-Alves, Victor Costa; Garruti, Deborah Dos Santos; Costa, José Maria Correia da; Clemente, Edmar

    2014-10-21

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

  8. Enzymatic modification of flaxseed fibers.

    PubMed

    Maijala, Pekka; Mäkinen, Marliina; Galkin, Sari; Fagerstedt, Kurt; Härkäsalmi, Tiina; Viikari, Liisa

    2012-11-01

    Flaxseed (Linum usitatissimum L.) fibers were modified by oxidoreductive and cellulolytic enzymes. The lignin amount and intrinsic plant peroxidase activity was evaluated by histochemical and spectrophotometric assays. Peroxidase activity was not found from bast fibers. The flaxseed fibers were further separated and treated with laccase to conjugate the model compounds, that is, the hydrophobic gallate molecules on fiber surfaces. Laccase was able to slowly oxidize fiber-conjugated phenolics, but no fundamental changes in fiber cell surface structure or notable coupling of the applied hydrophobic gallate molecules onto the fibers occurred, as revealed by Fourier transform infrared spectroscopy. The reactivity of the mature fibers was further investigated using cellulolytic enzymes. Cellobiohydrolase (CBH) and endoglucanase (EG)-rich enzyme preparations were applied to reach a hydrolysis degree of 1-6% (of the fiber dry matter) using a standard enzyme dosage. The CBH mixture altered the fiber surface morphology distinctly, and SEM images illustrated fibers in which the cellulose fibrils seemed to be loosened and partially hydrolyzed. In contrast, the effect of the EG-rich preparation without CBH activity was notable on the fiber surface, polishing the surfaces. The cellulolytic treatments were potentially interesting for specific enzymatic modifications of flax fiber surfaces, whereas the approach to use oxidoreductive enzyme treatments on mature linseed fibers offered little potential, obviously due to the low lignin content of the fibers.

  9. 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.

  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. Fiber optics for controls

    NASA Astrophysics Data System (ADS)

    Seng, Gary T.

    1987-11-01

    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.

  12. Fiber optic current probe

    NASA Astrophysics Data System (ADS)

    Wyntjes, G.; Fox, R.

    1984-02-01

    This report documents the results of Phase 1 research into a new type of Fiber Optic Current probe, suitable for high voltage, high current applications. The probe uses a stabilized two frequency HeNe laser to read the magnitude and sign of magnetic field induced circular birefringence in an optical fiber wound around a conductor. Measurements of both alternating and direct currents were demonstrated with a breadboard system. The system was tested at low voltages with currents of up to 4500 amperes peak and with up to 28 turns of optical fiber around the conductor. The response was found to increase linearly with the number of fiber turns. Experimental determinations of the system's frequency response and dynamic range were not possible due to our inability to generate large, fast current transients. The predicted frequency response is 100 kHz with an ability to read transient amplitudes of 300 times the nominal line current. Several single-mode fibers were used to form transducers, and the optimum fiber for further development was identified. The 2-frequency interrogation technique described worked entirely as predicted, and should be applicable to magnetic field measurements in general (i.e., charged particle beams, Tokamaks, antenna patterns, EMP testing, etc.).

  13. Emergence of fiber supercapacitors.

    PubMed

    Yu, Dingshan; Qian, Qihui; Wei, Li; Jiang, Wenchao; Goh, Kunli; Wei, Jun; Zhang, Jie; Chen, Yuan

    2015-02-01

    Supercapacitors (SCs) are energy storage devices which have high power density and long cycle life. Conventional SCs have two-dimensional planar structures. As a new family of SCs, fiber SCs utilize one-dimensional cylindrically shaped fibers as electrodes. They have attracted significant interest since 2011 and have shown great application potential either as micro-scale devices to complement or even replace micro-batteries in miniaturized electronics and microelectromechanical systems or as macro-scale devices for wearable electronics or smart textiles. This tutorial review provides an essential introduction to this new field. We first introduce the basics of performance evaluation for fiber SCs as a foundation to understand different research approaches and the diverse performance metrics reported in the literature. Next, we summarize the current state-of-the-art progress in structure design and electrode fabrication of fiber SCs. This is followed by a discussion on the integration of multiple fiber SCs and the combination with other energy harvesting or storage devices. Last, we present our perspectives on the future development of fiber SCs and highlight key technical challenges with the hope of stimulating further research progress. PMID:25420877

  14. 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.

  15. Determination of polycyclic aromatic hydrocarbons in Persian Gulf and Caspian Sea: gold nanoparticles fiber for a head space solid phase micro extraction.

    PubMed

    Karimi, Mohammad; Aboufazeli, Forouzan; Zhad, Hamid Reza Lotfi Zadeh; Sadeghi, Omid; Najafi, Ezzatollah

    2013-03-01

    A gold nanoparticles modified fused silica fiber was developed and used for the head space solid phase micro-extraction (HS-SPME) of polycyclic aromatic hydrocarbons (PAHs), including naphthalene, anthracene, acenaphthylene, phenanthrene, fluoranthene and pyrene. The effects of different parameters influencing the extraction efficiency including extraction temperature, extraction time, ionic strength, stirring rate and sample volume were examined and optimized. Linear ranges of 1-300 μg L(-1) for naphthalene, 0.5-250 μg L(-1) for anthracene, acenaphthylene and phenanthrene and 0.05-200 μg L(-1) for fluoranthene and pyrene were obtained. Detection limits were in the range of 10-200 μg L(-1). Single fiber repeatability and fiber to fiber reproducibility were less than 2.5 %-6.0 % and 8.5 %-13.6 %, respectively. Seawater samples were analyzed as real samples and good recoveries (91.9 %-105.3 %) were obtained for target analytes.

  16. Determination of polycyclic aromatic hydrocarbons in Persian Gulf and Caspian Sea: gold nanoparticles fiber for a head space solid phase micro extraction.

    PubMed

    Karimi, Mohammad; Aboufazeli, Forouzan; Zhad, Hamid Reza Lotfi Zadeh; Sadeghi, Omid; Najafi, Ezzatollah

    2013-03-01

    A gold nanoparticles modified fused silica fiber was developed and used for the head space solid phase micro-extraction (HS-SPME) of polycyclic aromatic hydrocarbons (PAHs), including naphthalene, anthracene, acenaphthylene, phenanthrene, fluoranthene and pyrene. The effects of different parameters influencing the extraction efficiency including extraction temperature, extraction time, ionic strength, stirring rate and sample volume were examined and optimized. Linear ranges of 1-300 μg L(-1) for naphthalene, 0.5-250 μg L(-1) for anthracene, acenaphthylene and phenanthrene and 0.05-200 μg L(-1) for fluoranthene and pyrene were obtained. Detection limits were in the range of 10-200 μg L(-1). Single fiber repeatability and fiber to fiber reproducibility were less than 2.5 %-6.0 % and 8.5 %-13.6 %, respectively. Seawater samples were analyzed as real samples and good recoveries (91.9 %-105.3 %) were obtained for target analytes. PMID:23183967

  17. Study on basalt fiber parameters affecting fiber-reinforced mortar

    NASA Astrophysics Data System (ADS)

    Orlov, A. A.; Chernykh, T. N.; Sashina, A. V.; Bogusevich, D. V.

