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Sample records for microextration spme fibers

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

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    Antonio Luiz Pires Valente

    2000-08-01

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

  2. Uptake of Radionuclide Metals by SPME Fibers

    International Nuclear Information System (INIS)

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

    2006-08-01

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

  3. Detection of Methyl Salicylate Transforted by Honeybees (Apis mellifera) Using Solid Phase Microextration (SPME) Fibers; TOPICAL

    International Nuclear Information System (INIS)

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

    2001-01-01

    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

  4. Detection of Methyl Salicylate Transforted by Honeybees (Apis mellifera) Using Solid Phase Microextration (SPME) Fibers

    Energy Technology Data Exchange (ETDEWEB)

    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.

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

    International Nuclear Information System (INIS)

    Umi Khairul Ahmad; Abdul Rahim Yacob; Selvaraju, Geetha

    2008-01-01

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

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

    International Nuclear Information System (INIS)

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

    2013-01-01

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

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

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    Wei Guan

    2012-03-01

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

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

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    Parviz Aberoomand Azar

    2013-01-01

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

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

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    Tajik Leila

    2017-09-01

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

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

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    Dongxia Ren

    2018-01-01

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

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

    Science.gov (United States)

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

    2018-01-01

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

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

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

    2017-11-01

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

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

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

    2016-01-15

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

  14. Usefulness of a PARAFAC decomposition in the fiber selection procedure to determine chlorophenols by means SPME-GC-MS.

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

    2012-05-01

    In this work, a procedure based on solid-phase microextraction and gas chromatography coupled with mass spectrometry is proposed to determine chlorophenols in water without derivatization. The following chlorophenols are studied: 2,4-dichlorophenol; 2,4,6-trichlorophenol; 2,3,4,6-tetrachlorophenol and pentachlorophenol. Three kinds of SPME fibers, polyacrylate, polydimethylsiloxane, and polydimethylsiloxane/divinylbenzene are compared to identify the most suitable one for the extraction process on the basis of two criteria: (a) to select the equilibrium time studying the kinetics of the extraction, and (b) to obtain the best values of the figures of merit. In both cases, a three-way PARAllel FACtor analysis decomposition is used. For the first step, the three-way experimental data are arranged as follows: if I extraction times are considered, the tensor of data, X, of dimensions I × J × K is generated by concatenating the I matrices formed by the abundances of the J m/z ions recorded in K elution times around the retention time for each chlorophenol. The second-order property of PARAFAC (or PARAFAC2) assesses the unequivocal identification of each chlorophenol, as consequence, the loadings in the first mode estimated by the PARAFAC decomposition are the kinetic profile. For the second step, a calibration based on a PARAFAC decomposition is used for each fiber. The best figures of merit were obtained with PDMS/DVB fiber. The values of decision limit, CCα, achieved are between 0.29 and 0.67 μg L(-1) for the four chlorophenols. The accuracy (trueness and precision) of the procedure was assessed. This procedure has been applied to river water samples.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-08-15

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

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

    International Nuclear Information System (INIS)

    Budziak, Dilma; Martendal, Edmar; Carasek, Eduardo

    2008-01-01

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

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

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    Celia Eliane de Lara da Silva

    2013-01-01

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

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

    Science.gov (United States)

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

    2018-02-05

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

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

    Science.gov (United States)

    Abdolhosseini, Sana; Ghiasvand, Alireza; Heidari, Nahid

    2017-09-01

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

  20. 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.

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    Reza Hosseinzadeh

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

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

    International Nuclear Information System (INIS)

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

    2009-01-01

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

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

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    D’Auria, M.

    2017-06-01

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

  3. Quantification of Carbonyl Compounds Generated from Ozone-Based Food Colorants Decomposition Using On-Fiber Derivatization-SPME-GC-MS

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    Wenda Zhu

    2014-12-01

    Full Text Available Fruit leathers (FLs production produces some not-to-specification material, which contains valuable ingredients like fruit pulp, sugars and acidulates. Recovery of FL for product recycling requires decolorization. In earlier research, we proved the efficiency of an ozone-based decolorization process; however, it produces carbonyls as major byproducts, which could be of concern. A headspace solid-phase microextraction with on-fiber derivatization followed by gas chromatography-mass spectrometry was developed for 10 carbonyls analysis in ozonated FL solution/suspension. Effects of dopant concentration, derivatization temperature and time were studied. The adapted method was used to analyze ozonated FL solution/suspension samples. Dopant concentration and derivatization temperature were optimized to 17 mg/mL and 60 °C, respectively. Competitive extraction was studied, and 5 s extraction time was used to avoid non-linear derivatization of 2-furfural. The detection limits (LODs for target carbonyls ranged from 0.016 and 0.030 µg/L. A much lower LOD (0.016 ppb for 2-furfural was achieved compared with 6 and 35 ppb in previous studies. Analysis results confirmed the robustness of the adapted method for quantification of carbonyls in recycled process water treated with ozone-based decolorization. Ethanal, hexanal, 2-furfural, and benzaldehyde were identified as byproducts of known toxicity but all found below levels for concern.

  4. The investigation of exposure to benzene, toluene, ethylbenzene and xylene (BTEX with Solid Phase Microextr action Method in gas station in Yazd province

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    Mohammad Hossein Mosaddegh Mehrjerdi

    2014-01-01

    Full Text Available Abstract Background: Benzene, toluene, ethylbenzene and xylene (BTEX are volatile organic compounds which their physical and chemical characteristics are similar. Evaporation of BTEX from gasoline in petrol station into the air causes gasoline station attendants expose to them. A new extraction method of volatile organic compounds is solid phase microextraction (SPME. The aim of this study is to optimize extraction conditions of BTEX from air samples and then determination of gasoline station air contamination with BTEX in Yazd. Material and Methods: In this study air samples were collected using Tedlar bags and then extracted and analyzed with SPME fiber and gas chromatography equipped with a flame ionization detector. Results: Our results indicate that PDMS/CAR has the best peak area in comparison with two other fibers The Optimized extraction and desorption times are estimated 3 and 1 minutes, respectively Mean concentration of benzene, toluene, ethyl benzene and xylene in gas station’s air were 1932±807, 667±405, 148±89, 340±216 µg/m3 respectively. Conclusion: Benzene mean concentration is above threshold limit value (0.5PPM. Whereas, toluene, ethylbenzene and xylene mean concentration are lower than threshold limit values.

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

    Science.gov (United States)

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

    2018-01-01

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

  6. Phytoscreening with SPME: Variability Analysis.

    Science.gov (United States)

    Limmer, Matt A; Burken, Joel G

    2015-01-01

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

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

    Science.gov (United States)

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

    2016-01-01

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

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

    International Nuclear Information System (INIS)

    Zuraidah Abdullah Munir; Norashikin Saim; Nurul Huda Mamat Ghani

    2008-01-01

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

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

    International Nuclear Information System (INIS)

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

    2013-01-01

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

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

    Science.gov (United States)

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

    2009-05-15

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

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

    OpenAIRE

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

    2010-01-01

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

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

    International Nuclear Information System (INIS)

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

    2009-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Sybille Merkle

    2015-06-01

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

  14. SPME GC/MS determination of organochlorine pesticides in water samples

    Directory of Open Access Journals (Sweden)

    Yerbolat Sailaukhanuly

    2013-05-01

    Full Text Available Headspace solid phase microextraction (HS-SPME in combination with gas chromatography and mass-spectrometry (GC/MS was studied for analysis of water samples. The organochlorine pesticides (OCPs, p,p'-DDT, p,p'-DDD, and p,p'-DDE were collected and analyzed by GC/MS. To select of effective fiber coatings four types of SPME fibers were examined and compared. The parameters effecting the efficiency of HS-SPME such as extraction and pre-incubation time and extraction temperature, effect of solvent nature, ionic strength were studied to obtain optimal parameters. The method was developed using spiked water samples in a concentration range  10 - 500 ng/L. The calibration curve was linear over the studied concentration range with r≥0.9925. The detection limits varied from 1.57 to 2.08 ng/L. An authentic water samples from contaminated lake with OCPs were analyzed by developed method.

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

    International Nuclear Information System (INIS)

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

    1995-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Rada Đurović

    2011-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Esmeraldo A. Cappelaro

    2015-03-01

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

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

    Directory of Open Access Journals (Sweden)

    Filipe Arantes Furtado

    2010-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Trine Bundgaard Andersen

    2015-06-01

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

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

    International Nuclear Information System (INIS)

    Zielińska, Katarzyna; Leeuwen, Herman P. van

    2014-01-01

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

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

    Science.gov (United States)

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

    2008-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Li, Bo; Shi, Yu-e; Cui, Jingcheng; Liu, Zhen; Zhang, Xiaoli; Zhan, Jinhua, E-mail: jhzhan@sdu.edu.cn

    2016-06-07

    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. - Graphical abstract: Au-coated ZnO NRs on stainless steel fiber were used as SERS-active SPME fiber with good extraction effect, high SERS sensitivity. Self-cleaning function of the fiber was achieved based on the photocatalytic degradation property of ZnO nanorods by UV irradiation. - Highlights: • Au-coated ZnO nanorods on stainless steel fiber as a SERS-active SPME fiber was fabricated. • The SERS-active SPME fiber can directly extract and detect the crystal violet and malachite green. • The SERS-active SPME fiber owns good extraction effect, and high SERS sensitivity. • Self-cleaning property of the fiber were achieved based on the photocatalytic degradation property of ZnO.

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

    International Nuclear Information System (INIS)

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

    2016-01-01

    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. - Graphical abstract: Au-coated ZnO NRs on stainless steel fiber were used as SERS-active SPME fiber with good extraction effect, high SERS sensitivity. Self-cleaning function of the fiber was achieved based on the photocatalytic degradation property of ZnO nanorods by UV irradiation. - Highlights: • Au-coated ZnO nanorods on stainless steel fiber as a SERS-active SPME fiber was fabricated. • The SERS-active SPME fiber can directly extract and detect the crystal violet and malachite green. • The SERS-active SPME fiber owns good extraction effect, and high SERS sensitivity. • Self-cleaning property of the fiber were achieved based on the photocatalytic degradation property of ZnO.

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

    Science.gov (United States)

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

    2018-02-12

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

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

    International Nuclear Information System (INIS)

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

    2010-01-01

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

  6. Fiber

    Science.gov (United States)

    ... meals instead of white rice. Add beans (kidney, black, navy, and pinto) to rice dishes for even more fiber. Spice up salads with berries and almonds, chickpeas, cooked artichokes, and beans (kidney, black, navy, or pinto). Use whole-grain (corn or ...

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

    Science.gov (United States)

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

    2016-09-07

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

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

    Directory of Open Access Journals (Sweden)

    Nassiba Baimatova

    2017-07-01

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

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

    OpenAIRE

    Korba, Korcan; Pelit, Levent; Okçu Pelit, Füsun; Özdokur, K. Volkan; Ertaş, Hasan; Eroğlu, Ahmet E.; Ertaş, Fatma Nil

    2013-01-01

    A robust in house solid-phase micro extraction (SPME) surface has been developed for the headspace (HS)-SPME determination of endocrine disruptor pesticides, namely, Chlorpyrifos, Penconazole, Procymidone, Bromopropylate and Lambda-Cyhalothrin in wine sample by using sodium dodecylsulfate doped polypyrrole SPME fiber. Pyrrole monomer was electrochemically polymerized on a stainless steel wire in laboratory conditions in virtue of diminishing the cost and enhancing the analyte retention on its...

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

    Science.gov (United States)

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

    2016-07-01

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

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

    Directory of Open Access Journals (Sweden)

    Pini Gláucia F.

    2004-01-01

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

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

    Science.gov (United States)

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

    2015-12-09

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

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

    International Nuclear Information System (INIS)

    Zhang Zhuomin; Wang Qingtang; Li Gongke

    2012-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Zhang Zhuomin [School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangzhou 510275 (China); Wang Qingtang [Key Laboratory of Analysis and Detection for Food Safety of Ministry of Education, College of Chemistry and Chemical Engineering, Fuzhou University, Fuzhou, Fujian 350002 (China); Li Gongke, E-mail: cesgkl@mail.sysu.edu.cn [School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangzhou 510275 (China)

    2012-05-21

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

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

    Science.gov (United States)

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

    2017-10-01

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

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

    Science.gov (United States)

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

    2005-01-01

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

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

    Science.gov (United States)

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

    2012-01-21

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

  18. Further research on the photo-SPME of triclosan

    Energy Technology Data Exchange (ETDEWEB)

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

    2006-04-15

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

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

    NARCIS (Netherlands)

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

    2013-01-01

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

  20. Headspace solid-phase microextraction (HS-SPME) combined with GC-MS as a process analytical technology (PAT) tool for monitoring the cultivation of C. tetani.

    Science.gov (United States)

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

    2018-04-15

    Vaccine production is a biological process in which variation in time and output is inevitable. Thus, the application of Process Analytical Technologies (PAT) will be important in this regard. Headspace solid - phase microextraction (HS-SPME) coupled with GC-MS can be used as a PAT for process monitoring. This method is suitable to chemical profiling of volatile organic compounds (VOCs) emitted from microorganisms. Tetanus is a lethal disease caused by Clostridium tetani (C. tetani) bacterium and vaccination is an ultimate way to prevent this disease. In this paper, SPME fiber was used for the investigation of VOCs emerging from C. tetani during cultivation. Different types of VOCs such as sulfur-containing compounds were identified and some of them were selected as biomarkers for bioreactor monitoring during vaccine production. In the second step, the portable dynamic air sampling (PDAS) device was used as an interface for sampling VOCs by SPME fibers. The sampling procedure was optimized by face-centered central composite design (FC-CCD). The optimized sampling time and inlet gas flow rates were 10 min and 2 m L s -1 , respectively. PDAS was mounted in exhausted gas line of bioreactor and 42 samples of VOCs were prepared by SPME fibers in 7 days during incubation. Simultaneously, pH and optical density (OD) were evaluated to cultivation process which showed good correlations with the identified VOCs (>80%). This method could be used for VOCs sampling from off-gas of a bioreactor to monitoring of the cultivation process. Copyright © 2018. Published by Elsevier B.V.

  1. Comparative Analyses of the Volatile Components of Citrus Aurantium L. Flowers Using Ultrasonic-Assisted Headspace SPME and Hydrodistillation Combined with GC-MS and Evaluation of their Antimicrobial Activities

    Directory of Open Access Journals (Sweden)

    Akram Rahimi

    2014-12-01

    Full Text Available The volatile components of Citrus aurantium L. flowers were characterized by GC-MS with two different extraction techniques, hydrodistillation (HD and ultrasonic-assisted headspace solid phase microextraction (UA-HS-SPME. In the SPME method, the volatile components of the samples, irradiated by ultrasonic radiation, were collected on a polydimethyl siloxane (PDMS commercial fiber as well as some manually prepared nanoporous fibers from the samples headspace. To reach the better results, the extraction conditions were carefully optimized for the PDMS fiber. Under the optimized conditions (i.e. sonication time 15 min, extraction time 30 min and extraction temperature 55 ºC, 54 compounds were identified by the UA-HS-SPME-GC/MS method. The essential oil components of Citrus aurantium L. flower samples from two different regions of Iran and new and old samples from the same region were compared to one another. The major components identified for the samples with both the SPME and HD methods were linalool, linalyl acetate, limonene, β-myrcene, geranyl acetate, and neryl acetate, respectively. However, a substantial variation in the percentages of the components was identified for different samples and different extraction methods. The antimicrobial activities of the oil were also examined against six standard bacteria. There was some activity against Enterococcus fecalis, Escherichia coli, and Bacillus cereus, indicating important biological activities of the oil.

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

  3. Cobalt oxide nanoparticles as a novel high-efficiency fiber coating for solid phase microextraction of benzene, toluene, ethylbenzene and xylene from aqueous solutions

    International Nuclear Information System (INIS)

    Gholivand, Mohammad Bagher; Shamsipur, Mojtaba; Shamizadeh, Mohammad; Moradian, Rostam; Astinchap, Bandar

    2014-01-01

    Highlights: • Co 3 O 4 nanoparticles were introduced as a novel SPME fiber coating. • The fiber was evaluated for the extraction of BTEX in combination with GC–MS. • The fiber showed extraction efficiencies better than a PDMS fiber toward BTEX. • The fiber was successfully applied to the determination of BTEX in real samples. - Abstract: In this work cobalt oxide nanoparticles were introduced for preparation of a novel solid phase microextraction (SPME) fiber coating. Chemical bath deposition (CBD) technique was used in order for synthesis and immobilization of the Co 3 O 4 nanomaterials on a Pt wire for fabrication of SPME fiber. The prepared cobalt oxide coating was characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD) analysis. The fiber was evaluated for the extraction of benzene, toluene, ethylbenzene and xylene (BTEX) in combination with GC–MS. A simplex optimization method was used to optimize the factors affecting the extraction efficiency. Under optimized conditions, the proposed fiber showed extraction efficiencies comparable to those of a commercial polydimethylsiloxane (PDMS) fiber toward the BTEX compounds. The repeatability of the fiber and its reproducibility, expressed as relative standard deviation (RSD), were lower than about 11%. No significant change was observed in the extraction efficiency of the new SPME fiber after over 50 extractions. The fiber was successfully applied to the determination of BTEX compounds in real samples. The proposed nanostructure cobalt oxide fiber is a promising alternative to the commercial fibers as it is robust, inexpensive and easily prepared

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

    Directory of Open Access Journals (Sweden)

    Don-Roger Parkinson

    2016-02-01

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

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

    Science.gov (United States)

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

    2018-07-01

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

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

    Science.gov (United States)

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

    2016-01-01

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

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

    Science.gov (United States)

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

    2018-03-01

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

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

    Science.gov (United States)

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

    2018-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Yan-Qin Yang

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2005-12-01

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

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

    International Nuclear Information System (INIS)

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

    2013-01-01

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

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

    International Nuclear Information System (INIS)

    Arantes Furtado, Filipe; Vieira Coelho, Gerson Luiz

    2012-01-01

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

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

    International Nuclear Information System (INIS)

    Lee, I-S.; Tsai, S.-W.

    2008-01-01

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

  14. Monolithic graphene fibers for solid-phase microextraction.

    Science.gov (United States)

    Fan, Jing; Dong, Zelin; Qi, Meiling; Fu, Ruonong; Qu, Liangti

    2013-12-13

    Monolithic graphene fibers for solid-phase microextraction (SPME) were fabricated through a dimensionally confined hydrothermal strategy and their extraction performance was evaluated. For the fiber fabrication, a glass pipeline was innovatively used as a hydrothermal reactor instead of a Teflon-lined autoclave. Compared with conventional methods for SPME fibers, the proposed strategy can fabricate a uniform graphene fiber as long as several meters or more at a time. Coupled to capillary gas chromatography (GC), the monolithic graphene fibers in a direct-immersion (DI) mode achieved higher extraction efficiencies for aromatics than those for n-alkanes, especially for polycyclic aromatic hydrocarbons (PAHs), thanks to π-π stacking interaction and hydrophobic effect. Additionally, the fibers exhibited excellent durability and can be repetitively used more than 160 times without significant loss of extraction performance. As a result, an optimum extraction condition of 40°C for 50min with 20% NaCl (w/w) was finally used for SPME of PAHs in aqueous samples. For the determination of PAHs in water samples, the proposed DI-SPME-GC method exhibited linear range of 0.05-200μg/L, limits of detection (LOD) of 4.0-50ng/L, relative standard deviation (RSD) less than 9.4% and 12.1% for one fiber and different fibers, respectively, and recoveries of 78.9-115.9%. The proposed method can be used for analysis of PAHs in environmental water samples. Copyright © 2013 Elsevier B.V. All rights reserved.

  15. Nuevos desarrollos metodológicos en SPME

    OpenAIRE

    Ríos Acevedo, John Jairo

    2016-01-01

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

  16. Determination of 17 kinds of banned organochlorine pesticides in water by activated carbon fiber-solid phase microextraction coupled with GC-MS.

    Science.gov (United States)

    Sun, Tonghua; Jia, Jinping; Zhong, Dengjie; Wang, Yalin

    2006-02-01

    Activated carbon fiber (ACF) as extraction fiber for solid-phase microextraction (SPME) and its application for the analysis of banned organochlorine pesticides (OCPs) were investigated. Firstly, ACF was activated by different concentration of zinc chloride, which indicated that ACF activated by 60% zinc chloride had a reasonable specific surface area, pore volume and pore distribution. Secondly, the parameters for the ACF-SPME procedure, the adsorption and desorption conditions, were also optimized when coupled with gas chromatography-mass spectrometry (GC-MS). Thirdly, the ACF-SPME was used to analyze 17 kinds of OCPs in water. The linearity of most pesticides was found to be between 0.2 and 50 microg/l with GC-MS under the selected ion monitoring (SIM) acquisition mode. The limits of detection (LOD) at the sub microg/l were obtained. The work demonstrated here shows that ACF is a promising alternative for the SPME procedure.

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

    Science.gov (United States)

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

    2012-11-15

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

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

    Science.gov (United States)

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

    2016-12-15

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

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

    OpenAIRE

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

    2016-01-01

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

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

    International Nuclear Information System (INIS)

    Siti Munirah Abd Wahib; Mohd Marsin Sanagi

    2016-01-01

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

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

    Science.gov (United States)

    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. Copyright © 2010 Elsevier B.V. All rights reserved.

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

    International Nuclear Information System (INIS)

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

    2010-01-01

    A new polyethylene glycol fiber was developed for solid-phase microextraction (SPME) of styrene by electrodepositing porous Zn film on Ag wire substrate followed by coating with polyethylene glycol sol-gel (Ag/Zn/PEG sol-gel fiber). The scanning electron micrographs of fibers surface revealed a highly porous structure. The extraction property of the developed fiber-to-styrene residue from polystyrene packaged food was investigated by headspace solid-phase microextraction (HS-SPME) and analyzed with a gas chromatograph coupled with flame ionization detection (GC-FID). The new Ag/Zn/PEG sol-gel fiber is simple to prepare, low cost, robust, has high thermal stability and long lifetime, up to 359 extractions. Repeatability of one fiber (n = 6) was in the range of 4.7-7.5% and fiber-to-fiber reproducibility (n = 4) for five concentration values were in the range 3.4-10%. This Ag/Zn/PEG sol-gel fiber was compared to two commercial SPME fibers, 75 μm carboxen/polydimethylsiloxane (CAR/PDMS) and 100 μm polydimethylsiloxane (PDMS). Under their optimum conditions, Ag/Zn/PEG sol-gel fiber showed the highest sensitivity and the lowest detection limit at 0.28 ± 0.01 ng mL -1 .

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

    Science.gov (United States)

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

    2011-03-01

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

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

    Directory of Open Access Journals (Sweden)

    Elisa Robotti

    2017-01-01

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

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

    Science.gov (United States)

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

    2018-01-18

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

  6. Cobalt oxide nanoparticles as a novel high-efficiency fiber coating for solid phase microextraction of benzene, toluene, ethylbenzene and xylene from aqueous solutions

    Energy Technology Data Exchange (ETDEWEB)

    Gholivand, Mohammad Bagher, E-mail: MB.Gholivand@yahoo.com [Department of Analytical Chemistry, Faculty of Chemistry, Razi University, Kermanshah (Iran, Islamic Republic of); Shamsipur, Mojtaba; Shamizadeh, Mohammad [Department of Analytical Chemistry, Faculty of Chemistry, Razi University, Kermanshah (Iran, Islamic Republic of); Moradian, Rostam; Astinchap, Bandar [Physics Department, Faculty of Science, Razi University, Kermanshah (Iran, Islamic Republic of); Nano Technology Research Laboratory, Razi University, Kermanshah (Iran, Islamic Republic of)

    2014-04-01

    Highlights: • Co{sub 3}O{sub 4} nanoparticles were introduced as a novel SPME fiber coating. • The fiber was evaluated for the extraction of BTEX in combination with GC–MS. • The fiber showed extraction efficiencies better than a PDMS fiber toward BTEX. • The fiber was successfully applied to the determination of BTEX in real samples. - Abstract: In this work cobalt oxide nanoparticles were introduced for preparation of a novel solid phase microextraction (SPME) fiber coating. Chemical bath deposition (CBD) technique was used in order for synthesis and immobilization of the Co{sub 3}O{sub 4} nanomaterials on a Pt wire for fabrication of SPME fiber. The prepared cobalt oxide coating was characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD) analysis. The fiber was evaluated for the extraction of benzene, toluene, ethylbenzene and xylene (BTEX) in combination with GC–MS. A simplex optimization method was used to optimize the factors affecting the extraction efficiency. Under optimized conditions, the proposed fiber showed extraction efficiencies comparable to those of a commercial polydimethylsiloxane (PDMS) fiber toward the BTEX compounds. The repeatability of the fiber and its reproducibility, expressed as relative standard deviation (RSD), were lower than about 11%. No significant change was observed in the extraction efficiency of the new SPME fiber after over 50 extractions. The fiber was successfully applied to the determination of BTEX compounds in real samples. The proposed nanostructure cobalt oxide fiber is a promising alternative to the commercial fibers as it is robust, inexpensive and easily prepared.

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

    Energy Technology Data Exchange (ETDEWEB)

    Steven Hawthorne

    2009-02-15

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

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

    Science.gov (United States)

    Kaykhaii, Massoud; Linford, Matthew R

    2017-03-04

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

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

    Directory of Open Access Journals (Sweden)

    Gülin Renda

    2016-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Shakeel-u- Rehman

    2017-05-01

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

  11. HS-SPME optimization and extraction of volatile compounds from soursop (Annona muricata L. pulp with emphasis on their characteristic impact compounds

    Directory of Open Access Journals (Sweden)

    Karen Leticia de SANTANA

    Full Text Available Abstract Aroma and taste are decisive factors in the selection of any food. The aim of this study was to extract the volatile compounds present in soursop (Annona muricata L. pulp by Solid-phase microextraction (SPME technique using 3 different fibers (DVB/CAR/ PDMS, CAR/PDMS and PDMS/DVB. An experimental design was set up to evaluate the best extraction conditions wherein the variables were adsorption temperature, ionic strength and pulp concentration. The separation of volatiles was performed in chromatographic columns of different polarity (polar and non-polar while volatile compounds were identified by analysis in high resolution gas chromatography system coupled with mass spectrometry. The results obtained using 3 different fibers revealed the capture of about 40 compounds. The CAR/PDMS fiber was more efficient for the capture of esters and DVB/CAR/PDMS fiber for terpenes. The optimum conditions for capture of higher number of volatiles for polar column were 45 °C for extraction, 15% of ionic strength and 50% of pulp concentration which resulted in separation of 87 compounds. Among the principal character impact compounds from soursop are (E-2-hexenoate, methyl hexenoate and linalool.

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

    DEFF Research Database (Denmark)

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

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

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

    DEFF Research Database (Denmark)

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

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

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

    Directory of Open Access Journals (Sweden)

    Liao Hsuan-Yu

    2016-01-01

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

  15. Poly(Dimethylsiloxane)-Poly(Vinyl Alcohol) Coated Solid Phase Micro extraction Fiber for Chloropyrifos Analysis

    International Nuclear Information System (INIS)

    Wan Aini Wan Ibrahim; Nor Fairul Zukry Ahmad Rasdy; Norfazilah Muhamad

    2016-01-01

    Traditional liquid - liquid extraction of pesticides consumes large volumes of organic solvent which are hazardous to the operator and is not environment friendly. Solid phase micro extraction (SPME) is a solvent less extraction method which is safer to the operator and is environmental friendly. A sol-gel hybrid fibre coating material, poly(dimethylsiloxane)-poly(vinyl alcohol) (PDMS-PVA) was synthesized and used in head space solid phase micro extraction (HS-SPME) of chloropyrifos. The thickness of the synthesised PDMS-PVA fiber coating was 13.5 μm and it is thermally stable up to 400 degree Celsius. The PDMS-PVA sol-gel hybrid fiber was also stable to two organic solvents tested; acetonitrile and dichloromethane (1 hour dipping) and showed no significant changes in extraction performance for chloropyrifos. Extracted chloropyrifos was analysed using gas chromatography electron capture detector (GC-ECD). Optimum SPME parameters affecting the PDMS-PVA HS-SPME performance namely extraction time (15 min), extraction temperature (50 degree Celsius), desorption time (5 min), desorption temperature (260 degree Celsius) and stirring rate (120 rpm) were used for extraction. It was found that HSSPME using PDMS-PVA sol-gel fiber gave significantly better extraction performance of chloropyrifos compared to commercial 100 μm PDMS fiber. The PDMS-PVA fiber showed excellent operational performances such as temperature stability (up to 380 degree Celsius), coating lifetime (up to 170 times use) and organic solvent stability. The PDMS-PVA-HS-SPME method showed excellent recovery for chloropyrifos from tomatoes (98.0 %, 5.9 % RSD) at 0.01 μg/ g spiked level (5 times lower than maximum residue limit set by European Union). (author)

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

    Directory of Open Access Journals (Sweden)

    Fernando Carvalho Silva

    1999-04-01

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

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

    Science.gov (United States)

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

    2017-02-15

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

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

    Science.gov (United States)

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

    2018-02-20

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

  19. Preparation by low-temperature nonthermal plasma of graphite fiber and its characteristics for solid-phase microextraction

    International Nuclear Information System (INIS)

    Luo Fan; Wu Zucheng; Tao Ping; Cong Yanqing

    2009-01-01

    Low-temperature nonthermal plasma has been used to prepare solid-phase microextraction (SPME) fibers with high adsorbability, long-term serviceability, and high reproducibility. Graphite rods serving as fiber precursors were treated by an air plasma discharged at 15.2-15.5 kV for a duration of 8 min. Sampling results revealed that the adsorptive capacity of the homemade fiber was 2.5-34.6 times that of a polyacrylate (PA) fiber for alcohols (methanol, ethanol, isopropyl alcohol, n-butyl alcohol), and about 1.4-1.6 times and 2.5-5.1 times that of an activated carbon fiber (ACF) for alcohols and BTEX (benzene, toluene, ethylbenzene, and xylenes), respectively. It is confirmed from FTIR (Fourier transform infrared spectrophotometer) and SEM (scanning electron microscope) analyses that the improvement in the adsorptive performance attributed to increased surface energy and roughness of the graphite fiber. Using gas chromatography (GC)-flame-ionization detector (FID), the limits of detection (LODs) of the alcohols and BTEX ranged between 0.19 and 3.75 μg L -1 , the linear ranges were between 0.6 and 35619 μg L -1 with good linearity (R 2 = 0.9964-0.9997). It was demonstrated that nonthermal plasma offers a fast and simple method for preparing an efficient graphite SPME fiber, and that SPME using the homemade fiber represents a sensitive and selective extraction method for the analysis of a wide range of organic compounds

  20. Preparation by low-temperature nonthermal plasma of graphite fiber and its characteristics for solid-phase microextraction.

