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Sample records for extraction thermal desorption

  1. Solid-phase extraction-thermal desorption-gas chromatography with mass selective detection for the determination of drugs in urine

    NARCIS (Netherlands)

    van Hout, MWJ; de Zeeuw, RA; Franke, JP; de Jong, GJ

    2003-01-01

    Solid-phase extraction (SPE) was combined with thermal desorption (TD) and gas chromatographic (GC) analysis to determine drugs in urine. The extraction was performed inside a fritted GC liner using about 5 mg TENAX that was inserted into the liner on top of the frit. After extraction, the liner was

  2. Cloud point extraction and gas chromatography with direct microvial insert thermal desorption for the determination of haloanisoles in alcoholic beverages.

    Science.gov (United States)

    Cacho, J I; Campillo, N; Viñas, P; Hernández-Córdoba, M

    2016-11-01

    A sensitive analytical procedure for the determination of four haloanisoles (2,4,6 trichloroanisole, 2,4,6-tribromoanisole, 2,3,4,6-tetrachloroanisole and pentachloroanisole) related with cork taint defects in wines, in different types of alcoholic beverages has been developed. The analytes were extracted from the matrix samples by cloud point extraction (CPE) using Triton X-114 heated to 75°C, and the surfactant rich phase was separated by centrifugation. By means of direct microvial insert thermal desorption, 20µL of the CPE obtained extract was submitted to gas chromatography-mass spectrometry (GC-MS) analysis. The parameters affecting the CPE and microvial insert thermal desorption were optimized. Quantification was carried by matrix-matched calibration using an internal standard. Detection limits ranged between 12.9 and 20.8ngL(-1), depending on the compound, for beer and wine samples, whereas for whiskies values in the 46.3-48ngL(-1) range were obtained, since these samples were diluted for analysis. Recoveries for alcoholic beverages were in the 89-111% range, depending on the analyte and the sample.

  3. Determination of parabens in house dust by pressurised hot water extraction followed by stir bar sorptive extraction and thermal desorption-gas chromatography-mass spectrometry.

    Science.gov (United States)

    Ramírez, Noelia; Marcé, Rosa Maria; Borrull, Francesc

    2011-09-16

    This study describes the development of a new method for determining p-hydroxybenzoic esters (parabens) in house dust. This optimised method was based on the pressurised hot water extraction (PHWE) of house dust, followed by the acetylation of the extracted parabens, stir bar sorptive extraction (SBSE) with a polydimethylsiloxane stir bar, and finally analysis using thermal desorption-gas chromatography-mass spectrometry (TD-GC-MS). The combination of SBSE and PHWE allows the analytes to be preconcentrated and extracted from the aqueous extract in a single step with minimal manipulation of the sample. Furthermore the in situ acetylation of parabens prior to SBSE improved their extraction efficiency and their GC-MS signal. The method showed recoveries of between 40 and 80%, good linearity, repeatability and reproducibility (paraben to 2.1 ng g(-1) for methyl paraben) and quantification (from 3.3 ng g(-1) for propyl paraben to 8.5 ng g(-1) for methyl paraben). The proposed method was applied to the analysis of house dust samples. All the target parabens were found in the samples. Methyl and propyl parabens were the most abundant, with concentrations up to 2440 ng g(-1) and 910 ng g(-1), respectively. The high levels of parabens found in the samples confirm the importance of determining organic contaminants in indoor environments.

  4. Dispersive micro solid-phase extraction for the rapid analysis of synthetic polycyclic musks using thermal desorption gas chromatography-mass spectrometry.

    Science.gov (United States)

    Chung, Wu-Hsun; Tzing, Shin-Hwa; Ding, Wang-Hsien

    2013-09-13

    A simple and solvent-free method for the rapid analysis of five synthetic polycyclic musks in water samples is described. The method involves the use of dispersive micro solid-phase extraction (D-μ-SPE) coupled with direct thermal desorption (TD) gas chromatography-mass spectrometry (GC-MS) operating in the selected-ion-storage (SIS) mode. The parameters affecting the extraction efficiency of the target analytes from water sample and the thermal desorption conditions in the GC injection-port were optimized using a central composite design method. The optimal extraction conditions involved immersing 3.2mg of a typical octadecyl (C18) bonded silica adsorbent (i.e., ENVI-18) in a 10mL water sample. After extraction by vigorously shaking for 1.0min, the adsorbents were collected and dried on a filter. The adsorbents were transferred to a micro-vial, which was directly inserted into GC temperature-programmed injector, and the extracted target analytes were then thermally desorbed in the GC injection-port at 337°C for 3.8min. The limits of quantitation (LOQs) were determined to be 1.2-3.0ng/L. Precision, as indicated by relative standard deviations (RSDs), was less than 9% for both intra- and inter-day analysis. Accuracy, expressed as the mean extraction recovery, was between 74 and 90%. A preliminary analysis of the river water samples revealed that galaxolide (HHCB) and tonalide (AHTN) were the two most common synthetic polycyclic musks present. Using a standard addition method, their concentrations were determined to in the range from 11 to 140ng/L.

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

    Science.gov (United States)

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

    2001-06-01

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

  6. Multi-residue off-flavour profiling in wine using stir bar sorptive extraction-thermal desorption-gas chromatography-mass spectrometry.

    Science.gov (United States)

    Franc, Céline; David, Frank; de Revel, Gilles

    2009-04-10

    A multi-residue method (MRM) for the detection and quantification of eight compounds responsible for off-flavours in wine using stir bar sorptive extraction (SBSE) followed by thermal desorption (TD) and gas chromatography-mass spectrometry (GC-MS) analysis is presented. The extraction and desorption conditions were optimised in order to get the best compromise for the simultaneous analysis of the eight target solutes, belonging to different chemical classes. The analytical conditions enable the quantification of the solutes below their respective organoleptic perception thresholds in wine. The method displayed good linearity over the concentration ranges explored in wine as well as excellent repeatability (RSD below 6%) and good reproducibility (RSD below 24%). The developed methodology was applied to the analysis of several wines and showed good agreement with the results collected with headspace solid-phase microextraction (HS-SPME) or liquid-liquid extraction (LLE) followed by GC-MS or electron capture detection (ECD). Good correlation was also found between the analytical and sensory results.

  7. Determination of five booster biocides in seawater by stir bar sorptive extraction-thermal desorption-gas chromatography-mass spectrometry.

    Science.gov (United States)

    Giráldez, I; Chaguaceda, E; Bujalance, M; Morales, E

    2013-01-04

    Stir bar sorptive extraction (SBSE) and thermal desorption (TD)-gas chromatography-mass spectrometry (GC-MS) have been optimized for the determination of five organic booster biocides (Chlorothalonil, Dichlofluanid, Sea-Nine 211, Irgarol 1051 and TCMTB) in seawater samples. The parameters affecting the desorption and absorption steps were investigated using 10 mL seawater samples. The optimised conditions consisted of an addition of 0.2 g mL(-1) KCl to the sample, which was extracted with 10mm length, 0.5mm film thickness stir bars coated with polydimethylsiloxane (PDMS), and stirred at 900 rpm for 90 min at room temperature (25 °C) in a vial. Desorption was carried out at 280 °C for 5 min under 50 mL min(-1) of helium flow in the splitless mode while maintaining a cryotrapping temperature of 20 °C in the programmed-temperature vaporization (PTV) injector of the GC-MS system. Finally, the PTV injector was ramped to a temperature of 280 °C and the analytes were separated in the GC and detected by MS using the selected-ion monitoring (SIM) mode. The detection limits of booster biocides were found to be in the range of 0.005-0.9 μg L(-1). The regression coefficients were higher than 0.999 for all analytes. The average recovery was higher than 72% (R.S.D.: 7-15%). All these figures of merit were established running samples in triplicate. This simple, accurate, sensitive and selective analytical method may be used for the determination of trace amounts of booster biocides in water samples from marinas.

  8. Simultaneous determination of preservatives in beverages, vinegar, aqueous sauces, and quasi-drug drinks by stir-bar sorptive extraction (SBSE) and thermal desorption GC-MS.

    Science.gov (United States)

    Ochiai, Nobuo; Sasamoto, Kikuo; Takino, Masahiko; Yamashita, Satoru; Daishima, Shigeki; Heiden, Arnd C; Hoffmann, Andreas

    2002-05-01

    A method for the simultaneous determination of seven preservatives - sorbic acid, benzoic acid, and p-hydroxybenzoic acid ethyl, isopropyl, propyl, isobutyl, and butyl esters - in beverages, vinegar, aqueous sauces, and quasi-drug drinks has been developed using the stir-bar sorptive extraction technique then thermal desorption GC-MS analysis. The extraction conditions - pH, sample volume, extraction temperature, salt addition, and extraction time - were examined. d5-Benzoic acid and p-hydroxybenzoic acid sec-butyl ester were added as surrogate internal standards to compensate for the effect of sample matrix and coexisting analytes on the sorptive extraction. The linearity of the method was good over the concentration range from 1 to 1000 microg mL(-1) for sorbic acid, 10-1000 microg mL(-1) for benzoic acid, and 0.1-100 microg mL(-1) for p-hydroxybenzoic acid ethyl, isopropyl, propyl, isobutyl, and butyl esters, and the correlation coefficients were higher than 0.9984. The limit of detection ranged from 0.015 to 3.3 microg mL(-1). The recoveries (95-105%) and precision (RSD: 0.86-6.0%) of the method were examined by analyzing a sparkling soft drink, white wine, red wine, balsamic vinegar, soy sauce, and quasi-drug drink samples fortified at the 5 to 50 microg mL(-1) level.

  9. Comparative study of thermal desorption and solvent extraction-gas chromatography-mass spectrometric analysis for the quantification of phthalates in polymers.

    Science.gov (United States)

    Kim, Jae Woo; Kim, Young-Min; Moon, Hye Mi; Hosaka, Akihiko; Watanabe, Chuichi; Teramae, Norio; Choe, Eun Kyung; Myung, Seung-Woon

    2016-06-17

    For the quantitative analysis of phthalates in polymers, a thermal desorption (TD)-GC-MS method was compared with solvent extraction (SE)-GC-MS methods which require the long pretreatment procedures using large amount of harmful organic solvents. Calibration curves of TD-GC-MS showed good linearity (r(2)>0.9997) and low method detection limit (phthalate polymer samples (test PTPSs) showed an RSD below 7.4% and acceptable recoveries (78.3-117.4%) as in the standard method of International Electrotechnical Commission. Even in a sample with a high concentration of phthalates (PTPS #3), the method also showed good recovery with low RSD values. The TD-GC-MS results were comparable with those results by SE-GC-MS methods, indicating that TD-GC-MS method also can be used for the quantification of phthalates in polymers. The average recovery (92-103%) and RSD (phthalates in polymers.

  10. Magic-angle thermal desorption mass spectroscopy

    Science.gov (United States)

    Pauls, Steven W.; Campbell, Charles T.

    1990-02-01

    Accurate quantitative measurements of desorption rates or adsorbate coverages in thermal desorption mass spectroscopy (TDS) using line-of-sight mass spectrometers are hindered by the fact that the angular distributions of desorption flux can vary widely from desorbate to desorbate, ranging from cos 1ø to cos 9 ø for most species studied to date (ø = polar angle from surface normal). These differences can easily lead to errors exceeding 400% in measuring the relative desorption rates of different species. We show here that, by placing the mass spectrometer's ion source or entrance aperture at a "magic-angle" ø mthese errors can be reduced to less than 26% maximum deviation (or ± 7% standard deviation). Depending upon the sample-to-detector distance, ø m varies from ~ 42° to 34°. It is recommended that TDS experiments be performed at this "magic-angle" for improvement in the quantitative accuracy of coverage or rate measurements.

  11. Analysis of trace contamination of phthalate esters in ultrapure water using a modified solid-phase extraction procedure and automated thermal desorption-gas chromatography/mass spectrometry.

    Science.gov (United States)

    Liu, Hsu-Chuan; Den, Walter; Chan, Shu-Fei; Kin, Kuan Tzu

    2008-04-25

    The present study was aimed to develop a procedure modified from the conventional solid-phase extraction (SPE) method for the analysis of trace concentration of phthalate esters in industrial ultrapure water (UPW). The proposed procedure allows UPW sample to be drawn through a sampling tube containing hydrophobic sorbent (Tenax TA) to concentrate the aqueous phthalate esters. The solid trap was then demoisturized by two-stage gas drying before subjecting to thermal desorption and analysis by gas chromatography-mass spectrometry. This process removes the solvent extraction procedure necessary for the conventional SPE method, and permits automation of the analytical procedure for high-volume analyses. Several important parameters, including desorption temperature and duration, packing quantity and demoisturizing procedure, were optimized in this study based on the analytical sensitivity for a standard mixture containing five different phthalate esters. The method detection limits for the five phthalate esters were between 36 ng l(-1) and 95 ng l(-1) and recovery rates between 15% and 101%. Dioctyl phthalate (DOP) was not recovered adequately because the compound was both poorly adsorbed and desorbed on and off Tenax TA sorbents. Furthermore, analyses of material leaching from poly(vinyl chloride) (PVC) tubes as well as the actual water samples showed that di-n-butyl phthalate (DBP) and di(2-ethylhexyl) phthalate (DEHP) were the common contaminants detected from PVC contaminated UPW and the actual UPW, as well as in tap water. The reduction of DEHP in the production processes of actual UPW was clearly observed, however a DEHP concentration of 0.20 microg l(-1) at the point of use was still being quantified, suggesting that the contamination of phthalate esters could present a barrier to the future cleanliness requirement of UPW. The work demonstrated that the proposed modified SPE procedure provided an effective method for rapid analysis and contamination

  12. Trace analysis of chlorophenols in river water samples by stir bar sorptive extraction with in situ derivatization and thermal desorption-gas chromatography-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Kawaguchi, M.; Ishii, Y.; Okanouchi, N.; Sakui, N.; Ito, R.; Inoue, K.; Nakazawa, H. [Hoshi Univ., Tokyo (Japan). Dept. of Analytical Chemistry, Faculty of Pharmaceutical Sciences; Saito, K. [Saitama Institute of Public Health, Saitama (Japan). Dioxin Research Group

    2004-09-15

    Many analytical methods for the determination of chlorophenols in water samples have been reported including gas chromatography-mass spectrometry (GC-MS). However, GC-MS was initially used for the determination of phenol compounds even though derivatization was required. The derivatization leads to sharper peaks and hence to better separation and higher sensitivity for the phenols. However, the derivatization faces the risk of contamination and hence an overestimation of chlorophenols concentration. In order to overcome these problems, in situ derivatization has been developed, which involves the simple addition of a reagent to a liquid sample. Recently, a new sorptive extraction technique that uses a stir bar coated with polydimethylsiloxane (PDMS) was developed. The technique is known as stir bar sorptive extraction (SBSE). We already reported that determination of 4-tert-octylphenol (OP) and 4-nonylphenol (NP) in river water4 and body fluid samples by using SBSE. In addition, SBSE with in situ derivatization has been successfully used in the determination of bisphenol A (BPA) in human body fluid samples6 and phenolic xenoestrogens in river water samples. The aim of this study is to determine trace amounts of chlorophenols in water samples by SBSE with in situ derivatization, followed by thermal desorption (TD)-GC-MS. The developed method was applied to determination of chlorophenols in river water samples.

  13. Determination of off-flavor compounds, 2-methylisoborneol and geosmin, in salmon fillets using stir bar sorptive extraction-thermal desorption coupled with gas chromatography-mass spectrometry.

    Science.gov (United States)

    Ruan, E D; Aalhus, J L; Summerfelt, S T; Davidson, J; Swift, B; Juárez, M

    2013-12-20

    A sensitive and solvent-less method for the determination of musty and earthy off-flavor compounds, 2-methylisoborneol (MIB) and geosmin (GSM), in salmon tissue was developed using stir bar sorptive extraction-thermal desorption coupled with gas chromatography-mass spectrometry (SBSE-TD-GCMS). MIB and GSM were solid phase extracted using polydimethylsiloxane (PDMS) coated stir bars, analyzed by gas chromatography, and detected in full scan mode of mass selective detector (MSD). Using this method, the calibration curves of MIB and GSM were linear in the range of 0.3-100ng/L, with a correlation coefficient above 0.999 and RSDs less than 4% (n=4). The limit of detection (LOD, S/N=3, n=6) and limit of quantification (LOQ, S/N=10, n=6) of MIB and GSM were both ∼0.3 and 1ng/L, respectively. The recoveries of MIB and GSM were 22% and 29% by spike in 30ng/L standard compounds, 23% and 30% by spike-in 100ng/L standard compounds in salmon tissue samples with good precision (<8% of RSDs, n=6), respectively. The recoveries of MIB and GSM were better than reported methodologies using SPME fibres (<10%) in fish tissue samples. This method was successfully applied to monitor and characterize depurated salmon fillet samples (0, 3, 6 and 10 days).

  14. Spatially resolved thermal desorption/ionization coupled with mass spectrometry

    Science.gov (United States)

    Jesse, Stephen; Van Berkel, Gary J; Ovchinnikova, Olga S

    2013-02-26

    A system and method for sub-micron analysis of a chemical composition of a specimen are described. The method includes providing a specimen for evaluation and a thermal desorption probe, thermally desorbing an analyte from a target site of said specimen using the thermally active tip to form a gaseous analyte, ionizing the gaseous analyte to form an ionized analyte, and analyzing a chemical composition of the ionized analyte. The thermally desorbing step can include heating said thermally active tip to above 200.degree. C., and positioning the target site and the thermally active tip such that the heating step forms the gaseous analyte. The thermal desorption probe can include a thermally active tip extending from a cantilever body and an apex of the thermally active tip can have a radius of 250 nm or less.

  15. Thermal desorption of deuterium implanted into beryllium

    Energy Technology Data Exchange (ETDEWEB)

    Markin, A.V.; Chernikov, V.N.; Zakharov, A.P. [Institute of Physical Chemistry, Moscow (Russian Federation)] [and others

    1995-09-01

    By means of TDS measurements it is shown that the desorption of deuterium from Be implanted with 5 keV D ions to fluences, {Phi}, from 1x10{sup 20} D/m{sup 2} to 1x10{sup 21} D/m{sup 2} proceeds in one high temperature stage B, while at {Phi} {ge} 1.2x10{sup 21}D/m{sup 2} one more stage A is added. The desorption maximum A is narrow and consists of two peaks A{sub 1} and A{sub 2} at about 460 K and 490 K, respectively. Peak A{sub 1} is attributed to the desorption of deuterium from the walls of opened channels formed under D ion implantation. Peak {sub A}2 is a consequence of the opening of a part of closed bubbles/channels to the outer surface. The position of maximum B shifts noticeably and nonsteadily on the fluence in a range from 850 to 1050 K. The origin of this maximum is the liberation of D atoms bound at vacancy complexes discussed previously by Wampler. The dependence of Tm(B) on the fluence is governed by the interaction of freely migrating D atoms with partly opened or fully closed gas cavity arrangements which are created under temperature ramping, but differently in specimens implanted with D ions to different fluences.

  16. Characterisation of the flavour profile from Graciano Vitis vinifera wine variety by a novel dual stir bar sorptive extraction methodology coupled to thermal desorption and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Arbulu, Maria; Sampedro, M Carmen; Sanchez-Ortega, Alicia; Gómez-Caballero, Alberto; Unceta, Nora; Goicolea, M Aranzazu; Barrio, Ramón J

    2013-05-13

    The aim of this work was to develop a new analytical technique for the study of the organoleptic compounds (flavour profile) of the Graciano Vitis vinifera wine variety. The cv. Graciano is a singular variety of red grapes with its origins in La Rioja and Navarra (northern Spain). This variety transfers an intense red colour, aroma and high acidity to musts and provides greater longevity and, consequently, a better capacity for ageing wine. A new dual-stir bar sorptive extraction approach coupled with thermal desorption (TD) and GC-MS has been used to extract the volatile and semivolatile compounds. In this extraction step, the optimal values for the experimental variables were obtained through the Response Surface Methodology (RSM). Full scan chromatogram data were evaluated with two deconvolution software tools, and the results were compared. The volatile and semivolatile components were identified with an MS match ≥80%. As a result, the flavour metabolome of the Graciano Vitis vinifera wine variety was obtained, and 205 metabolites were identified using different databases. These metabolites were grouped into esters, acids, alcohols, nitrogen compounds, furans, lactones, ketones, aldehydes, phenols, terpenes, norisoprenoids, sulphur compounds, acetals and pyrans. The majority of the metabolites observed had already been reported in the literature; however, this work also identified new, previously unreported metabolites in red wines, which may be characteristic of the Graciano variety. Copyright © 2013 Elsevier B.V. All rights reserved.

  17. Laser-induced thermal desorption of aniline from silica surfaces

    Science.gov (United States)

    Voumard, Pierre; Zenobi, Renato

    1995-10-01

    A complete study on the energy partitioning upon laser-induced thermal desorption of aniline from silica surfaces was undertaken. The measurements include characterization of the aniline-quartz adsorption system using temperature-programmed desorption, the extrapolation of quasiequilibrium desorption temperatures to the regime of laser heating rates on the order of 109-1010 K/s by computational means, measurement of the kinetic energy distributions of desorbing aniline using a pump-probe method, and the determination of internal energies with resonance-enhanced multiphoton ionization spectroscopy. The measurements are compared to calculations of the surface temperature rise and the resulting desorption rates, based on a finite-difference mathematical description of pulsed laser heating. While the surface temperature of laser-heated silica reaches about 600-700 K at the time of desorption, the translational temperature of laser-desorbed aniline was measured to be Tkin=420±60 K, Tvib was 360±60 K, and Trot was 350±100 K. These results are discussed using different models for laser-induced thermal desorption from surfaces.

  18. The study of 'microsurfaces' using thermal desorption spectroscopy

    Science.gov (United States)

    Thomas, M. E.; Poppa, H.; Pound, G. M.

    1979-01-01

    The use of a newly combined ultrahigh vacuum technique for studying continuous and particulate evaporated thin films using thermal desorption spectroscopy (TDS), transmission electron microscopy (TEM), and transmission electron diffraction (TED) is discussed. It is shown that (1) CO thermal desorption energies of epitaxially deposited (111) Ni and (111) Pd surfaces agree perfectly with previously published data on bulk (111) single crystal, (2) contamination and surface structural differences can be detected using TDS as a surface probe and TEM as a complementary technique, and (3) CO desorption signals from deposited metal coverages of one-thousandth of a monolayer should be detectable. These results indicate that the chemisorption properties of supported 'microsurfaces' of metals can now be investigated with very high sensitivity. The combined use of TDS and TEM-TED experimental methods is a very powerful technique for fundamental studies in basic thin film physics and in catalysis.

  19. Thermal Desorption of Helium Implanted in Tungsten at RT

    Institute of Scientific and Technical Information of China (English)

    ZHANGFu; XUZengyu; LIUXiang; CHENJiming; XUYing; N.Yoshida; H.Iwakiri

    2002-01-01

    Tungsten is envisaged as one of the main candidate materials for divertor plate of ITER and future fusion reactors. Due to D-T reaction, PFMs would suffer helium irradiation from plasma additional to the high heat loads. Helium retention and thermal desorption behavior are largely concerned.

  20. Development of a Method for the Quantitation of Three Thiols in Beer, Hop, and Wort Samples by Stir Bar Sorptive Extraction with in Situ Derivatization and Thermal Desorption-Gas Chromatography-Tandem Mass Spectrometry.

    Science.gov (United States)

    Ochiai, Nobuo; Sasamoto, Kikuo; Kishimoto, Toru

    2015-08-05

    A method for analysis of hop-derived polyfunctional thiols, such as 4-sulfanyl-4-methylpentan-2-one (4S4M2Pone), 3-sulfanylhexan-1-ol (3SHol), and 3-sulfanylhexyl acetate (3SHA), in beer, hop water extract, and wort at nanogram per liter levels was developed. The method employed stir bar sorptive extraction with in situ derivatization (der-SBSE) using ethyl propiolate (ETP), followed by thermal desorption and gas chromatography-tandem mass spectrometry (TD-GC-MS/MS) with selected reaction monitoring (SRM) mode. A prior step involved structural identification of the ETP derivatives of the thiols by TD-GC-quadrupole-time-of-flight mass spectrometry with parallel sulfur chemiluminescence detection (Q-TOF-MS/SCD) after similar der-SBSE. The der-SBSE conditions of the ETP concentration, buffer concentration, salt addition, and extraction time profiles were investigated, and the performance of the method was demonstrated with spiked beer samples. The limits of detection (LODs) (0.19-27 ng/L) are below the odor threshold levels of all analytes. The apparent recoveries at 10-100 ng/L (99-101%) and the repeatabilities [relative standard deviation (RSD) of 1.3-7.2%; n = 6] are also good. The method was successfully applied to the determination of target thiols at nanogram per liter levels in three kinds of beer samples (hopped with Cascade, Citra, and Nelson Sauvin) and the corresponding hop water extracts and wort samples. There was a clear correlation between the determined values and the characteristics of citrus hop aroma for each sample.

  1. PAH desorption from river floodplain soils using supercritical fluid extraction.

    Science.gov (United States)

    Yang, Yi; Cajthaml, Tomás; Hofmann, Thilo

    2008-12-01

    Sequential supercritical fluid extraction (SFE) was performed in order to estimate desorption of PAHs from river floodplain soils which contain coal and coal-derived particles. Original soils, soils' light fractions (rhoextractable contaminants ranged from decades for 2-4-ring PAHs and hundreds of years for 5-6-ring PAHs. We demonstrate that, despite high soil PAH concentrations which are due to coal and coal-derived particles, the general environmental risk is reduced by the very slow and extremely slow desorption rates.

  2. Thermally assisted desorption processes in electron bombarded alkali halides

    Energy Technology Data Exchange (ETDEWEB)

    Kolodziej, J.; Czuba, P.; Piatkowski, P.; Postawa, Z.; Kempter, V.; Szymonski, M. (Uniwersytet Jagiellonski, Cracow (Poland). Inst. Fizyki)

    The desorption of alkali and halogen atoms induced by the interaction of energetic electrons with surfaces of alkali halide crystals has been studied by means of an angular-resolved and mass-selected time-of-flight spectroscopy. It has been found that a considerable fraction of halogen atoms was ejected with hyperthermal energies of the order of 0.1 eV. However, alkali atoms and the remaining part of halogen emission had thermal (Maxwellian) spectra of kinetic energies. In this paper we will report on systematic investigations of these thermal desorption processes for single crystal (100) NaCl, KCl, KBr, RbBr, and Kl surfaces. The relative yield of the thermal component has been measured as a function of electron beam energy and beam current density at various sample temperatures. It will be shown that thermal halogen emission can be explained by thermally assisted diffusion of interstitial halogen atoms produced in the bulk of the crystal from decaying self-trapped excitons. The origin of the alkali atom component will be described as due to neutralization and subsequent thermal evaporation of excess alkali atoms from the halogen deficient surface. (Author).

  3. Thermal Desorption of Water-Ice in the Interstellar Medium

    CERN Document Server

    Fraser, H J; McCoustra, M R S; Williams, D A; Fraser, Helen J.; Collings, Mark P.; Coustra, Martin R.S. Mc; Williams, David A.

    2001-01-01

    Water (H2O) ice is an important solid constituent of many astrophysical environments. To comprehend the role of such ices in the chemistry and evolution of dense molecular clouds and comets, it is necessary to understand the freeze-out, potential surface reactivity, and desorption mechanisms of such molecular systems. Consequently, there is a real need from within the astronomical modelling community for accurate empirical molecular data pertaining to these processes. Here we give the first results of a laboratory programme to provide such data. Measurements of the thermal desorption of H2O ice, under interstellar conditions, are presented. For ice deposited under conditions that realistically mimic those in a dense molecular cloud, the thermal desorption of thin films (~50 molecular layers) is found to occur with zero order kinetics characterised by a surface binding energy, E_{des}, of 5773 +/- 60 K, and a pre-exponential factor, A, of 10^(30 +/- 2) molecules cm^-2 s^-1. These results imply that, in the den...

  4. Thermal desorption of helium from homogeneously implanted graphite

    Science.gov (United States)

    Jung, P.; Schroeder, H.

    1991-11-01

    Super-fine grain graphite (FGG) and pyrolytic carbon (PYC) of thicknesses around 200 μm were homogeneously implanted at room temperature with α-particles (0.5 MeV ≤ Eα ≤ 22 MeV). Thermal helium desorption spectrometry in the temperature range from 400 to 1900 K can be described by diffusion kinetics with an activation energy of 1.1 eV in FGG and about 0.75 eV in PYC. Desorption during temperature ramping at a constant rate of 0.83 K/s also shows significant differences of the two graphite species. It is found that in FGG and especially in PYC a considerable fraction of the implanted helium is retained even beyond 1000 K. This is in contrast to results reported after low energy implantations to high doses for various graphite species.

  5. Study of Thermal Desorption of Helium from Hydrogenated Zirconium

    Institute of Scientific and Technical Information of China (English)

    SUN Wei-Ming; WEI Yu-Cheng; SHI Li-Qun

    2006-01-01

    @@ A new method prepared for helium and hydrogen co-containing Zr films is presented to simulate aging metal tritides, in which direct current magnetron sputtering with a He/H/Ar mixture is used. The retained amount and depth profiles of helium and hydrogen are determined by elastic recoil detection analysis. Thermal desorption spectrometry is applied to investigate He thermal release and the effect of hydrogen. It is found that the hightemperature peaks with a large mount of helium release obviously shifted toward lower temperature at high hydrogen concentration, especially at the hydride transformation region, and that the shapes of the release peaks also changed due to the additional hydrogen. However, at the low-temperature releasing region the peak intense decreases when phase transformation takes place. The mechanism of helium thermal release and the effect of hydrogen are also discussed.

  6. Thermal desorption of circumstellar and cometary ice analogs

    CERN Document Server

    Martín-Doménech, Rafael; Bueno, Juan; Goesmann, Fred

    2014-01-01

    Thermal annealing of interstellar ices takes place in several stages of star formation. Knowledge of this process comes from a combination of astronomical observations and laboratory simulations under astrophysically relevant conditions. For the first time we present the results of temperature programmed desorption (TPD) experiments with pre-cometary ice analogs composed of up to five molecular components: H2 O, CO, CO2, CH3 OH, and NH3 . The experiments were performed with an ultra-high vacuum chamber. A gas line with a novel design allows the controlled preparation of mixtures with up to five molecular components. Volatiles desorbing to the gas phase were monitored using a quadrupole mass spectrometer, while changes in the ice structure and composition were studied by means of infrared spectroscopy. The TPD curves of water ice containing CO, CO2, CH3 OH, and NH3 present desorption peaks at temperatures near those observed in pure ice experiments, volcano desorption peaks after water ice crystallization, and...

  7. Thermal desorption of PCBs from contaminated soil with copper dichloride.

    Science.gov (United States)

    Liu, Jie; Qi, Zhifu; Li, Xiaodong; Chen, Tong; Buekens, Alfons; Yan, Jianhua; Ni, Mingjiang

    2015-12-01

    Copper dichloride is an important catalyst both in the dechlorination of chlorinated aromatic compounds and the formation of PCDD/Fs. The effect of copper dichloride on polychlorinated biphenyls (PCBs), polychlorinated dibenzo-p-dioxins (PCDDs), and polychlorinated dibenzofurans (PCDFs) was studied in treated soil and off gas after thermal desorption of PCB-contaminated soil at 300, 400, 500, 600 °C. The presence of copper dichloride clearly enhances thermal desorption by promoting PCBs removal, destruction, and dechlorination. After thermal treatment at 600 °C for 1 h, the removal efficiency and destruction efficiency for PCBs reached 98.1 and 93.9%, respectively. Compared with the positive influence on PCBs, copper dichloride catalyzed large amount of PCDFs formation at 300 °C, with the concentration ratio of 2.35. The effect of CuCl2 on PCDFs formation weakened with the rising temperature since PCDFs destruction became dominant under higher temperature. Different from PCDFs, PCDDs concentration in treated soil and off gas decreased continuously with the increasing temperature.

  8. Application of thermal desorption for the identification of mercury species in solids derived from coal utilization.

    Science.gov (United States)

    Rumayor, M; Diaz-Somoano, M; Lopez-Anton, M A; Martinez-Tarazona, M R

    2015-01-01

    The speciation of mercury is currently attracting widespread interest because the emission, transport, deposition and behaviour of toxic mercury species depend on its chemical form. The identification of these species in low concentrations is no easy task and it is even more complex in coal combustion products due to the fact that these products contain organic and mineral matter that give rise to broad peaks and make it difficult to carry out qualitative and quantitative analysis. In this work, a solution to this problem is proposed using a method based on thermal desorption. A sequential extraction procedure was employed for the comparison and validation of the method developed. Samples of fly ashes and soils were analyzed by both of these methods, and thermal desorption was found to be an appropriate technique for mercury speciation. Even in the case of low mercury contents, recovery percentages were close to 100%. The main mercury species identified in the samples studied were HgS and, to a lesser extent, HgO and HgSO4. In addition, although the presence of mercury complexes cannot be demonstrated, the desorption behaviour and sequential extraction results suggest that this element might be associated with the mineral matrix or with carbon particles in some of the solids. Copyright © 2014 Elsevier Ltd. All rights reserved.

  9. Wheat Growth in Soils Treated by Ex Situ Thermal Desorption.

    Science.gov (United States)

    O'Brien, Peter L; DeSutter, Thomas M; Casey, Francis X M; Wick, Abbey F; Khan, E

    2017-07-01

    Successful remediation of oil-contaminated agricultural land may include the goal of returning the land to prespill levels of agricultural productivity. This productivity may be measured by crop yield, quality, and safety, all of which are influenced by soil characteristics. This research was conducted to determine if these metrics are affected in hard red spring wheat ( L. cultivar Barlow) when grown in soils treated by ex situ thermal desorption (TD) compared with wheat grown in native topsoil (TS). Additionally, TD soils were mixed with TS at various ratios to assess the effectiveness of soil mixing as a procedure for enhancing productivity. In two greenhouse studies, TD soils alone produced similar amounts of grain and biomass as TS, although grain protein in TD soils was 22% (±7%) lower. After mixing TS into TD soils, the mean biomass and grain yield were reduced by up to 60%, but grain protein increased. These trends are likely the result of nutrient availability determined by soil organic matter and nutrient cycling performed by soil microorganisms. Thermal desorption soil had 84% (±2%) lower soil organic carbon than TS, and cumulative respiration was greatly reduced (66 ± 2%). From a food safety perspective, grain from TD soils did not show increased uptake of polycyclic aromatic hydrocarbons. Overall, this research suggests that TD soils are capable of producing safe, high-quality grain yields. Copyright © by the American Society of Agronomy, Crop Science Society of America, and Soil Science Society of America, Inc.

  10. Orbital dynamics of a solar sail accelerated by thermal desorption of coatings

    OpenAIRE

    2016-01-01

    In this study we considered a solar sail coated with materials that undergo thermal desorption at a specific temperature, as a result of heating by solar radiation at a particular heliocentric distance. Three different scenarios, that only differ in the way the sail approaches the Sun, were analyzed and compared. In every case once the perihelion is reached, the sail coat undergoes thermal desorption. When the desorption process ends, the sail then escapes the Solar System having the conventi...

  11. Apparatus for low temperature thermal desorption spectroscopy of portable samples

    Science.gov (United States)

    Stuckenholz, S.; Büchner, C.; Ronneburg, H.; Thielsch, G.; Heyde, M.; Freund, H.-J.

    2016-04-01

    An experimental setup for low temperature thermal desorption spectroscopy (TDS) integrated in an ultrahigh vacuum-chamber housing a high-end scanning probe microscope for comprehensive multi-tool surface science analysis is described. This setup enables the characterization with TDS at low temperatures (T > 22 K) of portable sample designs, as is the case for scanning probe optimized setups or high-throughput experiments. This combination of techniques allows a direct correlation between surface morphology, local spectroscopy, and reactivity of model catalysts. The performance of the multi-tool setup is illustrated by measurements of a model catalyst. TDS of CO from Mo(001) and from Mo(001) supported MgO thin films were carried out and combined with scanning tunneling microscopy measurements.

  12. ENRICHMENT OF TRACE AMOUNTS OF PESTICIDES IN POLLUTED WATER BY A NOVEL TYPE OF SOLID PHASE EXTRACTION ELEMENT FOR THEIR THERMAL DESORPTION GC/MS ANALYSIS%新型固相萃取器用于污染水样中痕量杀虫剂的浓缩及热解吸气相色谱-质谱分析

    Institute of Scientific and Technical Information of China (English)

    2003-01-01

    A novel type of solid-phase extraction element named"Magic Chemisorber" is developed for sorptive enrichment of dilute analytes from aqueous samples with high extraction efficiencies due to its capacious layer of sorbent polydimethylsiloxane.This extraction element combined with thermal desorption-gas chromatography/mass spectrometry using a pyrolysis-GC/MS system was applied to extract the pesticides from water samples over a concentration range of 10-3 to 103 μg*l-1.The method showed good li-nearity for the tested concentration range with regression coefficients of 0.995 for over 5 decades.Limits of detection at a sub-ng*l-1(ppt)level were achieved and the reproducibility of the measurements was found to be fairly good,with relative standard deviation below 8%.

  13. Orbital dynamics of a solar sail accelerated by thermal desorption of coatings

    CERN Document Server

    Ancona, Elena

    2016-01-01

    In this study we considered a solar sail coated with materials that undergo thermal desorption at a specific temperature, as a result of heating by solar radiation at a particular heliocentric distance. Three different scenarios, that only differ in the way the sail approaches the Sun, were analyzed and compared. In every case once the perihelion is reached, the sail coat undergoes thermal desorption. When the desorption process ends, the sail then escapes the Solar System having the conventional acceleration due to solar radiation pressure. Thermal desorption here comes as an additional source of solar sail acceleration beside traditional propulsion systems for extrasolar space exploration. The compared scenarios are the following: i. Hohmann transfer plus thermal desorption. In this scenario the sail would be carried as a payload to the perihelion with a conventional propulsion system by an Hohmann transfer from Earth's orbit to an orbit very close to the Sun (almost at 0.1 AU) and then be deployed there. i...

  14. Precursor ion scan profiles of acylcarnitines by atmospheric pressure thermal desorption chemical ionization tandem mass spectrometry.

    Science.gov (United States)

    Paglia, Giuseppe; D'Apolito, Oceania; Corso, Gaetano

    2008-12-01

    The fatty acyl esters of L-carnitine (acylcarnitines) are useful biomarkers for the diagnosis of some inborn errors of metabolism analyzed by liquid chromatography/tandem mass spectrometry. In this study the acylcarnitines were analyzed by atmospheric pressure thermal desorption chemical ionization using a commercial tandem mass spectrometer (APTDCI-MS/MS). The method is based on the precursor ion scan mode determination of underivatized acylcarnitines desorbed from samples by a hot desolvation gas flow and ionized by a corona pin discharge. During desorption/ionization step the temperature induces the degradation of acylcarnitines; nevertheless, the common fragment to all acylcarnitines [MH-59](+) is useful for analyzing their profile. APTDCI parameters, including angle of collection and incidence, gas flows and temperatures, were optimized for acylcarnitines. The experiments were performed drying 2 microL of an equimolar mixture of acylcarnitine standards on a glass slide. The specificity was evaluated by comparing product ion spectra and the precursor ion spectra of 85 m/z of acylcarnitines obtained by the APTDCI method and by electrospray ionization flow injection analysis (ESI-FIA). The method was also employed to analyze acylcarnitines extracted from a pathological dried blood spot and a control. The method enables analysis of biological samples and recognition of some acylcarnitines that are diagnostic markers of inherited metabolic diseases. The intrinsic high-throughput analysis of the ambient desorption ionization methods offers a new opportunity either for its potential application in clinical chemistry and for the expanded screening of some inborn errors of metabolism.

  15. Mercury speciation during in situ thermal desorption in soil

    Energy Technology Data Exchange (ETDEWEB)

    Park, Chang Min, E-mail: cmpark80@gmail.com; Katz, Lynn E.; Liljestrand, Howard M.

    2015-12-30

    Highlights: • Impact of soil conditions on distribution and phase transitions of Hg was identified. • Metallic Hg was slowly transformed to Hg{sup 0} gas until the temperature reached 358.15 K. • Phase change of HgCl{sub 2(s)} completely occurred without decomposition at 335.15 K. • HgS remained solid in dry soil sharply decreased in the narrow temperature range. • Hg gas can be easily captured with higher vapor pressures of soil compositions. - Abstract: Metallic mercury (Hg{sup 0}) and its compounds are highly mobile and toxic environmental pollutants at trace level. In situ thermal desorption (ISTD) is one of the soil remediation processes applying heat and vacuum simultaneously. Knowledge of thermodynamic mercury speciation is imperative to understand the fate and transport of mercury during thermal remediation and operate the treatment processes in a cost-effective manner. Hence, speciation model for inorganic mercury was developed over a range of environmental conditions to identify distribution of dissolved mercury species and potential transformations of mercury at near source environment. Simulation of phase transitions for metallic mercury, mercury(II) chloride and mercury sulfide with temperature increase showed that complete vaporization of metallic mercury and mercury(II) chloride were achieved below the boiling point of water. The effect of soil compositions on mercury removal was also evaluated to better understand thermal remediation process. Higher vapor pressures expected both from soil pore water and inorganic carbonate minerals in soil as well as creation of permeability were significant for complete vaporization and removal of mercury.

  16. Multivariate analysis of progressive thermal desorption coupled gas chromatography-mass spectrometry.

    Energy Technology Data Exchange (ETDEWEB)

    Van Benthem, Mark Hilary; Mowry, Curtis Dale; Kotula, Paul Gabriel; Borek, Theodore Thaddeus, III

    2010-09-01

    Thermal decomposition of poly dimethyl siloxane compounds, Sylgard{reg_sign} 184 and 186, were examined using thermal desorption coupled gas chromatography-mass spectrometry (TD/GC-MS) and multivariate analysis. This work describes a method of producing multiway data using a stepped thermal desorption. The technique involves sequentially heating a sample of the material of interest with subsequent analysis in a commercial GC/MS system. The decomposition chromatograms were analyzed using multivariate analysis tools including principal component analysis (PCA), factor rotation employing the varimax criterion, and multivariate curve resolution. The results of the analysis show seven components related to offgassing of various fractions of siloxanes that vary as a function of temperature. Thermal desorption coupled with gas chromatography-mass spectrometry (TD/GC-MS) is a powerful analytical technique for analyzing chemical mixtures. It has great potential in numerous analytic areas including materials analysis, sports medicine, in the detection of designer drugs; and biological research for metabolomics. Data analysis is complicated, far from automated and can result in high false positive or false negative rates. We have demonstrated a step-wise TD/GC-MS technique that removes more volatile compounds from a sample before extracting the less volatile compounds. This creates an additional dimension of separation before the GC column, while simultaneously generating three-way data. Sandia's proven multivariate analysis methods, when applied to these data, have several advantages over current commercial options. It also has demonstrated potential for success in finding and enabling identification of trace compounds. Several challenges remain, however, including understanding the sources of noise in the data, outlier detection, improving the data pretreatment and analysis methods, developing a software tool for ease of use by the chemist, and demonstrating our belief

  17. Thermal desorption of deuterium from modified carbon nanotubes and its correlation to the microstructure

    NARCIS (Netherlands)

    Lisowski, W.; Keim, E.G.; Berg, van den A.H.J.; Smithers, M.A.

    2006-01-01

    The process of deuterium desorption from single-wall carbon nanotubes (SWNTs) modified by atomic (D) and molecular (D2) deuterium treatment was investigated in an ultrahigh vacuum environment using thermal desorption mass spectroscopy (TDMS). Microstructural and chemical analyses of SWNT material, m

  18. Desorption of isopropyl alcohol from adsorbent with non-thermal plasma.

    Science.gov (United States)

    Shiau, Chen Han; Pan, Kuan Lun; Yu, Sheng Jen; Yan, Shaw Yi; Chang, Moo Been

    2016-11-24

    Effective desorption of isopropyl alcohol (IPA) from adsorbents with non-thermal plasma is developed. In this system, IPA is effectively adsorbed with activated carbon while dielectric barrier discharge is applied to replace the conventional thermal desorption process to achieve good desorption efficiency, making the treatment equipment smaller in size. Various adsorbents including molecular sieves and activated carbon are evaluated for IPA adsorption capacity. The results indicate that BAC has the highest IPA adsorption capacity (280.31 mg IPA/g) under the operating conditions of room temperature, IPA of 400 ppm, and residence time of 0.283 s among 5 adsorbents tested. For the plasma desorption process, the IPA selectivity of 89% is achieved with BAC as N2 is used as desorbing gas. In addition, as air or O2 is used as desorbing gas, the IPA desorption concentration is reduced, because air and O2 plasmas generate active species to oxidize IPA to form acetone, CO2, and even CO. Furthermore, the results of the durability test indicate that the amount of IPA desorbed increases with increasing desorption times and plasma desorption process has a higher energy efficiency if compared with thermal desorption. Overall, this study indicates that non-thermal plasma is a viable process for removing VOCs to regenerate adsorbent.

  19. Bonding configurations for nickelocene on Ag(100) and steric effects in thermal desorption

    Energy Technology Data Exchange (ETDEWEB)

    Borca, C.N.; Welipitiya, D.; Dowben, P.A.; Boag, N.M.

    2000-02-10

    The molecular adsorption and desorption of nickelocene, Ni(C{sub 5}H{sub 5}){sub 2}, on Ag(100) has been studied by coverage dependent angle-resolved thermal desorption. The angle-resolved thermal desorption of nickelocene is unusual in that the molecular orientation is seen to affect the angular dependence of molecular desorption. The coexistence of two chemisorption phases for molecular nickelocene adsorption on Ag(100) near the desorption temperature of approximately 230 K is identified. One phase, with the bonding configuration of the nickelocene molecular axis along the surface normal, appears to dominate at higher coverages. The results are discussed in the context of rehybridization and recent angle-resolved photoemission and high-resolution electron energy loss measurements.

  20. Decomposition kinetics study of zirconium hydride by interrupted thermal desorption spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Ma, Mingwang; Liang, Li; Tang, Binghua; Xiang, Wei; Wang, Yuan; Cheng, Yanlin; Tan, Xiaohua, E-mail: caepiee@163.com

    2015-10-05

    Highlights: • Interrupted TDS was applied to investigate the mechanism of ZrH{sub 2} decomposition. • The activation energies for the five desorption peaks were determined. • The origins of the five desorption peaks were identified. • The γZrH phase was observed at ambient conditions. - Abstract: Thermal desorption kinetics of zirconium hydride powder were studied using thermogravimetry and simultaneous thermal desorption spectroscopy. The activation energies for observed desorption peaks were estimated according to Kissinger relation. The intermediate phase composition was studied using X-ray diffraction by rapid cooling on different stages of heating. The origins of the peaks were described as the equilibrium hydrogen pressure of a number of consecutive phase regions that decomposition reaction passed through. The zirconium monohydride γZrH was observed for extended periods of time at ambient conditions, which has been supposed to be metastable for a long time.

  1. Adsorption, Diffusion and Thermal Desorption Features of Cyclopentane and Cyclohexane in Silicalite-1

    Institute of Scientific and Technical Information of China (English)

    DUAN, Lin-Hai; SONG, Li-Juan; ZHANG, Xiao-Tong; TANG, Ke; DAI, Zhen-Hua; SUN, Zhao-Lin

    2006-01-01

    Adsorption, diffusion and thermal desorption features of cyclopentane and cyclohexane in silicalite-1 have been investigated using the intelligent gravimetric technique. Both the saturation adsorption loadings and diffusion coefficient of cyclopentane were greater than those of cyclohexane. The diffusivity of cyclopentane was about one order of magnitude greater than that of cyclohexane at the same temperature and initial loading. For cyclopentane, there was only one kind of desorption process at adsorption loadings lower than 4 muc (molecule per unit cell), but two desorption processes appeared at the adsorption loadings higher than 4 muc. While for cyclohexane, one desorption process was found in the whole range of loadings. Both thermal desorption peaks of cyclopentane and cyclohexane moved to higher temperature region with increasing loading.

  2. Treating high-mercury-containing lamps using full-scale thermal desorption technology.

    Science.gov (United States)

    Chang, T C; You, S J; Yu, B S; Chen, C M; Chiu, Y C

    2009-03-15

    The mercury content in high-mercury-containing lamps are always between 400 mg/kg and 200,000 mg/kg. This concentration is much higher than the 260 mg/kg lower boundary recommended for the thermal desorption process suggested by the US Resource Conservation and Recovery Act. According to a Taiwan EPA survey, about 4,833,000 cold cathode fluorescent lamps (CCFLs), 486,000 ultraviolet lamps and 25,000 super high pressure mercury lamps (SHPs) have been disposed of in the industrial waste treatment system, producing 80, 92 and 9 kg-mercury/year through domestic treatment, offshore treatment and air emissions, respectively. To deal with this problem we set up a full-scale thermal desorption process to treat and recover the mercury from SHPs, fluorescent tube tailpipes, fluorescent tubes containing mercury-fluorescent powder, and CCFLs containing mercury-fluorescent powder and monitor the use of different pre-heating temperatures and desorption times. The experimental results reveal that the average thermal desorption efficiency of SHPs and fluorescent tube tailpipe were both 99.95%, while the average thermal desorption efficiencies of fluorescent tubes containing mercury-fluorescent powder were between 97% and 99%. In addition, a thermal desorption efficiency of only 69.37-93.39% was obtained after treating the CCFLs containing mercury-fluorescent powder. These differences in thermal desorption efficiency might be due to the complexity of the mercury compounds contained in the lamps. In general, the thermal desorption efficiency of lamps containing mercury-complex compounds increased with higher temperatures.

  3. Operable Unit 7-13/14 in situ thermal desorption treatability study work plan

    Energy Technology Data Exchange (ETDEWEB)

    Shaw, P.; Nickelson, D.; Hyde, R.

    1999-05-01

    This Work Plan provides technical details for conducting a treatability study that will evaluate the application of in situ thermal desorption (ISTD) to landfill waste at the Subsurface Disposal Area (SDA) at the Idaho National Engineering and Environmental Laboratory (INEEL). ISTD is a form of thermally enhanced vapor vacuum extraction that heats contaminated soil and waste underground to raise its temperature and thereby vaporize and destroy most organics. An aboveground vapor vacuum collection and treatment system then destroys or absorbs the remaining organics and vents carbon dioxide and water to the atmosphere. The technology is a byproduct of an advanced oil-well thermal extraction program. The purpose of the ISTD treatability study is to fill performance-based data gaps relative to off-gas system performance, administrative feasibility, effects of the treatment on radioactive contaminants, worker safety during mobilization and demobilization, and effects of landfill type waste on the process (time to remediate, subsidence potential, underground fires, etc.). By performing this treatability study, uncertainties associated with ISTD as a selected remedy will be reduced, providing a better foundation of remedial recommendations and ultimate selection of remedial actions for the SDA.

  4. Modelling of hydrogen thermal desorption spectrum in nonlinear dynamical boundary-value problem

    Science.gov (United States)

    Kostikova, E. K.; Zaika, Yu V.

    2016-11-01

    One of the technological challenges for hydrogen materials science (including the ITER project) is the currently active search for structural materials with various potential applications that will have predetermined limits of hydrogen permeability. One of the experimental methods is thermal desorption spectrometry (TDS). A hydrogen-saturated sample is degassed under vacuum and monotone heating. The desorption flux is measured by mass spectrometer to determine the character of interactions of hydrogen isotopes with the solid. We are interested in such transfer parameters as the coefficients of diffusion, dissolution, desorption. The paper presents a distributed boundary-value problem of thermal desorption and a numerical method for TDS spectrum simulation, where only integration of a nonlinear system of low order (compared with, e.g., the method of lines) ordinary differential equations (ODE) is required. This work is supported by the Russian Foundation for Basic Research (project 15-01-00744).

  5. Decomposition of thin titanium deuteride films; thermal desorption kinetics studies combined with microstructure analysis

    NARCIS (Netherlands)

    Lisowski, Wojciech; Keim, Enrico G.; Kaszkur, Zbigniew; Smithers, Mark A.

    2008-01-01

    The thermal evolution of deuterium from thin titanium films, prepared under UHV conditions and deuterated in situ at room temperature, has been studied by means of thermal desorption mass spectrometry (TDMS) and a combination of scanning electron microscopy (SEM), transmission electron microscopy (T

  6. Determination of off-flavor compounds, 2-methylisoborneol and geosmin, in salmon fillets using stir bar sorptive extraction–thermal desorption coupled with gas chromatography–mass spectrometry

    Science.gov (United States)

    A sensitive and solvent-less method for the determination of musty and earthy off-flavor compounds, 2-methylisoborneol (MIB) and geosmin (GSM), in salmon tissue was developed using stir bar sorptive extraction -thermal desorption coupled with gas chromatography -mass spectrometry (SBSE -TD -GCMS). M...

  7. Ocean Thermal Extractable Energy Visualization

    Energy Technology Data Exchange (ETDEWEB)

    Ascari, Matthew [Lockheed Martin Corporation, Bethesda, MD (United States)

    2012-10-28

    The Ocean Thermal Extractable Energy Visualization (OTEEV) project focuses on assessing the Maximum Practicably Extractable Energy (MPEE) from the world’s ocean thermal resources. MPEE is defined as being sustainable and technically feasible, given today’s state-of-the-art ocean energy technology. Under this project the OTEEV team developed a comprehensive Geospatial Information System (GIS) dataset and software tool, and used the tool to provide a meaningful assessment of MPEE from the global and domestic U.S. ocean thermal resources.

  8. Thermal desorption of CH4 retained in CO2 ice

    CERN Document Server

    Luna, R; Domingo, M; Satorre, M A

    2008-01-01

    CO2 ices are known to exist in different astrophysical environments. In spite of this, its physical properties (structure, density, refractive index) have not been as widely studied as those of water ice. It would be of great value to study the adsorption properties of this ice in conditions related to astrophysical environments. In this paper, we explore the possibility that CO2 traps relevant molecules in astrophysical environments at temperatures higher than expected from their characteristic sublimation point. To fulfil this aim we have carried out desorption experiments under High Vacuum conditions based on a Quartz Crystal Microbalance and additionally monitored with a Quadrupole Mass Spectrometer. From our results, the presence of CH4 in the solid phase above the sublimation temperature in some astrophysical scenarios could be explained by the presence of several retaining mechanisms related to the structure of CO2 ice.

  9. ECO LOGIC INTERNATIONAL GAS-PHASE CHEMICAL REDUCTION PROCESS - THE THERMAL DESORPTION UNIT - APPLICATIONS ANALYSIS REPORT

    Science.gov (United States)

    ELI ECO Logic International, Inc.'s Thermal Desorption Unit (TDU) is specifically designed for use with Eco Logic's Gas Phase Chemical Reduction Process. The technology uses an externally heated bath of molten tin in a hydrogen atmosphere to desorb hazardous organic compounds fro...