    2015-01-01

    This article considers the effect of different dosages and diameters of basalt fibers on tensile strength increase during bending of fiberboard-reinforced mortar samples. The optimal dosages of fiber, providing maximum strength in bending are revealed. The durability of basalt fiber in an environment of cement, by means of microscopic analysis of samples of fibers and fiberboard-reinforced mortar long-term tests is examined. The article also compares the behavior of basalt fiber in the cement stone environment to a glass one and reveals that the basalt fiber is not subject to destruction.

  18. 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.

  19. 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.

  20. 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

  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. ZBLAN Fiber Phase B Study

    NASA Technical Reports Server (NTRS)

    Workman, Gary L.; Smith, Guy A.

    1997-01-01

    A Phase B feasibility study will be performed for the study of the effects of microgravity on the preform processing and fiber pulling of ZBLAN optical glass. Continuing from the positive results achieved in the fiber annealing experiments in 20 second intervals at 0.001 g on the KC-135 and the 5 minute experiments on the SPAR rocket, experiments will continue to work towards design of a fiber sting to initiate fiber pulling operations in space. Anticipated results include less homogeneous nucleation than ground-based annealed fibers. Infrared Fiber Systems and Galileo are the participating industrial investigators.

  4. 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.

  5. Optical fiber interferometric spectrometer

    NASA Astrophysics Data System (ADS)

    Liu, Yong; Li, Baosheng; Liu, Yan; Zhai, Yufeng; Wang, An

    2006-02-01

    We design an optical fiber spectrometer based on optical fiber Mach-Zehnder interferometer. In optical fiber Fourier transform spectrometer spectra information is obtained by Fourier transform of interferogram, which recording intensity change vs. optical path difference. Optical path difference is generated by stretching one fiber arm which wound around fiber stretch drive by high power supply. Information from detector is linear with time rather than with optical path difference. In order to obtain high accuracy wavenumber, reference beam is used to control the optical path difference. Optical path difference is measured by reference laser interference fringe. Interferogram vs. optical path difference is resampled by Brault algorithm with information from reference beam and test beam. In the same condition, one-sided interferogram has higher resolution than that of two-sided interferogram. For one-sided interferogram, zero path difference position must be determined as accurately as possible, small shift will result in phase error. For practical experiment in laboratory, position shift is inevitable, so phase error correction must be considered. Zero order fringe is determined by curve fitting. Spectrum of light source is obtained from one-sided interferogram by Fourier cosine transform. A spectral resolution of about ~3.1 cm -1 is achieved. In practice, higher resolution is needed. This compact equipment will be used in emission spectra and absorption spectra, especially in infrared region.

  6. 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.

  7. Tapered fiber bundle couplers for high-power fiber amplifiers

    NASA Astrophysics Data System (ADS)

    Sliwinska, Dorota; Kaczmarek, Pawel; Abramski, Krzysztof M.

    2014-12-01

    In this work, we would like to demonstrate our results on performing (6+1)x1 tapered fiber bundle combiners using a trielectrode fiber splicing system. In our combiners we have used 9/80 μm (core/clad) diameter fibers as single-mode signal input ports. Using this fiber, instead of a conventional 9/125 μm single-mode fiber allowed us to reduce the taper ratio and therefore significantly increase the signal transmission. We have also performed power combiner which is based on the LMA fibers: input signal fiber 20/125μm and passive double clad fiber 25/300 μm at the output.

  8. Polydimethylsiloxane fibers for optical fiber sensor of displacement

    NASA Astrophysics Data System (ADS)

    Martincek, Ivan; Pudis, Dusan; Gaso, Peter

    2013-09-01

    The paper describes the preparation of polydimethylsiloxane (PDMS) fiber integrated on the conventional optical fibers and their use for optical fiber displacement sensor. PDMS fiber was made of silicone elastomer Sylgard 184 (Dow Corning) by drawing from partially cured silicone. Optical fiber displacement sensor using PDMS fiber is based on the measurement of the local minimum of optical signal in visible spectral range generated by intermodal interference of circularly symmetric modes. Position of the local minimum in spectral range varies by stretching the PDMS fiber of 230 μm in the wavelength range from 688 to 477 nm. In the stretched PDMS fiber is possible to determine the longitudinal displacement with an accuracy of approximately 1 micrometer.

  9. 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.

  10. 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.

  11. 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.

  12. Fiber optic calorimetry

    SciTech Connect

    Rudy, C.; Bayliss, S.; Bracken, D.; Bush, J.; Davis, P.

    1998-01-01

    A twin-bridge calorimeter using optical fiber as the sensor element was constructed and tested. This system demonstrates the principle and capability of using fiber for heat-flow measurements of special nuclear material. This calorimeter uses piezoelectric-generated phase-carrier modulation with subsequent electronic signal processing to allow phase shifts as small as 1 microradian ({mu}rad) to be measured. The sensing element consists of 21-m lengths of single-mode optical fiber wrapped around sample and reference chambers. The sensitivity of the calorimeter was determined to be 74 radians (rad) of phase shift per milliwatt of thermal power. One milliwatt of thermal power is equivalent to 400 mg of plutonium (6% {sup 240}Pu). The system noise base was about 0.2 rad, equivalent to about 1 mg of plutonium.

  13. Fiber Optic Calorimetry

    SciTech Connect

    Rudy, C.; Bayliss, S.; Bracken, D.; Bush, J.; Davis, P.

    1997-12-12

    A twin-bridge calorimeter using optical fiber as the sensor element was constructed and tested. This system demonstrates the principle and capability of using optical fibers for heat-flow measurements of special nuclear material. This calorimeter uses piezoelectric-generated phase-carrier modulation with subsequent electronic signal processes to allow phase shifts as small as 1 microradian ({micro}rad) to be measured. The sensing element consists of 21-m lengths of single-mode optical fiber wrapped around sample and reference chambers. The sensitivity of the calorimeter was determined to be 74 radians (rad) of phase shift per milliwatt of thermal power. One milliwatt of thermal power is equivalent to 400 mg of plutonium (6% {sup 240}Pu). The system noise base was about 0.2 rad, equivalent to about 1 mg of plutonium.

  14. Carbon Fibers Conductivity Studies

    NASA Technical Reports Server (NTRS)

    Yang, C. Y.; Butkus, A. M.