    Science.gov (United States)

    Luo, Fan; Wu, Zucheng; Tao, Ping; Cong, Yanqing

    2009-01-05

    Low-temperature nonthermal plasma has been used to prepare solid-phase microextraction (SPME) fibers with high adsorbability, long-term serviceability, and high reproducibility. Graphite rods serving as fiber precursors were treated by an air plasma discharged at 15.2-15.5 kV for a duration of 8 min. Sampling results revealed that the adsorptive capacity of the homemade fiber was 2.5-34.6 times that of a polyacrylate (PA) fiber for alcohols (methanol, ethanol, isopropyl alcohol, n-butyl alcohol), and about 1.4-1.6 times and 2.5-5.1 times that of an activated carbon fiber (ACF) for alcohols and BTEX (benzene, toluene, ethylbenzene, and xylenes), respectively. It is confirmed from FTIR (Fourier transform infrared spectrophotometer) and SEM (scanning electron microscope) analyses that the improvement in the adsorptive performance attributed to increased surface energy and roughness of the graphite fiber. Using gas chromatography (GC)-flame-ionization detector (FID), the limits of detection (LODs) of the alcohols and BTEX ranged between 0.19 and 3.75 microg L(-1), the linear ranges were between 0.6 and 35,619 microg L(-1) with good linearity (R(2)=0.9964-0.9997). It was demonstrated that nonthermal plasma offers a fast and simple method for preparing an efficient graphite SPME fiber, and that SPME using the homemade fiber represents a sensitive and selective extraction method for the analysis of a wide range of organic compounds.

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

    Science.gov (United States)

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

    2010-11-01

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

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

    NARCIS (Netherlands)

    Leslie, H.A.

    2006-01-01

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

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

    Directory of Open Access Journals (Sweden)

    N. Yassaa

    2010-11-01

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

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

    Science.gov (United States)

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

    2016-08-01

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

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

    Science.gov (United States)

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

    2016-02-01

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

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

    NARCIS (Netherlands)

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

    2009-01-01

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

  7. A novel polythiophene – ionic liquid modified clay composite solid phase microextraction fiber: Preparation, characterization and application to pesticide analysis

    International Nuclear Information System (INIS)

    Pelit, Füsun Okçu; Pelit, Levent; Dizdaş, Tuğberk Nail; Aftafa, Can; Ertaş, Hasan; Yalçınkaya, E.E.; Türkmen, Hayati; Ertaş, F.N.

    2015-01-01

    Highlights: • A novel polythiophene – ionic liquid modified clay surface has been prepared. • Polymerization was performed electrochemically on a stainless steel wire. • This material was used as a SPME fiber in head space mode. • This new SPME fiber was applied for analysis of pesticides in juice samples. • Fiber adsorption properties were improved by modification of ionic liquids. - Abstract: This report comprises the novel usage of polythiophene – ionic liquid modified clay surfaces for solid phase microextraction (SPME) fiber production to improve the analysis of pesticides in fruit juice samples. Montmorillonite (Mmt) clay intercalated with ionic liquids (IL) was co-deposited with polythiophene (PTh) polymer coated electrochemically on an SPME fiber. The surface of the fibers were characterized by using scanning electron microscopy (SEM). Operational parameters effecting the extraction efficiency namely; the sample volume and pH, adsorption temperature and time, desorption temperature and time, stirring rate and salt amount were optimized. In order to reveal the major effects, these eight factors were selected and Plackett–Burman Design was constructed. The significant parameters detected; adsorption and temperature along with the stirring rate, were further investigated by Box–Behnken design. Under optimized conditions, calibration graphs were plotted and detection limits were calculated in the range of 0.002–0.667 ng mL −1 . Relative standard deviations were no higher than 18%. Overall results have indicated that this novel PTh-IL-Mmt SPME surface developed by the aid of electrochemical deposition could offer a selective and sensitive head space analysis for the selected pesticide residues

  8. A novel polythiophene – ionic liquid modified clay composite solid phase microextraction fiber: Preparation, characterization and application to pesticide analysis

    Energy Technology Data Exchange (ETDEWEB)

    Pelit, Füsun Okçu, E-mail: fusun.okcu@ege.edu.tr; Pelit, Levent; Dizdaş, Tuğberk Nail; Aftafa, Can; Ertaş, Hasan; Yalçınkaya, E.E.; Türkmen, Hayati; Ertaş, F.N.

    2015-02-15

    Highlights: • A novel polythiophene – ionic liquid modified clay surface has been prepared. • Polymerization was performed electrochemically on a stainless steel wire. • This material was used as a SPME fiber in head space mode. • This new SPME fiber was applied for analysis of pesticides in juice samples. • Fiber adsorption properties were improved by modification of ionic liquids. - Abstract: This report comprises the novel usage of polythiophene – ionic liquid modified clay surfaces for solid phase microextraction (SPME) fiber production to improve the analysis of pesticides in fruit juice samples. Montmorillonite (Mmt) clay intercalated with ionic liquids (IL) was co-deposited with polythiophene (PTh) polymer coated electrochemically on an SPME fiber. The surface of the fibers were characterized by using scanning electron microscopy (SEM). Operational parameters effecting the extraction efficiency namely; the sample volume and pH, adsorption temperature and time, desorption temperature and time, stirring rate and salt amount were optimized. In order to reveal the major effects, these eight factors were selected and Plackett–Burman Design was constructed. The significant parameters detected; adsorption and temperature along with the stirring rate, were further investigated by Box–Behnken design. Under optimized conditions, calibration graphs were plotted and detection limits were calculated in the range of 0.002–0.667 ng mL{sup −1}. Relative standard deviations were no higher than 18%. Overall results have indicated that this novel PTh-IL-Mmt SPME surface developed by the aid of electrochemical deposition could offer a selective and sensitive head space analysis for the selected pesticide residues.

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

    Science.gov (United States)

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

    2016-05-12

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

  10. Sensing dissolved sediment porewater concentrations of persistent and bioaccumulative poolutants using disposable solid-phase microextraction fibers

    NARCIS (Netherlands)

    Mayer, P.; Vaes, W.H.J.; Wijnker, F.; Legierse, K.C.H.M.; Kraaij, R.H.; Tolls, J.; Hermens, J.L.M.

    2000-01-01

    Polymer coated glass fibers were applied as disposable samplers to measure dissolved concentrations of persistent and bioaccumulative pollutants (PBPs) in sediment porewater. The method is called matrix solid-phase microextraction (matrix-SPME), because it utilizes the entire sediment matrix as a

  11. Polypyrrole/hexagonally ordered silica nanocomposite as a novel fiber coating for solid-phase microextraction

    International Nuclear Information System (INIS)

    Gholivand, Mohammad Bagher; Abolghasemi, Mir Mahdi; Fattahpour, Peyman

    2011-01-01

    Highlights: → The polypyrrole/SBA15) nanocomposite was used as a novel coating for SPME fiber. → The proposed fiber was used for the extraction of polycyclic aromatic hydrocarbons. → The proposed SPME fiber is thermal stable, and it has a low limit of detection. → The SPME fiber was applied in polluted river water and wastewater samples. - Abstract: A highly porous fiber coated polypyrrole/hexagonally ordered silica (PPy/SBA15) materials were prepared for solid-phase microextraction (SPME). The PPy/SBA15 nanocomposite was synthesized by an in situ polymerization technique. The resulting material was characterized by the scanning electron microscopy, thermogravimetric analysis and differential thermal analysis. The prepared nanomaterial was immobilized onto a stainless steel wire for fabrication of the SPME fiber. The fiber was evaluated for the extraction of some polycyclic aromatic hydrocarbons (PAHs) from aqueous sample solutions in combination with gas chromatography-mass spectrometry (GC-MS). A one at-the-time optimization strategy was applied for optimizing the important extraction parameters such as extraction temperature, extraction time, ionic strength, stirring rate, desorption time and desorption temperature. In optimum conditions (extraction temperature 70 deg. C, extraction time 20 min, ionic strength 20% (W V -1 ), stirring rate 500 rpm, desorption temperature 270 deg. C, desorption time 5 min) the repeatability for one fiber (n = 3), expressed as relative standard deviation (R.S.D. %), was between 5.0% and 9.3% for the tested compounds. The quantitation limit for the studied compounds were between 13.3 and 66.6 pg mL -1 . The life span and stability of the PPy/SBA15 fiber are good, and it can be used more than 50 times at 260 deg. C without any significant change in sorption properties. The developed method offers the advantage of being simple to use, with shorter analysis times, lower cost of equipment, thermal stability of fiber and high

  12. Evaluation of a new method for chemical coating of aluminum wire with molecularly imprinted polymer layer. Application for the fabrication of triazines selective solid-phase microextraction fiber

    Energy Technology Data Exchange (ETDEWEB)

    Djozan, Djavanshir, E-mail: djozan@tabrizu.ac.ir [Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz (Iran, Islamic Republic of); Ebrahimi, Bahram [Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz (Iran, Islamic Republic of); Mahkam, Mehrdad [Chemistry Department, Azarbaijan University of Tarbiat Moallem, Tabriz (Iran, Islamic Republic of); Farajzadeh, Mir Ali [Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz (Iran, Islamic Republic of)

    2010-07-26

    A new solid-phase microextraction (SPME) fiber is fabricated through ultra violet irradiation polymerization of ametryn-molecularly imprinted polymer on the surface of anodized-silylated aluminum wire. The prepared fiber is durable with very good chemical and thermal stability which can be coupled to GC and GC/MS. The effective parameters on the fabrication and application procedures such as spraying mode, ultra violet irradiation (polymerization) time, number of sprayings and polymerizations, pH and ionic strength of sample and extraction time were optimized. This fiber shows high selectivity with great extraction capacity toward triazines. SPME and GC analysis of ametryn, prometryn, terbutryn, atrazine, simazine, propazine and cyanazine using the fabricated fiber result in the detection limits of 9, 32, 27, 43, 51, 74 and 85 ng mL{sup -1}, respectively. The reliability of the prepared fiber in real samples has been investigated and proved by using spiked tap water, rice, maize and onion samples.

  13. Evaluation of a new method for chemical coating of aluminum wire with molecularly imprinted polymer layer. Application for the fabrication of triazines selective solid-phase microextraction fiber

    International Nuclear Information System (INIS)

    Djozan, Djavanshir; Ebrahimi, Bahram; Mahkam, Mehrdad; Farajzadeh, Mir Ali

    2010-01-01

    A new solid-phase microextraction (SPME) fiber is fabricated through ultra violet irradiation polymerization of ametryn-molecularly imprinted polymer on the surface of anodized-silylated aluminum wire. The prepared fiber is durable with very good chemical and thermal stability which can be coupled to GC and GC/MS. The effective parameters on the fabrication and application procedures such as spraying mode, ultra violet irradiation (polymerization) time, number of sprayings and polymerizations, pH and ionic strength of sample and extraction time were optimized. This fiber shows high selectivity with great extraction capacity toward triazines. SPME and GC analysis of ametryn, prometryn, terbutryn, atrazine, simazine, propazine and cyanazine using the fabricated fiber result in the detection limits of 9, 32, 27, 43, 51, 74 and 85 ng mL -1 , respectively. The reliability of the prepared fiber in real samples has been investigated and proved by using spiked tap water, rice, maize and onion samples.

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

    International Nuclear Information System (INIS)

    Groenewold, Gary S.; Scott, Jill R.; Rae, Catherine

    2011-01-01

    Graphical abstract: Highlights: → A field vacuum extractor (FVE) nondestructively samples surface-adsorbed organics. → The FVE creates a modest vacuum over the surface, volatilizing surface organics. → A solid phase microextraction fiber (SPME) collects volatilized organics. → The SPME is easily analyzed using GC/MS. → The FVE enables collection chemical signatures from hard-to-sample surfaces. - Abstract: Recovery of chemical contaminants from fixed surfaces for analysis can be challenging, particularly if it is not possible to acquire a solid sample to be taken to the laboratory. A simple device is described that collects semi-volatile organic compounds from fixed surfaces by creating an enclosed volume over the surface, then generating a modest vacuum. A solid-phase microextraction (SPME) fiber is then inserted into the evacuated volume where it functions to sorb volatilized organic contaminants. The device is based on a syringe modified with a seal that is used to create the vacuum, with a perforable plunger through which the SPME fiber is inserted. The reduced pressure speeds partitioning of the semi-volatile compounds into the gas phase and reduces the boundary layer around the SPME fiber, which enables a fraction of the volatilized organics to partition into the SPME fiber. After sample collection, the SPME fiber is analyzed using conventional gas chromatography/mass spectrometry. The methodology has been used to collect organophosphorus compounds from glass surfaces, to provide a simple test for the functionality of the devices. Thirty minute sampling times (ΔT vac ) resulted in fractional recovery efficiencies that ranged from 10 -3 to >10 -2 , and in absolute terms, collection of low nanograms was demonstrated. Fractional recovery values were positively correlated to the vapor pressure of the compounds being sampled. Fractional recovery also increased with increasing ΔT vac and displayed a roughly logarithmic profile, indicating that an

  15. Amine-functionalized MIL-53(Al)-coated stainless steel fiber for efficient solid-phase microextraction of synthetic musks and organochlorine pesticides in water samples.

    Science.gov (United States)

    Xie, Lijun; Liu, Shuqin; Han, Zhubing; Jiang, Ruifen; Zhu, Fang; Xu, Weiqin; Su, Chengyong; Ouyang, Gangfeng

    2017-09-01

    The fiber coating is the key part of the solid-phase microextraction (SPME) technique, and it determines the sensitivity, selectivity, and repeatability of the analytical method. In this work, amine (NH 2 )-functionalized material of Institute Lavoisier (MIL)-53(Al) nanoparticles were successfully synthesized, characterized, and applied as the SPME fiber coating for efficient sample pretreatment owing to their unique structures and excellent adsorption properties. Under optimized conditions, the NH 2 -MIL-53(Al)-coated fiber showed good precision, low limits of detection (LODs) [0.025-0.83 ng L -1 for synthetic musks (SMs) and 0.051-0.97 ng L -1 for organochlorine pesticides (OCPs)], and good linearity. Experimental results showed that the NH 2 -MIL-53(Al) SPME coating was solvent resistant and thermostable. In addition, the extraction efficiencies of the NH 2 -MIL-53(Al) coating for SMs and OCPs were higher than those of commercially available SPME fiber coatings such as polydimethylsiloxane, polydimethylsiloxane-divinylbenzene, and polyacrylate. The reasons may be that the analytes are adsorbed on NH 2 -MIL-53(Al) primarily through π-π interactions, electron donor-electron acceptor interactions, and hydrogen bonds between the analytes and organic linkers of the material. Direct immersion (DI) SPME-gas chromatography-mass spectrometry methods based on NH 2 -MIL-53(Al) were successfully applied for the analysis of tap and river water samples. The recoveries were 80.3-115% for SMs and 77.4-117% for OCPs. These results indicate that the NH 2 -MIL-53(Al) coating may be a promising alternative to SPME coatings for the enrichment of SMs and OCPs.

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

    Science.gov (United States)

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

    2018-06-15

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

  17. Electrochemically modified carbon fiber bundles as selective sorbent for online solid-phase microextraction of sulfonamides

    International Nuclear Information System (INIS)

    Ling, Xu; Zhang, Wenpeng; Chen, Zilin

    2016-01-01

    The authors show that carbon fiber bundles electrochemically modified with the conducting polymer poly(3,4-ethylenedioxythiophene) (PEDOT) is a viable sorbent for online solid-phase microextraction (SPME) of the sulfonamides (sulfadiazine, sulfadimidine and sulfamethoxazole) prior to their determination by HPLC. The fibers were packed in a tube loop made from polyether ether ketone (PEEK) that was coupled to the HPLC system for online SPME. Preconcentration factors can reach values of up to 300, and the limit of detection (at an S/N ration of 3) can be as low as 0.05 ng⋅mL −1 . The method was applied to the analysis of the sulfonamides in spiked rat plasma with intra-day and inter-day RSDs of <3.33 and <4.57 %, and with recoveries in the range from 91.7 to 97.8 % in spiked plasma. The in-tube SPME was also applied to the determination of the 3 sulfonamides in rat plasma after oral administration (tablet powder) with high sensitivity. In addition to its efficient extraction, the PEEK tube based SPME has chemical and mechanical stability under even harsh conditions. (author)

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

    Science.gov (United States)

    Liu, Changjiao; Li, Yu

    2017-04-01

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

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

    Directory of Open Access Journals (Sweden)

    Michael H. Tunick

    2013-11-01

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

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

    Science.gov (United States)

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

    2017-06-01

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

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

    OpenAIRE

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

    2015-01-01

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

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

    Directory of Open Access Journals (Sweden)

    H. Heidari

    2009-08-01

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

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

    OpenAIRE

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

    2016-01-01

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

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

    Science.gov (United States)

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

    2016-10-25

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

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

    Science.gov (United States)

    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. Copyright

  6. In situ fabrication of nanostructured titania coating on the surface of titanium wire: A new approach for preparation of solid-phase microextraction fiber

    International Nuclear Information System (INIS)

    Cao Dandan; Lue Jianxia; Liu Jingfu; Jiang Guibin

    2008-01-01

    Nanostructured titania-based solid-phase microextraction (SPME) fibers were fabricated through the in situ oxidation of titanium wires with H 2 O 2 (30%, w/w) at 80 deg. C for 24 h. The obtained SPME fibers possess a ∼1.2 μm thick nanostructured coating consisting of ∼100 nm titania walls and 100-200 nm pores. The use of these fibers for headspace SPME coupled with gas chromatography with electron capture detection (GC-ECD) resulted in improved analysis of dichlorodiphenyltrichloroethane (DDT) and its degradation products. The presented method to detect DDT and its degradation products has high sensitivity (0.20-0.98 ng L -1 ), high precision (relative standard deviation R.S.D. = 9.4-16%, n = 5), a wide linear range (5-5000 ng L -1 ), and good linearity (coefficient of estimation R 2 = 0.991-0.998). As the nanostructured titania was in situ formed on the surface of a titanium wire, the coating was uniformly and strongly adhered on the titanium wire. Because of the inherent chemical stability of the titania coating and the mechanical durability of the titanium wire substrate, this new SPME fiber exhibited long life span (over 150 times)

  7. In situ fabrication of nanostructured titania coating on the surface of titanium wire: A new approach for preparation of solid-phase microextraction fiber

    Energy Technology Data Exchange (ETDEWEB)

    Cao Dandan [State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, P.O. Box 2871, Beijing 100085 (China); Environmental Science Division, School of Earth and Space Science, University of Science and Technology of China, Hefei, Anhui Province 230026 (China); Lue Jianxia [State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, P.O. Box 2871, Beijing 100085 (China); Liu Jingfu [State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, P.O. Box 2871, Beijing 100085 (China)], E-mail: jfliu@rcees.ac.cn; Jiang Guibin [State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, P.O. Box 2871, Beijing 100085 (China)

    2008-03-17

    Nanostructured titania-based solid-phase microextraction (SPME) fibers were fabricated through the in situ oxidation of titanium wires with H{sub 2}O{sub 2} (30%, w/w) at 80 deg. C for 24 h. The obtained SPME fibers possess a {approx}1.2 {mu}m thick nanostructured coating consisting of {approx}100 nm titania walls and 100-200 nm pores. The use of these fibers for headspace SPME coupled with gas chromatography with electron capture detection (GC-ECD) resulted in improved analysis of dichlorodiphenyltrichloroethane (DDT) and its degradation products. The presented method to detect DDT and its degradation products has high sensitivity (0.20-0.98 ng L{sup -1}), high precision (relative standard deviation R.S.D. = 9.4-16%, n = 5), a wide linear range (5-5000 ng L{sup -1}), and good linearity (coefficient of estimation R{sup 2} = 0.991-0.998). As the nanostructured titania was in situ formed on the surface of a titanium wire, the coating was uniformly and strongly adhered on the titanium wire. Because of the inherent chemical stability of the titania coating and the mechanical durability of the titanium wire substrate, this new SPME fiber exhibited long life span (over 150 times)

  8. Fiber webs

    Science.gov (United States)

    Roger M. Rowell; James S. Han; Von L. Byrd

    2005-01-01

    Wood fibers can be used to produce a wide variety of low-density three-dimensional webs, mats, and fiber-molded products. Short wood fibers blended with long fibers can be formed into flexible fiber mats, which can be made by physical entanglement, nonwoven needling, or thermoplastic fiber melt matrix technologies. The most common types of flexible mats are carded, air...

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Jie Yu Chen

    2009-08-01

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

  11. Comparative study of the sol-gel based solid phase microextraction fibers in extraction of naphthalene, fluorene, anthracene and phenanthrene from saffron samples extractants

    International Nuclear Information System (INIS)

    Sarafraz-Yazdi, A.; Ghaemi, F.; Amiri, A.

    2012-01-01

    We are introducing a method for the determination of some polycyclic aromatic hydrocarbons in aqueous saffron sample by direct immersion solid phase microextraction (SPME) and gas chromatography. A sol-gel technique is used for the preparation of the SPME fibers. Three kinds of sol-gel coatings on the fibers were tested and compared. They are composed of poly(dimethyl siloxane) (PDMS), poly(ethylene glycol) (PEG), and a poly(ethylene glycol) modified with multi-walled carbon nanotubes (PEG/CNTs). The effects of fiber coating, desorption time, desorption temperature, extraction time, stirring speed and salting effect were optimized. Under the optimal conditions, the detection limits (at S/N = 3) are 7-50, 5-50, and 1-10 pg mL -1 , respectively, for SPME fibers made from PDMS, PEG and PEG/CNTs. The relative standard deviations for one type of fiber are from 2.1% to 9.6% for all fibers (at n = 5), and in the range from 1.9% to 9.8% from batch to batch (for n = 3). (author)

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

    Directory of Open Access Journals (Sweden)

    H Heidari

    2012-05-01

    Full Text Available

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

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

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

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

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

    OpenAIRE

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

    2002-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2001-04-01

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

  15. Photorefractive Fibers

    National Research Council Canada - National Science Library

    Kuzyk, Mark G

    2003-01-01

    ... scope of the project. In addition to our work in optical limiting fibers, spillover results included making fiber-based light-sources, writing holograms in fibers, and developing the theory of the limits of the nonlinear...

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

    Science.gov (United States)

    Huang, Shu Rong; Palmer, Peter T.

    2017-01-01

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

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

    Science.gov (United States)

    Wang, ShuLing; Hu, Sheng; Xu, Hui

    2015-11-05

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

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

    Science.gov (United States)

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

    2015-07-06

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

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

    International Nuclear Information System (INIS)

    Guidotti, M.; Ravaioli, G.

    1999-01-01

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

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

    Science.gov (United States)

    Cao, Jianping; Liu, Ningrui; Zhang, Yinping

    2017-08-15

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

  1. Fiber dielectrophoresis

    International Nuclear Information System (INIS)

    Lipowicz, P.J.; Yeh, H.C.

    1988-01-01

    Dielectrophoresis is the motion of uncharged particles in nonuniform electric fields. We find that the theoretical dielectrophoretic velocity of a conducting fiber in an insulating medium is proportional to the square of the fiber length, and is virtually independent of fiber diameter. This prediction has been verified experimentally. The results point to the development of a fiber length classifier based on dielectrophoresis. (author)

  2. Application of novel activated carbon fiber solid-phase, microextraction to the analysis of chlorinated hydrocarbons in water by gas chromatography-mass spectrometry

    International Nuclear Information System (INIS)

    Sun Tonghua; Jia Jinping; Fang Nenghu; Wang Yalin

    2005-01-01

    This paper presents a study on the performance of activated carbon fiber (ACF) used as extraction fiber for solid-phase microextraction (SPME) and its application for analysis of chlorinated hydrocarbons in water. By means of evaluating scanning electron microscope (SEM) images, specific surface area, pore volume, pore distribution, and properties of adsorption and desorption, the optimal active concentration of phosphoric acid has been determined. Coupled with gas chromatograph-mass spectrometry (GC-MS), ACF-SPME is suitable for determination chlorinated hydrocarbons in water with headspace. Experimental parameters such as adsorption and desorption conditions were studied. The optimized method has an acceptable linearity, good precision, with R.S.D. values <10% for each compound. Compared with commercial fibers, ACF has many advantages such as better resistance to organic solvents, better endurance to high temperature and longer lifetime

  3. Preparation by low-temperature nonthermal plasma of graphite fiber and its characteristics for solid-phase microextraction

    Energy Technology Data Exchange (ETDEWEB)

    Luo Fan [Department of Environmental Engineering, State Key Laboratory of Clean Energy Utilization, Key Laboratory of Polluted Environment Remediation and Ecological Health, MOE, Zhejiang University, Hangzhou 310027 (China); Wu Zucheng [Department of Environmental Engineering, State Key Laboratory of Clean Energy Utilization, Key Laboratory of Polluted Environment Remediation and Ecological Health, MOE, Zhejiang University, Hangzhou 310027 (China)], E-mail: wuzc@zju.edu.cn; Tao Ping [Institute of Structural Mechanics, China Academy of Engineering Physics, Mianyang 621900 (China); Cong Yanqing [College of Environmental Science and Engineering, Zhejiang Gongshang University, Hangzhou 310012 (China)

    2009-01-05

    Low-temperature nonthermal plasma has been used to prepare solid-phase microextraction (SPME) fibers with high adsorbability, long-term serviceability, and high reproducibility. Graphite rods serving as fiber precursors were treated by an air plasma discharged at 15.2-15.5 kV for a duration of 8 min. Sampling results revealed that the adsorptive capacity of the homemade fiber was 2.5-34.6 times that of a polyacrylate (PA) fiber for alcohols (methanol, ethanol, isopropyl alcohol, n-butyl alcohol), and about 1.4-1.6 times and 2.5-5.1 times that of an activated carbon fiber (ACF) for alcohols and BTEX (benzene, toluene, ethylbenzene, and xylenes), respectively. It is confirmed from FTIR (Fourier transform infrared spectrophotometer) and SEM (scanning electron microscope) analyses that the improvement in the adsorptive performance attributed to increased surface energy and roughness of the graphite fiber. Using gas chromatography (GC)-flame-ionization detector (FID), the limits of detection (LODs) of the alcohols and BTEX ranged between 0.19 and 3.75 {mu}g L{sup -1}, the linear ranges were between 0.6 and 35619 {mu}g L{sup -1} with good linearity (R{sup 2} = 0.9964-0.9997). It was demonstrated that nonthermal plasma offers a fast and simple method for preparing an efficient graphite SPME fiber, and that SPME using the homemade fiber represents a sensitive and selective extraction method for the analysis of a wide range of organic compounds.

  4. Fiber Amplifiers

    DEFF Research Database (Denmark)

    Rottwitt, Karsten

    2017-01-01

    The chapter provides a discussion of optical fiber amplifiers and through three sections provides a detailed treatment of three types of optical fiber amplifiers, erbium doped fiber amplifiers (EDFA), Raman amplifiers, and parametric amplifiers. Each section comprises the fundamentals including...... the basic physics and relevant in-depth theoretical modeling, amplifiers characteristics and performance data as a function of specific operation parameters. Typical applications in fiber optic communication systems and the improvement achievable through the use of fiber amplifiers are illustrated....