  10. Offline thermal-desorption proton-transfer-reaction mass spectrometry to study composition of organic aerosol

    NARCIS (Netherlands)

    Timkovsky, J.; Dusek, U.; Henzing, J. S.; Kuipers, T. L.; Röckmann, T.; Holzinger, R.

    2015-01-01

    We present a novel approach to study the organic composition of aerosol filter samples using thermal-desorption proton-transfer-reaction mass spectrometry (TD-PTR-MS) in the laboratory. The method is tested and validated based on the comparison with in situ TD-PTR-MS measurements. In general, we obs

  11. Helium concentration measurement in tungsten fuzz-like nanostructures by means of thermal desorption spectroscopy

    NARCIS (Netherlands)

    Gasparyan, Y.; Efimov, V.; Bystrov, K.

    2016-01-01

    The concentration of helium in tungsten fuzz-like nanostructures has been measured by means of thermal desorption spectroscopy. Fuzz was formed on the W surface under intensive plasma irradiation at 1500 K. The helium content was measured first in the as-irradiated sample, and then in a similar samp

  12. Thermal desorption from surfaces with laser-induced defects

    Energy Technology Data Exchange (ETDEWEB)

    Szabelski, Pawel; Panczyk, Tomasz; Rudzinski, Wladyslaw

    2002-12-30

    Monte Carlo simulation method was used to mimic surface damage development caused by short laser pulses. The influence of pulsed laser irradiation on the creation of defect concentration was examined in the case of a model surface. In particular, the dependence of the intact surface area on a number of laser scans was studied and compared with the experimental results obtained for Rh(1 1 1) crystal face. Changes in the adsorptivoperties of the surface produced by laser irradiation are explained with the help of a simple geometric model connecting the laser intensity and the disordered area generated by a single laser shot. It was demonstrated that exponential decay of the Low Energy Electron Diffraction (LEED) signal with the number of laser scans, which is observed experimentally, may result directly from the overlapping of the laser spots created on the surface. This effect becomes enhanced when the laser intensity, hence the spot size, increases. The importance of laser-induced defects in the kinetics of catalytic/separation processes was examined in the case of temperature programmed desorption (TPD) spectra from surfaces subjected to a different number of laser shots. The spectra were simulated by employing the Monte Carlo method as well as by application of the absolute rate theory (ART) coupled with the mean field approximation. The results obtained with both methods were in a good agreement even when weak lateral interactions in the adsorbed phase were allowed.

  13. Impact of Thermal Decomposition on Thermal Desorption Instruments: Advantage of Thermogram Analysis for Quantifying Volatility Distributions of Organic Species.

    Science.gov (United States)

    Stark, Harald; Yatavelli, Reddy L N; Thompson, Samantha L; Kang, Hyungu; Krechmer, Jordan E; Kimmel, Joel R; Palm, Brett B; Hu, Weiwei; Hayes, Patrick L; Day, Douglas A; Campuzano-Jost, Pedro; Canagaratna, Manjula R; Jayne, John T; Worsnop, Douglas R; Jimenez, Jose L

    2017-08-01

    We present results from a high-resolution chemical ionization time-of-flight mass spectrometer (HRToF-CIMS), operated with two different thermal desorption inlets, designed to characterize the gas and aerosol composition. Data from two field campaigns at forested sites are shown. Particle volatility distributions are estimated using three different methods: thermograms, elemental formulas, and measured partitioning. Thermogram-based results are consistent with those from an aerosol mass spectrometer (AMS) with a thermal denuder, implying that thermal desorption is reproducible across very different experimental setups. Estimated volatilities from the detected elemental formulas are much higher than from thermograms since many of the detected species are thermal decomposition products rather than actual SOA molecules. We show that up to 65% of citric acid decomposes substantially in the FIGAERO-CIMS, with ∼20% of its mass detected as gas-phase CO2, CO, and H2O. Once thermal decomposition effects on the detected formulas are taken into account, formula-derived volatilities can be reconciled with the thermogram method. The volatility distribution estimated from partitioning measurements is very narrow, likely due to signal-to-noise limits in the measurements. Our findings indicate that many commonly used thermal desorption methods might lead to inaccurate results when estimating volatilities from observed ion formulas found in SOA. The volatility distributions from the thermogram method are likely the closest to the real distributions.

  14. Activation energy of thermal desorption of silicon oxide layers on silicon substrates

    Science.gov (United States)

    Enta, Yoshiharu; Osanai, Shodai; Ogasawara, Takahito

    2017-02-01

    Thermal desorption rates of silicon oxide layers, from 20 to 120 nm in thickness, on silicon substrates in vacuum have been accurately obtained from intervals between ring structures formed inside voids on the oxide layers. From the temperature dependence of the desorption rate, the activation energy and frequency factor of the desorption reaction have been derived as a function of the oxide thickness. The obtained values are compared with the previous studies, and as a result, the activation energy is found to be almost constant ( 4 eV) in a wide range of the oxide thickness. The frequency factor decreases as the inverse square of the oxide thickness. The decomposition kinetics of the oxide layer is also discussed from the obtained results.

  15. Non-isothermal kinetics of the thermal desorption of mercury from a contaminated soil

    Energy Technology Data Exchange (ETDEWEB)

    Lopez, F. A.; Sierra, M. J.; Rodriguez, O.; Millan, R.; Alguacil, F. J.

    2014-04-01

    The Almaden mining district (Ciudad Real, Spain) was the largest cinnabar (mercury sulphide) mine in the world. Its soils have high levels of mercury a consequence of its natural lithology, but often made much worse by its mining history. The present work examines the thermal desorption of two contaminated soils from the Almaden area under non-isothermal conditions in a N{sub 2} atmosphere, using differential scanning calorimetry (DSC). DSC was performed at different heating rates between room temperature and 600 degree centigrade. Desorption temperatures for different mercury species were determined. The Friedman, Flynn-Wall-Ozawa and Coasts Redfern methods were employed to determine the reaction kinetics from the DSC data. The activation energy and pre-exponential factor for mercury desorption were calculated. (Author)

  16. PCDD/F formation during thermal desorption of p,p'-DDT contaminated soil.

    Science.gov (United States)

    Zhao, Zhonghua; Ni, Mingjiang; Li, Xiaodong; Buekens, Alfons; Yan, Jianhua

    2017-05-01

    Thermal treatment of polychlorinated biphenyls (PCB) contaminated soil was shown in earlier work to generate polychlorinated dibenzo-p-dioxins (PCDD) and polychlorinated dibenzofurans (PCDF). In this study, the PCDD/F were studied arising during the remediation of p,p'-DDT contaminated soil by thermal desorption. Three kinds of soil (sandy, clayey and lateritic soil) were tested to investigate the effect of soil texture on PCDD/F formation. Those soils were artificially polluted with p,p'-DDT, obtaining a concentration level of 100 mg/kg. Thermal desorption experiments were conducted for 10 min at 300 °C in an air atmosphere. The total concentration of PCDD/F generated for three soils were 331, 803 and 865 ng/kg, respectively, and TeCDD and TeCDF were dominant among all PCDD/F congeners. After thermal desorption, the total amount of PCDD/F generated both in soil and in off-gas correlated positively with the amount of DDT added to soil. In addition, a possible pathway of the formation of PCDD/F was presented.

  17. Organic and inorganic decomposition products from the thermal desorption of atmospheric particles

    Science.gov (United States)

    Williams, Brent J.; Zhang, Yaping; Zuo, Xiaochen; Martinez, Raul E.; Walker, Michael J.; Kreisberg, Nathan M.; Goldstein, Allen H.; Docherty, Kenneth S.; Jimenez, Jose L.

    2016-04-01

    Atmospheric aerosol composition is often analyzed using thermal desorption techniques to evaporate samples and deliver organic or inorganic molecules to various designs of detectors for identification and quantification. The organic aerosol (OA) fraction is composed of thousands of individual compounds, some with nitrogen- and sulfur-containing functionality and, often contains oligomeric material, much of which may be susceptible to decomposition upon heating. Here we analyze thermal decomposition products as measured by a thermal desorption aerosol gas chromatograph (TAG) capable of separating thermal decomposition products from thermally stable molecules. The TAG impacts particles onto a collection and thermal desorption (CTD) cell, and upon completion of sample collection, heats and transfers the sample in a helium flow up to 310 °C. Desorbed molecules are refocused at the head of a gas chromatography column that is held at 45 °C and any volatile decomposition products pass directly through the column and into an electron impact quadrupole mass spectrometer. Analysis of the sample introduction (thermal decomposition) period reveals contributions of NO+ (m/z 30), NO2+ (m/z 46), SO+ (m/z 48), and SO2+ (m/z 64), derived from either inorganic or organic particle-phase nitrate and sulfate. CO2+ (m/z 44) makes up a major component of the decomposition signal, along with smaller contributions from other organic components that vary with the type of aerosol contributing to the signal (e.g., m/z 53, 82 observed here for isoprene-derived secondary OA). All of these ions are important for ambient aerosol analyzed with the aerosol mass spectrometer (AMS), suggesting similarity of the thermal desorption processes in both instruments. Ambient observations of these decomposition products compared to organic, nitrate, and sulfate mass concentrations measured by an AMS reveal good correlation, with improved correlations for OA when compared to the AMS oxygenated OA (OOA

  18. VAC*TRAX - thermal desorption for mixed wastes

    Energy Technology Data Exchange (ETDEWEB)

    McElwee, M.J.; Palmer, C.R. [RUST-Clemson Technical Center, Anderson, SC (United States)

    1995-10-01

    The patented VAC*TRAX process was designed in response to the need to remove organic constituents from mixed waste, waste that contains both a hazardous (RCRA or TSCA regulated) component and a radioactive component. Separation of the mixed waste into its hazardous and radioactive components allows for ultimate disposal of the material at existing, permitted facilities. The VAC*TRAX technology consists of a jacketed vacuum dryer followed by a condensing train. Solids are placed in the dryer and indirectly heated to temperatures as high as 2600{degrees}C, while a strong vacuum (down to 50 mm Hg absolute pressure) is applied to the system and the dryer is purged with a nitrogen carrier gas. The organic contaminants in the solids are thermally desorbed, swept up in the carrier gas and into the condensing train where they are cooled and recovered. The dryer is fitted with a filtration system that keeps the radioactive constituents from migrating to the condensate. As such, the waste is separated into hazardous liquid and radioactive solid components, allowing for disposal of these streams at a permitted incinerator or a radioactive materials landfill, respectively. The VAC*TRAX system is designed to be highly mobile, while minimizing the operational costs with a simple, robust process. These factors allow for treatment of small waste streams at a reasonable cost.

  19. Organic and inorganic decomposition products from the thermal desorption of atmospheric particles

    OpenAIRE

    Williams, Brent J.; Zhang, Yaping; Zuo, Xiaochen; Martinez, Raul E.; Walker, Michael J.; Kreisberg, Nathan M.; Goldstein, Allen H.; Docherty, Kenneth S.; Jimenez, Jose L.

    2016-01-01

    Atmospheric aerosol composition is often analyzed using thermal desorption techniques to evaporate samples and deliver organic or inorganic molecules to various designs of detectors for identification and quantification. The organic aerosol (OA) fraction is composed of thousands of individual compounds, some with nitrogen- and sulfur-containing functionality and, often contains oligomeric material, much of which may be susceptible to decomposition upon heating. Here we analy...

  20. Organic and inorganic decomposition products from the thermal desorption of atmospheric particles

    OpenAIRE

    B. J. Williams; Y. Zhang; X. Zuo; R. E. Martinez; Walker, M. J.; N. M. Kreisberg; Goldstein, A. H.; K. S. Docherty; Jimenez, J.L.

    2015-01-01

    Atmospheric aerosol composition is often analyzed using thermal desorption techniques to evaporate samples and deliver organic or inorganic molecules to various designs of detectors for identification and quantification. The organic aerosol (OA) fraction is composed of thousands of individual compounds, some with nitrogen- and sulfur-containing functionality, and often contains oligomeric material, much of which may be susceptible to decomposition upon heating. Here we analy...

  1. Layer resolved spectroscopy of potassium adsorbed on a Ru(001) surface: Photoemission and thermal desorption study

    Energy Technology Data Exchange (ETDEWEB)

    Hrbek, J. (Chemistry Department, Brookhaven National Laboratory, Upton, New York 11973 (US)); Shek, M. (Department of Physics, Hunter College of CUNY, New York, New York 10021); Sham, T.K. (Department of Chemistry, University of Western Ontario, London, Ontario N6A 5B7, Canada); Xu, G. (Chemistry Department, Brookhaven National Laboratory, Upton, New York, 11973)

    1989-11-01

    High-resolution photoemission spectroscopy and thermal desorption were used to study the coverage dependence of the K 3{ital p}{sub 3/2,1/2} core levels of K overlayers on Ru(001). Three doublets were observed to evolve sequentially and to shift to higher binding energy with increasing coverage of potassium. The doublets were assigned to photoemission from the interface (first layer), bulk'' (second layer), and surface (third layer). Spin--orbit splitting was observed for the first time in the condensed potassium phase by photoemission. The results are discussed in terms of the equivalent core approximation using a Born--Haber cycle. In the thermal desorption data three coverage regimes can be distinguished: a first layer desorbing with first-order kinetics and a strongly decreasing heat of adsorption ({ital E}{sub {ital A}} =2.80--0.87 eV); a second layer with zero-order desorption kinetics and {ital E}{sub {ital A}} =0.78 eV; a third layer and multilayers with the same kinetic order but with {ital E}{sub {ital A}} increasing from 0.78 to 0.93 eV, which is close to the heat of sublimation of potassium.

  2. Non-thermal desorption from interstellar dust grains via exothermic surface reactions

    CERN Document Server

    Garrod, R T; Herbst, E

    2007-01-01

    Aims: The gas-phase abundance of methanol in dark quiescent cores in the interstellar medium cannot be explained by gas-phase chemistry. In fact, the only possible synthesis of this species appears to be production on the surfaces of dust grains followed by desorption into the gas. Yet, evaporation is inefficient for heavy molecules such as methanol at the typical temperature of 10 K. It is necessary then to consider non-thermal mechanisms for desorption. But, if such mechanisms are considered for the production of methanol, they must be considered for all surface species. Methods: Our gas-grain network of reactions has been altered by the inclusion of a non-thermal desorption mechanism in which the exothermicity of surface addition reactions is utilized to break the bond between the product species and the surface. Our estimated rate for this process derives from a simple version of classical unimolecular rate theory with a variable parameter only loosely contrained by theoretical work. Results: Our results ...

  3. Defect annealing and thermal desorption of deuterium in low dose HFIR neutron-irradiated tungsten

    Energy Technology Data Exchange (ETDEWEB)

    Masashi Shimada; M. Hara; T. Otsuka; Y. Oya; Y. Hatano

    2014-05-01

    Accurately estimating tritium retention in plasma facing components (PFCs) and minimizing its uncertainty are key safety issues for licensing future fusion power reactors. D-T fusion reactions produce 14.1 MeV neutrons that activate PFCs and create radiation defects throughout the bulk of the material of these components. Recent studies show that tritium migrates and is trapped in bulk (>> 10 µm) tungsten beyond the detection range of nuclear reaction analysis technique [1-2], and thermal desorption spectroscopy (TDS) technique becomes the only established diagnostic that can reveal hydrogen isotope behavior in in bulk (>> 10 µm) tungsten. Radiation damage and its recovery mechanisms in neutron-irradiated tungsten are still poorly understood, and neutron-irradiation data of tungsten is very limited. In this paper, systematic investigations with repeated plasma exposures and thermal desorption are performed to study defect annealing and thermal desorption of deuterium in low dose neutron-irradiated tungsten. Three tungsten samples (99.99 at. % purity from A.L.M.T. Co., Japan) irradiated at High Flux Isotope Reactor at Oak Ridge National Laboratory were exposed to high flux (ion flux of (0.5-1.0)x1022 m-2s-1 and ion fluence of 1x1026 m-2) deuterium plasma at three different temperatures (100, 200, and 500 °C) in Tritium Plasma Experiment at Idaho National Laboratory. Subsequently, thermal desorption spectroscopy (TDS) was performed with a ramp rate of 10 °C/min up to 900 °C, and the samples were annealed at 900 °C for 0.5 hour. These procedures were repeated three (for 100 and 200 °C samples) and four (for 500 °C sample) times to uncover damage recovery mechanisms and its effects on deuterium behavior. The results show that deuterium retention decreases approximately 90, 75, and 66 % for 100, 200, and 500 °C, respectively after each annealing. When subjected to the same TDS recipe, the desorption temperature shifts from 800 °C to 600 °C after 1st annealing

  4. 搅拌棒萃取-热脱附/气质联用法测定水中2-MIB和土臭素%Determination of 2-Methylisoborneol and Geosmin in Water Using Stir Bar Sorptive Extraction-Thermal Desorption/Gas Chromatography Coupled with Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    范苓; 张晓赟; 秦宏兵; 顾海东

    2013-01-01

    A method using stir bar sorptive extraction ( SBSE)-thermal desorption ( TD)/gas chromatogra-phy coupled with mass spectrometry ( GCMS) was developed to determinate ultra-trace level of 2-methylisoborneol (2-MIB) and geosmin in water .SBSE and TD parameters were optimized through blank spiked sample .The method showed good linearity ( r>0 .999 ) over concentration range from 1 ng/L to 200 ng/L and high sensitivity ( the MDL of 2-MIB and geosmin were 0 .31 ng/L and 0 .15 ng/L respectively ) .The spiked recovery of blank and real samples ranged from 82 .4%to 116%with RSD <10%.%采用搅拌棒萃取-热脱附/气质联用法测定水中2-甲基异莰醇和土臭素,优化了搅拌棒萃取和热脱附进样的条件。试验表明:两种目标化合物在1.00 ng/L~200 ng/L范围内线性良好,2-甲基异莰醇的相关系数为0.9993,土臭素的相关系数为0.9997,方法检出限分别为0.31 ng/L和0.15 ng/L;空白和实际样品的加标回收率为82.4%~116%,测定结果的RSD<10%。

  5. Hydrogen solubility and diffusion in austenitic stainless steels studied with thermal desorption spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Yagodzinskyy, Y.; Todoshchenko, O.; Papula, S.; Haenninen, H. [Laboratory of Engineering Materials, School of Science and Technology, Aalto University, Espoo (Finland)

    2011-01-15

    Hydrogen solubility and diffusion in austenitic stainless steels, namely AISI 310, AISI 301LN and AISI 201, are studied with thermal desorption spectroscopy (TDS) after electrochemical potentiostatic hydrogen pre-charging. Temperature dependencies of hydrogen desorption for all studied steels manifest a complex main peak caused by hydrogen releasing from the steel lattice by diffusion. Depending on the steel and heating rate the peak is situated from 350 to 500 K and its shape reflects a specific of hydrogen diffusion in stainless steels, which are multicomponent alloys. Analysis of the TDS curves is based on the hydrogen diffusion model taking into account trapping of hydrogen atoms in the energetically deep interstitial positions in the steel crystal lattice. Diffusion coefficient of hydrogen and its total content after the same charging procedure are obtained from the TDS curves and compared for the studied steels. (Copyright copyright 2011 Wiley-VCH Verlag GmbH and Co. KGaA, Weinheim)

  6. Determination of metformin in mouse, rat, dog and human plasma samples by laser diode thermal desorption/atmospheric pressure chemical ionization tandem mass spectrometry.

    Science.gov (United States)

    Swales, John G; Gallagher, Richard; Peter, Raimund M

    2010-11-02

    A simple, rapid and robust high-throughput assay for the quantitative analysis of metformin in plasma from different species using laser diode thermal desorption interfaced with atmospheric chemical pressure ionization tandem mass spectrometry (LDTD-APCI-MSMS) was developed for use in a pharmaceutical discovery environment. In order to minimize sample preparation a generic protein precipitation method was used to extract metformin from the plasma. Laser diode thermal desorption is a relatively new sample introduction method, the optimization of the instrumental parameters are presented. The method was successfully applied to spiked mouse, rat, dog and human plasma samples and was subsequently used to determine the oral pharmacokinetics of metformin after dosing to male rats in order to support drug discovery projects. The deviations for intra-assay accuracy and precision across the four species were less than 30% at all calibration and quality control levels.

  7. Thermal desorption characterisation of molecularly imprinted polymers. Part I: A novel study using direct-probe GC-MS analysis.

    Science.gov (United States)

    Cummins, Wayne; Duggan, Patrick; McLoughlin, Peter

    2008-06-01

    A novel thermal desorption technique using a direct-probe device (Chromatoprobe) attached to a gas chromatograph-mass spectrometer is presented for the thermal pretreatment, characterisation and analysis of molecularly imprinted polymers. The technique is demonstrated as effective for the removal of volatile materials, including template and unreacted monomers, from methacrylic acid-ethylene glycol dimethacrylate copolymers imprinted with 2-aminopyridine. Mass spectrometry is a powerful technique for polymer bleed characterisation. Thermal desorption studies on reloaded template and related compounds are reported as a means of assessing polymer morphology, specific binding by imprinted polymers compared with reference non-imprinted polymers and selective binding by an imprinted polymer for its template. Calibration studies on the thermal desorption technique using an internal standard are presented with R(2) > 0.999. The technique provides a novel method for assessment of polymer thermal stability, composition and morphology.

  8. Surface reconstruction and thermal desorption: {O}/{Ag(110) } an experimental study

    Science.gov (United States)

    Canepa, M.; Salvietti, M.; Traverso, M.; Mattera, L.

    1995-07-01

    We have studied the associative desorption of oxygen from well-defined O( n×1)Ag(110) phases ( n ranging from 8 to 2) by thermal desorption mass spectrometry. Desorption peak profiles have been compared with calculations based on a lattice-gas model [V.P. Zhdanov, Surf. Sci. 277 (1992) 155] which takes into account the missing-row reconstruction of the substrate and adsorbate-adsorbate interactions along independent OAgO rows. The model works well at low coverage accurately reproducing the peak profiles. For the O(8 × 1), O(6 × 1) and O(4 × 1) phases, assuming a value of v = 10 15 s -1 for the pre-factor, values of ≈ 39 kcal/mol for the activation energy and ≈ -2.5 kcal/mol for the OO effective oxygen-oxygen interaction along OAgO rows are obtained. At high coverage the assumption of independence of OAgO chains is no longer valid and repulsive interactions perpendicularly to the chains have to be taken into account.

  9. Reliability of a BTEX radial diffusive sampler for thermal desorption: field measurements

    Science.gov (United States)

    Bruno, P.; Caputi, M.; Caselli, M.; de Gennaro, G.; de Rienzo, M.

    Radiello ®, a radial symmetry diffusive sampler, has been evaluated for its potential for ambient air quality monitoring, in particular for benzene, toluene, ethyl benzene, p-xylene, m-xylene, o-xylene (BTEX) measurements. BTEX were first sampled onto adsorbing cartridges before analyses were performed by thermal desorption and GC-MS. Tests were carried out to determine blank values and any storage effects. The results of an investigation into repeatability of the Radiello ® sampler and the influence of sampling time under field conditions are reported. Inter-comparison with automatic instruments is also illustrated.

  10. Thermal proton transfer reactions in ultraviolet matrix-assisted laser desorption/ionization.

    Science.gov (United States)

    Chu, Kuan Yu; Lee, Sheng; Tsai, Ming-Tsang; Lu, I-Chung; Dyakov, Yuri A; Lai, Yin Hung; Lee, Yuan-Tseh; Ni, Chi-Kung

    2014-03-01

    One of the reasons that thermally induced reactions are not considered a crucial mechanism in ultraviolet matrix-assisted laser desorption ionization (UV-MALDI) is the low ion-to-neutral ratios. Large ion-to-neutral ratios (10(-4)) have been used to justify the unimportance of thermally induced reactions in UV-MALDI. Recent experimental measurements have shown that the upper limit of the total ion-to-neutral ratio is approximately 10(-7) at a high laser fluence and less than 10(-7) at a low laser fluence. Therefore, reexamining the possible contributions of thermally induced reactions in MALDI may be worthwhile. In this study, the concept of polar fluid was employed to explain the generation of primary ions in MALDI. A simple model, namely thermal proton transfer, was used to estimate the ion-to-neutral ratios in MALDI. We demonstrated that the theoretical calculations of ion-to-neutral ratios exhibit the same trend and similar orders of magnitude compared with those of experimental measurements. Although thermal proton transfer may not generate all of the ions observed in MALDI, the calculations demonstrated that thermally induced reactions play a crucial role in UV-MALDI.

  11. Suppression of PCDD/Fs during thermal desorption of PCBs-contaminated soil.

    Science.gov (United States)

    Zhao, Zhonghua; Ni, Mingjiang; Li, Xiaodong; Buekens, Alfons; Yan, Jianhua

    2016-12-01

    Thermal treatment of polychlorinated biphenyls (PCBs) contaminated soil was shown in earlier work to generate new PCBs, as well as polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs). In this study, this thermal desorption was conducted with addition of three distinct inhibitors, including ammonium sulphate, urea and calcium oxide, to inhibit the formation of PCDDs and PCDFs when remediating PCBs-contaminated soil. Experiments were conducted for 40 min at 400 °C after adding 1 wt.% of inhibitor. Both the total PCDD/Fs and international toxic equivalent quantity (I-TEQ) reduced when inhibitors were introduced. Of the three compounds tested, CaO shows the highest inhibition efficiency, 92.2 % for total PCDD/Fs and 95.6 % for I-TEQ. The amount of CaO added also influences the suppression efficiency of PCDD/Fs. These results suggest that promoting desorption and destruction of precursors is probably the mechanism of suppression.

  12. Evaluation of minimum desorption temperatures of thermal compressors in adsorption refrigeration cycles

    Energy Technology Data Exchange (ETDEWEB)

    Saha, B.B.; El-Sharkawy, I.I.; Chakraborty, A.; Koyama, S.; Srinivasan, K. [Interdisciplinary Graduate School of Engineering Sciences, Kyushu University, 6-1 Kasuga-koen Kasuga, Fukuoka 816-8580 (Japan); Banker, N.D.; Dutta, P. [Department of Mechanical Engineering, Indian Institute of Science, Bangalore (India); Prasad, M. [Thermal Systems Division, ISRO Satellite Centre, Bangalore (India)

    2006-11-15

    The purpose of this paper is to identify the minimum desorption temperatures required to operate thermally driven adsorption beds of a solid sorption refrigeration system. The method is based on the evaluation of uptake efficiency of the adsorption bed and estimating there from conditions under which the compressor ceases to provide any throughput. The difference in the densities of the refrigerant between the inlet and outlet, the adsorption characteristics of the adsorbate-refrigerant pair and the void volume in the thermal compressor are the contributors to the manifestation of the desorption state. Among them, the void volume is a controllable parameter whose role is analogous to the clearance volume in a positive displacement compressor. The methodology has been tested out with three systems, namely, silica gel+water, activated carbon fiber+ethanol and activated carbon+HFC 134a systems. It is shown that waste heat at as low as 60{sup o}C can operate these systems which make them good energy conservation devices through recovery of low grade process waste heat. (author)

  13. Ion intensity and thermal proton transfer in ultraviolet matrix-assisted laser desorption/ionization.

    Science.gov (United States)

    Lu, I-Chung; Lee, Chuping; Chen, Hui-Yuan; Lin, Hou-Yu; Hung, Sheng-Wei; Dyakov, Yuri A; Hsu, Kuo-Tung; Liao, Chih-Yu; Lee, Yin-Yu; Tseng, Chien-Ming; Lee, Yuan-Tseh; Ni, Chi-Kung

    2014-04-17

    The ionization mechanism of ultraviolet matrix-assisted laser desorption/ionization (UV-MALDI) was investigated by measuring the total cation intensity (not including sodiated and potasiated ions) as a function of analyte concentration (arginine, histidine, and glycine) in a matrix of 2,4,6-trihydroxyacetophenone (THAP). The total ion intensity increased up to 55 times near the laser fluence threshold as the arginine concentration increased from 0% to 1%. The increases were small for histidine, and a minimal increase occurred for glycine. Time-resolved fluorescence intensity was employed to investigate how analytes affected the energy pooling of the matrix. No detectable energy pooling was observed for pure THAP and THAP/analyte mixtures. The results can be described by using a thermal proton transfer model, which suggested that thermally induced proton transfer is crucial in the primary ion generation in UV-MALDI.

  14. Optimising the Use of TRIzol-extracted Proteins in Surface Enhanced Laser Desorption/ Ionization (SELDI Analysis

    Directory of Open Access Journals (Sweden)

    Perlaky Laszlo

    2006-03-01

    Full Text Available Abstract Background Research with clinical specimens is always hampered by the limited availability of relevant samples, necessitating the use of a single sample for multiple assays. TRIzol is a common reagent for RNA extraction, but DNA and protein fractions can also be used for other studies. However, little is known about using TRIzol-extracted proteins in proteomic research, partly because proteins extracted from TRIzol are very resistant to solubilization. Results To facilitate the use of TRIzol-extracted proteins, we first compared the ability of four different common solubilizing reagents to solubilize the TRIzol-extracted proteins from an osteosarcoma cell line, U2-OS. Then we analyzed the solubilized proteins by Surface Enhanced Laser Desorption/ Ionization technique (SELDI. The results showed that solubilization of TRIzol-extracted proteins with 9.5 M Urea and 2% CHAPS ([3-[(3-cholamidopropyl-dimethylammonio]propanesulfonate] (UREA-CHAPS was significantly better than the standard 1% SDS in terms of solubilization efficiency and the number of detectable ion peaks. Using three different types of SELDI arrays (CM10, H50, and IMAC-Cu, we demonstrated that peak detection with proteins solubilized by UREA-CHAPS was reproducible (r > 0.9. Further SELDI analysis indicated that the number of ion peaks detected in TRIzol-extracted proteins was comparable to a direct extraction method, suggesting many proteins still remain in the TRIzol protein fraction. Conclusion Our results suggest that UREA-CHAPS performed very well in solubilizing TRIzol-extracted proteins for SELDI applications. Protein fractions left over after TRIzol RNA extraction could be a valuable but neglected source for proteomic or biochemical analysis when additional samples are not available.

  15. Helium implanted Eurofer97 characterized by positron beam Doppler broadening and Thermal Desorption Spectroscopy

    Science.gov (United States)

    Carvalho, I.; Schut, H.; Fedorov, A.; Luzginova, N.; Desgardin, P.; Sietsma, J.

    2013-11-01

    Reduced Activation Ferritic/Martensitic steels are being extensively studied because of their foreseen application in fusion and Generation IV fission reactors. To produce irradiation induced defects, Eurofer97 samples were implanted with helium at energies of 500 keV and 2 MeV and doses of 1 × 1015-1016 He/cm2, creating atomic displacements in the range 0.07-0.08 dpa. The implantation induced defects were characterized by positron beam Doppler Broadening (DB) and Thermal Desorption Spectroscopy (TDS). Results show that up to ˜600 K peaks that can be attributed to He desorption from overpressured HenVm (n > m) clusters and vacancy assisted mechanism in the case of helium in the substitutional position. The temperature range 600-1200 K is related to the formation of larger clusters HenVm (n < m). The dissociation of the HeV and the phase transition attributed to a sharp peak in the TDS spectra at 1200 K. Above this temperature, the release of helium from bubbles is observed.

  16. Comparative sorption and desorption behaviors of PFHxS and PFOS on sequentially extracted humic substances

    Institute of Scientific and Technical Information of China (English)

    Lixia Zhao; Yifeng Zhang; Shuhong Fang; Lingyan Zhu; Zhengtao Liu

    2014-01-01

    The sorption and desorption behaviors of two perfluoroalkane sulfonates (PFSAs),including perfluorohexane sulfonate (PFHxS) and perfluorooctane sulfonate (PFOS) on two humic acids (HAs) and humin (HM),which were extracted from a peat soil,were investigated.The sorption kinetics and isotherms showed that the sorption of PFOS on the humic substances (HSs) was much higher than PFHxS.For the same PFSA compound,the sorption on HSs followed the order of HM > HA2 > HA1.These suggest that hydrophobic interaction plays a key role in the sorption of PFSAs on HSs.The sorption capacities of PFSAs on HSs were significantly related to their aliphaticity,but negatively correlated to aromatic carbons,indicating the importance of aliphatic groups in the sorption of PFSAs.Compared to PFOS,PFHxS displayed distinct desorption hysteresis,probably due to irreversible pore deformation after sorption of PFHxS.The sorption of the two PFSAs on HSs decreased with an increase in pH in the solution.This is ascribed to the electrostatic interaction and hydrogen bonding at lower pH.Hydrophobic interaction might also be stronger at lower pH due to the aggregation of HSs.

  17. A Solid Trap and Thermal Desorption System with Application to a Medical Electronic Nose

    Directory of Open Access Journals (Sweden)

    Xuntao Xu

    2008-11-01

    Full Text Available In this paper, a solid trap/thermal desorption-based odorant gas condensation system has been designed and implemented for measuring low concentration odorant gas. The technique was successfully applied to a medical electronic nose system. The developed system consists of a flow control unit, a temperature control unit and a sorbent tube. The theoretical analysis and experimental results indicate that gas condensation, together with the medical electronic nose system can significantly reduce the detection limit of the nose system and increase the system’s ability to distinguish low concentration gas samples. In addition, the integrated system can remove the influence of background components and fluctuation of operational environment. Even with strong disturbances such as water vapour and ethanol gas, the developed system can classify the test samples accurately.

  18. Defect annealing and thermal desorption of deuterium in low dose HFIR neutron-irradiated tungsten

    Energy Technology Data Exchange (ETDEWEB)

    Shimada, Masashi, E-mail: Masashi.Shimada@inl.gov [Fusion Safety Program, Idaho National Laboratory, Idaho Falls, ID (United States); Hara, Masanori [Hydrogen Isotope Research Center, University of Toyama, Toyama (Japan); Otsuka, Teppei [Kyushu University, Interdisciplinary Graduate School of Engineering Science, Higashi-ku, Fukuoka (Japan); Oya, Yasuhisa [Radioscience Research Laboratory, Faculty of Science, Shizuoka University, Shizuoka (Japan); Hatano, Yuji [Hydrogen Isotope Research Center, University of Toyama, Toyama (Japan)

    2015-08-15

    Three tungsten samples irradiated at High Flux Isotope Reactor at Oak Ridge National Laboratory were exposed to deuterium plasma (ion fluence of 1 × 10{sup 26} m{sup −2}) at three different temperatures (100, 200, and 500 °C) in Tritium Plasma Experiment at Idaho National Laboratory. Subsequently, thermal desorption spectroscopy was performed with a ramp rate of 10 °C min{sup −1} up to 900 °C, and the samples were annealed at 900 °C for 0.5 h. These procedures were repeated three times to uncover defect-annealing effects on deuterium retention. The results show that deuterium retention decreases approximately 70% for at 500 °C after each annealing, and radiation damages were not annealed out completely even after the 3rd annealing. TMAP modeling revealed the trap concentration decreases approximately 80% after each annealing at 900 °C for 0.5 h.

  19. Thermal desorption from self-damaged tungsten exposed to deuterium atoms

    Energy Technology Data Exchange (ETDEWEB)

    Gasparyan, Yu.M., E-mail: gasparyan.yury@plasma.mephi.ru [National Research Nuclear University MEPhI (Moscow Engineering Physics Institute), Kashirskoe sh.31, 115409 Moscow (Russian Federation); Ogorodnikova, O.V. [National Research Nuclear University MEPhI (Moscow Engineering Physics Institute), Kashirskoe sh.31, 115409 Moscow (Russian Federation); Max-Planck-Institut für Plasmaphysik, EURATOM Association, Boltzmannstr. 2, D-85748 Garching (Germany); Efimov, V.S.; Mednikov, A.; Marenkov, E.D.; Pisarev, A.A. [National Research Nuclear University MEPhI (Moscow Engineering Physics Institute), Kashirskoe sh.31, 115409 Moscow (Russian Federation); Markelj, S.; Čadež, I. [Jožef Stefan Institute and Association EURATOM-MHEST, Jamova Cesta 39, 1000 Ljubljana (Slovenia)

    2015-08-15

    Deuterium retention in tungsten damaged by 2–20 MeV W ions and then exposed to D atoms was investigated by means of thermal desorption spectroscopy. Experimental data demonstrate a significant increase of deuterium retention in the presence of radiation defects. A remarkable amount of deuterium is trapped even at the temperature of 800 K. TDS spectra were simulated using the computer code DIFTRAP based on kinetic rate equations to derive parameters of deuterium interaction with radiation defects. It was shown that irradiation by MeV W ions forms in W a high concentration of strong traps with the detrapping energy of 1.7–2 eV. These traps play major role in the D retention at elevated temperatures. The experimental spectra have peculiarities that are not described by the standard modeling; and the reasons for that are discussed.

  20. Detection of deuterium trapping sites in tungsten by thermal desorption spectroscopy and positron annihilation spectroscopy

    Directory of Open Access Journals (Sweden)

    K. Sato

    2016-12-01

    Full Text Available Thermal desorption spectroscopy (TDS of tungsten implanted with D2+ ions was performed after irradiation with 8 MeV-electrons, 5.0keV-D2+, and 6.0 MeV-Fe3+. The release peak temperatures of the TDS spectra are discussed. Positron annihilation lifetime (PAL measurements of electron-irradiated tungsten were also performed, showing that single vacancies migrate a sufficient distance to arrive at a sink or meet interstitial-type defects during annealing at 673K. A decrease in the PAL was detected for single vacancies that contain deuterium atoms. The peak temperature of deuterium release from dislocations was lower than that from single vacancies. In samples irradiated with 6.0 MeV-Fe3+, the effect of Fe contamination on deuterium trapping and the deuterium release from voids were detected. These tendencies correspond to previous works.

  1. Annealing Behaviour of Helium Bubbles in Titanium Films by Thermal Desorption Spectroscopy and Positron Beam Analysis

    Institute of Scientific and Technical Information of China (English)

    LIU Chao-Zhuo; ZHOU Zhu-Ying; SHI Li-Qun; WANG Bao-Yi; HAO Xiao-Peng; ZHAO Guo-Qing

    2007-01-01

    @@ Helium-containing Ti films are prepared using magnetron sputtering in the helium-argon atmosphere. Isochronal annealing at different temperatures for an hour is employed to reveal the behaviour of helium bubble growth. Ion beam analysis is used to measure the retained helium content. Helium can release largely when annealing above 970 K. A thermal helium desorption spectroscopy system is constructed for assessment of the evolution of helium bubbles in the annealed samples by linear heating (0.4K/s) from room temperature to 1500K. Also, Doppler broadening measurements of positron annihilation radiation spectrum are performed by using changeable energy positron beam. Bubble coarsening evolves gradually below 680K, migration and coalescence of small bubbles dominates in the range of 680-970K, and the Ostwald ripening mechanism enlarges the bubbles with a massive release above 970K.

  2. MGP remediation using thermal desorption: emerging technology yields a permanent solution

    Energy Technology Data Exchange (ETDEWEB)

    Umfleet, D.E.; Bachman, S.A.; Highland, E. [Barr Engineering Company, Ann Arbor, MI (United States)

    1997-12-01

    An investigation of a former manufactured gas plant (MGP) at the site for Northwestern Public Service`s new operations buildings uncovered evidence of MGP residuals in the moist, clay-rich soils. On site-thermal desorption was selected as the remedial method. A low-temperature, counter-flow, direct-fired rotary desorber heats soils up to 1200{degree}F to volatilize organic fractions. Soils containing polyaromatic hydrocarbon (PAH) compounds were excavated, treated effectively, and reused at the site as backfill. For the approximately 47,000 tons of soil processed, remediation costs were 82 dollars per ton. Site-specific factors affecting project costs included the volume of soil treated, soil type and condition, inclement weather, and market conditions. Soils were treated to below state-approved performance criterion, and remediation of the site was completed just 18 months after the project began. 1 fig., 2 tabs.

  3. Analysis of organic contaminants from silicon wafer and disk surfaces by thermal desorption-GC-MS

    Science.gov (United States)

    Camenzind, Mark J.; Ahmed, Latif; Kumar, Anurag

    1999-03-01

    Organic contaminants can affect semiconductor wafer processing including gate oxide integrity, polysilicon growth, deep ultraviolet photoresist line-width, and cleaning & etching steps. Organophosphates are known to counter dope silicon wafers. Organic contaminants in disk drives can cause failures due to stiction or buildup on the heads. Therefore, it is important to identify organic contaminants adsorbed on wafer or disk surfaces and find their sources so they can be either completely eliminated or at least controlled. Dynamic headspace TD-GC-MS (Thermal Desorption-Gas Chromatography-Mass Spectrometry) methods are very sensitive and can be used to identify organic contaminants on disks and wafers, in air, or outgassing from running drives or their individual components.

  4. Quantification of Selected Vapour-Phase Compounds using Thermal Desorption-Gas Chromatography

    Directory of Open Access Journals (Sweden)

    McLaughlin DWJ

    2014-12-01

    Full Text Available A robust method for the analysis of selected vapour phase (VP compounds in mainstream smoke (MSS is described. Cigarettes are smoked on a rotary smoking machine and the VP that passes through the Cambridge filter pad collected in a TedlarA¯ bag. On completion of smoking, the bag contents are sampled onto an adsorption tube containing a mixed carbon bed. The tube is subsequently analysed on an automated thermal desorption (TD system coupled to a gas chromatography-flame ionization detector (GC-FID using a PoraPLOT-Q column. Quantification of 14 volatile compounds including the major carbonyls is achieved. Details of the method validation data are included in this paper. This method has been used to analyse the VP of cigarette MSS over a wide range of ‘tar’ deliveries and configurations with excellent repeatability. Results for the University of Kentucky reference cigarette 1R4F are in good agreement with reported values.

  5. DEMONSTRATION BULLETIN: THE ECO LOGIC THERMAL DESORPTION UNIT - MIDDLEGROUND LANDFILL - BAY CITY, MI - ELI ECO LOGIC INTERNATIONAL, INC.

    Science.gov (United States)

    ECO Logic has developed a thermal desorption unit 0"DU) for the treatment of soils contaminated with hazardous organic contaminants. This TDU has been designed to be used in conjunction with Eco Logic's patented gas-phase chemical reduction reactor. The Eco Logic reactor is the s...

  6. DEMONSTRATION BULLETIN: THE ECO LOGIC THERMAL DESORPTION UNIT - MIDDLEGROUND LANDFILL - BAY CITY, MI - ELI ECO LOGIC INTERNATIONAL, INC.

    Science.gov (United States)

    ECO Logic has developed a thermal desorption unit 0"DU) for the treatment of soils contaminated with hazardous organic contaminants. This TDU has been designed to be used in conjunction with Eco Logic's patented gas-phase chemical reduction reactor. The Eco Logic reactor is the s...

  7. Adsorption and desorption of DNA tuned by hydroxyl groups in graphite oxides-based solid extraction material.

    Science.gov (United States)

    Akceoglu, Garbis Atam; Li, Oi Lun; Saito, Nagahiro

    2015-12-01

    The extraction of DNA is the most crucial method used in molecular biology. Up to date silica matrices has been widely applied as solid support for selective DNA adsorption and extraction. However, since adsorption force of SiOH functional groups is much greater than that of desorption force, the DNA extraction efficiency of silica surfaces is limited. In order to increase the DNA extraction yield, a new surface with different functional groups which possess of greater desorption property is required. In this study, we proposed cellulose/graphite oxide (GO) composite as an alternative material for DNA adsorption and extraction. GO/Cellulose composite provides the major adsorption and desorption of DNA by COH, which belongs to alkyl or phenol type of OH functional group. Compared to SiOH, COH is less polarized and reactive, therefore the composite might provide a higher desorption of DNA during the elution process. The GO/cellulose composite were prepared in spherical structure by mixing urea, cellulose, NaOH, Graphite oxide and water. The concentration of GO within the composites were controlled to be 0-4.15 wt.%. The extraction yield of DNA increased with increasing weight percentage of GO. The highest yield was achieved at 4.15 wt.% GO, where the extraction efficiency was reported as 660.4 ng/μl when applying 2M GuHCl as the binding buffer. The absorbance ratios between 260 nm and 280 nm (A260/A280) of the DNA elution was demonstrated as 1.86, indicating the extracted DNA consisted of high purity. The results proved that GO/cellulose composite provides a simple method for selective DNA extraction with high extraction efficiency of pure DNA.

  8. Determination of persistent organic pollutants in solid environmental samples using accelerated solvent extraction and supercritical fluid extraction. Exhaustive extraction and sorption/desorption studies of PCBs

    Energy Technology Data Exchange (ETDEWEB)

    Bjoerklund, E.

    1998-10-01

    to verify that the developed SFE methods are exhaustive. It is quite clear though that there is no reason to continue using for example Soxhlet extraction, which should be replaced in routine laboratories. The possibility of utilizing SFE as a selective tool in sorption/desorption studies of POPs in natural sediments was also addressed. This second objective was proven successful and sediments could be characterized in terms of resistance towards desorption of bound analytes under supercritical conditions. These data could be correlated to desorption processes occurring under natural conditions. Additionally it could be verified that sorption of POPs from water to sediment is a very slow process requiring months or even years. This supports recent research results, demonstrating that distribution coefficients many times are underestimated since the system has not reached equilibrium 205 refs, 10 figs, 3 tabs

  9. Improved adsorption-desorption extraction applied to the partial characterization of the antilisterial bacteriocin produced by Carnobacterium maltaromaticum C2

    OpenAIRE

    Tulini,F. L; E.C.P De Martinis

    2010-01-01

    Bacteriocins are ribosomally produced peptides useful for food biopreservation. An improved adsorption-desorption process is proposed for the partial purification of the bacteriocin produced by the fish isolate Carnobacterium maltaromaticum C2. Analyzis of extract by SDS-PAGE indicated this method may offer an alternative to improve the yield of purification of bacteriocins.

  10. Improved adsorption-desorption extraction applied to the partial characterization of the antilisterial bacteriocin produced by Carnobacterium maltaromaticum C2.

    Science.gov (United States)

    Tulini, F L; De Martinis, E C P

    2010-04-01

    Bacteriocins are ribosomally produced peptides useful for food biopreservation. An improved adsorption-desorption process is proposed for the partial purification of the bacteriocin produced by the fish isolate Carnobacterium maltaromaticum C2. Analyzis of extract by SDS-PAGE indicated this method may offer an alternative to improve the yield of purification of bacteriocins.

  11. Improved adsorption-desorption extraction applied to the partial characterization of the antilisterial bacteriocin produced by Carnobacterium maltaromaticum C2

    Directory of Open Access Journals (Sweden)

    F. L Tulini

    2010-06-01

    Full Text Available Bacteriocins are ribosomally produced peptides useful for food biopreservation. An improved adsorption-desorption process is proposed for the partial purification of the bacteriocin produced by the fish isolate Carnobacterium maltaromaticum C2. Analyzis of extract by SDS-PAGE indicated this method may offer an alternative to improve the yield of purification of bacteriocins.

  12. Thermal desorption-gas chromatography for the determination of benzene, aniline, nitrobenzene and chlorobenzene in workplace air.

    Science.gov (United States)

    Patil, S F; Lonkar, S T

    1992-05-29

    Sampling on Tenax TA of different mesh sizes followed by thermal desorption and gas chromatography was evaluated as a simple method for the determination of benzene, aniline, nitrobenzene and chlorobenzene in the workplace air. An alternative sampling technique in place of pump sampling was developed. Quantitative recoveries were obtained in the mass range 0.04-10 micrograms. It was found that air humidity had no effect on recovery. The charged tubes can be stored at room temperature for 5 days with no change in recovery. The particle size of Tenax TA has no significant effect on adsorption and desorption.

  13. Non-isothermal kinetics of the thermal desorption of mercury from a contaminated soil

    Directory of Open Access Journals (Sweden)

    López, Félix A.

    2014-03-01

    Full Text Available The Almadén mining district (Ciudad Real, Spain was the largest cinnabar (mercury sulphide mine in the world. Its soils have high levels of mercury a consequence of its natural lithology, but often made much worse by its mining history. The present work examines the thermal desorption of two contaminated soils from the Almadén area under non-isothermal conditions in a N2 atmosphere, using differential scanning calorimetry (DSC. DSC was performed at different heating rates between room temperature and 600 °C. Desorption temperatures for different mercury species were determined. The Friedman, Flynn-Wall-Ozawa and Coasts–Redfern methods were employed to determine the reaction kinetics from the DSC data. The activation energy and pre-exponential factor for mercury desorption were calculated.El distrito minero de Almadén (Ciudad Real, España tiene la mayor mina de cinabrio (sulfuro de mercurio del mundo. Sus suelos tienen altos niveles de mercurio como consecuencia de su litología natural, pero a menudo su contenido en mercurio es mucho más alto debido a la historia minera de la zona. Este trabajo examina la desorción térmica de dos suelos contaminados procedentes de Almadén bajo condiciones isotérmicas en atmósfera de N2, empleando calorimetría diferencial de barrido (DSC. La calorimetría se llevó a cabo a diferentes velocidades de calentamiento desde temperatura ambiente hasta 600 °C. Se determinaron las diferentes temperaturas de desorción de las especies de mercurio presentes en los suelos. Para determinar la cinética de reacción a partir de los datos de DSC se utilizaron los métodos de Friedman, Flynn-Wall-Ozawa y Coasts–Redfern. Además se calcularon las energías de activación y los factores pre-exponenciales para la desorción del mercurio.

  14. Enhancing radiative energy transfer through thermal extraction

    Science.gov (United States)

    Tan, Yixuan; Liu, Baoan; Shen, Sheng; Yu, Zongfu

    2016-06-01

    Thermal radiation plays an increasingly important role in many emerging energy technologies, such as thermophotovoltaics, passive radiative cooling and wearable cooling clothes [1]. One of the fundamental constraints in thermal radiation is the Stefan-Boltzmann law, which limits the maximum power of far-field radiation to P0 = σT4S, where σ is the Boltzmann constant, S and T are the area and the temperature of the emitter, respectively (Fig. 1a). In order to overcome this limit, it has been shown that near-field radiations could have an energy density that is orders of magnitude greater than the Stefan-Boltzmann law [2-7]. Unfortunately, such near-field radiation transfer is spatially confined and cannot carry radiative heat to the far field. Recently, a new concept of thermal extraction was proposed [8] to enhance far-field thermal emission, which, conceptually, operates on a principle similar to oil immersion lenses and light extraction in light-emitting diodes using solid immersion lens to increase light output [62].Thermal extraction allows a blackbody to radiate more energy to the far field than the apparent limit of the Stefan-Boltzmann law without breaking the second law of thermodynamics. Thermal extraction works by using a specially designed thermal extractor to convert and guide the near-field energy to the far field, as shown in Fig. 1b. The same blackbody as shown in Fig. 1a is placed closely below the thermal extractor with a spacing smaller than the thermal wavelength. The near-field coupling transfers radiative energy with a density greater than σT4. The thermal extractor, made from transparent and high-index or structured materials, does not emit or absorb any radiation. It transforms the near-field energy and sends it toward the far field. As a result, the total amount of far-field radiative heat dissipated by the same blackbody is greatly enhanced above SσT4, where S is the area of the emitter. This paper will review the progress in thermal

  15. MERCURY QUANTIFICATION IN SOILS USING THERMAL DESORPTION AND ATOMIC ABSORPTION SPECTROMETRY: PROPOSAL FOR AN ALTERNATIVE METHOD OF ANALYSIS

    Directory of Open Access Journals (Sweden)

    Liliane Catone Soares

    2015-08-01

    Full Text Available Despite the considerable environmental importance of mercury (Hg, given its high toxicity and ability to contaminate large areas via atmospheric deposition, little is known about its activity in soils, especially tropical soils, in comparison with other heavy metals. This lack of information about Hg arises because analytical methods for determination of Hg are more laborious and expensive compared to methods for other heavy metals. The situation is even more precarious regarding speciation of Hg in soils since sequential extraction methods are also inefficient for this metal. The aim of this paper is to present a technique of thermal desorption associated with atomic absorption spectrometry, TDAAS, as an efficient tool for quantitative determination of Hg in soils. The method consists of the release of Hg by heating, followed by its quantification by atomic absorption spectrometry. It was developed by constructing calibration curves in different soil samples based on increasing volumes of standard Hg2+ solutions. Performance, accuracy, precision, and quantification and detection limit parameters were evaluated. No matrix interference was detected. Certified reference samples and comparison with a Direct Mercury Analyzer, DMA (another highly recognized technique, were used in validation of the method, which proved to be accurate and precise.

  16. Coupling Laser Diode Thermal Desorption with Acoustic Sample Deposition to Improve Throughput of Mass Spectrometry-Based Screening.

    Science.gov (United States)

    Haarhoff, Zuzana; Wagner, Andrew; Picard, Pierre; Drexler, Dieter M; Zvyaga, Tatyana; Shou, Wilson

    2016-02-01

    The move toward label-free screening in drug discovery has increased the demand for mass spectrometry (MS)-based analysis. Here we investigated the approach of coupling acoustic sample deposition (ASD) with laser diode thermal desorption (LDTD)-tandem mass spectrometry (MS/MS). We assessed its use in a cytochrome P450 (CYP) inhibition assay, where a decrease in metabolite formation signifies CYP inhibition. Metabolite levels for 3 CYP isoforms were measured as CYP3A4-1'-OH-midazolam, CYP2D6-dextrorphan, and CYP2C9-4'-OH-diclofenac. After incubation, samples (100 nL) were acoustically deposited onto a stainless steel 384-LazWell plate, then desorbed by an infrared laser directly from the plate surface into the gas phase, ionized by atmospheric pressure chemical ionization (APCI), and analyzed by MS/MS. Using this method, we achieved a sample analysis speed of 2.14 s/well, with bioanalytical performance comparable to the current online solid-phase extraction (SPE)-based MS method. An even faster readout speed was achieved when postreaction sample multiplexing was applied, where three reaction samples, one for each CYP, were transferred into the same well of the LazWell plate. In summary, LDTD coupled with acoustic sample deposition and multiplexing significantly decreased analysis time to 0.7 s/sample, making this MS-based approach feasible to support high-throughput screening (HTS) assays.

  17. In situ ionic liquid dispersive liquid-liquid microextraction and direct microvial insert thermal desorption for gas chromatographic determination of bisphenol compounds.

    Science.gov (United States)

    Cacho, Juan Ignacio; Campillo, Natalia; Viñas, Pilar; Hernández-Córdoba, Manuel

    2016-01-01

    A new procedure based on direct insert microvial thermal desorption injection allows the direct analysis of ionic liquid extracts by gas chromatography and mass spectrometry (GC-MS). For this purpose, an in situ ionic liquid dispersive liquid-liquid microextraction (in situ IL DLLME) has been developed for the quantification of bisphenol A (BPA), bisphenol Z (BPZ) and bisphenol F (BPF). Different parameters affecting the extraction efficiency of the microextraction technique and the thermal desorption step were studied. The optimized procedure, determining the analytes as acetyl derivatives, provided detection limits of 26, 18 and 19 ng L(-1) for BPA, BPZ and BPF, respectively. The release of the three analytes from plastic containers was monitored using this newly developed analytical method. Analysis of the migration test solutions for 15 different plastic containers in daily use identified the presence of the analytes at concentrations ranging between 0.07 and 37 μg L(-1) in six of the samples studied, BPA being the most commonly found and at higher concentrations than the other analytes.