    1980-01-01

    In an attempt to understand the process of electrical conduction in polyacrylonitrile (PAN)-based carbon fibers, calculations were carried out on cluster models of the fiber consisting of carbon, nitrogen, and hydrogen atoms using the modified intermediate neglect of differential overlap (MINDO) molecular orbital (MO) method. The models were developed based on the assumption that PAN carbon fibers obtained with heat treatment temperatures (HTT) below 1000 C retain nitrogen in a graphite-like lattice. For clusters modeling an edge nitrogen site, analysis of the occupied MO's indicated an electron distribution similar to that of graphite. A similar analysis for the somewhat less stable interior nitrogen site revealed a partially localized II electron distribution around the nitrogen atom. The differences in bonding trends and structural stability between edge and interior nitrogen clusters led to a two-step process proposed for nitrogen evolution with increasing HTT.

  15. Femtosecond Fiber Lasers

    NASA Astrophysics Data System (ADS)

    Bock, Katherine J.

    This thesis focuses on research I have done on ytterbium-doped femtosecond fiber lasers. These lasers operate in the near infrared region, lasing at 1030 nm. This wavelength is particularly important in biomedical applications, which includes but is not limited to confocal microscopy and ablation for surgical incisions. Furthermore, fiber lasers are advantageous compared to solid state lasers in terms of their cost, form factor, and ease of use. Solid state lasers still dominate the market due to their comparatively high energy pulses. High energy pulse generation in fiber lasers is hindered by either optical wave breaking or by multipulsing. One of the main challenges for fiber lasers is to overcome these limitations to achieve high energy pulses. The motivation for the work done in this thesis is increasing the output pulse peak power and energy. The main idea of the work is that decreasing the nonlinearity that acts on the pulse inside the cavity will prevent optical wave breaking, and thus will generate higher energy pulses. By increasing the output energy, ytterbium-doped femtosecond fiber lasers can be competitive with solid state lasers which are used commonly in research. Although fiber lasers tend to lack the wavelength tuning ability of solid state lasers, many biomedical applications take advantage of the 1030 microm central wavelength of ytterbium-doped fiber lasers, so the major limiting factor of fiber lasers in this field is simply the output power. By increasing the output energy without resorting to external amplification, the cavity is optimized and cost can remain low and economical. During verification of the main idea, the cavity was examined for possible back-reflections and for components with narrow spectral bandwidths which may have contributed to the presence of multipulsing. Distinct cases of multipulsing, bound pulse and harmonic mode-locking, were observed and recorded as they may be of more interest in the future. The third

  16. 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. PMID:27506352

  17. 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.

    PubMed

    Eganhouse, Robert P; DiFilippo, Erica L

    2015-10-01

    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. PMID:26346188

  18. The crucial fiber components and gain fiber for high power ytterbium-doped fiber laser

    NASA Astrophysics Data System (ADS)

    Liao, Lei; Liu, Peng; Xing, Ying-Bin; Wang, Yi-Bo; Dai, Neng-Li; Li, Jin-Yan; He, Bing; Zhou, Jun

    2015-08-01

    We have demonstrated a kW continuous-wave ytterbium-doped all-fiber laser oscillator with 7×1 fused fiber bundle combiner, fiber Bragg grating (FBG) and double-clad gain fiber fabricated by corresponding technologies. The results of experiment that the oscillator had operated at 1079.48nm with 80.94% slope efficiency without the influence of temperature and non-linear effects indicate that fiber components and gain fiber were suitable to high power environment. No evidence of the signal power roll-over showed that this oscillator possess the capacity to highest output with available pump power.

  19. 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.

  20. 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.

  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 bundle endocytoscopy

    PubMed Central

    Hughes, Michael; Chang, Tou Pin; Yang, Guang-Zhong

    2013-01-01

    Endocytoscopy is an optical biopsy technique which uses a miniaturized camera to capture white light microscopy images through an endoscope. We have developed an alternative design that instead relays images to an external camera via a coherent fiber bundle. In this paper we characterize the device and demonstrate microscopy of porcine tissue ex vivo. One advantage of our approach is the ease with which other bundle-compatible imaging modalities can be deployed simultaneously. We show this by acquiring quasi-simultaneous endocytoscopy and fluorescence confocal endomicroscopy images through a single fiber bundle. This opens up possibilities for multi-modal endomicroscopy, combining white light and fluorescence imaging. PMID:24409380

  3. 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

  4. 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,

  5. Boron nitride converted carbon fiber

    DOEpatents

    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.

  6. High-Speed Fiber Switches

    NASA Astrophysics Data System (ADS)

    Margulis, Walter; Tarasenko, Oleksandr; Yu, Zhangwei; Fonjallaz, Pierre-Yves; Knape, Harald

    2008-10-01

    All-fiber optical switches based on fiber with electrodes exhibit transition times <10 ns. The devices are monolithic and robust, they are simple and could potentially be manufactured at low cost. The insertion loss is extremely low and the devices are compatible with single mode fiber technology. Two types of switches are discussed, one based on polarization rotation, the other one relying on the wavelength shift of a fiber Bragg grating (FBG).

  7. Compound fiber ring resonator: Theory

    SciTech Connect

    Zhang, J.; Lit, J.W.Y.

    1994-06-01

    A compound fiber ring resonator is made with a Fabry-Perot etalon built inside a fiber ring that is fed through a 2 x 2 directional single-mode fiber coupler. It is theoretically analyzed by an unfolded equivalent model and a transfer-matrix method. The output intensities are presented, and four cases are discussed. The results may be useful in applications such as fiber spectrum analyzers, sensors, and lasers. 25 refs., 9 figs.

  8. 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.

  9. 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)

  10. 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.

  11. 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.

  12. 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)

  13. 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)

  14. 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.

  15. Direct spinning of fiber supercapacitor.

    PubMed

    Xu, Tong; Ding, Xiaoteng; Liang, Yuan; Zhao, Yang; Chen, Nan; Qu, Liangti

    2016-06-16

    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.

  16. 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.

  17. 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

  18. Whole Grains and Fiber

    MedlinePlus

    ... fiber. Some examples of refined grains are wheat flour, enriched bread and white rice. Most refined grains are enriched , which means that ... grains. Some examples of enriched grains are wheat flour, enriched bread and white rice. Eating whole grains provides important health benefits: Many ...

  19. Electrodes with fiber structure

    NASA Technical Reports Server (NTRS)

    Benczur-Uermoessy, G.; Berger, G.; Haschka, F.

    1986-01-01

    An electrode framework with a fiber structure, universally applicable in alkaline storage battery systems, was developed and readied for production. Storage batteries with these electrodes present higher energy and power densities and are economical to produce. The design is applicable to all rechargable storage batteries and might replace the previous variety of designs.

  20. 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.

  1. 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.

  2. 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.