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

    Science.gov (United States)

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

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

    NARCIS (Netherlands)

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

    2010-01-01

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

  7. A molybdenum disulfide/reduced graphene oxide fiber coating coupled with gas chromatography-mass spectrometry for the saponification-headspace solid-phase microextraction of polychlorinated biphenyls in food.

    Science.gov (United States)

    Lv, Fangying; Gan, Ning; Cao, Yuting; Zhou, You; Zuo, Rongjie; Dong, Youren

    2017-11-24

    In this work, the molybdenum disulfide/reduced graphene oxide (MoS 2 /RGO) composite material was synthesized as a fiber coating to extract seven indicator polychlorinated biphenyls (PCBs; PCB28, PCB52, PCB101, PCB118, PCB138, PCB153, and PCB180) present in food via a saponification-headspace solid-phase microextraction assay (saponification-HS-SPME). The MoS 2 /RGO coating was prepared and deposited on a stainless steel wire with the help of a silicone sealant and used as an SPME fiber. The alkali solution dissolved the fat and helped in releasing the PCBs present in milk to the headspace for extraction under 100°C. Following desorption in the inlet, the targets were quantified by gas chromatography-mass spectrometry. The effects of sorbent dosage, extraction time, added salts, and stirring rate on the extraction efficiency were investigated. The new coating was able to adsorb a higher amount of analytes, which was about 1.1-2.9 times in comparison with the commercially available SPME fiber (coated with divinylbenzene/carboxen/polydimethylsiloxane). It also showed the highest adsorption capability toward PCBs, which was 1.5-2.7 times that of the prepared RGO modified fiber. Moreover, MoS 2 also showed a strong affinity toward PCBs in a manner similar to its affinity for graphene. The developed method is simple and environmentally friendly as it does not require any organic solvents. Furthermore, it exhibits good sensitivity with detection limits less than 0.1ngmL -1 , linearity (0.25-100ngmL -1 ), and reproducibility (relative standard deviation below 10% for n=3). The novel SPME fibers are inexpensive, reusable, and can be easily prepared and manipulated. In addition, the saponification-HS-SPME assay was also found to be suitable for screening persistent organic pollutants in dairy products. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. Simultaneous determination of salicylic, 3-methyl salicylic, 4-methyl salicylic, acetylsalicylic and benzoic acids in fruit, vegetables and derived beverages by SPME-LC-UV/DAD.

    Science.gov (United States)

    Aresta, Antonella; Zambonin, Carlo

    2016-03-20

    Salicylic and benzoic acid are phenolic acids occurring in plant cells, thus they can be present in fruit and vegetables at various levels. They possess anti-inflammatory and antimicrobial properties, however they may induce symptoms and health problems in a small percentage of the population. Therefore, a low phenolic acid diet may be of clinical benefit to such individuals. In order to achieve this goal, the concentration of these substances in different food and beverages should be assessed. The present work describes for the first time a new method, based on solid phase microextraction (polydimethylsiloxane-divinylbenzene fiber) coupled to liquid chromatography with UV diode array detection, for the simultaneous determination of salicylic acid, 3-methyl salicylic acid, 4-methyl salicylic acid, acetylsalicylic acid and benzoic acid in selected fruit, vegetables and beverages. All the aspects influencing fiber adsorption (time, temperature, pH, salt addition) and desorption (desorption and injection time, desorption solvent mixture composition) of the analytes have been investigated. An isocratic separation was performed using an acetonitrile-phosphate buffer (pH 2.8; 2 mM) mixture (70:30, v/v) as the mobile phase. The estimated LOD and LOQ values (μg/mL) were in the range 0.002-0.028 and 0.007-0.095. The within-day and day-to-day precision values (RSD%) were between 4.7-6.1 and 6.6-9.4, respectively. The method has been successfully applied to the analysis of fava beans, blueberries, kiwi, tangerines, lemons, oranges and fruit juice (lemon and blueberry) samples. The major advantage of the method is that it only requires simple homogenization and/or centrifugation and dilution steps prior to SPME and injection in the LC system. Copyright © 2016 Elsevier B.V. All rights reserved.

  9. A comparison of sample preparation methods for extracting volatile organic compounds (VOCs) from equine faeces using HS-SPME.

    Science.gov (United States)

    Hough, Rachael; Archer, Debra; Probert, Christopher

    2018-01-01

    Disturbance to the hindgut microbiota can be detrimental to equine health. Metabolomics provides a robust approach to studying the functional aspect of hindgut microorganisms. Sample preparation is an important step towards achieving optimal results in the later stages of analysis. The preparation of samples is unique depending on the technique employed and the sample matrix to be analysed. Gas chromatography mass spectrometry (GCMS) is one of the most widely used platforms for the study of metabolomics and until now an optimised method has not been developed for equine faeces. To compare a sample preparation method for extracting volatile organic compounds (VOCs) from equine faeces. Volatile organic compounds were determined by headspace solid phase microextraction gas chromatography mass spectrometry (HS-SPME-GCMS). Factors investigated were the mass of equine faeces, type of SPME fibre coating, vial volume and storage conditions. The resultant method was unique to those developed for other species. Aliquots of 1000 or 2000 mg in 10 ml or 20 ml SPME headspace were optimal. From those tested, the extraction of VOCs should ideally be performed using a divinylbenzene-carboxen-polydimethysiloxane (DVB-CAR-PDMS) SPME fibre. Storage of faeces for up to 12 months at - 80 °C shared a greater percentage of VOCs with a fresh sample than the equivalent stored at - 20 °C. An optimised method for extracting VOCs from equine faeces using HS-SPME-GCMS has been developed and will act as a standard to enable comparisons between studies. This work has also highlighted storage conditions as an important factor to consider in experimental design for faecal metabolomics studies.

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

    Science.gov (United States)

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

    2009-05-30

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

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

    Science.gov (United States)

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

    2013-06-15

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

  12. Electrophoretic deposition of graphene oxide onto carbon fibers for in-tube solid-phase microextraction.

    Science.gov (United States)

    Feng, Juanjuan; Wang, Xiuqin; Tian, Yu; Bu, Yanan; Luo, Chuannan; Sun, Min

    2017-09-29

    Carbon fibers (CFs) were functionalized with graphene oxide (GO) by an electrophoretic deposition (EPD) method for in-tube solid-phase microextraction (SPME). GO-CFs were filled into a poly(ether ether ketone) (PEEK) tube to obtain a fibers-in-tube SPME device, which was connected with high performance liquid chromatography (HPLC) equipment to build online SPME-HPLC system. Compared with CFs, GO-CFs presented obviously better extraction performance, due to excellent adsorption property and large surface area of GO. Using ten polycyclic aromatic hydrocarbons (PAHs) as model analytes, the important extraction conditions were optimized, such as sample flow rate, extraction time, organic solvent content and desorption time. An online analysis method was established with wide linear range (0.01-50μgL -1 ) and low detection limits (0.001-0.004μgL -1 ). Good sensitivity resulted from high enrichment factors (1133-3840) of GO-CFs in-tube device towards PAHs. The analysis method was used to online determination of PAHs in wastewater samples. Some target analytes were detected and relative recoveries were in the range of 90.2-112%. It is obvious that the proposed GO-CFs in-tube device was an efficient extraction device, and EPD could be used to develop nanomaterials functionalized sorbents for sample preparation. Copyright © 2017 Elsevier B.V. All rights reserved.

  13. Multiwalled carbon nanotubes coated fibers for solid-phase microextraction of polybrominated diphenyl ethers in water and milk samples before gas chromatography with electron-capture detection.

    Science.gov (United States)

    Wang, Jun-Xia; Jiang, Dong-Qing; Gu, Zhi-Yuan; Yan, Xiu-Ping

    2006-12-22

    Determination of polybrominated diphenyl ethers (PBDEs) in environmental samples has raised great concerns due to the widespread use of PBDEs and their potential risk to humans. Solid-phase microextraction (SPME) is a fast, simple, cost-effective, and green sample preparation technique and is widely used for environmental analysis, but reports on the application of SPME for determination of PBDEs are very limited, and only a few publications dealing with commercial SPME fibers are available for extraction of PBDEs. Herein, we report a novel SPME method using multiwalled carbon nanotubes (MWCNTs) as the SPME fiber coating for gas chromatography with electron-capture detection (GC-ECD) of PBDEs in environmental samples. The MWCNTs coating gave much higher enhancement factors (616-1756) than poly (5% dibenzene-95% dimethylsiloxane) coating (139-384) and activated carbon coating (193-423). Thirty-minute extraction of 10 mL of sample solution using the MWCNTs coated fiber for GC-ECD determination yielded the limits of detection of 3.6-8.6 ng L(-1) and exhibited good linearity of the calibration functions (r(2)>0.995). The precision (RSD%, n=4) for peak area and retention time at the 500 ng L(-1) level was 6.9-8.8% and 0.6-0.9%, respectively. The developed method was successfully applied for the analysis of real samples including local river water, wastewater, and milk samples. The recovery of the PBDEs at 500 ng L(-1) spiked in these samples ranged from 90 to 119%. No PBDEs were detected in the river water and skimmed milk samples, whereas in the wastewater sample, 134-215 ng L(-1) of PBDEs were found. The PBDEs were detected in all whole fat milk samples, ranging from 13 to 484 ng L(-1). In a semiskimmed milk sample, only BDE-47 was found at 21 ng L(-1).

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

    Energy Technology Data Exchange (ETDEWEB)

    Nomngongo, Philiswa N.; Ngila, J. Catherine, E-mail: jcngila@uj.ac.za

    2014-08-01

    This study reports a simple and efficient method for the determination of trace Cd, Cu, Fe, Pb and Zn in diesel and gasoline samples by inductively coupled plasma mass spectrometry after matrix removal and analyte pre-concentration using hollow fiber-solid phase microextraction (HF–SPME). The optimization of HF-SPME procedure was carried out using two-level full factorial and central composite designs. Four factors (variables), that are, sample solution pH, acceptor phase amount, extraction time and eluent concentration were optimized. Under the optimized experimental conditions, the precision was ≤ 3% (C = 10 μg L{sup −1}, n = 15), limits of detection and quantification ranged from 0.1 to 0.3 μg L{sup −1} and 0.3–0.9 μg L{sup −1}, respectively, and the maximum preconcentration factor was 30. The HF-SPME method was applied for the determination of trace metals in real gasoline and diesel samples. - Highlights: • Hollow fiber solid phase microextraction of metal ions in diesel and gasoline • Use of hollow fiber-supported sol–gel combined with cation exchange resin • Optimization of HF-SPME using multivariate techniques • Determination of Cd, Cu, Fe, Pb and Zn using ICP–MS • Relatively low LOD and LOQ.

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

    International Nuclear Information System (INIS)

    Nomngongo, Philiswa N.; Ngila, J. Catherine

    2014-01-01

    This study reports a simple and efficient method for the determination of trace Cd, Cu, Fe, Pb and Zn in diesel and gasoline samples by inductively coupled plasma mass spectrometry after matrix removal and analyte pre-concentration using hollow fiber-solid phase microextraction (HF–SPME). The optimization of HF-SPME procedure was carried out using two-level full factorial and central composite designs. Four factors (variables), that are, sample solution pH, acceptor phase amount, extraction time and eluent concentration were optimized. Under the optimized experimental conditions, the precision was ≤ 3% (C = 10 μg L −1 , n = 15), limits of detection and quantification ranged from 0.1 to 0.3 μg L −1 and 0.3–0.9 μg L −1 , respectively, and the maximum preconcentration factor was 30. The HF-SPME method was applied for the determination of trace metals in real gasoline and diesel samples. - Highlights: • Hollow fiber solid phase microextraction of metal ions in diesel and gasoline • Use of hollow fiber-supported sol–gel combined with cation exchange resin • Optimization of HF-SPME using multivariate techniques • Determination of Cd, Cu, Fe, Pb and Zn using ICP–MS • Relatively low LOD and LOQ

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

    Science.gov (United States)

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

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

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

    Directory of Open Access Journals (Sweden)

    Kenneth G. Furton

    2007-08-01

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

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

    DEFF Research Database (Denmark)

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

    2015-01-01

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

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

    Directory of Open Access Journals (Sweden)

    García, Carmen

    2009-07-01

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

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

    Directory of Open Access Journals (Sweden)

    Lauren E. Musumeci

    2015-07-01

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

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

    Science.gov (United States)

    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).

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

    OpenAIRE

    Kuželová, Kristýna

    2015-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Aiêrta C. C. da Silva

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

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

    Directory of Open Access Journals (Sweden)

    René Arzuffi

    2009-06-01

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

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

    Directory of Open Access Journals (Sweden)

    Batoul Benyelles

    2014-12-01

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

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

    Directory of Open Access Journals (Sweden)

    Kazuki Saito

    2013-04-01

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

  7. Determination of tetrachloroethylene and other volatile halogenated organic compounds in oil wastes by headspace SPME GC-MS

    Energy Technology Data Exchange (ETDEWEB)

    Fabbri, D.; Bezzi, R.; Torri, C.; Galletti, P.; Tagliavini, E. [Bologna Univ., Ravenna (Italy). Lab. of Chemistry, C.I.R.S.A

    2007-09-15

    Oil wastes and slops are complex mixtures of hydrocarbons, which may contain a variety of contaminants including tetrachloroethylene (perchloroethylene, PCE) and other volatile halogenated organic compounds (VHOCs). The analytical determination of PCE at trace levels in petroleum-derived matrices is difficult to carry out in the presence of large amounts of hydrocarbon matrix components. In the following study, we demonstrate that headspace solid-phase microextraction (HS-SPME) combined with GC-MS analysis can be applied for the rapid measurement of PCE concentration in oil samples. The HS-SPME method was developed using liquid paraffin as matrix matching reference material for external and internal calibration and optimisation of experimental parameters. The limit of quantitation was 0.05 mg kg{sup -1}, and linearity was established up to 25 mg kg{sup -1}. The HS-SPME method was extended to several VHOCs, including trichloroethylene (TCE) in different matrices and was applied to the quantitative analysis of PCE and TCE in real samples.

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

    Directory of Open Access Journals (Sweden)

    Mei Song

    2015-04-01

    Full Text Available 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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2006-08-15

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

  10. SPME-GC-MS analysis of commercial henna samples (Lawsonia inermis L.).

    Science.gov (United States)

    Mengoni, Tamara; Peregrina, Dolores Vargas; Censi, Roberta; Cortese, Manuela; Ricciutelli, Massimo; Maggi, Filippo; Di Martino, Piera

    2016-01-01

    The aim of this work was to provide a characterisation of volatile constituents from different commercial batches of henna (Lawsonia inermis) leaves of different geographic origin. Headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC-MS) was used for the purpose. A total of 72 components were identified by GC-MS in the headspace of different henna samples which proved to differ considerably from each other, because they were characterised by different classes of components, mainly aliphatic compounds (9.0-64.7%), terpenoids (5.8-45.5%) and aromatics (7.9-45.2%), with alkanes (0.9-18.5%), aldehydes (2.1-18.8%) and carboxylic acids (3.1-29.3%), monoterpenes (3.4-30.0%) and sesquiterpenes (0.8-23.7%) and phenyl propanoids (0.6-43.1%), being the most abundant, respectively. Major representatives of these groups were n-hexadecane (0.5-4.7%), (2E)-hexenal (0.5-11.7%) and acetic acid (2.8-24.5%), limonene (0.8-14.7%), carvol (3.8-7.1%), geranyl acetone (1.4-7.9%) and (E)-caryophyllene (3.3-8.4%), and (E)-anethole (0.6-35.0%), respectively. We assume that factors such as the manufacturing process, the storage conditions and the different geographic origin of the samples may contribute to such variability.

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

    Directory of Open Access Journals (Sweden)

    Fabrizio Cincotta

    2015-07-01

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

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

    Directory of Open Access Journals (Sweden)

    Zhen Ding

    2014-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Ezequias P. Siqueira

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

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

    Directory of Open Access Journals (Sweden)

    EDUARDO CORPAS IGUARÁN

    2017-07-01

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

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

    Science.gov (United States)

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

    2018-03-01

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

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

    Science.gov (United States)

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

    2016-05-01

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

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

    Science.gov (United States)

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

    2013-11-01

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

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

    Science.gov (United States)

    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. Copyright © 2015 Elsevier B.V. All rights reserved.

  19. Preparation of three-dimensional mesoporous polymer in situ polymerization solid phase microextraction fiber and its application to the determination of seven chlorophenols.

    Science.gov (United States)

    Wang, Xuemei; Wang, Huan; Huang, Pengfei; Ma, Xiaomin; Lu, Xiaoquan; Du, Xinzhen

    2017-01-06

    A superior solid-phase microextraction (SPME) fiber-coating material, three dimensional order mesoporous polymers with Ia-3d bicontinuous cubic structure (3D-OMPs) was in situ coated on a stainless steel wire by solvent evaporation induced self-assembly (EISA) and thermo-polymerization. Fourier-transform infrared spectrometry (FTIR), transmission electron microscopy (TEM), scanning electron microscopy (SEM), small-angel X-ray diffraction (SAXRD), N 2 adsorption-desorption transmission, and thermogravimetry analysis (TGA) were applied to the characterization of the synthesized 3D-OMPs coating. The performance and feasibility of the homemade fiber was evaluated through direct immersion (DI) SPME followed by high-performance liquid chromatography-UV detector (HPLC-UV) for the simultaneous extraction of seven chlorophenols in water samples. Under the optimum conditions, the prepared fiber exhibited excellent extraction properties as compared to three commercial fibers, the DI-SPME-HPLC-UV method showed low limits of detection (0.32-1.85μgL -1 ), wide linear ranges (5.0-1000μgL -1 ), and acceptable reproducibility (relative standard deviation, RSD<7.6% for one fiber, RSD<8.9% for fiber to fiber). Moreover, the method was further successfully applied to the analysis of seven CPs in real samples with good recoveries (80.5-99.5%) and satisfactory precisions (RSD<9.2%). It was confirmed that the proposed method has high sensitivity, outstanding selectivity and good reproducibility to the determination of trace CPs in the environmental water. Copyright © 2016 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

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

    2017-10-23

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

  1. Two Fiber Optical Fiber Thermometry

    Science.gov (United States)

    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.

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

    International Nuclear Information System (INIS)

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

    2016-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-03-24

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

  4. Chemically bonded carbon nanotubes on modified gold substrate as novel unbreakable solid phase microextraction fiber

    International Nuclear Information System (INIS)

    Bagheri, H.; Ayazi, Z.; Sistani, H.

    2011-01-01

    A new technique is introduced for preparation of an unbreakable fiber using gold wire as a substrate for solid phase microextraction (SPME). A gold wire is used as a solid support, onto which a first film is deposited that consists of a two-dimensional polymer obtained by hydrolysis of a self-assembled monolayer of 3-(trimethoxysilyl)-1-propanthiol. This first film is covered with a layer of 3-(triethoxysilyl)-propylamine. Next, a stationary phase of oxidized multi-walled carbon nanotubes was chemically bound to the surface. The synthetic strategy was verified by Fourier transform infrared spectroscopy and scanning electron microscopy. Thermal stability of new fiber was examined by thermogravimetric analysis. The applicability of the novel coating was verified by its employment as a SPME fiber for isolation of diazinon and fenthion, as model compounds. Parameters influencing the extraction process were optimized to result in limits of detection as low as 0.2 ng mL -1 for diazinon, and 0.3 ng mL -1 for fenthion using the time-scheduled selected ion monitoring mode. The method was successfully applied to real water, and the recoveries for spiked samples were 104% for diazinon and 97% for fenthion. (author)

  5. Headspace solid-phase microextraction (HS-SPME) and liquid-liquid extraction (LLE): comparison of the performance in classification of ecstasy tablets. Part 2.

    Science.gov (United States)

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

    2008-11-20

    Headspace solid-phase microextraction (HS-SPME) is assessed as an alternative to liquid-liquid extraction (LLE) currently used for 3,4-methylenedioxymethampethamine (MDMA) profiling. Both methods were compared evaluating their performance in discriminating and classifying samples. For this purpose 62 different seizures were analysed using both extraction techniques followed by gas chromatography-mass spectroscopy (GC-MS). A previously validated method provided data for HS-SPME, whereas LLE data were collected applying a harmonized methodology developed and used in the European project CHAMP. After suitable pre-treatment, similarities between sample pairs were studied using the Pearson correlation. Both methods enable to distinguish between samples coming from the same pre-tabletting batches and samples coming from different pre-tabletting batches. This finding emphasizes the use of HS-SPME as an effective alternative to LLE, with additional advantages such as sample preparation and a solvent-free process.

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

    Science.gov (United States)

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

    2003-11-19

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

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

    DEFF Research Database (Denmark)

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

    2008-01-01

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

  8. 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

    International Nuclear Information System (INIS)

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

    2014-01-01

    Graphical abstract: - Highlights: • A novel SPME fiber based on polypyrrole/montmorillonite nanocomposites with highly porous and thermal stability was prepared. • The two-dimensional separation technique, GC–IMS, was used for analysis of complex matrices extracted by SPME. • Direct and simultaneous analysis of diazinon and fenthion in various real samples was successfully accomplished. - Abstract: 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

  9. 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

    Energy Technology Data Exchange (ETDEWEB)

    Jafari, Mohammad T., E-mail: jafari@cc.iut.ac.ir; Saraji, Mohammad; Sherafatmand, Hossein

    2014-03-01

    Highlights: • A novel SPME fiber based on polypyrrole/montmorillonite nanocomposites with highly porous and thermal stability was prepared. • The two-dimensional separation technique, GC–IMS, was used for analysis of complex matrices extracted by SPME. • Direct and simultaneous analysis of diazinon and fenthion in various real samples was successfully accomplished. Abstract: 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

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

    Directory of Open Access Journals (Sweden)

    Emy Komatsu

    2004-10-01

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

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

    KAUST Repository

    Caupos, Emilie

    2014-10-04

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

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

    International Nuclear Information System (INIS)

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

    2006-01-01

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

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

    Science.gov (United States)

    Giri, Anupam; Zelinkova, Zuzana; Wenzl, Thomas

    2017-12-01

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

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

    Directory of Open Access Journals (Sweden)

    Pascual Serra-Mora

    2018-02-01

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

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

    Science.gov (United States)

    Deng, Chunhui; Song, Guoxin; Hu, Yaoming

    2004-12-01

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

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

    Science.gov (United States)

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

    2012-09-01

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

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-01-27

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

  19. Low-fiber diet

    Science.gov (United States)

    ... residue; Low-fiber diet; Fiber restricted diet; Crohn disease - low fiber diet; Ulcerative colitis - low fiber diet; ... them if they do not contain seeds or pulp: Yellow squash (without seeds) Spinach Pumpkin Eggplant Potatoes, ...

  20. Photovoltaic fibers

    Science.gov (United States)

    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

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

    Science.gov (United States)

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

    2012-01-01

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

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

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

    International Nuclear Information System (INIS)

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

    2006-01-01

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

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

    Science.gov (United States)

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

    2007-01-01

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

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

    International Nuclear Information System (INIS)

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

    2016-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-08-17

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

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

    Science.gov (United States)

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

    2016-01-04

    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. Copyright © 2015 Elsevier B.V. All rights reserved.

  8. Polyoxotungstate nanoclusters supported on silica as an efficient solid-phase microextraction fiber of polycyclic aromatic hydrocarbons

    International Nuclear Information System (INIS)

    Abolghasemi, Mir Mahdi; Yousefi, Vahid; Rafiee, Ezzat

    2014-01-01

    A highly porous silica-supported tungstophosphoric acid (PW) nanocluster was prepared for use in solid-phase microextraction (SPME) of polycyclic aromatic hydrocarbons (PAHs). The PWs represent a class of discrete transition metal-oxide nanoclusters and their structures resemble discrete fragments of metal-oxide structures of definite size and shape. Transition metal-oxide nanoclusters display large structural diversity, and their monodisperse sizes can be tuned from several Ångstroms up to 10 nm. The highly porous silica-supported tungstophosphoric acid nanocluster material is found to be capable of efficiently extracting PAHs from aqueous sample solutions. The nanomaterial was immobilized on a stainless steel wire for fabrication of the SPME fiber. Following thermal desorption, the PAHs were quantified by GC-MS. Analytical merits include limits of detection that range from 0.02 to 0.1 pg mL −1 and a dynamic range as wide as from 0.001 to 100 ng mL −1 . Under optimum conditions, the repeatability for one fiber (n = 3), expressed as the relative standard deviation, is between 4.3 % and 8.6 %. The method is simple, rapid, and inexpensive. The thermal stability of the fiber and the high relative recovery make this method superior to conventional methods of extraction. (author)

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

    Science.gov (United States)

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

    2010-06-23

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

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

    Directory of Open Access Journals (Sweden)

    Jazmín Osorio Monsalve

    2016-11-01

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

  11. A screening method for polycyclic aromatic hydrocarbons determination in water by headspace SPME with GC-FID

    Energy Technology Data Exchange (ETDEWEB)

    Zuazagoitia, D.; Millan, E.; Garcia, R. [Univ. of Pais Vasco, Donostia-San Sebastian (Spain). Dept. of Applied Chemistry

    2007-11-15

    A simple method for determination of polycyclic aromatic hydrocarbons (PAHs) in water using headspace solid-phase microextraction (HS-SPME) with gas chromatography-flame ionisation detector (GC-FID) was developed. In order to obtain the convenient experimental conditions for HS-SPME extraction an experimental design with two steps was accomplished. A 2{sup 6-2} fractional factorial design and central composite design (CCD) considering three significant factors were used. Naphthalene, anthracene and fluoranthene were chosen as representatives of two, three and four aromatic rings, and the global response of three PAHs was used for the results, evaluation. The chosen extraction conditions were: 85 {mu}m polyacrylate fibre; 50 C temperature; 60 min time; 20 mL-dissolution volume (in 40 mL glass vial); without salt addition; and 2 min desorption time. The procedure was extended to other seven PAHs (acenaphthylene, acenaphthene, fluorene, phenanthrene, pyrene, chrysene and benzo(a)anthracene) and the analytical characteristics were checked. The limit of detection (LOD) was from 0.08 (anthracene) to 0.20 {mu}g L{sup -1} (naphthalene). The precision expressed as relative standard deviation (RSD in %) using 50 {mu}g L{sup -1} of each analyte ranged from 6.8 to 17 %. The method was applied to the analysis of the surface waters and leaching waters of contaminated soils from Gipuzkoa (North Spain). The PAHs were not detected in surface water samples. Most of the PAHs were found in the leachates from contaminated soils showing a maximum global value of 75.5 {mu}g L{sup -1}. (orig.)

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

    Science.gov (United States)

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

    2011-01-01

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

  13. Application Specific Optical Fibers

    OpenAIRE

    Pal, Bishnu P.

    2010-01-01

    In this chapter we have attempted to provide a unified summary description of the most important propagation characteristics of an optical fiber followed by discussion on several variety of special fibers for realizing fiber amplifiers, dispersion compensating fibers, microstructured optical fibers, and so on. Even though huge progress has been made on development of optical fibers for telecom application, a need for developing special fibers, not necessarily for telecom alone, has arisen. Th...

  14. 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.

    Science.gov (United States)

    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. Copyright © 2016 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

    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. Copyright © 2016 Elsevier B.V. All rights reserved.

  16. Determination of semi-volatile additives in wines using SPME and GC-MS.

    Science.gov (United States)

    Sagandykova, Gulyaim N; Alimzhanova, Mereke B; Nurzhanova, Yenglik T; Kenessov, Bulat

    2017-04-01

    Parameters of headspace solid-phase microextraction, such as fiber coating (85μm CAR/PDMS), extraction time (2min for white and 3min for red wines), temperature (85°C), pre-incubation time (15min) were optimized for identification and quantification of semi-volatile additives (propylene glycol, sorbic and benzoic acids) in wines. To overcome problems in their determination, an evaporation of the wine matrix was performed. Using the optimized method, screening of 25 wine samples was performed, and the presence of propylene glycol, sorbic and benzoic acids was found in 22, 20 and 6 samples, respectively. Analysis of different wines using a standard addition approach showed good linearity in concentration ranges 0-250, 0-125, and 0-250mg/L for propylene glycol, sorbic and benzoic acids, respectively. The proposed method can be recommended for quality control of wine and disclosing adulterated samples. Copyright © 2016 Elsevier Ltd. All rights reserved.

  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.