  18. Broad spectrum infrared thermal desorption of wipe-based explosive and narcotic samples for trace mass spectrometric detection.

    Science.gov (United States)

    Forbes, Thomas P; Staymates, Matthew; Sisco, Edward

    2017-08-07

    Wipe collected analytes were thermally desorbed using broad spectrum near infrared heating for mass spectrometric detection. Employing a twin tube filament-based infrared emitter, rapid and efficiently powered thermal desorption and detection of nanogram levels of explosives and narcotics was demonstrated. The infrared thermal desorption (IRTD) platform developed here used multi-mode heating (direct radiation and secondary conduction from substrate and subsequent convection from air) and a temperature ramp to efficiently desorb analytes with vapor pressures across eight orders of magnitude. The wipe substrate experienced heating rates up to (85 ± 2) °C s(-1) with a time constant of (3.9 ± 0.2) s for 100% power emission. The detection of trace analytes was also demonstrated from complex mixtures, including plastic-bonded explosives and exogenous narcotics, explosives, and metabolites from collected artificial latent fingerprints. Manipulation of the emission power and duration directly controlled the heating rate and maximum temperature, enabling differential thermal desorption and a level of upstream separation for enhanced specificity. Transitioning from 100% power and 5 s emission duration to 25% power and 30 s emission enabled an order of magnitude increase in the temporal separation (single seconds to tens of seconds) of the desorption of volatile and semi-volatile species within a collected fingerprint. This mode of operation reduced local gas-phase concentrations, reducing matrix effects experienced with high concentration mixtures. IRTD provides a unique platform for the desorption of trace analytes from wipe collections, an area of importance to the security sector, transportation agencies, and customs and border protection.

  19. Characterisation of Dissolved Organic Carbon by Thermal Desorption - Proton Transfer Reaction - Mass Spectrometry

    Science.gov (United States)

    Materić, Dušan; Peacock, Mike; Kent, Matthew; Cook, Sarah; Gauci, Vincent; Röckmann, Thomas; Holzinger, Rupert

    2017-04-01

    Dissolved organic carbon (DOC) is an integral component of the global carbon cycle. DOC represents an important terrestrial carbon loss as it is broken down both biologically and photochemically, resulting in the release of carbon dioxide (CO2) to the atmosphere. The magnitude of this carbon loss can be affected by land management (e.g. drainage). Furthermore, DOC affects autotrophic and heterotrophic processes in aquatic ecosystems, and, when chlorinated during water treatment, can lead to the release of harmful trihalomethanes. Numerous methods have been used to characterise DOC. The most accessible of these use absorbance and fluorescence properties to make inferences about chemical composition, whilst high-performance size exclusion chromatography can be used to determine apparent molecular weight. XAD fractionation has been extensively used to separate out hydrophilic and hydrophobic components. Thermochemolysis or pyrolysis Gas Chromatography - Mass Spectrometry (GC-MS) give information on molecular properties of DOC, and 13C NMR spectroscopy can provide an insight into the degree of aromaticity. Proton Transfer Reaction - Mass Spectrometry (PTR-MS) is a sensitive, soft ionisation method suitable for qualitative and quantitative analysis of volatile and semi-volatile organic vapours. So far, PTR-MS has been used in various environmental applications such as real-time monitoring of volatile organic compounds (VOCs) emitted from natural and anthropogenic sources, chemical composition measurements of aerosols etc. However, as the method is not compatible with water, it has not been used for analysis of organic traces present in natural water samples. The aim of this work was to develop a method based on thermal desorption PTR-MS to analyse water samples in order to characterise chemical composition of dissolved organic carbon. We developed a clean low-pressure evaporation/sublimation system to remove water from samples and thermal desorption system to introduce

  20. GoAmazon 2014/15 Thermal Desorption Chemical Ionization Mass Spectrometer (TDCIMS) Field Campaign Report

    Energy Technology Data Exchange (ETDEWEB)

    Smith, JN [Univ. of California, Irvine, CA (United States)

    2016-04-01

    The Thermal Desorption Chemical Ionization Mass Spectrometer (TDCIMS) deployment to the U.S. Department of Energy (DOE)’s Atmospheric Radiation Measurement (ARM) Climate Research Facility T3 site in Manacapuru, Brazil, was motivated by two main scientific objectives of the Green Ocean Amazon (GoAmazon) 2014/15 field campaign. 1) Study the interactions between anthropogenic and biogenic emissions by determining important molecular species in ambient nanoparticles. To address this, TDCIMS data will be combined with coincident measurements such as gas-phase sulfuric acid to determine the contribution of sulfuric acid condensation to nucleation and growth. We can then compare that result to TDCIMS-derived nanoparticle composition to determine the fraction of growth that can be attributed to the uptake of organic compounds. The molecular composition of sampled particles will also be used to attribute specific chemical species and mechanisms to growth, such as the condensation of low-volatility species or the oligomerization of α-dicarbonyl compounds. 2) Determine the source of new ambient nanoparticles in the Amazon. The hypothesis prior to measurements was that potassium salts formed from the evaporation of primary particles emitted by fungal spores can provide a unique and important pathway for new particle production in the Amazon basin. To explore this hypothesis, the TDCIMS recorded the mass spectra of sampled ambient particles using a protonated water cluster Chemical Ionization Mass Spectrometer (CIMS). Laboratory tests performed using potassium salts show that the TDCIMS can detect potassium with high sensitivity with this technique.

  1. Inelastic scattering of OH radicals from organic liquids: isolating the thermal desorption channel.

    Science.gov (United States)

    King, Kerry L; Paterson, Grant; Rossi, Giovanni E; Iljina, Marija; Westacott, Robin E; Costen, Matthew L; McKendrick, Kenneth G

    2013-08-21

    Inelastic scattering of OH radicals from liquid surfaces has been investigated experimentally. An initially translationally and rotationally hot distribution of OH was generated by 193 nm photolysis of allyl alcohol. These radicals were scattered from an inert reference liquid, perfluorinated polyether (PFPE), and from the potentially reactive hydrocarbon liquids squalane (C30H62, 2,6,10,15,19,23-hexamethyltetracosane) and squalene (C30H50, trans-2,6,10,15,19,23-hexamethyltetracosa-2,6,10,14,18,22-hexaene). The scattered OH v = 0 products were detected by laser-induced fluorescence. Strong correlations were observed between the translational and rotational energies of the products. The high-N levels are translationally hot, consistent with a predominantly direct, impulsive scattering mechanism. Impulsive scattering also populates the lower-N levels, but a component of translationally relaxed OH, with thermal-desorption characteristics, can also be seen clearly for all three liquids. More of this translationally and rotationally relaxed OH survives from squalane than from squalene. Realistic molecular dynamics simulations confirm that double-bond sites are accessible at the squalene surface. This supports the proposition that relaxed OH may be lost on squalene via an addition mechanism.

  2. Implications of Using Thermal Desorption to Remediate Contaminated Agricultural Soil: Physical Characteristics and Hydraulic Processes.

    Science.gov (United States)

    O'Brien, Peter L; DeSutter, Thomas M; Casey, Francis X M; Derby, Nathan E; Wick, Abbey F

    2016-07-01

    Given the recent increase in crude oil production in regions with predominantly agricultural economies, the determination of methods that remediate oil contamination and allow for the land to return to crop production is increasingly relevant. Ex situ thermal desorption (TD) is a technique used to remediate crude oil pollution that allows for reuse of treated soil, but the properties of that treated soil are unknown. The objectives of this research were to characterize TD-treated soil and to describe implications in using TD to remediate agricultural soil. Native, noncontaminated topsoil and subsoil adjacent to an active remediation site were separately subjected to TD treatment at 350°C. Soil physical characteristics and hydraulic processes associated with agricultural productivity were assessed in the TD-treated samples and compared with untreated samples. Soil organic carbon decreased more than 25% in both the TD-treated topsoil and the subsoil, and total aggregation decreased by 20% in the topsoil but was unaffected in the subsoil. The alteration in these physical characteristics explains a 400% increase in saturated hydraulic conductivity in treated samples as well as a decrease in water retention at both field capacity and permanent wilting point. The changes in soil properties identified in this study suggest that TD-treated soils may still be suitable for sustaining vegetation, although likely at a slightly diminished capacity when directly compared with untreated soils.

  3. Rapid determination of nicotine in urine by direct thermal desorption ion trap mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Wise, M.B.; Ilgner, R.H.; Guerin, M.R.

    1990-01-01

    The measurement of nicotine and cotinine in physiological fluids (urine, blood serum, and saliva) is widely used as a means of assessing human exposure to environmental tobacco smoke (ETS). Although numerous analytical methods exist for these measurements, they generally involve extensive sample preparation which increases cost and decreases sample throughput. We report the use of thermal desorption directly into an ion trap mass spectrometer (ITMS) for the rapid determination of nicotine and cotinine in urine. A 1{mu}L aliquot of urine is injected into a specially designed inlet and flash vaporized directly into an ITMS through an open-split capillary restrictor interface. Isobutane chemical ionization is used to generate (M+H){sup +} ions of the analytes and collision induced dissociation is used to generate characteristic fragment ions which are used to confirm their identity. Quantification is achieved by integrating the ion current for the characteristic ions and comparing with an external working curve. Detection limits are approximately 50 pg per analyte and the sample turnaround time is approximately 3 minutes without the need for extensive sample preparation. 12 refs., 5 figs.

  4. Atomic force microscope controlled topographical imaging and proximal probe thermal desorption/ionization mass spectrometry imaging.

    Science.gov (United States)

    Ovchinnikova, Olga S; Kjoller, Kevin; Hurst, Gregory B; Pelletier, Dale A; Van Berkel, Gary J

    2014-01-21

    This paper reports on the development of a hybrid atmospheric pressure atomic force microscopy/mass spectrometry imaging system utilizing nanothermal analysis probes for thermal desorption surface sampling with subsequent atmospheric pressure chemical ionization and mass analysis. The basic instrumental setup and the general operation of the system were discussed, and optimized performance metrics were presented. The ability to correlate topographic images of a surface with atomic force microscopy and a mass spectral chemical image of the same surface, utilizing the same probe without moving the sample from the system, was demonstrated. Co-registered mass spectral chemical images and atomic force microscopy topographical images were obtained from inked patterns on paper as well as from a living bacterial colony on an agar gel. Spatial resolution of the topography images based on pixel size (0.2 μm × 0.8 μm) was better than the resolution of the mass spectral images (2.5 μm × 2.0 μm), which were limited by current mass spectral data acquisition rate and system detection levels.

  5. Age determination of ballpoint pen ink by thermal desorption and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Bügler, Jürgen H; Buchner, Hans; Dallmayer, Anton

    2008-07-01

    Two main approaches can be used for determining the age of an ink: indirect dating and direct dating. Indirect dating is based on the chemical analysis of an ink followed by comparison with known samples in a reference collection. The collection should contain information about the inks including the market introduction dates. This approach may allow for an anachronism to be detected. The second concept is based on measuring ink components that change with age. The analysis of solvents in ballpoint inks may be a useful parameter for determining the age of ink on paper. In a previous study, the authors demonstrated that thermal desorption of ink directly from paper, followed by chemical analysis using gas chromatography-mass spectrometry (GC-MS), is a promising procedure for characterizing ink-binder resins and solvents. Preliminary tests showed that monitoring the evaporation of ink solvent from ink on paper is not a suitable method for ink dating. Thermal analysis of ink on paper in two steps revealed that fresh ink releases a relative amount of solvent at a certain low temperature in a defined period of time, which decreases as the ink ages. As a consequence, this relative amount of solvent released at a certain low temperature, and its decrease with time, can be used to estimate ink age. This age-dependent parameter was studied in 85 different inks ranging in age from 1 week to 1.5 years. It was found that some inks showed a significant decrease of this parameter up to an age of several months, and that the aging process can be monitored within this period. For other inks, however, the age-dependent parameter decreases relatively fast, e.g., within a few days, to a constant level, which can be too fast for casework. Based on these results, a general procedure for assessing the age of ballpoint pen inks on paper was developed.

  6. Effects of He, D interaction on thermal desorption of He and D2 and microstructural evolution in pure Fe

    Science.gov (United States)

    Xu, Q.; Zhang, J.

    2016-10-01

    He and H atoms are produced in (n, α) and (n, p) nuclear reactions. In fusion reactors, energetic T and D, being isotopes of H, and He particles damage the surface materials. To investigate the He-D interaction, Fe, which is a model metal of choice in ferritic stainless steel that is used in fusion reactors, was irradiated separately by He or D2 ions and by combinations of He + D2 or D2 + He ions with the energy of 5 keV. The dose for single-species irradiation and each step of double-species irradiation was 1.0 × 1020 ions/m2. Thermal desorption analysis indicates that, in the case of single ion species irradiation, thermal desorption of D occurs at temperatures below 700 K, while the main thermal desorption of He occurs at 750 K and above 1200 K. The binding energy of He and defects is higher than that of D and defects. In the case of irradiation with combinations of ions species, however, the obtained thermal desorption spectra are the same, although the peak intensities are different, suggesting that the He-D interaction is weak. The sorption of D is more predominant for irradiations with He + D2. On the microstructure level, the irradiated samples exhibited larger voids following combined irradiations compared with those for irradiation with a single ion species after annealing to 1323 K. During the He + D2 irradiation, D atoms are effectively trapped owing to the defects induced by pre-irradiation with He.

  7. Polychlorinated dibenzo-p-dioxin and polychlorinated dibenzofuran formation and emission in the thermal desorption waste treatment process

    Energy Technology Data Exchange (ETDEWEB)

    Leckey, J.H.

    1995-03-01

    It is extremely unlikely that significant amounts of polychlorinated dibenzo-p-dioxins (PCDDs) or polychlorinated dibenzofurans (PCDFs) will be emitted in the off-gas stream from the thermal desorption process, or the treated waste, particularly if the baseline design and anticipated operating conditions of the enhanced bench-scale (EBS) system are used. However, because of the acute toxicity of these compounds and because most of the data on their formation have been extrapolated from studies more related to incineration and fire conditions than thermal desorption, specific laboratory tests and specific EBS runs should be performed to monitor the rate of emission of PCDDs and PCDFs under thermal desorption conditions. In general, the following four conditions need to exist for significant amounts of PCDD or PCDF to be formed: (1) the presence of fly ash; (2) the presence of an oxidizing source; (3) a suitable temperature, and (4) the presence of a suitable precursor. Although the EBS system provides some of these conditions, it is unlikely that enough fly ash will be produced in the system to allow a significant amount of PCDD or PCDF formation. Additionally, particulate matter controls will be used to remove airborne particulates from the gas phase. If PCDD/Fs are presented in a waste stream being evaluated in the EBS, they will likely volatilize in the kiln and subsequently condense in the venturi scrubber system.

  8. Filtration efficiency validation of glass wool during thermal desorption-gas chromatography-mass spectrometer analysis of fine atmospheric particles.

    Science.gov (United States)

    Hao, Liang; Wu, Dapeng; Ding, Kun; Meng, Hu; Yan, Xiaohui; Guan, Yafeng

    2015-02-06

    Thermal desorption-gas chromatography-mass spectrometer (TD-GC-MS) technique has been widely used for analysis of semi-violate organic compounds on atmospheric aerosol. To prevent GC column from being damaged by fine solid particles during thermal desorption process, glass wool as filter mat is indispensible. However, the filtration efficiency has never been validated. In this paper, the most penetrating particle size and the minimum packing thickness of glass wool were calculated based on classical filtration theory. According to the calculation results, packing parameters of glass wool were optimized experimentally using silica particles. It is demonstrated that glass wool with a packing thickness of 30 mm, solidity of 0.039 can effectively block these fine solid particles from penetrating at normal thermal desorption conditions (T=300°C, u=0.4-4 cm/s). Finally, the filtration efficiency of glass wool was further confirmed with real PM2.5 samples. Under the validated filtration condition, TD-GC-MS was applied for the analysis of non-polar organic compounds on real PM2.5 samples, and very good results were obtained.

  9. Identification of sink spots in two thermal desorption GC/MS systems for the analysis of polycyclic aromatic hydrocarbons.

    Science.gov (United States)

    Li, Yingjie; Zhu, Jiping

    2017-04-08

    Thermal desorption (TD) GC/MS has been used for the analysis of polycyclic aromatic hydrocarbons (PAHs) and other semi-volatile organic compounds. However, thermal desorption recovery of PAHs have not been well studied and the cause of PAH residues in a TD system has not been clearly understood. Our results showed that low volatility of PAHs can lead to their incomplete recovery in a TD system: for the PAHs with low vapour pressures, up to 10% and 3% could be lost in a two-stage (TS) TD system and a short-path (SP) TD system, respectively. Within the TSTD system, the majority of residues were found in the 4-port valve and in the spot where internal trap and the 4-port valve connects. Within the SPTD system, residues were largely confined to the tube needle connecting the sample tube and GC injection port as well as inside the injection port. Since the volatility of PAHs can represent the range typical of semi-volatile organic compounds (SVOCs), our results have a wide implication for the thermal desorption of SVOCs in general. Crown Copyright © 2017. Published by Elsevier B.V. All rights reserved.

  10. Enhancing radiative energy transfer through thermal extraction

    Directory of Open Access Journals (Sweden)

    Tan Yixuan

    2016-06-01

    Full Text Available Thermal radiation plays an increasingly important role in many emerging energy technologies, such as thermophotovoltaics, passive radiative cooling and wearable cooling clothes [1]. One of the fundamental constraints in thermal radiation is the Stefan-Boltzmann law, which limits the maximum power of far-field radiation to P0 = σT4S, where σ is the Boltzmann constant, S and T are the area and the temperature of the emitter, respectively (Fig. 1a. In order to overcome this limit, it has been shown that near-field radiations could have an energy density that is orders of magnitude greater than the Stefan-Boltzmann law [2-7]. Unfortunately, such near-field radiation transfer is spatially confined and cannot carry radiative heat to the far field. Recently, a new concept of thermal extraction was proposed [8] to enhance far-field thermal emission, which, conceptually, operates on a principle similar to oil immersion lenses and light extraction in light-emitting diodes using solid immersion lens to increase light output [62].Thermal extraction allows a blackbody to radiate more energy to the far field than the apparent limit of the Stefan-Boltzmann law without breaking the second law of thermodynamics.

  11. Carbamazepine in municipal wastewater and wastewater sludge: ultrafast quantification by laser diode thermal desorption-atmospheric pressure chemical ionization coupled with tandem mass spectrometry.

    Science.gov (United States)

    Mohapatra, D P; Brar, S K; Tyagi, R D; Picard, P; Surampalli, R Y

    2012-09-15

    In this study, the distribution of the anti-epileptic drug carbamazepine (CBZ) in wastewater (WW) and aqueous and solid phases of wastewater sludge (WWS) was carried out. A rapid and reliable method enabling high-throughput sample analysis for quicker data generation, detection, and monitoring of CBZ in WW and WWS was developed and validated. The ultrafast method (15s per sample) is based on the laser diode thermal desorption-atmospheric pressure chemical ionization (LDTD-APCI) coupled to tandem mass spectrometry (MS/MS). The optimization of instrumental parameters and method application for environmental analysis are presented. The performance of the novel method was evaluated by estimation of extraction recovery, linearity, precision and detection limit. The method detection limits was 12 ng L(-1) in WW and 3.4 ng g(-1) in WWS. The intra- and inter-day precisions were 8% and 11% in WW and 6% and 9% in WWS, respectively. Furthermore, three extraction methods, ultrasonic extraction (USE), microwave-assisted extraction (MAE) and accelerated solvent extraction (ASE) with three different solvent condition such as methanol, acetone and acetonitrile:ethyle acetate (5:1, v/v) were compared on the basis of procedural blank and method recovery. Overall, ASE showed the best extraction efficiency with methanol as compared to USE and MAE. Furthermore, the quantification of CBZ in WW and WWS samples showed the presence of contaminant in all stages of the treatment plant.

  12. Leidenfrost phenomenon-assisted thermal desorption (LPTD) and its application to open ion sources at atmospheric pressure mass spectrometry.

    Science.gov (United States)

    Saha, Subhrakanti; Chen, Lee Chuin; Mandal, Mridul Kanti; Hiraoka, Kenzo

    2013-03-01

    This work describes the development and application of a new thermal desorption technique that makes use of the Leidenfrost phenomenon in open ion sources at atmospheric pressure for direct mass spectrometric detection of ultratrace levels of illicit, therapeutic, and stimulant drugs, toxicants, and peptides (molecular weight above 1 kDa) in their unaltered state from complex real world samples without or with minor sample pretreatment. A low temperature dielectric barrier discharge ion source was used throughout the experiments and the analytical figures of merit of this technique were investigated. Further, this desorption technique coupled with other ionization sources such as electrospray ionization (ESI) and dc corona discharge atmospheric pressure chemical ionization (APCI) in open atmosphere was also investigated. The use of the high-resolution 'Exactive Orbitrap' mass spectrometer provided unambiguous identification of trace levels of the targeted compounds from complex mixtures and background noise; the limits of detection for various small organic molecules and peptides treated with this technique were at the level of parts per trillion and 10(-9) M, respectively. The high sensitivity of the present technique is attributed to the spontaneous enrichment of analyte molecules during the slow evaporation of the solvent, as well as to the sequential desorption of molecules from complex mixtures based on their volatilities. This newly developed desorption technique is simple and fast, while molecular ions are observed as the major ions.

  13. Trapping state of hydrogen isotopes in carbon and graphite investigated by thermal desorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Atsumi, H. [Department of Electric and Electronic Engineering, Kinki University, Higashiosaka (Japan); Tanabe, T. [Interdisciplinary Graduat School of Engineering Sciences, Kyushu University, Fukuoka (Japan); Shikama, T. [Institute for Materials Research, Tohoku University, Sendai (Japan)

    2015-03-15

    Thermal desorption spectrometry (TDS) has been investigated to obtain fundamental information of tritium behavior in graphite and carbon materials especially at high temperatures. 29 brands of graphite, HOPG, glassy carbon and CFC materials charged with deuterium gas are tested up to the temperature of 1735 K with a heating rate of 0.1 K/s. TDS spectra have five peaks at 600-700 K, around 900 K, 1200 K, 1300-1450 K and 1600-1650 K. The amounts of released deuterium have been compared with crystallographic parameters derived from XRD analysis. The results can be summarized as follows. First, TDS spectra of deuterium were quite varied among the samples tested, such as existence of peaks, peak temperatures and release amounts of deuterium. Secondly, TDS spectra may consist of five peaks, which are peak 1 (600-700 K), peak 2 (around 900 K), peak 3 (around 1200 K), peak 4 (1300-1450 K) and peak 5 (1600-1650 K). Thirdly, the correlations between the estimated surface area of edge surface and the total amount of released deuterium could be observed for peaks 4 and 5. Fourthly, high energy trapping site (peak 5) may exist even at edge surface or a near surface region, not only for intercalary. And fifth, in order to obtain the lower tritium retention for graphite and CFC materials, the material should be composed of a filler grain with a smaller crystallite size or having the smaller net edge surface in its structure. It is shown that heat treatment does not reduce originally existing trapping sites but trapping sites generated by neutron irradiation for instance can be reduced in some degree.

  14. Direct thermal desorption of semivolatile organic compounds from diffusion denuders and gas chromatographic analysis for trace concentration measurement.

    Energy Technology Data Exchange (ETDEWEB)

    Tobias, D. E.; Perlinger, J. A.; Morrow, P. S.; Doskey, P. V.; Perram, D.L.; Environmental Science Division; Michigan Technological Univ.

    2007-01-01

    A novel method for collection and analysis of vapor-phase semivolatile organic compounds (SOCs) in ambient air is presented. The method utilizes thermal desorption of SOCs trapped in diffusion denuders coupled with cryogenic preconcentration on Tenax-TA and analysis by high resolution gas chromatography (GC)-electron-capture detection (ECD). The sampling and analysis methods employ custom-fabricated multicapillary diffusion denuders, a hot gas spike (HGS) apparatus to load known quantities of thermally stable standards into diffusion denuders prior to sample collection, a custom-fabricated oven to thermally desorb SOCs from the diffusion denuder, and a programmable temperature vaporization (PTV) inlet containing a liner packed with Tenax-TA for effective preconcentration of the analytes and water management. High flow rates into the PTV inlet of 750 mL min-1during thermal desorption are ca. a factor of ten greater than typically used. To improve resolution and retention time stability, the thermal desorption and PTV inlet programming procedure includes three steps to prevent water from entering the analytic column while effectively transferring the analytes into the GC system. The instrumentation and procedures provide virtually complete and consistent transfer of analytes collected from ambient air into the GC evidenced by recovery of seven replicates of four internal standards of 90.7 {+-} 4.0-120 {+-} 23% (mean {+-} 95% confidence interval, CI). Retention time based compound identification is facilitated by low retention time variability with an average 95% CI of 0.024 min for sixteen replicates of eight standards. Procedure details and performance metrics as well as ambient sampling results are presented.

  15. Direct thermal desorption of semivolatile organic compounds from diffusion denuders and gas chromatographic analysis for trace concentration measurement.

    Science.gov (United States)

    Tobias, David E; Perlinger, Judith A; Morrow, Patrick S; Doskey, Paul V; Perram, David L

    2007-01-26

    A novel method for collection and analysis of vapor-phase semivolatile organic compounds (SOCs) in ambient air is presented. The method utilizes thermal desorption of SOCs trapped in diffusion denuders coupled with cryogenic preconcentration on Tenax-TA and analysis by high resolution gas chromatography (GC)-electron-capture detection (ECD). The sampling and analysis methods employ custom-fabricated multicapillary diffusion denuders, a hot gas spike (HGS) apparatus to load known quantities of thermally stable standards into diffusion denuders prior to sample collection, a custom-fabricated oven to thermally desorb SOCs from the diffusion denuder, and a programmable temperature vaporization (PTV) inlet containing a liner packed with Tenax-TA for effective preconcentration of the analytes and water management. High flow rates into the PTV inlet of 750mLmin(-1)during thermal desorption are ca. a factor of ten greater than typically used. To improve resolution and retention time stability, the thermal desorption and PTV inlet programming procedure includes three steps to prevent water from entering the analytic column while effectively transferring the analytes into the GC system. The instrumentation and procedures provide virtually complete and consistent transfer of analytes collected from ambient air into the GC evidenced by recovery of seven replicates of four internal standards of 90.7+/-4.0-120+/-23% (mean+/-95% confidence interval, CI). Retention time based compound identification is facilitated by low retention time variability with an average 95% CI of 0.024min for sixteen replicates of eight standards. Procedure details and performance metrics as well as ambient sampling results are presented.

  16. Rapid identification of pesticides in human oral fluid for emergency management by thermal desorption electrospray ionization/mass spectrometry.

    Science.gov (United States)

    Lee, Chi-Wei; Su, Hung; Chen, Peng-Yu; Lin, Shiang-Jiun; Shiea, Jentaie; Shin, Shyi-Jang; Chen, Bai-Hsiun

    2016-02-01

    Self-poisoning with pesticides accounts for approximately one-third of all suicides worldwide. To expedite rescue in the emergency department, it is essential to develop a point-of-care analytical method for rapid identification of ingested pesticides. In this study, five of the most common pesticides ingested by self-poisoning patients in Taiwan were analyzed from oral fluid samples. Pesticide-oral fluid mixtures were applied on a cotton swab and then transferred into methanol. A metallic probe was used to sample the methanol solution for subsequent thermal desorption-electrospray ionization mass spectrometry analysis. Altogether, pesticide sampling, transfer, desorption, ionization, and detection took less than 1 min. The reproducibility of this method (n = 6) was shown in the observed low-relative standard deviation (four human subjects by thermal desorption-electrospray ionization mass spectrometry were between 1-10 ppb with relative standard deviation 10.7%. Moreover, in this study, linear responses of five pesticides in oral fluid with concentrations between 1 ppb-1 ppm (R2 between 0.9938 and 0.9988) were observed. As the whole analytical process is extremely short, this technique allows for early non-invasive point-of-care identification of pesticides in the oral fluid of self-poisoning patients in the emergency room, providing important toxicological information for decision-making during critical resuscitation.

  17. Evaluation of Water Repellency in Petroleum Drilling Cuttings Treated by Thermal Desorption: Implications for Use in Construction and Agriculture

    Science.gov (United States)

    Domínguez-Rodríguez, Verónica I.; Guzmán-Osorio, Francisco J.; Adams Schroeder, Randy H.; Bautista-Margulis, Raúl G.

    2010-05-01

    Thermal desorption is one of many methods used for the remediation of hydrocarbon contaminated soils and similar materials. It has several advantages over competing technologies, especially with respect to treatment times. While the biological treatment of contaminated soils may take several months depending principally on the type of hydrocarbons and starting concentration, thermal desorption typically takes less than one month, depending on the treatment capacities of the equipment involved, and the volume of material requiring treatment. In the petroleum producing region of southeastern Mexico, this has been one of the principal methods used for the treatment of drilling cuttings, due mostly to the short time required. As with most remediation projects, as well as in the treatment of exploration and production (E&P) wastes, the criteria used to consider the remediation finalized is the concentration of hydrocarbons in the treated material. This is based on the supposition that at some (relatively low) hydrocarbon concentration, the toxicological affects are reduced to acceptable levels. However, little attention has been paid to the physical-chemical properties of supposedly treated material, which may suffer from water repellency, especially in thermal treatment methods. This could greatly reduce the options for final use of treated materials, especially to support plant growth. Conversely, there may be some construction uses of treated material in which some water repellence could be beneficial (caps for land fills, for example). Considering the relevance of the physical-chemical impacts of petroleum on soil and similar materials, we felt it was important to evaluate the efficiency of the principal method used to treat E&P wastes in Mexico (thermal desporption) based on these factors. In this study different operating conditions (temperature and residence time) of a sub-pilot scale thermal desorption unit were evaluated with respect not only to reduction in

  18. Quantification of diesel exhaust gas phase organics by a thermal desorption proton transfer reaction mass spectrometer

    Directory of Open Access Journals (Sweden)

    M. H. Erickson

    2012-02-01

    Full Text Available A new approach was developed to measure the total abundance of long chain alkanes (C12 and above in urban air using thermal desorption with a proton transfer reaction mass spectrometer (PTR-MS. These species are emitted in diesel exhaust and may be important precursors to secondary organic aerosol production in urban areas. Long chain alkanes undergo dissociative proton transfer reactions forming a series of fragment ions with formula CnH2n+1. The yield of the fragment ions is a function of drift conditions. At a drift field strength of 80 Townsends, the most abundant ion fragments from C10 to C16 n-alkanes were m/z 57, 71 and 85. The PTR-MS is insensitive to n-alkanes less than C8 but displays an increasing sensitivity for larger alkanes. Higher drift field strengths yield greater normalized sensitivity implying that the proton affinity of the long chain n-alkanes is less than H2O. Analysis of diesel fuel shows the mass spectrum was dominated by alkanes (CnH2n+1, monocyclic aromatics, and an ion group with formula CnH2n−1 (m/z 97, 111, 125, 139. The PTR-MS was deployed in Sacramento, CA during the Carbonaceous Aerosols and Radiative Effects Study field experiment in June 2010. The ratio of the m/z 97 to 85 ion intensities in ambient air matched that found in diesel fuel. Total diesel exhaust alkane concentrations calculated from the measured abundance of m/z 85 ranged from the method detection limit of ~1 μg m−3 to 100 μg m−3 in several air pollution episodes. The total diesel exhaust alkane concentration determined by this method was on average a factor of 10 greater than the sum of alkylbenzenes associated with spark ignition vehicle exhaust.

  19. The use of thermal desorption in monitoring for the chemical weapons demilitarization program.

    Science.gov (United States)

    Harper, Martin

    2002-10-01

    Under international treaty, the United States and Russia are disposing of their aging stockpile of chemical weapons. Incineration and chemical neutralization are options for sites in the United States, although Russia prefers the latter. The storage and disposal of bulk and chemical agents and weapons involve unique hazards of handling extremely toxic materials. There are three major areas of concern--the storage stockpile, the disposal area, and the discovery and destruction of "found" material not considered part of the stockpile. Methods have been developed to detect the presence of chemical agents in the air, and these are used to help assure worker protection and the safety of the local population. Exposure limits for all chemical agents are low, sometimes nanograms per cubic meter for worker control limits and picograms per cubic meter for general population limits. There are three types of monitoring used in the USA: alarm, confirmation, and historical. Alarm monitors are required to give relatively immediate real-time responses to agent leaks. They are simple to operate and rugged, and provide an alarm in near real-time (generally a few minutes). Alarm monitors for the demilitarization program are based on sorbent pre-concentration followed by thermal desorption and simple gas chromatography. Alarms may need to be confirmed by another method, such as sample tubes collocated with the alarm monitor and analyzed in a laboratory by more sophisticated chromatography. Sample tubes are also used for historical perimeter monitoring, with sample periods typically of 12 h. The most common detector is the flame photometric detector, in sulfur or phosphorous mode, although others, such as mass-selective detectors, also have been used. All agents have specific problems with collection, chromatography and detection. Monitoring is not made easier by interferences from pesticide spraying, busy roadways or military firing ranges. Exposure limits drive the requirements for

  20. Optimization of a Dynamic Headspace-Thermal Desorption-Gas Chromatography/Mass Spectrometry procedure for the determination of furfurals in vinegars.

    Science.gov (United States)

    Manzini, Simona; Durante, Caterina; Baschieri, Carlo; Cocchi, Marina; Sighinolfi, Simona; Totaro, Sara; Marchetti, Andrea

    2011-08-15

    The use of a Dynamic Headspace System (DHS) device combined with a Thermal Desorption Unit (TDU) interfaced to a Gas Chromatography/Mass Spectrometry (GC/MS) system is proposed for the determination of furfurals in oenological products. An experimental design protocol has been employed for the optimization of the instrumental settings concerning DHS and TDU extraction and desorption steps. It has been possible to individuate the following optimized conditions: incubation temperature 40°C, purge volume 800 mL, dry volume 1500 mL, TDU hold time 5 min and incubation time 10 min. The performance of two different SPE sorbents, namely Tenax TA and Tenax GR used for the furfurals trapping, was investigated too. The developed DHS sampling procedure showed good reproducibility values with a RSD% lower than 10% for all the monitored species. The optimized experimental settings have been used to determine furfurals in several vinegar samples obtained by traditional procedure starting from cooked grape musts, i.e. in Aceto Balsamico Tradizionale di Modena (ABTM). In fact, the control of these species is extremely important for quality and safety issues.

  1. Analysis of trimethoprim, lincomycin, sulfadoxin and tylosin in swine manure using laser diode thermal desorption-atmospheric pressure chemical ionization-tandem mass spectrometry.

    Science.gov (United States)

    Solliec, Morgan; Massé, Daniel; Sauvé, Sébastien

    2014-10-01

    A new extraction method coupled to a high throughput sample analysis technique was developed for the determination of four veterinary antibiotics. The analytes belong to different groups of antibiotics such as chemotherapeutics, sulfonamides, lincosamides and macrolides. Trimethoprim (TMP), sulfadoxin (SFX), lincomycin (LCM) and tylosin (TYL) were extracted from lyophilized manure using a sonication extraction. McIlvaine buffer and methanol (MeOH) were used as extraction buffers, followed by cation-exchange solid phase extraction (SPE) for clean-up. Analysis was performed by laser diode thermal desorption-atmospheric pressure chemical-ionization (LDTD-APCI) tandem mass spectrometry (MS/MS) with selected reaction monitoring (SRM) detection. The LDTD is a high throughput sample introduction method that reduces total analysis time to less than 15s per sample, compared to minutes when using traditional liquid chromatography (LC). Various SPE parameters were optimized after sample extraction: the stationary phase, the extraction solvent composition, the quantity of sample extracted and sample pH. LDTD parameters were also optimized: solvent deposition, carrier gas, laser power and corona discharge. The method limit of detection (MLD) ranged from 2.5 to 8.3 µg kg(-1) while the method limit of quantification (MLQ) ranged from 8.3 to 28µgkg(-1). Calibration curves in the manure matrix showed good linearity (R(2)≥ 0.996) for all analytes and the interday and intraday coefficients of variation were below 14%. Recoveries of analytes from manure ranged from 53% to 69%. The method was successfully applied to real manure samples. Copyright © 2014 Elsevier B.V. All rights reserved.

  2. Thermal decomposition of AlH{sub 3} studied by in situ synchrotron X-ray diffraction and thermal desorption spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Maehlen, J.P. [Institute for Energy Technology, P.O. Box 40, Kjeller No-2027 (Norway); Yartys, V.A. [Institute for Energy Technology, P.O. Box 40, Kjeller No-2027 (Norway)], E-mail: volodymyr.yartys@ife.no; Denys, R.V. [Institute for Energy Technology, P.O. Box 40, Kjeller No-2027 (Norway); Physico-Mechanical Institute of the National Academy of Science of Ukraine, 5, Naukova Str., 79601 Lviv (Ukraine); Fichtner, M.; Frommen, Ch. [Institute of Nanotechnology, Forschungszentrum Karlsruhe GmbH, P.O. Box 30640, D-76021 Karlsruhe (Germany); Bulychev, B.M. [Chemistry Department, Moscow State University, Leninskie Gori, Moscow 119992, MSU, Chemistry Department (Russian Federation); Pattison, P.; Emerich, H.; Filinchuk, Y.E.; Chernyshov, D. [Swiss-Norwegian Beam Line, ESRF, BP 220, F-38043 Grenoble (France)

    2007-10-31

    The thermal decomposition of alane was investigated by application of synchrotron X-ray diffraction (SR-XRD) and thermal desorption spectroscopy (TDS). Two polymorphs were studied, {alpha}- and {gamma}-AlH{sub 3}. Activation energies, anisotropic volume expansions, and phase transformation paths were found. In addition, the crystal structure data, including structure of hydrogen sublattice, and small charge transfer from the aluminium towards the hydrogen sites were observed during a high-resolution SR-XRD study of {alpha}-AlH{sub 3}.

  3. Development of a thermal desorption-gas chromatography-mass spectrometry method for determining personal care products in air.

    Science.gov (United States)

    Ramírez, Noelia; Marcé, Rosa Maria; Borrull, Francesc

    2010-06-25

    This study describes the development of a new analytical method for determining 14 personal care products (PCPs) - nine synthetic musks, four parabens and one insect repellent - in air samples. The method is based on active sampling on sorbent tubes and thermal desorption-gas chromatography-mass spectrometry analysis, and is rapid, sensitive and drastically reduces the risk of sample contamination. Three kinds of tubes and traps were tested, those filled with Tenax TA being the most suitable for this study. Method validation showed good repeatability and reproducibility, low detection limits (between 0.03 ng m(-3) for DPMI and 12.5 ng m(-3) for propyl paraben) and good linearity for all compounds. Stability during storage indicated that samples must be kept refrigerated at 4 degrees C and analysed within 1 week of collection. The applicability of the technique to real samples was tested in different indoor and outdoor atmospheres. The total PCP values for indoor air ranged from 135 ng m(-3) in a pharmacy to 2838 ng m(-3) in a hairdresser's, whereas the values for outdoor air ranged from 14 ng m(-3) for a suburban environment to 26 ng m(-3) for an urban environment. In general, the most abundant synthetic musks were galaxolide (5.9-1256 ng m(-3)), musk xylene (1.6-766 ng m(-3)) and tonalide (1.1-138 ng m(-3)). Methyl and ethyl paraben (2.4-313 ng m(-3) and 1.8-117 ng m(-3), respectively) were the most abundant parabens. Although thermal desorption methods have been widely used for determining volatile organic compounds, they are rarely used with semi-volatile compounds. This study thus demonstrates that the thermal desorption method performs well with semi-volatile compounds and, for the first time, that it can be used for determining PCPs.

  4. Monitoring of PAHs in air by collection on XAD-2 adsorbent then microwave-assisted thermal desorption coupled with headspace solid-phase microextraction and gas chromatography with mass spectrometric detection.

    Science.gov (United States)

    Wei, Ming-Chi; Chang, Wan-Ting; Jen, Jen-Fon

    2007-02-01

    Microwave-assisted thermal desorption (MAD) coupled to headspace solid-phase microextraction (HS-SPME) has been studied for in-situ, one-step, sample preparation for PAHs collected on XAD-2 adsorbent, before gas chromatography with mass spectrometric detection. The PAHs on XAD-2 were desorbed into the extraction solution, evaporated into the headspace by use of microwave irradiation, and absorbed directly on a solid-phase microextraction fiber in the headspace. After desorption from the SPME fiber in the hot GC injection port, PAHs were analyzed by GC-MS. Conditions affecting extraction efficiency, for example extraction solution, addition of salt, stirring speed, SPME fiber coating, sampling temperature, microwave power and irradiation time, and desorption conditions were investigated. Experimental results indicated that extraction of 275 mg XAD-2, containing 10-200 ng PAHs, with 10-mL ethylene glycol-1 mol L(-1) NaCl solution, 7:3, by irradiation with 120 W for 40 min (the same as the extraction time), and collection with a PDMS-DVB fiber at 35 degrees C, resulted in the best extraction efficiency. Recovery was more than 80% and RSD was less than 14%. Optimum desorption was achieved by heating at 290 degrees C for 5 min. Detection limits varied from 0.02 to 1.0 ng for different PAHs. A real sample was obtained by using XAD-2 to collect smoke from indoor burning of joss sticks. The amounts of PAHs measured varied from 0.795 to 2.53 ng. The method is a simple and rapid procedure for determination of PAHs on XAD-2 absorbent, and is free from toxic organic solvents.

  5. SPS extraction kicker magnet thermal analysis

    CERN Document Server

    Timmins, M

    2004-01-01

    As the SPS accelerator will be used for the CNGS project and as LHC injector, the proton beams passing through its extraction kickers will have a much higher intensity than in the past. The image currents generated by this beam may provoke a temperature increase in the magnet's ferrite core to temperatures above the Curie temperature, unless the heat produced is effectively removed. A further complication arises from the fact that a high voltage is applied to the ferrites. The solution adopted consists in transferring the heat via Aluminium Nitride insulators to a water cooling circuit. The heat transfer analysis and the calculated thermal distribution of the magnet are presented.

  6. The thermal desorption of CO2 from amine carbamate solutions for the 13C isotope enrichment

    Science.gov (United States)

    Dronca, S.; Varodi, C.; Gligan, M.; Stoia, V.; Baldea, A.; Hodor, I.

    2012-02-01

    The CO2 desorption from amine carbamate in non-aqueous solvents is of major importance for isotopic enrichment of 13C. A series of experiments were carried out in order to set up the conditions for the CO2 desorption. For this purpose, a laboratory- scale plant for 13C isotope separation by chemical exchange between CO2 and amine carbamate was designed and used. The decomposition of the carbamate solution was mostly produced in the desorber and completed in the boiler. Two different-length desorbers were used, at different temperatures and liquid flow rates of the amine-non-aqueous solvent solutions. The residual CO2 was determined by using volumetric and gaschromatographic methods. These results can be used for enrichment of 13C by chemical exchange between CO2 and amine carbamate in nonaqueous solvents.

  7. Biological functioning of PAH-polluted and thermal desorption-treated soils assessed by fauna and microbial bioindicators.

    Science.gov (United States)

    Cébron, Aurélie; Cortet, Jérôme; Criquet, Stéven; Biaz, Asmaa; Calvert, Virgile; Caupert, Cécile; Pernin, Céline; Leyval, Corinne

    2011-11-01

    A large number of soil bioindicators were used to assess biological diversity and activity in soil polluted with polycyclic aromatic hydrocarbons (PAHs) and the same soil after thermal desorption (TD) treatment. Abundance and biodiversity of bacteria, fungi, protozoa, nematodes and microarthropods, as well as functional parameters such as enzymatic activities and soil respiration, were assessed during a two year period of in situ monitoring. We investigated the influence of vegetation (spontaneous vegetation and Medicago sativa) and TD treatment on biological functioning. Multivariate analysis was performed to analyze the whole data set. A principal response curve (PRC) technique was used to evaluate the different treatments (various vegetation and contaminated vs. TD soil) contrasted with control (bare) soil over time. Our results indicated the value of using a number of complementary bioindicators, describing both diversity and functions, to assess the influence of vegetation on soil and discriminate polluted from thermal desorption (TD)-treated soil. Plants had an influence on the abundance and activity of all organisms examined in our study, favoring the whole trophic chain development. However, although TD-treated soil had a high abundance and diversity of microorganisms and fauna, enzymatic activities were weak because of the strong physical and chemical modifications of this soil. Copyright © 2011 Institut Pasteur. Published by Elsevier Masson SAS. All rights reserved.

  8. Application of Thermal Desorption Unit (TDU) to treat low-toxicity mineral oil base cuttings in Barinas District, Venezuela

    Energy Technology Data Exchange (ETDEWEB)

    Rendon, Ruben [Petroleos de Venezuela, Caracas (Venezuela); Luzardo, Janeth; Alcoba, Alcides [M-I SWACO, Houston, TX (United States)

    2008-07-01

    The potential environmental impact of oil-based drill cuttings is generating increased scrutiny in the oil and gas industry. If left untreated, oil-based cuttings not only increase the risk of environmental liabilities, but also affect revenue, as drilling generates wastes that in most cases require special treatment before disposal. Consequently, the oil industry is looking for technologies to help minimize environmental liabilities. Accordingly, the Barinas District of PDVSA has started a pilot trial to treat oil-based drilling cuttings by applying thermal desorption technology. The main objective of this technology is recovering trapped hydrocarbons, while minimizing wastes and preparing solids to be disposed of through a mobile treatment plant. This novel technology has been used worldwide to treat organic pollutants in soil. Thermal desorption is a technology based on the application of heat in soils polluted with organic compounds. With this technology, target temperatures vary according to the type and concentration of detected pollutants along with its characterization, in such a way that compounds are disposed of by volatilization. As part of the integral waste management development along with the pilot trial for hydrocarbon-contaminated solid waste treatment, trials on soils were undertaken by applying process-generated ashes in equally-sized bins, with different mixtures (ashes, ashes organic material, ashes-organic material-sand, ashes-land). The resulting process offers an immediate soil remediation and final disposal solution for toxic and dangerous waste. (author)

  9. Ion-to-Neutral Ratios and Thermal Proton Transfer in Matrix-Assisted Laser Desorption/Ionization.

    Science.gov (United States)

    Lu, I-Chung; Chu, Kuan Yu; Lin, Chih-Yuan; Wu, Shang-Yun; Dyakov, Yuri A; Chen, Jien-Lian; Gray-Weale, Angus; Lee, Yuan-Tseh; Ni, Chi-Kung

    2015-07-01

    The ion-to-neutral ratios of four commonly used solid matrices, α-cyano-4-hydroxycinnamic acid (CHCA), 2,5-dihydroxybenzoic acid (2,5-DHB), sinapinic acid (SA), and ferulic acid (FA) in matrix-assisted laser desorption/ionization (MALDI) at 355 nm are reported. Ions are measured using a time-of-flight mass spectrometer combined with a time-sliced ion imaging detector. Neutrals are measured using a rotatable quadrupole mass spectrometer. The ion-to-neutral ratios of CHCA are three orders of magnitude larger than those of the other matrices at the same laser fluence. The ion-to-neutral ratios predicted using the thermal proton transfer model are similar to the experimental measurements, indicating that thermal proton transfer reactions play a major role in generating ions in ultraviolet-MALDI.

  10. Thermal desorption of deuterium from Be, and Be with helium bubbles

    Energy Technology Data Exchange (ETDEWEB)

    Fedorov, A.V.; Van Veen, A.; Busker, G.J. [Delft Univ. of Technology (Netherlands). Interfaculty Reactor Inst.

    1998-01-01

    Deuterium desorption measurements carried out on a single-crystalline beryllium sample are presented. Deuterium ions were implanted at room temperature at the energy of 0.7 and 1.2 keV up to doses ranging from 10{sup 19} to 3.6 x 10{sup 21} m{sup -2}. In order to eliminate the influence of the beryllium-oxide surface layer, before the implantation the surface of the sample was cleaned by argon sputtering. After the implantation the sample was annealed up to 1200 K at a constant rate of 10 K/s. Deuterium released from the sample was monitored by a calibrated quadrupole mass-spectrometer. The desorption spectra revealed two different contributions. One is a well defined and very narrow peak centered around 450 K. This peak is observed only at high implantation doses > 7.8 x 10{sup 20} m{sup -2}, which is close to the deuterium saturation limit of 0.3 D/Be and is related to deuterium release from blisters or interconnected bubbles. The activation energy of 1.1 eV and the threshold implantation dose are consistent with the values reported in literature. The second contribution in the release spectra is found in the temperature range from 600 to 900 K and is present throughout the whole range of the implantation doses. The activation energies corresponding to this release lie in the range between 1.8 and 2.5 eV and are ascribed to the release from deuterium-vacancy type of defects. In a number of experiments the deuterium implantation was preceded by helium implantation followed by partial annealing to create helium bubbles. The resulting deuterium desorption spectra indicate that deuterium detrapping from helium bubbles is characterized by an activation energy of 2.7 eV. (author)

  11. Essential oil extraction with concentrating solar thermal energy

    OpenAIRE

    Veynandt, François

    2015-01-01

    Material complementari del cas estudi "Essential oil extraction with concentrating solar thermal energy”, part component del llibre "Case studies for developing globally responsible engineers" Peer Reviewed

  12. Direct Detection of Pharmaceuticals and Personal Care Products from Aqueous Samples with Thermally-Assisted Desorption Electrospray Ionization Mass Spectrometry

    Science.gov (United States)

    Campbell, Ian S.; Ton, Alain T.; Mulligan, Christopher C.

    2011-07-01

    An ambient mass spectrometric method based on desorption electrospray ionization (DESI) has been developed to allow rapid, direct analysis of contaminated water samples, and the technique was evaluated through analysis of a wide array of pharmaceutical and personal care product (PPCP) contaminants. Incorporating direct infusion of aqueous sample and thermal assistance into the source design has allowed low ppt detection limits for the target analytes in drinking water matrices. With this methodology, mass spectral information can be collected in less than 1 min, consuming ~100 μL of total sample. Quantitative ability was also demonstrated without the use of an internal standard, yielding decent linearity and reproducibility. Initial results suggest that this source configuration is resistant to carryover effects and robust towards multi-component samples. The rapid, continuous analysis afforded by this method offers advantages in terms of sample analysis time and throughput over traditional hyphenated mass spectrometric techniques.

  13. Thermal desorption study of catalytic systems. Communication 20. Adsorption of water vapors on the calcium aluminate components of catalysts

    Energy Technology Data Exchange (ETDEWEB)

    Nissenbaum, V.D.; Danyushevskii, V.Y.; Golosman, E.Z.; Rubinstein, A.M.; Yakerson, V.I.

    1985-05-01

    Ca aluminates are used as a component of catalysts of gas-phase processes, some of which take place with the participation of water. Nickel calcium aluminate catalysts are thus used for hydrogenation of CO and CO/sub 2/ to CH/sub 4/ and water; zinc calcium aluminate catalysts are used for sulfur purification of process gases, where water is liberated during sulfiding of ZnO; and copper zinc calcium aluminate catalysts are used in low-temperature conversion of CO with water vapor. It is also known that Ca aluminates undergo various transformations in aqueous media with the formation of Ca hydroaluminates. This paper discusses the adsorption of water from the gas phase on calcium aluminate systems, which was investigated by the thermal desorption method. Samples of varying phase composition, different CaO/Al/sub 2/O/sub 3/ ratios, and specific surface areas were also studied and are reported on here.

  14. Affinity mesh screen materials for selective extraction and analysis of antibiotics using transmission mode desorption electrospray ionization mass spectrometry.

    Science.gov (United States)

    Yang, Samuel H; Wang, Evelyn H; Gurak, John A; Bhawal, Sumit; Deshmukh, Rajendrasing; Wijeratne, Aruna B; Edwards, Brian L; Foss, Frank W; Timmons, Richard B; Schug, Kevin A

    2013-06-25

    The extraction of active compounds from natural sources has shown to be an effective approach to drug discovery. However, the isolation and identification of natural products from complex extracts can be an arduous task. A novel approach to drug discovery is presented through the use of polymer screens functionalized with an l-lysine-d-alanine-d-alanine (Kaa) peptide to create new affinity capture mesh screen materials. The Kaa sequence is a well-characterized specific binding site for antibiotics that inhibit cell wall synthesis in Gram-positive bacteria. The detailed synthesis and characterization of these novel screen materials are presented in this work. Polypropylene mesh screens were first coated with a poly(acrylic acid) film by pulsed plasma polymerization. The synthesized Kaa peptide was then covalently attached to carboxylic acid groups through a condensation reaction. An analysis of captured compounds was performed in a rapid fashion with transmission-mode desorption electrospray ionization (TM-DESI) mass spectrometry. A proof of principle was demonstrated to show the ability of the novel affinity capture materials to select for a macrocyclic antibiotic, vancomycin, over a negative control compound, spectinomycin. With further development, this method may provide a rapid screening technique for new antibacterial compounds, for example, those extracted from natural product sources having a limited supply. Here, we show that the screen can capture vancomycin preferentially over spectinomycin in a spiked extract of tea leaves.

  15. Analysis of roasted and unroasted Pistacia terebinthus volatiles using direct thermal desorption-GCxGC-TOF/MS.

    Science.gov (United States)

    Gogus, F; Ozel, M Z; Kocak, D; Hamilton, J F; Lewis, A C

    2011-12-01

    The objective of this study was to determine the effects of roasting time on volatile components of Pistacia terebinthus L., a fruit growing wild in Turkey. The whole fruit samples were pan roasted for 0, 5, 10, 15, 20 and 25min at 200°C. Volatile compounds were isolated and identified using the direct thermal desorption (DTD) method coupled with comprehensive gas chromatography - time of flight mass spectrometry (GCxGC-TOF/MS). The major components of the fresh hull of P. terebinthus were α-pinene (10.37%), limonene (8.93%), β-pinene (5.53%), 2-carene (4.47%) and γ-muurolene (4.29%). Eighty-three constituents were characterised from the volatiles of fresh whole P. terebinthus fruits obtained by direct thermal desorption with α-pinene (9.62%), limonene (5.54%), γ-cadinane (5.48%), β-pinene (5.46%), β-caryophyllene (5.24%) being the major constituents. The type and the number of constituents characterised were observed to change with differing roasting times. Limonene (5.56%), α-pinene (4.84%), 5-methylfurfural (4.78%), 5-hydroxymethylfurfural (5-HMF, 3.89%), dimethylmetoxyfuranone (3.67%) and 3-methyl-2(5H)furanone (3.12%) were identified as the major components among the 104 compounds characterised in the volatiles of P. terebinthus, roasted for 25min. In addition, volatiles of fully roasted P. terebinthus fruits contained furans and furanones (15.42%), pyridines (4.45%) and benzene derivatives (3.81%) as the major groups.