  3. 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.

  4. 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.

  5. 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

  6. 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…

  7. 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.

  8. 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).

  9. Cryogenic Fiber Optic Sensors Based on Fiber Bragg Gratings

    NASA Astrophysics Data System (ADS)

    Swinehart, P. R.; Maklad, M.; Courts, S. S.

    2008-03-01

    Fiber optic sensing has many favorable characteristics—a single fiber can be used to multiplex multiple sensors along the length of the fiber, fiber optic sensing is immune to electromagnetic noise and is inherently safe for combustible liquids and atmospheres. Previously, fiber optic sensors based on fiber Bragg gratings (FBGs) have been demonstrated for cryogenic use for both temperature and strain sensing, but often little data is supplied as to the reproducibility or unit-to-unit uniformity of these sensors. Lake Shore Cryotronics has manufactured fiber optic cryogenic temperature sensors based on Bragg gratings using novel packaging techniques. The temperature response and reproducibility is reported from 80K to 480K for glass-packaged sensors, and a calibration for a high sensitivity, wide range zinc-packaged sensor is reported.

  10. 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.

  11. In situ growth of IRMOF-3 combined with ionic liquids to prepare solid-phase microextraction fibers.

    PubMed

    Zheng, Juan; Li, Siyan; Wang, Ying; Li, Lei; Su, Chengyong; Liu, Hong; Zhu, Fang; Jiang, Ruifen; Ouyang, Gangfeng

    2014-06-01

    A superior solid-phase microextraction (SPME) fiber-coating material, IRMOF-3@ILs/PDMS, was prepared by the in situ growth of IRMOF-3 onto stainless-steel wires and protection with ionic liquids (ILs) and polydimethylsiloxane (PDMS). The ILs can efficiently prevent the substantial cracking of IRMOF-3 caused by moisture, and a thin PDMS film can protect the IRMOF-3@ILs material to achieve a much better extraction efficiency as well as excellent resistance to high temperature and high humidity. This IRMOF-3@ILs/PDMS coating possessed a porous structure, a rough surface and an increased lifespan (by at least 100 times) compared with that of IRMOF-3. The coating was evaluated by analyzing four polycyclic aromatic hydrocarbons (PAHs) in water, and good precision (<7.7%), low detection limits (12.0-15.4 ng L(-1)), and wide linearity (50-20,000 ng L(-1)) were achieved under the optimized conditions. The fiber was successfully applied to the sensitive analysis of PAHs in rainwater by coupling it with gas chromatography-mass spectrometry (GC-MS).

  12. Modal interference fiber optic sensor

    NASA Astrophysics Data System (ADS)

    Kondrat, Marcin; Szustakowski, Mieczyslaw; Gorka, Andrzej; Palka, Norbert; Zyczkowski, Marek; Niznik, Sylwester

    2004-11-01

    Modal Interference Fiber Optic Sensor (MIFOS) for permanent monitoring of the network is presented. A mechanical disturbance of a fiber cable influences on intensity distribution at the end-face of a multimode fiber. Variations in interfering images are analysed by means of a digital processing unit that determines the alarm in case of unauthorized access along the whole length of the fiber. A contrast of an interference pattern and a procedure of fiber optic selection for the sensor are shown. A simple criterion that bases on changes of local maximums positions of the interference patterns is applied. A laboratory arrangement of the sensor and its experimental research are shown.

  13. 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.

  14. Fiber gyroscope with birefringence modulation

    NASA Astrophysics Data System (ADS)

    Carrara, S. L. A.; Kim, B. Y.; Shaw, H. J.

    1987-03-01

    A theoretical analysis of the nonreciprocal phase error in a highly-birefringent fiber gyroscope is presented, characterizing the different types of errors and their sources in a general form. These error terms are due to polarization cross coupling in the fiber and in the fiber components and can be reduced by modulating the magnitude of the fiber birefringence at appropriate locations in the optical circuit and by balancing the optical power between the two polarization eigenmodes of the fiber at the input of the interferometer. Experimental results demonstrating these techniques show a 20 dB relief on the performance requirements of the polarizer usually employed for drift reduction.

  15. Multimetallic Electrodeposition on Carbon Fibers

    NASA Astrophysics Data System (ADS)

    Böttger-Hiller, F.; Kleiber, J.; Böttger, T.; Lampke, T.

    2016-03-01

    Efficient lightweight design requires intelligent materials that meet versatile functions. One approach is to extend the range of properties of carbon fiber reinforced plastics (CFRP) by plating the fiber component. Electroplating leads to metalized layers on carbon fibers. Herein only cyanide-free electrolytes where used. Until now dendrite-free layers were only obtained using current densities below 1.0 A dm-2. In this work, dendrite-free tin and copper coatings were achieved by pre-metalizing the carbon fiber substrates. Furthermore, applying a combination of two metals with different sized thermal expansion coefficient lead to a bimetallic coating on carbon fiber rovings, which show an actuatory effect.

  16. 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.

  17. Gasifiable carbon-graphite fibers

    NASA Technical Reports Server (NTRS)

    Humphrey, Marshall F. (Inventor); Ramohalli, Kumar N. R. (Inventor); Dowler, Warren L. (Inventor)

    1982-01-01

    Fine, carbon-graphite fibers do not combust during the combustion of a composite and are expelled into the air as fine conductive particles. Coating of the fibers with a salt of a metal having a work function below 4.2 eV such as an alkaline earth metal salt, e.g., calcium acetate, catalytically enhances combustion of the fibers at temperatures below 1000.degree. C. such that the fibers self-support combustion and burn to produce a non-conductive ash. Fire-polishing the fibers before application of the coating is desirable to remove sizing to expose the carbon surface to the catalyst.

  18. Silica optical fibers: technology update

    NASA Astrophysics Data System (ADS)

    Krohn, David A.; McCann, Brian P.

    1995-05-01

    Silica-core optical fibers have long been the standard delivery medium for medical laser delivery systems. Their high strength, excellent flexibility, and low cost continue to make them the fiber of choice for systems operating from 300 to 2200 nm. An overview of the current fiber constructions available to the industry is reviewed. Silicone-clad fibers, hard- fluoropolymer clad fibers and silica-clad fibers are briefly compared in terms of mechanical and optical properties. The variety of fiber coatings available is also discussed. A significant product development of silica fiber delivery systems has been in side-firing laser delivery systems for Urology. These devices utilize silica-core fibers to project the laser energy at a substantial lateral angle to the conventional delivery system, typically 40 to 100 degrees off axis. Many unique distal tips have been designed to meet the needs of this potentially enormous application. There are three primary technologies employed in side-firing laser delivery systems: reflection off of an attached medium; reflection within an angle-polished fiber through total internal reflection; and reflection from both an angle-polished fiber and an outside medium. Each technology is presented and compared on the basis of operation modality, transmission efficiency, and power-handling performance.