    Science.gov (United States)

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

    2014-01-17

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

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

    Science.gov (United States)

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

    2015-08-15

    Furfural (Fu) and hydroxymethylfurfural (HMFu) are extracted using a dodecylbenzenesulfonate-doped polypyrrole coating as a fiber for headspace solid phase microextraction (HS-SPME) method in baby formula samples and detected using ion mobility spectrometry (IMS). Sample pH, salt effect, extraction time and temperature were investigated and optimized as effective parameters in HS-SPME. The calibration curves were linear in the range of 20-300 ng g(-1) (R(2)>0.99). Limits of detection for Fu and HMFu were 6 ng g(-1) and 5 ng g(-1), respectively. The RSD% of Fu and HMFu for five analyses was 4.4 and 4.9, respectively. The proposed method was successfully applied to determine of Fu and HMFu in the different baby formula samples with satisfactory result. The results were in agreement with those obtained using HPLC analysis. The HS-SPME-IMS is precise, selective and sensitive analytical method for determination of Fu and HMFu in baby formula samples, without any derivatization process. Copyright © 2015 Elsevier Ltd. All rights reserved.

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

    Directory of Open Access Journals (Sweden)

    A. M. Elias

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

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

    Directory of Open Access Journals (Sweden)

    Annarita Panighel

    2014-12-01

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

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

    Science.gov (United States)

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

    2016-08-17

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

  2. Analysis of the volatiles in the headspace above the plasmodium and sporangia of the slime mould (Physarum polycephalum) by SPME-GCMS

    OpenAIRE

    Kateb, Huda al; Costello, Ben de Lacy

    2013-01-01

    Solid phase micro-extraction (SPME) coupled with Gas Chromatography Mass Spectrometry (GC-MS) was used to extract and analyse the volatiles in the headspace above the plasmodial and sporulating stages of the slime mould Physarum Polycephalum. In total 115 compounds were identified from across a broad range of chemical classes. Although more (87) volatile organic compounds (VOCs) were identified when using a higher incubation temperature of 75oC, a large number of compounds (79) were still ide...

  3. Porous Aromatic Framework 48/Gel Hybrid Material Coated Solid-Phase Microextraction Fiber for the Determination of the Migration of Styrene from Polystyrene Food Contact Materials.

    Science.gov (United States)

    Jin, Yuanyuan; Li, Zhongyue; Yang, Lei; Xu, Jun; Zhao, Le; Li, Zhonghao; Niu, Jiajia

    2017-01-17

    A novel solid-phase microextraction (SPME) fiber was fabricated by a porous aromatic framework 48 (PAF-48)/gel hybrid material through a sol-gel process. PAF-48 is a porous organic framework (POF) material that was polymerized from 1,3,5-triphenylbenzene. The uniform pore structure, high surface area, continuous conjugate network, and hydrophobicity make PAF-48 expected to have special abilities to absorb and extract styrene as well as some other harmful volatile aromatic compounds (VACs). The PAF-48/gel-coated fiber was explored for the extraction of styrene and six VACs (benzene, toluene, ethylbenzene, and xylenes) from aqueous food simulants followed by gas chromatography (GC) separation. The fiber was found to be very sensitive for the determination of the target molecules with wide linear ranges (0.1-200 or 500 μg·kg -1 ), low limits of detection (LODs, 0.003-0.060 μg·kg -1 ), acceptable precisions (intraday relative standard deviation, RSD 200 times). Particularly for styrene, the PAF-48/gel-coated fiber exhibited a much lower LOD (0.006 μg·kg -1 ) compared with most of the reported fibers. Moreover, the PAF-48/gel-coated fiber had a high extraction selectivity for styrene and VACs over alcohols, phenols, aromatic amines, and alkanes and show a molecular sieving effect for the different molecule sizes. Finally, the PAF-48/gel-coated SPME fiber was successfully applied in GC for the determination of the specific migrations of styrene and VACs from polystyrene (PS) plastic food contact materials (FCMs).

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

    Science.gov (United States)

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

    2014-12-29

    A new, efficient, and environmental friendly solid-phase microextraction (SPME) medium based on β-cyclodextrin (β-CD)-modified carbon nanotubes (CNTs) and a hollow fiber (HF) was prepared. Functionalized β-CD was covalently linked to the surface of the carboxylic CNTs and then the obtained nanocomposite was immobilized into the wall pores of HFs under ultrasonic-assisted effect. The scanning electron microscope was used to inspect surface characteristics of fibers, demonstrating the presence of nanocomposites in their wall pores. The reinforced HF was employed in SPME, and its extraction performance was evaluated by analyzing 1-naphthaleneacetic acid (NAA) and 2-naphthoxyacetic acid (2-NOA) in vegetables. Without any tedious clean-up procedure, analytes were extracted from the sample to the adsorbent and organic solvent immobilized in HFs and then desorbed in acetonitrile prior to chromatographic analysis. Under the optimized extraction conditions, the method provided 275- and 283-fold enrichment factors of NAA and 2-NOA, low limits of detection and quantification (at an ngg(-1) level), satisfactory spiked recoveries, good inter-fiber repeatability, and batch-to-batch reproducibility. The selectivity of the developed fiber was investigated to three structurally similar compounds and two reference compounds with recognition coefficients up to 3.18. The obtained results indicate that the newly developed fiber is a feasible, selective, green, and cost-effective microextraction medium and could be successfully applied for extraction and determination of naphthalene-derived plant hormones in complex matrices. Copyright © 2014 Elsevier B.V. All rights reserved.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2002-03-01

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

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

    Science.gov (United States)

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

    2016-09-10

    A procedure based on headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography/mass spectrometry (GC/MS) has been developed for the determination of most commonly used drugs of abuse in sweat of drivers stopped during roadside controls. DrugWipe 5A sweat screening device was used to collect sweat by a specific pad rubbed gently over forehead skin surface. The procedure involved an acid hydrolysis, a HS-SPME extraction for drugs of abuse but Δ(9)-tetrahydrocannabinol, which was directly extracted in alkaline medium HS-SPME conditions, a GC separation of analytes by a capillary column and MS detection by electron impact ionisation. The method was linear from the limit of quantification (LOQ) to 50ng drug per pad (r(2)≥0.99), with an intra- and inter-assay precision and accuracy always less than 15% and an analytical recovery between 95.1% and 102.8%, depending on the considered analyte. Using the validated method, sweat from 60 apparently intoxicated drivers were found positive to one or more drugs of abuse, showing sweat patches testing as a viable economic and simple alternative to conventional (blood and/or urine) and non conventional (oral fluid) testing of drugs of abuse in drugged drivers. Copyright © 2016 Elsevier B.V. All rights reserved.

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

    International Nuclear Information System (INIS)

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

    2002-01-01

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

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

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

    Science.gov (United States)

    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. Copyright © 2012 Elsevier B.V. All rights reserved.

  10. Hollow mesoporous carbon spheres-based fiber coating for solid-phase microextraction of polycyclic aromatic hydrocarbons.

    Science.gov (United States)

    Hu, Xingru; Liu, Chao; Li, Jiansheng; Luo, Rui; Jiang, Hui; Sun, Xiuyun; Shen, Jinyou; Han, Weiqing; Wang, Lianjun

    2017-10-20

    In this study, a novel hollow mesoporous carbon spheres-based fiber (HMCSs-F) was fabricated to immobilize HMCSs onto a stainless steel wire for solid-phase microextraction (SPME). Characterization results showed that the HMCSs-F possessed a large specific surface area, high porosity and uniform pore size. To demonstrate the extraction performance, a series of polycyclic aromatic hydrocarbons (PAHs) was chosen as target analytes. The experimental parameters including extraction and desorption conditions were optimized. Compared to commercial fibers, the HMCSs-F exhibited better extraction efficiency for PAHs. More interestingly, a good extraction selectivity for PAHs from the complex matrix was observed in these HMCSs-F. The enhanced SPME performance was attributed to the unique pore structure and special surface properties of the HMCSs. Furthermore, under the optimum conditions, the limits of detection (LODs) for the HMCSs-F were in the range of 0.20-1.15ngL -1 with a corresponding relative standard deviation that was below 8.6%. The method was successfully applied for the analysis of PAHs in actual environmental water samples with recoveries ranging from 85.9% to 112.2%. These results imply that the novel HMCSs-F have potential application in environmental water analysis. Copyright © 2017 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

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

    2017-02-01

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

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

    Science.gov (United States)

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

    2016-09-01

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

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

    Science.gov (United States)

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

    2016-03-15

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

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

    Science.gov (United States)

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

    2017-03-01

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

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

    Science.gov (United States)

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

    2017-03-01

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

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

    Directory of Open Access Journals (Sweden)

    Carlos Sanz

    2018-04-01

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

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

    Science.gov (United States)

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

    2017-10-01

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

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

    Science.gov (United States)

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

    2014-05-15

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

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

    Science.gov (United States)

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

    2018-04-01

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

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

    International Nuclear Information System (INIS)

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

    2003-01-01

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

  1. Fibered F-Algebra

    OpenAIRE

    Kleyn, Aleks

    2007-01-01

    The concept of F-algebra and its representation can be extended to an arbitrary bundle. We define operations of fibered F-algebra in fiber. The paper presents the representation theory of of fibered F-algebra as well as a comparison of representation of F-algebra and of representation of fibered F-algebra.

  2. Photonic crystal fibers

    DEFF Research Database (Denmark)

    Lægsgaard, Jesper; Hansen, K P; Nielsen, M D

    2003-01-01

    Photonic crystal fibers having a complex microstructure in the transverse plane constitute a new and promising class of optical fibers. Such fibers can either guide light through total internal reflection or the photonic bandgap effect, In this paper, we review the different types and applications...... of photonic crystal fibers with particular emphasis on recent advances in the field....

  3. Photonic crystal fibers -

    DEFF Research Database (Denmark)

    Libori, Stig E. Barkou

    2002-01-01

    . Such micro-structured fibers are the ones most often trated in literature concerning micro-structured fibers. These micro-structured fibers offer a whole range of novel wave guiding characteristics, including the possibility of fibers that guide only one mode irrespective of the frequency of light...

  4. Fiber optic connector

    Science.gov (United States)

    Rajic, Slobodan; Muhs, Jeffrey D.

    1996-01-01

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

  5. 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

    International Nuclear Information System (INIS)

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

    2014-01-01

    Graphical abstract: - Highlights: • A novel solid-phase microextraction (SPME) fiber was prepared using sol–gel technology. • Sol–gel coating was performed on stainless steel substrate. • The new fibers are robust and unbreakable with temperature stability. • The fibers were used for extraction of PAHs from aqueous samples. - Abstract: 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

  6. 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

    Energy Technology Data Exchange (ETDEWEB)

    Es-haghi, Ali, E-mail: a.eshaghi@rvsri.ac.ir [Department of Physico Chemistry, Razi Vaccine and Serum Research Institute, PO Box 31975/148, Karaj (Iran, Islamic Republic of); Hosseininasab, Valiallah; Bagheri, Habib [Environmental and Bio-Analytical Laboratories, Department of Chemistry, Sharif University of Technology, PO Box 11365-9516, Tehran (Iran, Islamic Republic of)

    2014-02-01

    Highlights: • A novel solid-phase microextraction (SPME) fiber was prepared using sol–gel technology. • Sol–gel coating was performed on stainless steel substrate. • The new fibers are robust and unbreakable with temperature stability. • The fibers were used for extraction of PAHs from aqueous samples. Abstract: 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⁻¹with 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.

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

    Directory of Open Access Journals (Sweden)

    Jorge G. Figueroa

    2016-07-01

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

  8. Nonlinear Photonic Crystal Fibers

    DEFF Research Database (Denmark)

    Hansen, Kim Per

    2004-01-01

    Despite the general recession in the global economy and the collapse of the optical telecommunication market, research within specialty fibers is thriving. This is, more than anything else, due to the technology transition from standard all-glass fibers to photonic crystal fibers, which, instead....... The freedom to design the dispersion profile of the fibers is much larger and it is possible to create fibers, which support only a single spatial mode, regardless of wavelength. In comparison, the standard dispersion-shifted fibers are limited by a much lower index-contrast between the core and the cladding...... in 1996, and are today on their way to become the dominating technology within the specialty fiber field. Whether they will replace the standard fiber in the more traditional areas like telecommunication transmission, is not yet clear, but the nonlinear photonic crystal fibers are here to stay....

  9. Optical Fiber Fusion Splicing

    CERN Document Server

    Yablon, Andrew D

    2005-01-01

    This book is an up-to-date treatment of optical fiber fusion splicing incorporating all the recent innovations in the field. It provides a toolbox of general strategies and specific techniques that the reader can apply when optimizing fusion splices between novel fibers. It specifically addresses considerations important for fusion splicing of contemporary specialty fibers including dispersion compensating fiber, erbium-doped gain fiber, polarization maintaining fiber, and microstructured fiber. Finally, it discusses the future of optical fiber fusion splicing including silica and non-silica based optical fibers as well as the trend toward increasing automation. Whilst serving as a self-contained reference work, abundant citations from the technical literature will enable readers to readily locate primary sources.

  10. Amplitude-modulated fiber-ring laser

    DEFF Research Database (Denmark)

    Caputo, J. G.; Clausen, Carl A. Balslev; Sørensen, Mads Peter

    2000-01-01

    Soliton pulses generated by a fiber-ring laser are investigated by numerical simulation and perturbation methods. The mathematical modeling is based on the nonlinear Schrödinger equation with perturbative terms. We show that active mode locking with an amplitude modulator leads to a self......-starting of stable solitonic pulses from small random noise, provided the modulation depth is small. The perturbative analysis leads to a nonlinear coupled return map for the amplitude, phase, and position of the soliton pulses circulating in the fiber-ring laser. We established the validity of this approach...

  11. Head Space Solid Phase Micro-Extraction (HS - SPME of volatile organic compounds produced by Sporidiobolus salmonicolor (CBS 2636

    Directory of Open Access Journals (Sweden)

    Eunice Valduga

    2010-12-01

    Full Text Available The aim of the present study was the assessment of volatile organic compounds produced by Sporidiobolus salmonicolor (CBS 2636 using methyl and ethyl ricinoleate, ricinoleic acid and castor oil as precursors. The analysis of the volatile organic compounds was carried out using Head Space Solid Phase Micro-Extraction (HS - SPME. Factorial experimental design was used for investigating extraction conditions, verifying stirring rate (0-400 rpm, temperature (25-60 ºC, extraction time (10-30 minutes, and sample volume (2-3 mL. The identification of volatile organic compounds was carried out by Gas Chromatography with Mass Spectrum Detector (GC/MSD. The conditions that resulted in maximum extraction were: 60 ºC, 10 minutes extraction, no stirring, sample volume of 2.0 mL, and addition of saturated KCl (1:10 v/v. In the bio-production of volatile organic compounds the effect of stirring rate (120-200 rpm, temperature (23-33 ºC, pH (4.0-8.0, precursor concentration (0.02-0.1%, mannitol (0-6%, and asparagine concentration (0-0.2% was investigated. The bio-production at 28 ºC, 160 rpm, pH 6,0 and with the addition of 0.02% ricinoleic acid to the medium yielded the highest production of VOCs, identified as 1,4-butanediol, 1,2,2-trimethylciclopropilamine, beta-ionone; 2,3-butanodione, pentanal, tetradecane, 2-isononenal, 4-octen-3-one, propanoic acid, and octadecane.

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

    Science.gov (United States)

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

    2016-01-01

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

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

    Science.gov (United States)

    Zhu, Jia; Wang, Ying; Zeng, Lin

    2016-08-01

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

  14. Volatiles and primary metabolites profiling in two Hibiscus sabdariffa (roselle) cultivars via headspace SPME-GC-MS and chemometrics.

    Science.gov (United States)

    Farag, Mohamed A; Rasheed, Dalia M; Kamal, Islam M

    2015-12-01

    Hibiscus sabdariffa (roselle) is a plant of considerable commercial importance worldwide as functional food due to its organic acids, mucilage, anthocyanins, macro and micro-nutrients content. Although Hibiscus flowers are emerging as very competitive targets for phytochemical studies, very little is known about their volatile composition and or aroma, such knowledge can be suspected to be relevant for understanding its olfactory and taste properties. To provide insight into Hibiscus flower aroma composition and for its future use in food and or pharmaceutical industry, volatile constituents from 2 cultivars grown in Egypt, viz. Aswan and Sudan-1 were profiled using solid-phase microextraction (SPME) coupled to GCMS. A total of 104 volatiles were identified with sugar and fatty acid derived volatiles amounting for the major volatile classes. To reveal for cultivar effect on volatile composition in an untargeted manner, multivariate data analysis was applied. Orthogonal projection to latent structures-discriminant analysis (OPLS-DA) revealed for 1-octen-3-ol versus furfural/acetic acid enrichment in Aswan and Sudan-1 cvs., respectively. Primary metabolites contributing to roselle taste and nutritional value viz. sugars and organic acids were profiled using GC-MS after silylation. The impact of probiotic bacteria on roselle infusion aroma profile was further assessed and revealed for the increase in furfural production with Lactobacillus plantarum inoculation and without affecting its anthocyanin content. This study provides the most complete map for volatiles, sugars and organic acids distribution in two Hibiscus flower cultivars and its fermented product. Copyright © 2015 Elsevier Ltd. All rights reserved.

  15. Ceramic fiber reinforced filter

    Science.gov (United States)

    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.

  16. Steel fiber reinforced concrete

    International Nuclear Information System (INIS)

    Baloch, S.U.

    2005-01-01

    Steel-Fiber Reinforced Concrete is constructed by adding short fibers of small cross-sectional size .to the fresh concrete. These fibers reinforce the concrete in all directions, as they are randomly oriented. The improved mechanical properties of concrete include ductility, impact-resistance, compressive, tensile and flexural strength and abrasion-resistance. These uniqlte properties of the fiber- reinforcement can be exploited to great advantage in concrete structural members containing both conventional bar-reinforcement and steel fibers. The improvements in mechanical properties of cementitious materials resulting from steel-fiber reinforcement depend on the type, geometry, volume fraction and material-properties of fibers, the matrix mix proportions and the fiber-matrix interfacial bond characteristics. Effects of steel fibers on the mechanical properties of concrete have been investigated in this paper through a comprehensive testing-programme, by varying the fiber volume fraction and the aspect-ratio (Lid) of fibers. Significant improvements are observed in compressive, tensile, flexural strength and impact-resistance of concrete, accompanied by marked improvement in ductility. optimum fiber-volume fraction and aspect-ratio of steel fibers is identified. Test results are analyzed in details and relevant conclusions drawn. The research is finally concluded with future research needs. (author)

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

    Science.gov (United States)

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

    2017-11-01

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

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

    International Nuclear Information System (INIS)

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

    2009-01-01

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

  19. Fiber optics in adverse environments

    International Nuclear Information System (INIS)

    Lyous, P.B.

    1982-01-01

    Radiation effects in optical fibers are considered, taking into account recent progress in the investigation of radiation resistant optical fibers, radiation damage in optical fibers, radiation-induced transient absorption in optical fibers, X-ray-induced transient attenuation at low temperatures in polymer clad silica (PCS) fibers, optical fiber composition and radiation hardness, the response of irradiated optical waveguides at low temperatures, and the effect of ionizing radiation on fiber-optic waveguides. Other topics explored are related to environmental effects on components of fiber optic systems, and radiation detection systems using optical fibers. Fiber optic systems in adverse environments are also discussed, giving attention to the survivability of Army fiber optics systems, space application of fiber optics systems, fiber optic wavelength multiplexing for civil aviation applications, a new fiber optic data bus topology, fiber optics for aircraft engine/inlet control, and application of fiber optics in high voltage substations

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

    OpenAIRE

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

    2016-01-01

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

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

    Science.gov (United States)

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

    2014-12-01

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

  2. Fiber Optics Technology.

    Science.gov (United States)

    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)

  3. Fiber Optics Instrumentation Development

    Science.gov (United States)

    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.

  4. Shaped fiber composites

    Science.gov (United States)

    Kinnan, Mark K.; Roach, Dennis P.

    2017-12-05

    A composite article is disclosed that has non-circular fibers embedded in a polymer matrix. The composite article has improved damage tolerance, toughness, bending, and impact resistance compared to composites having traditional round fibers.

  5. Advances in Fiber Lasers

    National Research Council Canada - National Science Library

    Morse, T

    1999-01-01

    Most of the time of this contract has been devoted toward improvements in optical fiber lasers and toward gathering experience to improve our program in high power, cladding pumped optical fiber lasers...

  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.

    Science.gov (United States)

    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. Copyright © 2016 Elsevier B.V. All rights reserved.

  7. Hierarchically Structured Electrospun Fibers

    Science.gov (United States)

    2013-01-07

    in the natural lotus and silver ragwort leaves. Figure 4. Examples of electrospun bio-mimics of natural hierarchical structures. (A) Lotus leaf...B) pillared poly(methyl methacrylate) (PMMA) electrospun fiber mimic; (C) silver ragwort leaf; (D) electrospun fiber mimic made from nylon 6 and...domains containing the protein in the surrounding EVA fibers [115]. A wide variety of core-shell fibers have been generated, including PCL/ gelatin

  8. Superlattice Microstructured Optical Fiber

    Science.gov (United States)

    Tse, Ming-Leung Vincent; Liu, Zhengyong; Cho, Lok-Hin; Lu, Chao; Wai, Ping-Kong Alex; Tam, Hwa-Yaw

    2014-01-01

    A generic three-stage stack-and-draw method is demonstrated for the fabrication of complex-microstructured optical fibers. We report the fabrication and characterization of a silica superlattice microstructured fiber with more than 800 rhomboidally arranged air-holes. A polarization-maintaining fiber with a birefringence of 8.5 × 10−4 is demonstrated. The birefringent property of the fiber is found to be highly insensitive to external environmental effects, such as pressure. PMID:28788693

  9. Solid-phase microextraction Ni-Ti fibers coated with functionalised silica particles immobilized in a sol-gel matrix.

    Science.gov (United States)

    Azenha, Manuel; Ornelas, Mariana; Fernando Silva, A

    2009-03-20

    One of the possible approaches for the development of novel solid-phase microextraction (SPME) fibers is the physical deposition of porous materials onto a support using high-temperature epoxy glue. However, a major drawback arises from decomposition of epoxy glue at temperatures below 300 degrees C and instability in some organic solvents. This limitation motivated us to explore the possibility of replacing the epoxy glue with a sol-gel film, thermally more stable and resistant to organic solvents. We found that functionalised silica particles could be successfully attached to a robust Ni-Ti wire by using a UV-curable sol-gel film. The particles were found to be more important than the sol-gel layer during the microextraction process, as shown by competitive extraction trials and by the different extraction profiles observed with differently functionalised particles. If a quality control microscopic-check aiming at the rejection of fibers exhibiting unacceptably low particle load was conducted, acceptable (6-14%) reproducibility of preparation of C(18)-silica fibers was observed, and a strong indication of the durability of the fibers was also obtained. A cyclohexyldiol-silica fiber was used, as a simple example of applicability, for the successful determination of benzaldehyde, acetophenone and dimethylphenol at trace level in spiked tap water. Recoveries: 95-109%; limits of detection: 2-7 microg/L; no competition effects within the studied range (

  10. High-fiber foods

    Science.gov (United States)

    ... page: //medlineplus.gov/ency/patientinstructions/000193.htm High-fiber foods To use the sharing features on this page, ... Read food labels carefully to see how much fiber they have. Choose foods that have higher amounts of fiber, such as ...

  11. Resonant filtered fiber amplifiers

    DEFF Research Database (Denmark)

    Alkeskjold, Thomas Tanggaard; Laurila, Marko; Olausson, Christina Bjarnal Thulin

    2013-01-01

    In this paper we present our recent result on utilizing resonant/bandgap fiber designs to achieve high performance ytterbium doped fiber amplifers for achieving diffraction limited beam quality in large mode area fibers, robust bending performance and gain shaping for long wavelength operation...

  12. Fiber Singular Optics

    OpenAIRE

    A. V. Volyar

    2002-01-01

    The present review is devoted to the optical vortex behavior both in free space and optical fibers. The processes of the vortex transformations in perturbed optical fibers are analyzed on the base of the operator of the spin – orbit interaction in order to forecast the possible ways of manufacturing the vortex preserving fibers and their applications in supersensitive optical devices.

  13. Superconducting tin core fiber

    International Nuclear Information System (INIS)

    Homa, Daniel; Liang, Yongxuan; Hill, Cary; Kaur, Gurbinder; Pickrell, Gary

    2015-01-01

    In this study, we demonstrated superconductivity in a fiber with a tin core and fused silica cladding. The fibers were fabricated via a modified melt-draw technique and maintained core diameters ranging from 50-300 microns and overall diameters of 125-800 microns. Superconductivity of this fiber design was validated via the traditional four-probe test method in a bath of liquid helium at temperatures on the order of 3.8 K. The synthesis route and fiber design are perquisites to ongoing research dedicated all-fiber optoelectronics and the relationships between superconductivity and the material structures, as well as corresponding fabrication techniques. (orig.)

  14. Gas chromatographic-mass spectrometric analysis of urinary volatile organic metabolites: Optimization of the HS-SPME procedure and sample storage conditions.

    Science.gov (United States)

    Živković Semren, Tanja; Brčić Karačonji, Irena; Safner, Toni; Brajenović, Nataša; Tariba Lovaković, Blanka; Pizent, Alica

    2018-01-01

    Non-targeted metabolomics research of human volatile urinary metabolome can be used to identify potential biomarkers associated with the changes in metabolism related to various health disorders. To ensure reliable analysis of urinary volatile organic metabolites (VOMs) by gas chromatography-mass spectrometry (GC-MS), parameters affecting the headspace-solid phase microextraction (HS-SPME) procedure have been evaluated and optimized. The influence of incubation and extraction temperatures and times, coating fibre material and salt addition on SPME efficiency was investigated by multivariate optimization methods using reduced factorial and Doehlert matrix designs. The results showed optimum values for temperature to be 60°C, extraction time 50min, and incubation time 35min. The proposed conditions were applied to investigate urine samples' stability regarding different storage conditions and freeze-thaw processes. The sum of peak areas of urine samples stored at 4°C, -20°C, and -80°C up to six months showed a time dependent decrease over time although storage at -80°C resulted in a slight non-significant reduction comparing to the fresh sample. However, due to the volatile nature of the analysed compounds, more than two cycles of freezing/thawing of the sample stored for six months at -80°C should be avoided whenever possible. Copyright © 2017 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

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

    2016-08-01

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

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

    Science.gov (United States)

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

    2016-02-15

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

  17. Airclad fiber laser technology

    DEFF Research Database (Denmark)

    Hansen, Kim P.; Olausson, Christina Bjarnal Thulin; Broeng, Jes

    2011-01-01

    High-power fiber lasers and amplifiers have gained tremendous momentum in the last 5 years. Many of the traditional manufacturers of gas and solid-state lasers are now pursuing the fiber-based systems, which are displacing the conventional technology in many areas. High-power fiber laser systems...... require reliable fibers with large cores, stable mode quality, and good power handling capabilities-requirements that are all met by the airclad fiber technology. In the present paper we go through many of the building blocks needed to build high-power systems and we show an example of a complete airclad...... laser system. We present the latest advancements within airclad fiber technology including a new 100 m single-mode polarization-maintaining rod-type fiber capable of amplifying to megawatt power levels. Furthermore, we describe the novel airclad-based pump combiners and their use in a completely...

  18. Airclad fiber laser technology

    DEFF Research Database (Denmark)

    Hansen, Kim P.; Olausson, Christina Bjarnal Thulin; Broeng, Jes

    2008-01-01

    High-power fiber lasers and amplifiers have gained tremendous momentum in the last five years, and many of the traditional manufactures of gas and solid-state lasers are pursuing the attractive fiber-based systems, which are now displacing the old technology in many areas. High-power fiber laser...... systems require specially designed fibers with large cores and good power handling capabilities - requirements that are all met by the airclad fiber technology. In the present paper we go through many of the building blocks needed to build high-power systems and we show an example of a complete airclad...... laser system. We present the latest advancements within airclad fiber technology including a new 70 μm single-mode polarization-maintaining rod-type fiber capable of amplifying to MW power levels. Furthermore we describe the novel airclad based pump combiners and their use in a completely monolithic 350...

  19. Hierarchically Structured Electrospun Fibers

    Directory of Open Access Journals (Sweden)

    Nicole E. Zander

    2013-01-01

    Full Text Available Traditional electrospun nanofibers have a myriad of applications ranging from scaffolds for tissue engineering to components of biosensors and energy harvesting devices. The generally smooth one-dimensional structure of the fibers has stood as a limitation to several interesting novel applications. Control of fiber diameter, porosity and collector geometry will be briefly discussed, as will more traditional methods for controlling fiber morphology and fiber mat architecture. The remainder of the review will focus on new techniques to prepare hierarchically structured fibers. Fibers with hierarchical primary structures—including helical, buckled, and beads-on-a-string fibers, as well as fibers with secondary structures, such as nanopores, nanopillars, nanorods, and internally structured fibers and their applications—will be discussed. These new materials with helical/buckled morphology are expected to possess unique optical and mechanical properties with possible applications for negative refractive index materials, highly stretchable/high-tensile-strength materials, and components in microelectromechanical devices. Core-shell type fibers enable a much wider variety of materials to be electrospun and are expected to be widely applied in the sensing, drug delivery/controlled release fields, and in the encapsulation of live cells for biological applications. Materials with a hierarchical secondary structure are expected to provide new superhydrophobic and self-cleaning materials.