  16. Characterization of olive oil volatiles by multi-step direct thermal desorption-comprehensive gas chromatography-time-of-flight mass spectrometry using a programmed temperature vaporizing injector

    NARCIS (Netherlands)

    de Koning, S.; Kaal, E.; Janssen, H.-G.; van Platerink, C.; Brinkman, U.A.Th.

    2008-01-01

    The feasibility of a versatile system for multi-step direct thermal desorption (DTD) coupled to comprehensive gas chromatography (GC × GC) with time-of-flight mass spectrometric (TOF-MS) detection is studied. As an application the system is used for the characterization of fresh versus aged olive oi

  17. 24-HOUR DIFFUSIVE SAMPLING OF 1,3-BUTADIENE IN AIR ONTO CARBOPACK X SOLID ADSORBENT FOLLOWED BY THERMAL DESORPTION/GC/MS ANALYSIS - FEASIBILITY STUDY

    Science.gov (United States)

    Diffusive sampling of 1,3-butadiene for 24 hr onto the graphitic adsorbent Carbopack X packed in a stainless steel tube badge (6.3 mm o.d., 5 mm i.d., and 90 mm in length) with analysis by thermal desorption/gas chromatography (GC)/mass spectrometry (MS) has been evaluated in con...

  18. Thermal Desorption/Ultraviolet Photolysis Process Technology Research, Test, and Evaluation Performed at the Naval Construction Battalion Center, Gulfport, Mississippi, for the USAF Installation Restoration Program. Volume 2

    Science.gov (United States)

    1987-12-01

    packed in ice. Sampling of vent gas and off- gases from the two thermal desorption technologies will be performie using procedures and techniques...solvent used in it. wash with hot voat Cenaslunug detergent.. inse with copioua aMunts of tap water and severa2 portioc of distilled voter. Drain d4y

  19. Modeling of the Kinetics of Supercritical Fluid Extraction of Lipids from Microalgae with Emphasis on Extract Desorption.

    Science.gov (United States)

    Sovová, Helena; Nobre, Beatriz P; Palavra, António

    2016-05-27

    Microalgae contain valuable biologically active lipophilic substances such as omega-3 fatty acids and carotenoids. In contrast to the recovery of vegetable oils from seeds, where the extraction with supercritical CO₂ is used as a mild and selective method, economically viable application of this method on similarly soluble oils from microalgae requires, in most cases, much higher pressure. This paper presents and verifies hypothesis that this difference is caused by high adsorption capacity of microalgae. Under the pressures usually applied in supercritical fluid extraction from plants, microalgae bind a large fraction of the extracted oil, while under extremely high CO₂ pressures their adsorption capacity diminishes and the extraction rate depends on oil solubility in supercritical CO₂. A mathematical model for the extraction from microalgae was derived and applied to literature data on the extraction kinetics in order to determine model parameters.

  20. Modeling of the Kinetics of Supercritical Fluid Extraction of Lipids from Microalgae with Emphasis on Extract Desorption

    Directory of Open Access Journals (Sweden)

    Helena Sovová

    2016-05-01

    Full Text Available Microalgae contain valuable biologically active lipophilic substances such as omega-3 fatty acids and carotenoids. In contrast to the recovery of vegetable oils from seeds, where the extraction with supercritical CO2 is used as a mild and selective method, economically viable application of this method on similarly soluble oils from microalgae requires, in most cases, much higher pressure. This paper presents and verifies hypothesis that this difference is caused by high adsorption capacity of microalgae. Under the pressures usually applied in supercritical fluid extraction from plants, microalgae bind a large fraction of the extracted oil, while under extremely high CO2 pressures their adsorption capacity diminishes and the extraction rate depends on oil solubility in supercritical CO2. A mathematical model for the extraction from microalgae was derived and applied to literature data on the extraction kinetics in order to determine model parameters.

  1. Combined effects of DOM extracted from site soil/compost and biosurfactant on the sorption and desorption of PAHs in a soil-water system.

    Science.gov (United States)

    Yu, Hui; Huang, Guo-he; An, Chun-jiang; Wei, Jia

    2011-06-15

    The combined effects of DOM and biosurfactant on the sorption/desorption behavior of phenanthrene (PHE) and pyrene (PYR) in soil water systems were systematically investigated. Two origins of DOMs (extracted from soil and extracted from food waste compost) and an anionic biosurfactant (rhamnolipid) were introduced. The presence of DOM in the aqueous phase could decrease the sorption of PAHs, thus influence their mobility. Desorption enhancement for both PHE and PYR in the system with compost DOM was greater than that in the soil DOM system. This is due to the differences in specific molecular structures and functional groups of two DOMs. With the co-existence of biosurfactant and DOM, partitioning is the predominant process and the desorption extent was much higher than the system with DOM or biosurfactant individually. For PHE, the desorption enhancement of combined DOM and biosurfactant was larger than the sum of DOM or biosurfactant; however desorption enhancement for PYR in the combined system was less than the additive enhancement in two individual system under low PAH concentration. This could be explained as the competition sorption among PAHs, DOM and biosurfactant. The results of this study will help to clarify the transport of petroleum pollutants in the remediation of HOCs-contaminated soils.

  2. Thin-layer chromatography and mass spectrometry coupled using proximal probe thermal desorption with electrospray or atmospheric pressure chemical ionization.

    Science.gov (United States)

    Ovchinnikova, Olga S; Van Berkel, Gary J

    2010-06-30

    An atmospheric pressure proximal probe thermal desorption sampling method coupled with secondary ionization by electrospray or atmospheric pressure chemical ionization was demonstrated for the mass spectrometric analysis of a diverse set of compounds (dyestuffs, pharmaceuticals, explosives and pesticides) separated on various high-performance thin-layer chromatography plates. Line scans along or through development lanes on the plates were carried out by moving the plate relative to a stationary heated probe positioned close to or just touching the stationary phase surface. Vapors of the compounds thermally desorbed from the surface were drawn into the ionization region of a combined electrospray ionization/atmospheric pressure chemical ionization source where they merged with reagent ions and/or charged droplets from a corona discharge or an electrospray emitter and were ionized. The ionized components were then drawn through the atmospheric pressure sampling orifice into the vacuum region of a triple quadrupole mass spectrometer and detected using full scan, single ion monitoring, or selected reaction monitoring mode. Studies of variable parameters and performance metrics including the proximal probe temperature, gas flow rate into the ionization region, surface scan speed, read-out resolution, detection limits, and surface type are discussed.

  3. Thermal desorption counter-flow introduction atmospheric pressure chemical ionization for direct mass spectrometry of ecstasy tablets.

    Science.gov (United States)

    Inoue, Hiroyuki; Hashimoto, Hiroaki; Watanabe, Susumu; Iwata, Yuko T; Kanamori, Tatsuyuki; Miyaguchi, Hajime; Tsujikawa, Kenji; Kuwayama, Kenji; Tachi, Noriyuki; Uetake, Naohito

    2009-09-01

    A novel approach to the analysis of ecstasy tablets by direct mass spectrometry coupled with thermal desorption (TD) and counter-flow introduction atmospheric pressure chemical ionization (CFI-APCI) is described. Analytes were thermally desorbed with a metal block heater and introduced to a CFI-APCI source with ambient air by a diaphragm pump. Water in the air was sufficient to act as the reactive reagent responsible for the generation of ions in the positive corona discharge. TD-CFI-APCI required neither a nebulizing gas nor solvent flow and the accompanying laborious optimizations. Ions generated were sent in the direction opposite to the air flow by an electric field and introduced into an ion trap mass spectrometer. The major ions corresponding to the protonated molecules ([M + H](+)) were observed with several fragment ions in full scan mass spectrometry (MS) mode. Collision-induced dissociation of protonated molecules gave characteristic product-ion mass spectra and provided identification of the analytes within 5 s. The method required neither sample pretreatment nor a chromatographic separation step. The effectiveness of the combination of TD and CFI-APCI was demonstrated by application to the direct mass spectrometric analysis of ecstasy tablets and legal pharmaceutical products.

  4. Demonstration Testing of a Thermal Desorption Unit to Receive and Treat Waste with Unlimited Concentration of PCBs - 13437

    Energy Technology Data Exchange (ETDEWEB)

    Orton, Timothy L. [EnergySolutions, 423 West 300 South, Salt Lake City, UT 84101 (United States); Palmer, Carl R. [TD.X Associates LP, 148 South Dowlen Road, PMB 700, Beaumont, TX 77707 (United States)

    2013-07-01

    For the last nine years, EnergySolutions and TD*X Associates LP have teamed up to provide the most comprehensive organic removal treatment process in the radioactive waste industry. The high performance thermal desorption unit (HP-TDU) located at the EnergySolutions Clive facility in Utah has successfully processed over 1,850 tons of organically contaminated radioactive mixed waste. Products from the HP-TDU system include a radioactively contaminated dry solid material that can be disposed in the on-site landfill and an organic condensate with high thermal energy content that is generally below background radiation and capable of free-release to a non-radioactive incinerator. Over the years, Permits and approvals have been obtained through the state of Utah, United States Environmental Protection Agency (USEPA) Region 8, and USEPA headquarters that enable the treatment of several waste categories including volatile and semi-volatile organic compounds, combustion-coded (CMBST) compounds, volatile metals, and polychlorinated biphenyls (PCBs). The unit has recently successfully completed Demonstration Testing for PCB concentrations up to 660,000 ppm (parts per million). Solid processed material from this Demonstration Testing was less than two ppm PCBs in three separate treatment runs; reprocessing or additional treatment was not needed to meet this limit. Through post-demonstration permitting, the system is unlimited in scope as approval has been given to receive and solidify up to pure PCBs down to this processing limit concentration to complete treatment of mixed waste. (authors)

  5. Precautions for in-injection port thermal desorption-gas chromatography/mass spectrometry (TD-GC/MS) as applied to aerosol filter samples

    Science.gov (United States)

    Ho, Steven Sai Hang; Chow, Judith C.; Watson, John G.; Ting Ng, Louisa Pan; Kwok, Yuk; Ho, K. F.; Cao, Junji

    2011-03-01

    In-injection port thermal desorption-gas chromatography/mass spectrometry (TD-GC/MS) allows for analysis for >130 non-polar organic compounds on small quartz-fiber filter samples without extraction chemicals. TD-GC/MS has been applied to samples from long-term U.S. networks since it is cost effective and less labor intensive. However, analysis of large numbers of samples results in sensitivity reductions over time. Instrument sensitivity and reproducibility were examined after 100, 200, and 500 sample analyses. Analyses of standards between batches of heavily loaded samples from China and Japan showed signal decreases of 28-78% for major organic classes. In the GC injection port, residues can accumulate on the gold-plated seal resulting in analyte adsorption as well as elevating signal background. Decreases in signal response were 28-43% for n-alkanes, 33-45% for hopanes and steranes, 28-56% for PAHs, and 38-78% for phthalates when the gold-plated seal was not replaced after 500 TD-GC/MS sample analyses. Limits of detection (LODs) also increased by 14-76% for the targeted non-polar organic compounds. Residues trapped in the capillary column head can cause peak broadening and overlap. The GC/MS system, including the injection port and gold seal, the column head (where the eluted sample is pre-concentrated), and the ion source should be cleaned after every batch of 50-100 samples.

  6. Determination of dithiocarbamate pesticides in occupational hygiene sampling devices using the isooctane method and comparison with an automatic thermal desorption (ATD) method.

    Science.gov (United States)

    Coldwell, Matthew R; Pengelly, Ian; Rimmer, Duncan A

    2003-01-10

    Two new methods for the determination of dithiocarbamate pesticides in occupational hygiene sampling devices are described. Dithiocarbamate spiked occupational hygiene sampling devices, consisting of glass fibre (GF/A) filters, cotton pads, cotton gloves and disposable overalls, were reduced under acidic conditions and the CS2 evolved as a decomposition product was extracted into isooctane. The isooctane was then analysed using gas chromatography with mass spectrometry, for CS2, which provided a quantitative result for dithiocarbamates. Recoveries obtained were generally within a 70-110% range and reproducibilities better than 15% RSD were typically achieved. The method has been successfully applied to samples collected during occupational exposure surveys. A second method employing automatic thermal desorption-gas chromatography-mass spectrometry (ATD-GC-MS) has also been developed and applied to the direct analysis of GF/A (airborne) samples. The method relies on the thermal degradation of dithiocarbamates to release CS2, which is used to quantify the analytes. Thiram spiked GF/A filters gave an average recovery of 107% with an RSD of 4%. The performance of the two analytical methods were directly compared by analysing sub-portions of GF/A filters collected during a survey to evaluate occupational exposures to thiram during seed treatment operations. Both methods performed well for the analysis of airborne (GF/A) samples and produced results in good agreement. ATD-GC-MS is the preferred method for studies involving GF/A (airborne) samples only. Because of the wider applicability of the isooctane method for other sampling devices, it is the preferred choice when carrying out surveys which require a dermal as well as respirable exposure assessment.

  7. Determination of trace organic impurities in water using thermal desorption from XAD resin

    Energy Technology Data Exchange (ETDEWEB)

    Ryan, J.P.; Fritz, J.S.

    1978-10-01

    A small water sample (20 to 250 ml) is passed through a small tube containing XAD-4 resin; this effectively retains the organic impurities present in the water. This tube is connected to the permanent apparatus and the sorbed organics are thermally transferred to a small Tenex pre-column while the water vapor is vented. The pre-column is closed off, preheated to 275 to 280/sup 0/C, and then a valve is opened to plug-inject the vaporized sample into a gas chromatograph. The procedure works well for a variety of model organic compounds added to water and can be used for the analysis of actual water samples.

  8. Total microcystins analysis in water using laser diode thermal desorption-atmospheric pressure chemical ionization-tandem mass spectrometry.

    Science.gov (United States)

    Roy-Lachapelle, Audrey; Fayad, Paul B; Sinotte, Marc; Deblois, Christian; Sauvé, Sébastien

    2014-04-11

    A new approach for the analysis of the cyanobacterial microcystins (MCs) in environmental water matrices has been developed. It offers a cost efficient alternative method for the fast quantification of total MCs using mass spectrometry. This approach permits the quantification of total MCs concentrations without requiring any derivatization or the use of a suite of MCs standards. The oxidation product 2-methyl-3-methoxy-4-phenylbutyric acid (MMPB) was formed through a Lemieux oxidation and represented the total concentration of free and bound MCs in water samples. MMPB was analyzed using laser diode thermal desorption-atmospheric pressure chemical ionization coupled to tandem mass spectrometry (LDTD-APCI-MS/MS). LDTD is a robust and reliable sample introduction method with ultra-fast analysis time (0.999). Limits of detection and quantification were 0.2 and 0.9 μg L(-1), respectively. These values are comparable with the WHO (World Health Organization) guideline of 1 μg L(-1) for total microcystin-LR congener in drinking water. Accuracy and interday/intraday variation coefficients were below 15%. Matrix effect was determined with a recovery of 91%, showing no significant signal suppression. This work demonstrates the use of the LDTD-APCI-MS/MS interface for the screening, detection and quantification of total MCs in complex environmental matrices.

  9. An Optimized Adsorbent Sampling Combined to Thermal Desorption GC-MS Method for Trimethylsilanol in Industrial Environments

    Directory of Open Access Journals (Sweden)

    Jae Hwan Lee

    2012-01-01

    Full Text Available Trimethylsilanol (TMSOH can cause damage to surfaces of scanner lenses in the semiconductor industry, and there is a critical need to measure and control airborne TMSOH concentrations. This study develops a thermal desorption (TD-gas chromatography (GC-mass spectrometry (MS method for measuring trace-level TMSOH in occupational indoor air. Laboratory method optimization obtained best performance when using dual-bed tube configuration (100 mg of Tenax TA followed by 100 mg of Carboxen 569, n-decane as a solvent, and a TD temperature of 300°C. The optimized method demonstrated high recovery (87%, satisfactory precision (<15% for spiked amounts exceeding 1 ng, good linearity (R2=0.9999, a wide dynamic mass range (up to 500 ng, low method detection limit (2.8 ng m−3 for a 20-L sample, and negligible losses for 3-4-day storage. The field study showed performance comparable to that in laboratory and yielded first measurements of TMSOH, ranging from 1.02 to 27.30 μg/m3, in the semiconductor industry. We suggested future development of real-time monitoring techniques for TMSOH and other siloxanes for better maintenance and control of scanner lens in semiconductor wafer manufacturing.

  10. Thermal desorption solid-phase microextraction inlet for differential mobility spectrometry.

    Science.gov (United States)

    Rainsberg, Matthew R; de Harrington, Peter B

    2005-06-01

    A splitless thermal desorber unit that interfaces a differential mobility spectrometry (DMS) sensor has been devised. This device was characterized by the detection of benzene, toluene, and xylene (BTX) in water. The detection of BTX in water is important for environmental monitoring, and ion mobility measurements are traditionally difficult for hydrocarbons in water because water competes for charge and quenches the hydrocarbon signals. This paper reports the use of a DMS with a photoionization source that is directly coupled to a solid-phase microextraction (SPME) desorber. The separation and detection capabilities of the DMS were demonstrated using BTX components. Detection limits for benzene, toluene, and m-xylene were 75, 50, and 5 microg mL(-1), respectively.

  11. Modeling of the Kinetics of Supercritical Fluid Extraction of Lipids from Microalgae with Emphasis on Extract Desorption.

    OpenAIRE

    Helena Sovová; Beatriz P. Nobre; António Palavra

    2016-01-01

    Microalgae contain valuable biologically active lipophilic substances such as omega-3 fatty acids and carotenoids. In contrast to the recovery of vegetable oils from seeds, where the extraction with supercritical CO2 is used as a mild and selective method, economically viable application of this method on similarly soluble oils from microalgae requires, in most cases, much higher pressure. This paper presents and verifies hypothesis that this difference is caused by high adsorption capacity o...

  12. Thermal desorption gas chromatography and positron annihilation spectroscopy, contribution to alpha decay studies in actinide-doped matrices

    Energy Technology Data Exchange (ETDEWEB)

    Roudil, D.; Jegou, C.; Vella, F.; Folch, B.; Broudic, V. [Commissariat a l' energie Atomique, Rhone Valley Research Center, 30200 Bagnols-sur-Ceze (France); Pik, R. [CNRS-CRPG, 54506 Vandoeuvre-les-Nancy (France); Barthe, M. F. [CNRS-CEMHTI, 45071 Orleans (France); Cuney, M. [Universite de Nancy, CNRS, CREGU, 54506 Vandoeuvre-les-Nancy (France); Pipon, Y. [IPNL CNRS, IN2P3 UMR 5822, 69622 Villeurbanne (France)

    2009-07-01

    A thermal desorption system coupled with a gas analyzer has been adapted and nuclearized to investigate He behavior in actinide-doped samples used to simulate alpha decay aging. This technique widely used in standard laboratories allows measurements of the helium balance and reduced diffusion coefficients, and a preliminary evaluation of helium locations (related to defects and thermal annealing). In our system implemented in a hot cell, small samples are annealed at up to 1100 C degrees in controlled atmosphere. They are inserted in a 10 to 20 cm{sup 3} vessel connected to a micro gas chromatography detector. Initial system calibration allowed concentration measurements within about 10%. Comparisons with the CNRS/CRPG rare gas analysis laboratory at Nancy (France) were applied on natural uranium oxides originating from Oklo (Gabon) and Mistamisk (Canada). The latest results obtained on Mistamisk samples are in good agreement, with a maximum relative deviation of 14%. The data were used to determine the activation energy of about 1 eV.at{sup -1}. On (U,Pu)O{sub 2} and PuO{sub 2} samples the experiments highlight the impact of defects (up to 100 dpa) on He mobility. The defect population must now be characterized to improve our knowledge of He/defect interactions and mechanisms. In addition and synergy to the macroscopic release measurements by gas chromatography, positron annihilation spectroscopy, an effective nondestructive technique for vacancy defect investigation, was also developed and nuclearized in our hot cell laboratory as part of a project supported by the NOMADE and MATINEX research groups. Specific protocols for doped sample analysis were also developed and validated with UO{sub 2} and (U,Pu)O{sub 2} samples. (authors)

  13. Fate of As(V)-treated nano zero-valent iron: determination of arsenic desorption potential under varying environmental conditions by phosphate extraction.

    Science.gov (United States)

    Dong, Haoran; Guan, Xiaohong; Lo, Irene M C

    2012-09-01

    Nano zero-valent iron (NZVI) offers a promising approach for arsenic remediation, but the spent NZVI with elevated arsenic content could arouse safety concerns. This study investigated the fate of As(V)-treated NZVI (As-NZVI), by examining the desorption potential of As under varying conditions. The desorption kinetics of As from As-NZVI as induced by phosphate was well described by a biphasic rate model. The effects of As(V)/NZVI mass ratio, pH, and aging time on arsenic desorption from As-NZVI by phosphate were investigated. Less arsenic desorption was observed at lower pH or higher As(V)/NZVI mass ratio, where stronger complexes (bidentate) formed between As(V) and NZVI corrosion products as indicated by FTIR analysis. Compared with the fresh As-NZVI, the amount of phosphate-extractable As significantly decreased in As-NZVI aged for 30 or 60 days. The results of the sequential extraction experiments demonstrated that a larger fraction of As was sorbed in the crystalline phases after aging, making it less susceptible to phosphate displacement. However, at pH 9, a slightly higher proportion of phosphate-extractable As was observed in the 60-day sample than in the 30-day sample. XPS results revealed the transformation of As(V) to more easily desorbed As(III) during aging and a higher As(III)/As(V) ratio in the 60-day sample at pH 9, which might have resulted in the higher desorption.

  14. The effect of chars and their water extractable organic carbon (WEOC) fractions on atrazine adsorption-desorption processes

    Science.gov (United States)

    Cavoski, I.; Jablonowski, N.; Burauel, P.; Miano, T.

    2012-04-01

    Chars are carbonaceous material produced from different type of biomass by pyrolysis. They are known as highly effective adsorbents for atrazine therefore limiting its degradation and its diffusion into the aqueous phase. The aim of the present work is to study the effects of different chars and char's derived WEOC on atrazine sorption-desorption processes. The five chars been used in this study derived from: 1) fast pyrolysis from hard wood (FP1); 2) flash pyrolysis from soft wood (FP2); 3) slow pyrolysis from deciduous wood (CC); 4) gasification from deciduous wood (GC) and 5) the market, purchased as activated charcoal standard (AC). Short-term batch equilibration tests were conducted to assess the sorption-desorption behavior of 14C-labeled atrazine on the chars, with a special focus on the desorption behavior using successive dilution method with six consecutive desorption step. Chars and their WEOC were physically and chemically characterized. Results demonstrate that biomass and pyrolysis process used to produce chars affect their physical and chemical properties, and atrazine adsorption-desorption behavior. Atrazine desorption resulted from the positive and competitive interactions between WEOC and chars surfaces. WEOC pool play important role in atrazine adsorption-desorption behavior. FP1 and FP2 with higher concentration of WEOC showed higher desorption rates, whereas GC, CC and AC with insignificant WEOC concentration strongly adsorb atrazine with low desorption rates. According to our results, when high WEOC pools chars are concerned, an increase in atrazine desorption can be observed but further studies would help in confirming the present results.

  15. Comparison of two common adsorption materials for thermal desorption gas chromatography - mass spectrometry of biogenic volatile organic compounds.

    Science.gov (United States)

    Marcillo, Andrea; Jakimovska, Viktorija; Widdig, Anja; Birkemeyer, Claudia

    2017-09-08

    Volatile organic compounds (VOCs) are commonly collected from gaseous samples by adsorption to materials such as the porous polymer Tenax TA. Adsorbed compounds are subsequently released from these materials by thermal desorption (TD) and separated then by gas chromatography (GC) with flame ionization (FID) or mass spectrometry (MS) detection. Tenax TA is known to be particularly suitable for non-polar to semipolar volatiles, however, many volatiles from environmental and biological samples possess a rather polar character. Therefore, we tested if the polymer XAD-2, which so far is widely used to adsorb organic compounds from aqueous and organic solvents, could provide a broader coverage for (semi)polar VOCs during gas-phase sampling. Mixtures of volatile compounds covering a wide range of volatility (bp. 20-256°C) and different chemical classes were introduced by liquid spiking into sorbent tubes with one of the two porous polymers, Tenax TA or XAD-2, and analyzed by TD/GC-MS. At first, an internal standard mixture composed of 17 authentic standards was used to optimize desorption temperature with respect to sorbent degradation and loading time for calibration. Secondly, we tested the detectability of a complex standard mixture composed of 57 volatiles, most of them common constituents of the body odor of mammals. Moreover, the performance of XAD-2 compared with Tenax TA was assessed as limit of quantitation and linearity for the internal standard mixture and 33 compounds from the complex standard mixture. Volatiles were analyzed in a range between 0.01-∼250ng/tube depending on the compound and material. Lower limits of quantitation were between 0.01 and 3 ng±0.9). Interestingly, we found different kinetics for compound adsorption with XAD-2, and a partially better sensitivity in comparison with Tenax TA. For these analytes, XAD-2 might be recommended as an alternative of Tenax TA for TD/GC-MS analysis. Copyright © 2017 Elsevier B.V. All rights reserved.

  16. Survival and growth of Alfalfa (Medicago sativa l.) inoculated with an am fungus (Glomus intraradices) in contaminated soils treated with two different remediation technologies (bio-pile and thermal desorption)

    Energy Technology Data Exchange (ETDEWEB)

    Norini, M.P.; Beguiristain, Th.; Leyval, C. [LIMOS UMR 7137 CNRS-UHP Nancy - Faculty of Sciences, 54 - Vandoeuvre-les-Nancy (France)

    2005-07-01

    (Medicago sativa L.), inoculated or not with an AM fungus (Glomus intraradices) and fertilized with Hewitt solution. Control non-inoculated and non-fertilized plants were included. There was four replicates per treatment. After 2 months, plant survival and growth was measured, as well as mycorrhizal colonization of roots. PAH in rhizosphere soils was analyzed using ASE and GC-FID. Major and trace elements in plants were analyzed after acid digestion using ICP. AM fungal and bacterial communities present in roots and rhizosphere were also analysed after DNA extraction with a PCR-TGGE technique. Plant survival rate was significantly lower in the soil treated with bio-pile than in untreated soil. Non-inoculated and non fertilized alfalfa biomass was lower with soil treated with bio-pile and thermal desorption than with untreated soil. Mycorrhizal inoculation as well as fertilization significantly improved alfalfa growth in the soil treated with bio-pile. In the soil treated with thermal desorption, shoot and root biomass were significantly higher with mycorrhizal inoculation and fertilization. Estimation of root colonization showed that the roots of un-inoculated plants growing on the untreated contaminated soil contained indigenous mycorrhizal fungi. With the soil treated with bio-pile, mycorrhizal colonization of un-inoculated plants was significantly lower, while no colonization was observed in the roots in the soil treated with thermal desorption. Inoculation with a mycorrhizal fungus increased root colonization rate in both treated soils. It also significantly increased the number of rhizobia nodules. Phosphorus concentration in plant roots and shoots was significantly improved by mycorrhizal inoculation in soil treated with thermal desorption. Data on PAH concentration in soils and fungal and bacterial communities will be also presented and discussed.

  17. Thermal desorption characterisation of molecularly imprinted polymers. Part II: Use of direct probe GC-MS analysis to study crosslinking effects.

    Science.gov (United States)

    Holland, Niamh; Duggan, Patrick; Owens, Eleanor; Cummins, Wayne; Frisby, June; Hughes, Helen; McLoughlin, Peter

    2008-06-01

    A powerful method utilising direct probe thermal desorption GC-MS is presented for the study of molecularly imprinted polymers (MIPs). A series of 2-aminopyridine (2-apy)-imprinted methacrylic acid-ethyleneglycol dimethacrylate (MAA-EGDMA) copolymers were prepared under identical conditions but with varying amounts of EGDMA (crosslinking monomer). The use of appropriate temperature programmes permitted template removal, and the subsequent assessment of polymer affinity and specificity, all of which were found to be dependent on polymer composition and morphology. The system was sufficiently sensitive to identify a specific response of imprinted polymers over nonimprinted counterparts. Correlations were found to exist between thermal desorption analysis and solution phase binding, which was assessed by UV spectroscopy, where specificity was found to diminish with decreasing EGDMA concentration. This was attributed to the increased number of free carboxyl groups in those polymers containing a lower percentage of EGDMA. Thermal desorption profiles obtained for the analyte were found to be unaffected by the physical and chemical properties of the solvent used for analyte reloading.

  18. Ultra high vacuum high precision low background setup with temperature control for thermal desorption mass spectroscopy (TDA-MS) of hydrogen in metals.

    Science.gov (United States)

    Merzlikin, Sergiy V; Borodin, S; Vogel, D; Rohwerder, M

    2015-05-01

    In this work, a newly developed UHV-based high precision low background setup for hydrogen thermal desorption analysis (TDA) of metallic samples is presented. Using an infrared heating with a low thermal capacity enables a precise control of the temperature and rapid cool down of the measurement chamber. This novel TDA-set up is superior in sensitivity to almost every standard hydrogen analyzer available commercially due to the special design of the measurement chamber, resulting in a very low hydrogen background. No effects of background drift characteristic as for carrier gas based TDA instruments were observed, ensuring linearity and reproducibility of the analysis. This setup will prove to be valuable for detailed investigations of hydrogen trapping sites in steels and other alloys. With a determined limit of detection of 5.9×10(-3)µg g(-1) hydrogen the developed instrument is able to determine extremely low hydrogen amounts even at very low hydrogen desorption rates. This work clearly demonstrates the great potential of ultra-high vacuum thermal desorption mass spectroscopy instrumentation.

  19. Combined Atomic Force Microscope-Based Topographical Imaging and Nanometer Scale Resolved Proximal Probe Thermal Desorption/Electrospray Ionization-Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Ovchinnikova, Olga S [ORNL; Nikiforov, Maxim [ORNL; Bradshaw, James A [ORNL; Jesse, Stephen [ORNL; Van Berkel, Gary J [ORNL

    2011-01-01

    Nanometer scale proximal probe thermal desorption/electrospray ionization mass spectrometry (TD/ESI-MS) was demonstrated for molecular surface sampling of caffeine from a thin film using a 30 nm diameter nano-thermal analysis (nano-TA) probe tip in an atomic force microscope (AFM) coupled via a vapor transfer line and ESI interface to a MS detection platform. Using a probe temperature of 350 C and a spot sampling time of 30 s, conical desorption craters 250 nm in diameter and 100 nm deep were created as shown through subsequent topographical imaging of the surface within the same system. Automated sampling of a 5 x 2 array of spots, with 2 m spacing between spots, and real time selective detection of the desorbed caffeine using tandem mass spectrometry was also demonstrated. Estimated from the crater volume (~2x106 nm3), only about 10 amol (2 fg) of caffeine was liberated from each thermal desorption crater in the thin film. These results illustrate a relatively simple experimental setup and means to acquire in automated fashion sub-micrometer scale spatial sampling resolution and mass spectral detection of materials amenable to TD. The ability to achieve MS-based chemical imaging with 250 nm scale spatial resolution with this system is anticipated.

  20. Thermal stability of liquid antioxidative extracts from pomegranate peel

    Science.gov (United States)

    This research was carried out to assess the potential of using the natural antioxidants in pomegranate peel extracts as replacement for synthetic antioxidants. As a result the thermal stability of pomegranate peel extract products during sterilization and storage, and its effect on industrial, color...

  1. Diffusive uptake in passive and active adsorbent sampling using thermal desorption tubes.

    Science.gov (United States)

    Batterman, Stuart; Metts, Tricia; Kalliokoski, Pentti

    2002-12-01

    Low flow active sampling techniques collecting vapors and gases using thermally desorbable adsorbents are now feasible and desirable in many applications as they permit long integration times, the potential for miniaturized sampling configurations, and other advantages. At very low air flow rates (estimates of the tortuosity and porosity of the glass wool packing used to retain the adsorbent, parameters needed to estimate diffusive fluxes in passive and active sampling; (4) a demonstration that orifice-equipped low flow active samplers can reduce diffusive uptake and improve precision, and (5) a model predicting the saturated adsorbent layer that helps to account for the gradual decline in uptake rates seen in passive sampling. Diffusive uptake will depend on the tube configuration and diffusion coefficient of the substance of interest, but for conventional sampling tubes (0.4-0.5 cm id, 1.5 cm air gap), sample flow rates should be maintained above 1 to 4 ml min(-1) to keep errors below 5%. Laboratory experiments showed close agreement with theoretical calculations, and the field study using 1 to 4 d sampling periods and 0.3 ml min(-1) flows demonstrated that the orifice-equipped samplers essentially eliminated diffusive uptake. No significant practical difficulties are encountered using orifices, e.g., pressure drop is minimal. Experimental estimates of tortuosity (0.79 +/- 0.02) and porosity (0.92 +/- 0.10) of the glass wool packing (0.3 cm length) represent relatively little resistance to diffusion; however, variation in the packing and adsorbent placement can degrade the precision achievable by passive samplers. Diffusion barriers, consisting most simply of an orifice, may be used to lower the diffusive uptake. A needle-type orifice permits flows below 0.1 ml min(-1) and is suitable for sampling periods as long as several weeks, and it provided greater precision than conventional open-ended sampling tubes (8% compared to 13%). Finally, the gradual decrease in

  2. Adsorption, desorption, and film formation of quinacridone and its thermal cracking product indigo on clean and carbon-covered silicon dioxide surfaces

    Science.gov (United States)

    Scherwitzl, Boris; Lassnig, Roman; Truger, Magdalena; Resel, Roland; Leising, Günther; Winkler, Adolf

    2016-09-01

    The evaporation of quinacridone from a stainless steel Knudsen cell leads to the partial decomposition of this molecule in the cell, due to its comparably high sublimation temperature. At least one additional type of molecules, namely indigo, could be detected in the effusion flux. Thermal desorption spectroscopy and atomic force microscopy have been used to study the co-deposition of these molecules on sputter-cleaned and carbon-covered silicon dioxide surfaces. Desorption of indigo appears at temperatures of about 400 K, while quinacridone desorbs at around 510 K. For quinacridone, a desorption energy of 2.1 eV and a frequency factor for desorption of 1 × 1019 s-1 were calculated, which in this magnitude is typical for large organic molecules. A fraction of the adsorbed quinacridone molecules (˜5%) decomposes during heating, nearly independent of the adsorbed amount, resulting in a surface composed of small carbon islands. The sticking coefficients of indigo and quinacridone were found to be close to unity on a carbon covered SiO2 surface but significantly smaller on a sputter-cleaned substrate. The reason for the latter can be attributed to insufficient energy dissipation for unfavorably oriented impinging molecules. However, due to adsorption via a hot-precursor state, the sticking probability is increased on the surface covered with carbon islands, which act as accommodation centers.

  3. Atomic Force Microscopy Thermally-Assisted Microsampling with Atmospheric Pressure Temperature Ramped Thermal Desorption/Ionization-Mass Spectrometry Analysis.

    Science.gov (United States)

    Hoffmann, William D; Kertesz, Vilmos; Srijanto, Bernadeta R; Van Berkel, Gary J

    2017-02-20

    The use of atomic force microscopy controlled nanothermal analysis probes for reproducible spatially resolved thermally assisted sampling of micrometer-sized areas (ca. 11 × 17 μm wide × 2.4 μm deep) from relatively low number-average molecular weight (Mn mass spectrometric analysis. The procedure and mechanism for material pickup, the sampling reproducibility and sampling size are discussed, and the oligomer distribution information available from slow temperature ramps versus ballistic temperature jumps is presented. For the Mn = 970 P2VP, the Mn and polydispersity index determined from the mass spectrometric data were in line with both the label values from the sample supplier and the value calculated from the simple infusion of a solution of polymer into the commercial atmospheric pressure chemical ionization source on this mass spectrometer. With a P2VP sample of higher Mn (Mn = 2070 and 2970), intact oligomers were still observed (as high as m/z 2793 corresponding to the 26-mer), but a significant abundance of thermolysis products were also observed. In addition, the capability for confident identification of the individual oligomers by slowly ramping the probe temperature and collecting data-dependent tandem mass spectra was also demonstrated. The material type limits to the current sampling and analysis approach as well as possible improvements in nanothermal analysis probe design to enable smaller area sampling and to enable controlled temperature ramps beyond the present upper limit of about 415 °C are also discussed.

  4. Evaluation of two adsorbents for diffusive sampling and thermal desorption-gas chromatographic analysis of monoterpenes in air.

    Science.gov (United States)

    Sunesson, A L; Sundgren, M; Levin, J O; Eriksson, K; Carlson, R

    1999-02-01

    Tube type samplers with two different adsorbents, Chromosorb 106 and Tenax TA, were evaluated by laboratory experiments and field tests for simultaneous diffusive sampling of alpha-pinene, beta-pinene and delta 3-carene and subsequent thermal desorption-gas chromatographic analysis. No statistically significant effects of exposure time, concentrations of monoterpenes or relative humidity were found for samplers with Chromosorb 106 when running a factorial design, with the exception of the adsorption of delta 3-carene, for which some weak effects were noted. Samplers with Tenax TA were affected by the sampling time as well as the concentration for all terpenes, with a strong interaction effect between these two factors. The terpenes showed good storage stability on both adsorbents. No effect of back-diffusion was noted when using Chromosorb 106, while Tenax TA showed some back-diffusion effects. The uptake rates, in ml min-1, for the terpenes on Chromosorb 106 were 0.36 for alpha-pinene, 0.36 for beta-pinene and 0.40 for delta 3-carene. The corresponding average values on Tenax TA were 0.30 for alpha-pinene, 0.32 for beta-pinene and 0.38 for delta 3-carene. The field validation proved that diffusive sampling on Chromosorb 106 agreed well with pumped sampling on charcoal for stationary samples, while the personal samples indicated a discrepancy of 25% between Chromosorb 106 and charcoal samples. Tenax TA generally gave lower results than Chromosorb 106 in all field samples. Samplers packed with Chromosorb 106 could be used to monitor terpene levels in workplaces such as sawmills. The major advantages with this method are the sampling procedure, which is simple to perform compared to other techniques, the easily automated analysis procedure and the possibility to reuse the samplers.

  5. Characterization of thermal desorption with the Deans-switch technique in gas chromatographic analysis of volatile organic compounds.

    Science.gov (United States)

    Ou-Yang, Chang-Feng; Huang, Ying-Xue; Huang, Ting-Jyun; Chen, Yong-Shen; Wang, Chieh-Heng; Wang, Jia-Lin

    2016-09-02

    This study presents a novel application based on the Deans-switch cutting technique to characterize the thermal-desorption (TD) properties for gas chromatographic (GC) analysis of ambient volatile organic compounds (VOCs). Flash-heating of the sorbent bed at high temperatures to desorb trapped VOCs to GC may easily produce severe asymmetric or tailing GC peaks affecting resolution and sensitivity if care is not taken to optimize the TD conditions. The TD peak without GC separation was first examined for the quality of the TD peak by analyzing a standard gas mixture from C2 to C12 at ppb level. The Deans switch was later applied in two different stages. First, it was used to cut the trailing tail of the TD peak, which, although significantly improved the GC peak symmetry, led to more loss of the higher boiling compounds than the low boiling ones, thus suggesting compound discrimination. Subsequently, the Deans switch was used to dissect the TD peak into six 30s slices in series, and an uneven distribution in composition between the slices were found. A progressive decrease in low boiling compounds and increase in higher boiling ones across the slices indicated severe inhomogeneity in the TD profile. This finding provided a clear evidence to answer the discrimination problem found with the tail cutting approach to improve peak symmetry. Through the use of the innovated slicing method based on the Deans-switch cutting technique, optimization of TD injection for highly resolved, symmetric and non-discriminated GC peaks can now be more quantitatively assessed and guided.

  6. Hydrogen sulphide in human nasal air quantified using thermal desorption and selected ion flow tube mass spectrometry.

    Science.gov (United States)

    Wondimu, Taddese; Wang, Rui; Ross, Brian

    2014-09-01

    The discovery that hydrogen sulphide (H2S) acts as a gasotransmitter when present at very low concentrations (sub-parts per billion (ppbv)) has resulted in the need to quickly quantify trace amounts of the gas in complex biological samples. Selected ion flow tube mass spectrometry (SIFT-MS) is capable of real-time quantification of H2S but many SIFT-MS instruments lack sufficient sensitivity for this application. In this study we investigate the utility of combining thermal desorption with SIFT-MS for quantifying H2S in the 0.1-1 ppbv concentration range. Human orally or nasally derived breath, and background ambient air, were collected in sampling bags and dried by passing through CaCl2 and H2S pre-concentrated using a sorbent trap optimised for the capture of this gas. The absorbed H2S was then thermally desorbed and quantified by SIFT-MS. H2S concentrations in ambient air, nasal breath and oral breath collected from 10 healthy volunteers were 0.12  ±  0.02 (mean ± SD), 0.40  ±  0.11 and 3.1  ±  2.5 ppbv respectively, and in the oral cavity H2S, quantified by SIFT-MS without pre-concentration, was present at 13.5  ±  8.6 ppbv. The oral cavity H2S correlates well with oral breath H2S but not with nasal breath H2S, suggesting that oral breath H2S derives mainly from the oral cavity but nasal breath is likely pulmonary in origin. The successful quantification of such low concentrations of H2S in nasal air using a rapid analytical procedure paves the way for the straightforward analysis of H2S in breath and may assist in elucidating the role that H2S plays in biological systems.

  7. Measurement of toxic volatile organic compounds in indoor air of semiconductor foundries using multisorbent adsorption/thermal desorption coupled with gas chromatography-mass spectrometry.

    Science.gov (United States)

    Wu, Chien-Hou; Lin, Ming-Nan; Feng, Chien-Tai; Yang, Kuang-Ling; Lo, Yu-Shiu; Lo, Jiunn-Guang

    2003-05-09

    A method for the qualitative and quantitative analysis of volatile organic compounds (VOCs) in the air of class-100 clean rooms at semiconductor fabrication facilities was developed. Air samples from two semiconductor factories were collected each hour on multisorbent tubes (including Carbopack B, Carbopack C, and Carbosieve SIII) with a 24-h automatic active sampling system and analyzed using adsorption/thermal desorption coupled with gas chromatography-mass spectrometry. Experimental parameters, including thermal desorption temperature, desorption time, and cryofocusing temperature, were optimized. The average recoveries and the method detection limits for the target compounds were in the range 94-101% and 0.31-0.89 ppb, respectively, under the conditions of a 1 L sampling volume and 80% relative humidity. VOCs such as acetone, isopropyl alcohol, 2-heptanone, and toluene, which are commonly used in the semiconductor and electronics industries, were detected and accurately quantified with the established method. Temporal variations of the analyte concentrations observed were attributed to the improper use of organic solvents during operation.

  8. Thermal transformation of bioactive caffeic acid on fumed silica seen by UV-Vis spectroscopy, thermogravimetric analysis, temperature programmed desorption mass spectrometry and quantum chemical methods.

    Science.gov (United States)

    Kulik, Tetiana V; Lipkovska, Natalia O; Barvinchenko, Valentyna M; Palyanytsya, Borys B; Kazakova, Olga A; Dudik, Olesia O; Menyhárd, Alfréd; László, Krisztina

    2016-05-15

    Thermochemical studies of hydroxycinnamic acid derivatives and their surface complexes are important for the pharmaceutical industry, medicine and for the development of technologies of heterogeneous biomass pyrolysis. In this study, structural and thermal transformations of caffeic acid complexes on silica surfaces were studied by UV-Vis spectroscopy, thermogravimetric analysis, temperature programmed desorption mass spectrometry (TPD MS) and quantum chemical methods. Two types of caffeic acid surface complexes are found to form through phenolic or carboxyl groups. The kinetic parameters of the chemical reactions of caffeic acid on silica surface are calculated. The mechanisms of thermal transformations of the caffeic chemisorbed surface complexes are proposed. Thermal decomposition of caffeic acid complex chemisorbed through grafted ester group proceeds via three parallel reactions, producing ketene, vinyl and acetylene derivatives of 1,2-dihydroxybenzene. Immobilization of phenolic acids on the silica surface improves greatly their thermal stability.

  9. Solar thermal extraction of copper from sulfides

    Energy Technology Data Exchange (ETDEWEB)

    Winkel, L.; Guesdon, C.; Sturzenegger, M.

    2003-03-01

    With the aim to develop a solar-driven process for the extraction of copper from sulfide concentrates re-search on the decomposition of copper sulfides under inert atmospheres has been initiated. Thermogravimetric measurements on chalcocite (Cu{sub 2}S) revealed that copper is formed already at 1823 K. Chalcopyrite (CuFeS{sub 2}) also disintegrates at this temperature, although at a lower rate. Copper and iron have been identified in the solid residue. The results confirm the feasibility of copper extraction by direct decomposition of sulfides under atmospheric pressure. The decomposition under inert atmosphere prevents generation of SO{sub 2}, and is beneficial to the removal of volatile impurities. Chemical equilibrium calculations for CuFeS{sub 2} contaminated with enargite (Cu{sub 3}AsS{sub 4}) have shown that the absence of an oxidic slag allows for a complete evaporation of arsenic and subsequent separation. (author)

  10. Threshold character of temperatures on deuterium thermal desorption in Mg-V composite grown atom-by-atom

    Science.gov (United States)

    Neklyudov, I. M.; Morozov, O. M.; Kulish, V. G.; Zhurba, V. I.; Galitskiy, A. G.; Lomino, N. S.; Kuprin, A. S.; Ovcharenko, V. D.; Reshetnyak, E. N.

    2012-08-01

    The plasma evaporation-sputtering method was applied to make composite materials of the Mg-V system. The ion-implanted deuterium desorption temperature variations as a function of the component concentration were studied. It has been established that, by introducing vanadium into magnesium, the deuterium desorption temperature can be appreciably decreased (to 300-330 K) in comparison with the case of deuterium desorption from magnesium (~800 K). A step-like form of the curve of deuterium desorption temperature evidences on the presence of two different structure states of the Mg-V system depending on the ratio of components. The deuterium temperature decrease can be caused by filamentary inclusions formed, in the process of composite making and annealing, by the insoluble component (vanadium) atoms providing the deuterium diffusion from the sample at a lower temperature (channels for deuterium diffusion through the surface barrier). A necessary high diffusion mobility of deuterium is provided by the amorphous state of Mg83+xVx samples. The deuterium desorption data obtained on the example of Mg-V and Mg-Zr composites provide support for further research into hydrogen storage materials containing low-soluble chemical elements in the alloy components.

  11. Thermal desorption GC-MS as a tool to provide PAH certified standard reference material on particulate matter quartz filters.

    Science.gov (United States)

    Grandesso, Emanuela; Pérez Ballesta, Pascual; Kowalewski, Konrad

    2013-02-15

    Reference materials for particulate matter (PM) on filter media are not available for the quantification of polycyclic aromatic hydrocarbons (PAHs) in ambient air. This is due to the difficulty of obtaining reference material that has a homogeneous distribution on a filter surface that is large enough for characterization and distribution. High volume sample filters from different locations and seasons were considered to validate the feasibility of the use of quartz filters as reference material for PAH concentrations. A rapid thermal desorption (TD) technique coupled with gas chromatography/mass spectroscopy was applied to characterise the material for the content of fifteen different PAHs. TD technique allowed for rapid and accurate analysis of small sections of filter (5mm diameter), leaving enough material for the production of twenty sub-filter cuts (42 mm diameter) that could be used for distribution and control. Stability and homogeneity tests required for material certification were performed as indicated by the ISO guide 34:2009 and ISO 35:2006. The contribution of the heterogeneous distribution of PAHs on the filter surface resulted generally lower than 10% and higher for more volatile PAHs. One year of storage at -18°C indicated no significant variation in PAH concentrations. Nevertheless, a methodology for shipping and storing of the filter material at ambient temperature in especially designed plastic envelopes, was also shown to allow for stabile concentrations within twenty days. The method accuracy was confirmed by the analysis of NIST SRM 1649a (urban dust) and PAH concentrations were validated against the reference values obtained from an inter-laboratory exercise. In the case of benzo[a]pyrene for masses quantified between 100 pg and 10 ng the TD method provided expanded uncertainties of circa 10%, while the inter-laboratory reference value uncertainties ranged between 15 and 20%. The evaluation of these results supports the use of the presented

  12. Low-flow active and passive sampling of VOCs using thermal desorption tubes: theory and application at an offset printing facility.

    Science.gov (United States)

    Batterman, Stuart; Metts, Tricia; Kalliokoski, Pentti; Barnett, Emily

    2002-06-01

    While air sampling techniques using adsorbent-based collection, thermal desorption and chromatographic analysis have found a niche in ambient air sampling, occupational applications have been more limited. This paper evaluates the use of thermal desorption techniques for low flow active and passive sampling configurations which allow conveniently long duration sampling in occupational settings and other high concentration environments. The use of an orifice enables flows as low as 0.5 ml min(-1) and sampling periods up to several days without significant biases. A model is used to predict sampling rates of a passive sampler encompassing an orifice, a void space, glass wool, and the adsorbent. Laboratory and field tests conducted at a commercial offset printing facility, which contained a variety of volatile organic compounds (primarily aromatic but also a few chlorinated and terpene compounds at levels from 1 to 67,000 microg m(-3)), are used to evaluate the approach. Tenax GR and Carbosieve SIII, both singly and together, were employed as adsorbents. Side-by-side tests comparing high flow, low flow and passive samplers show excellent agreement and high linearity (r = 0.95) for concentrations spanning nearly five orders of magnitude. Active samplers were tested at flows as low as 0.5 ml min(-1), compared to typical flows up to 40 ml min(-1). Passive samplers demonstrated a linear range and agreement with predictions for adsorbate loadings from approximately 1 ng to nearly 10 microg. Using a chemical mass balance receptor model, concentrations in the facility were apportioned to solvents, inks and other indoor and outdoor sources. Overall, the use of low flow active and passive sampling approaches employing thermal desorption techniques provides good performance and tremendous flexibility that facilitates use in many applications, including workplace settings.

  13. THE IMPORTANCE OF ORGANIC MATTER DISTRIBUTION AND EXTRACT SOIL:SOLUTION RATIO ON THE DESORPTION OF HEAVY METALS FROM SOILS

    Science.gov (United States)

    The lability (mobility and bioavailability) of metals varies significantly with soil properties for similar total soil metal concentrations. We studied desorption of Cu, Ni and Zn, from 15 diverse, unamended soils. These studies included evaluation of the effects of soil:solution...

  14. SEMICONDUCTOR DEVICES: Deep submicron PDSOI thermal resistance extraction

    Science.gov (United States)

    Jianhui, Bu; Jinshun, Bi; Linmao, Xi; Zhengsheng, Han

    2010-09-01

    Deep submicron partially depleted silicon on insulator (PDSOI) MOSFETs with H-gate were fabricated based on the 0.35 μm SOI process developed by the Institute of Microelectronics of the Chinese Academy of Sciences. Because the self-heating effect (SHE) has a great influence on SOI, extractions of thermal resistance were done for accurate circuit simulation by using the body-source diode as a thermometer. The results show that the thermal resistance in an SOI NMOSFET is lower than that in an SOI PMOSFET; and the thermal resistance in an SOI NMOSFET with a long channel is lower than that with a short channel. This offers a great help to SHE modeling and parameter extraction.

  15. Thermal extraction analysis of five Los Azufres production wells

    Energy Technology Data Exchange (ETDEWEB)

    Kruger, Paul; Quijano, Luis

    1995-01-26

    Thermal energy extraction from five wells supplying 5-MWe wellhead generators in three zones of the Los Azufres geothermal field has been examined from production and chemical data compiled over 14-years of operation. The data, as annual means, are useful in observing small-scale changes in reservoir performance with continuous production. The chemical components are chloride for quality control and the geothermometer elements for reservoir temperatures. The flowrate and fluid enthalpy data are used to calculate the thermal extraction rates. Integration of these data provides an estimate of the total energy extracted from the zone surrounding the well. The combined production and chemical geothermometer data are used to model the produced fluid as coming from just-penetrating wells for which the annual produced mass originates from a series of concentric hemispheric shells moving out into the reservoir. Estimates are made of the drawdown distance into the reservoir and the far-field conditions.

  16. Micro-solid-phase extraction coupled to desorption electrospray ionization-high-resolution mass spectrometry for the analysis of explosives in soil.

    Science.gov (United States)

    Bianchi, Federica; Gregori, Adolfo; Braun, Gabriele; Crescenzi, Carlo; Careri, Maria

    2015-01-01

    Home-made micro-solid-phase extraction (SPE) cartridges using different adsorbent materials were tested for the desorption electrospray ionization-high-resolution mass spectrometry (DESI-HRMS) determination of explosives like 2,4,6-trinitrotoluene, cyclotrimethylene-trinitramine, cyclotetramethylene-tetranitramine, pentaerythritol tetranitrate, and trinitrophenylmethylnitramine in soil samples. Quantitation limits in the low nanogram per kilogram range proved the reliability of the method for the detection of explosives at ultra-trace levels. The reduced sample preparation allowed for low costs and high-throughput analyses. Finally, the superior extraction capability of the method was proved by obtaining DESI-HRMS responses at least five times higher than those achieved by performing DESI-HRMS analyses of solid-liquid extracts spotted onto commercial polytetrafluoroethylene slides.

  17. On-line derivatization for hourly measurements of gas- and particle-phase Semi-Volatile oxygenated organic compounds by Thermal desorption Aerosol Gas chromatography (SV-TAG

    Directory of Open Access Journals (Sweden)

    G. Isaacman

    2014-07-01

    Full Text Available Laboratory oxidation studies have identified a large number of oxygenated organic compounds that can be used as tracers to understand sources and oxidation chemistry of atmospheric particulate matter. Quantification of these compounds in ambient environments has traditionally relied on low time-resolution collection of filter samples followed by offline sample treatment with a derivatizing agent to allow analysis by gas chromatography of otherwise non-elutable organic chemicals with hydroxyl groups. We present here an automated in situ instrument for the measurement of highly polar organic semi-volatile and low-volatility compounds in both the gas- and particle-phase with hourly time-resolution. The dual-cell Semi-Volatile Thermal desorption Aerosol Gas chromatograph (SV-TAG with derivatization collects particle-only and combined particle-plus-vapor samples on two parallel sampling cells that are analyzed in series by thermal desorption into helium saturated with derivatizing agent. Introduction of MSTFA, a silylating agent, yields complete derivatization of all tested compounds, including alkanoic acids, polyols, diacids, sugars, and multifunctional compounds. In laboratory tests, derivatization is found to be highly reproducible (< 3% variability. During field deployment, a regularly injected internal standard is used to correct for variability in detector response, derivatization efficiency, desorption efficiency, and transfer efficiency. Error in quantification from instrument fluctuations is found to be less than 10% for hydrocarbons and less than 15% for all oxygenates for which a functionally similar internal standard is available. After internal standard corrections, calibration curves are found to be linear for all compounds over the span of one month with comparable response on both of the parallel sampling cells.