  19. [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.

  20. 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.

  1. Single mode fiber and twin-core fiber connection technique for in-fiber integrated interferometer

    NASA Astrophysics Data System (ADS)

    Yuan, Tingting; Zhang, Xiaotong; Guan, Chunying; Yang, Xinghua; Yuan, Libo

    2015-09-01

    A novel twin-core fiber connector has been made by two side-polished fibers. By using side polishing technique, we present a connector based on the twin-core fiber (TCF) and two D-shaped single-core fibers. After simple alignment and splicing, all fiber miniaturizing connector can be obtained. Two cores can operate independently and are non-interfering. The coupling loss of this connector is low and the fabrication technologies are mature. The connector device could be used for sensors or particle trapping.

  2. 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.

  3. 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.

  4. Optical fiber smartphone spectrometer.

    PubMed

    Hossain, Md Arafat; Canning, John; Cook, Kevin; Jamalipour, Abbas

    2016-05-15

    An optical fiber-based smartphone spectrometer incorporating an endoscopic fiber bundle is demonstrated. The endoscope allows transmission of the smartphone camera LED light to a sample, removing complications from varying background illumination. The reflected spectra collected from a surface or interface is dispersed onto the camera CMOS using a reflecting diffraction grating. A spectral resolution as low as δλ∼2.0  nm over a bandwidth of Δλ∼250  nm is obtained using a slit width, ωslit=0.7  mm. The instrument has vast potential in a number of industrial applications including agricultural produce analysis. Spectral analysis of apples shows straightforward measurement of the pigments anthocyanins, carotenoid, and chlorophyll, all of which decrease with increasing storage time. PMID:27176971

  5. 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.

  6. 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.

  7. Fiber optic TV direct

    NASA Astrophysics Data System (ADS)

    Kassak, John E.

    1991-12-01

    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.

  8. 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.

  9. 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.

  10. Hydrogen loading to the optic fibers for fiber grating sensors

    NASA Astrophysics Data System (ADS)

    Xiao, Chun; Zhang, Wen-yu; Zhu, Yuan; Pan, Zhi-yong

    2014-12-01

    In this paper, fibers with different depths of hermetically coated carbon are hydrogen loaded and radiated, and it's found that too thick of carbon layer around fiber can't bring best radiation-resistant properties, because the thick carbon layer would make the entering of hydrogen difficult although it can help to stop the hydrogen escaping. We also research the duration of saturated hydrogen loading under the temperature of 60°C and 100°C respectively, and it's found that after 120h and 48h, the fibers' photo sensitivities tend to be flat. We also reload hydrogen into the fibers which have been loaded once, and these fibers are etched then, this help us to deep understand the mechanism of hydrogen loading for the fiber gratings.

  11. Piezoelectric ceramic fibers for active fiber composites: a comparative study

    NASA Astrophysics Data System (ADS)

    Kornmann, Xavier; Huber, Christian; Elsener, Hans-Rudolf

    2003-08-01

    The morphology and the free strain performances of three different piezoelectric ceramic fibers used for the manufacture of active fiber composites (AFCs) have been investigated. The morphology of the fibers has a direct influence on the manufacture of the AFCs. Fibers with non-uniform diameters are more difficult to contact with the interdigitated electrodes and can be the cause of irreparable damages in AFCs. An indirect method requiring the use of a simple analytical model is proposed to evaluate the free strain of active fiber composites. This indirect method presents a relatively good agreement with direct free strain measurements performed with strain gages glued on both sides of an AFC. The results show a systematic difference of ca. 20 % between the indirect and the direct methods. However, the indirect method did not permit to see differences of piezoelectric performance between the types of fibers.

  12. Homogenization of long fiber reinforced composites including fiber bending effects

    NASA Astrophysics Data System (ADS)

    Poulios, Konstantinos; Niordson, Christian F.

    2016-09-01

    This paper presents a homogenization method, which accounts for intrinsic size effects related to the fiber diameter in long fiber reinforced composite materials with two independent constitutive models for the matrix and fiber materials. A new choice of internal kinematic variables allows to maintain the kinematics of the two material phases independent from the assumed constitutive models, so that stress-deformation relationships, can be expressed in the framework of hyper-elasticity and hyper-elastoplasticity for the fiber and the matrix materials respectively. The bending stiffness of the reinforcing fibers is captured by higher order strain terms, resulting in an accurate representation of the micro-mechanical behavior of the composite. Numerical examples show that the accuracy of the proposed model is very close to a non-homogenized finite-element model with an explicit discretization of the matrix and the fibers.

  13. 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.

  14. Comparisons of methods measuring fiber maturity and fineness of Upland cotton fibers containing different degree of fiber cell wall development.

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Fiber maturity and fineness are important physical properties of cotton fibers affecting qualities of fibers and yarns. A number of direct and indirect methods are used for measuring fiber maturity and fineness from mature fibers that are thick secondary cell walls composed of almost pure cellulose....

  15. Critical reviews of fiber-optic communication technology Optical fibers

    NASA Astrophysics Data System (ADS)

    Kapron, F. P.

    The review begins with brief highlights of the history of fiber optics, followed by a discussion of the attributes of shortwave and longwave transmission. This leads to an investigation of various fiber types, short-haul considerations, and then single-mode aspects. Specialty fiber is briefly covered, followed by a survey of several research trends today that will lead to new systems capabilities in the future. No references are given, since hundreds would be necessary to make the list even partially complete.

  16. 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

    2015-08-01

    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.

  17. 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

    2015-08-01

    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. PMID:26138604

  18. 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.

  19. 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

  20. 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. PMID:22666011

  1. 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

  2. Multichannel laser-fiber vibrometer

    NASA Astrophysics Data System (ADS)

    Dudzik, Grzegorz; Waz, Adam; Kaczmarek, Pawel; Antonczak, Arkadiusz; Sotor, Jaroslaw; Krzempek, Karol; Sobon, Grzegorz; Abramski, Krzysztof M.

    2013-01-01

    For the last few years we were elaborating the laser-fiber vibrometer working at 1550 nm. Our main stress was directed towards different aspects of research: analysis of scattered light, efficient photodetection, optimization of the fiber-free space interfaces and signal processing. As a consequence we proposed the idea of a multichannel fiber vibrometer based on well developed telecommunication technique - Wavelength Division Multiplexing (WDM). One of the most important parts of a fiber-laser vibrometer is demodulation electronic section. The distortion, nonlinearity, offset and added noise of measured signal come from electronic circuits and they have direct influence on finale measuring results. We present the results of finished project "Developing novel laser-fiber monitoring technologies to prevent environmental hazards from vibrating objects" where we have constructed a 4-channel WDM laser-fiber vibrometer.

  3. 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.