  20. Fiber optics in SHIVA

    International Nuclear Information System (INIS)

    Severyn, J.; Parker, J.

    1978-01-01

    SHIVA is a twenty arm laser which is controlled with a network of fifty computers, interconnected with digital fiber optic links. Three different fiber optic systems employed on the Shiva laser will be described. Two of the systems are for digital communications, one at 9600 baud and the other at 1 megabaud. The third system uses fiber optics to distribute diagnostic triggers with subnanosecond jitter

  1. Continuous Fiber Ceramic Composites

    Energy Technology Data Exchange (ETDEWEB)

    Fareed, Ali [Honeywell Advanced Composites Inc. (HACI), Newark, DE (United States); Craig, Phillip A. [Honeywell Advanced Composites Inc. (HACI), Newark, DE (United States)

    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.

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

    Science.gov (United States)

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

    2018-02-01

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

  3. Agave Americana Leaf Fibers

    Directory of Open Access Journals (Sweden)

    Ashish Hulle

    2015-02-01

    Full Text Available The growing environmental problems, the problem of waste disposal and the depletion of non-renewable resources have stimulated the use of green materials compatible with the environment to reduce environmental impacts. Therefore, there is a need to design products by using natural resources. Natural fibers seem to be a good alternative since they are abundantly available and there are a number of possibilities to use all the components of a fiber-yielding crop; one such fiber-yielding plant is Agave Americana. The leaves of this plant yield fibers and all the parts of this plant can be utilized in many applications. The “zero-waste” utilization of the plant would enable its production and processing to be translated into a viable and sustainable industry. Agave Americana fibers are characterized by low density, high tenacity and high moisture absorbency in comparison with other leaf fibers. These fibers are long and biodegradable. Therefore, we can look this fiber as a sustainable resource for manufacturing and technical applications. Detailed discussion is carried out on extraction, characterization and applications of Agave Americana fiber in this paper.

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

    Science.gov (United States)

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

    2016-11-01

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

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

    Directory of Open Access Journals (Sweden)

    Douglas B. Fonseca

    2007-01-01

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

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

    Science.gov (United States)

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

    2015-08-05

    A simple solid phase microextraction method based on molecularly imprinted polymer sorbent in the hollow fiber (MIP-HF-SPME) combined with fiber optic-linear array spectrophotometer has been applied for the extraction and determination of diclofenac in environmental and biological samples. The effects of different parameters such as pH, times of extraction, type and volume of the organic solvent, stirring rate and donor phase volume on the extraction efficiency of the diclofenac were investigated and optimized. Under the optimal conditions, the calibration graph was linear (r(2)=0.998) in the range of 3.0-85.0 μg L(-1) with a detection limit of 0.7 μg L(-1) for preconcentration of 25.0 mL of the sample and the relative standard deviation (n=6) less than 5%. This method was applied successfully for the extraction and determination of diclofenac in different matrices (water, urine and plasma) and accuracy was examined through the recovery experiments. Copyright © 2015 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

    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.

  8. USDA Flax fiber utilization research

    Science.gov (United States)

    The United States is pursuing natural fibers as sustainable, environmentally friendly sources for a variety of industrial applications. Flax (Linum usitatissimum L.) fiber offers many possibilities towards this goal. Research on flax fiber production, processing, and standards development is urgen...

  9. Ultrafine PBI fibers and yarns

    Science.gov (United States)

    Leal, J. R.; Tan, M.

    1979-01-01

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

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

    Science.gov (United States)

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

    2018-06-13

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

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

    Science.gov (United States)

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

    2017-04-05

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

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

    Directory of Open Access Journals (Sweden)

    Igor Lukić

    2017-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Taliana Kênia Alves BEZERRA

    2016-03-01

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

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

    Science.gov (United States)

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

    2016-11-01

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

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

    Directory of Open Access Journals (Sweden)

    Aikaterini Koutsaviti

    2016-05-01

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

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

    Directory of Open Access Journals (Sweden)

    Catarina Silva

    2014-01-01

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

  17. Assessing a traceability technique in fresh oranges (Citrus sinensis L. Osbeck) with an HS-SPME-GC-MS method. Towards a volatile characterisation of organic oranges.

    Science.gov (United States)

    Cuevas, Francisco Julián; Moreno-Rojas, José Manuel; Ruiz-Moreno, María José

    2017-04-15

    A targeted approach using HS-SPME-GC-MS was performed to compare flavour compounds of 'Navelina' and 'Salustiana' orange cultivars from organic and conventional management systems. Both varieties of conventional oranges showed higher content of ester compounds. On the other hand, higher content of some compounds related with the geranyl-diphosphate pathway (neryl and geranyl acetates) and some terpenoids were found in the organic samples. Furthermore, the partial least square discriminant analysis (PLS-DA) achieved an effective classification for oranges based on the farming system using their volatile profiles (90 and 100% correct classification). To our knowledge, it is the first time that a comparative study dealing with farming systems and orange aroma profile has been performed. These new insights, taking into account local databases, cultivars and advanced analytical tools, highlight the potential of volatile composition for organic orange discrimination. Copyright © 2016 Elsevier Ltd. All rights reserved.

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

    Science.gov (United States)

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

    2017-11-15

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

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

    Science.gov (United States)

    Lukić, Igor; Horvat, Ivana

    2017-03-01

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

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

    OpenAIRE

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

    2016-01-01

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

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

    Science.gov (United States)

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

    2005-04-01

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

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

    Science.gov (United States)

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

    2011-09-01

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

  3. Applications of nonlinear fiber optics

    CERN Document Server

    Agrawal, Govind

    2008-01-01

    * The only book describing applications of nonlinear fiber optics * Two new chapters on the latest developments: highly nonlinear fibers and quantum applications* Coverage of biomedical applications* Problems provided at the end of each chapterThe development of new highly nonlinear fibers - referred to as microstructured fibers, holey fibers and photonic crystal fibers - is the next generation technology for all-optical signal processing and biomedical applications. This new edition has been thoroughly updated to incorporate these key technology developments.The bo

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

    Science.gov (United States)

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

    2017-04-01

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

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

    Science.gov (United States)

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

    2003-09-01

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

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

    Science.gov (United States)

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

    2000-01-10

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

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

    Science.gov (United States)

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

    2011-07-15

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

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

    International Nuclear Information System (INIS)

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

    2014-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-04-01

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

  10. Multimode optical fiber

    Science.gov (United States)

    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).

  11. Fiber Lasers V

    DEFF Research Database (Denmark)

    Hansen, Kim P.; Olausson, Christina Bjarnal Thulin; Broeng, Jes

    2008-01-01

    laser system. We present the latest advancements within airclad fiber technology including a new 70 μm single-mode polarization-maintaining rod-type fiber capable of amplifying to MW power levels. Furthermore we describe the novel airclad based pump combiners and their use in a completely monolithic 350...

  12. Fiber Sensor Technology Today

    Science.gov (United States)

    Hotate, Kazuo

    2006-08-01

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

  13. Ways to Boost Fiber

    Science.gov (United States)

    ... can help to lower cholesterol. Third, it helps prevent constipation and diverticulosis. And fourth, adequate fiber from food ... is similar to a new sponge; it needs water to plump up pass smoothly. If you ... or constipation. Before you reach for the fiber supplements, consider ...

  14. Quartz fiber calorimeter

    International Nuclear Information System (INIS)

    Akchurin, N.; Doulas, S.; Ganel, O.; Gershtein, Y.; Gavrilov, V.; Kolosov, V.; Kuleshov, S.; Litvinsev, D.; Merlo, J.-P.; Onel, Y.; Osborne, D.; Rosowsky, A.; Stolin, V.; Sulak, L.; Sullivan, J.; Ulyanov, A.; Wigmans, R.; Winn, D.

    1996-01-01

    A calorimeter with optical quartz fibers embedded into an absorber matrix was proposed for the small angle region of the CMS detector at LHC (CERN). This type of calorimeter is expected to be radiation hard and to produce extremely fast signal. Some results from beam tests of the quartz fiber calorimeter prototype are presented. (orig.)

  15. High-density multicore fibers

    DEFF Research Database (Denmark)

    Takenaga, K.; Matsuo, S.; Saitoh, K.

    2016-01-01

    High-density single-mode multicore fibers were designed and fabricated. A heterogeneous 30-core fiber realized a low crosstalk of −55 dB. A quasi-single-mode homogeneous 31-core fiber attained the highest core count as a single-mode multicore fiber.......High-density single-mode multicore fibers were designed and fabricated. A heterogeneous 30-core fiber realized a low crosstalk of −55 dB. A quasi-single-mode homogeneous 31-core fiber attained the highest core count as a single-mode multicore fiber....

  16. Green insulation: hemp fibers

    Energy Technology Data Exchange (ETDEWEB)

    Anon,

    2011-09-15

    Indian hemp (Cannabis indica) is known for its psychotropic values and it is banned in most countries. However, industrial hemp (Cannabis sativa) is known for its tough fibers. Several manufactures in Europe including, small niche players, have been marketing hemp insulation products for several years. Hemp is a low environmental impact material. Neither herbicide nor pesticide is used during the growth of hemp. The fibers are extracted in a waste-free and chemical-free mechanical process. Hemp can consume CO2 during its growth. In addition, hemp fiber can be disposed of harmlessly by composting or incineration at the end of its life. Hemp fibers are processed and treated only minimally to resist rot and fungal activity. There is little health risk when producing and installing the insulation, thanks to the absence of toxic additive. Its thermal resistance is comparable to mineral wool. But the development and marketing of hemp fibers may be restricted in North America.

  17. Raman fiber lasers

    CERN Document Server

    2017-01-01

    This book serves as a comprehensive, up-to-date reference about this cutting-edge laser technology and its many new and interesting developments. Various aspects and trends of Raman fiber lasers are described in detail by experts in their fields. Raman fiber lasers have progressed quickly in the past decade, and have emerged as a versatile laser technology for generating high power light sources covering a spectral range from visible to mid-infrared. The technology is already being applied in the fields of telecommunication, astronomy, cold atom physics, laser spectroscopy, environmental sensing, and laser medicine. This book covers various topics relating to Raman fiber laser research, including power scaling, cladding and diode pumping, cascade Raman shifting, single frequency operation and power amplification, mid-infrared laser generation, specialty optical fibers, and random distributed feedback Raman fiber lasers. The book will appeal to scientists, students, and technicians seeking to understand the re...

  18. Birefringent hollow core fibers

    DEFF Research Database (Denmark)

    Roberts, John

    2007-01-01

    Hollow core photonic crystal fiber (HC-PCF), fabricated according to a nominally non-birefringent design, shows a degree of un-controlled birefringence or polarization mode dispersion far in excess of conventional non polarization maintaining fibers. This can degrade the output pulse in many...... applications, and places emphasis on the development of polarization maintaining (PM) HC-PCF. The polarization cross-coupling characteristics of PM HC-PCF are very different from those of conventional PM fibers. The former fibers have the advantage of suffering far less from stress-field fluctuations...... and an increased overlap between the polarization modes at the glass interfaces. The interplay between these effects leads to a wavelength for optimum polarization maintenance, lambda(PM), which is detuned from the wavelength of highest birefringence. By a suitable fiber design involving antiresonance of the core...

  19. Fiber optic hydrophone

    Science.gov (United States)

    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.

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

    Science.gov (United States)

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

    2014-03-21

    Metal-organic frameworks (MOFs) have received considerable attention as novel sorbents for sample preparation due to their fascinating structures and functionalities such as large surface area, good thermal stability, and uniform structured nanoscale cavities. Here, we report the application of a thermal and solvent stable MOF MIL-88B with nanosized bipyramidal cages and large surface area for solid-phase microextraction (SPME) of polychlorinated biphenyls (PCBs). Novel MIL-88B coated fiber was fabricated via an in situ hydrothermal growth of MIL-88B film on etched stainless steel fiber. The MIL-88B coated fiber gave large enhancement factors (757-2243), low detection limits (0.45-1.32ngL(-1)), and good linearity (5-200ngL(-1)) for PCBs. The relative standard deviation (RSD) for six replicate extractions of PCBs at 100ngL(-1) on MIL-88B coated fiber ranged from 4.2% to 8.7%. The recoveries for spiked PCBs (10ngL(-1)) in water and soil samples were in the range of 79.7-103.2%. Besides, the MIL-88B coated fiber was stable enough for 150 extraction cycles without significant loss of extraction efficiency. The developed method was successfully applied to the determination of PCBs in water samples and soil samples. Copyright © 2014 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

    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.

  2. Analysis of carbonyl compounds via headspace solid-phase microextraction with on-fiber derivatization and gas chromatographic-ion trap tandem mass spectrometric determination of their O-(2,3,4,5,6-pentafluorobenzyl)oxime derivatives

    Energy Technology Data Exchange (ETDEWEB)

    Schmarr, Hans-Georg [Dienstleistungszentrum Laendlicher Raum (DLR) Rheinpfalz, Breitenweg 71, D-67435 Neustadt an der Weinstrasse (Germany)], E-mail: hans-georg.schmarr@dlr.rlp.de; Potouridis, Theodoros; Ganss, Sebastian; Sang, Wei; Koepp, Benedikt; Bokuz, Ursula; Fischer, Ulrich [Dienstleistungszentrum Laendlicher Raum (DLR) Rheinpfalz, Breitenweg 71, D-67435 Neustadt an der Weinstrasse (Germany)

    2008-06-09

    An improved method for the analysis of carbonyls is described utilizing a headspace solid-phase microextraction (HS-SPME) step and on-fiber derivatization with O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine (PFBHA) hydrochloride. Thermal desorption of the oxime derivatives formed on the fiber is followed by gas chromatographic separation coupled to an ion trap tandem mass spectrometer (GC-ITMS). Selecting specific fragment ions within the electron ionization (EI{sup +}) mass spectra of these oxime derivatives as precursor ions for MS-MS fragmentation provides a suitable method for the target analysis of individual carbonyl classes, such as alkanals, (E)-2-alkenals, (E,E)-2,4-alkadienals, and others. Retention indices on polar as well as on apolar stationary phases along with EI{sup +} mass spectra patterns are presented for a large set of oxime derivatives, giving valuable information needed for unambiguous assignment of substances in complex sample matrices. The fast sample preparation and derivatization step via HS-SPME can be automated and is applicable to a variety of biological samples and foodstuffs, allowing rapid and sensitive screening analyses of important aldehydic biomarkers and aroma active compounds.

  3. Fiber Pulling Apparatus

    Science.gov (United States)

    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

  4. Fiber Optic Microphone

    Science.gov (United States)

    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.

  5. Optical fiber spectrophotometer

    International Nuclear Information System (INIS)

    Zhuang Weixin; Tian Guocheng; Ye Guoan; Zhou Zhihong; Cheng Weiwei; Huang Lifeng; Liu Suying; Tang Yanji; Hu Jingxin; Zhao Yonggang

    1998-12-01

    A method called 'Two Arm's Photo out and Electricity Send-back' is introduced. UV-365 UV/VIS/NIR spectrophotometer has been reequipped by this way with 5 meters long optical fiber. Another method called 'One Arm's Photo out and Photo Send-back' is also introduced. λ 19 UV/VIS/NIR spectrophotometer has been reequipped by this way with 10 meters long optical fiber. Optical fiber spectrophotometer can work as its main set. So it is particularly applicable to radio activity work

  6. Chemistry Research of Optical Fibers.

    Science.gov (United States)

    1982-09-27

    BROADENING IN OPTICAL FIBERS Herbert B. Rosenstock* Naval Research Laboratory Washington, DC 20375 ABSTRACT A light pulse transmitted through a fiber...Marcatili, Marcuse , and Personick, "Dispersion Properties of Fibers" (Ch. 4 in "Optical Fiber Telecommunications," S. E. Miller and A. C. Chynoweth, eds

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

    Science.gov (United States)

    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.

  8. Fiber optics standard dictionary

    CERN Document Server

    Weik, Martin H

    1997-01-01

    Fiber Optics Vocabulary Development In 1979, the National Communications System published Technical InfonnationBulle­ tin TB 79-1, Vocabulary for Fiber Optics and Lightwave Communications, written by this author. Based on a draft prepared by this author, the National Communications System published Federal Standard FED-STD-1037, Glossary of Telecommunications Terms, in 1980 with no fiber optics tenns. In 1981, the first edition of this dictionary was published under the title Fiber Optics and Lightwave Communications Standard Dictionary. In 1982, the then National Bureau of Standards, now the National Institute of Standards and Technology, published NBS Handbook 140, Optical Waveguide Communications Glossary, which was also published by the General Services Admin­ istration as PB82-166257 under the same title. Also in 1982, Dynamic Systems, Inc. , Fiberoptic Sensor Technology Handbook, co-authored and edited by published the this author, with an extensive Fiberoptic Sensors Glossary. In 1989, the handbook w...

  9. Fiber Optics: No Illusion.

    Science.gov (United States)

    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)

  10. Fiber optic gas sensor

    Science.gov (United States)

    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. Photonic Crystal Fibers

    National Research Council Canada - National Science Library

    Kristiansen, Rene E

    2005-01-01

    This report results from a contract tasking Crystal Fibre A/S as follows: Crystal Fibre will conduct research and development of large mode area, dual clad multi-core Yb-doped photonic crystal fiber...

  12. Fiber Laser Array

    National Research Council Canada - National Science Library

    Simpson, Thomas

    2002-01-01

    ...., field-dependent, loss within the coupled laser array. During this program, Jaycor focused on the construction and use of an experimental apparatus that can be used to investigate the coherent combination of an array of fiber lasers...

  13. Robust Fiber Coatings

    National Research Council Canada - National Science Library

    Goettler, Richard

    2002-01-01

    The highly desired ceramic matrix composite is the one in which the high strength and strain-to-failure is achieved through judicious selection of a fiber coating that can survive the high-temperature...

  14. Fiber Optic Bragg Gratings

    National Research Council Canada - National Science Library

    Battiato, James

    1998-01-01

    Coupled mode theory was used to model reflection fiber gratings. The effects of experimental parameters on grating characteristics were modeled for both uniform and non-uniform grating profiles using this approach...

  15. Cerenkov fiber sampling calorimeters

    International Nuclear Information System (INIS)

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

    1994-01-01

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

  16. Fiber optics welder

    Science.gov (United States)

    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.

  17. FIBER OPTIC LIGHTING SYSTEMS

    Directory of Open Access Journals (Sweden)

    Munir BATUR

    2013-01-01

    Full Text Available Recently there have been many important and valuable developments in the communication industry. The huge increase in the sound, data and visual communications has caused a parallel increase in the demand for systems with wider capacity, higher speed and higher quality. Communication systems that use light to transfer data are immensely increased. There have recently many systems in which glass or plastic fiber cables were developed for light wave to be transmitted from a source to a target place. Fiber optic systems, are nowadays widely used in energy transmission control systems, medicine, industry and lighting. The basics of the system is, movement of light from one point to another point in fiber cable with reflections. Fiber optic lighting systems are quite secure than other lighting systems and have flexibility for realizing many different designs. This situation makes fiber optics an alternative for other lighting systems. Fiber optic lighting systems usage is increasing day-by-day in our life. In this article, these systems are discussed in detail.

  18. Electrospun amplified fiber optics.

    Science.gov (United States)

    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.

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

    Science.gov (United States)

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

    2016-04-01

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

  20. Continuous Natural Fiber Reinforced Thermoplastic Composites by Fiber Surface Modification

    Directory of Open Access Journals (Sweden)

    Patcharat Wongsriraksa

    2013-01-01

    Full Text Available Continuous natural fiber reinforced thermoplastic materials are expected to replace inorganic fiber reinforced thermosetting materials. However, in the process of fabricating the composite, it is difficult to impregnate the thermoplastic resin into reinforcement fiber because of the high melt viscosity. Therefore, intermediate material, which allows high impregnation during molding, has been investigated for fabricating continuous fiber reinforced thermoplastic composite by aligning resin fiber alongside reinforcing fiber with braiding technique. This intermediate material has been called “microbraid yarn (MBY.” Moreover, it is well known that the interfacial properties between natural fiber and resin are low; therefore, surface treatment on continuous natural fiber was performed by using polyurethane (PU and flexible epoxy (FLEX to improve the interfacial properties. The effect of surface treatment on the mechanical properties of continuous natural fiber reinforced thermoplastic composites was examined. From these results, it was suggested that surface treatment by PU with low content could produce composites with better mechanical properties.

  1. Thulium fiber laser lithotripsy using a muzzle brake fiber tip

    Science.gov (United States)

    Hutchens, Thomas C.; Gonzalez, David A.; Irby, Pierce B.; Fried, Nathaniel M.

    2017-02-01

    The Thulium fiber laser (TFL) is being explored as an alternative to Holmium:YAG laser for lithotripsy. TFL beam profile allows coupling of higher power into smaller fibers than multimode Holmium laser beam, without proximal fiber tip degradation. A smaller fiber provides more space in ureteroscope working channel for increased saline irrigation and allows maximum ureteroscope flexion. However, distal fiber tip burnback increases as fiber diameter decreases. Previous studies utilizing hollow steel sheaths around recessed distal fiber tips reduced fiber burnback, but increased retropulsion. In this study, a "fiber muzzle brake" was tested for reducing fiber burnback and stone retropulsion. TFL lithotripsy studies were performed at 1908 nm, 35 mJ, 500 μs, and 300 Hz using a 100-μm-core fiber. The optimal stainless steel muzzle brake tip tested consisted of a 1-cm-long, 560-μm-OD, 360-μm-ID tube with 275-μm thru hole located 250-μm from the distal end. The fiber tip was recessed a distance of 500 μm. Stone phantom retropulsion, fiber tip burnback, and calcium oxalate stone ablation studies were performed, ex vivo. Small stones with a mass of 40 +/- 4 mg and 4-mm-diameter were ablated over a 1.5-mm sieve in 25 +/- 4 s (n=10), without distal fiber tip burnback. Reduction in stone phantom retropulsion distance by 50% and 85% was observed when using muzzle brake tips versus 100-μm-core bare fibers and hollow steel tip fibers. The muzzle brake fiber tip provided efficient stone ablation, reduced stone retropulsion, and minimal fiber degradation during TFL lithotripsy.

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

    Science.gov (United States)

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

    2017-12-01

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

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

    Science.gov (United States)

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

    2014-03-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-05-29

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

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

  6. Cellulosic Fibers: Effect of Processing on Fiber Bundle Strength

    DEFF Research Database (Denmark)

    Thygesen, Anders; Madsen, Bo; Thomsen, Anne Belinda

    2011-01-01

    A range of differently processed cellulosic fibers from flax and hemp plants were investigated to study the relation between processing of cellulosic fibers and fiber bundle strength. The studied processing methods are applied for yarn production and include retting, scutching, carding, and cotto......A range of differently processed cellulosic fibers from flax and hemp plants were investigated to study the relation between processing of cellulosic fibers and fiber bundle strength. The studied processing methods are applied for yarn production and include retting, scutching, carding...

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

    Science.gov (United States)

    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.

  8. Optical fiber stripper positioning apparatus

    Science.gov (United States)

    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.

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

    Directory of Open Access Journals (Sweden)

    Léa L. F. Costa

    2008-01-01

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

  10. Natural Fiber Composites: A Review

    Energy Technology Data Exchange (ETDEWEB)

    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.

  11. Enhanced radiation resistant fiber optics

    International Nuclear Information System (INIS)

    Lyons, P.B.; Looney, L.D.

    1993-01-01

    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

  12. Fiber-optic technology review

    International Nuclear Information System (INIS)

    Lyons, P.B.

    1980-01-01

    A history of fiber technology is presented. The advantages of fiber optics are discussed (bandwidth, cost, weight and size, nonmetallic construction and isolation). Some aspects of the disadvantages of fiber systems briefly discussed are fiber and cable availability, fiber components, radiation effects, receivers and transmitters, and material dispersion. Particular emphasis over the next several years will involve development of fibers and systems optimized for use at wavelengths near 1.3 μm and development of wavelengths multiplexers for simultaneous system operation at several wavelengths

  13. Enhanced radiation resistant fiber optics

    Science.gov (United States)

    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.

  14. Anisotropic elliptic optical fibers

    Science.gov (United States)

    Kang, Soon Ahm

    1991-05-01

    The exact characteristic equation for an anisotropic elliptic optical fiber is obtained for odd and even hybrid modes in terms of infinite determinants utilizing Mathieu and modified Mathieu functions. A simplified characteristic equation is obtained by applying the weakly guiding approximation such that the difference in the refractive indices of the core and the cladding is small. The simplified characteristic equation is used to compute the normalized guide wavelength for an elliptical fiber. When the anisotropic parameter is equal to unity, the results are compared with the previous research and they are in close agreement. For a fixed value normalized cross-section area or major axis, the normalized guide wavelength lambda/lambda(sub 0) for an anisotropic elliptic fiber is small for the larger value of anisotropy. This condition indicates that more energy is carried inside of the fiber. However, the geometry and anisotropy of the fiber have a smaller effect when the normalized cross-section area is very small or very large.

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

    Science.gov (United States)

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

    2017-04-15

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

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

    Science.gov (United States)

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

    2015-01-01

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

  17. Impact of Microbial Composition of Cambodian Traditional Dried Starters (Dombea on Flavor Compounds of Rice Wine: Combining Amplicon Sequencing With HP-SPME-GCMS

    Directory of Open Access Journals (Sweden)

    Sokny Ly

    2018-05-01

    Full Text Available Dombae is a traditional ferment starter which has been used for starchy based wine production in Cambodia. However, the production technology of rice wine in Cambodia is not optimized. The current study aimed to investigate the microbiota associated in five ferment starters and the effect of a traditional fermentation process using a metagenomics sequencing analysis and HS-SPME-GCMS for the characterization of the aromatic profiles at the end of fermentation. Most of bacteria identified in this study were lactic acid bacteria including Weissella cibaria, Pediococcus sp. MMZ60A, Lactobacillus fermentum, and Lactobacillus plantarum. Saccharomyces cerevisiae and Saccharomycopsis fibuligera were found to be abundant yeasts while the only amylolytic filamentous fungus was Rhizopus oryzae. A total of 25 aromatic compounds were detected and identified as esters, alcohols, acids, ketones and aldehydes. The alcohol group was dominant in each rice wine. Significant changes were observed at the level of microbial communities during fermentation, suggesting microbial succession for the assimilation of starch and subsequently assimilation of fermentation by-products leading to the production of flavor compounds. At this level, the presence of Weissella, Pediococcus, and Lactobacillus genus was strongly correlated with most of the flavor compounds detected.

  18. Impact of Microbial Composition of Cambodian Traditional Dried Starters (Dombea) on Flavor Compounds of Rice Wine: Combining Amplicon Sequencing With HP-SPME-GCMS

    Science.gov (United States)

    Ly, Sokny; Mith, Hasika; Tarayre, Cédric; Taminiau, Bernard; Daube, Georges; Fauconnier, Marie-Laure; Delvigne, Frank

    2018-01-01

    Dombae is a traditional ferment starter which has been used for starchy based wine production in Cambodia. However, the production technology of rice wine in Cambodia is not optimized. The current study aimed to investigate the microbiota associated in five ferment starters and the effect of a traditional fermentation process using a metagenomics sequencing analysis and HS-SPME-GCMS for the characterization of the aromatic profiles at the end of fermentation. Most of bacteria identified in this study were lactic acid bacteria including Weissella cibaria, Pediococcus sp. MMZ60A, Lactobacillus fermentum, and Lactobacillus plantarum. Saccharomyces cerevisiae and Saccharomycopsis fibuligera were found to be abundant yeasts while the only amylolytic filamentous fungus was Rhizopus oryzae. A total of 25 aromatic compounds were detected and identified as esters, alcohols, acids, ketones and aldehydes. The alcohol group was dominant in each rice wine. Significant changes were observed at the level of microbial communities during fermentation, suggesting microbial succession for the assimilation of starch and subsequently assimilation of fermentation by-products leading to the production of flavor compounds. At this level, the presence of Weissella, Pediococcus, and Lactobacillus genus was strongly correlated with most of the flavor compounds detected. PMID:29867806

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

    Science.gov (United States)

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

    2017-04-15

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

  20. Chemical composition analysis of the essential oil of Solanumn nigrum L. by HS/SPME method and calculation of the biochemical coefficients of the components

    Directory of Open Access Journals (Sweden)

    Avat (Arman Taherpour

    2017-05-01

    Full Text Available The volatile constituents of the essential oil of wild Solanumn nigrum L. obtained from the Kurdistan of Iraq were extracted by head-space/solid-phase micro-extraction (HS/SPME and were analyzed by gas chromatography (GC and gas chromatography/mass spectrometry (GC/MS. Of a total of twenty compounds in the oil, all of them were identified. The main components were as follows: Dillapiole (22.22%, α-Cadinol (16.47%, para-Cymene (10.01%, (E-1-(2,6,6-Trimethyl-1,3-cyclohexadien-1-yl-2-buten-1-one or β-damascenone (9.08%, α-Phellandrene (8.48%, β-Pinene (5.93%, α-Bisabolol acetate (4.53%, (Z,E-4,6,8-Megastigmatriene (4.09%, Phytol (2.49%, Linalyl butanoate (2.13%, 8-methylene-tricyclo[3.2.1.0(2,4]octane (2.60% and Limonene (2.03%. Some physicochemical properties, such as the logarithm of calculated octanol–water partitioning coefficients (logKow and total biodegradation (TBd in mol/h were calculated for compounds 1–20 from S. nigrum L.