  18. Online derivatization for hourly measurements of gas- and particle-phase semi-volatile oxygenated organic compounds by thermal desorption aerosol gas chromatography (SV-TAG)

    Science.gov (United States)

    Isaacman, G.; Kreisberg, N. M.; Yee, L. D.; Worton, D. R.; Chan, A. W. H.; Moss, J. A.; Hering, S. V.; Goldstein, A. H.

    2014-12-01

    Laboratory oxidation studies have identified a large number of oxygenated organic compounds that can be used as tracers to understand sources and oxidation chemistry of atmospheric particulate matter. Quantification of these compounds in ambient environments has traditionally relied on low-time-resolution collection of filter samples followed by offline sample treatment with a derivatizing agent to allow analysis by gas chromatography of otherwise non-elutable organic chemicals with hydroxyl groups. We present here an automated in situ instrument for the measurement of highly polar organic semi-volatile and low-volatility compounds in both the gas- and particle-phase with hourly quantification of mass concentrations and gas-particle partitioning. The dual-cell semi-volatile thermal desorption aerosol gas chromatograph (SV-TAG) with derivatization collects particle-only and combined particle-plus-vapor samples on two parallel sampling cells that are analyzed in series by thermal desorption into helium saturated with derivatizing agent. Introduction of MSTFA (N-methyl-N-(trimethylsilyl)trifluoroacetamide), a silylating agent, yields complete derivatization of all tested compounds, including alkanoic acids, polyols, diacids, sugars, and multifunctional compounds. In laboratory tests, derivatization is found to be highly reproducible (regularly injected internal standard is used to correct for variability in detector response, consumption of the derivatization agent, desorption efficiency, and transfer losses. Error in quantification from instrument fluctuations is found to be less than 10% for hydrocarbons and less than 15% for all oxygenates for which a functionally similar internal standard is available, with an uncertainty of 20-25% in measurements of particle fraction. After internal standard corrections, calibration curves are found to be linear for all compounds over the span of 1 month, with comparable response on both of the parallel sampling cells.

  19. On-line derivatization for hourly measurements of gas- and particle-phase Semi-Volatile oxygenated organic compounds by Thermal desorption Aerosol Gas chromatography (SV-TAG)

    Science.gov (United States)

    Isaacman, G.; Kreisberg, N. M.; Yee, L. D.; Worton, D. R.; Chan, A. W. H.; Moss, J. A.; Hering, S. V.; Goldstein, A. H.

    2014-07-01

    Laboratory oxidation studies have identified a large number of oxygenated organic compounds that can be used as tracers to understand sources and oxidation chemistry of atmospheric particulate matter. Quantification of these compounds in ambient environments has traditionally relied on low time-resolution collection of filter samples followed by offline sample treatment with a derivatizing agent to allow analysis by gas chromatography of otherwise non-elutable organic chemicals with hydroxyl groups. We present here an automated in situ instrument for the measurement of highly polar organic semi-volatile and low-volatility compounds in both the gas- and particle-phase with hourly time-resolution. The dual-cell Semi-Volatile Thermal desorption Aerosol Gas chromatograph (SV-TAG) with derivatization collects particle-only and combined particle-plus-vapor samples on two parallel sampling cells that are analyzed in series by thermal desorption into helium saturated with derivatizing agent. Introduction of MSTFA, a silylating agent, yields complete derivatization of all tested compounds, including alkanoic acids, polyols, diacids, sugars, and multifunctional compounds. In laboratory tests, derivatization is found to be highly reproducible (regularly injected internal standard is used to correct for variability in detector response, derivatization efficiency, desorption efficiency, and transfer efficiency. Error in quantification from instrument fluctuations is found to be less than 10% for hydrocarbons and less than 15% for all oxygenates for which a functionally similar internal standard is available. After internal standard corrections, calibration curves are found to be linear for all compounds over the span of one month with comparable response on both of the parallel sampling cells.

  20. Evaluation of a simple protein extraction method for species identification of clinically relevant staphylococci by matrix-assisted laser desorption ionization-time of flight mass spectrometry.

    Science.gov (United States)

    Matsuda, Naoto; Matsuda, Mari; Notake, Shigeyuki; Yokokawa, Hirohide; Kawamura, Yoshiaki; Hiramatsu, Keiichi; Kikuchi, Ken

    2012-12-01

    In clinical microbiology, bacterial identification is labor-intensive and time-consuming. A solution for this problem is the use of matrix-assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF MS). In this study, we evaluated a modified protein extraction method of identification performed on target plates (on-plate extraction method) with MALDI-TOF (Bruker Microflex LT with Biotyper version 3.0) and compared it to 2 previously described methods: the direct colony method and a standard protein extraction method (standard extraction method). We evaluated the species of 273 clinical strains and 14 reference strains of staphylococci. All isolates were characterized using the superoxide dismutase A sequence as a reference. For the species identification, the on-plate, standard extraction, and direct colony methods identified 257 isolates (89.5%), 232 isolates (80.8%), and 173 isolates (60.2%), respectively, with statistically significant differences among the three methods (P extraction method is at least as good as standard extraction in identification rate and has the advantage of a shorter processing time.

  1. Effect of Ultrasound on Desorption Equilibrium

    Institute of Scientific and Technical Information of China (English)

    秦炜; 原永辉; 戴猷元

    2001-01-01

    Effects of ultrasound on intensification of separation process were investigated through the experiment of desorption equilibrium behavior. Tri-butyl phosphate (TBP) on NKA-X resin and phenol on a solvent impregnated resin, CL-TBP resin, were used for desorption processes. The desorption rate was measured with and without ultrasound. Desorption equilibrium was studied under various ultrasonic power densities or thermal infusion. Results showed that the desorption rate with ultrasound was much higher than that with normal thermal infusion. Both ultrasound and thermal infusion broke the desorption equilibrium existed at room temperature. However, after the systems were cooled down, the amount of solute desorbed in the liquid phase in the presence of ultrasound was much higher than that at the temperature corresponding to the same ultrasound power. It is proved that the initial desorption equilibrium was broken as a result of the spot energy effect of ultrasound.

  2. Highly hydrogen-sensitive thermal desorption spectroscopy system for quantitative analysis of low hydrogen concentration (∼1 × 10(16) atoms/cm(3)) in thin-film samples.

    Science.gov (United States)

    Hanna, Taku; Hiramatsu, Hidenori; Sakaguchi, Isao; Hosono, Hideo

    2017-05-01

    We developed a highly hydrogen-sensitive thermal desorption spectroscopy (HHS-TDS) system to detect and quantitatively analyze low hydrogen concentrations in thin films. The system was connected to an in situ sample-transfer chamber system, manipulators, and an rf magnetron sputtering thin-film deposition chamber under an ultra-high-vacuum (UHV) atmosphere of ∼10(-8) Pa. The following key requirements were proposed in developing the HHS-TDS: (i) a low hydrogen residual partial pressure, (ii) a low hydrogen exhaust velocity, and (iii) minimization of hydrogen thermal desorption except from the bulk region of the thin films. To satisfy these requirements, appropriate materials and components were selected, and the system was constructed to extract the maximum performance from each component. Consequently, ∼2000 times higher sensitivity to hydrogen than that of a commercially available UHV-TDS system was achieved using H(+)-implanted Si samples. Quantitative analysis of an amorphous oxide semiconductor InGaZnO4 thin film (1 cm × 1 cm × 1 μm thickness, hydrogen concentration of 4.5 × 10(17) atoms/cm(3)) was demonstrated using the HHS-TDS system. This concentration level cannot be detected using UHV-TDS or secondary ion mass spectroscopy (SIMS) systems. The hydrogen detection limit of the HHS-TDS system was estimated to be ∼1 × 10(16) atoms/cm(3), which implies ∼2 orders of magnitude higher sensitivity than that of SIMS and resonance nuclear reaction systems (∼10(18) atoms/cm(3)).

  3. Detection of gaseous compounds by needle trap sampling and direct thermal-desorption photoionization mass spectrometry: concept and demonstrative application to breath gas analysis.

    Science.gov (United States)

    Kleeblatt, Juliane; Schubert, Jochen K; Zimmermann, Ralf

    2015-02-01

    A fast detection method to analyze gaseous organic compounds in complex gas mixtures was developed, using a needle trap device (NTD) in conjunction with thermal-desorption photoionization time-of-flight mass spectrometry (TD-PI-TOFMS). The mass spectrometer was coupled via a deactivated fused silica capillary to an injector of a gas chromatograph. In the hot injector, the analytes collected on the NTD were thermally desorbed and directly transferred to the PI-TOFMS ion source. The molecules are softly ionized either by single photon ionization (SPI, 118 nm) or by resonance enhanced multiphoton ionization (REMPI, 266 nm), and the molecular ion signals are detected in the TOF mass analyzer. Analyte desorption and the subsequent PI-TOFMS detection step only lasts ten seconds. The specific selectivity of REMPI (i.e., aromatic compounds) and universal ionization characteristics render PI-MS as a promising detection system. As a first demonstrative application, the alveolar phase breath gas of healthy, nonsmoking subjects was sampled on NTDs. While smaller organic compounds such as acetone, acetaldehyde, isoprene, or cysteamine can be detected in the breath gas with SPI, REMPI depicts the aromatic substances phenol and indole at 266 nm. In the breath gas of a healthy, smoking male subject, several xenobiotic substances such as benzene, toluene, styrene, and ethylbenzene can be found as well. Furthermore, the NTD-REMPI-TOFMS setup was tested for breath gas taken from a mechanically ventilated pig under continuous intravenous propofol (2,6-diisopropylphenol, narcotic drug) infusion.

  4. Application of GC-MS with a SPME and thermal desorption technique for determination of dimethylamine and trimethylamine in gaseous samples for medical diagnostic purposes.

    Science.gov (United States)

    Wzorek, Beata; Mochalski, Paweł; Sliwka, Ireneusz; Amann, Anton

    2010-06-01

    Biogenic amines are interesting compounds which may be of use for medical diagnosis or therapeutic monitoring. The present paper deals with the problems that occur with concentration determination of dimethylamine (DMA) and trimethylamine (TMA). These occur in the breath of people suffering from renal disease. The measurement of amines present in trace concentrations requires the application of suitable analytical methods during sampling, storage and preconcentration. This is particularly so due to their polar and basic properties. In this paper, the application of solid phase microextraction (SPME) and thermal desorption (TD) with subsequent measurement by GC-MS for the determination of amines is discussed. For DMA, preconcentration by SPME did not give satisfactory results. TMA may be analysed using SPME preconcentration with an LOD of 1.5 ppb. Thermal desorption with Tenax as the adsorbing material allows reliable concentration determination for TMA (LOD = 0.5 ppb) and DMA (LOD = 4.6 ppb). DMA cannot be stored reliably in Tedlar bags and longer storage on Tenax (with subsequent TD) does not give good repeatability of results. For TMA, storage can be done on Tenax or in bags, the best results for the latter being achieved with Flex Foil bags.

  5. Critical role of a pre-purge setup in the thermal desorption analysis of volatile organic compounds by gas chromatography with mass spectrometry.

    Science.gov (United States)

    Kim, Yong-Hyun; Kim, Ki-Hyun

    2015-07-01

    In general, volatile organic compounds in ambient air are quantified by following a well-defined standard calibration procedure using a gas-/liquid-phase standard. If the liquid standard is analyzed by a thermal desorption, the solvent effect is unavoidable through the alteration of breakthrough properties or retention times. To learn more about the variables of the thermal desorption-based analysis, the effect of pre-purge conditions was evaluated for 18 volatile organic compounds with different types of sorbent tube materials by fixing standard volume (1 μL) and flow rate (100 mL/min). The gas phase calibration was also carried out as reference for the non-solvent effect. A single tube filled with Tenax TA exhibited the least solvent effect with the short pre-purge (1 min), while being subject to the breakthrough at or above 10 min pre-purge. For a three-bed sorbent tube with Carboxen 1000, at least 10 min of pre-purge was needed for the compounds with a retention time close to methanol (e.g., propanal). Another three-bed tube with Carbopack X reduced the solvent effect efficiently for a short pre-purge (2 min) without the breakthrough. As such, the solvent effect can be adjusted by the proper control of the sorbent tube application.

  6. Thermal extraction: enhancing thermal emission of finite size macroscopic blackbody to far-field vacuum

    CERN Document Server

    Yu, Zongfu; Zhang, Torbjorn Skauli Gang; Wang, Hailiang; Fan, Shanhui

    2012-01-01

    The understanding of far-field thermal radiation had directly led to the discovery of quantum mechanics a century ago, and is of great current practical importance for applications in energy conversions, radiative cooling, and thermal control. It is commonly assumed that for any macroscopic thermal emitter, its maximal emitted power within any given frequency range cannot exceed that of a blackbody with the same surface area. In contrast to such conventional wisdom, here we propose, and experimentally demonstrate, that the emitted power from a finite size macroscopic blackbody to far field vacuum can be significantly enhanced, within the constraint of the second law of thermodynamics. To achieve such an enhancement, the thermal body needs to have internal electromagnetic density of states (DOS) greater than that of vacuum, and one needs to provide a thermal extraction mechanism to enable the contributions of all internal modes to far field radiation.

  7. Extraction Techniques for Polycyclic Aromatic Hydrocarbons in Soils

    Directory of Open Access Journals (Sweden)

    E. V. Lau

    2010-01-01

    Full Text Available This paper aims to provide a review of the analytical extraction techniques for polycyclic aromatic hydrocarbons (PAHs in soils. The extraction technologies described here include Soxhlet extraction, ultrasonic and mechanical agitation, accelerated solvent extraction, supercritical and subcritical fluid extraction, microwave-assisted extraction, solid phase extraction and microextraction, thermal desorption and flash pyrolysis, as well as fluidised-bed extraction. The influencing factors in the extraction of PAHs from soil such as temperature, type of solvent, soil moisture, and other soil characteristics are also discussed. The paper concludes with a review of the models used to describe the kinetics of PAH desorption from soils during solvent extraction.

  8. Micro-solid phase extraction followed by thermal extraction coupled with gas chromatography-mass selective detector for the determination of polybrominated diphenyl ethers in water.

    Science.gov (United States)

    Naing, Nyi Nyi; Li, Sam Fong Yau; Lee, Hian Kee

    2016-08-05

    A method of analyzing environmental contaminants in water based on micro-solid phase extraction (μ-SPE) followed by thermal extraction (TE) and a cold-trapping step, coupled with gas chromatography-mass selective detection (GC-MSD) was developed and validated. μ-SPE-TE- GC-MSD was employed in the determination of five polybrominated diphenyl ethers. The μ-SPE sorbent was chitosan-graphene oxide (CS-GO) composite, which was prepared by mixing CS and GO by means of ultrasonication. The CS in the composite was cross-linked with glutaraldehyde. After μ-SPE, the analytes in the extract were extracted thermally in a thermal desorption unit tube combined with a cooled injection system, coupled to GC-MSD. The extraction conditions were optimized for the detection of the target compounds in water. This method provided linearity ranges of between 0.1 and 20μgL(-1) (depending on the analytes), with coefficients of determination, r(2), ≥0.9982. The calculated relative recoveries were between 71.52 and 96.15% whereas precision (based on % relative standard deviations) was between 3.54 and 11.36%. The method showed limit of detection and limit of quantification ranges of between 0.007 and 0.016μgL(-1), and between 0.023 and 0.054μgL(-1), for the two groups of analytes, respectively. The method was applied to the determination of the target analytes in water.

  9. Ultra-fast cyclosporin A quantitation in whole blood by Laser Diode Thermal Desorption-tandem mass spectrometry; comparison with High Performance Liquid Chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Jourdil, Jean-François; Picard, Pierre; Meunier, Cécile; Auger, Serge; Stanke-Labesque, Françoise

    2013-12-17

    In the last decade the quantitation of immunosuppressive drugs has seen vast improvements in analytical methods, optimizing time, accuracy of analysis and cost. Laser Diode Thermal Desorption (LDTD) coupled to Atmospheric Pressure Chemical ionization-tandem mass spectrometry (APCI-MS/MS) represents a technological breakthrough that removes the chromatographic separation step and thereby significantly increases the analytical throughput for the quantitation of cyclosporin A (CsA) in whole blood for therapeutic drug monitoring (TDM). A simple protein precipitation step was used prior to depositing 5 μL of the extract on a 96-well LazWell™ plate and CsA was quantified by LDTD-APCI-MS/MS. The laser pattern was set to ramp from 0 to 45% laser power within 2 s. The APCI parameters were set to negative needle voltage (-2 μA), carrier gas temperature (30°C) and air flow rate (3 L min(-1)). The negative ion single reaction monitoring transitions for CsA and its internal standard cyclosporin D (CsD) were respectively m/z 1201.1/1088.9 and m/z 1214.8/1102.8; obtained with a collision energy of -40 V. The analysis was achieved within 9 s from sample to sample. The extraction procedure yielded high recovery (92%; RSD=9.4%, n=6). The lower limit of quantitation was fixed at the first level of calibration: 23.5 ng mL(-1) (accuracy=112.3%; RSD=9.6%; n=6) and a blank+6 point linear regression up to 965 ng mL(-1) was used. Using 4 levels of quality control (QC), intra-day assays (n=6) ranged from 93.5 to 95.7% (bias) and from 3.4 to 13.1% (RSD) while inter-day assays (n=6) ranged from 92.9 to 105.3% (bias) and from 4.9 to 7.5% (RSD). An inter-sample contamination of CsA of 2.3% was calculated that was considered negligible with respect to the range of CsA concentrations. Whole blood samples (120) from patients under CsA treatment were analyzed by LDTD-APCI-MS/MS and HPLC-ESI-MS/MS, the gold standard reference method for CsA quantification. Both methods agreed (P≥0.99), with a

  10. Occupational exposure to complex mixtures of volatile organic compounds in ambient air: desorption from activated charcoal using accelerated solvent extraction can replace carbon disulfide?

    Science.gov (United States)

    Fabrizi, Giovanni; Fioretti, Marzia; Rocca, Lucia Mainero

    2013-01-01

    A desorption study of 57 volatile organic compounds (VOCs) has been conducted by use of accelerated solvent extraction (ASE) and gas chromatography-mass spectrometry. Different solvents were tested to extract activated charcoal tubes with the objective of replacing carbon disulfide, used in official methods, because of its highly toxic health and environmental effects. Extraction conditions, for example temperature and number of cycles, were investigated and optimized. The definitive extraction procedure selected was use of acetone at 150 °C and two consecutive extraction cycles at a pressure of 1,500 psi. Considering a sample volume of 0.005 Nm(3), corresponding to a sampling time of 8 h at a flow rate of 0.01 L min(-1), the method was validated over the concentration range 65-26,300 μg Nm(-3). The lowest limit of quantification was 6 μg Nm(-3), and recovery for the 93 % of analytes ranged from 65 to 102 %. For most of the compounds, relative standard deviations were less than 15 % for inter and intra-day precision. Uncertainty of measurement was also determined: the relative expanded uncertainty was always below 29.6 %, except for dichlorodifluoromethane. This work shows that use of friendlier solvent, for example acetone, coupled with use of ASE, can replace use of CS(2) for chemical removal of VOCs from activated charcoal. ASE has several advantages over traditional solvent-extraction methods, including shorter extraction time, minimum sample manipulation, high reproducibility, and less extraction discrimination. No loss of sensitivity occurs and there is also a salutary effect on bench workers' health and on the smell of laboratory air.

  11. Novel characterization of the adsorption sites in large pore metal-organic frameworks: combination of X-ray powder diffraction and thermal desorption spectroscopy.

    Science.gov (United States)

    Soleimani-Dorcheh, Ali; Dinnebier, Robert E; Kuc, Agnieszka; Magdysyuk, Oxana; Adams, Frank; Denysenko, Dmytro; Heine, Thomas; Volkmer, Dirk; Donner, Wolfgang; Hirscher, Michael

    2012-10-05

    The preferred adsorption sites of xenon in the recently synthesized metal-organic framework MFU-4l(arge) possessing a bimodal pore structure (with pore sizes of 12 Å and 18.6 Å) were studied via the combination of low temperature thermal desorption spectroscopy and in situ X-ray powder diffraction. The diffraction patterns were collected at 110 K and 150 K according to the temperature of the desorption maxima. The maximum entropy method was used to reconstruct the electron density distribution of the structure and to localize the adsorbed xenon using refined data of the Xe-filled and empty sample. First principles calculations revealed that Xe atoms exclusively occupy the Wyckoff 32f position at approximately 2/3 2/3 2/3 along the body diagonal of the cubic crystal structure. At 110 K, Xe atoms occupy all 32 f positions (8 atoms per pore) while at 150 K the occupancy descends to 25% (2 atoms per pore). No Xe occupation of the small pores is observed by neither experimental measurements nor theoretical studies.

  12. Thermal desorption studies of isotopically-labeled oxygen-induced superconductivity in La sub 2 CuO sub 4+. delta

    Energy Technology Data Exchange (ETDEWEB)

    Shinn, N.D.; Bartram, M.E.; Schirber, J.E.; Overmyer, D.L.; Rogers, J.W. Jr. (Sandia National Labs., Albuquerque, NM (USA)); Fisk, Z.; Cheong, S.W. (Los Alamos National Lab., NM (USA))

    1990-01-01

    Isotopically-labeled oxygen enrichment and thermal desorption mass spectroscopy (TDMS) have been combined to study interstitial oxygen desorption from superconducting La{sub 2}CuO{sub 4+{delta}} ({delta} {le} 0.032). Single crystal samples of magnetic insulating La{sub 2}CuO{sub 4.00} were annealed at 860K under 1--3 kbar oxygen pressure for 12--100 hours to yield hole-doped, superconducting La{sub 2}CuO{sub 4+{delta}} samples with 35K < {Tc} < 40K. Whereas no TDMS signals were observed for the insulator, rapid bursts (FWHM < 0.5 sec) of molecular oxygen were observed above 350K while heating the superconductor at less than 1 K sec{sup {minus}1} in high vacuum. A kinetic model is proposed in which the interstitial oxygen diffuses to internal grain boundaries and defects during heating, thereby inducing stress in the lattice as it attempts to revert to the LaCuO{sub 4.00} crystal structure. This stress is relieved by lattice fracture at grain boundaries during the TDMS experiment, releasing the trapped oxygen from the sample as micro-cracks are formed. In addition, the facile oxygen exchange between interstitial and lattice oxygen sites has been discovered by TDMS and weight gain measurements from isotopically-enriched crystals, supporting the structural model of Chaillout, et al. in which the interstitial oxygen atom dimerizes with a lattice oxygen ion.

  13. Use of thermal desorption gas chromatography-olfactometry/mass spectrometry for the comparison of identified and unidentified odor active compounds emitted from building products containing linseed oil

    DEFF Research Database (Denmark)

    Clausen, P. A.; Knudsen, Henrik Nellemose; Larsen, K.

    2008-01-01

    The emission of odor active volatile organic compounds (VOCs) from a floor oil based on linseed oil, the linseed oil itself and a low-odor linseed oil was investigated by thermal desorption gas chromatography combined with olfactometry and mass spectrometry (TD-GC-O/MS). The oils were applied...... identified by GC-MS. While 92 VOCs were detected from the oil used in the floor oil, only 13 were detected in the low-odor linseed oil. The major odor active VOCs were aldehydes and carboxylic acids. Spearmen rank correlation of the GC-O profiles showed that the odor profile of the linseed oil likely...... influenced the odor profile of the floor oil based on this linseed oil....

  14. Use of thermal desorption gas chromatography-olfactometry/mass spectrometry for the comparison of identified and unidentified odor active compounds emitted from building products containing linseed oil

    DEFF Research Database (Denmark)

    Clausen, P. A.; Knudsen, Henrik Nellemose; Larsen, K.

    2008-01-01

    The emission of odor active volatile organic compounds (VOCs) from a floor oil based on linseed oil, the linseed oil itself and a low-odor linseed oil was investigated by thermal desorption gas chromatography combined with olfactometry and mass spectrometry (TD-GC-O/MS). The oils were applied...... identified by GC-MS. While 92 VOCs were detected from the oil used in the floor oil, only 13 were detected in the low-odor linseed oil. The major odor active VOCs were aldehydes and carboxylic acids. Spearmen rank correlation of the GC-O profiles showed that the odor profile of the linseed oil likely...... influenced the odor profile of the floor oil based on this linseed oil....

  15. Measurement of Passive Uptake Rates for Volatile Organic Compounds on Commercial Thermal Desorption Tubes and the Effect of Ozone on Sampling

    Energy Technology Data Exchange (ETDEWEB)

    Maddalena, Randy [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States); Parra, Amanda [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States); Russell, Marion [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States); Lee, Wen-Yee [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)

    2013-05-01

    Diffusive or passive sampling methods using commercially filled axial-sampling thermal desorption tubes are widely used for measuring volatile organic compounds (VOCs) in air. The passive sampling method provides a robust, cost effective way to measure air quality with time-averaged concentrations spanning up to a week or more. Sampling rates for VOCs can be calculated using tube geometry and Fick’s Law for ideal diffusion behavior or measured experimentally. There is evidence that uptake rates deviate from ideal and may not be constant over time. Therefore, experimentally measured sampling rates are preferred. In this project, a calibration chamber with a continuous stirred tank reactor design and constant VOC source was combined with active sampling to generate a controlled dynamic calibration environment for passive samplers. The chamber air was augmented with a continuous source of 45 VOCs ranging from pentane to diethyl phthalate representing a variety of chemical classes and physiochemical properties. Both passive and active samples were collected on commercially filled Tenax TA thermal desorption tubes over an 11-day period and used to calculate passive sampling rates. A second experiment was designed to determine the impact of ozone on passive sampling by using the calibration chamber to passively load five terpenes on a set of Tenax tubes and then exposing the tubes to different ozone environments with and without ozone scrubbers attached to the tube inlet. During the sampling rate experiment, the measured diffusive uptake was constant for up to seven days for most of the VOCs tested but deviated from linearity for some of the more volatile compounds between seven and eleven days. In the ozone experiment, both exposed and unexposed tubes showed a similar decline in terpene mass over time indicating back diffusion when uncapped tubes were transferred to a clean environment but there was no indication of significant loss by ozone reaction.

  16. Diclofenac in municipal wastewater treatment plant: quantification using laser diode thermal desorption--atmospheric pressure chemical ionization--tandem mass spectrometry approach in comparison with an established liquid chromatography-electrospray ionization-tandem mass spectrometry method.

    Science.gov (United States)

    Lonappan, Linson; Pulicharla, Rama; Rouissi, Tarek; Brar, Satinder K; Verma, Mausam; Surampalli, Rao Y; Valero, José R

    2016-02-12

    Diclofenac (DCF), a prevalent non-steroidal anti-inflammatory drug (NSAID) is often detected in wastewater and surface water. Analysis of the pharmaceuticals in complex matrices is often laden with challenges. In this study a reliable, rapid and sensitive method based on laser diode thermal desorption/atmospheric pressure chemical ionization (LDTD/APCI) coupled with tandem mass spectrometry (MS/MS) has been developed for the quantification of DCF in wastewater and wastewater sludge. An established conventional LC-ESI-MS/MS (liquid chromatography-electrospray ionization-tandem mass spectrometry) method was compared with LDTD-APCI-MS/MS approach. The newly developed LDTD-APCI-MS/MS method reduced the analysis time to 12s in lieu of 12 min for LC-ESI-MS/MS method. The method detection limits for LDTD-APCI-MS/MS method were found to be 270 ng L(-1) (LOD) and 1000 ng L(-1) (LOQ). Furthermore, two extraction procedures, ultrasonic assisted extraction (USE) and accelerated solvent extraction (ASE) for the extraction of DCF from wastewater sludge were compared and ASE with 95.6 ± 7% recovery was effective over USE with 86 ± 4% recovery. The fate and partitioning of DCF in wastewater (WW) and wastewater sludge (WWS) in wastewater treatment plant was also monitored at various stages of treatment in Quebec Urban community wastewater treatment plant. DCF exhibited affinity towards WW than WWS with a presence about 60% of DCF in WW in contrary with theoretical prediction (LogKow=4.51).

  17. In situ liquid-liquid extraction as a sample preparation method for matrix-assisted laser desorption/ionization MS analysis of polypeptide mixtures

    DEFF Research Database (Denmark)

    Kjellström, Sven; Jensen, Ole Nørregaard

    2003-01-01

    A novel liquid-liquid extraction (LLE) procedure was investigated for preparation of peptide and protein samples for matrix-assisted laser desorption/ionization mass spectrometry (MALDI MS). LLE using ethyl acetate as the water-immiscible organic solvent enabled segregation of hydrophobic...... matrix to the organic solvent enhanced the efficiency of the LLE-MALDI MS method for analysis of hydrophobic peptides and proteins. LLE-MALDI MS enabled the detection of the hydrophobic membrane protein bacteriorhodopsin as a component in a simple protein mixture. Peptide mixtures containing...... phosphorylated, glycosylated, or acylated peptides were successfully separated and analyzed by the in situ LLE-MALDI MS technique and demonstrate the potential of this method for enhanced separation and structural analysis of posttranslationally modified peptides in proteomics research....

  18. An extraction method of positive blood cultures for direct identification of Candida species by Vitek MS matrix-assisted laser desorption ionization time of flight mass spectrometry.

    Science.gov (United States)

    Lavergne, Rose-Anne; Chauvin, Pamela; Valentin, Alexis; Fillaux, Judith; Roques-Malecaze, Christine; Arnaud, Sylvie; Menard, Sandie; Magnaval, Jean-François; Berry, Antoine; Cassaing, Sophie; Iriart, Xavier

    2013-08-01

    Candida spp. are an important cause of nosocomial bloodstream infections. Currently, complete identification of yeasts with conventional methods takes several days. We report here the first evaluation of an extraction method associated with the Vitek MS matrix-assisted laser desorption ionization time of flight mass spectrometry for direct identification of Candida species from positive blood cultures. We evaluated this protocol with blood cultures that were inoculated with reference and routine isolates (eight reference strains, 30 patients isolates and six mixed cultures containing two strains of different Candida species), or from patients with candidemia (28 isolates). This method performed extremely well (97% correct identification) with blood cultures of single Candida spp. and significantly reduced the time of diagnosis. Nevertheless, subculture remains indispensable to test fungal resistance and to detect mixed infections.

  19. Reproducibility of serum protein profiling by systematic assessment using solid-phase extraction and matrix-assisted laser desorption/ionization mass spectrometry

    DEFF Research Database (Denmark)

    Callesen, Anne K; Christensen, René Depont; Madsen, Jonna S

    2008-01-01

    for serum protein profiling we investigated a range of sample preparation techniques and developed a statistical method based on repeated analyses for evaluation of protein-profiling performance of MALDI MS. Two different solid-phase extraction (SPE) methods were investigated, namely custom......Protein profiling of human serum by matrix-assisted laser desorption/ionization mass spectrometry (MALDI MS) is potentially a new diagnostic tool for early detection of human diseases, including cancer. Sample preparation is a key issue in MALDI MS and the analysis of complex samples such as serum......-made microcolumns and commercially available magnetic beads. Using these two methods, nineteen different sample preparation methods for serum profiling by MALDI MS were systematically tested with regard to matrix selection, stationary phase, selectivity, and reproducibility. Microcolumns were tested with regard...

  20. Analysis of the chemical composition of organic aerosol at the Mt. Sonnblick observatory using a novel high mass resolution thermal-desorption proton-transfer-reaction mass-spectrometer (hr-TD-PTR-MS)

    NARCIS (Netherlands)

    Holzinger, R.|info:eu-repo/dai/nl/337989338; Kasper-Giebl, A.; Staudinger, M.; Schauer, G.; Roeckmann, T.|info:eu-repo/dai/nl/304838233

    2010-01-01

    For the first time a high mass resolution thermal desorption proton transfer reaction mass spectrometer (hr-TD-PTR-MS) was deployed in the field to analyze the composition of the organic fraction of aerosols. We report on measurements from the remote Mt. Sonnblick observatory in the Austrian alps

  1. Hydrogen desorption from nanostructured magnesium hydride composites

    Directory of Open Access Journals (Sweden)

    Brdarić Tanja P.

    2007-01-01

    Full Text Available The influence of 3d transition metal addition (Fe, Co and Ni on the desorption properties of magnesium hydride were studied. The ball milling of MgH2-3d metal blends was performed under Ar. Microstructural and morphological characterization were performed by XRD and SEM analysis, while the hydrogen desorption properties were investigated by DSC. The results show a strong correlation between the morphology and thermal stability of the composites. The complex desorption behavior (the existence of more than one desorption peak was correlated with the dispersion of the metal additive particles that appear to play the main role in the desorption. The desorption temperature can be reduced by more than 100 degrees if Fe is added as additive. The activation energy for H2 desorption from the MgH2-Fe composite is 120 kJ/mol, implying that diffusion controls the dehydration process.

  2. Development of a new multi-residue laser diode thermal desorption atmospheric pressure chemical ionization tandem mass spectrometry method for the detection and quantification of pesticides and pharmaceuticals in wastewater samples.

    Science.gov (United States)

    Boisvert, Michel; Fayad, Paul B; Sauvé, Sébastien

    2012-11-19

    A new solid phase extraction (SPE) method coupled to a high throughput sample analysis technique was developed for the simultaneous determination of nine selected emerging contaminants in wastewater (atrazine, desethylatrazine, 17β-estradiol, ethynylestradiol, norethindrone, caffeine, carbamazepine, diclofenac and sulfamethoxazole). We specifically included pharmaceutical compounds from multiple therapeutic classes, as well as pesticides. Sample pre-concentration and clean-up was performed using a mixed-mode SPE cartridge (Strata ABW) having both cation and anion exchange properties, followed by analysis by laser diode thermal desorption atmospheric pressure chemical ionization coupled to tandem mass spectrometry (LDTD-APCI-MS/MS). The LDTD interface is a new high-throughput sample introduction method, which reduces total analysis time to less than 15s per sample as compared to minutes with traditional liquid-chromatography coupled to tandem mass spectrometry (LC-MS/MS). Several SPE parameters were evaluated in order to optimize recovery efficiencies when extracting analytes from wastewater, such as the nature of the stationary phase, the loading flow rate, the extraction pH, the volume and composition of the washing solution and the initial sample volume. The method was successfully applied to real wastewater samples from the primary sedimentation tank of a municipal wastewater treatment plant. Recoveries of target compounds from wastewater ranged from 78% to 106%, the limit of detection ranged from 30 to 122ng L(-1) while the limit of quantification ranged from 90 to 370ng L(-1). Calibration curves in the wastewater matrix showed good linearity (R(2)≥0.991) for all target analytes and the intraday and interday coefficient of variation was below 15%, reflecting a good precision.

  3. H{sub 2} thermal desorption and hydride conversion reactions in Li cells of TiH{sub 2}/C amorphous nanocomposites

    Energy Technology Data Exchange (ETDEWEB)

    Vitucci, F.M., E-mail: francesco.vitucci@roma1.infn.it [CNR-ISC, U.O.S. La Sapienza, Piazzale A. Moro 5, 00185 Roma (Italy); Paolone, A. [CNR-ISC, U.O.S. La Sapienza, Piazzale A. Moro 5, 00185 Roma (Italy); Brutti, S. [CNR-ISC, U.O.S. La Sapienza, Piazzale A. Moro 5, 00185 Roma (Italy); Dipartimento di Scienze, Univ. Basilicata, V.le Ateneo Lucano, 10, 85100 Potenza (Italy); Munaò, D.; Silvestri, L.; Panero, S. [Dipartimento di Chimica, Sapienza Univ. Roma, P.le A. Moro 5, 00185 Roma (Italy); Reale, P. [ENEA – Centro Ricerche Casaccia,via Anguillarese 301, 00100 Roma (Italy)

    2015-10-05

    Highlights: • Galvanostatic measurements on amorphous TiH{sub 2} is reported. • Variation of ball milling pre-treatment vary the first discharge capacity. • Relation between thermal H{sub 2} desorption and electrochemical properties is proposed. - Abstract: Here we investigate the properties of amorphous TiH{sub 2}/carbon nanocomposites as possible active material in lithium cells. Several TiH{sub 2}/C mixtures are prepared by a mechanochemical route, by varying the carbon/hydride ratio. Materials are tested in electrochemical cells versus lithium metal in EC:DMC LiPF{sub 6} electrolyte by galvanostatic cycling (GC) and are characterized by X-ray diffraction, transmission electron microscopy, thermogravimetry and mass spectrometry. Thermal dehydrogenation processes are altered by the mechanochemical treatment of the sample: milling decreases the hydrogen content of the hydride. On the other hand, the mechanochemical grinding increases the specific capacity delivered during the first GC discharge. We suggest that the electrochemical process is the result of a delicate balance between the absolute quantity of hydrogen and its availability for the hydride conversion reaction.

  4. Analysis of volatile organic compounds released from the decay of surrogate human models simulating victims of collapsed buildings by thermal desorption-comprehensive two-dimensional gas chromatography-time of flight mass spectrometry.

    Science.gov (United States)

    Agapiou, A; Zorba, E; Mikedi, K; McGregor, L; Spiliopoulou, C; Statheropoulos, M

    2015-07-01

    Field experiments were devised to mimic the entrapment conditions under the rubble of collapsed buildings aiming to investigate the evolution of volatile organic compounds (VOCs) during the early dead body decomposition stage. Three pig carcasses were placed inside concrete tunnels of a search and rescue (SAR) operational field terrain for simulating the entrapment environment after a building collapse. The experimental campaign employed both laboratory and on-site analytical methods running in parallel. The current work focuses only on the results of the laboratory method using thermal desorption coupled to comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry (TD-GC×GC-TOF MS). The flow-modulated TD-GC×GC-TOF MS provided enhanced separation of the VOC profile and served as a reference method for the evaluation of the on-site analytical methods in the current experimental campaign. Bespoke software was used to deconvolve the VOC profile to extract as much information as possible into peak lists. In total, 288 unique VOCs were identified (i.e., not found in blank samples). The majority were aliphatics (172), aromatics (25) and nitrogen compounds (19), followed by ketones (17), esters (13), alcohols (12), aldehydes (11), sulfur (9), miscellaneous (8) and acid compounds (2). The TD-GC×GC-TOF MS proved to be a sensitive and powerful system for resolving the chemical puzzle of above-ground "scent of death".

  5. Analysis of volatile organic compounds in water by dynamic stripping, thermal desorption, cryofocusing, and capillary gas chromatography (journal version)

    Energy Technology Data Exchange (ETDEWEB)

    Vandegrift, S.A.

    1988-01-01

    A dynamic headspace procedure developed for the determination of volatile organic compounds (VOCs) in water is described. The VOCs are purged from a water sample with an inert gas, transferring them to a tube packed with Tenax adsorbent. The adsorbent tube, or trap, is thermally desorbed, the analytes cryofocused, and subsequently transferred to a capillary column gas chromatograph.

  6. Thermal desorption characteristics of CO, O2 and CO2 on non-porous water, crystalline water and silicate surfaces at sub-monolayer and multilayer coverages

    CERN Document Server

    Noble, J A; Dulieu, F; Fraser, H J

    2011-01-01

    The desorption characteristics of molecules on interstellar dust grains are important for modelling the behaviour of molecules in icy mantles and, critically, in describing the solid-gas interface. In this study, a series of laboratory experiments exploring the desorption of three small molecules from three astrophysically relevant surfaces are presented. The desorption of CO, O2 and CO2 at both sub-monolayer and multilayer coverages was investigated from non-porous water, crystalline water and silicate surfaces. Experimental data was modelled using the Polanyi-Wigner equation to produce a mathematical description of the desorption of each molecular species from each type of surface, uniquely describing both the monolayer and multilayer desorption in a single combined model. The implications of desorption behaviour over astrophysically relevant timescales are discussed.

  7. Serum protein profiling by miniaturized solid-phase extraction and matrix-assisted laser desorption/ionization mass spectrometry

    DEFF Research Database (Denmark)

    Callesen, Anne K; Mohammed, Shabaz; Bunkenborg, Jakob;

    2005-01-01

    for translation of MALDI-MS based diagnostic methods to clinical applications. We have investigated a number of MALDI matrices and several miniaturized solid-phase extraction (SPE) methods for serum protein concentration and desalting with the aim of generating reproducible, high-quality protein profiles by MALDI...... mass spectra (m/z 1000-12,000) to be obtained from serum. In a proof-of-principle application, SPE with chelating material and MALDI-MS identified protein peaks in serum that had been previously reported for distinguishing a person diagnosed with breast cancer from a control. These preliminary results...

  8. The gas chromatographic determination of volatile fatty acids in wastewater samples: evaluation of experimental biases in direct injection method against thermal desorption method.

    Science.gov (United States)

    Ullah, Md Ahsan; Kim, Ki-Hyun; Szulejko, Jan E; Cho, Jinwoo

    2014-04-11

    The production of short-chained volatile fatty acids (VFAs) by the anaerobic bacterial digestion of sewage (wastewater) affords an excellent opportunity to alternative greener viable bio-energy fuels (i.e., microbial fuel cell). VFAs in wastewater (sewage) samples are commonly quantified through direct injection (DI) into a gas chromatograph with a flame ionization detector (GC-FID). In this study, the reliability of VFA analysis by the DI-GC method has been examined against a thermal desorption (TD-GC) method. The results indicate that the VFA concentrations determined from an aliquot from each wastewater sample by the DI-GC method were generally underestimated, e.g., reductions of 7% (acetic acid) to 93.4% (hexanoic acid) relative to the TD-GC method. The observed differences between the two methods suggest the possibly important role of the matrix effect to give rise to the negative biases in DI-GC analysis. To further explore this possibility, an ancillary experiment was performed to examine bias patterns of three DI-GC approaches. For instance, the results of the standard addition (SA) method confirm the definite role of matrix effect when analyzing wastewater samples by DI-GC. More importantly, their biases tend to increase systematically with increasing molecular weight and decreasing VFA concentrations. As such, the use of DI-GC method, if applied for the analysis of samples with a complicated matrix, needs a thorough validation to improve the reliability in data acquisition.

  9. Separation and analysis of trace volatile formaldehyde in aquatic products by a MoO₃/polypyrrole intercalative sampling adsorbent with thermal desorption gas chromatography and mass spectrometry.

    Science.gov (United States)

    Ma, Yunjian; Zhao, Cheng; Zhan, Yisen; Li, Jianbin; Zhang, Zhuomin; Li, Gongke

    2015-05-01

    An in situ embedded synthesis strategy was developed for the preparation of a MoO3 /polypyrrole intercalative sampling adsorbent for the separation and analysis of trace volatile formaldehyde in aquatic products. Structural and morphological characteristics of the MoO3 /polypyrrole intercalative adsorbent were investigated by a series of characterization methods. The MoO3 /polypyrrole sampling adsorbent possessed a higher sampling capacity and selectivity for polar formaldehyde than commonly used commercial adsorbent Tenax TA. Finally, the MoO3 /polypyrrole adsorbent was packed in the thermal desorption tube that was directly coupled to gas chromatography with mass spectrometry for the analysis of trace volatile formaldehyde in aquatic products. Trace volatile formaldehyde from real aquatic products could be selectively sampled and quantified to be 0.43-6.6 mg/kg. The detection limit was achieved as 0.004 μg/L by this method. Good recoveries for spiked aquatic products were achieved in range of 75.0-108% with relative standard deviations of 1.2-9.0%. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Ion mobility spectrometry-mass spectrometry studies of ion processes in air at atmospheric pressure and their application to thermal desorption of 2,4,6-trinitrotoluene

    Science.gov (United States)

    Sabo, Martin; Malásková, Michaela; Matejčík, Štefan

    2014-02-01

    In this study we have investigated the negative reactant ion formation in a negative corona discharge (CD) using the corona discharge ion mobility spectrometry orthogonal acceleration time-of-flight (CD-IMS-oaTOF) technique. The reactant ions were formed in the CD operating in the reverse gas flow mode at an elevated temperature of 363.5 K in synthetic and ambient air. Under these conditions mainly O_{2}^{-} and their clusters were formed. We have also studied the influence of CCl4 admixture to air (dopant gas) on the composition of the reactant ions, which resulted in the formation of Cl- and its clusters with a reduced ion mobility of 3.05 cm2 V-1 s-1 as a major reactant ion peak. Additional IMS peaks with reduced ion mobilities of 2.49, 2.25 and 2.03 cm2 V-1 s-1 were detected, and Cl- · (NO2) and Cl- · (NO)n(n = 2, 3) anions were identified. The negative reactant ions were used to detect 2,4,6 trinitrotoluene (TNT) using the thermal desorption (TD) technique using a CD-IMS instrument. Using TD sampling and a negative CD ion source doped by CCl4 we have achieved a limit of detection of 350 pg for direct surface analysis of TNT.

  11. Volatile organic compounds in air at urban and industrial areas in the Tarragona region by thermal desorption and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Ras, Maria Rosa; Marcé, Rosa Maria; Borrull, Francesc

    2010-02-01

    Annual trends of a group of 66 volatile organic compounds (VOCs), containing 20 ozone precursors, were the aim of a sampling campaign carried out for a year in air at urban and industrial areas from Tarragona region. VOCs were determined by active collection on multisorbent tubes, followed by thermal desorption and gas chromatography-mass spectrometry. The analytical method was developed and validated, showing good levels of detection and quantification, recoveries, precision, and linearity for all the compounds in the range being studied. All the industrial and urban samples taken during the sampling campaign were similar in their qualitative composition. The most abundant compound in all urban and industrial sites was i-pentane, with concentrations between 15.2 and 202.1 microg m(-3) in urban sites and between 1.3 and 98.6 microg m(-3) in industrial sites. In urban sites, the following compounds in order of abundance were toluene, n-pentane, m,p-xylene, and o-xylene, with maximum levels of 150.6, 45.8, 42.3, and 31.7 microg m(-3), respectively. In industrial sites, the most abundant compounds depended on the sampled site.

  12. Direct quantitative analysis of phthalate esters as micro-contaminants in cleanroom air and wafer surfaces by auto-thermal desorption--gas chromatography--mass spectrometry.

    Science.gov (United States)

    Kang, Yuhao; Den, Walter; Bai, Hsunling; Ko, Fu-Hsiang

    2005-04-01

    This study established an analytical method for the trace analyses of two phthalate esters, including diethyl phthalate (DEP) and di-n-butyl phthalate (DBP), known as the major constituents of cleanroom micro-contamination detrimental to the reliability of semiconductor devices. Using thermal desorption coupled with a GC-MS system, standard tubes were prepared by delivering liquid standards pre-vaporized by a quasi-vaporizer into Tenax GR tubes for calibration. This method was capable of achieving detection limits of 0.05 microg m(-3) for 0.1 m3 air samples and 0.03 ng cm(-2) for 150-mm wafer surface density. Actual samples collected from a semiconductor cleanroom showed that the concentration of DBP in a polypropylene wafer box (0.45 microg m(-3)) was nearly four times higher than that in the cleanroom environment (0.12 microg m(-3)). The surface contamination of DBP was 0.67 ng cm(-2) for a wafer stored in the wafer box for 24 h. Furthermore, among the three types of heat-resistant O-ring materials tested, Kalrez was found to be particularly suitable for high-temperature processes in semiconductor cleanrooms due to their low emissions of organic vapors. This analytical procedure should serve as an effective monitoring method for the organic micro-contamination in cleanroom environments.

  13. Thermal desorption/tunable vacuum-ultraviolet time-of-flight photoionization aerosol mass spectrometry for investigating secondary organic aerosols in chamber experiments.

    Science.gov (United States)

    Fang, Wenzheng; Gong, Lei; Shan, Xiaobin; Liu, Fuyi; Wang, Zhenya; Sheng, Liusi

    2011-12-01

    This paper describes thermal desorption/tunable vacuum-ultraviolet photoionization time-of-flight aerosol mass spectrometry (TD-VUV-TOF-PIAMS) for the real-time analysis of secondary organic aerosols (SOAs) in smog chamber experiments. SOAs are sampled directly from atmospheric pressure and are focused through an aerodynamic lens assembly into the mass spectrometer. Once the particles have entered the source region, they impact on a heater and are vaporized. The nascent vapor is then softly ionized by tunable VUV synchrotron radiation. TD-VUV-TOF-PIAMS was used in conjunction with the smog chamber to study SOA formation from the photooxidation of toluene with hydroxyl radicals. The ionization energies (IEs) of these SOA products are sometimes very different with each other. As the ideal photon source is tunable, its energy can be adjusted for each molecular to be ionized. The mass spectra obtained at different photon energies are then to be useful for molecular identification. Real-time analysis of the mass spectra of SOAs is compared with previous off-line measurements. These results illustrate the potential of TD-VUV-TOF-PIAMS for direct molecular characterization of SOAs in smog chamber experiments.

  14. Development of a thermal desorption gas chromatography-mass spectrometry method for quantitative determination of haloanisoles and halophenols in wineries' ambient air.

    Science.gov (United States)

    Camino-Sánchez, F J; Ruiz-García, J; Zafra-Gómez, A

    2013-08-30

    An analytical method for the detection and quantification of haloanisoles and their corresponding halophenols in wineries' ambient air was developed. The target analytes were haloanisoles and halophenols, reported by previous scientific literature as responsible for wine taint. A calibrated pump and active tubes filled with Tenax GR™ were used for sampling. These tubes were thermally desorbed and analyzed using gas chromatography-triple quadrupole mass spectrometry in the selected reaction monitoring mode. The adsorption efficiencies of five commercial sampling tubes filled with different materials were evaluated. The efficiencies of the selected adsorbent were close to 100% for all sampled compounds. Desorption, chromatographic and mass spectrometric conditions were accurately optimized allowing very low limits of quantification and wide linear ranges. The limits of quantification in ambient air ranged from 0.8pgtube(-1) for 2,4,6-trichlorophenol, to 28pgtube(-1) for pentachlorophenol. These results are of great importance because human sensory threshold for haloanisoles is very low. The chromatographic method was also validated and the instrumental precision and trueness were established, a maximum RSD of 9% and a mean recovery of 91-106% were obtained. The proposed method involves an easy and sensitive technique for the early detection of haloanisoles and their precursor halophenols in ambient air avoiding contamination of wine or winery facilities.

  15. Quantification approach for assessment of sparkling wine volatiles from different soils, ripening stages, and varieties by stir bar sorptive extraction with liquid desorption.

    Science.gov (United States)

    Coelho, Elisabete; Coimbra, Manuel A; Nogueira, J M F; Rocha, Sílvia M

    2009-03-01

    Stir bar sorptive extraction with liquid desorption followed by large volume injection coupled to gas chromatography-quadrupole mass spectrometry (SBSE-LD/LVI-GC-qMS) was applied for the quantification of varietal and fermentative volatiles in sparkling wines. The analytical data were performed by using suitable standards of monoterpene hydrocarbons (alpha-pinene), monoterpenols (linalool), sesquiterpenoids (E,E-farnesol, Z-nerolidol, and guaiazulene), C(13) norisoprenoids (beta-ionone), aliphatic and aromatic alcohols (hexanol and 2-phenylethanol), and esters (hexyl acetate and ethyl decanoate) as model compounds. The wine volatiles were quantified using the structurally related standards. The methodology showed good linearity over the concentration range tested, with correlation coefficients ranging from 0.950 to 0.997, and a reproducibility of 9-18%. The SBSE-LD/LVI-GC-qMS methodology allowed, in a single run, the quantification of 71 wine volatiles that can be quantified accurately at levels lower than their respective olfactory thresholds. This methodology was used for assessment of sparkling wine volatiles from different soils, ripening stages, and varieties. The variety and soil influenced significantly the volatile composition of sparkling wines; lower effect was observed for the ripening stage of grapes picked up one week before or after the maturity state.

  16. Reversed phase liquid chromatography hyphenated to continuous flow-extractive desorption electrospray ionization-mass spectrometry for analysis and charge state manipulation of undigested proteins.

    Science.gov (United States)

    Li, Li; Yang, Samuel H; Vidova, Veronika; Rice, Elisa M; Wijeratne, Aruna B; Havlíček, Vladimír; Schug, Kevin A

    2015-01-01

    The application of continuous flow-extractive desorption electrospray ionization (CF-EDESI), an ambient ionization source demonstrated previously for use with intact protein analysis, is expanded here for the coupling of reversed phase protein separations to mass spectrometry. This configuration allows the introduction of charging additives to enhance detection without affecting the chromatographic separation mechanism. Two demonstrations of the advantages of CF-EDESI are presented in this work. First, a proof-of- principle is presented to demonstrate the applicability of hyphenation of liquid chromatography (LC) to CF- EDESI. LC-CF-EDESI-MS has good sensitivity compared to LC-electrospray ionization (ESI)-mass spectrometry. Second, the supercharging mechanism investigated in CF-EDESI provides an insight into a highly debated supercharging process in ESI. The results indicate that the mechanism of protein charging seen in HPLC-CF-EDESI is different from supercharging phenomena in conventional ESI. The surface tension mechanism and binding mechanism may both contribute to protein supercharging in ESI.

  17. Studies of properties of complex carbon-silica adsorbents used in sorption-desorption processes (solid-phase extraction)

    Energy Technology Data Exchange (ETDEWEB)

    Rudzinski, W. [Maria Curie-Sklodowska Univ., Lublin (Poland). Faculty of Chemistry; Gierak, A. [Maria Curie-Sklodowska Univ., Lublin (Poland). Faculty of Chemistry; Leboda, R. [Maria Curie-Sklodowska Univ., Lublin (Poland). Faculty of Chemistry; Dabrowski, A. [Maria Curie-Sklodowska Univ., Lublin (Poland). Faculty of Chemistry

    1995-08-01

    Adsorption properties of carbon and carbon-silica adsorbents, prepared by n-octanol and glucose pyrolysis and catalytic decomposition of n-butane, have been studied regarding their applicability for the extraction and concentration of phenol, its nitro- and chloro-derivatives and trihalomethanes [THM] from aqueous solutions in the concentration range of 2 to 20 mg/l. The adsorbents investigated have been subjected to various physico-chemical processes (hydrothermal treatment, oxidation, silanization) in order to improve their efficiency. The adsorption isotherms measured correspond well to the Freundlich equation. A good correlation have been observed between the values of the Freundlich constant k and the adsorbent efficiency. The investigation has been carried out using the ``off line`` method, and recovery rates for the compounds studied as high as 40-100% have been obtained. (orig.)