  4. 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.

  5. Comparison of fiber polishing techniques

    SciTech Connect

    Hanlet, P.; Marcus, M.; Lindenmeyer, C.

    1999-03-30

    Many D0 Run II detectors currently in production rely on scintillating tile and fiber technology. In general, light from active scintillating elements or calibration signals is transported to the photodetection system along optical fiber pathways. Building a tile/fiber detector requires very conscientious technical support and a high degree of quality control; polishing fibers is one of the most delicate of tasks involved. This note compares three methods used to polish Hewlett Packard HFBR-RUS500 fiber. This type of fiber is expected to be used in both the Muon Scintillator Counters (MSC) and the InterCryostat Detector (ICD) calibration systems to transport light from the LED distribution block to the photomultiplier tubes.

  6. 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.

  7. Fiber laser development for LISA

    NASA Astrophysics Data System (ADS)

    Numata, Kenji; Chen, Jeffrey R.; Camp, Jordan

    2010-05-01

    We have developed a linearly-polarized Ytterbium-doped fiber ring laser with single longitudinal-mode output at 1064 nm 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 100 kHz. It appears that our fiber ring laser is promising for space applications where robustness of fiber optics is desirable.

  8. Communicating On The Moon Via Fiber Optics

    NASA Technical Reports Server (NTRS)

    Lutes, George F.

    1992-01-01

    Report discusses feasibility of communicating over long distances on Moon via fiber optics. Compares fiber-optic and microwave technologies, concluding fiber optics offer less consumption of power, less weight, less bulk, and lower cost. Present commercial fiber-optic technology appears usable on Moon with minor modifications. Includes tutorial chapter on fiber-optic-communication technology and chapter on efforts to improve technology.

  9. 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.

  10. Producing Silicon Carbide/Silicon Nitride Fibers

    NASA Technical Reports Server (NTRS)

    1986-01-01

    Manufacturing process makes CxSiyNz fibers. Precursor fibers spun from extruding machine charged with polycarbosilazane resin. When pyrolyzed, resin converted to cross-linked mixture of silicon carbide and silicon nitride, still in fiber form. CxSiyNz fibers promising substitutes for carbon fibers in high-strength, low-weight composites where high electrical conductivity unwanted.

  11. Dissemination, redissemination and fiber life

    NASA Technical Reports Server (NTRS)

    Eiber, W.

    1979-01-01

    The technical background of dissemination of carbon fibers as well as the possibility of redissemination and fiber life are outlined. Plume spread and weather, measures of pollution and of damage potential, and parameters controlling dissemination patterns are among the topics discussed. It is shown that the redissemination rate off hard surfaces decreases with time and that fiber length decreases with time. Redissemination from vegetated land is shown to be insignificant.

  12. Actuating Fibers: Design and Applications.

    PubMed

    Stoychev, Georgi V; Ionov, Leonid

    2016-09-21

    Actuators are devices capable of moving or controlling objects and systems by applying mechanical force on them. Among all kinds of actuators with different shapes, fibrous ones deserve particular attention. In spite of their apparent simplicity, actuating fibers allow for very complex actuation behavior. This review discusses different approaches for the design of actuating fibers, and their advantages and disadvantages. We also discuss the prospects for the design of fibers with advanced architectures and complex actuation behavior. PMID:27571481

  13. Fiber Sagnac interferometer temperature sensor

    SciTech Connect

    Starodumov, A.N.; Zenteno, L.A.; Monzon, D.; De La Rosa, E.

    1997-01-01

    A modified Sagnac interferometer-based fiber temperature sensor is proposed. Polarization independent operation and high temperature sensitivity of this class of sensors make them cost effective instruments for temperature measurements. A comparison of the proposed sensor with Bragg grating and long-period grating fiber sensors is derived. A temperature-induced spectral displacement of 0.99 nm/K is demonstrated for an internal stress birefringent fiber-based Sagnac interferometer. {copyright} {ital 1997 American Institute of Physics.}

  14. Electrochromic fiber-shaped supercapacitors.

    PubMed

    Chen, Xuli; Lin, Huijuan; Deng, Jue; Zhang, Ye; Sun, Xuemei; Chen, Peining; Fang, Xin; Zhang, Zhitao; Guan, Guozhen; Peng, Huisheng

    2014-12-23

    An electrochromic fiber-shaped super-capacitor is developed by winding aligned carbon nanotube/polyaniline composite sheets on an elastic fiber. The fiber-shaped supercapacitors demonstrate rapid and reversible chromatic transitions under different working states, which can be directly observed by the naked eye. They are also stretchable and flexible, and are woven into textiles to display designed signals in addition to storing energy.

  15. Source of released carbon fibers

    NASA Technical Reports Server (NTRS)

    Bell, V. L.

    1979-01-01

    The potential for the release of carbon fibers from aircraft crashes/fires is addressed. Simulation of the conditions of aircraft crash fires in order to predict the quantities and forms of fibrous materials which might be released from civilian aircraft crashes/fires is considered. Figures are presented which describe some typical fiber release test activities together with some very preliminary results of those activities. The state of the art of carbon fiber release is summarized as well as some of the uncertainties concerning accidental fiber release.

  16. Photonic crystal fibers in biophotonics

    NASA Astrophysics Data System (ADS)

    Tuchin, Valery V.; Skibina, Julia S.; Malinin, Anton V.

    2011-12-01

    We observed recent experimental results in area of photonic crystal fibers appliance. Possibility of creation of fiberbased broadband light sources for high resolution optical coherence tomography is discussed. Using of femtosecond pulse laser allows for generation of optical radiation with large spectral width in highly nonlinear solid core photonic crystal fibers. Concept of exploitation of hollow core photonic crystal fibers in optical sensing is demonstrated. The use of photonic crystal fibers as "smart cuvette" gives rise to efficiency of modern optical biomedical analysis methods.

  17. Annealing of silicon optical fibers

    NASA Astrophysics Data System (ADS)

    Gupta, N.; McMillen, C.; Singh, R.; Podila, R.; Rao, A. M.; Hawkins, T.; Foy, P.; Morris, S.; Rice, R.; Poole, K. F.; Zhu, L.; Ballato, J.

    2011-11-01

    The recent realization of silicon core optical fibers has the potential for novel low insertion loss rack-to-rack optical interconnects and a number of other uses in sensing and biomedical applications. To the best of our knowledge, incoherent light source based rapid photothermal processing (RPP) was used for the first time to anneal glass-clad silicon core optical fibers. X-ray diffraction examination of the silicon core showed a considerable enhancement in the length and amount of single crystallinity post-annealing. Further, shifts in the Raman frequency of the silicon in the optical fiber core that were present in the as-drawn fibers were removed following the RPP treatment. Such results indicate that the RPP treatment increases the local crystallinity and therefore assists in the reduction of the local stresses in the core, leading to more homogenous fibers. The dark current-voltage characteristics of annealed silicon optical fiber diodes showed lower leakage current than the diodes based on as-drawn fibers. Photons in UV and vacuum ultraviolet (VUV) regions play a very important role in improving the bulk and carrier transport properties of RPP-treated silicon optical fibers, and the resultant annealing permits a path forward to in situ enhancement of the structure and properties of these new crystalline core optical fibers.