  1. Raman spectroscopy, electronic microscopy and SPME-GC-MS to elucidate the mode of action of a new antimicrobial food packaging material.

    Science.gov (United States)

    Clemente, Isabel; Aznar, Margarita; Salafranca, Jesús; Nerín, Cristina

    2017-02-01

    One critical challenge when developing a new antimicrobial packaging material is to demonstrate the mode of action of the antimicrobials incorporated into the packaging. For this task, several analytical techniques as well as microbiology are required. In this work, the antimicrobial properties of benzyl isothiocyanate, allyl isothiocyanate and essential oils of cinnamon and oregano against several moulds and bacteria have been evaluated. Benzyl isothiocyanate showed the highest antimicrobial activity and it was selected for developing the new active packaging material. Scanning electron microscopy and Raman spectroscopy were successfully used to demonstrate the mode of action of benzyl isothiocyanate on Escherichia coli. Bacteria exhibited external modifications such as oval shape and the presence of septum surface, but they did not show any disruption or membrane damage. To provide data on the in vitro action of benzyl isothiocyanate and the presence of inhibition halos, the transfer mechanism to the cells was assessed using solid-phase microextraction-gas chromatography-mass spectrometry. Based on the transfer system, action mechanism and its stronger antimicrobial activity, benzyl isothiocyanate was incorporated to two kinds of antimicrobial labels. The labels were stable and active for 140 days against two mould producers of ochratoxin A; Penicillium verrucosum is more sensitive than Aspergillus ochraceus. Details about the analytical techniques and the results obtained are shown and discussed. Graphical Abstract Antimicrobial evaluation of pure compounds, incorporation in the packaging and study for mode of action on S. coli by Raman, SEM and SPME-GC-MS.

  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.

    Science.gov (United States)

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

    2016-08-01

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

  3. Non-destructive profiling of volatile organic compounds using HS-SPME/GC-MS and its application for the geographical discrimination of white rice.

    Science.gov (United States)

    Lim, Dong Kyu; Mo, Changyeun; Lee, Dong-Kyu; Long, Nguyen Phuoc; Lim, Jongguk; Kwon, Sung Won

    2018-01-01

    The authenticity determination of white rice is crucial to prevent deceptive origin labeling and dishonest trading. However, a non-destructive and comprehensive method for rapidly discriminating the geographical origins of white rice between countries is still lacking. In the current study, we developed a volatile organic compound based geographical discrimination method using headspace solid-phase microextraction coupled to gas chromatography-mass spectrometry (HS-SPME/GC-MS) to discriminate rice samples from Korea and China. A partial least squares discriminant analysis (PLS-DA) model exhibited a good classification of white rice between Korea and China (accuracy = 0.958, goodness of fit = 0.937, goodness of prediction = 0.831, and permutation test p-value = 0.043). Combining the PLS-DA based feature selection with the differentially expressed features from the unpaired t-test and significance analysis of microarrays, 12 discriminatory biomarkers were found. Among them, hexanal and 1-hexanol have been previously known to be associated with the cultivation environment and storage conditions. Other hydrocarbon biomarkers are novel, and their impact on rice production and storage remains to be elucidated. In conclusion, our findings highlight the ability to rapidly discriminate white rice from Korea and China. The developed method maybe useful for the authenticity and quality control of white rice. Copyright © 2017. Published by Elsevier B.V.

  4. Aroma volatiles obtained at harvest by HS-SPME/GC-MS and INDEX/MS-E-nose fingerprint discriminate climacteric behaviour in melon fruit.

    Science.gov (United States)

    Chaparro-Torres, Libia A; Bueso, María C; Fernández-Trujillo, Juan P

    2016-05-01

    Melon aroma volatiles were extracted at harvest from juice of a climacteric near-isogenic line (NIL) SC3-5-1 with two quantitative trait loci (QTLs) introgressed which produced climacteric behaviour and its non-climacteric parental (PS) using two methodologies of analysis: static headspace solid phase micro-extraction (HS-SPME) by gas chromatography-mass spectrometry (GC-MS) and inside needle dynamic extraction (INDEX) by MS-based electronic nose (MS-E-nose). Of the 137 volatiles compounds identified, most were found at significantly higher concentrations in SC3-5-1 than in PS in both seasons. These volatiles were mostly esters, alcohols, sulfur-derived esters and even some aldehydes and others. The number of variables with high correlation values was reduced by using correlation network analysis. Partial least squares-discriminant analysis (PLS-DA) achieved the correct classification of PS and SC3-5-1. The ions m/z 74, 91, 104, 105, 106 and 108, mainly volatile derivatives precursor phenylalanine, were the most discriminant in SC3-5-1 and PS. As many as 104 QTLs were mapped in season 1 and at least 78 QTLs in each season with an effect above the PS mean. GC-MS gave better discrimination than E-nose. Most of the QTLs that mapped in both seasons enhanced aroma volatiles associated with climacteric behaviour. © 2015 Society of Chemical Industry.

  5. Determination of Hazardous VOCs and Nicotine Released from Mainstream Smoke by the Combination of the SPME and GC-MS Methods

    Directory of Open Access Journals (Sweden)

    Sudhir Kumar Pandey

    2010-01-01

    Full Text Available In this study, the contents of nicotine and volatile organic compounds (VOCs in mainstream smoke (MSS were analyzed using samples of four cigarette types consisting of two common brands (R and E with full (F and light (L flavor, coded with R-F, R-L, E-F, and E-L. These cigarettes were also analyzed after removing the filter portions with the assignment of a new sample code of (N as the third letter (e.g., R-L-N. A total of 44 VOCs (including nicotine were quantified by the combination of the SPME and GC-MS methods. Out of the 44 VOCs, 10 were identified as hazardous air pollutants listed by the U.S. EPA, while their concentrations exceeded the reference exposure limits set by various agencies. A clear distinction was apparent in the concentration levels of VOCs between different brands or between full and light flavors. Nicotine concentrations varied greatly between different cigarettes types of the R brand, whereas such changes were insignificant in the counterpart E brand. This thus suggests that light-flavor cigarettes do not necessarily guarantee low doses of carcinogens (and tar than regular cigarettes, as their differences can be balanced by the inhaling behavior of the smoker.

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

    Science.gov (United States)

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

    2016-05-25

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

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

    Science.gov (United States)

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

    2016-04-01

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

  8. Study of aroma formation and transformation during the manufacturing process of Biluochun green tea in Yunnan Province by HS-SPME and GC-MS.

    Science.gov (United States)

    Wang, Chen; Lv, Shidong; Wu, Yuanshuang; Lian, Ming; Gao, Xuemei; Meng, Qingxiong

    2016-10-01

    Biluochun is a typical non-fermented tea and is also famous for its unique aroma in China. Few studies have been performed to evaluate the effect of the manufacturing process on the formation and content of its aroma. The volatile components were extracted at different manufacturing process steps of Biluochun green tea using fully automated headspace solid-phase microextraction (HS-SPME) and further characterised by gas chromatography-mass spectrometry (GC-MS). Among 67 volatile components collected, the fractions of linalool oxides, β-ionone, phenylacetaldehyde, aldehydes, ketones, and nitrogen compounds were increased while alcohols and hydrocarbons declined during the manufacturing process. The aroma compounds decreased the most during the drying steps. We identified a number of significantly changed components that can be used as markers and quality control during the producing process of Biluochun. The drying step played a major role in the aroma formation of green tea products and should be the most important step for quality control. © 2016 Society of Chemical Industry. © 2016 Society of Chemical Industry.

  9. Non-destructive profiling of volatile organic compounds using HS-SPME/GC–MS and its application for the geographical discrimination of white rice

    Directory of Open Access Journals (Sweden)

    Dong Kyu Lim

    2018-01-01

    Full Text Available The authenticity determination of white rice is crucial to prevent deceptive origin labeling and dishonest trading. However, a non-destructive and comprehensive method for rapidly discriminating the geographical origins of white rice between countries is still lacking. In the current study, we developed a volatile organic compound based geographical discrimination method using headspace solid-phase microextraction coupled to gas chromatography–mass spectrometry (HS-SPME/GC–MS to discriminate rice samples from Korea and China. A partial least squares discriminant analysis (PLS-DA model exhibited a good classification of white rice between Korea and China (accuracy = 0.958, goodness of fit = 0.937, goodness of prediction = 0.831, and permutation test p-value = 0.043. Combining the PLS-DA based feature selection with the differentially expressed features from the unpaired t-test and significance analysis of microarrays, 12 discriminatory biomarkers were found. Among them, hexanal and 1-hexanol have been previously known to be associated with the cultivation environment and storage conditions. Other hydrocarbon biomarkers are novel, and their impact on rice production and storage remains to be elucidated. In conclusion, our findings highlight the ability to rapidly discriminate white rice from Korea and China. The developed method maybe useful for the authenticity and quality control of white rice.

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

    Science.gov (United States)

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

    2018-03-01

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

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

    Science.gov (United States)

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

    2004-12-15

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

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

    Science.gov (United States)

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

    2011-04-01

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

  13. Hybrid Fiber Layup and Fiber-Reinforced Polymeric Composites Produced Therefrom

    Science.gov (United States)

    Barnell, Thomas J. (Inventor); Garrigan, Sean P. (Inventor); Rauscher, Michael D. (Inventor); Dietsch, Benjamin A. (Inventor); Cupp, Gary N. (Inventor)

    2018-01-01

    Embodiments of a hybrid fiber layup used to form a fiber-reinforced polymeric composite, and a fiber-reinforced polymeric composite produced therefrom are disclosed. The hybrid fiber layup comprises one or more dry fiber strips and one or more prepreg fiber strips arranged side by side within each layer, wherein the prepreg fiber strips comprise fiber material impregnated with polymer resin and the dry fiber strips comprise fiber material without impregnated polymer resin.

  14. Graphene fiber: a new trend in carbon fibers

    OpenAIRE

    Zhen Xu; Chao Gao

    2015-01-01

    New fibers with increased strength and rich functionalities have been untiringly pursued by materials researchers. In recent years, graphene fiber has arisen as a new carbonaceous fiber with high expectations in terms of mechanical and functional performance. In this review, we elucidated the concept of sprouted graphene fibers, including strategies for their fabrication and their basic structural attributes. We examine the rapid advances in the promotion of mechanical/functional properties o...

  15. Optical fiber switch

    Science.gov (United States)

    Early, James W.; Lester, Charles S.

    2002-01-01

    Optical fiber switches operated by electrical activation of at least one laser light modulator through which laser light is directed into at least one polarizer are used for the sequential transport of laser light from a single laser into a plurality of optical fibers. In one embodiment of the invention, laser light from a single excitation laser is sequentially transported to a plurality of optical fibers which in turn transport the laser light to separate individual remotely located laser fuel ignitors. The invention can be operated electro-optically with no need for any mechanical or moving parts, or, alternatively, can be operated electro-mechanically. The invention can be used to switch either pulsed or continuous wave laser light.

  16. Fiber Optic Calorimetry

    International Nuclear Information System (INIS)

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

    1997-01-01

    A twin-bridge calorimeter using optical fiber as the sensor element was constructed and tested. This system demonstrates the principle and capability of using 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 (microrad) 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% 240 Pu). The system noise base was about 0.2 rad, equivalent to about 1 mg of plutonium

  17. Femtosecond Fiber Lasers

    Science.gov (United States)

    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

  18. Higher Order Mode Fibers

    DEFF Research Database (Denmark)

    Israelsen, Stine Møller

    This PhD thesis considers higher order modes (HOMs) in optical fibers. That includes their excitation and characteristics. Within the last decades, HOMs have been applied both for space multiplexing in optical communications, group velocity dispersion management and sensing among others......-radial polarization as opposed to the linear polarization of the LP0X modes. The effect is investigated numerically in a double cladding fiber with an outer aircladding using a full vectorial modesolver. Experimentally, the bowtie modes are excited using a long period grating and their free space characteristics...... and polarization state are investigated. For this fiber, the onset of the bowtie effect is shown numerically to be LP011. The characteristics usually associated with Bessel-likes modes such as long diffraction free length and selfhealing are shown to be conserved despite the lack of azimuthal symmetry...

  19. Fiber optic calorimetry

    International Nuclear Information System (INIS)

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

    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 optical fibers 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 microrad 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 rad of phase shift per mW of thermal power. One milliwatt of thermal power is equivalent to 400 mg of plutonium (6% 240 Pu). The system noise base was about 0.2 rad, equivalent to about 1 mg of plutonium

  20. Fiber optic calorimetry

    International Nuclear Information System (INIS)

    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 (μrad) 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% 240 Pu). The system noise base was about 0.2 rad, equivalent to about 1 mg of plutonium

  1. Multibeam fiber laser cutting

    DEFF Research Database (Denmark)

    Olsen, Flemming Ove; Hansen, Klaus Schütt; Nielsen, Jakob Skov

    2009-01-01

    The appearance of the high power high brilliance fiber laser has opened for new possibilities in laser materials processing. In laser cutting this laser has demonstrated high cutting performance compared to the dominating Cutting laser, the CO2 laser. However, quality problems in fiber......-laser cutting have until now limited its application to metal cutting. In this paper the first results of proof-of-principle Studies applying a new approach (patent pending) for laser cutting with high brightness and short wavelength lasers will be presented. In the approach, multibeam patterns are applied...... to control the melt flow out of the cut kerf resulting in improved cut quality in metal cutting. The beam patterns in this study are created by splitting up beams from two single mode fiber lasers and combining these beams into a pattern in the cut kerf. The results are obtained with a total of 550 W...

  2. Monolithic Yb-fiber femtosecond laser using photonic crystal fiber

    DEFF Research Database (Denmark)

    Liu, Xiaomin; Lægsgaard, Jesper; Turchinovich, Dmitry

    2008-01-01

    We demonstrate, both experimentally and theoretically, an environmentally stable monolithic all-PM modelocked femtosecond Yb-fiber laser, with laser output pulse compressed in a spliced-on low-loss hollow-core photonic crystal fiber. Our laser provides direct fiber-end delivery of 4 nJ pulses...

  3. K3-fibered Calabi-Yau threefolds II, singular fibers

    OpenAIRE

    Hunt, Bruce

    1999-01-01

    In part I of this paper we constructed certain fibered Calabi-Yaus by a quotient construction in the context of weighted hypersurfaces. In this paper look at the case of K3 fibrations more closely and study the singular fibers which occur. This differs from previous work since the fibrations we discuss have constant modulus, and the singular fibers have torsion monodromy.

  4. Single fiber pullout from hybrid fiber reinforced concrete

    NARCIS (Netherlands)

    Markovich, I.; Van Mier, J.G.M.; Walraven, J.C.

    2001-01-01

    Hybrid fiber reinforcement can be very efficient for improving the tensile response of the composite. In such materials, fibers of different geometries can act as bridging mechanisms over cracks of different widths. The fiber bridging efficiency depends on the interface properties, which makes

  5. Fluoride glass fiber optics

    CERN Document Server

    Aggarwal, Ishwar D

    1991-01-01

    Fluoride Glass Fiber Optics reviews the fundamental aspects of fluoride glasses. This book is divided into nine chapters. Chapter 1 discusses the wide range of fluoride glasses with an emphasis on fluorozirconate-based compositions. The structure of simple fluoride systems, such as BaF2 binary glass is elaborated in Chapter 2. The third chapter covers the intrinsic transparency of fluoride glasses from the UV to the IR, with particular emphasis on the multiphonon edge and electronic edge. The next three chapters are devoted to ultra-low loss optical fibers, reviewing methods for purifying and

  6. Nonlinear fiber optics

    CERN Document Server

    Agrawal, Govind

    2012-01-01

    Since the 4e appeared, a fast evolution of the field has occurred. The 5e of this classic work provides an up-to-date account of the nonlinear phenomena occurring inside optical fibers, the basis of all our telecommunications infastructure as well as being used in the medical field. Reflecting the big developments in research, this new edition includes major new content: slow light effects, which offers a reduction in noise and power consumption and more ordered network traffic-stimulated Brillouin scattering; vectorial treatment of highly nonlinear fibers; and a brand new chapter o

  7. Silicon photonics for multicore fiber communication

    DEFF Research Database (Denmark)

    Ding, Yunhong; Kamchevska, Valerija; Dalgaard, Kjeld

    2016-01-01

    We review our recent work on silicon photonics for multicore fiber communication, including multicore fiber fan-in/fan-out, multicore fiber switches towards reconfigurable optical add/drop multiplexers. We also present multicore fiber based quantum communication using silicon devices.......We review our recent work on silicon photonics for multicore fiber communication, including multicore fiber fan-in/fan-out, multicore fiber switches towards reconfigurable optical add/drop multiplexers. We also present multicore fiber based quantum communication using silicon devices....

  8. Fiber-optic seismic sensor

    International Nuclear Information System (INIS)

    Finch, G. W.; Udd, E.

    1985-01-01

    A vibration sensor is constructed by providing two preferably matched coils of fiber-optic material. When the sensor experiences vibration, a differential pressure is exerted on the two fiber coils. The differential pressure results in a variation in the relative optical path lengths between the two fibers so that light beams transmitted through the two fibers are differently delayed, the phase difference therebetween being a detectable indication of the vibration applied to the sensor

  9. Tunable femtosecond Cherenkov fiber laser

    DEFF Research Database (Denmark)

    Liu, Xiaomin; Svane, Ask Sebastian; Lægsgaard, Jesper

    2014-01-01

    We demonstrate electrically-tunable femtosecond Cherenkov fiber laser output at the visible range. Using an all-fiber, self-starting femtosecond Yb-doped fiber laser as the pump source and nonlinear photonic crystal fiber link as the wave-conversion medium, ultrafast, milliwatt-level, tunable...... and spectral isolated Cherenkov radiation at visible wavelengths are reported. Such a femtosecond Cherenkov laser source is promising for practical biophotonics applications....

  10. 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

    Science.gov (United States)

    Eganhouse, Robert P.; DiFilippo, Erica L

    2015-01-01

    A method is described for determination of ten DDT-related compounds in marine pore water based on equilibrium solid-phase microextraction (SPME) using commercial polydimethylsiloxane-coated optical fiber with analysis by automated thermal desorption-gas chromatography/mass spectrometry (TD-GC/MS). Thermally cleaned fiber was directly exposed to sediments and allowed to reach equilibrium under static conditions at the in situ field temperature. Following removal, fibers were rinsed, dried and cut into appropriate lengths for storage in leak-tight containers at -20°C. Analysis by TD-GC/MS under full scan (FS) and selected ion monitoring (SIM) modes was then performed. Pore-water method detection limits in FS and SIM modes were estimated at 0.05-2.4ng/L and 0.7-16pg/L, respectively. Precision of the method, including contributions from fiber handling, was less than 10%. Analysis of independently prepared solutions containing eight DDT compounds yielded concentrations that were within 6.9±5.5% and 0.1±14% of the actual concentrations in FS and SIM modes, respectively. The use of optical fiber with automated analysis allows for studies at high temporal and/or spatial resolution as well as for monitoring programs over large spatial and/or long temporal scales with adequate sample replication. This greatly enhances the flexibility of the technique and improves the ability to meet quality control objectives at significantly lower cost.

  11. A silica fiber coated with a ZnO-graphene oxide nanocomposite with high specific surface for use in solid phase microextraction of the antiepileptic drugs diazepam and oxazepam.

    Science.gov (United States)

    Alizadeh, Reza; Salami, Maryam; Seidi, Shahram

    2018-06-02

    A novel ZnO-graphene oxide nanocomposite was prepared and is shown to be a viable coating on fused silica fibers for use in solid phase microextraction (SPME) of diazepam and oxazepam from urine, this followed by thermal desorption and gas chromatographic quantitation using a flame ionization detector. A central composite design was used to optimize extraction time, salt percentage, sample pH and desorption time. Limits of detection are 0.5 μg·L -1 for diazepam and 1.0 μg·L -1 for oxazepam. Repeatability and reproducibility for one fiber (n = 4), expressed as the relative standard deviation at a concentration of 50 μg·L -1 , are 8.3 and 11.3% for diazepam, and 6.7 and 10.1% for oxazepam. The fiber-to-fiber reproducibility is Graphical abstract A hydrothermal method was introduced for preparation of ZnO- GO nano composite on a fused silica fiber as solid phase microextraction with high mechanical, chemical stability and long service life.

  12. In-fiber integrated Michelson interferometer.

    Science.gov (United States)

    Yuan, Libo; Yang, Jun; Liu, Zhihai; Sun, Jiaxing

    2006-09-15

    A novel fiber-optic in-fiber integrated Michelson interferometer has been proposed and demonstrated. It consists of a segment of two-core fiber with a mirrored fiber end. The sensing characteristics based on the two-core fiber bending, corresponding to the shift of the phase of the two-core in-fiber integrated Michelson interferometer, are investigated.

  13. Transient attenuation in optical fibers

    International Nuclear Information System (INIS)

    Hopkins, A.A.; Kelly, R.E.; Looney, L.D.; Lyons, P.B.

    1984-01-01

    Low and high energy pulsed electron beams were used to generate radiation-induced transient attenuation in high-OH, Suprasil core, PCS fibers, demonstrating the energy dependence of the radiation damage and recovery mechanisms. A radiation resistant low-OH fiber was studied and its performance contrasted to that of high-OH materials. Several fibers with differing core compositions were also studied

  14. Fiber Optics and Library Technology.

    Science.gov (United States)

    Koenig, Michael

    1984-01-01

    This article examines fiber optic technology, explains some of the key terminology, and speculates about the way fiber optics will change our world. Applications of fiber optics to library systems in three major areas--linkage of a number of mainframe computers, local area networks, and main trunk communications--are highlighted. (EJS)

  15. Water-core Fresnel fiber

    NARCIS (Netherlands)

    Martelli, C.; Canning, J.; Lyytikainen, K.; Groothoff, N.

    2005-01-01

    A water core photonic crystal Fresnel fiber exploiting a hole distribution on zone plates of a cylindrical waveguide was developed and characterized. This fiber has similar guiding properties as the pristine air-hole guiding fiber although a large loss edge ~900nm is observed indicating that the

  16. Optical fibers for FTTH application

    Science.gov (United States)

    Guzowski, Bartlomiej; Tosik, Grzegorz; Lisik, Zbigniew; Bedyk, Michal; Kubiak, Andrzej

    2013-07-01

    In this paper the specifics of FTTH (Fiber To The Home) networks in terms of requirements for optical fibers has been presented. Optical fiber samples used in FTTH applications acquired from the worldwide leading manufacturers were subjected to small diameter mandrel wraps tests. The detailed procedures of performed tests and the measurement results has been presented.

  17. Photonic-crystal fibers gyroscope

    Directory of Open Access Journals (Sweden)

    Ali Muse Haider

    2015-01-01

    Full Text Available In this paper we proposed to use of a photonic crystal fiber with an inner hollow defect. The use of such fibers is not affected by a material medium on the propagation of optical radiation. Photonic crystal fibers present special properties and capabilities that lead to an outstanding potential for sensing applications

  18. Thermal properties of Fiber ropes

    DEFF Research Database (Denmark)

    Bossolini, Elena; Nielsen, Ole Wennerberg; Oland, Espen

    There is a trend within the oil and gas market to shift from steel wire ropes to fiber ropes for lifting, hoisting and mooring applications. The cost of fiber ropes is about 2-3 times that of steel wire ropes, but the natural buoyancy of fiber ropes reduces the overall weight resulting in smaller...

  19. Shedding Light on Fiber Optics.

    Science.gov (United States)

    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)

  20. Fabrication of Optical Fiber Devices

    Science.gov (United States)

    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.

  1. Microstructured Fibers: Design and Applications

    DEFF Research Database (Denmark)

    Bjarklev, Anders Overgaard; Broeng, Jes

    2006-01-01

    Holey fibers, in which airholes are introduced in the cladding region and extended in the axial direction of the fiber, have been known since the early days of silica waveguide research. Early work demonstrated the first low-loss fibers, which featured very small silica cores held in air by thin...

  2. Illustrative white matter fiber bundles

    NARCIS (Netherlands)

    Otten, R.J.G.; Vilanova, A.; Wetering, van de H.M.M.

    2010-01-01

    Diffusion Tensor Imaging (DTI) has made feasible the visualization of the fibrous structure of the brain whitematter. In the last decades, several fiber-tracking methods have been developed to reconstruct the fiber tracts fromDTI data. Usually these fiber tracts are shown individually based on some

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

    NARCIS (Netherlands)

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

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

  4. Bluebonnet Fiber Collages

    Science.gov (United States)

    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…

  5. The dentate mossy fibers

    DEFF Research Database (Denmark)

    Blaabjerg, Morten; Zimmer, Jens

    2007-01-01

    Hippocampal mossy fibers are the axons of the dentate granule cells and project to hippocampal CA3 pyramidal cells and mossy cells of the dentate hilus (CA4) as well as a number of interneurons in the two areas. Besides their role in hippocampal function, studies of which are still evolving...

  6. Optical Fiber Protection

    Science.gov (United States)

    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

  7. Optical Fiber Spectroscopy

    Science.gov (United States)

    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.

  8. Fiber and Your Child

    Science.gov (United States)

    ... meals instead of white rice. Add beans (kidney, black, navy, and pinto) to rice dishes for even more fiber. Spice up salads with berries and almonds, chickpeas, artichoke hearts, and beans (kidney, black, navy, or pinto). Use whole-grain (corn or ...

  9. Polymer-Derived Ceramic Fibers

    Science.gov (United States)

    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.

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

    Directory of Open Access Journals (Sweden)

    DENILES DEL CARMEN DE ARCO R

    2011-12-01

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

  11. Improved Optical Fiber Chemical Sensors

    Science.gov (United States)

    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.

  12. Solid fiber Z-pinches

    International Nuclear Information System (INIS)

    Lindemuth, I.R.

    1989-01-01

    One- and two-dimensional magnetohydrodynamic computations have been performed to study the behavior of solid deuterium fiber Z-pinch experiments performed at Los Alamos and the Naval Research Laboratory. The computations use a tabulated atomic data base and ''cold-start'' initial conditions. The computations predict that the solid fiber persists longer in existing experiments than previously expected and that the discharge actually consists of a relatively low-density, hot plasma which has been ablated from the fiber. The computations exhibit m = 0 behavior in the hot, exterior plasma prior to complete ablation of the solid fiber. The m = 0 behavior enhances the fiber ablation rate. 10 refs., 5 figs

  13. Introduction to optical fiber sensors

    International Nuclear Information System (INIS)

    Moukdad, S.