  18. Electronic structure and Schottky-barrier formation on GaAs (100) surfaces prepared by thermal desorption of a protective arsenic coating

    Energy Technology Data Exchange (ETDEWEB)

    Spindt, C.J.; Yamada, M.; Meissner, P.L.; Miyano, K.E.; Kendelewicz, T.; Herrera-Gomez, A.; Spicer, W.E. (Stanford Electronics Laboratories, Stanford University, Stanford, California 94305-4055 (United States)); Arko, A.J. (Los Alamos National Laboratory, Los Alamos, New Mexico 87545 (United States))

    1992-05-15

    Soft-x-ray photoemission spectroscopy has been used to characterize GaAs(100) surfaces and interfaces grown by molecular-beam epitaxy and prepared by the thermal desorption of a protective As coating. The samples studied were grown and arsenic capped identically to those used in a previous study (Brillson {ital et} {ital al}., J. Vac. Sci. Technol. B 6, 1263 (1988)). In this previous work, unpinned'' Schottky-barrier formation was reported, with barrier heights over a wide (0.75-eV) range. This is a striking result, as it was previously believed that all metals will pin GaAs surfaces in a narrow energy range near the middle of the band gap. This large range of barrier heights later led to the suggestion that the (100) surface could become an insulating layer that could screen out the effects of metal-induced gap states. Motivated by this work, we have studied Al and Au Schottky barriers since the deposition of these two metals gave the extreme low and high barriers in the 0.75-eV range. We have also characterized the clean surfaces prepared by desorbing the As caps at different temperatures. The As 3{ital d} and Ga 3{ital d} core levels showed that the surface stoichiometry could be varied significantly with the desorption temperature. The As 3{ital d} line shape was found to be the best indication of the surface stoichiometry after the anneal. The valence-band spectra did not show any strong features which could be used to determine when the sample was completely decapped. The electronic structure of the surface layer was investigated experimentally, and no evidence of an insulating reconstruction was found. In our study of band bending, we found that the low-doped samples used here and in the earlier study showed significant photovoltages resulting in incorrect band-bending measurements. We also found that the Au measurements are made difficult by the presence of core-level shifts due to Au-Ga alloying.

  19. Thermal desorption and recycling of volatile selective binders used in solid wastes deashing; Desorption thermique et recyclage d'agglomerants selectifs volatils utilises en decendrage de residus solides

    Energy Technology Data Exchange (ETDEWEB)

    Bensakhria, A.; Sajet, P.; Antonini, G. [Universite de Technologie de Compiegne, Centre de Recherches de Royallieu UMR 6067, Genie des Procedes Industriels, 60 - Compiegne (France)

    2001-07-01

    A pilot unit for the deashing of coal tailings by selective agglomeration and recovery of the binder/water mixture by azeotropic desorption of binders has been tested. The effect of different experiment parameters on the deashing efficiency, on the recovery and recycling of the binding agent have been tested. A 90% deashing level with a 94% recovery of the carbonaceous matter has been obtained with a recycling level of about 82% for the agglomerating agent. (J.S.)

  20. Determination of Glycol Ethers in Ambient Air by Adsorption Sampling and Thermal Desorption with GC/MS Analysis: Performance Evaluation and Field Application

    Directory of Open Access Journals (Sweden)

    Young-Kyo Seo

    2012-01-01

    Full Text Available Some of glycol ethers, such as 2-methoxyethanol (2-ME and 2-ethoxyethanol (2-EE are known to be toxic and classified as hazardous air pollutants in USA, Japan and Germany. In Korea, however, there has been no study conducted so far for these compounds in ambient air. In addition, no clear methodologies for the measurement of glycol ethers have been yet established. We carried out this study to evaluate a sampling and analytical method for the determination of glycol ethers, in ambient air samples collected in specific industrial areas of South Korea. To measure glycol ethers, adsorption sampling and thermal desorption with GC/MS analysis were used in this study. The analytical method showed good repeatability, linearity and sensitivity. The lower detection limits were estimated to be approximately 0.3∼0.5 ppb. Based on storage tests, it was suggested that samples should be analyzed within two weeks. It was also demonstrated that this method can be used for the simultaneous measurement of glycol ethers and other aromatic VOCs such as benzene, toluene, and xylenes. Field sampling campaign was carried out at 2 sites, located in a large industrial area, from October 2006 to June 2007, and a total of 480 samples were collected seasonally. Among them, 2-ME was not detected from any samples, while 2-EE and 2-Ethyloxyethylacetate (2-EEA were found in 7 and 70 samples, respectively. The measured concentrations of 2-EE and 2-EEA for samples were ranged from 0.7-2.5 ppb and from 0.5-10.5 ppb, respectively. To our knowledge, this is the first measurement report for glycol ethers in the ambient atmosphere not only in Korea but also the rest of the world.

  1. Au and Al Schottky barrier formation on GaAs (100) surfaces prepared by thermal desorption of a protective arsenic coating

    Energy Technology Data Exchange (ETDEWEB)

    Spindt, C.J.; Yamada, M.; Meissner, P.L.; Miyano, K.E.; Herrera, A.; Spicer, W.E. (Stanford Electronics Laboratories, Stanford University, Stanford, California 94305-4055 (US)); Arko, A.J. (Los Alamos National Laboratory, Los Alamos, New Mexico 87545 (US))

    1991-07-01

    Soft x-ray photoemission spectroscopy has been used to investigate the initial stages of Schottky barrier formation on GaAs (100) surfaces prepared by the thermal desorption of an As cap. This work was motivated by a previous study (Brillson {ital et} {ital al}., J. Vac. Sci. Technol. B {bold 6}, 1263 (1988)) of identically grown and capped samples which reported unpinned'' Schottky barrier formation, with barrier heights falling over a wide range (0.75 eV) of energies. This large energy range is a striking result, as a considerable number of prior studies on both (110) and (100) surfaces have found that all metals will pin in a narrow (0.25 eV) range near midgap. Since Au and Al are the extremes of the larger 0.75 eV span of Schottky barriers, we have studied the deposition of these two metals. We found that the barrier height measurements on the low doped {ital n}-type samples used in this work and in the paper referenced above are affected by photovoltaic effects, even at room temperature. These photovoltaic effects cause shifts in the band bending, which are an artifact of the measurement. We also performed measurements on more heavily doped samples, and the photovoltaic effects were removed. In addition, we point out that Au--Ga alloying makes the case of Au potentially misleading. With the photovoltaic effects removed, and the Au--Ga alloying carefully accounted for, we found that the barriers heights for Au and Al differ by only 0.25 eV.

  2. MOF-5 metal-organic framework as sorbent for in-field sampling and preconcentration in combination with thermal desorption GC/MS for determination of atmospheric formaldehyde.

    Science.gov (United States)

    Gu, Zhi-Yuan; Wang, Gen; Yan, Xiu-Ping

    2010-02-15

    Metal-organic frameworks (MOFs) are one kind of highly porous crystalline materials, which are constructed by metal-containing inorganic nodes and organic linkers. With large surface area and high thermal stability, MOFs have great potential as sorbents for the preconcentration of trace analytes. However, such application of MOFs to the analysis of real samples has not been reported before. Here we report the utilization of MOF-5 as sorbent for in-field sampling and preconcentration of atmospheric formaldehyde before thermal desorption (TD) GC/MS (TD-GC/MS) determination without the need for any chemical derivatization. MOF-5 gave a 53 and 73 times better concentration effect than Tenax TA (organic polymers) and Carbograph 1TD (graphitized carbon black), respectively, for TD-GC/MS determination of formaldehyde. MOF-5 showed good performance for in-field sampling and preconcentration of formaldehyde from air samples with a relative humidity less than 45%. The collected formaldehyde on MOF-5 sorbent was stable for at least 72 h at room temperature before TD-GC/MS analysis. One tube packed with 300 mg of MOF-5 lasted 200 cycles of adsorption/TD without significant loss of collection efficiency. The breakthrough volume of such a tube was 1.2 L of 28.35 mg m(-3) formaldehyde at a sampling flow rate of 100 mL min(-1). The use of MOF-5 for in-field sampling and preconcentration in combination with TD-GC/MS for the determination of formaldehyde offered a linear range covering 3 orders of magnitude, and a detection limit of 0.6 microg m(-3). The precision for six replicate cycles of in-field sampling and preconcentration for TD-GC/MS determination using one 300 mg MOF-5 packed tube ranged from 2.8% to 5.3%. The tube-to-tube reproducibility of three MOF-5 tubes prepared in parallel was 7.7%. The developed method was applied to analysis of local indoor and outdoor air samples for formaldehyde and validated by the standard method TO-11A of the United States Environmental

  3. Influence of Vegetation on the In Situ Bacterial Community and Polycyclic Aromatic Hydrocarbon (PAH) Degraders in Aged PAH-Contaminated or Thermal-Desorption-Treated Soil▿ †

    Science.gov (United States)

    Cébron, Aurélie; Beguiristain, Thierry; Faure, Pierre; Norini, Marie-Paule; Masfaraud, Jean-François; Leyval, Corinne

    2009-01-01

    The polycyclic aromatic hydrocarbon (PAH) contamination, bacterial community, and PAH-degrading bacteria were monitored in aged PAH-contaminated soil (Neuves-Maisons [NM] soil; with a mean of 1,915 mg of 16 PAHs·kg−1 of soil dry weight) and in the same soil previously treated by thermal desorption (TD soil; with a mean of 106 mg of 16 PAHs·kg−1 of soil dry weight). This study was conducted in situ for 2 years using experimental plots of the two soils. NM soil was colonized by spontaneous vegetation (NM-SV), planted with Medicago sativa (NM-Ms), or left as bare soil (NM-BS), and the TD soil was planted with Medicago sativa (TD-Ms). The bacterial community density, structure, and diversity were estimated by real-time PCR quantification of the 16S rRNA gene copy number, temporal thermal gradient gel electrophoresis fingerprinting, and band sequencing, respectively. The density of the bacterial community increased the first year during stabilization of the system and stayed constant in the NM soil, while it continued to increase in the TD soil during the second year. The bacterial community structure diverged among all the plot types after 2 years on site. In the NM-BS plots, the bacterial community was represented mainly by Betaproteobacteria and Gammaproteobacteria. The presence of vegetation (NM-SV and NM-Ms) in the NM soil favored the development of a wider range of bacterial phyla (Alphaproteobacteria, Betaproteobacteria, Gammaproteobacteria, Verrucomicrobia, Actinobacteria, Firmicutes, and Chloroflexi) that, for the most part, were not closely related to known bacterial representatives. Moreover, under the influence of the same plant, the bacterial community that developed in the TD-Ms was represented by different bacterial species (Alphaproteobacteria, Betaproteobacteria, Gammaproteobacteria, and Actinobacteria) than that in the NM-Ms. During the 2 years of monitoring, the PAH concentration did not evolve significantly. The abundance of gram-negative (GN

  4. Extraction of thermal parameters of microbolometer infrared detectors using electrical measurement

    Science.gov (United States)

    Karunasiri, R. P. G.; Xu, Gu; Chen, G. X.; Sridhar, U.

    1998-10-01

    The performance of microbolometer infrared sensors is typically characterized by its thermal time constant, heat capacitance, and thermal conductance. Therefore, the determination of these parameters accurately and efficiently is of considerable interest for the design and operation of microbolometer infrared sensors. Usually, the thermal time constant is obtained by measuring the frequency response of microbolometers under infrared excitation and the thermal conductance and capacity are extracted using electrical measurement. In this paper, a technique is described to extract all three parameters using a single electrical measurement. In the measurement, we have employed a Wheatstone Bridge consisting of a bolometer and three reference resistors. The resistance of the bolometer changes as a result of self-heating under an external bias which in turn generates an output voltage across the Bridge. The time dependence of the output voltage was used to extract thermal parameters of the bolometer. We believe this technique is useful in determining the thermal parameters of microbolometer based sensors.

  5. Green Ocean Amazon (GoAmazon) 2014/15. Semi-Volatile Thermal Desorption Aerosol Gas Chromatograph (SVTAG) Field Campaign Report

    Energy Technology Data Exchange (ETDEWEB)

    Goldstein, A. H. [Univ. of California, Berkeley, CA (United States); Yee, L. D. [Univ. of California, Berkeley, CA (United States); Issacman-VanWertz, G. [Univ. of California, Berkeley, CA (United States); Wernis, R. A. [Univ. of California, Berkeley, CA (United States)

    2016-03-01

    In areas where biogenic emissions are oxidized in the presence of anthropogenic pollutants such as SO2, NOx, and black carbon, it has become increasingly apparent that secondary organic aerosol (SOA) formation from biogenic volatile organic compounds (VOCs) is substantially enhanced. Research is urgently needed to elucidate fundamental processes of natural and anthropogenically influenced VOC oxidation and the contribution of these processes to SOA formation. GoAmazon 2014/15 afforded study of the chemical transformations in the region downwind of Manaus, Brazil, where local biogenic VOC emissions are high, and their chemical oxidation can be studied both inside and outside of the urban plume to differentiate the role of anthropogenic influence on secondary aerosol formation during oxidation of these natural VOC emissions. To understand the connection between primary biogenic VOC emissions and their secondary products that form aerosols, we made time-resolved molecular level measurements by deploying a Semi-Volatile Thermal Desorption Aerosol Gas Chromatograph (SV-TAG) and a sequential filter sampler during two intensive operational periods (IOPs) of the GoAmazon 2014/15 field campaign. The SV-TAG measured semi-volatile organic compounds in both the gas and particle phases and the sequential filter sampler collected aerosols on quartz fiber filters in four-hour increments used for offline analysis. SV-TAG employed novel online derivatization that provided chemical speciation of highly oxygenated or functionalized compounds that comprise a substantial fraction of secondary organic aerosols, yet are poorly characterized. It also provided partitioning of these compounds between the vapor and particle phases at sufficient time resolution to define the importance of competing atmospheric processes. These measurements were supported by offline analysis of the filters using two-dimensional gas chromatography (GC x GC) with high-resolution time-of-flight mass spectrometry

  6. Determination of a wide range of volatile organic compounds in ambient air using multisorbent adsorption/thermal desorption and gas chromatography/mass spectrometry

    Science.gov (United States)

    Pankow, J.F.; Luo, W.; Isabelle, L.M.; Bender, D.A.; Baker, R.J.

    1998-01-01

    Adsorption/thermal desorption with multisorbent air-sampling cartridges was developed for the determination of 87 method analytes including halogenated alkanes, halogenated alkenes, ethers, alcohols, nitriles, esters, ketones, aromatics, a disulfide, and a furan. The volatilities of the compounds ranged from that of dichlorofluoromethane (CFC12) to that of 1,2,3- trichlorobenzene. The eight most volatile compounds were determined using a 1.5-L air sample and a sample cartridge containing 50 mg of Carbotrap B and 280 mg of Carboxen 1000; the remaining 79 compounds were determined using a 5-L air sample and a cartridge containing 180 mg of Carbotrap B and 70 mg of Carboxen 1000. Analysis and detection were by gas chromatography/mass spectrometry. The minimum detectable level (MDL) concentration values ranged from 0.01 parts per billion by volume (ppbv) for chlorobenzene to 0.4 ppbv for bromomethane; most of the MDL values were in the range 0.02-0.06 ppbv. No breakthrough was detected with the prescribed sample volumes. Analyte stability on the cartridges was very good. Excellent recoveries were obtained with independent check standards. Travel spike recoveries ranged from 90 to 110% for 72 of the 87 compounds. The recoveries were less than 70% for bromomethane and chloroethene and for a few compounds such as methyl acetate that are subject to losses by hydrolysis; the lowest travel spike recovery was obtained for bromomethane (62%). Blank values for all compounds were either below detection or very low. Ambient atmospheric sampling was conducted in New Jersey from April to December, 1997. Three sites characterized by low, moderate, and high densities of urbanization/traffic were sampled. The median detected concentrations of the compounds were either similar at all three sites (as with the chlorofluorocarbon compounds) or increased with the density of urbanization/traffic (as with dichloromethane, MTBE, benzene, and toluene). For toluene, the median detected

  7. Thermal Parameter Extraction of a Multilayered System by a Genetic Algorithm

    Science.gov (United States)

    Kuriakose, M.; Depriester, M.; Mascot, M.; Longuemart, S.; Fasquelle, D.; Carru, J. C.; Sahraoui, A. Hadj

    2013-09-01

    Submicron multilayer systems are nowadays used in many common applications such as electronic systems, fuel cells, etc. A knowledge of the layer’s thermal properties are of main interest for thermal management in such systems. Thus, the aim of this study is to investigate thermal parameters of a commercially available multilayered system (Pt-Ti-SiO-Si) using the photothermal radiometry technique. Here, a genetic algorithm is used for extracting thermal parameters of this typical four-layer wafer system. The obtained results can be used as a reference for thermal studies of thin layers coated on the top of such wafers, where they act as a deposition substrate.

  8. Segmentation techniques for extracting humans from thermal images

    CSIR Research Space (South Africa)

    Dickens, JS

    2011-11-01

    Full Text Available A pedestrian detection system for underground mine vehicles is being developed that requires the segmentation of people from thermal images in underground mine tunnels. A number of thresholding techniques are outlined and their performance on a...

  9. The Application of Thermal Plasma to Extraction Metallurgy and Related Fields

    Science.gov (United States)

    Akashi, K.

    1980-01-01

    Various applications of thermal plasma to extraction metallurgy and related fields are surveyed, chiefly on the basis of documents published during the past two or three years. Applications to melting and smelting, to thermal decomposition, to reduction, to manufacturing of inorganic compounds, and to other fields are considered.

  10. Comparing PAH availability from manufactured gas plant soils and sediments with chemical and biological tests. 1. PAH release during water desorption and supercritical carbon dioxide extraction.

    Science.gov (United States)

    Hawthorne, Steven B; Poppendieck, Dustin G; Grabanski, Carol B; Loehr, Raymond C

    2002-11-15

    Soil and sediment samples from oil gas (OG) and coal gas (CG) manufactured gas plant (MGP) sites were selected to represent a range of PAH concentrations (150-40,000 mg/kg) and sample matrix compositions. Samples varied from vegetated soils to lampblack soot and had carbon contents from 3 to 87 wt %. SFE desorption (120 min) and water/XAD2 desorption (120 days) curves were determined and fit with a simple two-site model to determine the rapid-released fraction (F) for PAHs ranging from naphthalene to benzo[ghi]perylene. F values varied greatly among the samples, from ca. 10% to >90% for the two- and three-ring PAHs and from water desorption agreed well (linear correlation coefficient, r2 = 0.87, slope = 0.93), but SFE yielded higher F values for the OG samples. These behaviors were attributed to the stronger ability of carbon dioxide than water to desorb PAHs from the highly aromatic (hard) carbon of the OG matrixes, while carbon dioxide and water showed similar abilities to desorb PAHs from the more polar (soft) carbon of the CG samples. The combined SFE and water desorption approaches should improve the understanding of PAH sequestration and release from contaminated soils and sediments and provide the basis for subsequent studies using the same samples to compare PAH release with PAH availability to earthworms.

  11. Application of hybrid microwave thermal extraction techniques for mulberry root bark

    OpenAIRE

    Wang Cheng-Chi; Yau Her-Terng

    2013-01-01

    The main focus of this paper is the extraction of compounds from the mulberry root bark using a hybrid microwave thermal process. The shearing mechanism and an integrated circulation system, which increases the rate of contact between the solvent and extractive, are studied. The results are analyzed by the Taguchi method and verified by high performance liquid chromatography. Furthermore, the optimal operating parameters of the extraction of mulberry root b...

  12. Continuous soil VOCl measurements with automated flux chambers and micro-ECD gas chromatography coupled with the thermal desorption and cooled injection systems

    Science.gov (United States)

    Molodovskaya, M. S.; Svensson, T.; Pitts, A.; Delmonte, J.; Nesic, Z.; Oberg, G.

    2010-12-01

    automated chamber was continuously pumped through the glass tubes filled with carbon-based absorbent (Carbotrap 300) to capture and retain VOCl. At the end of each measurement period, the tubes are brought back to the lab, and the content is analyzed by Agilent 7890 GC/micro-ECD coupled with the Gerstel Thermal Desorption System (TDS) and Cooled Injection System (CIS). The ultra sensitive micro-ECD detection and high-efficiency capillary column (Rtx®-VMS, 20m x 0.18mm ID x 1.0µm) allows rapid separation and quantification of the mid-weight VOCl such as chloroform, carbon tetrachloride, 1,1,1-trichloroethane and bromochloromethane. The GC-method dynamic range is linear within 0.1-200.0ng, and the analytical precision is determined to be 4%. The described system can be used for the analysis of soil/atmosphere exchange of VOCl at the detection limit of 1.9ng m-2 h-1, which is far below previously reported average soil emission levels from forest soils. The high precision GC analysis combined with the automatic chambers makes it possible to study the high spatial and temporal variability of soil VOCl fluxes.

  13. First field application of a thermal desorption resonance-enhanced multiphoton-ionisation single particle time-of-flight mass spectrometer for the on-line detection of particle-bound polycyclic aromatic hydrocarbons.

    Science.gov (United States)

    Oster, Markus; Elsasser, Michael; Schnelle-Kreis, Jürgen; Zimmermann, Ralf

    2011-12-01

    The on-line analysis of single aerosol particles with mass spectrometrical methods is an important tool for the investigation of aerosols. Often, a single laser pulse is used for one-step laser desorption/ionisation of aerosol particles. Resulting ions are detected with time-of-flight mass spectrometry. With this method, the detection of inorganic compounds is possible. The detection of more fragile organic compounds and carbon clusters can be accomplished by separating the desorption and the ionisation in two steps, e.g. by using two laser pulses. A further method is, using a heated metal surface for thermal desorption of aerosol particles. If an ultraviolet laser is used for ionisation, a selective ionisation of polycyclic aromatic hydrocarbons (PAH) and alkylated PAH is possible via a resonance-enhanced multiphoton-ionisation process. Laser velocimetry allows individual laser triggering for single particles and additionally delivers information on aerodynamic particle diameters. It was shown that particles deriving from different combustion sources can be differentiated according to their PAH patterns. For example, retene, a C(4)-alkylated phenanthrene derivative, is a marker for the combustion of coniferous wood. In this paper, the first field application of a thermal desorption resonance-enhanced multiphoton-ionisation single particle time-of-flight mass spectrometer during a measurement campaign in Augsburg, Germany in winter 2010 is presented. Larger PAH-containing particles (i.e. with aerodynamic diameters larger than 1 μm), which are suspected to be originated by re-suspension processes of agglomerated material, were in the focus of the investigation. Due to the low concentration of these particles, an on-line virtual impactor enrichment system was used. The detection of particle-bound PAH in ambient particles in this larger size region was possible and in addition, retene could be detected on several particles, which allows to identify wood combustion as

  14. Protective coatings preventing hydrogen desorption from titanium during ion irradiation

    Science.gov (United States)

    Evsin, A. E.; Begrambekov, L. B.; Dovganyuk, S. S.; Kaplevsky, A. S.; Shutikova, M. I.

    2017-05-01

    Effect of yttria and titanium nitride coatings on features of deuterium desorption from titanium layer is investigated. It is shown that both coatings significantly raise the temperature of maximum of deuterium thermal desorption from titanium under linear heating and prevent desorption under prolonged keeping at the operating temperature of a neutron tube target. However, under irradiation with ions of H2 + O2 plasma the barrier properties of titanium nitride appear to degrade.

  15. Thermal stability of anthocyanin extract of Hibiscus sabdariffa L. in the presence of beta-cyclodextrin.

    Science.gov (United States)

    Mourtzinos, Ioannis; Makris, Dimitris P; Yannakopoulou, Konstantina; Kalogeropoulos, Nick; Michali, Iliana; Karathanos, Vaios T

    2008-11-12

    The thermal stability of anthocyanin extract isolated from the dry calyces of Hibiscus sabdariffa L. was studied over the temperature range 60-90 degrees C in aqueous solutions in the presence or absence of beta-cyclodextrin (beta-CD). The results indicated that the thermal degradation of anthocyanins followed first-order reaction kinetics. The temperature-dependent degradation was adequately modeled by the Arrhenius equation, and the activation energy for the degradation of H. sabdariffa L. anthocyanins during heating was found to be approximately 54 kJ/mol. In the presence of beta-CD, anthocyanins degraded at a decreased rate, evidently due to their complexation with beta-CD, having the same activation energy. The formation of complexes in solution was confirmed by nuclear magnetic resonance studies of beta-CD solutions in the presence of the extract. Moreover, differential scanning calorimetry revealed that the inclusion complex of H. sabdariffa L. extract with beta-CD in the solid state was more stable against oxidation as compared to the free extract, as the complex remained intact at temperatures 100-250 degrees C where the free extract was oxidized. The results obtained clearly indicated that the presence of beta-CD improved the thermal stability of nutraceutical antioxidants present in H. sabdariffa L. extract, both in solution and in solid state.

  16. Desorption of 137Cs+ from mosses

    Directory of Open Access Journals (Sweden)

    OLGICA NEDIC

    2002-09-01

    Full Text Available Mosses are biomonitors that accumulate large amounts of various pollutants, including radionuclides. In this work we investigated the possibility of 137Cs extraction from mosses, as well as the significance of species specificity on the efficiency of 137Cs desorption. Salt and acid solutions were used as extraction media. It was shown that a 5 % solution of both ammonium oxalate and phosphoric acid was able to desorb 81.8 % of 137Cs+ from Homalothecium sericeum, which was 39.9 % more than desorption from water. At the same time, most of the desorbed 137Cs+ was incorporated in crystals that precipitated from the solution. An interspecies difference in respect to 137Cs+ desorption was noticed.

  17. Graphene/TiO2 nanocomposite based solid-phase extraction and matrix-assisted laser desorption/ionization time-of-flight mass spectrometry for lipidomic profiling of avocado (Persea americana Mill.).

    Science.gov (United States)

    Shen, Qing; Yang, Mei; Li, Linqiu; Cheung, Hon-Yeung

    2014-12-10

    Phospholipids possess important physiological, structural and nutritional functions in biological systems. This study described a solid-phase extraction (SPE) method, employing graphene and titanium dioxide (G/TiO2) nanocomposite as sorbent, for the selective isolation and enrichment of phospholipids from avocado (Persea americana Mill.). Based on the principal that the phosphoryl group in the phospholipid can interact with TiO2 via a bridging bidentate mode, an optimum condition was established for SPE, and was successfully applied to prepare avocado samples. The extracts were monitored by matrix-assisted laser desorption ionization time-of-flight/tandem mass spectrometry (MALDI-TOF/MS) in both positive-ion and negative-ion modes. Results showed that phospholipids could be efficiently extracted in a clean manner by G/TiO2 based SPE. In addition, the signals of phospholipids were enhanced while the noise was reduced. Some minor peaks became more obvious. In conclusion, the nanocomposite material of G/TiO2 was proved to be a promising sorbent for selective separation of phospholipids from crude lipid extract.

  18. Transformation and removal of wood extractives from pulp mill sludge using wet oxidation and thermal hydrolysis.

    Science.gov (United States)

    Baroutian, Saeid; Robinson, Murray; Smit, Anne-Marie; Wijeyekoon, Suren; Gapes, Daniel

    2013-10-01

    In order to remove wood extractive compounds from pulp mill sludge and thereby enhancing anaerobic digestibility, samples were subjected to either oxidative hydrothermal treatment (wet oxidation) or non-oxidative hydrothermal treatment (thermal hydrolysis). Treatments were carried out at 220 °C with initial pressure of 20 bar. More than 90% destruction of extractive compounds was observed after 20 min of wet oxidation. Wet oxidation eliminated 95.7% of phenolics, 98.6% fatty acids, 99.8% resin acids and 100% of phytosterols in 120 min. Acetic acid concentration increased by approximately 2 g/l after 120 min of wet oxidation. This has potential for rendering sludge more amenable to anaerobic digestion. In contrast thermal hydrolysis was found to be ineffective in degrading extractive compounds. Wet oxidation is considered to be an effective process for removal of recalcitrant and inhibitive compounds through hydrothermal pre-treatment of pulp mill sludge.

  19. Thermal Properties of Simulated and High-Level Waste Solutions Used for the Solvent Extraction Demonstration

    Energy Technology Data Exchange (ETDEWEB)

    Fondeur, F.F.

    2001-06-27

    Researchers measured the heat capacity and thermal conductivity of supernate from a blend of Tank 37H and 44F, of a simulant of this blend, and of a simulant specifically designed for solvent extraction experiments. The measured heat capacity of the blend from the Tanks 37H and 44F equaled 0.871 cal/(g degrees C). The simulant of this blend produced an identical result. The heat capacity of the simulant designed for solvent extraction testing equaled 0.859 cal/(g degrees C). All three solutions have thermal conductivities in the range of 0.54 to 0.6 Watts/(m degrees C). The slight variation in the thermophysical properties of these solutions successfully explains the different flowmeter readings observed during the real waste demonstration of the solvent extraction technology.

  20. Determination of phosphine and other fumigants in air samples by thermal desorption and 2D heart-cutting gas chromatography with synchronous SIM/Scan mass spectrometry and flame photometric detection.

    Science.gov (United States)

    Fahrenholtz, Svea; Hühnerfuss, Heinrich; Baur, Xaver; Budnik, Lygia Therese

    2010-12-24

    Fumigants and volatile industrial chemicals are particularly hazardous to health when a freight container is fumigated or the contaminated material is introduced into its enclosed environment. Phosphine is now increasingly used as a fumigant, after bromomethane--the former fumigant of choice--has been banned by the Montreal Protocol. We have enhanced our previously established thermal desorption-gas chromatography-mass spectrometry (TD-GC-MS) method by integrating a second gas chromatographic dimension and a flame photometric detector to allow the simultaneous detection of phosphine and volatile organic compounds (VOCs), providing a novel application. A thermal desorption system is coupled to a two dimensional gas chromatograph using both mass spectrometric and flame photometric detection (TD-2D-GC-MS/FPD). Additionally, the collection of mass spectrometric SIM and Scan data has been synchronised, so only a single analysis is now sufficient for qualitative scanning of the whole sample and for sensitive quantification. Though detection limits for the herewith described method are slightly higher than in the previous method, they are in the low μL m(-3) range, which is not only below the respective occupational exposure and intervention limits but also allows the detection of residual contamination after ventilation. The method was developed for the separation and identification of 44 volatile substances. For 12 of these compounds (bromomethane, iodomethane, dichloromethane, 1,2-dichlorethane, benzene, tetrachloromethane, 1,2-dichloropropane, toluene, trichloronitromethane, ethyl benzene, phosphine, carbon disulfide) the method was validated as we chose the target compounds due to their relevance in freight container handling.

  1. Thermal desorption-multiphoton ionization time-of-flight mass spectrometry of individual aerosol particles: a simplified approach for online single-particle analysis of polycyclic aromatic hydrocarbons and their derivatives.

    Science.gov (United States)

    Bente, Matthias; Sklorz, Martin; Streibel, Thorsten; Zimmermann, Ralf

    2009-04-01

    Online single-particle (SP) laser mass spectrometry (MS) is an important tool for fundamental and applied aerosol research. Usually laser desorption/ionization (LDI) is applied for ablation and ionization of atoms and molecular fragments from the nanometer- or micrometer-sized air-borne particles and time-of-flight analysers (TOFMS) are used for mass-selective detection of mainly inorganic analytes. The detection of molecular organic compounds is solely possible under very special experimental conditions and extremely dependent on the particle matrix and thus limited to special applications. Very recently it was shown that by implementation of a two-step laser desorption (LD) resonance-enhanced multiphoton ionization (REMPI) postionization approach the single-particulate molecular signature of polycyclic aromatic hydrocarbons (PAH) and their derivatives can be recorded (LD-REMPI-SP-TOFMS). By this, particles from different sources could be differentiated via the patterns of specific molecular source tracers such as retene for soft wood combustion or larger PAH as indicator for gasoline car emissions. One drawback of the LD-REMPI-SP-TOFMS method in particular for field applications is, however, the necessity of operation and adjustment of two lasers. In this paper the successful implementation of a thermal desorption step in single-particle mass spectrometry is described (TD-REMPI-SP-TOFMS). After size determination by particle velocimetry, individual particles are thermally desorbed on a heated surface in the ion source of the TOFMS. Desorbed molecules are ionized subsequently by REMPI, which addresses selectively PAH and molecular trace indicators. The TD-REMPI-SP-TOFMS concept was tested with reference particles and applied for automotive exhaust and ambient monitoring. The comparison of the results with the ones obtained by the two-laser approach (LD-REMPI-SP-TOFMS) indicates that the patented TD-REMPI-SP-TOFMS technology presented here is nearly equally well

  2. A microwave-mediated saponification of galactosylceramide and galactosylceramide I3-sulfate and identification of their lyso-compounds by delayed extraction matrix-assisted laser desorption ionization time-of-flight mass spectrometry.

    Science.gov (United States)

    Taketomi, T; Hara, A; Uemura, K; Kurahashi, H; Sugiyama, E

    1996-07-16

    Small amounts of galactosylceramide (cerebroside) and galactosylceramide I3-sulfate (sulfatide) obtained from porcine spinal cord and equine kidney were deacylated by a rapid method of microwave-mediated saponification to prepare their lyso-compounds. Mass spectra of their protonated or deprotonated molecular ion peaks were detected by recently developed new technology of a delayed extraction matrix-assisted laser desorption ionization time-of-flight mass spectrometer with reflector detector in positive or negative ion mode. Long chain bases of lysocerebroside and lysosulfatide were different between porcine spinal cord and equine kidney, but similar to each other in the same organ, suggesting their common synthetic pathway. It is noted that the new rapid method can be similarly applied to the deacylation of both cerebroside and sulfatide in contrast to our classical method which was able to be applied to cerebroside, but not to sulfatide.

  3. Analysis of Volatile Components of Fresh and Cooked Frankincense by Thermal Desorption and GC/MS%热脱附-气相色谱/质谱联用法分析生、炙乳香挥发性成分

    Institute of Scientific and Technical Information of China (English)

    吴岳华; 周围; 张雅珩; 魏荣霞

    2013-01-01

    为了研究天然乳香的挥发性成分及生、炙乳香挥发性成分的异同,为乳香挥发油的工艺优化和品质评估提供科学的依据,同时为固体挥发性成分分析提供新思路,采用热脱附-气相色谱/质谱联用技术直接对自然状态下乳香颗粒的挥发性成分进行分析.结合NIST 08标准谱库检索和Mass WorksTM质谱解析软件的分析结果,在分离出的40余种挥发性成分中,最终确定出20种化学成分.结果表明:生、炙乳香中的挥发性成分主要由单萜、醇及酯类物质构成,其中以醋酸辛酯含量最高,约占挥发性成分的50%;其次为1-辛醇、芳樟醇、乙酸龙脑酯,在生乳香中的含量分别为19.44%、2.27%、2.64%,在炙乳香中的含量分别为9.12%、2.61%、1.33%.%In order to make clear the natural volatile composition of frankincense and the differences between fresh frankincense and cooked frankincense, to provide a scientific basis on improving techniques and evaluating qualities of frankincense volatile oil, and to offer a new method to analyse volatile composition from solid for reference, the volatile components of natural fresh and cooked frankincense were extracted and determined directly by thermal desorption and gas chromatography-mass spectrornetry(GC/MS). More than 40 components are separated and 20 components are identified by comparing their mass spectra with those contained in the NIST mass spectral database and Mass Works?software. The results show that the main components includ terpenes, alcohol and esters et al,n-octyl acetate is the most important volatile components to frankincense. The normalized peak areas exceed 50% both in fresh frankincense and cooked frankincense,followed by 1-octanol, lina-lool and bornyl acetate, the normalized peak areas in fresh frankincense are 19. 44%, 2. 27% and 2. 64%, in cooked frankincense are 9. 12%, 2. 61% and 1. 33%, respectively.

  4. Inhibition of thermal induced protein denaturation of extract/fractions of Withania somnifera and isolated withanolides.

    Science.gov (United States)

    Khan, Murad Ali; Khan, Haroon; Rauf, Abdul; Ben Hadda, Taibi

    2015-01-01

    This study describes the in vitro inhibition of protein denaturation of extract/fractions of Withania somnifera and isolated withanolides including 20β hydroxy-1-oxo(22R)-witha-2,5,24 trienolide (1), (20R,22R-14α,20α)-dihydroxy-1-oxowitha-2,5,16,24 tetraenolide (2). The results showed that the extract/fractions of the plant evoked profound inhibitory effect on thermal-induced protein denaturation. The chloroform fraction caused the most dominant attenuation of 68% at 500 μg/mL. The bioactivity-guided isolation from chloroform fraction led to the isolation of compounds 1 and 2 that showed profound protein inhibition with 78.05% and 80.43% effect at 500 μg/mL and thus strongly complimented the activity of extract/fractions. In conclusion, extract/fractions of W. somnifera possessed strong inhibition of protein denaturation that can be attributed to these isolated withanolides.

  5. Pressurized liquid extraction of Aglaonema sp. iminosugars: Chemical composition, bioactivity, cell viability and thermal stability.

    Science.gov (United States)

    Rodríguez-Sánchez, S; Martín-Ortiz, A; Carrero-Carralero, C; Ramos, S; Sanz, M L; Soria, A C

    2016-08-01

    Pressurized liquid extraction of Aglaonema sp. iminosugars has been optimized. A single cycle under optimal conditions (80mg, 100°C, 2min) was enough to extract ⩾96% of most iminosugars. Further incubation with Saccharomyces cerevisiae for 5h removed coextracted interfering low molecular weight carbohydrates from extracts of different Aglaonema cultivars. A complete characterization of these extracts was carried out by gas chromatography-mass spectrometry: three iminosugars were tentatively identified for the first time; α-homonojirimycin and 2,5-dideoxy-2,5-imino-d-mannitol were the major iminosugars determined. α-Glucosidase inhibition activity, cell viability and thermal stability of Aglaonema extracts were also evaluated. Extracts with IC50 for α-glucosidase activity in the 0.010-0.079mgmL(-1) range showed no decrease of Caco-2 cell viability at concentrations lower than 125μgmL(-1) and were stable at 50°C for 30days. These results highlight the potential of Aglaonema extracts as a source of bioactives to be used as functional ingredients.

  6. Determination of trichloromethane in workplace air by thermal desorption-gas chromatography%工作场所空气中三氯甲烷的热脱附气相色谱联用测定法

    Institute of Scientific and Technical Information of China (English)

    刘浏; 胡晓宇; 庞平; 傅佳; 钟磊

    2013-01-01

    To establish a method for determination of trichloromethane in workplace air by thermal desorption-gas chromatography.[Methods] The trichloromethane samples were collected from workplace air by Air Toxics adsorption tube,injection was conducted after desorption with Pekin Elmer Tubo Matrix AFD 650 thermal desorption instrument,and detection was performed by flame ionization detector.The retention time was adopted in qualitative analysis,and peak area was applied in quantitative evaluation.The laboratory examination and simulate experiments were conducted according to the Determination methods of air chemicals in workplace.[Results] The standard curve was linear in the content ranges of 0-300 μl,and the regression equation was Y =16.6 X + 2.8,r =1.000.The detection limit was 0.88 μg.The minimum detectable concentration was 0.20 mg/m3 while the sampling volume was 4.5 L.The repeatability was good,the relative standard deviation (RSD) was 3.14%-6.15%,the desorption efficiency was 103.0%-83.7%,and the sampling efficiency was 100%.The samples could be stably stored for 3 days in Air Toxics adsorption tube.[Conclusion] The method is simple and rapid,with high sensitivity,which is suitable for determination of trichloromethane in workplace air.%目的 建立测定工作场所空气中三氯甲烷的热脱附-气相色谱联用检测方法.方法 工作场所空气中的三氯甲烷用Air Toxics吸附管采样,用Pekin Elmer Tubo Matrix ATD-650热脱附仪脱附后进样,经毛细管色谱柱分离,氢火焰离子化检测器检测,以保留时间定性,峰面积定量.方法研究按照《工作场所空气中化学物质测定方法》的要求进行实验室实验及模拟现场实验.结果 该方法在0 ~ 300μl范围内呈线性关系,峰面积与含量的回归方程为Y=16.6X +2.8;r=1.000;检出限为0.88μg,当采样体积为4.5L时最低检出浓度为0.20 mg/m3;方法的重现性较好,不同浓度的相对标准偏差为3.14% ~6,15

  7. THERMAL AND THERMODYNAMIC CHARACTERIZATION OF A DYE POWDER FROM LIQUID TURMERIC EXTRACTS BY SPRAY DRYING

    Directory of Open Access Journals (Sweden)

    Aura Yazmin Coronel Delgado

    2016-01-01

    Full Text Available This study aimed to evaluate the thermodynamic properties of sorption isotherms and glass transition temperature (Tg and the thermal properties of a dye powder obtained from turmeric extracts using spray drying. The sorption isotherms were evaluated at 15, 25 and 35 ºC using the dynamic gravimetric method, wherein the isotherm data of the experiment were fit to GAB and BET models. Likewise, the Tg was measured using differential scanning calorimetry (DSC. Thermogravimetric analysis (TGA was used to determine the mass loss, and the thermal properties (heat capacity, diffusivity and thermal conductivity were determined using transient flow method. The results demonstrated that the GAB model best fit the adsorption data. The DSC analysis presented a glass transition temperature of 65.35 ºC and a loss of volatiles at 178.07 ºC. The TGA analysis indicated a considerable mass loss starting at 193 ºC, resulting in degradation of the product. The thermal properties demonstrated a heat capacity of 2.45 J/g ºC, a thermal conductivity of 0.164 ±0.001 W/mK and a thermal diffusivity of 8.7x10-8 ± 0.000 m2/s

  8. 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.

  9. Experimental DC extraction of the thermal resistance of bipolar transistors taking into account the Early effect

    Science.gov (United States)

    d'Alessandro, Vincenzo

    2017-01-01

    This paper presents three methods to experimentally extract the thermal resistance of bipolar transistors taking into account the Early effect. The approaches are improved variants of recently-proposed techniques relying on common-base DC measurements. The accuracy is numerically verified by making use of a compact model calibrated on I-V characteristics of state-of-the-art SOG BJTs and SiGe:C HBTs.

  10. Fatty acid profiling of raw human plasma and whole blood using direct thermal desorption combined with gas chromatography-mass spectrometry

    NARCIS (Netherlands)

    Akoto, Lawrence; Vreuls, Rene J. J.; Irth, Hubertus; Pel, Roel; Stellaard, Frans

    2008-01-01

    Gas chromatography (GC) has in recent times become an important tool for the fatty acid profiling of human blood and plasma. An at-line procedure used in the fatty acid profiling of whole/intact aquatic micro-organisms without any sample preparation was adapted for this work. A direct thermal

  11. Fatty acid profiling of raw human plasma and whole blood using direct thermal desorption combined with gas chromatography–mass spectrometry

    NARCIS (Netherlands)

    Akoto, L.; Vreuls, R.J.J.; Irth, H.; Pel, R.; Stellaard, F.

    2008-01-01

    Gas chromatography (GC) has in recent times become an important tool for the fatty acid profiling of human blood and plasma. An at-line procedure used in the fatty acid profiling of whole/intact aquatic micro-organisms without any sample preparation was adapted for this work. A direct thermal

  12. Coal liquefaction process streams characterization and evaluation. Characterization of coal-derived materials by field desorption mass spectrometry, two-dimensional nuclear magnetic resonance, supercritical fluid extraction, and supercritical fluid chromatography/mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Campbell, J.A.; Linehan, J.C.; Robins, W.H. [Battelle Pacific Northwest Lab., Richland, WA (United States)

    1992-07-01

    Under contract from the DOE , and in association with CONSOL Inc., Battelle, Pacific Northwest Laboratory (PNL) evaluated four principal and several complementary techniques for the analysis of non-distillable direct coal liquefaction materials in support of process development. Field desorption mass spectrometry (FDMS) and nuclear magnetic resonance (NMR) spectroscopic methods were examined for potential usefulness as techniques to elucidate the chemical structure of residual (nondistillable) direct coal liquefaction derived materials. Supercritical fluid extraction (SFE) and supercritical fluid chromatography/mass spectrometry (SFC/MS) were evaluated for effectiveness in compound-class separation and identification of residual materials. Liquid chromatography (including microcolumn) separation techniques, gas chromatography/mass spectrometry (GC/MS), mass spectrometry/mass spectrometry (MS/MS), and GC/Fourier transform infrared (FTIR) spectroscopy methods were applied to supercritical fluid extracts. The full report authored by the PNL researchers is presented here. The following assessment briefly highlights the major findings of the project, and evaluates the potential of the methods for application to coal liquefaction materials. These results will be incorporated by CONSOL into a general overview of the application of novel analytical techniques to coal-derived materials at the conclusion of CONSOL`s contract.

  13. APPLICATION OF ULTRASOUND THERMAL PROCESS ON EXTRACTING FLAVOR AND CAFFEINE OF COFFEE

    Directory of Open Access Journals (Sweden)

    Cheng-Chi Wang

    2011-01-01

    Full Text Available In this research, our focus is the use of ultrasound thermal process to extract flavor and caffeine from coffee. The different operating conditions for extraction experiments are executed and the results are also compared. The results show that coffee flavor is not enhanced with the increase of temperature because the volatile degree of coffee flavor components is quick and easy to be reached at high temperatures. From the experimental results, it can be found that using low vibration frequency is better than using high vibration frequency. Also, caffeine will be reached into the saturated state at the 15th second of the extracting time and the quantity of caffeine augments with the increase of temperature.

  14. A comparison of techniques for extracting emissivity information from thermal infrared data for geologic studies

    Science.gov (United States)

    Hook, Simon J.; Gabell, A. R.; Green, A. A.; Kealy, P. S.

    1992-01-01

    This article evaluates three techniques developed to extract emissivity information from multispectral thermal infrared data. The techniques are the assumed Channel 6 emittance model, thermal log residuals, and alpha residuals. These techniques were applied to calibrated, atmospherically corrected thermal infrared multispectral scanner (TIMS) data acquired over Cuprite, Nevada in September 1990. Results indicate that the two new techniques (thermal log residuals and alpha residuals) provide two distinct advantages over the assumed Channel 6 emittance model. First, they permit emissivity information to be derived from all six TIMS channels. The assumed Channel 6 emittance model only permits emissivity values to be derived from five of the six TIMS channels. Second, both techniques are less susceptible to noise than the assumed Channel 6 emittance model. The disadvantage of both techniques is that laboratory data must be converted to thermal log residuals or alpha residuals to facilitate comparison with similarly processed image data. An additional advantage of the alpha residual technique is that the processed data are scene-independent unlike those obtained with the other techniques.

  15. Desorption of Lipases Immobilized on Octyl-Agarose Beads and Coated with Ionic Polymers after Thermal Inactivation. Stronger Adsorption of Polymers/Unfolded Protein Composites

    Directory of Open Access Journals (Sweden)

    Jose J. Virgen-Ortíz

    2017-01-01

    Full Text Available Lipases from Candida antarctica (isoform B and Rhizomucor miehei (CALB and RML have been immobilized on octyl-agarose (OC and further coated with polyethylenimine (PEI and dextran sulfate (DS. The enzymes just immobilized on OC supports could be easily released from the support using 2% SDS at pH 7, both intact or after thermal inactivation (in fact, after inactivation most enzyme molecules were already desorbed. The coating with PEI and DS greatly reduced the enzyme release during thermal inactivation and improved enzyme stability. However, using OC-CALB/RML-PEI-DS, the full release of the immobilized enzyme to reuse the support required more drastic conditions: a pH value of 3, a buffer concentration over 2 M, and temperatures above 45 °C. However, even these conditions were not able to fully release the thermally inactivated enzyme molecules from the support, being necessary to increase the buffer concentration to 4 M sodium phosphate and decrease the pH to 2.5. The formation of unfolded protein/polymers composites seems to be responsible for this strong interaction between the octyl and some anionic groups of OC supports. The support could be reused five cycles using these conditions with similar loading capacity of the support and stability of the immobilized enzyme.

  16. Effects of soil particle size and organic matter content on thermal desorption of polybrominated diphenyl ether%土壤粒径及有机质对多溴二苯醚热脱附的影响

    Institute of Scientific and Technical Information of China (English)

    傅海辉; 黄启飞; 朱晓华; 何洁; 唐振武; 孟昭福

    2013-01-01

    Under laboratory conditions,the two effect factors of soil particle size and organic matter content were studied in order to give the theory basis PBDEs of thermal desorption from contaminated soils.The results showed that the removal rates of PBDEs from different particle sizes of soils(75,75 ~ 125,125 ~ 250,250 ~425 and 425 ~ 850 μm) contaminated by PBDEs were 49.53%,73.88%,79.39%,83.56%,87.09%,respectively.The total removal rate of PBDEs increased with the particle size increasing,and BDE209 was removed more easily than BDE206,BDE207 and BDE208 from soils.In addition,the PBDEs removal rate from the soil oxidated with H2O2 was higher than that from the original soil with the same PBDEs concentration below 450℃,which showed that soil organic matter may inhibit the thermal desorption of PBDEs.%在实验室条件下,研究了土壤粒径与土壤有机质含量对多溴二苯醚(PBDEs)热脱附的影响,以期为PBDEs污染土壤热脱附修复提供理论依据.实验结果表明,300℃停留30 min条件下,粒径为<75、75~ 125、125~250、250 ~425和425~ 850 μm的土壤中PBDEs去除率分别为49.53%、73.88%、79.39%、83.56%和87.09%,PBDEs总去除率随粒径的增大而增大,土壤BDE209较BDE206、BDE207和BDE208更易于脱除.此外,温度低于450℃时,H2O2氧化部分去除有机质后土壤中PBDEs的去除率较原土高;表明,土壤有机质可能抑制土壤中PBDEs的热脱附.

  17. Studies on extracting solutions of endohedral rare-earth metallofullerenes by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    孙大勇; 刘志强; 刘子阳; 郭兴华; 徐文国; 刘淑莹

    1997-01-01

    Thirteen extracting solutions of rare-earth metallofullerenes containing La,Ce,Pr,Nd Sm,Eu,Gd,Tb,Dy,Ho,Er,Tm and Yb respectively have been investigated by means of matrix-assisted laser desorpuon/ ionization time-of-flight mass spectrometry.The influences of the positive-ion/negative-ion mode,laser intensity,ma trix and mass discrimination to the analytical results are studied,based on which the optimal analytical conditions have been determined.The results show that the extracting solutions contain large quantities of rare-earth metallofullerenes besides empty fullerenes.On the basis of comparing their relative intensities,the different structure stabilities and solubilities of metallofullerenes with different rare-earth metals encapsulated into the fullerene cages,as well as some possible reasons to those differences,are discussed.

  18. Method development towards qualitative and semi-quantitative analysis of multiple pesticides from food surfaces and extracts by desorption electrospray ionization mass spectrometry as a preselective tool for food control.

    Science.gov (United States)

    Gerbig, Stefanie; Stern, Gerold; Brunn, Hubertus E; Düring, Rolf-Alexander; Spengler, Bernhard; Schulz, Sabine

    2017-03-01

    Direct analysis of fruit and vegetable surfaces is an important tool for in situ detection of food contaminants such as pesticides. We tested three different ways to prepare samples for the qualitative desorption electrospray ionization mass spectrometry (DESI-MS) analysis of 32 pesticides found on nine authentic fruits collected from food control. Best recovery rates for topically applied pesticides (88%) were found by analyzing the surface of a glass slide which had been rubbed against the surface of the food. Pesticide concentration in all samples was at or below the maximum residue level allowed. In addition to the high sensitivity of the method for qualitative analysis, quantitative or, at least, semi-quantitative information is needed in food control. We developed a DESI-MS method for the simultaneous determination of linear calibration curves of multiple pesticides of the same chemical class using normalization to one internal standard (ISTD). The method was first optimized for food extracts and subsequently evaluated for the quantification of pesticides in three authentic food extracts. Next, pesticides and the ISTD were applied directly onto food surfaces, and the corresponding calibration curves were obtained. The determination of linear calibration curves was still feasible, as demonstrated for three different food surfaces. This proof-of-principle method was used to simultaneously quantify two pesticides on an authentic sample, showing that the method developed could serve as a fast and simple preselective tool for disclosure of pesticide regulation violations. Graphical Abstract Multiple pesticide residues were detected and quantified in-situ from an authentic set of food items and extracts in a proof of principle study.

  19. A novel quantitation approach for maximizing detectable targets for offensive/volatile odorants with diverse functional groups by thermal desorption-gas chromatography-mass spectrometry

    Science.gov (United States)

    Kim, Yong-Hyun; Kim, Ki-Hyun

    2016-07-01

    A multitude of analytical systems are needed to analyze diverse odorants with various functionalities. In this study, an experimental method was developed to assess the maximum covering range of odorants using a single experimental setup consisting of a thermal desorber-gas chromatography-mass spectrometry system. To this end, a total of 20 offensive odorants (aldehyde, ketone, ester, alcohol, aromatic, sulfide, amine, and carboxyl) were selected and tested by a single system. The analytical results of standards and environmental samples were evaluated in a number of respects. In the analysis of the standards, all targets were quantified via Carbopack (C + B + X) tube sampling while operating the thermal desorber at -25 °C. The method detection limits of 18 targets (exception of 2 out of the 20 targets: acetaldehyde and methanethiol) were excellent (mean 0.04 ± 0.03 ppb) in terms of their odor threshold values (74.7 ± 140 ~ 624 ± 1,729 ppb). The analysis of organic fertilizer plant samples at a pig farm (slurry treatment facility, compost facility, and ambient air) confirmed the presence of 18 odorants from 0.03 ppb (dimethyldisulfide, ambient sample) to 522 ppb (methyl ethyl ketone, slurry treatment facility). As such, our method allowed simultaneous quantitation of most key odorants with sufficient reliability and sensitivity.

  20. A novel quantitation approach for maximizing detectable targets for offensive/volatile odorants with diverse functional groups by thermal desorption-gas chromatography-mass spectrometry.

    Science.gov (United States)

    Kim, Yong-Hyun; Kim, Ki-Hyun

    2016-07-11

    A multitude of analytical systems are needed to analyze diverse odorants with various functionalities. In this study, an experimental method was developed to assess the maximum covering range of odorants using a single experimental setup consisting of a thermal desorber-gas chromatography-mass spectrometry system. To this end, a total of 20 offensive odorants (aldehyde, ketone, ester, alcohol, aromatic, sulfide, amine, and carboxyl) were selected and tested by a single system. The analytical results of standards and environmental samples were evaluated in a number of respects. In the analysis of the standards, all targets were quantified via Carbopack (C + B + X) tube sampling while operating the thermal desorber at -25 °C. The method detection limits of 18 targets (exception of 2 out of the 20 targets: acetaldehyde and methanethiol) were excellent (mean 0.04 ± 0.03 ppb) in terms of their odor threshold values (74.7 ± 140 ~ 624 ± 1,729 ppb). The analysis of organic fertilizer plant samples at a pig farm (slurry treatment facility, compost facility, and ambient air) confirmed the presence of 18 odorants from 0.03 ppb (dimethyldisulfide, ambient sample) to 522 ppb (methyl ethyl ketone, slurry treatment facility). As such, our method allowed simultaneous quantitation of most key odorants with sufficient reliability and sensitivity.

  1. Fast and solvent-free quantitation of boar taint odorants in pig fat by stable isotope dilution analysis-dynamic headspace-thermal desorption-gas chromatography/time-of-flight mass spectrometry.