  18. Density of intercalated graphite fibers

    NASA Technical Reports Server (NTRS)

    Gaier, James R.; Slabe, Melissa E.

    1990-01-01

    The density of Amoco P-55, P-75, P-100, and P-120 pitch-based graphite fibers and their intercalation compounds with bromine, iodine monochloride, and copper (II) chloride have been measured using a density gradient column. The distribution of densities within a fiber type is found to be a sensitive indicator of the quality of the intercalation reaction. In all cases the density was found to increase, indicating that the mass added to the graphite is dominant over fiber expansion. Density increases are small (less than 10 percent) giving credence to a model of the intercalated graphite fibers which have regions which are intercalated and regions which are not.

  19. Density of intercalated graphite fibers

    NASA Technical Reports Server (NTRS)

    Gaier, James R.; Slabe, Melissa E.

    1989-01-01

    The density of Amoco P-55, P-75, P-100, and P-120 pitch-based graphite fibers and their intercalation compounds with bromine, iodine monochloride, and copper (II) chloride have been measured using a density gradient column. The distribution of densities within a fiber type is found to be a sensitive indicator of the quality of the intercalation reaction. In all cases the density was found to increase, indicating that the mass added to the graphite is dominant over fiber expansion. Density increases are small (less than 10 percent) giving credence to a model of the intercalated graphite fibers which have regions which are intercalated and regions which are not.

  20. 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. PMID:25624035

  1. 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.

  2. Wear of metal fiber brushes

    NASA Astrophysics Data System (ADS)

    Brown, Lloyd Perryman, Jr.

    The goal of this dissertation was determining the wear mechanism of metal fiber brushes on commutators and slip rings with the goal of achieving the lowest possible wear rate. To this end, metal fiber brushes were operated, while conducting direct current, on gold-plated copper rotors with and without unfilled gaps to simulate slip rings and commutators, respectively. Wear rates on unfilled-groove commutators were found to be only modestly higher than on slip ring style rotors. Three possible causes for enhanced metal fiber brush wear on commutators were considered: (i) accelerated "adhesive" wear controlled by contact spots, (ii) fatigue induced wear and (iii) "fiber chopping". Similarly, SEM analysis of fiber tips and wear particles produced scant, if any, evidence of fiber chopping, which would occur as, again, fiber tips extend elastically into the commutator grooves and small slices of them would be "chopped" off by oncoming edges of commutator bars. Finally considered was "modified chopping", wherein fiber tips would be dragged over groove edges, resulting in tensile fracture and chopping. Only a single fiber fragment showed damage that might be compatible with that mechanism. Moreover, the fact that it was exemplified by a single tenuous case, rules it out as significant. The same conclusion also follows from comparing commutator wear rates with that on slip rings. These show good correlation in terms of effective brush pressure, which on commutators is increased because only bars conduct current and gaps do not support load. (Abstract shortened by UMI.)

  3. 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.

  4. Development of a SPME-GC-MS method for the determination of volatile compounds in Shanxi aged vinegar and its analytical characterization by aroma wheel.

    PubMed

    Zhu, Hong; Zhu, Jie; Wang, Lili; Li, Zaigui

    2016-01-01

    A solid-phase microextraction followed by gas chromatography-mass spectrometry method was developed to determine the volatile compounds in Shanxi aged vinegar. The optimal extraction conditions were: 50 °C for 20 min with a PDMS/DVB fiber. This analytical method was validated and showed satisfactory repeatability (0.5 %

  5. 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.

  6. Fiber reinforced superalloys

    NASA Technical Reports Server (NTRS)

    Petrasek, Donald W.; Signorelli, Robert A.; Caulfield, Thomas; Tien, John K.

    1987-01-01

    Improved performance of heat engines is largely dependent upon maximum cycle temperatures. Tungsten fiber reinforced superalloys (TFRS) are the first of a family of high temperature composites that offer the potential for significantly raising hot component operating temperatures and thus leading to improved heat engine performance. This status review of TFRS research emphasizes the promising property data developed to date, the status of TFRS composite airfoil fabrication technology, and the areas requiring more attention to assure their applicability to hot section components of aircraft gas turbine engines.

  7. Fiber optic sensing system

    NASA Technical Reports Server (NTRS)

    Adamovsky, Grigory (Inventor)

    1991-01-01

    A fiber optic interferometer utilizes a low coherence light emitting diode (LED) laser as a light source which is filtered and driven at two RF frequencies, high and low, that are specific to the initial length of the resonator chamber. A displacement of a reflecting mirror changes the length traveled by the nonreferencing signal. The low frequency light undergoes destructive interference which reduces the average intensity of the wave while the high frequency light undergoes constructive interference which increases the average intensity of the wave. The ratio of these two intensity measurements is proportional to the displacement incurred.

  8. Fiber optic geophysical sensors

    DOEpatents

    Homuth, E.F.

    1991-03-19

    A fiber optic geophysical sensor is described 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. 2 figures.

  9. Fiber optic systems for mobile platforms II

    SciTech Connect

    Lewis, N.E.; Moore, E.L.

    1988-01-01

    This book contains papers presented at the symposium of International Society for Optical Engineering. Topics covered/include: Fiber optic pressure sensor for internal combustion engine; Automotive fiber optic technology: application issues; and Fiber optic guided missile.

  10. Genetics Home Reference: small fiber neuropathy

    MedlinePlus

    ... Home Health Conditions small fiber neuropathy small fiber neuropathy Enable Javascript to view the expand/collapse boxes. ... PDF Open All Close All Description Small fiber neuropathy is a condition characterized by severe pain attacks ...

  11. Stronger Carbon Fibers for Reinforced Plastics

    NASA Technical Reports Server (NTRS)

    Cagliostro, D. E.; Lerner, N. R.

    1983-01-01

    Process makes fibers 70 percent stronger at lower carbonization temperature. Stronger carbon fibers result from benzoic acid pretreatment and addition of acetylene to nitrogen carbonizing atmosphere. New process also makes carbon fibers of higher electrical resistance -- an important safety consideration.