    1991-01-01

    Optical fiber sensors have many advantages over other types of sensors, for example: Low weight, immunity from EMI, electrical isolation, chemical passivity, and high sensitivity. In this seminar, a brief explanation of the optical fiber sensors, their use, and their advantages will be given. After, a description of the main optical fiber sensor components will be presented. Principles of some kinds of optical fiber sensors will be presented, and the principle of the fiber-optic rotation sensor and its realization will be discussed in some details, as well as its main applications. (author). 5 refs, 8 figs, 2 tabs

  14. (E-2-Nonenal determination in brazilian beers using headspace solid-phase microextraction and gas chromatographic coupled mass spectrometry (HS-SPME-GC-MS Determinação de (E-2-nonenal em cervejas brasileiras utilizando microextração em fase sólida do headspace e cromatografia gasosa acoplada a espectrometria de massas

    Directory of Open Access Journals (Sweden)

    Rodrigo Scherer

    2010-05-01

    Full Text Available (E-2-nonenal is considered an important off-flavor of beer, related to the flavor of beer staling. In this study, a new method for determination of (E-2-nonenal in beer using headspace solid-phase microextraction and gas chromatographic coupled mass spectrometry (HS-SPME-GC-MS was developed and applied in Brazilian beer samples. The extractions were carried out in CAR-PDMS (carboxen-polydimethylsiloxane fiber and the best results were found with 15 minutes of equilibrium and 90 minutes of extraction at 50 °C. The method was linear in the range from 0.02 to 4.0 μg.L-1 with correlation coefficient of 0.9994. The limits of detection and quantification were 0.01 and 0.02 μg.L-1, respectively. 96.5% of recovery and 4% precision (RSD were obtained in the fortification of beer samples with 2.0 μg.L-1 of (E-2-nonenal. The developed method proved to be simple, efficient and highly sensitive to the determination of this analyte being easily applied in the quality control of the brewery. (E-2-nonenal was found in all beer samples analyzed with levels between 0.17 and 0.42 μg.L-1.O (E-2-nonenal é considerado um importante off-flavor da cerveja, sendo relacionado ao sabor de cerveja envelhecida. Neste estudo, um novo método para determinação de (E-2-nonenal em cerveja usando microextração em fase sólida do headspace e cromatografia a gás acoplada à espectrometria de massa (HS-SPME-GC-MS foi desenvolvido e aplicado em amostras de cerveja brasileira. As extrações foram realizadas utilizando a fibra CAR/PDMS (carboxen/polidimetilsiloxano, com 15 minutos de tempo de equilíbrio e 90 minutos de exposição da fibra a 50 °C. O método foi linear na faixa de 0,02 e 4,0 μg.L-1, com coeficiente de correlação de 0,9994. Os limites de detecção e quantificação foram 0,01 e 0,02 μg.L-1, respectivamente. Foram obtidos 96,5% de recuperação e 4% de variação entre replicatas de amostras de cerveja fortificadas com 2,0 μg.L-1 de (E-2-nonenal. O m

  15. Bonding Properties of Basalt Fiber and Strength Reduction According to Fiber Orientation

    OpenAIRE

    Choi, Jeong-Il; Lee, Bang

    2015-01-01

    The basalt fiber is a promising reinforcing fiber because it has a relatively higher tensile strength and a density similar to that of a concrete matrix as well as no corrosion possibility. This study investigated experimentally the bonding properties of basalt fiber with cementitious material as well as the effect of fiber orientation on the tensile strength of basalt fiber for evaluating basalt fiber?s suitability as a reinforcing fiber. Single fiber pullout tests were performed and then th...

  16. Fiber optics: A brief introduction

    International Nuclear Information System (INIS)

    Gruchalla, M.E.

    1989-01-01

    A basic introduction into the principles of fiber optics is presented. A review of both the underlying physical principles and the individual elements of typical fiber-optic systems are presented. The optical phenomenon of total internal reflection is reviewed. The basic construction of the optical fiber is presented. Both step-index and graded-index fiber designs are reviewed. Multimode and single-mode fiber constructions are considered and typical performance parameters given. Typical optical-fiber bandwidth and loss characteristics are compared to various common coaxial cables, waveguides, and air transmission. The constructions of optical-fiber cables are reviewed. Both loose-tube and tightly-buffered designs are considered. Several optical connection approaches are presented. Photographs of several representative optical connectors are included. Light Emitting Diode and Laser Diode emitters for fiber-optic applications are reviewed, and some advantages and shortcomings of each are considered. The phenomenon of modal noise is briefly explained. Both PIN and Avalanche photodetectors are reviewed and their performance parameters compared. Methods of data transmission over optical fiber are introduced. Principles of Wavelength, Frequency, and Time Division Multiplexing are briefly presented. The technology of fiber-optic sensors is briefly reviewed with basic principles introduced. The performance of a fiber-optic strain sensor is included as a practical example. 7 refs., 10 figs

  17. All-Fiber Raman Probe

    DEFF Research Database (Denmark)

    Brunetti, Anna Chiara

    by means of fiber components. Assuming the possibility to use a fiber laser with a fundamental radiation at 1064nm, in-fiber efficient second harmonic generation is achieved by optically poling the core of the waveguide delivering the excitation light to the sample. In this way, Raman spectroscopy...... in the visible range can be performed. The simultaneous delivery of the excitation light and collection of the Raman signal from the sample are achieved by means of a doubleclad fiber, whose core and inner cladding act as \\independent" transmission channels. A double-clad fiber coupler allows for the recovery...... of the collected Raman scattering from the inner-cladding region of the double-clad fiber, thus replacing the bulk dichroic component normally used to demultiplex the pump and Raman signal. A tunable Rayleigh-rejection filter based on a liquid filled-photonic bandgap fiber is also demonstrated in this work...

  18. Determination of Volatile Organic Compounds (VOCs from Wrapping Films and Wrapped PDO Italian Cheeses by Using HS-SPME and GC/MS

    Directory of Open Access Journals (Sweden)

    Sara Panseri

    2014-06-01

    Full Text Available 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.

  19. Determination of Selected Aromas in Marquette and Frontenac Wine Using Headspace-SPME Coupled with GC-MS and Simultaneous Olfactometry

    Directory of Open Access Journals (Sweden)

    Somchai Rice

    2018-03-01

    Full Text Available Understanding the aroma profile of wines made from cold climate grapes is needed to help winemakers produce quality aromatic wines. The current study aimed to add to the very limited knowledge of aroma-imparting compounds in wines made from the lesser-known Frontenac and Marquette cultivars. Headspace solid-phase microextraction (SPME and gas chromatography-mass spectrometry (GC-MS with simultaneous olfactometry was used to identify and quantify selected, aroma-imparting volatile organic compounds (VOC in wines made from grapes harvested at two sugar levels (22° Brix and 24° Brix. Aroma-imparting compounds were determined by aroma dilution analysis (ADA. Odor activity values (OAV were also used to aid the selection of aroma-imparting compounds. Principal component analysis and hierarchical clustering analysis indicated that VOCs in wines produced from both sugar levels of Marquette grapes are similar to each other, and more similar to wines produced from Frontenac grapes harvested at 24° Brix. Selected key aroma compounds in Frontenac and Marquette wines were ethyl hexanoate, ethyl isobutyrate, ethyl octanoate, and ethyl butyrate. OAVs >1000 were reported for three aroma compounds that impart fruity aromas to the wines. This study provides evidence that aroma profiles in Frontenac wines can be influenced by timing of harvesting the berries at different Brix. Future research should focus on whether this is because of berry development or accumulation of aroma precursors and sugar due to late summer dehydration. Simultaneous chemical and sensory analyses can be useful for the understanding development of aroma profile perceptions for wines produced from cold-climate grapes.

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

    Directory of Open Access Journals (Sweden)

    Lourdes García-Vico

    2017-01-01

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

  1. Identification of Volatile Components of Liverwort (Porella cordaeana Extracts Using GC/MS-SPME and Their Antimicrobial Activity

    Directory of Open Access Journals (Sweden)

    Maria Elisabetta Guerzoni

    2012-06-01

    Full Text Available Chemical constituents of liverwort (Porella cordaeana extracts have been identified using solid-phase microextraction-gas chromatography mass spectrometry (SPME-GC/MS. The methanol, ethanol and ethyl acetate extracts were rich in terpenoids such as sesquiterpene hydrocarbons (53.12%, 51.68%, 23.16%, and monoterpene hydrocarbons (22.83%, 18.90%, 23.36%, respectively. The dominant compounds in the extracts were β-phellandrene (15.54%, 13.66%, 12.10% and β-caryophyllene (10.72%, 8.29%, 7.79%, respectively. The antimicrobial activity of the extracts was evaluated against eleven food microorganisms using the microdilution and disc diffusion methods. The minimum inhibitory concentration (MIC varied from 0.50 to 2.00 mg/mL for yeast strains (Saccharomyces cerevisiae 635, Zygosacharomyces bailii 45, Aerobasidium pullulans L6F, Pichia membranaefaciens OC 71, Pichia membranaefaciens OC 70, Pichia anomala CBS 5759, Pichia anomala DBVPG 3003 and Yarrowia lipolytica RO13, and from 1.00 to 3.00 mg/mL for bacterial strains (Salmonella enteritidis 155, Escherichia coli 555 and Listeria monocytogenes 56Ly. Methanol extract showed better activity in comparison with ethanol and ethyl acetate extracts. High percentages of monoterpene and sesquiterpene hydrocarbons could be responsible for the better antimicrobial activity.

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

    Directory of Open Access Journals (Sweden)

    Shidong Lv

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

    Science.gov (United States)

    Goryński, Krzysztof; Kiedrowicz, Alicja; Bojko, Barbara

    2016-08-05

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

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

    Science.gov (United States)

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

    2017-01-14

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

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

    Science.gov (United States)

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

    2008-05-01

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

  6. Volatile compound changes during shelf life of dried Boletus edulis: comparison between SPME-GC-MS and PTR-ToF-MS analysis.

    Science.gov (United States)

    Aprea, Eugenio; Romano, Andrea; Betta, Emanuela; Biasioli, Franco; Cappellin, Luca; Fanti, Marco; Gasperi, Flavia

    2015-01-01

    Drying process is commonly used to allow long time storage of valuable porcini mushrooms (Boletus edulis). Although considered a stable product dried porcini flavour changes during storage. Monitoring of volatile compounds during shelf life may help to understand the nature of the observed changes. In the present work two mass spectrometric techniques were used to monitor the evolution of volatile compounds during commercial shelf life of dried porcini. Solid phase microextraction (SPME) coupled to gas chromatography - mass spectrometry (GC-MS) allowed the identification of 66 volatile compounds, 36 of which reported for the first time, monitored during the commercial shelf life of dried porcini. Proton transfer reaction - time of flight - mass spectrometry (PTR-ToF-MS) , a direct injection mass spectrometric technique, was shown to be a fast and sensitive instrument for the general monitoring of volatile compound evolution during storage of dried porcini. Furthermore, PTR-ToF-MS grants access to compounds whose determination would otherwise require lengthy pre-concentration and/or derivatization steps such as ammonia and small volatile amines. The two techniques, both used for the first time to study dried porcini, provided detailed description of time evolution of volatile compounds during shelf life. Alcohols, aldehydes, ketones and monoterpenes diminish during the storage while carboxylic acids, pyrazines, lactones and amines increase. The storage temperature modifies the rate of the observed changes influencing the final quality of the dried porcini. We showed the advantages of both techniques, suggesting a strategy to be adopted to follow time evolution of volatile compounds in food products during shelf life, based on the identification of compounds by GC-MS and the rapid time monitoring by PTR-ToF-MS measurements in order to maximize the advantages of both techniques. Copyright © 2015 John Wiley & Sons, Ltd.

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

    Science.gov (United States)

    Aguilar-Cisneros, Blanca O; López, Mercedes G; Richling, Elke; Heckel, Frank; Schreier, Peter

    2002-12-18

    By use of headspace SPME sampling and a PLOT column, on-line capillary gas chromatography-isotope ratio mass spectrometry was employed in the combustion (C) and the pyrolysis (P) modes (HRGC-C/P-IRMS) to determine the delta(13)C(VPDB) and delta(18)O(VSMOW) values of ethanol in authentic (n = 14) and commercial tequila samples (n = 15) as well as a number of other spirits (n = 23). Whereas with delta(13)C(VPDB) values ranging from -12.1 to -13.2 per thousand and from -12.5 to -14.8 per thousand similar variations were found for 100% agave and mixed tequilas, respectively, the delta(18)O(VSMOW) data differed slightly within these categories: ranges from +22.1 to +22.8 per thousand and +20.8 to +21.7 per thousand were determined for both the authentic 100% agave and mixed products, respectively. The data recorded for commercial tequilas were less homogeneous; delta(13)C(VPDB) data from -10.6 to -13.9 per thousand and delta(18)O(VSMOW) values from +15.5 to +22.7 per thousand were determined in tequilas of both categories. Owing to overlapping data, attempts to differentiate between white, rested, and aged tequilas within each of the two categories failed. In addition, discrimination of tequila samples from other spirits by means of delta(13)C(VPDB) and delta(18)O(VSMOW) data of ethanol was restricted to the products originating from C(3) as well as C(4)/CAM raw materials.

  8. 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.

    Science.gov (United States)

    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). Copyright © 2014 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

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

    2016-11-01

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

  10. Chemically modified carbon fibers and their applications

    International Nuclear Information System (INIS)

    Ermolenko, I.N.; Lyubliner, I.P.; Gulko, N.V.

    1990-01-01

    This book gives a comprehensive review about chemically modified carbon fibers (e.g. by incorporation of other elements) and is structured as follows: 1. Types of carbon fibers, 2. Structure of carbon fibers, 3. Properties of carbon fibers, 4. The cellulose carbonization process, 5. Formation of element-carbon fiber materials, 6. Surface modification of carbon fibers, and 7. Applications of carbon fibers (e.g. adsorbents, catalysts, constituents of composites). (MM)

  11. Multispot fiber laser welding

    DEFF Research Database (Denmark)

    Schutt Hansen, Klaus

    This dissertation presents work and results achieved in the field of multi beam fiber laser welding. The project has had a practical approach, in which simulations and modelling have been kept at a minimum. Different methods to produce spot patterns with high power single mode fiber lasers have...... been examined and evaluated. It is found that both diamond turned DOE’s in zinc sulphide and multilevel etched DOE’s (Diffractive Optical Elements) in fused silica have a good performance. Welding with multiple beams in a butt joint configuration has been tested. Results are presented, showing it has...... been possible to control the welding width in incremental steps by adding more beams in a row. The laser power was used to independently control the keyhole and consequently the depth of fusion. An example of inline repair of a laser weld in butt joint configuration was examined. Zinc powder was placed...

  12. Fiber optic fluid detector

    Science.gov (United States)

    Angel, S.M.

    1987-02-27

    Particular gases or liquids are detected with a fiber optic element having a cladding or coating of a material which absorbs the fluid or fluids and which exhibits a change of an optical property, such as index of refraction, light transmissiveness or fluoresence emission, for example, in response to absorption of the fluid. The fluid is sensed by directing light into the fiber optic element and detecting changes in the light, such as exit angle changes for example, that result from the changed optical property of the coating material. The fluid detector may be used for such purposes as sensing toxic or explosive gases in the atmosphere, measuring ground water contamination or monitoring fluid flows in industrial processes, among other uses. 10 figs.

  13. Fiber optic fluid detector

    Science.gov (United States)

    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.

  14. Optical fiber communications

    CERN Document Server

    Keiser, Gerd

    2008-01-01

    The fourth edition of this popular text and reference book presents the fundamental principles for understanding and applying optical fiber technology to sophisticated modern telecommunication systems. Optical-fiber-based telecommunication networks have become a major information-transmission-system, with high capacity links encircling the globe in both terrestrial and undersea installations. Numerous passive and active optical devices within these links perform complex transmission and networking functions in the optical domain, such as signal amplification, restoration, routing, and switching. Along with the need to understand the functions of these devices comes the necessity to measure both component and network performance, and to model and stimulate the complex behavior of reliable high-capacity networks.

  15. Stable fiber interferometer

    International Nuclear Information System (INIS)

    Izmajlov, G.N.; Nikolaev, F.A.; Ozolin, V.V.; Grigor'yants, V.V.; Chamorovskij, Yu.K.

    1989-01-01

    The problem of construction the long-base Michelson interferometer for gravitational wave detection is discussed. Possible sources of noise and instability are considered. It is shown that evacuation of fiber interferometer, the winding of its arms on the glass ceramic bases, stabilization of radiation source frequency and seismic isolation of the base allow one to reduce its instability to the level, typical of mirror interferometer with the comparable optical base. 10 refs.; 2 figs

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

    Directory of Open Access Journals (Sweden)

    Valente Antonio Luiz Pires

    1998-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Wilma Regina Barrionuevo

    2001-04-01

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

  18. Deriving muscle fiber diameter from recorded single fiber potential.

    Science.gov (United States)

    Zalewska, Ewa

    2017-12-01

    The aim of the study was to estimate muscle fiber diameters through analysis of single muscle fiber potentials (SFPs) recorded in the frontalis muscle of a healthy subject. Our previously developed analytical and graphic method to derive fiber diameter from the analysis of the negative peak duration and the amplitude of SFP, was applied to a sample of ten SFPs recorded in vivo. Muscle fiber diameters derived from the simulation method for the sample of frontalis muscle SFPs are consistent with anatomical data for this muscle. The results confirm the utility of proposed simulation method. Outlying data could be considered as the result of a contribution of other fibers to the potential recorded using an SFEMG electrode. Our graphic tool provides a rapid estimation of muscle fiber diameter. Copyright © 2017 Elsevier Masson SAS. All rights reserved.

  19. Carbon fiber reinforced asphalt concrete

    International Nuclear Information System (INIS)

    Jahromi, Saeed G.

    2008-01-01

    Fibers are often used in the manufacture of other materials. For many years, they have been utilized extensively in numerous applications in civil engineering. Fiber-reinforcement refers to incorporating materials with desired properties within some other materials lacking those properties. Use of fibers is not a new phenomenon, as the technique of fiber-reinforced bitumen began early as 1950. In all industrialized countries today, nearly all concretes used in construction are reinforced. A multitude of fibers and fiber materials are being introduced in the market regularly. The present paper presents characteristics and properties of carbon fiber-reinforced asphalt mixtures, which improve the performance of pavements. To evaluate the effect of fiber contents on bituminous mixtures, laboratory investigations were carried out on the samples with and without fibers. During the course of this study, various tests were undertaken, applying Marshall Test indirect tensile test, creep test and resistance to fatigue cracking by using repeated load indirect tensile test. Carbon fiber exhibited consistency in results and as such it was observed that the addition of fiber does affect the properties of bituminous mixtures, i.e. an increase in its stability and decrease in the flow value as well as an increase in voids in the mix. Results indicate that fibers have the potential to resist structural distress in pavement, in the wake of growing traffic loads and thus improve fatigue by increasing resistance to cracks or permanent deformation. On the whole, the results show that the addition of carbon fiber will improve some of the mechanical properties like fatigue and deformation in the flexible pavement. (author)

  20. Monolithic femtosecond Yb-fiber laser with photonic crystal fibers

    DEFF Research Database (Denmark)

    Liu, Xiaomin; Lægsgaard, Jesper; Turchinovich, Dmitry

    We demonstrate a monolithic stable SESAM-modelocked self-starting Yb-fiber laser. A novel PM all-solid photonic bandgap fiber is used for intra-cavity of dispersion management. The ex-cavity final pulse compression is performed in a spliced-on PM hollow-core photonic crystal fiber. The laser...... directly delivers 9 nJ pulses of 275 fs duration with pulse repetition of 26.7MHz....

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

    DEFF Research Database (Denmark)

    Poulios, Konstantinos; Niordson, Christian Frithiof

    2016-01-01

    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...... 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...

  2. Raman fiber distributed feedback lasers.

    Science.gov (United States)

    Westbrook, Paul S; Abedin, Kazi S; Nicholson, Jeffrey W; Kremp, Tristan; Porque, Jerome

    2011-08-01

    We demonstrate fiber distributed feedback (DFB) lasers using Raman gain in two germanosilicate fibers. Our DFB cavities were 124 mm uniform fiber Bragg gratings with a π phase shift offset from the grating center. Our pump was at 1480 nm and the DFB lasers operated on a single longitudinal mode near 1584 nm. In a commercial Raman gain fiber, the maximum output power, linewidth, and threshold were 150 mW, 7.5 MHz, and 39 W, respectively. In a commercial highly nonlinear fiber, these figures improved to 350 mW, 4 MHz, and 4.3 W, respectively. In both lasers, more than 75% of pump power was transmitted, allowing for the possibility of substantial amplification in subsequent Raman gain fiber. © 2011 Optical Society of America

  3. Flexible optical fiber sensor based on polyurethane

    DEFF Research Database (Denmark)

    Kaysir, Md Rejvi; Stefani, Alessio; Lwin, Richard

    Polyurethane (PU) based hollow core fibers are investigated as optical sensors. The flexibility of PU fibers makes it suitable for sensing mechanical perturbations. We fabricated a PU fiber using the fiber drawing method, characterized the fiber and experimentally demonstrated a simple way...... to measure deformation, in the form of applied pressure....

  4. A fiber-optic polarimetric demonstration kit

    International Nuclear Information System (INIS)

    Eftimov, T; Dimitrova, T L; Ivanov, G

    2012-01-01

    A simple and multifunctional fiber-optic polarimetric kit on the basis of highly birefringent single-mode fibers is presented. The fiber-optic polarimetric kit allows us to perform the following laboratory exercises: (i) fiber excitation and the measurement of numerical aperture, (ii) polarization preservation and (iii) obtain polarization-sensitive fiberized interferometers.

  5. Dynamic drainage of froth with wood fibers

    Science.gov (United States)

    J.Y. Zhu; Freya Tan

    2005-01-01

    Understanding froth drainage with fibers (or simply called fiber drainage in froth) is important for improving fiber yield in the flotation deinking operation. In this study, the data of water and fiber mass in foams collected at different froth heights were used to reconstruct the time dependent and spatially resolved froth density and fiber volumetric concentration...

  6. Fiber optic sensor and method for making

    Science.gov (United States)

    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.

  7. Electrochromic fiber-shaped supercapacitors.

    Science.gov (United States)

    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. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. System for testing optical fibers

    Science.gov (United States)

    Golob, John E. [Olathe, KS; Looney, Larry D. [Los Alamos, NM; Lyons, Peter B. [Los Alamos, NM; Nelson, Melvin A. [Santa Barbara, CA; Davies, Terence J. [Santa Barbara, CA

    1980-07-15

    A system for measuring a combination of optical transmission properties of fiber optic waveguides. A polarized light pulse probe is injected into one end of the optical fiber. Reflections from discontinuities within the fiber are unpolarized whereas reflections of the probe pulse incident to its injection remain polarized. The polarized reflections are prevented from reaching a light detector whereas reflections from the discontinuities reaches the detector.

  9. Fiber-Optic Sensor Facility

    Data.gov (United States)

    Federal Laboratory Consortium — FUNCTION: Constructs and evaluates fiber-optic sensors for a variety of measurands. These measurands include acoustic, pressure, magnetic, and electric field as well...

  10. Development of scintillating fiber tracker

    International Nuclear Information System (INIS)

    Ishikawa, Shuzo; Kawai, Toshihide; Kozaki, Tetsuo

    1995-01-01

    In order to use thin scintillating fiber (diameter 500 micron) as a particle tracking detector, we have developed a method to construct precise multi-layer scintillating fiber sheets. We have also developed dedicated machines for this purpose. This paper presents the details of the method and the machines. Using these machines, we have produced fiber sheets for CERN WA95/CHORUS, which intend to detect a neutrino oscillation in the νμ-ντ channel using Hybrid Emulsion Set-up. Fiber Trackers are used as a vertex detector which support the neutrino event location in the nuclear emulsion target. (author)

  11. Fiber Tracking Cylinder Nesting

    International Nuclear Information System (INIS)

    Stredde, H.

    1999-01-01

    The fiber tracker consists of 8 concentric carbon fiber cylinders of varying diameters, from 399mm to 1032.2mm and two different lengths. 1.66 and 2.52 meters. Each completed cylinder is covered over the entire o.d. with scintillating fiber ribbons with a connector on each ribbon. These ribbons are axial (parallel to the beam line) at one end and stereo (at 3 deg. to the beam line) at the other. The ribbon connectors have dowel pins which are used to match with the connectors on the wave guide ribbons. These dowel pins are also used during the nesting operation, locating and positioning measurements. The nesting operation is the insertion of one cylinder into another, aligning them with one another and fastening them together into a homogeneous assembly. For ease of assembly. the nesting operation is accomplished working from largest diameter to smallest. Although the completed assembly of all 8 cylinders glued and bolted together is very stiff. individual cylinders are relatively flexible. Therefore. during this operation, No.8 must be supported in a manner which maintains its integrity and yet allows the insertion of No.7. This is accomplished by essentially building a set of dummy end plates which replicate a No.9 cylinder. These end plates are mounted on a wheeled cart that becomes the nesting cart. Provisions for a protective cover fastened to these rings has been made and will be incorporated in finished product. These covers can be easily removed for access to No.8 and/or the connection of No.8 to No.9. Another wheeled cart, transfer cart, is used to push a completed cylinder into the cylinder(s) already mounted in the nesting cart.

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

    Directory of Open Access Journals (Sweden)

    Katieli Martins Todisco

    2014-10-01

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

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

    Science.gov (United States)

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

    2016-10-02

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

  14. 1H NMR and SPME-GC/MS study of hydrolysis, oxidation and other reactions occurring during in vitro digestion of non-oxidized and oxidized sunflower oil. Formation of hydroxy-octadecadienoates.

    Science.gov (United States)

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

    2017-01-01

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

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

    Science.gov (United States)

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

    2017-05-01

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

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

    Science.gov (United States)

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

    2017-07-05

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

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

    Science.gov (United States)

    Yassaa, Noureddine; Williams, Jonathan

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

  18. Fiber sample presentation system for spectrophotometer cotton fiber color measurements

    Science.gov (United States)

    The Uster® High Volume Instrument (HVI) is used to class U.S. cotton for fiber color, yielding the industry accepted, cotton-specific color parameters Rd and +b. The HVI examines a 9 square inch fiber sample, and it is also used to test large AMS standard cotton “biscuits” or rectangles. Much inte...

  19. Random fiber laser based on artificially controlled backscattering fibers.

    Science.gov (United States)

    Wang, Xiaoliang; Chen, Daru; Li, Haitao; She, Lijuan; Wu, Qiong

    2018-01-10

    The random fiber laser (RFL), which is a milestone in laser physics and nonlinear optics, has attracted considerable attention recently. Most previously reported RFLs are based on distributed feedback of Rayleigh scattering amplified through the stimulated Raman-Brillouin scattering effect in single-mode fibers, which require long-distance (tens of kilometers) single-mode fibers and high threshold, up to watt level, due to the extremely small Rayleigh scattering coefficient of the fiber. We proposed and demonstrated a half-open-cavity RFL based on a segment of an artificially controlled backscattering single-mode fiber with a length of 210 m, 310 m, or 390 m. A fiber Bragg grating with a central wavelength of 1530 nm and a segment of artificially controlled backscattering single-mode fiber fabricated by using a femtosecond laser form the half-open cavity. The proposed RFL achieves thresholds of 25 mW, 30 mW, and 30 mW, respectively. Random lasing at a wavelength of 1530 nm and extinction ratio of 50 dB is achieved when a segment of 5 m erbium-doped fiber is pumped by a 980 nm laser diode in the RFL. A novel RFL with many short cavities has been achieved with low threshold.

  20. Carbon Fiber Biocompatibility for Implants

    Directory of Open Access Journals (Sweden)

    Richard Petersen

    2016-01-01

    Full Text Available 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.

  1. Polymer optical fiber bragg grating sensors

    DEFF Research Database (Denmark)

    Stefani, Alessio; Yuan, Scott Wu; Andresen, Søren

    2010-01-01

    Fiber-optical accelerometers based on polymer optical fiber Bragg gratings are reported. We have written fiber Bragg gratings for 1550 nm and 850 nm operations, characterized their temperature and strain response, and tested their performance in a prototype accelerometer....

  2. Extraction and characterization of Retama monosperma fibers

    African Journals Online (AJOL)

    XPERT

    monosperma leaves and their mechanical, physical and chemical characteristics. The fibers .... The hook was removed gently, and the behavior of the fiber was observed ..... fibers reinforced cement mortar slabs: a comparative study. Cement.

  3. Actively doped solid core Photonic Bandgap Fiber

    DEFF Research Database (Denmark)

    Broeng, Jes; Olausson, Christina Bjarnal Thulin; Lyngsøe, Jens Kristian

    2010-01-01

    Solid photonic bandgap fibers offer distributed spectral filtering with extraordinary high suppression. This opens new possibilities of artificially tailoring the gain spectrum of fibers. We present record-performance of such fibers and outline their future applications....

  4. Fiber breakage phenomena in long fiber reinforced plastic preparation

    International Nuclear Information System (INIS)

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

    2015-01-01

    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. (paper)

  5. High-birefringent photonic crystal fiber

    DEFF Research Database (Denmark)

    Libori, Stig E. Barkou; Broeng, Jes; Knudsen, Erik

    2001-01-01

    A highly birefringent photonic crystal fiber design is analysed. Birefringence up to 10-3 is found. Random fluctuations in the cladding design are analysed, and the fiber is found to be a feasible polarization maintaining fiber.......A highly birefringent photonic crystal fiber design is analysed. Birefringence up to 10-3 is found. Random fluctuations in the cladding design are analysed, and the fiber is found to be a feasible polarization maintaining fiber....

  6. Quantitive DNA Fiber Mapping

    Energy Technology Data Exchange (ETDEWEB)

    Lu, Chun-Mei; Wang, Mei; Greulich-Bode, Karin M.; Weier, Jingly F.; Weier, Heinz-Ulli G.