    Science.gov (United States)

    Fischer, Jochen; Haas, Torsten; Leppert, Jan; Lammers, Peter Schulze; Horner, Gerhard; Wüst, Matthias; Boeker, Peter

    2014-09-01

    Boar taint is a specific off-odour of boar meat products, known to be caused by at least three unpleasant odorants, with very low odour thresholds. Androstenone is a boar pheromone produced in the testes, whereas skatole and indole originate from the microbial breakdown of tryptophan in the intestinal tract. A new procedure, applying stable isotope dilution analysis (SIDA) and dynamic headspace-thermal desorption-gas chromatography/time-of-flight mass spectrometry (dynHS-TD-GC/TOFMS) for the simultaneous quantitation of these boar taint compounds in pig fat was elaborated and validated in this paper. The new method is characterised by a simple and solvent-free dynamic headspace sampling. The deuterated compounds d3-androstenone, d3-skatole and d6-indole were used as internal standards to eliminate matrix effects. The method validation performed revealed low limits of detection (LOD) and quantitation (LOQ) with high accuracy and precision, thus confirming the feasibility of the new dynHS-TD-GC/TOFMS approach for routine analysis.

  2. 大孔树脂对桑黄多糖提取液中色素的吸附与解吸特性研究%Adsorption and desorption characteristics of macroporous resins to pigments of Phellinus linteus polysaccharide extraction

    Institute of Scientific and Technical Information of China (English)

    秦俊哲; 程伟; 杜军国

    2013-01-01

    In order to select a kind of resin which is better on purification of polysaccharide extracted from the fruiting bodies of Phellinus Igniarius. Compared the effects of DA201 and other 5 kinds of macroporous resins in the proessing of decolorization and removal effects of liquid protein. On static adsorption and desorption experiments, select the DA201 resin for static adsorption kinetics and desorption characteristics, investigated the resin saturated adsorption, decolorization rate, protein removing rate and total sugar retention rate. The results show: DA201 resin showed a good effects of deproteinization and decolorization, and total sugar retention rate was high. For the specific polysaccharide extraction, flow rate at 1. 0 mL/min, DA201 resin column to make protein and pigment adsorption reached saturation, need continuous sampling 10 multiple column volume (BV) at least, distilled water and 50% ethanol elution desorption effects was suitable. DA201 resin was suitable for the decolorization of polysaccharide,In order to make full use of DA201 resin adsorption properties, the string column method can be considered in industrial production.%为了选择对桑黄多糖提取液纯化效果较好的树脂,比较了DA201等5种大孔吸附树脂对桑黄多糖提取液的脱色和除蛋白质效果.对5种树脂进行静态吸附与解吸试验,选择DA201树脂研究静态吸附动力学曲线及其解吸特性,考察树脂的饱和吸附量、脱色率、蛋白质脱除率及总糖的保留率.DA201树脂对桑黄多糖提取液中的蛋白质和色素的吸附较多,表明其脱蛋白和脱色效果较好,且多糖的回收率较高.对于特定的多糖提取液,流速1.0 mL/min,过DA201树脂柱要使蛋白质和色素达到吸附饱和,需要连续进样10多个柱床体积(BV),蒸馏水和50%乙醇洗脱解吸效果均较好.DA201树脂较适于桑黄多糖提取液的初步纯化,为了充分发挥DA201树脂的吸附性能,工业生产上可考虑采用串柱法.

  3. Extraction of Thermal Performance Values from Samples in the Lunar Dust Adhesion Bell Jar

    Science.gov (United States)

    Gaier, James R.; Siamidis, John; Larkin, Elizabeth M. G.

    2010-01-01

    A simulation chamber has been developed to test the performance of thermal control surfaces under dusty lunar conditions. The lunar dust adhesion bell jar (LDAB) is a diffusion pumped vacuum chamber (10(exp -8) Torr) built to test material samples less than about 7 cm in diameter. The LDAB has the following lunar dust simulant processing capabilities: heating and cooling while stirring in order to degas and remove adsorbed water; RF air-plasma for activating the dust and for organic contaminant removal; RF H/He-plasma to simulate solar wind; dust sieving system for controlling particle sizes; and a controlled means of introducing the activated dust to the samples under study. The LDAB is also fitted with an in situ Xe arc lamp solar simulator, and a cold box that can reach 30 K. Samples of thermal control surfaces (2.5 cm diameter) are introduced into the chamber for calorimetric evaluation using thermocouple instrumentation. The object of this paper is to present a thermal model of the samples under test conditions and to outline the procedure to extract the absorptance, emittance, and thermal efficiency from the pristine and sub-monolayer dust covered samples.

  4. Extraction of thermal Green's function using diffuse fields: a passive approach applied to thermography

    Science.gov (United States)

    Capriotti, Margherita; Sternini, Simone; Lanza di Scalea, Francesco; Mariani, Stefano

    2016-04-01

    In the field of non-destructive evaluation, defect detection and visualization can be performed exploiting different techniques relying either on an active or a passive approach. In the following paper the passive technique is investigated due to its numerous advantages and its application to thermography is explored. In previous works, it has been shown that it is possible to reconstruct the Green's function between any pair of points of a sensing grid by using noise originated from diffuse fields in acoustic environments. The extraction of the Green's function can be achieved by cross-correlating these random recorded waves. Averaging, filtering and length of the measured signals play an important role in this process. This concept is here applied in an NDE perspective utilizing thermal fluctuations present on structural materials. Temperature variations interacting with thermal properties of the specimen allow for the characterization of the material and its health condition. The exploitation of the thermographic image resolution as a dense grid of sensors constitutes the basic idea underlying passive thermography. Particular attention will be placed on the creation of a proper diffuse thermal field, studying the number, placement and excitation signal of heat sources. Results from numerical simulations will be presented to assess the capabilities and performances of the passive thermal technique devoted to defect detection and imaging of structural components.

  5. Desorption process of deuterium from zircaloys and their oxides

    Energy Technology Data Exchange (ETDEWEB)

    Nakamichi, Haruo; Kinoshita, Chiken; Hara, Masahiro [Kyushu Univ., Fukuoka (Japan)

    1997-11-01

    It is well known that hydrogen behavior plays an important role on the oxidation process of zircaloys. We have investigated the desorption process of deuterium from three kinds of zircaloys (Zry-2, Zry-4 and high-Fe and Ni-Zry-2) and their oxides using thermal desorption spectrometry (TDS). The purpose of the present paper is to get insight into the effect of alloying elements on the desorption behavior of deuterium from the zircaloys and their oxides. We have also performed in-situ observations through TEM for getting the relation between the desorption process and microstructural evolution. The desorption of D{sub 2} implanted by an ion accelerator occurs in two stages; the first and the second stages appear at around 350 K and around 700 K for the metallic zircaloys, respectively. For their oxide films, on the other hand, the desorption rate of D{sub 2} is much higher than that for the metallic zircaloys. It is found that the desorption rate depends strongly on the kind of zircaloys, especially on the concentration of Fe and Ni. From TEM result, it is found that the first desorption stage for the metallic specimens is correlated to the dissolution of the hydrides. (author)

  6. Laser desorption of NO from a thick C 60 film

    Science.gov (United States)

    Hoger, T.; Marzok, C.; Jongma, R. T.; Zacharias, H.

    2006-09-01

    The desorption of NO molecules from a thick C 60 film is reported. A thermal desorption spectrum indicates two adsorption sites with binding energies of Eb = 0.30 eV and 0.55 eV. For laser desorption the fullerene surface is exposed to NO and excited by 7 ns UV laser pulses. Desorbing NO molecules are recorded state selectively as well as time resolved. The time-of-flight measurement indicates three different desorption pathways. A fast channel shows rovibronic temperatures of Trot( v″ = 0) = 370 K, Trot( v″ = 1) = 390 K and Tvib = 610 K as well as strong rotational-translational coupling. The desorption yield for the fast channel increases linearly with pulse energy with a desorption cross section of σ = (5.1 ± 0.9) × 10 -17 cm 2. Dominating the signal for small J″ values is a slow channel with low rotational and translational temperatures of about 110 K. We assign this peak to a laser-induced thermal desorption. For large pump-probe delays the data deviate from the Maxwellian flux distribution and a third channel appears with extremely late arrival times.

  7. Pedestrian detection in thermal images: An automated scale based region extraction with curvelet space validation

    Science.gov (United States)

    Lakshmi, A.; Faheema, A. G. J.; Deodhare, Dipti

    2016-05-01

    Pedestrian detection is a key problem in night vision processing with a dozen of applications that will positively impact the performance of autonomous systems. Despite significant progress, our study shows that performance of state-of-the-art thermal image pedestrian detectors still has much room for improvement. The purpose of this paper is to overcome the challenge faced by the thermal image pedestrian detectors, which employ intensity based Region Of Interest (ROI) extraction followed by feature based validation. The most striking disadvantage faced by the first module, ROI extraction, is the failed detection of cloth insulted parts. To overcome this setback, this paper employs an algorithm and a principle of region growing pursuit tuned to the scale of the pedestrian. The statistics subtended by the pedestrian drastically vary with the scale and deviation from normality approach facilitates scale detection. Further, the paper offers an adaptive mathematical threshold to resolve the problem of subtracting the background while extracting cloth insulated parts as well. The inherent false positives of the ROI extraction module are limited by the choice of good features in pedestrian validation step. One such feature is curvelet feature, which has found its use extensively in optical images, but has as yet no reported results in thermal images. This has been used to arrive at a pedestrian detector with a reduced false positive rate. This work is the first venture made to scrutinize the utility of curvelet for characterizing pedestrians in thermal images. Attempt has also been made to improve the speed of curvelet transform computation. The classification task is realized through the use of the well known methodology of Support Vector Machines (SVMs). The proposed method is substantiated with qualified evaluation methodologies that permits us to carry out probing and informative comparisons across state-of-the-art features, including deep learning methods, with six

  8. Aerial visible-thermal infrared hyperspectral feature extraction technology and its application to object identification

    Science.gov (United States)

    Jie-lin, Zhang; Jun-hu, Wang; Mi, Zhou; Yan-ju, Huang; Ding, Wu

    2014-03-01

    Based on aerial visible-thermal infrared hyperspectral imaging system (CASI/SASI/TASI) data, field spectrometer data and multi-source geological information, this paper utilizes the hyperspectral data processing and feature extraction technology to identify uranium mineralization factors, the spectral features of typical tetravalent, hexavalent uranium minerals and mineralization factors are established, and hyperspectral logging technology for drill cores and trench also are developed, the relationships between radioactive intensity and spectral characteristics are built. Above methods have been applied to characterize uranium mineralization setting of granite-type and sandstone-type uranium deposits in south and northwest China, the successful outcomes of uranium prospecting have been achieved.

  9. Thermal alteration of water extractable organic matter in climosequence soils from the Sierra Nevada, California

    Science.gov (United States)

    Santos, Fernanda; Russell, David; Berhe, Asmeret Asefaw

    2016-11-01

    In the next decades, the influence of wildfires in controlling the cycling and composition of soil organic matter (SOM) globally and in the western U.S. is expected to grow. While the impact of fires on bulk SOM has been extensively studied, the extent at which heating of soil affects the soluble component of SOM remains unclear. Here we investigated the thermal transformations of water-extractable organic matter (WEOM) by examining the changes in the distribution of carbon (C) functional groups in WEOM from soils heated at low and intermediate temperatures. WEOM (exported from soils to rivers in the Sierra Nevada and beyond.

  10. Study on pyrolysis gas in thermal extraction of Bai Yinhua lignite with industrial washing oil

    Science.gov (United States)

    Cui, Y. M.; Lian, X. P.; Zhao, F. Y.; Xu, Y. Q.; Hu, Y. Q.; Yuan, Z. K.; Hao, X. R.

    2016-08-01

    Industrial washing oil as solvent, pyrolysis gas produced from Bai Yinhua lignite during thermal extraction was studied by gas chromatography. The effects of temperature and solvent coal ration on coal pyrolysis gas were investigated. The results showed that: Pyrolysis gas produced mainly in CO, CO2, O2, H2, CH4, and so on, in which the total amount of oxygen containing compounds nearly 40%, significant effects of deoxidation was achieved. The increase of heat extraction temperature can significantly increase the degree of bond breaking and the gas formation rate, the gas yield and the rate of oxygen increase significantly, while the gas yield increases with the decrease of the solvent coal ration.

  11. Correlation of skin blanching and percutaneous absorption for glucocorticoid receptor agonists by matrix-assisted laser desorption ionization mass spectrometry imaging and liquid extraction surface analysis with nanoelectrospray ionization mass spectrometry.

    Science.gov (United States)

    Marshall, Peter; Toteu-Djomte, Valerie; Bareille, Philippe; Perry, Hayley; Brown, Gillian; Baumert, Mark; Biggadike, Keith

    2010-09-15

    Matrix-assisted laser desorption/ionization-mass spectrometry imaging (MALDI-MSI) and liquid extraction surface analysis (LESA) with nanoelectrospray ionization mass spectrometry (nESI-MS) have both been successfully employed to determine the degree of percutaneous absorption of three novel nonsteroid glucocorticoid receptor (GR) agonists in porcine ear sections. Historically, the ability of a glucocorticoid to elicit a skin blanching response when applied at low dose in ethanol solution to the forearms of healthy human volunteers has been a reliable predictor of their topical anti-inflammatory activity. While all three nonsteroidal GR agonists under investigation caused a skin blanching effect, the responses did not correlate with in vitro GR agonist potencies and different time courses were also observed for the skin blanching responses. MALDI MSI and LESA with nESI-MS were used to investigate and understand these different responses. The findings of the investigation was that the depth of porcine skin penetration correlates to the degree of skin blanching obtained for the same three compounds in human volunteers.

  12. Identification of blood culture isolates directly from positive blood cultures by use of matrix-assisted laser desorption ionization-time of flight mass spectrometry and a commercial extraction system: analysis of performance, cost, and turnaround time.

    Science.gov (United States)

    Lagacé-Wiens, Philippe R S; Adam, Heather J; Karlowsky, James A; Nichol, Kimberly A; Pang, Paulette F; Guenther, Jodi; Webb, Amanda A; Miller, Crystal; Alfa, Michelle J

    2012-10-01

    Matrix-assisted laser desorption ionization-time of flight (MALDI-TOF) mass spectrometry represents a revolution in the rapid identification of bacterial and fungal pathogens in the clinical microbiology laboratory. Recently, MALDI-TOF has been applied directly to positive blood culture bottles for the rapid identification of pathogens, leading to reductions in turnaround time and potentially beneficial patient impacts. The development of a commercially available extraction kit (Bruker Sepsityper) for use with the Bruker MALDI BioTyper has facilitated the processing required for identification of pathogens directly from positive from blood cultures. We report the results of an evaluation of the accuracy, cost, and turnaround time of this method for 61 positive monomicrobial and 2 polymicrobial cultures representing 26 species. The Bruker MALDI BioTyper with the Sepsityper gave a valid (score, >1.7) identification for 85.2% of positive blood cultures with no misidentifications. The mean reduction in turnaround time to identification was 34.3 h (P blood cultures and 26.5 h in a more practical setting where conventional identification or identification from subcultures was required for isolates that could not be directly identified by MALDI-TOF. Implementation of a MALDI-TOF-based identification system for direct identification of pathogens from blood cultures is expected to be associated with a marginal increase in operating costs for most laboratories. However, the use of MALDI-TOF for direct identification is accurate and should result in reduced turnaround time to identification.

  13. Picrocrocin kinetics in aqueous saffron spice extracts (Crocus sativus L.) upon thermal treatment.

    Science.gov (United States)

    Sánchez, Ana M; Carmona, Manuel; Jarén-Galán, Manuel; Mosquera, M Isabel Mínguez; Alonso, Gonzalo L

    2011-01-12

    The kinetics of picrocrocin degradation in aqueous extracts of saffron upon thermal treatment from 5 to 70 °C have been studied, together with the degradation of purified picrocrocin in water at 100 °C. The best fits to experimental data were found for a second-order kinetics model. Picrocrocin showed high stability with half-life periods (t(1/2)) ranging from >3400 h at 5 °C in saffron extracts to 9 h in the experiments with purified picrocrocin at 100 °C. In saffron extracts, the evolution of the rate constant (k) with temperature showed maximum values at 35 °C, and filtration of the extracts contributed to picrocrocin stability. In the case of purified picrocrocin, the generation of safranal in the first 5 h (yield up to 7.4%) was confirmed. Spectrometric parameters used in saffron quality control (E(1cm)(1%) 257 nm and ΔΕ(pic)) were not appropriate for documenting the evolution of picrocrocin.

  14. Waveguide-based extraction of near-field electromagnetic radiation: a new method for thermal energy conversion?

    CERN Document Server

    Poole, Zsolt L

    2016-01-01

    Energy in a useful form is a vital resource and hence there is a continuous strive to improve existing technologies and to find new ones that address that basic need. The conversion of thermal energy is the primary source of generating electrical energy from a broad range of sources such as, for example coal, oil, natural gas, solar, geothermal, and nuclear energy. A common need in all cases is the ability to efficiently extract the generated electromagnetic and thermal energy and to convert it to electricity. The current methods of thermal energy extraction are based on heat engines, thermoelectric, and thermophotovoltaic conversion. In this report a method based on the direct extraction of Electromagnetic energy from the thermal near-field through the use of optical waveguides, is presented.

  15. Evaluation of Ion Exchange and Sorbing Materials for Their Adsorption/Desorption Performane towards Anthocyanins, Total Phenolics, and Sugars from a Grape Pomace Extract

    Directory of Open Access Journals (Sweden)

    Evangelos D. Trikas

    2017-03-01

    Full Text Available Byproducts of winery industries are treated, in many cases, as useless wastes constituting not only a major disposal problem but also not providing any additional profit to the industries. However, these byproducts could be utilized as a source of various phenolic compounds, such as anthocyanins, that could be used as nutraceuticals or natural colorants. Nine materials were tested and evaluated for their ability to retain and elute anthocyanins, total phenolics, and sugars from a grape pomace extract. The materials tested were the ion exchange Amberlite IRA 400 Cl−, Lewatit TP 208 and Lewatit TP 260, and the sorbing Chromosorb G-HP, Amberite XAD 2, Zeocros CA 150, Chemviron Carbon, Oasis HLB (hydrophilic-lipophilic balance and Isolute C8 end-capped (EC. The two materials with the higher anthocyanins recovery rate, Oasis HLB and Isolute C8 (EC, were further examined for their anthocyanin capacities which were calculated as 5.76 mg·cm−3 and 3.06 mg·cm−3 respectively. Furthermore, their behavior pattern towards anthocyanins of various molecular weights was investigated using a liquid chromatography coupled with mass spectrometry (LC-PDA-MS system.

  16. Beryllium Desorption from Sediments

    Science.gov (United States)

    Boschi, V.; Willenbring, J. K.

    2015-12-01

    Beryllium isotopes have provided a useful tool in the field of geochronology and geomorphology over the last 25 years. The amount of cosmogenic meteoric 10Be and native 9Be absorbed to soils often scales with the residence time and chemical weathering of sediments in a landscape, respectively. Thus, the concentrations in river sediment may be used to quantify the denudation of specific watersheds. When deposited in ocean sediment, these concentrations are thought to record the history of denudation on Earth over the last ~10 Ma. The use of both isotopes often relies on the premise of beryllium retention to sediment surfaces in order to preserve a landscape's erosion and weathering signature. Changes in setting, en route from the soil to fluvial system to the ocean, can cause beryllium desorption and may preclude some applications of the 10Be/9Be system. Four mechanisms were tested to determine the desorption potential of beryllium including a reduction in pH, an increase in ionic strength and complexation with soluble organic and inorganic species. These processes have the potential to mobilize beryllium into solution. For example, by both reducing the pH and increasing the ionic strength, competition for adsorption sites increases, potentially liberating beryllium from the sediment surface. In addition, organic and inorganic ligands can complex beryllium causing it to become mobilized. To determine which of these alterations influence beryllium desorption and to quantify the effect, we prepared separate solutions of beryllium bound to minerals and organic compounds and measured beryllium concentrations in solution before and after adjusting the pH, ionic strength, and changing inorganic and organic ligand concentrations. We conclude from our observations that overall, beryllium sorbed to organic compounds was more resistant to desorption relative to mineral-associated beryllium. Among the methods tested, a reduction in pH resulted in the greatest amount of

  17. Au and Al Schottky barrier formation on GaAs (100) surfaces prepared by thermal desorption of a protective arsenic coating

    Energy Technology Data Exchange (ETDEWEB)

    Spindt, C.J.; Yamada, M.; Meissner, P.L.; Miyano, K.E.; Herrera, A.; Spicer, W.E. (Stanford Univ., CA (United States). Stanford Electronics Labs.); Arko, A.J. (Los Alamos National Lab., NM (United States)); Woodall, J.M.; Pettit, G.D. (International Business Machines Corp., Yorktown Heights, NY (United States). Thomas J. Watson Research Center)

    1991-01-01

    Photoelectron spectroscopy has been used as a tool to investigate the initial stages of Schottky barrier formation on GaAs (100) surfaces. This is a popular technique that has been used by many researchers in the past to measure the band bending (or shift) of the valence band and conduction band (a measure of the Schottky barrier shift), while the Fermi level remains fixed at the system ground (i.e., the ground of the spectrometer). Metal deposition on a semiconductor surface can alter the Schottky barrier at the surface and pin the Fermi level near the middle of the energy gap. Extremely clean and crystallographically perfect surfaces are required in this study. Toward this end, a method of protecting the GaAs surface was employed which consists of capping the GaAs surface with a layer of As. Upon introduction into the high vacuum system the As is thermally desorbed, revealing a pure GaAs surface. Our work was motivated by a previous study (Brillson et al) on similarly capped specimens, which suggested that metal overlayers do not pin the Schottky barrier in GaAs. Barrier heights varied by as much as 0.75 eV between Al and Au overlayers. This large energy range is a striking result in view of the fact that a considerable number of prior studies on both (110) and (100) surfaces have found that all metals will pin within a narrow (0.25 eV) range at midgap. We repeated the measurements of Brillson on the identically doped samples used in their study using two extreme range metals of Au and Al as overlayers. We found that the barrier height measurements on low doped n-type samples used in this work and in the previous work are affected by photovoltaic effects, even at room temperature. This was determined from taking spectra at a number of temperatures between 20 K and room temperature and looking for shifts. 16 refs., 7 figs.

  18. Potential Applications of Concentrated Solar Thermal Technologies in the Australian Minerals Processing and Extractive Metallurgical Industry

    Science.gov (United States)

    Eglinton, Thomas; Hinkley, Jim; Beath, Andrew; Dell'Amico, Mark

    2013-12-01

    The Australian minerals processing and extractive metallurgy industries are responsible for about 20% of Australia's total greenhouse gas (GHG) emissions. This article reviews the potential applications of concentrated solar thermal (CST) energy in the Australian minerals processing industry to reduce this impact. Integrating CST energy into these industries would reduce their reliance upon conventional fossil fuels and reduce GHG emissions. As CST technologies become more widely deployed and cheaper, and as fuel prices rise, CST energy will progressively become more competitive with conventional energy sources. Some of the applications identified in this article are expected to become commercially competitive provided the costs for pollution abatement and GHG mitigation are internalized. The areas of potential for CST integration identified in this study can be classed as either medium/low-temperature or high-temperature applications. The most promising medium/low-grade applications are electricity generation and low grade heating of liquids. Electricity generation with CST energy—also known as concentrated solar power—has the greatest potential to reduce GHG emissions out of all the potential applications identified because of the 24/7 dispatchability when integrated with thermal storage. High-temperature applications identified include the thermal decomposition of alumina and the calcination of limestone to lime in solar kilns, as well as the production of syngas from natural gas and carbonaceous materials for various metallurgical processes including nickel and direct reduced iron production. Hybridization and integration with thermal storage could enable CST to sustain these energy-intensive metallurgical processes continuously. High-temperature applications are the focus of this paper.

  19. Analysis of the Volatile Organic Components in Malus hupenhensis Rehd Leaves by Direct Thermal Desorption Gas Chromatography-mass Spectrometry%湖北海棠叶挥发性成分的 DTD-GC/MS 分析∗

    Institute of Scientific and Technical Information of China (English)

    王宵; 杜业云; 杨志斌; 李晖; 杨柳

    2015-01-01

    The method of direct thermal desorption (DTD)combed with gas chromatography-mass spectrometry (GC/MS)was applied to analyze the volatile organic components in leaves of Malus hupenhensis for the first time,and 46 kinds of volatile organic components were identified.The main chemical components were hydrocarbons,esters,alcohols,ke-tones,vinyl,aldehydes and so on.8 kinds of components can be used as spice additives,5 types can be used for medical purposes,2 kinds can be used as insecticides.This method of analyzing Malus hupenhensis leaves components had good re-peatability,and was simple,efficient,sensitive and environment-friendly.%采用直接热脱附—气相色谱/质谱联用技术(DTD-GC/MS)首次分析了湖北海棠叶挥发性成分,共检测鉴定出有效成分46种,主要包括烷烃类、酯类、醇类、酮类、烯类、醛类等化合物。其中,8种可用作香料添加剂,5种可作医疗用途,2种可用于杀虫剂。采用直接热脱附—气相色谱/质谱法分析湖北海棠叶挥发成分重现性好、操作简单、效率高、绿色环保。

  20. Development and validation of a method for air-quality and nuisance odors monitoring of volatile organic compounds using multi-sorbent adsorption and gas chromatography/mass spectrometry thermal desorption system.

    Science.gov (United States)

    Ribes, Alejandra; Carrera, Guillem; Gallego, Eva; Roca, Xavier; Berenguer, M A José; Guardino, Xavier

    2007-01-26

    An analytical method based on thermal desorption (TD) coupled to gas chromatography (GC) and mass spectrometry detection (MS) has been developed and validated for the determination of a wide range of odor nuisance and air-quality volatile organic compounds (VOC) in air. New generation isocyanates, isocyanato- and isothiocyanatocyclohexane, have been included for the first time as target compounds due to their high occurrence in air samples. A dynamic air sampling method to trap gas and vapor on multi-sorbent tubes using portable pump equipment has been also developed. Sorbent tubes were filled with Carbotrap (70mg), Carbopack X (100mg) and Carboxen-569 (90mg). Validation of the TD-GC-MS method showed good selectivity, sensibility and precision according to Compendium Method TO-17 (US Environment Protection Agency) criteria. Limits of detection (signal-to-noise=3, ng in tube) ranges were 0.004-0.03ng (alcanes), 0.001-0.1ng (aromatics), 0.03-14ng (aldehydes), 0.003-7ng (alcohols), 0.003-0.04ng (chlorides), 0.02-0.5ng (esters), 0.002-0.1ng (ketones), 0.01-0.53ng (terpenes), 14-97ng (amides), 0.2-10ng (isocyanates) and 0.001ng (carbon disulfide). The linear dynamic range was over 3-5 orders of magnitude, depending of the VOC. TD-GC-MS analysis was reproducible, with relative standard deviation (n=5) within 20%. VOCs breakthrough examination showed no significant losses when about 2000ng standard was prepared. In order to evaluate the performance of the developed method on real samples, several industrial and urban air samples were analysed. VOCs were found to be stable on the sorbent tubes for at least 1 week when stored at 4 degrees C.

  1. Extraction of Oil from an Aqueous Emulsion by Coupling Thermal Swing with a Capillary Pump.

    Science.gov (United States)

    Biswas, Saheli; Caram, Hugo; Gupta, Ramesh; Chaudhury, Manoj K

    2016-10-11

    Separation of oil from water is an area of increasing interest because of the ever-increasing emphasis on reducing discharge of oily wastewater streams and for managing accidental oil spills. While several methods to separate oil from water are available, the current methods often require elaborate processing steps and/or have low extraction rates. Here, we report two simple and potentially inexpensive methods of separating oil from aqueous emulsions. The first method employs hydrophobized glass wool in a pressure-driven capillary pump, while the second method employs novel zeolite pellets the exterior surface of which is hydrophobic. These pellets selectively absorb oil from an aqueous emulsion, which can subsequently be recovered using thermal swing with hot fluid at a temperature far below the boiling point of the oil. Separation of oil with a very high yield (ca. 97%) appears possible using a combination of the two methods.

  2. Evaluation of the pH and thermal stabilities of rosella anthocyanin extracts under solar light

    Directory of Open Access Journals (Sweden)

    Kahtan A. Askar

    2015-09-01

    Full Text Available Anthocyanin is considered as an unstable pigment, undergoes gradual degradation processes throughout the storage or use. The degradation of Rosella anthocyanin extract (RAE in different pH solutions was studied under solar light and compared with solutions kept in the dark. It appears that RAE solutions under solar light were suffering rapid degradation than those kept in the dark. Moreover, RAE samples at higher pH values showed faster rates of degradation than those with lower pH values. A mechanism for degradation was suggested through the formation of hydroxyl radical which is responsible for demineralization process. It is also appears that as the initial concentration of the dye increases, the requirement needed for degradation increased as well. The thermal degradation behavior of RAE at temperature range 25–60 °C under solar light showed first order kinetics with low activation energies.

  3. Mechanical and thermal properties of polylactic acid composites reinforced with cellulose nanoparticles extracted from kenaf fibre

    Science.gov (United States)

    Ketabchi, Mohammad Reza; Khalid, Mohammad; Thevy Ratnam, Chantara; Walvekar, Rashmi

    2016-12-01

    Different approaches have been attempted to use biomass as filler for production of biodegradable polymer composites. In this study, cellulose nanoparticles (CNP) extracted from kenaf fibres were used to produce polylactic acid (PLA) based biodegradable nanocomposites. CNP concentration was varied from 1-5 wt. % and blended with PLA using Brabender twin-screw compounder. Effects of CNP loading on the mechanical, thermal and dynamic properties of PLA were investigated. Studies on the morphological properties and influence of CNP loading on the properties of CNP/PLA nanocomposite were also conducted. The results show an adequate compatibility between CNP and PLA matrix. Moreover, addition of 3 wt. % of CNP improved the PLA tensile strength by 25%.

  4. Applicability of an in-House Saponin-Based Extraction Method in Bruker Biotyper Matrix-Assisted Laser Desorption/Ionization Time-of-Flight Mass Spectrometry System for Identification of Bacterial and Fungal Species in Positively Flagged Blood Cultures

    Directory of Open Access Journals (Sweden)

    Jung-Yien Chien

    2016-09-01

    Full Text Available We used an in-house saponin-based extraction method to evaluate the performance of the Bruker Biotyper matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF/MS system for the identification of bacteria and fungi in 405 positively flagged blood culture bottles. Results obtained from MALDI-TOF/MS were compared with those obtained using conventional phenotypic identification methods. Of the 405 positively flagged blood culture bottles, 365 showed monomicrobal growth and were correctly identified to the species (72.1% or genus (89.6% level using the Bruker Biotyper system. The remaining 40 positively flagged blood culture bottles showed polymicrobial growth. Of them, 82.5% (n=33 of the isolates were correctly identified to the species level and 92.5% (n=37 to the genus level using the Bruker Biotyper system. The overall accuracy of identification to the genus level in flagged blood cultures was 89.5% for Gram-positive organisms, 93.5% for Gram-negative pathogens and 71.9% for fungi. Confidence scores were 1.500 for 307 (75.8% bottles, 1.700 for 249 (61.5% bottles and 2.000 for 142 (35.1% bottles. None of the yeast cultures yielded scores 1.700. Using an identification-score cutoff of 1.500, the MALDI Biotyper correctly identified 99.2% of Gram-positive bacteria, 97.6% of Gram-negative bacteria and 100% of yeast isolates to the genus level and 77.6% of Gram-positive bacteria, 87.1% of Gram-negative bacteria and 100.0% of yeast isolates to the species level. The overall rate of identification using our protocol was 89.9% (364/405 for genus level identification and 73.1% (296/405 for species level identification. Yeast isolates yielded the lowest confidence scores, which compromised the accuracy of identification. Further optimization of the protein extraction procedure in positive blood cultures is needed to improve the rate of identification.

  5. TESVE model for design of soil vapor extraction systems with thermal enhancement

    Energy Technology Data Exchange (ETDEWEB)

    Ghuman, A. [Lowney Associates, Mountain View, CA (United States); Wong, K. [Air Force, McClellan AFB, CA (United States); Singh, S. [URS Consultants, Inc., Sacramento, CA (United States)

    1994-12-31

    Soil vapor extraction (SVE) is a popular and effective technology for removal of volatile organic compounds (VOCs), from the subsurface soils. The performance of SVE systems is based on three key parameters: the rate of mass removal, the time required to achieve cleanup goals, and the cost of cleanup. These performance parameters depend on physical and chemical factors such as the rate and pattern of air flow through the affected soils, contaminant type, and the degree of partitioning between the vapor-, liquid-, dissolved- and adsorbed- phase. The effectiveness of SVE can be enhanced by raising the soil temperature. This is done using various methods including electrical heating, and hot air volatilization. TESVE (Thermally-Enhanced Soil Vapor Extraction), a multi-component, non-isothermal, three dimensional software model, is a powerful tool in evaluating the feasibility of SVE, optimizing design, predicting performance, and, ultimately reducing cleanup costs. The TESVE model was run for a SVE site at McClellan Air Force Base, California. Four SVE design scenarios were modeled for removal of trichloroethylene (TCE) from the subsurface soil.

  6. Study of Thermal Activated CO2 Extraction Processes from Carbonate Apatites Using Gas Chromatography

    Directory of Open Access Journals (Sweden)

    V.N. Kuznetsov

    2015-10-01

    Full Text Available The study of carbonate in the structure of carbonate-containing apatites (CCA is an actual problem due to the similarity of such systems to natural apatites of mammalian bone tissue. The search of the optimal synthesis procedures was also carried out in order to obtain carbonate apatites with the highest rate of carbonate ions incorporation into the apatite structure. The analysis of carbonate-group temperature behavior in apatites of various origin helps to understand their structural and functional roles in biologically relevant apatite materials. The thermal extraction and accumulation of CO2 from biogenic and geological apatites is also of interest for the further carbon isotope analysis with accelerating mass-spectrometry. X-ray diffraction analysis, infrared spectroscopy and scanning electron microscopy as well as self-proposed gas chromatography method with thermo-programmed probe extraction were used for carbonate temperature behavior study. This new method allows determining CO2 concentration released from CCA during annealing. The defined changes in carbonate apatite structure depending on synthesis procedure were observed.

  7. Study of the mechanisms of heavy-ion induced desorption on accelerator-relevant materials; Untersuchung der Mechanismen schwerioneninduzierter Desorption an beschleunigerrelevanten Materialien

    Energy Technology Data Exchange (ETDEWEB)

    Bender, Markus

    2008-02-22

    The ion beam loss induced desorption is a performance limitation for low charge state heavy ion accelerators. If charge exchanged projectile ions get lost onto the beam pipe, desorption of gas is stimulated resulting in a pressure increase inside of the synchrotron and thus, a dramatically reduction of the beam life time. To minimize the amount of desorbed gas an experimental program has been started to measure the desorption yields (released gas molecules per incident ion) of various materials and different projectile ions. The present work is a contribution to the understanding of the physical processes behind the ion beam loss induced desorption. The yield measurements by the pressure rise method have been combined for the rst time with in situ ion beam analysis technologies such as ERDA and RBS. With this unique method the desorption behavior of a sample can be correlated to its surface and bulk properties. The performed experiments with 1,4 MeV/u Xenon-Ions show that the ion induced desorption is mainly a surface effect. Sputtered oxide layers or impurities do not contribute to the desorbed gas significantly. Nevertheless bulk properties play an important role in the desorption strength. Pure metallic samples desorb less gas than isolating materials under swift heavy ion irradiation. From the experimental results it was possible to estimate the desorption yields of various materials under ion bombardment by means of an extended inelastic thermal-spike-model. The extension is the combination of the thermal-spike's temperature map with thermal desorption. Within this model the ion induced desorption can be regarded as the release of adsorbates from a transient overheated spot on the samples surface around the ion impact. Finally a copper substrate with a gold coated surface was developed and proposed as a suitable material for a beam loss collimator with minimum desorption to ensure the performance of GSI's SIS18 in high current beam operation. (orig.)

  8. Technical Note: Fast two-dimensional GC-MS with thermal extraction for anhydro-sugars in fine aerosols

    Science.gov (United States)

    A fast two-dimensional gas chromatography (GC-MS) method that uses heart-cutting and thermal extraction (TE) and requires no chemical derivatization is developed for the determination of anhydro-sugars in fine aerosols. Evaluation of the TE-GC-GC-MS method shows high average rela...

  9. Measurement of breakthrough volumes of volatile chemical warfare agents on a poly(2,6-diphenylphenylene oxide)-based adsorbent and application to thermal desorption-gas chromatography/mass spectrometric analysis.

    Science.gov (United States)

    Kanamori-Kataoka, Mieko; Seto, Yasuo

    2015-09-04

    To establish adequate on-site solvent trapping of volatile chemical warfare agents (CWAs) from air samples, we measured the breakthrough volumes of CWAs on three adsorbent resins by an elution technique using direct electron ionization mass spectrometry. The trapping characteristics of Tenax(®) TA were better than those of Tenax(®) GR and Carboxen(®) 1016. The latter two adsorbents showed non-reproducible breakthrough behavior and low VX recovery. The specific breakthrough values were more than 44 (sarin) L/g Tenax(®) TA resin at 20°C. Logarithmic values of specific breakthrough volume for four nerve agents (sarin, soman, tabun, and VX) showed a nearly linear correlation with the reciprocals of their boiling points, but the data point of sulfur mustard deviated from this linear curve. Next, we developed a method to determine volatile CWAs in ambient air by thermal desorption-gas chromatography (TD-GC/MS). CWA solutions that were spiked into the Tenax TA(®) adsorbent tubes were analyzed by a two-stage TD-GC/MS using a Tenax(®) TA-packed cold trap tube. Linear calibration curves for CWAs retained in the resin tubes were obtained in the range between 0.2pL and 100pL for sarin, soman, tabun, cyclohexylsarin, and sulfur mustard; and between 2pL and 100pL for VX and Russian VX. We also examined the stability of CWAs in Tenax(®) TA tubes purged with either dry or 50% relative humidity air under storage conditions at room temperature or 4°C. More than 80% sarin, soman, tabun, cyclohexylsarin, and sulfur mustard were recovered from the tubes within 2 weeks. In contrast, the recoveries of VX and Russian VX drastically reduced with storage time at room temperature, resulting in a drop to 10-30% after 2 weeks. Moreover, we examined the trapping efficiency of Tenax TA(®) adsorbent tubes for vaporized CWA samples (100mL) prepared in a 500mL gas sampling cylinder. In the concentration range of 0.2-2.5mg/m(3), >50% of sarin, soman, tabun, cyclohexylsarin, and HD were

  10. Extraction of temperature dependent electrical resistivity and thermal conductivity from silicon microwires self-heated to melting temperature

    Science.gov (United States)

    Bakan, Gokhan; Adnane, Lhacene; Gokirmak, Ali; Silva, Helena

    2012-09-01

    Temperature-dependent electrical resistivity, ρ(T), and thermal conductivity, k(T), of nanocrystalline silicon microwires self-heated to melt are extracted by matching simulated current-voltage (I-V) characteristics to experimental I-V characteristics. Electrical resistivity is extracted from highly doped p-type wires on silicon dioxide in which the heat losses are predominantly to the substrate and the self-heating depends mainly on ρ(T) of the wires. The extracted ρ(T) decreases from 11.8 mΩ cm at room-temperature to 5.2 mΩ cm at 1690 K, in reasonable agreement with the values measured up to ˜650 K. Electrical resistivity and thermal conductivity are extracted from suspended highly doped n-type silicon wires in which the heat losses are predominantly through the wires. In this case, measured ρ(T) (decreasing from 20.5 mΩ cm at room temperature to 12 mΩ cm at 620 K) is used to extract ρ(T) at higher temperatures (decreasing to 1 mΩ cm at 1690 K) and k(T) (decreasing from 30 W m-1 K-1 at room temperature to 20 W m-1 K-1 at 1690 K). The method is tested by using the extracted parameters to model wires with different dimensions. The experimental and simulated I-V curves for these wires show good agreement up to high voltage and temperature levels. This technique allows extraction of the electrical resistivity and thermal conductivity up to very high temperatures from self-heated microstructures.

  11. Simple sample transfer technique by internally expanded desorptive flow for needle trap devices.

    Science.gov (United States)

    Eom, In-Yong; Pawliszyn, Janusz

    2008-07-01

    Needle trap devices (NTDs) are improving in simplicity and usefulness for sampling volatile organic compounds (VOCs) since their first introduction in early 2000s. Three different sample transfer methods have been reported for NTDs to date. All methods use thermal desorption and simultaneously provide desorptive flow to transfer desorbed VOCs into a GC separation column. For NTDs having 'side holes', GC carrier gas enters a 'side hole' and passes through sorbent particles to carry desorbed VOCs, while for NTD not having a 'side hole', clean air as desorptive flow can be provided through a needle head by a air tight syringe to sweep out desorbed VOCs or water vapor has been reported recently to be used as desorptive flow. We report here a new simple sample transfer technique for NTDs, in which no side holes and an external desorptive flow are required. When an NTD enriched by a mixture of benzene, toluene, ethylbenzene, and xylene (BTEX) or n-alkane mixture (C6-C15) is exposed to the hot zone of GC injector, the expanding air above the packed sorbent transfers the desorbed compounds from the sorbent to the GC column. This internal air expansion results in clean and sharp desorption profiles for BTEX and n-alkane mixture with no carryover. The effect of desorption temperature, desorption time, and overhead volumes was studied. Decane having vapor pressure of approximately 1 Torr at 20 degrees C showed approximately 1% carryover at the moderate thermal desorption condition (0.5 min at 250 degrees C).

  12. Ocean Thermal Extractable Energy Visualization- Final Technical Report on Award DE-EE0002664. October 28, 2012

    Energy Technology Data Exchange (ETDEWEB)

    Ascari, Matthew B.; Hanson, Howard P.; Rauchenstein, Lynn; Van Zwieten, James; Bharathan, Desikan; Heimiller, Donna; Langle, Nicholas; Scott, George N.; Potemra, James; Nagurny, N. John; Jansen, Eugene

    2012-10-28

    The Ocean Thermal Extractable Energy Visualization (OTEEV) project focuses on assessing the Maximum Practicably Extractable Energy (MPEE) from the world's ocean thermal resources. MPEE is defined as being sustainable and technically feasible, given today's state-of-the-art ocean energy technology. Under this project the OTEEV team developed a comprehensive Geospatial Information System (GIS) dataset and software tool, and used the tool to provide a meaningful assessment of MPEE from the global and domestic U.S. ocean thermal resources. The OTEEV project leverages existing NREL renewable energy GIS technologies and integrates extractable energy estimated from quality-controlled data and projected optimal achievable energy conversion rates. Input data are synthesized from a broad range of existing in-situ measurements and ground-truthed numerical models with temporal and spatial resolutions sufficient to reflect the local resource. Energy production rates are calculated for regions based on conversion rates estimated for current technology, local energy density of the resource, and sustainable resource extraction. Plant spacing and maximum production rates are then estimated based on a default plant size and transmission mechanisms. The resulting data are organized, displayed, and accessed using a multi-layered GIS mapping tool, http://maps.nrel.gov/mhk_atlas with a user-friendly graphical user interface.

  13. Extracting Concrete Thermal Characteristics from Temperature Time History of RC Column Exposed to Standard Fire

    OpenAIRE

    Jung J. Kim; Kwang-Soo Youm; Reda Taha, Mahmoud M.

    2014-01-01

    A numerical method to identify thermal conductivity from time history of one-dimensional temperature variations in thermal unsteady-state is proposed. The numerical method considers the change of specific heat and thermal conductivity with respect to temperature. Fire test of reinforced concrete (RC) columns was conducted using a standard fire to obtain time history of temperature variations in the column section. A thermal equilibrium model in unsteady-state condition was developed. The ther...

  14. Analysis of the thermal energy requirements for the extraction of leaf protein concentrate from some green plants

    Energy Technology Data Exchange (ETDEWEB)

    Tangka, Julius K. [Dschang Univ., Dept. of Agricultural Engineering, Dschang (Cameroon)

    2003-12-01

    Extraction of protein from the leaves of green plants is very important because of the high cost of conventional forms of protein such as meat, milk and fish. In order to design machinery for this extraction, and also to embark on leaf protein concentrate extraction, it is necessary to measure and analyse the energy requirements to carry out each process involved in the extraction, using different plant species. Experiments were carried out to determine the amount of crude protein, and the thermal energy required to extract leaf protein concentrate, from juices obtained from the leaves of some plant species. Leaves from the following plants were selected: cassava (Manihot esculanta), Siam weed (Chromolaena odorata), bitter leaf (Vernonia amygdalina), gliricidia (Gliricidia maculata) and thorny tree (Hura crepetans). The leaves from the plant species were macerated in a laboratory pulper. Juice was obtained from the samples using perforated cylinders and a hydraulic press. The specific heat capacity of the juices was determined using the cooling curve method. The values of the heat capacities were used to calculate the amount of thermal energy required to raise the temperature of each juice from its normal temperature of about 25 deg C to a total protein coagulation temperature of about 80 deg C. The crude protein content of the extract was determined using the Kjeldal method. Results indicate that the green coagulum extracted from all the juices all have a protein content of at least 37%. The thermal energy required to coagulate protein from the juices ranges from 1.59 kJ kg{sup -1} for Hura crepetans to 2.7 kJ kg{sup -1} for Vernonia amygdalina. The energy requirement to obtain crude protein (CP) ranges from 8 kJ kg{sup -1} [CP] with Bura crepetans to 182 kJ kg{sup -1} [CP] with Vernonia amygdalina. Both results are statistically significant at the 0.01 confidence interval. It is concluded that the choice of plant species can significantly lower the thermal energy

  15. Photon stimulated desorption of and nuclear resonant scattering by noble gas atoms at solid surfaces

    CERN Document Server

    Ikeda, Akihiko

    2015-01-01

    When a noble gas atom approaches a solid surface, it is adsorbed via the Van der Waals force, which is called physisorption. In this thesis, several experimental results concerning physisorbed atoms at surfaces are presented. First, photon stimulated desorption of Xe atoms from a Au substrate using nano-second laser is presented. With the time-of-flight measurements, the translational temperature and the desorption yield of desorbing Xe as a function of laser fluence are obtained. It is discovered that there are non-thermal and thermal desorption pathways. It is discussed that the former path involves a transient formation of the negative ion of Xe. The desorption flux dependence of the thermal pathway is also investigated. We found that at a large desorption fluxes the desorption flow is thermalized due to the post-desorption collisions. The resultant velocity and the temperature of the flow is found to be in good agreement with the theoretical predictions based on the Knudsen layer formation. Lastly, nuclea...

  16. Experimental study of water effects on gas desorption during high-pressure water injection

    Institute of Scientific and Technical Information of China (English)

    ZHANG Guo-hua; LIU Xian-xin; BI Ye-wu; PU Wen-long

    2011-01-01

    For the question of applying high-pressure water injection to increase gas extraction efficiency by increasing the permeability of water to drive gas action,an independently designed gas desorption experimental measuring device was used under the condition of external solution invasion.The law of water effect on gas desorption was obtained after water invasion through experiment for the first time.The results show that water's later invasion not only can make the quantity of gas desorption greatly reduced,but also can make gas desorption end early.Therefore,when evaluating the applications of high-pressure water injection to increase gas extraction efficiency,we should take water damaging effects on gas desorption into account.

  17. Effect of Ultrasound on Desorption Equilibrium%超声场对氢键缔合体系解吸平衡的影响研究

    Institute of Scientific and Technical Information of China (English)

    秦炜; 原永辉; 戴猷元

    2001-01-01

    Effects of ultrasound on intensification of separation process were investigated through the experiment of desorption equilibrium behavior. Tri-butyl phosphate (TBP) on NKA-Ⅱ resin and phenol on a solvent impregnated resin, CL-TBP resin, were used for desorption processes. The desorption rate was measured with and without ultrasound. Desorption equilibrium was studied under various ultrasonic power densities or thermal infusion. Results showed that the desorption rate with ultrasound was much higher than that with normal thermal infusion. Both ultrasound and thermal infusion broke the desorption equilibrium existed at room temperature. However, after the systems were cooled down, the amount of solute desorbed in the liquid phase in the presence of ultrasound was much higher than that at the temperature corresponding to the same ultrasound power. It is proved that the initial desorption equilibrium was broken as a result of the spot energy effect of ultrasound.``

  18. Extracting Concrete Thermal Characteristics from Temperature Time History of RC Column Exposed to Standard Fire

    Directory of Open Access Journals (Sweden)

    Jung J. Kim

    2014-01-01

    Full Text Available A numerical method to identify thermal conductivity from time history of one-dimensional temperature variations in thermal unsteady-state is proposed. The numerical method considers the change of specific heat and thermal conductivity with respect to temperature. Fire test of reinforced concrete (RC columns was conducted using a standard fire to obtain time history of temperature variations in the column section. A thermal equilibrium model in unsteady-state condition was developed. The thermal conductivity of concrete was then determined by optimizing the numerical solution of the model to meet the observed time history of temperature variations. The determined thermal conductivity with respect to temperature was then verified against standard thermal conductivity measurements of concrete bricks. It is concluded that the proposed method can be used to conservatively estimate thermal conductivity of concrete for design purpose. Finally, the thermal radiation properties of concrete for the RC column were estimated from the thermal equilibrium at the surface of the column. The radiant heat transfer ratio of concrete representing absorptivity to emissivity ratio of concrete during fire was evaluated and is suggested as a concrete criterion that can be used in fire safety assessment.

  19. Extracting concrete thermal characteristics from temperature time history of RC column exposed to standard fire.

    Science.gov (United States)

    Kim, Jung J; Youm, Kwang-Soo; Reda Taha, Mahmoud M

    2014-01-01

    A numerical method to identify thermal conductivity from time history of one-dimensional temperature variations in thermal unsteady-state is proposed. The numerical method considers the change of specific heat and thermal conductivity with respect to temperature. Fire test of reinforced concrete (RC) columns was conducted using a standard fire to obtain time history of temperature variations in the column section. A thermal equilibrium model in unsteady-state condition was developed. The thermal conductivity of concrete was then determined by optimizing the numerical solution of the model to meet the observed time history of temperature variations. The determined thermal conductivity with respect to temperature was then verified against standard thermal conductivity measurements of concrete bricks. It is concluded that the proposed method can be used to conservatively estimate thermal conductivity of concrete for design purpose. Finally, the thermal radiation properties of concrete for the RC column were estimated from the thermal equilibrium at the surface of the column. The radiant heat transfer ratio of concrete representing absorptivity to emissivity ratio of concrete during fire was evaluated and is suggested as a concrete criterion that can be used in fire safety assessment.

  20. Linking desorption kinetics to phenanthrene biodegradation in soil

    Energy Technology Data Exchange (ETDEWEB)

    Rhodes, Angela H.; McAllister, Laura E. [Lancaster Environment Centre, Lancaster University, Lancaster LA1 4YQ (United Kingdom); Semple, Kirk T., E-mail: k.semple@lancaster.ac.u [Lancaster Environment Centre, Lancaster University, Lancaster LA1 4YQ (United Kingdom)

    2010-05-15

    The desorption of polycyclic aromatic hydrocarbons (PAHs) often exhibits a biphasic profile similar to that observed for biodegradation whereby an initial rapid phase of degradation or desorption is followed by a phase of much slower transformation or release. Most investigations to-date have utilised a polymeric sorbent, such as Tenax, to characterise desorption, which is methodologically unsuitable for the analysis of soil. In this study, desorption kinetics of {sup 14}C-phenanthrene were measured by consecutive extraction using aqueous solutions of hydroxypropyl-beta-cyclodextrin (HPCD). The data indicate that the fraction extracted after 24 h generally approximated the linearly sorbed, rapidly desorbing fraction (F{sub rap}), calculated using a three-compartment model. A good linear correlation between phenanthrene mineralised and F{sub rap} was observed (r{sup 2} = 0.89; gradient = 0.85; intercept = 8.20). Hence HPCD extraction (24 h) and first-order three-compartment modelling appear to provide an operationally straightforward tool for estimating mass-transfer limited biodegradation in soil. - Aqueous hydroxypropyl-beta-cyclodextrin (HPCD) solutions can predict the rapidly desorbing and microbially degradable fractions of phenanthrene in soils.

  1. ESR studies on the thermal decomposition of trimethylamine oxide to formaldehyde and dimethylamine in jumbo squid (Dosidicus gigas) extract.

    Science.gov (United States)

    Zhu, Junli; Jia, Jia; Li, Xuepeng; Dong, Liangliang; Li, Jianrong

    2013-12-15

    The effects of ferrous iron, heating temperature and different additives on the decomposition of trimethylamine oxide (TMAO) to formaldehyde (FA) and dimethylamine (DMA) and generation of free radicals in jumbo squid (Dosidicus gigas) extract during heating were evaluated by electron spin resonance (ESR). The thermal decomposition of TMAO to TMA, DMA and FA and free radical signals was observed in squid extract, whereas no DMA, FA and free radical signals were detected in cod extract or in aqueous TMAO solution in vitro at high temperatures. Significant increase in levels of DMA, FA and radicals intensity were observed in squid extract and TMAO solution in the presence of ferrous iron with increasing temperature. Hydrogen peroxide stimulated the production of DMA, FA and ESR signals in squid extract, while citric acid, trisodium citrate, calcium chloride, tea polyphenols and resveratrol had the opposite effect. Similar ESR spectra of six peaks regarded as amminium radical were detected in the squid extract and TMAO-iron(II) solution, suggesting that the amminium radical was involved in the decomposition of TMAO. Copyright © 2013 Elsevier Ltd. All rights reserved.

  2. Hydrogen absorption and desorption in nanocrystalline LaMg{sub 2}Ni

    Energy Technology Data Exchange (ETDEWEB)

    Di Chio, M. [Dipartimento di Chimica IFM and NIS-Centre of Excellence, Universita di Torino, Via P. Giuria, 9-10125 Torino (Italy); Schiffini, L. [Dipartimento di Chimica, Universita di Sassari, Via Vienna, 2-07100 Sassari (Italy); Enzo, S. [Dipartimento di Chimica, Universita di Sassari, Via Vienna, 2-07100 Sassari (Italy); Cocco, G. [Dipartimento di Chimica, Universita di Sassari, Via Vienna, 2-07100 Sassari (Italy); Baricco, M. [Dipartimento di Chimica IFM and NIS-Centre of Excellence, Universita di Torino, Via P. Giuria, 9-10125 Torino (Italy)]. E-mail: marcello.baricco@unito.it

    2007-05-31

    Hydrogen absorption and desorption properties in LaMg{sub 2}Ni compound are presented. Nanostructured phases have been obtained by means of ball milling in order to study the influence of the microstructure on the absorption/desorption properties. The structural and hydriding properties were examined by X-ray diffraction, thermal analysis, hydrogen pressure-composition and thermal desorption measurements. Ball milling of as-cast compound gives a significant refinement of the microstructure. Hydrogenation at 443 K leads to the formation of LaMg{sub 2}NiH{sub 7}, but at higher temperatures (523 K) LaH{sub 2} is produced. Two hours of ball milling promote the formation of LaH{sub 2} under hydrogenation at 443 K. Thermal desorption up to 983 K of hydrogenated samples leads again to parent LaMg{sub 2}Ni phase.