  12. 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

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

    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

  14. Carbon Fiber Biocompatibility for Implants

    PubMed Central

    Petersen, Richard

    2016-01-01

    Carbon fibers have multiple potential advantages in developing high-strength biomaterials with a density close to bone for better stress transfer and electrical properties that enhance tissue formation. As a breakthrough example in biomaterials, a 1.5 mm diameter bisphenol-epoxy/carbon-fiber-reinforced composite rod was compared for two weeks in a rat tibia model with a similar 1.5 mm diameter titanium-6-4 alloy screw manufactured to retain bone implants. Results showed that carbon-fiber-reinforced composite stimulated osseointegration inside the tibia bone marrow measured as percent bone area (PBA) to a great extent when compared to the titanium-6-4 alloy at statistically significant levels. PBA increased significantly with the carbon-fiber composite over the titanium-6-4 alloy for distances from the implant surfaces of 0.1 mm at 77.7% vs. 19.3% (p < 10−8) and 0.8 mm at 41.6% vs. 19.5% (p < 10−4), respectively. The review focuses on carbon fiber properties that increased PBA for enhanced implant osseointegration. Carbon fibers acting as polymer coated electrically conducting micro-biocircuits appear to provide a biocompatible semi-antioxidant property to remove damaging electron free radicals from the surrounding implant surface. Further, carbon fibers by removing excess electrons produced from the cellular mitochondrial electron transport chain during periods of hypoxia perhaps stimulate bone cell recruitment by free-radical chemotactic influences. In addition, well-studied bioorganic cell actin carbon fiber growth would appear to interface in close contact with the carbon-fiber-reinforced composite implant. Resulting subsequent actin carbon fiber/implant carbon fiber contacts then could help in discharging the electron biological overloads through electrochemical gradients to lower negative charges and lower concentration. PMID:26966555

  15. Coating Carbon Fibers With Platinum

    NASA Technical Reports Server (NTRS)

    Effinger, Michael R.; Duncan, Peter; Coupland, Duncan; Rigali, Mark J.

    2007-01-01

    A process for coating carbon fibers with platinum has been developed. The process may also be adaptable to coating carbon fibers with other noble and refractory metals, including rhenium and iridium. The coated carbon fibers would be used as ingredients of matrix/fiber composite materials that would resist oxidation at high temperatures. The metal coats would contribute to oxidation resistance by keeping atmospheric oxygen away from fibers when cracks form in the matrices. Other processes that have been used to coat carbon fibers with metals have significant disadvantages: Metal-vapor deposition processes yield coats that are nonuniform along both the lengths and the circumferences of the fibers. The electrical resistivities of carbon fibers are too high to be compatible with electrolytic processes. Metal/organic vapor deposition entails the use of expensive starting materials, it may be necessary to use a furnace, and the starting materials and/or materials generated in the process may be hazardous. The present process does not have these disadvantages. It yields uniform, nonporous coats and is relatively inexpensive. The process can be summarized as one of pretreatment followed by electroless deposition. The process consists of the following steps: The surfaces of the fiber are activated by deposition of palladium crystallites from a solution. The surface-activated fibers are immersed in a solution that contains platinum. A reducing agent is used to supply electrons to effect a chemical reduction in situ. The chemical reduction displaces the platinum from the solution. The displaced platinum becomes deposited on the fibers. Each platinum atom that has been deposited acts as a catalytic site for the deposition of another platinum atom. Hence, the deposition process can also be characterized as autocatalytic. The thickness of the deposited metal can be tailored via the duration of immersion and the chemical activity of the solution.

  16. Monolithic fiber end cap collimator for high-power free-space fiber-fiber coupling.

    PubMed

    Zhou, Xuanfeng; Chen, Zilun; Wang, Zefeng; Hou, Jing

    2016-05-20

    In this paper, we present the design, construction, and testing of a monolithic fiber end cap collimator for high-power free-space fiber-fiber coupling applications. The collimator is based on a large-sized fiber end cap and a spherical lens design on the output facet. Values of the spot size and working distance are theoretically analyzed based on Gaussian approximation and ABCD transmission matrix. The free-space fiber-fiber coupling process is also analyzed for different lens curvature radii and coupling distances. In the experiment, a collimated laser beam is obtained with Rayleigh length of about 400 mm. A high-power laser with 1.1 kW output is tested on the end cap collimator, which only heats up by 7°C at the output facet without active cooling. Free-space fiber-fiber coupling between two 20/400 μm fibers is achieved based on these collimators, with measured coupling loss lower than 0.3 dB. PMID:27411125

  17. Fiber breakage phenomena in long fiber reinforced plastic preparation

    NASA Astrophysics Data System (ADS)

    Huang, Chao-Tsai; Tseng, Huan-Chang; Vlcek, Jiri; Chang, Rong-Yeu

    2015-07-01

    Due to the high demand of smart green, the lightweight technologies have become the driving force for the development of automotives and other industries in recent years. Among those technologies, using short and long fiber-reinforced plastics (FRP) to replace some metal components can reduce the weight of an automotive significantly. However, the microstructures of fibers inside plastic matrix are too complicated to manage and control during the injection molding through the screw, the runner, the gate, and then into the cavity. This study focuses on the fiber breakage phenomena during the screw plastification. Results show that fiber breakage is strongly dependent on screw design and operation. When the screw geometry changes, the fiber breakage could be larger even with lower compression ratio.

  18. Mode-locked fiber lasers based on doped fiber arrays.

    PubMed

    Zhang, Xiao; Song, Yanrong

    2014-05-10

    We designed a new kind of mode-locked fiber laser based on fiber arrays, where the central core is doped. A theoretical model is given for an all-fiber self-starting mode-locked laser based on this kind of doped fiber array. Two different kinds of fiber lasers with negative dispersion and positive dispersion are simulated and discussed. The stable mode-locked pulses are generated from initial noise conditions by the realistic parameters. The process of self-starting mode-locking multipulse transition and the relationship between the energy of the central core and the propagation distance of the pulses are discussed. Finally, we analyze the difference between the averaged mode-locked laser and the discrete mode-locked laser.

  19. Graphite fiber intercalation: Basic properties of copper chloride intercalated fibers

    NASA Technical Reports Server (NTRS)

    Jaworske, D. A.; Miller, J. D.

    1986-01-01

    In situ resistance measurements were used to follow the intercalation of copper chloride in pitch-based fibers. Subsequent single fiber resistivity measurements reveal a large range of resistivities, from 13 to 160 micro-ohms cm. Additional density measurements reveal a bimodal distribution of mass densities. The dense fibers have lower resistivities and correspond to the stage III compound identified by X-ray diffraction. Neither resistivity nor density correlate with diameter. Both energy dispersive spectroscopy and mass density data suggest that excess chlorine resides in the intercalated fiber, resulting in a stoichiometry of C4.9n CuCl2.5 (where n is the stage number) for the denser fibers. Finally, thermogravimetric analysis shows a 33 percent loss in mass upon heating to 700C. This loss in mass is attributed to loss of both chlorine and carbon.

  20. 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%.