    2008-01-28

    Several hybridization-based methods used to delineate single copy or repeated DNA sequences in larger genomic intervals take advantage of the increased resolution and sensitivity of free chromatin, i.e., chromatin released from interphase cell nuclei. Quantitative DNA fiber mapping (QDFM) differs from the majority of these methods in that it applies FISH to purified, clonal DNA molecules which have been bound with at least one end to a solid substrate. The DNA molecules are then stretched by the action of a receding meniscus at the water-air interface resulting in DNA molecules stretched homogeneously to about 2.3 kb/{micro}m. When non-isotopically, multicolor-labeled probes are hybridized to these stretched DNA fibers, their respective binding sites are visualized in the fluorescence microscope, their relative distance can be measured and converted into kilobase pairs (kb). The QDFM technique has found useful applications ranging from the detection and delineation of deletions or overlap between linked clones to the construction of high-resolution physical maps to studies of stalled DNA replication and transcription.

  7. Optical fiber powered pressure sensor

    International Nuclear Information System (INIS)

    Schweizer, P.; Neveux, L.; Ostrowsky, D.B.

    1987-01-01

    In the system described, a pressure sensor and its associated electronics are optically powered by a 20 mw laser and a photovoltaic cell via an optical fiber. The sensor is periodically interrogated and sends the measures obtained back to the central unit using an LED and a second fiber. The results obtained as well as the expected evolution will be described

  8. Microstructured hollow fibers for ultrafiltration

    NARCIS (Netherlands)

    Culfaz, Pmar Zeynep; Culfaz, P.Z.; Rolevink, Hendrikus H.M.; van Rijn, C.J.M.; Lammertink, Rob G.H.; Wessling, Matthias

    2010-01-01

    Hollow fiber ultrafiltration membranes with a corrugated outer microstructure were prepared from a PES/PVP blend. The effect of spinning parameters such as air gap, take-up speed, polymer dope viscosity and coagulation value on the microstructure and membrane characteristics was investigated. Fibers

  9. Fiber optic-based biosensor

    Science.gov (United States)

    Ligler, Frances S.

    1991-01-01

    The NRL fiber optic biosensor is a device which measures the formation of a fluorescent complex at the surface of an optical fiber. Antibodies and DNA binding proteins provide the mechanism for recognizing an analyze and immobilizing a fluorescent complex on the fiber surface. The fiber optic biosensor is fast, sensitive, and permits analysis of hazardous materials remote from the instrumentation. The fiber optic biosensor is described in terms of the device configuration, chemistry for protein immobilization, and assay development. A lab version is being used for assay development and performance characterization while a portable device is under development. Antibodies coated on the fiber are stable for up to two years of storage prior to use. The fiber optic biosensor was used to measure concentration of toxins in the parts per billion (ng/ml) range in under a minute. Immunoassays for small molecules and whole bacteria are under development. Assays using DNA probes as the detection element can also be used with the fiber optic sensor, which is currently being developed to detect biological warfare agents, explosives, pathogens, and toxic materials which pollute the environment.

  10. Handbook of fiber optics theory and applications

    CERN Document Server

    Yeh, Chai

    2013-01-01

    Dr. Yeh supplies a firm theoretical foundation in such topics as propagation of light through fibers, fiber fabrication, loss mechanisms, and dispersion properties. He then expands from this into such practical areas as fiber splicing, measuring loss in fibers, fiber-based communications networks, remote fiber sensors, and integrated optics. Whether involved in fiber optics research, design, or practical implementation of systems, this handbook will be extremely useful.Key Features* Here is a comprehensive, ""one-stop"" reference with state-of-the-art information on fiber optics Included is da

  11. Radiation damage in optical fibers

    International Nuclear Information System (INIS)

    Lyons, P.B.; Looney, L.D.; Ogle, J.W.

    1983-01-01

    Optical fibers provide important advantages over coaxial cables for many data transmission applications. Some of these applications require that the fibers transmit data during a radiation pulse. Other applications utilize the fiber as a radiation-to-light transducer. In either case, radiation-induced luminescence and absorption must be understood. Most studies of radiation effects in fibers have emphasized time scales of interest in telecommunication systems, from the msec to hour range. Few studies have concentrated on response at times below 1 + s. At Los Alamos, both laboratory electron accelerators and nuclear tests have been used as radiation sources to probe this early time region. The use of a fiber (or any optical medium) as a Cerenkov radiation-to-light transducer is discussed. Since the radiation induces attenuation in the medium, the light output is not proportional to the radiation input. The nonlinearity introduced by this attenuation is calculated

  12. Photometric device using optical fibers

    International Nuclear Information System (INIS)

    Boisde, Gilbert; Perez, J.-J.

    1981-02-01

    Remote measurements in radioactive environment are now possible with optical fibers. Measurement instruments developed by CEA are constitued of: - an optical probe (5 mm to 1 meter optical path length), - a photometric measurement device, - optical fiber links. 'TELEPHOT' is a photometric device for industrial installations. It is uses interferentiel filters for 2 to 5 simultaneous wave lengths. 'CRUDMETER' measures the muddiness of water. It can be equipped with a high sensitivity cell of 50 cm optical path length tested up to 250 bars. Coupling a double beam spectrophotometer to a remote optical probe, up to 1 meter optical path length, is carried out by means of an optical device using optical fibers links, eventually several hundred meter long. For these equipments special step index large core fibers, 1 to 1.5 mm in diameter, have been developed as well connectors. For industrial control and research these instruments offer new prospect thanks to optical fibers use [fr

  13. Benefits of glass fibers in solar fiber optic lighting systems.

    Science.gov (United States)

    Volotinen, Tarja T; Lingfors, David H S

    2013-09-20

    The transmission properties and coupling of solar light have been studied for glass core multimode fibers in order to verify their benefits for a solar fiber optic lighting system. The light transportation distance can be extended from 20 m with plastic fibers to over 100 m with the kind of glass fibers studied here. A high luminous flux, full visible spectrum, as well as an outstanding color rendering index (98) and correlated color temperature similar to the direct sun light outside have been obtained. Thus the outstanding quality of solar light transmitted through these fibers would improve the visibility of all kinds of objects compared to fluorescent and other artificial lighting. Annual relative lighting energy savings of 36% in Uppsala, Sweden, and 76% in Dubai were estimated in an office environment. The absolute savings can be doubled by using glass optical fibers, and are estimated to be in the order of 550 kWh/year in Sweden and 1160 kWh/year in Dubai for one system of only 0.159 m(2) total light collecting area. The savings are dependent on the fiber length, the daily usage time of the interior, the type of artificial lighting substituted, the system light output flux, and the available time of sunny weather at the geographic location.

  14. Green Fiber Bottle

    DEFF Research Database (Denmark)

    Didone, Mattia; Tosello, Guido

    has to have an inner coating barrier. The most reliable solution proposed is to coat the inner walls with silicon dioxide, which is not biodegradable but rather environmentally inert. To enhance the environmental footprint and sustainability of the bottle, and to be competitive with the existing...... technologies, the manufacturing technology for the production of the bottle has to offer the possibility of significant energy savings. Molded pulp products are made from wood fibers dispersed in water, and then they are formed, drained and dried. A relatively large quantity of resources (i.e. energy and time......) is consumed during the drying process. It is in this process stage that an innovative way of drying the products can be exploited by using the concept of impulse drying. Impulse drying is an advance drying technique in which water is removed from a wet paper pulp by the combination of mechanical pressure...

  15. Carbon Fiber from Biomass

    Energy Technology Data Exchange (ETDEWEB)

    Milbrandt, Anelia [Clean Energy Manufacturing Analysis Center, Godlen, CO (United States); Booth, Samuel [Clean Energy Manufacturing Analysis Center, Godlen, CO (United States)

    2016-09-01

    Carbon fiber (CF), known also as graphite fiber, is a lightweight, strong, and flexible material used in both structural (load-bearing) and non-structural applications (e.g., thermal insulation). The high cost of precursors (the starting material used to make CF, which comes predominately from fossil sources) and manufacturing have kept CF a niche market with applications limited mostly to high-performance structural materials (e.g., aerospace). Alternative precursors to reduce CF cost and dependence on fossil sources have been investigated over the years, including biomass-derived precursors such as rayon, lignin, glycerol, and lignocellulosic sugars. The purpose of this study is to provide a comprehensive overview of CF precursors from biomass and their market potential. We examine the potential CF production from these precursors, the state of technology and applications, and the production cost (when data are available). We discuss their advantages and limitations. We also discuss the physical properties of biomass-based CF, and we compare them to those of polyacrylonitrile (PAN)-based CF. We also discuss manufacturing and end-product considerations for bio-based CF, as well as considerations for plant siting and biomass feedstock logistics, feedstock competition, and risk mitigation strategies. The main contribution of this study is that it provides detailed technical and market information about each bio-based CF precursor in one document while other studies focus on one precursor at a time or a particular topic (e.g., processing). Thus, this publication allows for a comprehensive view of the CF potential from all biomass sources and serves as a reference for both novice and experienced professionals interested in CF production from alternative sources.

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

    Directory of Open Access Journals (Sweden)

    Murat Yilmaztekin

    2014-01-01

    Full Text Available 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.

  17. Analysis of volatile components of cape gooseberry (Physalis peruviana L.) grown in Turkey by HS-SPME and GC-MS.

    Science.gov (United States)

    Yilmaztekin, Murat

    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.

  18. Fabrication of elastomeric silk fibers.

    Science.gov (United States)

    Bradner, Sarah A; Partlow, Benjamin P; Cebe, Peggy; Omenetto, Fiorenzo G; Kaplan, David L

    2017-09-01

    Methods to generate fibers from hydrogels, with control over mechanical properties, fiber diameter, and crystallinity, while retaining cytocompatibility and degradability, would expand options for biomaterials. Here, we exploited features of silk fibroin protein for the formation of tunable silk hydrogel fibers. The biological, chemical, and morphological features inherent to silk were combined with elastomeric properties gained through enzymatic crosslinking of the protein. Postprocessing via methanol and autoclaving provided tunable control of fiber features. Mechanical, optical, and chemical analyses demonstrated control of fiber properties by exploiting the physical cross-links, and generating double network hydrogels consisting of chemical and physical cross-links. Structure and chemical analyses revealed crystallinity from 30 to 50%, modulus from 0.5 to 4 MPa, and ultimate strength 1-5 MPa depending on the processing method. Fabrication and postprocessing combined provided fibers with extensibility from 100 to 400% ultimate strain. Fibers strained to 100% exhibited fourth order birefringence, revealing macroscopic orientation driven by chain mobility. The physical cross-links were influenced in part by the drying rate of fabricated materials, where bound water, packing density, and microstructural homogeneity influenced cross-linking efficiency. The ability to generate robust and versatile hydrogel microfibers is desirable for bottom-up assembly of biological tissues and for broader biomaterial applications. © 2017 Wiley Periodicals, Inc.

  19. New all-fiber velocimeter

    International Nuclear Information System (INIS)

    Weng Jidong; Tan Hua; Hu Shaolou; Ma Yun; Wan Xiang

    2005-01-01

    A new all-fiber velocity interferometer system for any reflector (AFVISAR) was developed. It was conceived and realized with the purpose of using it as the basic measuring element of a complete system for multiple point velocity measurements. Its main features are that it works at 532 nm and partly adopts the multimode optical fiber. The velocimeter consists of only fibers or fiber coupled components and has no optic elements such as optic lenses or reflectors. It is therefore very compact and easy to operate. Unlike the conventional AFVISAR, which uses single-mode optic fiber components, the laser beam in this new interferometer system arrives at and reflects from the target surface through a multimode optical fiber component, and then enters and interferes in a [3x3] single-mode fiber coupler. Its working principle is elaborated on in this article. Preliminary experiments using a split Hopkins pressure bar (SHPB) device show that the new interferometer can successfully measure the velocity profiles of the metal specimen along the axial or radial direction. Further experiments on a one-stage gas gun are under consideration

  20. Dimensional stability of natural fibers

    Energy Technology Data Exchange (ETDEWEB)

    Driscoll, Mark S. [Ultraviolet Light/Electron Beam (UV/EB) Technology Center, State University of New York College of Environmental Science and Forestry (SUNY-ESF), 1 Forestry Drive, Syracuse, NY 13210 (United States); Smith, Jennifer L.; Woods, Sean; Tiss, Kenneth J. [Ultraviolet Light/Electron Beam (UV/EB) Technology Center, State University of New York College of Environmental Science and Forestry (SUNY-ESF), 1 Forestry Drive, Syracuse, NY 13210 and Sustainable Construction Management and Engineering, SUNY-ESF (United States); Larsen, L. Scott [New York State Energy Research and Development Authority (NYSERDA), 17 Columbia Circle, Albany, NY 12203 (United States)

    2013-04-19

    One of the main problems associated with the use of natural fibers as reinforcing agents in composites is their uptake of moisture. Many natural fibers are lignocellulosic, which causes them to swell and shrink as the amount of available moisture changes. Swelling and shrinking can cause composites to prematurely fail. This paper presents the results of a preliminary study that considers the use of two different low molecular weight monomers, hydroxyethyl methacrylate (HEMA) and hydroxyethyl acrylate (HEA), polymerized by electron beam ionizing radiation, to dimensionally stabilize natural fibers. Eight different treatments consisting of varying amounts of monomer, encapsulating agent, and cross-linkers, were evaluated for their ability to dimensionally stabilize sisal fiber. Results indicate that both polymerized HEA and HEMA can reduce the swelling of sisal fiber. The effectiveness of HEA and HEMA can be further enhanced with the use of a cross-linker (SR 454). The use of hydroxylated monomers to dimensionally stabilize natural fibers may play an important role in reducing delamination and improving fiber-resin adhesion in composites.

  1. Dimensional stability of natural fibers

    International Nuclear Information System (INIS)

    Driscoll, Mark S.; Smith, Jennifer L.; Woods, Sean; Tiss, Kenneth J.; Larsen, L. Scott

    2013-01-01

    One of the main problems associated with the use of natural fibers as reinforcing agents in composites is their uptake of moisture. Many natural fibers are lignocellulosic, which causes them to swell and shrink as the amount of available moisture changes. Swelling and shrinking can cause composites to prematurely fail. This paper presents the results of a preliminary study that considers the use of two different low molecular weight monomers, hydroxyethyl methacrylate (HEMA) and hydroxyethyl acrylate (HEA), polymerized by electron beam ionizing radiation, to dimensionally stabilize natural fibers. Eight different treatments consisting of varying amounts of monomer, encapsulating agent, and cross-linkers, were evaluated for their ability to dimensionally stabilize sisal fiber. Results indicate that both polymerized HEA and HEMA can reduce the swelling of sisal fiber. The effectiveness of HEA and HEMA can be further enhanced with the use of a cross-linker (SR 454). The use of hydroxylated monomers to dimensionally stabilize natural fibers may play an important role in reducing delamination and improving fiber-resin adhesion in composites.

  2. Optical Fiber Sensors Based on Fiber Ring Laser Demodulation Technology.

    Science.gov (United States)

    Xie, Wen-Ge; Zhang, Ya-Nan; Wang, Peng-Zhao; Wang, Jian-Zhang

    2018-02-08

    A review for optical fiber sensors based on fiber ring laser (FRL) demodulation technology is presented. The review focuses on the principles, main structures, and the sensing performances of different kinds of optical fiber sensors based on FRLs. First of all, the theory background of the sensors has been discussed. Secondly, four different types of sensors are described and compared, which includes Mach-Zehnder interferometer (MZI) typed sensors, Fabry-Perot interferometer (FPI) typed sensors, Sagnac typed sensors, and fiber Bragg grating (FBG) typed sensors. Typical studies and main properties of each type of sensors are presented. Thirdly, a comparison of different types of sensors are made. Finally, the existing problems and future research directions are pointed out and analyzed.

  3. Multiplexed displacement fiber sensor using thin core fiber exciter.

    Science.gov (United States)

    Chen, Zhen; Hefferman, Gerald; Wei, Tao

    2015-06-01

    This letter reports a multiplexed optical displacement sensor using a thin core fiber (TCF) exciter. The TCF exciter is followed by a stripped single mode optical fiber. A small section of buffer is used as the movable component along the single mode fiber. Ultra-weak cladding mode reflection (< - 75 dB) was employed to probe the refractive index discontinuity between the air and buffer coating boundary. The position change of the movable buffer segment results in a delay change of the cladding mode reflection. Thus, it is a measure of the displacement of the buffer segment with respect to the glass fiber. The insertion loss of one sensor was measured to be less than 3 dB. A linear relationship was evaluated between the measurement position and absolute position of the moving actuator. Multiplexed capability was demonstrated and no cross talk was found between the sensors.

  4. SBIR-Long fluoride fiber

    Science.gov (United States)

    Jaeger, Raymond E.; Vacha, Lubos J.

    1987-08-01

    This report summarizes results obtained under a program aimed at developing new techniques for fabricating long lengths of heavy metal fluoride glass (HMFG) optical fiber. A new method for overcladding conventional HMFG preforms with a low melting oxide glass was developed, and improvements in the rotational casting method were made to increase preform length. The resulting composite glass canes consist of a fluoride glass overcoat layer to enhance strength and chemical durability. To show feasibility, prototype optical fiber preforms up to 1.6 cm in diameter with lengths of 22 cm were fabricated. These were drawn into optical fibers with lengths up to 900 meters.

  5. All-fiber polarization switch

    Science.gov (United States)

    Knape, Harald; Margulis, Walter

    2007-03-01

    We report an all-fiber polarization switch made out of silica-based microstructured fiber suitable for Q-switching all-fiber lasers. Nanosecond high-voltage pulses are used to heat and expand an internal electrode to cause λ/2-polarization rotation in less than 10 ns for 1.5 μm light. The 10 cm long component has an experimentally measured optical insertion loss of 0.2 dB and a 0-10 kHz repetition frequency capacity and has been durability tested for more than 109 pulses.

  6. Use of optical fibers in spectrophotometry

    Science.gov (United States)

    Ramsey, Lawrence W.

    1988-01-01

    The use of single or small numbers of fiber optic fibers in astronomical spectroscopy with the goal of greater spectrophotometric and radial velocity accuracy is discussed. The properties of multimode step index fibers which are most important for this application are outlined, as are laboratory tests of currently available fibers.

  7. Optical fiber communication — An overview

    Indian Academy of Sciences (India)

    Fabrication of single mode fibers is very difficult and so the fiber is .... of waveguide dispersion depends on the fiber design like core radius, since the .... production reducing the water content in the fiber to below 10 parts per billion. 5. ..... Connectors of the same type must be compatible from one manufacturer to another. 3.

  8. Optical Fiber Thermometer Based on Fiber Bragg Gratings

    Science.gov (United States)

    Rosli, Ekbal Bin; Mohd. Noor, Uzer

    2018-03-01

    Fiber Bragg grating has generated much interest in use as sensors to measure strain, temperature, and other physical parameters. It also the most common component used to develop this sensor with the advantages of simple, intrinsic sensing elements, electrically passive operation, EMI immunity, high sensitivity, compact size and potentially low cost [6]. This paper reports the design of an optical fiber thermometer based on fiber Bragg gratings. The system was developed for detecting temperature and strain by monitoring the shift of Bragg wavelength. The shifting of Bragg wavelength is used to indicate the temperature and strain due to the change in the surrounding temperature and strain. When the temperature and strain reach the exact wavelength level of the system, the temperature and strain value will display on the Arduino liquid crystal display (LCD). The optical fiber will provide the broadband light source and after passing the FBG the Bragg wavelength into the optical spectrum analyzer (OSA). The system is based on FBG as a physical quantity sensor. The temperatures measured is taken from the water bath and that of the strain is provided by amount of slotted mass used. The outcome of this project is to characterize the Bragg wavelength shifting from the fiber Bragg grating output. As the conclusion, this project provides an efficient optical fiber thermometer in measuring temperature and strain in order to replace the use of conventional electrical instruments.

  9. Enhancing Optical Communications with Brand New Fibers

    DEFF Research Database (Denmark)

    Morioka, Toshio; Awaji, Yoshinari; Ryf, Roland

    2012-01-01

    Optical fibers have often been considered to offer effectively infinite capacity to support the rapid traffic growth essential to our information society. However, as demand has grown and technology has developed, we have begun to realize that there is a fundamental limit to fiber capacity of ~ 100...... Tb/s per fiber for systems based on conventional single-core single-mode optical fiber as the transmission medium. This limit arises from the interplay of a number of factors including the Shannon limit, optical fiber nonlinearities, the fiber fuse effect, as well as optical amplifier bandwidth...... new fibers for space-division multiplexing and mode-division multiplexing....

  10. Ethanol extraction of phytosterols from corn fiber

    Science.gov (United States)

    Abbas, Charles; Beery, Kyle E.; Binder, Thomas P.; Rammelsberg, Anne M.

    2010-11-16

    The present invention provides a process for extracting sterols from a high solids, thermochemically hydrolyzed corn fiber using ethanol as the extractant. The process includes obtaining a corn fiber slurry having a moisture content from about 20 weight percent to about 50 weight percent solids (high solids content), thermochemically processing the corn fiber slurry having high solids content of 20 to 50% to produce a hydrolyzed corn fiber slurry, dewatering the hydrolyzed corn fiber slurry to achieve a residual corn fiber having a moisture content from about 30 to 80 weight percent solids, washing the residual corn fiber, dewatering the washed, hydrolyzed corn fiber slurry to achieve a residual corn fiber having a moisture content from about 30 to 80 weight percent solids, and extracting the residual corn fiber with ethanol and separating at least one sterol.

  11. Direct writing of fiber optic components in photonic crystal fibers and other specialty fibers

    Science.gov (United States)

    Fernandes, Luis Andre; Sezerman, Omur; Best, Garland; Ng, Mi Li; Kane, Saidou

    2016-04-01

    Femtosecond direct laser writing has recently shown great potential for the fabrication of complex integrated devices in the cladding of optical fibers. Such devices have the advantage of requiring no bulk optical components and no breaks in the fiber path, thus reducing the need for complicated alignment, eliminating contamination, and increasing stability. This technology has already found applications using combinations of Bragg gratings, interferometers, and couplers for the fabrication of optical filters, sensors, and power monitors. The femtosecond laser writing method produces a local modification of refractive index through non-linear absorption of the ultrafast laser pulses inside the dielectric material of both the core and cladding of the fiber. However, fiber geometries that incorporate air or hollow structures, such as photonic crystal fibers (PCFs), still present a challenge since the index modification regions created by the writing process cannot be generated in the hollow regions of the fiber. In this work, the femtosecond laser method is used together with a pre-modification method that consists of partially collapsing the hollow holes using an electrical arc discharge. The partial collapse of the photonic band gap structure provides a path for femtosecond laser written waveguides to couple light from the core to the edge of the fiber for in-line power monitoring. This novel approach is expected to have applications in other specialty fibers such as suspended core fibers and can open the way for the integration of complex devices and facilitate miniaturization of optical circuits to take advantage of the particular characteristics of the PCFs.

  12. Carbon Fiber Technology Facility (CFTF)

    Data.gov (United States)

    Federal Laboratory Consortium — Functionally within the MDF, ORNL operates DOE’s unique Carbon Fiber Technology Facility (CFTF)—a 42,000 ft2 innovative technology facility and works with leading...

  13. Nanomechanics of electrospun phospholipid fiber

    Energy Technology Data Exchange (ETDEWEB)

    Mendes, Ana C., E-mail: anac@food.dtu.dk, E-mail: ioach@food.dtu.dk; Chronakis, Ioannis S., E-mail: anac@food.dtu.dk, E-mail: ioach@food.dtu.dk [Technical University of Denmark, DTU-Food, Søltofts Plads B227, DK-2800, Kgs. Lyngby (Denmark); Nikogeorgos, Nikolaos; Lee, Seunghwan [Department of Mechanical Engineering, Technical University of Denmark, DK-2800 Kgs. Lyngby (Denmark)

    2015-06-01

    Electrospun asolectin phospholipid fibers were prepared using isooctane as a solvent and had an average diameter of 6.1 ± 2.7 μm. Their mechanical properties were evaluated by nanoindentation using Atomic Force Microscopy, and their elastic modulus was found to be approximately 17.2 ± 1 MPa. At a cycle of piezo expansion-retraction (loading-unloading) of a silicon tip on a fiber, relatively high adhesion was observed during unloading. It is proposed that this was primarily due to molecular rearrangements at the utmost layers of the fiber caused by the indentation of the hydrophilic tip. The phospholipid fibers were shown to be stable in ambient conditions, preserving the modulus of elasticity up to 24 h.

  14. Nanomechanics of electrospun phospholipid fiber

    DEFF Research Database (Denmark)

    Mendes, Ana Carina Loureiro; Nikogeorgos, Nikolaos; Lee, Seunghwan

    2015-01-01

    Electrospun asolectin phospholipid fibers were prepared using isooctane as a solvent and had an average diameter of 6.1 +/- 2.7 mu m. Their mechanical properties were evaluated by nanoindentation using Atomic Force Microscopy, and their elastic modulus was found to be approximately 17.2 +/- 1MPa....... At a cycle of piezo expansion-retraction (loading-unloading) of a silicon tip on a fiber, relatively high adhesion was observed during unloading. It is proposed that this was primarily due to molecular rearrangements at the utmost layers of the fiber caused by the indentation of the hydrophilic tip....... The phospholipid fibers were shown to be stable in ambient conditions, preserving the modulus of elasticity up to 24 h. (c) 2015 AIP Publishing LLC....

  15. Fiber Optics: A Bright Future.

    Science.gov (United States)

    Rice, James, Jr.

    1980-01-01

    Presents an overview of the impact of fiber optics on telecommunications and its application to information processing and library services, including information retrieval, news services, remote transmission of library services, and library networking. (RAA)

  16. Application of Fiber Optic Instrumentation

    Science.gov (United States)

    Richards, William Lance; Parker, Allen R., Jr.; Ko, William L.; Piazza, Anthony; Chan, Patrick

    2012-01-01

    Fiber optic sensing technology has emerged in recent years offering tremendous advantages over conventional aircraft instrumentation systems. The advantages of fiber optic sensors over their conventional counterparts are well established; they are lighter, smaller, and can provide enormous numbers of measurements at a fraction of the total sensor weight. After a brief overview of conventional and fiber-optic sensing technology, this paper presents an overview of the research that has been conducted at NASA Dryden Flight Research Center in recent years to advance this promising new technology. Research and development areas include system and algorithm development, sensor characterization and attachment, and real-time experimentally-derived parameter monitoring for ground- and flight-based applications. The vision of fiber optic smart structure technology is presented and its potential benefits to aerospace vehicles throughout the lifecycle, from preliminary design to final retirement, are presented.

  17. High performance polyethylene nanocomposite fibers

    Directory of Open Access Journals (Sweden)

    A. Dorigato

    2012-12-01

    Full Text Available A high density polyethylene (HDPE matrix was melt compounded with 2 vol% of dimethyldichlorosilane treated fumed silica nanoparticles. Nanocomposite fibers were prepared by melt spinning through a co-rotating twin screw extruder and drawing at 125°C in air. Thermo-mechanical and morphological properties of the resulting fibers were then investigated. The introduction of nanosilica improved the drawability of the fibers, allowing the achievement of higher draw ratios with respect to the neat matrix. The elastic modulus and creep stability of the fibers were remarkably improved upon nanofiller addition, with a retention of the pristine tensile properties at break. Transmission electronic microscope (TEM images evidenced that the original morphology of the silica aggregates was disrupted by the applied drawing.

  18. All-optical fiber compressor

    International Nuclear Information System (INIS)

    Ivanov, Luben M.

    2015-01-01

    A simple all-optical fiber compressor, based on an idea of dispersion management using a fiber of positive dispersion in the first part and of negative dispersion in the second one at the working wavelength, is investigated. The method allows a combination of the advantages of the classic fiber-grating and of the multisoliton compression. It is possible to improve substantially the quality of the compressed pulse compared to the multisoliton compression. The compression factor could be increased up to 2-2.5 times when the fraction of the input pulse energy appearing within the compressed pulse enhances more than 2 times. Thus, the peak power of the compressed pulse is able to increase about 5 times and the quality of the obtained pulses should be comparable with those obtained by the fiber-grating compressor

  19. Influence of forming conditions on fiber tilt

    Science.gov (United States)

    David W. Vahey; John M. Considine; Michael A. and MacGregor

    2013-01-01

    Fiber tilt describes the projection of fiber length in the thickness direction of paper. The projection is described by the tilt angle of fibers with respect to the plane of the sheet. A simple model for fiber tilt is based on jet-to-wire velocity differential in combination with cross-flows on the wire. The tilt angle of a fiber is found to vary as the sine of its in-...

  20. Engineering modes in optical fibers with metamaterial

    DEFF Research Database (Denmark)

    Yan, Min; Mortensen, Asger; Qiu, Min

    2009-01-01

    In this paper, we report a preliminary theoretical study on optical fibers with fine material inclusions whose geometrical inhomogeneity is almost indistinguishable by the operating wavelength.We refer to such fibers as metamaterial optical fibers, which can conceptually be considered...... as an extension from the previously much publicized microstructured optical fibers. Metamaterials can have optical properties not obtainable in naturally existing materials, including artificial anisotropy as well as graded material properties. Therefore, incorporation of metamaterial in optical fiber designs can...