  3. Monomer Adsorption-Desorption Processes

    Institute of Scientific and Technical Information of China (English)

    KE Jian-Hong; LIN Zhen-Quan; CHEN Xiao-Shuang

    2009-01-01

    We propose an adsorption-desorption model for a deposit growth system, in which the adsorption and desorption of particles coexist. By means of the generalized rate equation we investigate the cluster (island) size distribution in the dynamic equilibrium state. The results show that the evolution behaviour of the system depends crucially on the details of the rate kernels. The cluster size distribution can take the ecale-frse power-law form in some cases, while it grows exponentially with size in other cases.

  4. On plate graphite supported sample processing for simultaneous lipid and protein identification by matrix assisted laser desorption ionization mass spectrometry.

    Science.gov (United States)

    Calvano, Cosima Damiana; van der Werf, Inez Dorothé; Sabbatini, Luigia; Palmisano, Francesco

    2015-05-01

    The simultaneous identification of lipids and proteins by matrix assisted laser desorption ionization-mass spectrometry (MALDI-MS) after direct on-plate processing of micro-samples supported on colloidal graphite is demonstrated. Taking advantages of large surface area and thermal conductivity, graphite provided an ideal substrate for on-plate proteolysis and lipid extraction. Indeed proteins could be efficiently digested on-plate within 15 min, providing sequence coverages comparable to those obtained by conventional in-solution overnight digestion. Interestingly, detection of hydrophilic phosphorylated peptides could be easily achieved without any further enrichment step. Furthermore, lipids could be simultaneously extracted/identified without any additional treatment/processing step as demonstrated for model complex samples such as milk and egg. The present approach is simple, efficient, of large applicability and offers great promise for protein and lipid identification in very small samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. Laser induced-thermal lens spectrometry after cloud point extraction for the determination of trace amounts of palladium

    Science.gov (United States)

    Shokoufi, N.; Shemirani, F.; Shokoufi, M.

    2009-10-01

    Cloud point extraction (CPE) in combination with thermal lens spectrometry (TLS) has been developed for the preconcentration and determination of palladium. TLS and CPE methods have good matching conditions for the combination because TLS is a suitable method for the analysis of low volume samples obtained after CPE. Palladium was complexed with 1-(2-pyridylazo)-2-naphthol (PAN) as a complexing agent in an aqueous medium and concentrated by octylphenoxypolyethoxyethanol (Triton X-114) as a surfactant. After the phase separation at 60 °C based on the cloud point extraction of the mixture, the surfactant-rich phase was dried and the remaining phase was dissolved using 20 μL of carbon tetrachloride. The obtained solution was introduced into a quartz microcell and the analyte was determined by laser induced-thermal lens spectrometry (LI-TLS). The single-laser TLS was used as a sensitive method for the determination of palladium-PAN complex in 20 μL of the sample. Under optimum conditions, the analytical curve was linear for the concentration range of 0.3-60 ng mL -1 and the detection limit was 0.04 ng mL -1. The enhancement factor of 460 was achieved for 10 mL samples containing the analyte and relative standard deviations were lower than 5%. The developed method was successfully applied to the extraction and determination of palladium in water samples.

  6. Hydrogen desorption in nanocrystalline MgH{sub 2} thin films at room temperature

    Energy Technology Data Exchange (ETDEWEB)

    Ares, J.R., E-mail: joser.ares@uam.e [Dpto. de Fisica de Materiales, Facultad de Ciencias, Universidad Autonoma de Madrid, Cantoblanco, 28049, Madrid (Spain); Leardini, F.; Diaz-Chao, P.; Bodega, J. [Dpto. de Fisica de Materiales, Facultad de Ciencias, Universidad Autonoma de Madrid, Cantoblanco, 28049, Madrid (Spain); Koon, D.W. [Physics Department, St Lawrence University, Canton, NY, 13617 (United States); Ferrer, I.J.; Fernandez, J.F.; Sanchez, C. [Dpto. de Fisica de Materiales, Facultad de Ciencias, Universidad Autonoma de Madrid, Cantoblanco, 28049, Madrid (Spain)

    2010-04-16

    Hydrogen desorption process of Pd-capped magnesium hydride thin films of different thicknesses was investigated. Decomposition of magnesium hydride into magnesium under air exposure is observed in all investigated films. During decomposition no novel crystalline phases are detected. Desorption process was qualitatively analysed and it was concluded that is thermodynamically driven controlled by a nucleation and growth or by an interphase controlled mechanism. Moreover, H-kinetics investigation of desorption process was carried out by thermal desorption spectroscopy. Decomposition of MgH{sub 2} films occurs at T{sub d} {approx} 148 {sup o}C and the process seems to be controlled by a bidimensional interphase mechanism with an activation energy of 135 {+-} 20 kJ/mol H{sub 2}. No significant influence of thickness and crystallite size on desorption temperature is observed and obtained activation energy is similar to that of milled bulk magnesium.

  7. SPS Ion Induced Desorption Experiment

    CERN Multimedia

    Maximilien Brice

    2003-01-01

    This experiment will give a study about the induced desorption from heavy ion (Indium ion run from week 45 in SPS T4-H8 area) impacting LHC type graphite collimator. 4 different samples are located in the 4 chambers 90° one to each other: pure graphite, graphite with copper coating, graphite with NEG coating, 316LN stainless steal (reference).

  8. Development of Axial Compressor Heat-Extraction Capability for Thermal Management Applications Project

    Data.gov (United States)

    National Aeronautics and Space Administration — ATA Engineering, Inc. (ATA) proposes a small business innovation research (SBIR) program for a novel compressor heat-extraction development program in response to...

  9. EXTRACT

    DEFF Research Database (Denmark)

    Pafilis, Evangelos; Buttigieg, Pier Luigi; Ferrell, Barbra

    2016-01-01

    The microbial and molecular ecology research communities have made substantial progress on developing standards for annotating samples with environment metadata. However, sample manual annotation is a highly labor intensive process and requires familiarity with the terminologies used. We have the...... and text-mining-assisted curation revealed that EXTRACT speeds up annotation by 15-25% and helps curators to detect terms that would otherwise have been missed.Database URL: https://extract.hcmr.gr/....

  10. Extraction chromatographic methods in the sample preparation sequence for thermal ionization mass spectrometric analysis of plutonium isotopes.

    Science.gov (United States)

    Grate, Jay W; O'Hara, Matthew J; Farawila, Anne F; Douglas, Matthew; Haney, Morgan M; Petersen, Steven L; Maiti, Tapas C; Aardahl, Christopher L

    2011-12-01

    A sample preparation sequence for actinide isotopic analysis by thermal ionization mass spectrometry (TIMS) is described that includes column-based extraction chromatography as the first separation step, followed by anion-exchange column separations. The sequence is designed to include a wet ashing step after the extraction chromatography to prevent any leached extractant or oxalic acid eluent reagents from interfering with subsequent separations, source preparation, or TIMS ionization. TEVA resin and DGA resin materials, containing extractants that consist only of C, N, O, and H atoms, were investigated for isolation of plutonium. Radiotracer level studies confirmed expected high yields from column-based separation procedures. Femtogram-level studies were carried out with TIMS detection, using multiple monoisotopic spikes applied sequentially throughout the separation sequence. Pu recoveries were 87% and 86% for TEVA and DGA resin separations, respectively. The Pu recoveries from 400 μL anion-exchange column separation sequences were 89% and 93% for trial sequences incorporating TEVA and DGA resin. Thus, a prior extraction chromatography step in the sequence did not interfere with the subsequent anion-exchange separation when a simple wet ash step was carried out in between these column separations. The average measurement efficiency for Pu, encompassing the chemical separation recoveries and the TIMS ionization efficiency, was 2.73% ± 0.77% (2σ) for the DGA resin trials and 2.67% ± 0.54% for the TEVA resin trials, compared to 3.41% and 2.37% (average 2.89%) for two control trials. These compare with an average measurement efficiency of 2.78% ± 1.70%, n = 33 from process benchmark analyses using Pu spikes processed through a sequence of oxalate precipitation, wet ash, iron hydroxide precipitation, and anion-exchange column separations. We conclude that extraction chromatography can be a viable separation procedure as part of a multistep sequence for TIMS

  11. 气相色谱与热解吸联用技术在室内环境检测领域的应用及进展%Application and Development of Gas Chromatography Hyphenated with Thermal Desorption in the Field of Indoor Environment Testing

    Institute of Scientific and Technical Information of China (English)

    贾祥焱

    2012-01-01

    It is a brief introduction of gas chromatography and the application and development of gas chromatography hyphenated with thermal desorption in the test benzene and TVOC of indoor environment testing,and puts forward outlook and prospect in it.It provides favorable value in the development of gas chromatographic technique in indoor environment testing.%简要介绍了气相色谱法,及其与热解吸联用在民用建筑工程室内环境检测中检测苯、TVOC的应用和进展。并提出了气相色谱与热解吸联用技术的前景与展望,为气相色谱技术在室内环境检测领域的发展提供有利价值。

  12. Thermal Stability Study of the Grape Seeds Extracts in the Aqueous Solutions

    Directory of Open Access Journals (Sweden)

    Carmen Pop

    2015-05-01

    Full Text Available This study was carried out to evaluate the effect of parameters the extraction process of grape seeds extracts on the bioactive compounds. The aqueous extracts were screened for total polyphenol content and total flavonoid content wich were determined spectrophotometrically using a modified Folin-Ciocalteu method, respectively a chromogenic system of NaNO2–Al (NO33–NaOH based method. The antioxidant activity was determined using DPPH method while  their polyphenolic composition by means of HPLC-DAD- MS/ ESI(+ analysis. Total phenols content and flavonoid content varied between 37.835 and 31.830 mg GAE/g, 23.420 and 17.645 mg QE/g respectively in Fetească Neagră seeds; between 24.265 and 27.065 mg GAE/g, 17.970 and 15.205 mg QE/g respectively in Fetească Regală seeds. All extracts showed remarkable DPPH radical-scavenging activity ranging from 94.110 to 95.515%. The study revealed 14 phenolic compounds belonging to the following groups: flavan-3-ol monomers, proanthocyanidins, hydroxycinnamic acid and hydroxybenzoic acid derivatives. Quantitative differences among the varieties and the level of temperature applied of  the extraction process were observed. The results suggested that the heat treatment of grape seeds liberated phenolic compounds having a significant effect in increasing the amounts of active when a 90°C extraction temperature was used.

  13. Antioxidant Activity and Thermal Stability of Oleuropein and Related Phenolic Compounds of Olive Leaf Extract after Separation and Concentration by Salting-Out-Assisted Cloud Point Extraction.

    Science.gov (United States)

    Stamatopoulos, Konstantinos; Katsoyannos, Evangelos; Chatzilazarou, Arhontoula

    2014-04-08

    A fast, clean, energy-saving, non-toxic method for the stabilization of the antioxidant activity and the improvement of the thermal stability of oleuropein and related phenolic compounds separated from olive leaf extract via salting-out-assisted cloud point extraction (CPE) was developed using Tween 80. The process was based on the decrease of the solubility of polyphenols and the lowering of the cloud point temperature of Tween 80 due to the presence of elevated amounts of sulfates (salting-out) and the separation from the bulk solution with centrifugation. The optimum conditions were chosen based on polyphenols recovery (%), phase volume ratio (Vs/Vw) and concentration factor (Fc). The maximum recovery of polyphenols was in total 95.9%; Vs/Vw was 0.075 and Fc was 15 at the following conditions: pH 2.6, ambient temperature (25 °C), 4% Tween 80 (w/v), 35% Na₂SO₄ (w/v) and a settling time of 5 min. The total recovery of oleuropein, hydroxytyrosol, luteolin-7-O-glucoside, verbascoside and apigenin-7-O-glucoside, at optimum conditions, was 99.8%, 93.0%, 87.6%, 99.3% and 100.0%, respectively. Polyphenolic compounds entrapped in the surfactant-rich phase (Vs) showed higher thermal stability (activation energy (Ea) 23.8 kJ/mol) compared to non-entrapped ones (Ea 76.5 kJ/mol). The antioxidant activity of separated polyphenols remained unaffected as determined by the 1,1-diphenyl-2-picrylhydrazyl method.

  14. Antioxidant Activity and Thermal Stability of Oleuropein and Related Phenolic Compounds of Olive Leaf Extract after Separation and Concentration by Salting-Out-Assisted Cloud Point Extraction

    Directory of Open Access Journals (Sweden)

    Konstantinos Stamatopoulos

    2014-04-01

    Full Text Available A fast, clean, energy-saving, non-toxic method for the stabilization of the antioxidant activity and the improvement of the thermal stability of oleuropein and related phenolic compounds separated from olive leaf extract via salting-out-assisted cloud point extraction (CPE was developed using Tween 80. The process was based on the decrease of the solubility of polyphenols and the lowering of the cloud point temperature of Tween 80 due to the presence of elevated amounts of sulfates (salting-out and the separation from the bulk solution with centrifugation. The optimum conditions were chosen based on polyphenols recovery (%, phase volume ratio (Vs/Vw and concentration factor (Fc. The maximum recovery of polyphenols was in total 95.9%; Vs/Vw was 0.075 and Fc was 15 at the following conditions: pH 2.6, ambient temperature (25 °C, 4% Tween 80 (w/v, 35% Na2SO4 (w/v and a settling time of 5 min. The total recovery of oleuropein, hydroxytyrosol, luteolin-7-O-glucoside, verbascoside and apigenin-7-O-glucoside, at optimum conditions, was 99.8%, 93.0%, 87.6%, 99.3% and 100.0%, respectively. Polyphenolic compounds entrapped in the surfactant-rich phase (Vs showed higher thermal stability (activation energy (Ea 23.8 kJ/mol compared to non-entrapped ones (Ea 76.5 kJ/mol. The antioxidant activity of separated polyphenols remained unaffected as determined by the 1,1-diphenyl-2-picrylhydrazyl method.

  15. 氯苯类易挥发有机污染土壤异位低温热脱附实例研究%Case Study On Ex-situ Remediation of Chlorobenzene-Like Volatile Organic Compounds (VOCs) Contaminated Soil With Technique of Low-Temperature Thermal Desorption

    Institute of Scientific and Technical Information of China (English)

    王湘徽; 祝欣; 龙涛; 邓绍坡; 林玉锁; 胡韬

    2016-01-01

    The technique of low⁃temperature thermal desorption was used to remedy chlorobenzene⁃like VOCs contaminated soil. Results show that VOCs were effectively removed after the treatment, with removal rate reaching 85% or more for all the tested VOCs. In field trials, a specialized soil remediation machine KH200 was used to crush the soil and have it mixed with lime in full⁃closed operation to avoid dust pollution. Through raising soil temperature and lowering soil water content, desorption and volatilization of VOC was effectively accelerated. All the findings in the experiment demon⁃strate that the use of the technique of low⁃temperature thermal desorption and the KH200 equipment is a promising ap⁃proach to efficient and low cost remediation of contaminated soils in sites of deserted chemical plants.%针对南京市某大型化工企业退役场地,结合场地修复目标,使用生石灰对场地氯苯类挥发性有机污染物( VOCs)污染土壤进行异位低温热脱附处理。实验室试验结果表明,该方法可有效去除土壤中的VOCs,处理后各污染物去除率均达85%以上。在现场试验中,采用专业土壤修复设备KH200进行土壤破碎和药剂混合,处理过程全封闭运行,可有效降低扬尘等问题。通过投加生石灰提高土壤温度、降低土壤含水量的方法,有效地促进了土壤中VOCs的解吸和挥发,是一种高效率、低成本的土壤修复技术,经过KH200修复设备处理后土壤中各污染物均达到场地修复目标,具备工程应用可行性。

  16. Adsorption/desorption of phenanthrene on contaminated soils

    Energy Technology Data Exchange (ETDEWEB)

    Saada, A.; Gaboriau, H.; Amalric, L.; Crouzet, C. [BRGM, Orleans (France)

    2003-07-01

    Polycyclic Aromatic Hydrocarbons (PAH) are persistent environmental contaminants whose behaviour has been thoroughly studies because of their genotoxicity. One of the main processes governing PAH evolution is adsorption onto soil matrices due to the marked hydrophobic properties of this group of pollutants. In this study, pehnanthrene adsorption and desorption were measured for: - an untreated polluted soil (S) from a former coking plant - the same soil washed with toluene in a soxhlet extractor (S{sub w}), which enables the pollutants (PAH and tar) to be extracted from the soil - the fine fraction (<50 {mu}m) of the washed soil (S{sub f}), - a mineral (kaolinite) representative of the polluted soil (K), - the mineral coated with the tar extracted from the polluted soil (K-T). Isotherms of phenanthrene adsorption/desorption on K, K-T and S shows that the hysteresis between the adsorption and desorption isotherms increases 1) with the organic matter content, and 2) for the untreated soil S containing endogenic bacteria, in addition to organic matter. This indicates that tar-type organic matter is capable of reducing the release of phenanthrene by forming bonded residue. For the untreated soil S, endogenic bacteria consume phenanthrene as it is desorbed. Consequently, the desorption isotherm for S is almost horizontal, as if no desorption had taken place. This study has demonstrated the effect that the type of organic matter has on PAH fate, and thus the need to take this into account, particularly where tar is concerned, when assessing the adsorption capacity of soils. (orig.)

  17. Kinetics and thermodynamics of the thermal inactivation of polyphenol oxidase in an aqueous extract from Agaricus bisporus.

    Science.gov (United States)

    Gouzi, Hicham; Depagne, Christophe; Coradin, Thibaud

    2012-01-11

    The kinetics and thermodynamics of the thermal inactivation of polyphenol oxidase (PPO) in an aqueous extract from mushroom Agaricus bisporus (J.E. Lange) Imbach was studied, using pyrocatechol as a substrate. Optimal conditions for enzymatic studies were determined to be pH 7.0 and 35-40 °C. The kinetics of PPO-catalyzed oxidation of pyrocatechol followed the Haldane model with an optimum substrate concentration of 20 mM. Thermal inactivation of PPO was examined in more detail between 50 and 73 °C and in relation to exposure time. Obtained monophasic kinetics were adequately described by a first-order model, with significant inactivation occurring with increasing temperature (less than 10% preserved activity after 6 min at 65 °C). Arrhenius plot determination and calculated thermodynamic parameters suggest that the PPO in aqueous extract from Agaricus bisporus mushroom is a structurally robust yet temperature-sensitive biocatalyst whose inactivation process is mainly entropy-driven.

  18. A replica technique for extracting precipitates from neutron-irradiated or thermal-aged vanadium alloys for TEM analysis

    Energy Technology Data Exchange (ETDEWEB)

    Fukumoto, K., E-mail: fukumoto@u-fukui.ac.jp; Iwasaki, M.

    2014-06-01

    A carbon replica technique has been developed to extract precipitates from vanadium alloys. Using this technique, precipitation phases can be extracted from neutron-irradiated or thermal-aged V–4Cr–4Ti alloys. Precipitate identification using EDS X-ray analysis and electron diffraction was facilitated. Only NaCl type of Ti(OCN) precipitate was formed in the thermal-aged V–4Cr–4Ti alloys at 600 °C for 20 h and cation sub-lattice was only occupied by Ti atoms. However, the thin plate of precipitates with NaCl type of crystallographic structure could be seen in the V–4Cr–4Ti alloys irradiated at 593 °C in the JOYO fast reactor. The precipitate contained chromium and vanadium atoms on the cation sub-lattice as well as titanium atoms. It is considered that the phase of MX type (M = Ti, V, Cr and X = O, N, C) is a metastable phase under neutron irradiation.

  19. A replica technique for extracting precipitates from neutron-irradiated or thermal-aged vanadium alloys for TEM analysis

    Science.gov (United States)

    Fukumoto, K.; Iwasaki, M.

    2014-06-01

    A carbon replica technique has been developed to extract precipitates from vanadium alloys. Using this technique, precipitation phases can be extracted from neutron-irradiated or thermal-aged V-4Cr-4Ti alloys. Precipitate identification using EDS X-ray analysis and electron diffraction was facilitated. Only NaCl type of Ti(OCN) precipitate was formed in the thermal-aged V-4Cr-4Ti alloys at 600 °C for 20 h and cation sub-lattice was only occupied by Ti atoms. However, the thin plate of precipitates with NaCl type of crystallographic structure could be seen in the V-4Cr-4Ti alloys irradiated at 593 °C in the JOYO fast reactor. The precipitate contained chromium and vanadium atoms on the cation sub-lattice as well as titanium atoms. It is considered that the phase of MX type (M = Ti, V, Cr and X = O, N, C) is a metastable phase under neutron irradiation.

  20. Extraction of work from a single thermal bath in the quantum regime

    NARCIS (Netherlands)

    Allahverdyan, A.

    2000-01-01

    The stationary state of a quantum particle strongly coupled to a quantum thermal bath is known to be non-Gibbsian, due to entanglement with the bath. For harmonic potentials, where the system can be described by effective temperatures, thermodynamic relations are shown to take a generalized Gibbsian

  1. Thermal properties of natural nanostructured hydroxyapatite extracted from fish bone waste

    Science.gov (United States)

    Coelho, T. M.; Nogueira, E. S.; Weinand, W. R.; Lima, W. M.; Steimacher, A.; Medina, A. N.; Baesso, M. L.; Bento, A. C.

    2007-04-01

    In a previous study, natural hydroxyapatite (HAp) from the bones of Brazilian river fish was calcined at 900 °C (4-12 h), and optical characterization using the near infrared photoacoustic spectroscopy technique enabled the establishment of 8 h as the best calcination time for nanostructure stabilization when milled in a high-energy milling device [T. M. Coelho, E. S. Nogueira, W. R. Weinand, W. M. Lima, A. Steimacher, A. N. Medina, M. L. Baesso, and A. C. Bento, J. Appl. Phys. 100, 094312 (2006)]. The fish wastes used were from species such as pintado (Pseudoplatystoma corruscans), jaú (Paulicea lutkeni), and cachara (Pseudoplatystoma fasciatum). In this study, the characterization of the thermal properties of the same natural HAp is discussed for samples milled from 0 to 32 h, with nanostructures from 80 to 24 nm. The powders were pressed into disks at 350 MPa and sintered for 4 h at 1000 °C. Thermophysical parameters were obtained by thermal wave interferometry and nonadiabatic relaxation calorimetry. Results for thermal diffusivity and thermal conductivity showed that the parameters increase with milling time, although they present a transition (a plateau) in the interval from 8 to 16 h. Two different slopes were observed and this was interpreted as being due to the size of the crystallites, which fall rapidly, dropping from 80 nm to near 22 nm when milling time is increased from 0 to 16 h, and forming agglomerates up to 32 h.

  2. Synthesis and Hydrogen Desorption Properties of Aluminum Hydrides.

    Science.gov (United States)

    Jeong, Wanseop; Lee, Sang-Hwa; Kim, Jaeyong

    2016-03-01

    Aluminum hydride (AlH3 or alane) is known to store maximum 10.1 wt.% of hydrogen at relatively low temperature (hydrogen desorption are still not clear. To understand the desorption properties of hydrogen in alane, thermodynamically stable α-AlH3 was synthesized by employing an ethereal reaction method. The dependence of pathways on phase formation and the properties of hydrogen evolution were investigated, and the results were compared with the ones for γ-AlH3. It was found that γ-AlH3 requires 10 degrees C higher than that of γ-AlH3 to form, and its decomposition rate demonstrated enhanced endothermic stabilities. For desorption, all hydrogen atoms of alane evolved under an isothermal condition at 138 degrees C in less than 1 hour, and the sample completely transformed to pure aluminum. Our results show that the total amount of desorbed hydrogen from α-AlH3 exceeded 9.05 wt.%, with a possibility of further increase. Easy synthesis, thermal stability, and a large amount of hydrogen desorption of alane fulfill the requirements for light-weight hydrogen storage materials once the pathway of hydrogen cycling is provided.

  3. Hydrogen desorption from hydrogen fluoride and remote hydrogen plasma cleaned silicon carbide (0001) surfaces

    Energy Technology Data Exchange (ETDEWEB)

    King, Sean W., E-mail: sean.king@intel.com; Tanaka, Satoru; Davis, Robert F. [Department of Materials Science and Engineering, North Carolina State University, Raleigh, North Carolina 27695 (United States); Nemanich, Robert J. [Department of Physics, North Carolina State University, Raleigh, North Carolina 27695 (United States)

    2015-09-15

    Due to the extreme chemical inertness of silicon carbide (SiC), in-situ thermal desorption is commonly utilized as a means to remove surface contamination prior to initiating critical semiconductor processing steps such as epitaxy, gate dielectric formation, and contact metallization. In-situ thermal desorption and silicon sublimation has also recently become a popular method for epitaxial growth of mono and few layer graphene. Accordingly, numerous thermal desorption experiments of various processed silicon carbide surfaces have been performed, but have ignored the presence of hydrogen, which is ubiquitous throughout semiconductor processing. In this regard, the authors have performed a combined temperature programmed desorption (TPD) and x-ray photoelectron spectroscopy (XPS) investigation of the desorption of molecular hydrogen (H{sub 2}) and various other oxygen, carbon, and fluorine related species from ex-situ aqueous hydrogen fluoride (HF) and in-situ remote hydrogen plasma cleaned 6H-SiC (0001) surfaces. Using XPS, the authors observed that temperatures on the order of 700–1000 °C are needed to fully desorb C-H, C-O and Si-O species from these surfaces. However, using TPD, the authors observed H{sub 2} desorption at both lower temperatures (200–550 °C) as well as higher temperatures (>700 °C). The low temperature H{sub 2} desorption was deconvoluted into multiple desorption states that, based on similarities to H{sub 2} desorption from Si (111), were attributed to silicon mono, di, and trihydride surface species as well as hydrogen trapped by subsurface defects, steps, or dopants. The higher temperature H{sub 2} desorption was similarly attributed to H{sub 2} evolved from surface O-H groups at ∼750 °C as well as the liberation of H{sub 2} during Si-O desorption at temperatures >800 °C. These results indicate that while ex-situ aqueous HF processed 6H-SiC (0001) surfaces annealed at <700 °C remain terminated by some surface C–O and

  4. THERMO-HYDRO-MECHANICAL MODELING OF WORKING FLUID INJECTION AND THERMAL ENERGY EXTRACTION IN EGS FRACTURES AND ROCK MATRIX

    Energy Technology Data Exchange (ETDEWEB)

    Robert Podgorney; Chuan Lu; Hai Huang

    2012-01-01

    Development of enhanced geothermal systems (EGS) will require creation of a reservoir of sufficient volume to enable commercial-scale heat transfer from the reservoir rocks to the working fluid. A key assumption associated with reservoir creation/stimulation is that sufficient rock volumes can be hydraulically fractured via both tensile and shear failure, and more importantly by reactivation of naturally existing fractures (by shearing), to create the reservoir. The advancement of EGS greatly depends on our understanding of the dynamics of the intimately coupled rock-fracture-fluid-heat system and our ability to reliably predict how reservoirs behave under stimulation and production. Reliable performance predictions of EGS reservoirs require accurate and robust modeling for strongly coupled thermal-hydrological-mechanical (THM) processes. Conventionally, these types of problems have been solved using operator-splitting methods, usually by coupling a subsurface flow and heat transport simulators with a solid mechanics simulator via input files. An alternative approach is to solve the system of nonlinear partial differential equations that govern multiphase fluid flow, heat transport, and rock mechanics simultaneously, using a fully coupled, fully implicit solution procedure, in which all solution variables (pressure, enthalpy, and rock displacement fields) are solved simultaneously. This paper describes numerical simulations used to investigate the poro- and thermal- elastic effects of working fluid injection and thermal energy extraction on the properties of the fractures and rock matrix of a hypothetical EGS reservoir, using a novel simulation software FALCON (Podgorney et al., 2011), a finite element based simulator solving fully coupled multiphase fluid flow, heat transport, rock deformation, and fracturing using a global implicit approach. Investigations are also conducted on how these poro- and thermal-elastic effects are related to fracture permeability

  5. Early detection and classification of powdery mildew-infected rose leaves using ANFIS based on extracted features of thermal images

    Science.gov (United States)

    Jafari, Mehrnoosh; Minaei, Saeid; Safaie, Naser; Torkamani-Azar, Farah

    2016-05-01

    Spatial and temporal changes in surface temperature of infected and non-infected rose plant (Rosa hybrida cv. 'Angelina') leaves were visualized using digital infrared thermography. Infected areas exhibited a presymptomatic decrease in leaf temperature up to 2.3 °C. In this study, two experiments were conducted: one in the greenhouse (semi-controlled ambient conditions) and the other, in a growth chamber (controlled ambient conditions). Effect of drought stress and darkness on the thermal images were also studied in this research. It was found that thermal histograms of the infected leaves closely follow a standard normal distribution. They have a skewness near zero, kurtosis under 3, standard deviation larger than 0.6, and a Maximum Temperature Difference (MTD) more than 4. For each thermal histogram, central tendency, variability, and parameters of the best fitted Standard Normal and Laplace distributions were estimated. To classify healthy and infected leaves, feature selection was conducted and the best extracted thermal features with the largest linguistic hedge values were chosen. Among those features independent of absolute temperature measurement, MTD, SD, skewness, R2l, kurtosis and bn were selected. Then, a neuro-fuzzy classifier was trained to recognize the healthy leaves from the infected ones. The k-means clustering method was utilized to obtain the initial parameters and the fuzzy "if-then" rules. Best estimation rates of 92.55% and 92.3% were achieved in training and testing the classifier with 8 clusters. Results showed that drought stress had an adverse effect on the classification of healthy leaves. More healthy leaves under drought stress condition were classified as infected causing PPV and Specificity index values to decrease, accordingly. Image acquisition in the dark had no significant effect on the classification performance.

  6. Copper desorption from Gelidium algal biomass.

    Science.gov (United States)

    Vilar, Vítor J P; Botelho, Cidália M S; Boaventura, Rui A R

    2007-04-01

    Desorption of divalent copper from marine algae Gelidium sesquipedale, an algal waste (from agar extraction industry) and a composite material (the algal waste immobilized in polyacrylonitrile) was studied in a batch system. Copper ions were first adsorbed until saturation and then desorbed by HNO(3) and Na(2)EDTA solutions. Elution efficiency using HNO(3) increases as pH decreases. At pH=1, for a solid to liquid ratio S/L=4gl(-1), elution efficiency was 97%, 95% and 88%, the stoichiometric coefficient for the ionic exchange, 0.70+/-0.02, 0.73+/-0.05 and 0.76+/-0.06 and the selectivity coefficient, 0.93+/-0.07, 1.0+/-0.3 and 1.1+/-0.3, respectively, for algae Gelidium, algal waste and composite material. Complexation of copper ions by EDTA occurs in a molar proportion of 1:1 and the elution efficiency increases with EDTA concentration. For concentrations of 1.4, 0.88 and 0.57 mmoll(-1), the elution efficiency for S/L=4gl(-1), was 91%, 86% and 78%, respectively, for algae Gelidium, algal waste and composite material. The S/L ratio, in the range 1-20gl(-1), has little influence on copper recovery by using 0.1M HNO(3). Desorption kinetics was very fast for all biosorbents. Kinetic data using HNO(3) as eluant were well described by the mass transfer model, considering the average metal concentration in the solid phase and the equilibrium relationship given by the mass action law. The homogeneous diffusion coefficient varied between 1.0 x 10(-7)cm(2)s(-1) for algae Gelidium and 3.0 x 10(-7)cm(2)s(-1) for the composite material.

  7. Synergic solvent extraction and thermal studies of fluorinated beta-diketone-organophosphorus adduct complexes of lanthanide and related elements

    Energy Technology Data Exchange (ETDEWEB)

    Mitchell, James Winfield [Iowa State Univ., Ames, IA (United States)

    1970-01-01

    (VI), U(IV), Ca(II), Y(III), FE(III), Zn(II), CU(II) and some lanthanide elements. The utility of the extraction systems, HTFA in benzene, HTFA-TBP in cyclohexane and HHFA-TBP in cyclohexane, for analytical separations of SC(III), FE(III), UOx -2 and TH(IV) from the rare earths and of the rare earths from Al(III) was demonstrated. A literature review containing the available information on the extraction of various cations by HTFA is given. On the basis of this information and the reported distribution curves, conditions for the separation of certain cations from each other and from the reare earths were suggested. Trends in thermal stability and volatility of chelates of the lanthanide and releated elements were obtained from thermogravimetric anlaysis of the hydrated and mixed chelates. Significant improvements in thermal stability of rare earth chelates were obtained by displacement of hydrated water upon adduct formation with TBP.

  8. 2,5-Dihydroxybenzoic acid: laser desorption/ionisation as a function of elevated temperature

    Science.gov (United States)

    Wallace, W. E.; Arnould, M. A.; Knochenmuss, R.

    2005-03-01

    The temperature dependence of laser desorption/ionization (LDI) ion yields has been measured for 2,5-dihydroxybenzoic acid (2,5-DHB) single crystals from room temperature to 160 °C using time-of-flight (TOF) mass spectrometry. A steep rise in ion production occurs at 90 °C, achieving a maximum at 120 °C, then decreases sharply to a minimum at 140 °C, and returns to a second maximum at 150 °C. Above 160 °C, useful information could not be obtained because of rapid volatilization of the sample into the vacuum. The overall trend in ion production, but not some of the details, is well described by a recent two-step theory of the laser desorption/ionization process, which takes into account the temperature-dependent effects of plume expansion. Measuring the background vacuum composition with a quadrupole mass spectrometer residual gas analyzer (RGA) showed an increase in thermal desorption of 2,5-DHB starting at 90 °C and maximizing at 130 °C. The increased neutral production by thermal desorption is believed to be the cause of the decrease in LDI ion production due to reduced pooling probabilities for laser-excited 2,5-DHB molecules. Thermal dehydration, condensation, and decarboxylation increase the volume of gas released at high temperatures which also serve to decrease LDI ion production at elevated temperatures. Lastly, to confirm the mass spectrometry results, the thermal desorption of 2,5-DHB single crystals under vacuum was measured using a quartz-crystal microbalance (QCM). The onset of desorption was found to occur at 90 °C and the maximum desorption rate was found at 135 °C.

  9. Enhancing magnetic properties of anisotropic NdDyFeCoNbCuB powder by applying magnetic field at high temperature during hydrogen desorption

    Institute of Scientific and Technical Information of China (English)

    LUO Jianjun; P.De Rango; D.Fruchart; MEI Jinna; HU Rui; LI Jinshan; ZHOU Lian

    2010-01-01

    Anisotropic powder was prepared with precursor (NdDy)-(FeCoNbCu)-B sintered magnets by hydrogen decrepitation,desorption,and subsequent annealing treatment.The hydrogen desorption was performed in magnetic fields of 0,1,3,and 5 T.The orientation of tetragonal phase grains of the powder was evaluated from the hysteresis loops measured by extraction magnetometer.Residual hydrogen content of the powder was evaluated by thermal-magnetic analysis.The powder with Hcj,Br,and (BH)max of 1138 kA.m-1,1.029 T,and 172.5 kJ.m-3,respectively,was achieved under the condition of the magnetic field of 3 T.Magnetic properties of the powder,especially,the remanence of the powder,are enhanced upon magnetic fields,which is due to better orientation of powder particles and less residual hydrogen in the powder resulted from the magnetic field during the hydrogen desorption process.

  10. Magnesium growth in magnesium deuteride thin films during deuterium desorption

    Energy Technology Data Exchange (ETDEWEB)

    Checchetto, R., E-mail: riccardo.checchetto@unitn.it [Dipartimento di Fisica and CNISM, Università di Trento, Via Sommarive 14, I-38123 Trento (Italy); Miotello, A. [Dipartimento di Fisica and CNISM, Università di Trento, Via Sommarive 14, I-38123 Trento (Italy); Mengucci, P.; Barucca, G. [Dipartimento di Fisica e Ingegneria dei Materiali e del Territorio, Università Politecnica delle Marche, I-60131 Ancona (Italy)

    2013-12-15

    Highlights: ► Highly oriented Pd-capped magnesium deuteride thin films. ► The MgD{sub 2} dissociation was studied at temperatures not exceeding 100 °C. ► The structure of the film samples was analyzed by XRD and TEM. ► The transformation is controlled by the re-growth velocity of the Mg layers. ► The transformation is thermally activated, activation energy value of 1.3 ± 0.1 eV. -- Abstract: Pd- capped nanocrystalline magnesium thin films having columnar structure were deposited on Si substrate by e-gun deposition and submitted to thermal annealing in D{sub 2} atmosphere to promote the metal to deuteride phase transformation. The kinetics of the reverse deuteride to metal transformation was studied by Thermal Desorption Spectroscopy (TDS) while the structure of the as deposited and transformed samples was analyzed by X-rays diffraction and Transmission Electron Microscopy (TEM). In Pd- capped MgD{sub 2} thin films the deuteride to metal transformation begins at the interface between un-reacted Mg and transformed MgD{sub 2} layers. The D{sub 2} desorption kinetics is controlled by MgD{sub 2}/Mg interface effects, specifically the re-growth velocity of the Mg layers. The Mg re-growth has thermally activated character and shows an activation energy value of 1.3 ± 0.1 eV.

  11. Alkaline Extraction of Cobia (Rachycentroncanadum Proteins: Physicochemical characteristics, functional and thermal properties

    Directory of Open Access Journals (Sweden)

    Sabrina de La Rocha

    2015-04-01

    Full Text Available Cobia (Rachycentroncanadum is an important emerging species in Brazilian mariculture. The aim of the study was to obtain and characterize a protein isolate from cobia muscle using chemical extraction process by alkaline solubilization and isoelectric precipitation of proteins. The extraction yield was 98.17g/100g protein on a dry basis. The highest solubility and water holding capacity (WHC of cobiaprotein isolate (CPI was obtained at pH 11and 21.9mL of water per gram of protein. The electrophoretic profiles revealed masses characteristic of myofibrillar proteins (myosin and actin. The main peaks identified by qualitative spectroscopy analysis of the infrared spectrawere characteristic of peptide bonds such as amide I and amide II. The highest fusion and degradation points of CPI were 259.1°C and 378°C, respectively. The results showed that the CPI has great biotechnological value in various industrial areas that require a product of high protein value.

  12. Keratins extracted from Merino wool and Brown Alpaca fibres: thermal, mechanical and biological properties of PLLA based biocomposites.

    Science.gov (United States)

    Fortunati, E; Aluigi, A; Armentano, I; Morena, F; Emiliani, C; Martino, S; Santulli, C; Torre, L; Kenny, J M; Puglia, D

    2015-02-01

    Keratins extracted from Merino wool (KM) and Brown Alpaca fibres (KA) by sulphitolysis and commercial hydrolyzed keratins (KH) were used as fillers in poly(l-lactic) acid based biocomposites processed by solvent casting in chloroform. Different contents (1 wt.% and 5 wt.%) of keratins were considered and the morphological, thermal, mechanical, chemical and biological behaviours of the developed PLLA biocomposites were investigated. The results confirmed that surface morphologies of biocomposites revealed specific round-like surface topography function of different microsized keratin particles in different weight contents, such as the analysis of bulk morphologies which confirmed a phase adhesion strictly dependent by the keratin source. Transparency and thermal responses were deeply affected by the presence of the different keratins and their interaction with the PLLA matrix. Tensile test results underlined the possibility to modulate the mechanical behaviour of PLLA selecting the keratin type and content in order to influence positively the elastic and/or plastic response. It was demonstrated that surface characteristics of PLLA/KA systems also influenced the bovine serum albumin adsorption, moreover PLLA and PLLA biocomposites based on different kinds of keratins supported the culture of human bone-marrow mesenchymal stem cells, indicating that these biocomposites could be useful materials for medical applications.

  13. Catalitic effect of Co on hydrogen desorption form nanostucturated magnesium hydride

    Directory of Open Access Journals (Sweden)

    Matović Ljiljana Lj.

    2008-01-01

    Full Text Available To study the influence of 3d transition metal addition on desorption kinetics of MgH2 ball milling of MgH2-Co blends was performed under Ar. Microstructural and morphological characterization, performed by XRD and SEM, show a huge correlation with thermal stability and hydrogen desorption properties investigated by DSC. A complex desorption behavior is correlated with the dispersion of the metal additive particles on hydride matrix. The activation energy for H2 desorption from MgH2-Co composite was calculated from both non-isothermal and isothermal methods to be 130 kJ/mol which means that mutually diffusion and nucleation and growth of new phase control the dehydration process.

  14. Comparison of Three Methods for Extraction of Volatile Lipid Oxidation Products from Food Matrices for GC–MS Analysis

    DEFF Research Database (Denmark)

    Thomsen, Birgitte Raagaard; Yesiltas, Betül; Sørensen, Ann-Dorit Moltke

    2016-01-01

    The aim of this study was to compare three different collection methods; purge and trap, solid phase micro extraction and automated dynamic headspace/thermal desorption, all followed by GC–MS analysis used for the measurements of concentrations of volatile oxidation products in three different food...... matrices, namely oil, emulsion and milk. The linearity ranges of calibration curves obtained by the three different methods were compared for oil samples. Overall, the results showed that the three collection methods were comparable, although there were large differences in the linearity range...... of the calibration curves depending on the collection method. However, some challenges were observed for solid phase micro extraction and automated dynamic headspace/thermal desorption, namely, competition problems and overestimation of concentration by calibration curves, respectively. Based on the results, we...

  15. Characteristics and applications of gas desorption with excavation disturbances in coal mining

    Institute of Scientific and Technical Information of China (English)

    Jiachen Wang; Renlun Wu; Peng Zhang

    2015-01-01

    According to the deficiency of experiment system for gas adsorption and desorption in coal mass, a large scale experiment system is developed independently by researchers. This experiment system is composed of primary and auxiliary boxes, power transmission system, mining system, loading system, gas charging system, data monitoring and intelligent acquisition system. The maximum experiment coal consumption is 1200 kg, the mining system is developed to conduct experiment for gas desorption under excavating disturbance, and the plane-charging cribriform ventilation device is developed to realize uniform ventilation for experiment coal sample, which is accord with the actual gas source situation of coal bed. The desorption characteristics of gas in coal are experimentally studied under the conditions of nature and mining using the experiment system. The results show that, compare with nature condition, the permeability of coal and the velocity of gas desorption could significantly increase under the influence of coal pressure relief and destruction caused by mining, and the degree of gas desorption could somewhat increase too. Finally, pressure relief gas extraction of current seam and adjacent seams after mining in a certain coal mine of Yangquan mining area are introduced, and the gas desorption experiment results is verified by analyzing the effect of gas extraction.

  16. Investigation of high pressure steaming (HPS) as a thermal treatment for lipid extraction from Chlorella vulgaris.

    Science.gov (United States)

    Aguirre, Ana-Maria; Bassi, Amarjeet

    2014-07-01

    Biofuels from algae are considered a technically viable energy source that overcomes several of the problems present in previous generations of biofuels. In this research high pressure steaming (HPS) was studied as a hydrothermal pre-treatment for extraction of lipids from Chlorella vulgaris, and analysis by response surface methodology allowed finding operational points in terms of target temperature and algae concentration for high lipid and glucose yields. Within the range covered by these experiments the best conditions for high bio-crude yield are temperatures higher than 174°C and low biomass concentrations (<5 g/L). For high glucose yield there are two suitable operational ranges, either low temperatures (<105°C) and low biomass concentrations (<4 g/L); or low temperatures (<105°C) and high biomass concentrations (<110 g/L). High pressure steaming is a good hydrothermal treatment for lipid recovery and does not significantly change the fatty acids profile for the range of temperatures studied.

  17. Photo- and thermally stimulated luminescence of polyminerals extracted from herbs and spices

    Science.gov (United States)

    Cruz-Zaragoza, E.; Marcazzó, J.; Chernov, V.

    2012-08-01

    Ionizing radiation processing is a widely employed method for preservative treatment of foodstuffs. Usually it is possible to detect irradiated herbs and spices by resorting to luminescence techniques, in particular photo- and thermostimulated luminescence. For these techniques to be useful, it is necessary to characterize the response to radiation of each particular herb or spice. In this work, the thermoluminescence (TL) and photostimulated luminescence (PSL) properties of inorganic polymineral fractions extracted from commercial herbs and spices previously irradiated for disinfestation purposes have been analyzed. Samples of mint, cinnamon, chamomile, paprika, black pepper, coriander and Jamaica flower were irradiated from 50 to 400 Gy by using a beta source. The X-ray diffraction (XRD) analysis has shown that the mineral fractions consist mainly of quartz and feldspars. The PSL and TL response as a function of the absorbed dose, and their fading at room temperature have been determined. The TL glow curves have been deconvolved in order to obtain characteristic kinetics parameters in each case. The results of this work show that PSL and TL are reliable techniques for detection and analysis of irradiated foodstuffs.

  18. A numerical study of EGS heat extraction process based on a thermal non-equilibrium model for heat transfer in subsurface porous heat reservoir

    Science.gov (United States)

    Chen, Jiliang; Jiang, Fangming

    2016-02-01

    With a previously developed numerical model, we perform a detailed study of the heat extraction process in enhanced or engineered geothermal system (EGS). This model takes the EGS subsurface heat reservoir as an equivalent porous medium while it considers local thermal non-equilibrium between the rock matrix and the fluid flowing in the fractured rock mass. The application of local thermal non-equilibrium model highlights the temperature-difference heat exchange process occurring in EGS reservoirs, enabling a better understanding of the involved heat extraction process. The simulation results unravel the mechanism of preferential flow or short-circuit flow forming in homogeneously fractured reservoirs of different permeability values. EGS performance, e.g. production temperature and lifetime, is found to be tightly related to the flow pattern in the reservoir. Thermal compensation from rocks surrounding the reservoir contributes little heat to the heat transmission fluid if the operation time of an EGS is shorter than 15 years. We find as well the local thermal equilibrium model generally overestimates EGS performance and for an EGS with better heat exchange conditions in the heat reservoir, the heat extraction process acts more like the local thermal equilibrium process.

  19. Improved hydrogen desorption from lithium hydrazide by alkali metal hydride

    Energy Technology Data Exchange (ETDEWEB)

    Zeng, Liang, E-mail: liangzeng@hiroshima-u.ac.jp [Institute for Advanced Materials Research, Hiroshima University, 1-3-1 Kagamiyama, Higashi-Hiroshima 739-8530 (Japan); Miyaoka, Hiroki [Institute for Sustainable Sciences and Development, Hiroshima University, 1-3-1 Kagamiyama, Higashi-Hiroshima 739-8530 (Japan); Ichikawa, Takayuki; Kojima, Yoshitsugu [Institute for Advanced Materials Research, Hiroshima University, 1-3-1 Kagamiyama, Higashi-Hiroshima 739-8530 (Japan)

    2013-12-15

    Highlights: •LiH can dramatically improve the hydrogen desorption properties of LiNHNH{sub 2}. •KH doping had positive effect in promoting the hydrogen desorption properties of LiNHNH{sub 2}–LiH mixture. •The reaction mechanism between LiNHNH{sub 2} and LiH was studied and discussed. -- Abstract: Lithium hydrazide (LiNHNH{sub 2}), which is a white solid with 8.0 mass% of theoretical hydrogen content, was synthesized from a reaction between anhydrous hydrazine and n-butyllithium in diethyl ether. The thermodynamic properties of this compound and its detailed decomposition pathways had been investigated in our previous work. However, a number of undesired gaseous products such as hydrazine (N{sub 2}H{sub 4}) and ammonia (NH{sub 3}) were generated during the thermal decomposition of LiNHNH{sub 2}. In this work, alkali metal hydride was used to suppress the impurities in the desorbed hydrogen and improved the hydrogen desorption properties. The reaction mechanism between LiNHNH{sub 2} and LiH was also studied and discussed in this paper.

  20. Laser-induced acoustic desorption (LIAD) mass spectrometry.

    Science.gov (United States)

    Dow, Alex M; Wittrig, Ashley R; Kenttämaa, Hilkka I

    2012-01-01

    Large thermally labile molecules were not amenable to mass spectrometric analysis until the development of atmospheric pressure evaporation/ionization methods, such as electrospray ionization (ESI) and matrix-assisted laser desorption/ionization (MALDI), since attempts to evaporate these molecules by heating induces degradation of the sample. While ESI and MALDI are relatively soft desorption/ionization techniques, they are both limited to preferential ionization of acidic and basic analytes. This limitation has been the driving force for the development of other soft desorption/ionization techniques. One such method employs laser-induced acoustic desorption (LIAD) to evaporate neutral sample molecules into mass spectrometers. LIAD utilizes acoustic waves generated by a laser pulse in a thin metal foil. The acoustic waves travel through the foil and cause desorption of neutral molecules that have been deposited on the opposite side of the foil. One of the advantages of LIAD is that it desorbs low-energy molecules that can be ionized by a variety of methods, thus allowing the analysis of large molecules that are not amenable to ESI and MALDI. This review covers the generation of acoustic waves in foils via a laser pulse, the parameters affecting the generation of acoustic waves, possible mechanisms for desorption of neutral molecules, as well as the various uses of LIAD by mass spectrometrists. The conditions used to generate acoustic or stress waves in solid materials consist of three regimes: thermal, ablative, and constrained. Each regime is discussed, in addition to the mechanisms that lead to the ablation of the metal from the foil and generation of acoustic waves for two of the regimes. Previously proposed desorption mechanisms for LIAD are presented along with the flaws associated with some of them. Various experimental parameters, such as the exact characteristics of the laser pulse and foil used, are discussed. The internal and kinetic energy of the neutral

  1. Surface oxidation and water desorption of CdS

    Institute of Scientific and Technical Information of China (English)

    陈正石; 李庆霖; 金振声

    1996-01-01

    The surface oxidation and HP desorption of powder CdS were studied by means of X-ray photoetectron spectroscopy (XPS), quadrupole mass spectrometry (QMS) and in-situ FTIR. The results show that with the changes of surface composition and the elongation of store time of CdS there are four types of H2O thermally desorbed at different temperatures. It has also been found that through high-temperature air treatment for a short time the oxidized surface layer of CdS can prevent O2 and H2O in air from further attacking the inner CdS molecules.

  2. Protein extraction from Mycobacterium avium subsp. paratuberculosis: Comparison of methods for analysis by sodium dodecyl sulphate polyacrylamide gel electrophoresis, native PAGE and surface enhanced laser desorption/ionization time of flight mass spectrometry.

    Science.gov (United States)

    Gumber, Sanjeev; Taylor, Deborah L; Whittington, Richard J

    2007-01-01

    Mycobacterium paratuberculosis causes Johne's disease, a chronic bowel disease in ruminants worldwide and is currently incurable. This study was conducted to compare methods for examining the proteome of M. paratuberculosis. SDS-PAGE, native PAGE and SELDI-TOF-MS were compared and the efficacy of various lysis buffers was assessed. Chaotropic agents (Urea CHAPS and potassium thiocyanate) and non-ionic detergent (Tween20 and Triton X-100) extracts were compared on three different ProteinChip surfaces along with two energy absorbing molecules (EAM): EAM-1 proprietary formulation and sinapinic acid (Ciphergen). Urea CHAPS was efficient for extraction of proteins and their detection on all the ProteinChip surfaces. However, potassium thiocyanate was the most effective buffer, leading to detection of the greatest number of protein peaks on the immobilized metal affinity chromatography (IMAC) surface. Sinapinic acid was more efficient than the EAM-1 proprietary formulation and resulted in additional peaks with higher intensity for both the low and the medium molecular weight range proteins. Intra-chip and inter-chip coefficient of variation for mass/charge varied from 0.01% to 0.07% and 0.00% to 0.08%, respectively. SELDI-TOF-MS was an efficient tool for the protein profiling of M. paratuberculosis and will be useful for investigation of novel proteins, although SDS-PAGE/2D gel electrophoresis is recommended for study of high molecular weight species. All buffers were suitable for protein extraction for SDS-PAGE, while Tween20 was best for native PAGE.

  3. Glyphosate sorption and desorption in soils with distinct phosphorus levels

    Energy Technology Data Exchange (ETDEWEB)

    Prata, Fabio [BIOAGRI Labs., Piracicaba, SP (Brazil). Div. de Quimica. Lab. de Radioquimica; Cardinali, Vanessa Camponez do Brasil; Tornisielo, Valdemar Luiz; Regitano, Jussara Borges [Sao Paulo Univ., Piracicaba, SP (Brazil). Escola Superior de Agricultura Luiz de Queiroz. Dept. de Ciencias Exatas; Lavorenti, Arquimedes [Centro de Energia Nuclear na Agricultura (CENA), Piracicaba, SP (Brazil). Secao de Toxicologia

    2003-03-01

    The sorption of glyphosate by soils occurs due to the inner sphere complex formation with metals of soil oxides, which are related to the soil phosphate adsorption capacity. The aim of this study was to evaluate the effects of increasing rates of phosphorus on sorption and desorption of glyphosate in three soils with different mineralogical attributes. Soils were a Rhodic Kandiudalf, an Anionic Acrudox and a Typic Humaquept. Soil samples were amended with Kh{sub 2}PO{sub 4} at equivalent rates of 0; 1,000; 5,000; 20,000 and 50,000 kg ha{sup -1} of P{sub 2}O{sub 5}, which are high from the agricultural point of view, but necessary in order to perform sorption and desorption studies. The experimental design consisted of a completely randomized factorial: 2 soils x 5 phosphorus rates and 3 replicates. For the sorption experiments, five glyphosate solutions were employed (0.42; 0.84; 1.68; 3.36 and 6.72 mg L{sup -1}), with a {sup 14}C radioactivity of 0.233 kBq mL{sup -1}. Four steps of the desorption procedures withCaCl{sub 2} 0.01 mol L{sup -1} and one extraction with Mehlich 3 were performed only at one concentration (0.84 mol L{sup -1}). Soil samples were afterwards biologically oxidized to establish the radioactive balance. Glyphosate competes with phosphorus for specific sorption sites, but this competition becomes important when phosphorus is present at rates higher than 1,000 mg dm{sup -3}. Moreover, a small amount of applied glyphosate was extracted (<10%), and the extraction increased with increasing soil phosphorus content. (author)

  4. Glyphosate sorption and desorption in soils with distinct phosphorus levels

    Directory of Open Access Journals (Sweden)

    Prata Fábio

    2003-01-01

    Full Text Available The sorption of glyphosate by soils occurs due to the inner sphere complex formation with metals of soil oxides, which are related to the soil phosphate adsorption capacity. The aim of this study was to evaluate the effects of increasing rates of phosphorus on sorption and desorption of glyphosate in three soils with different mineralogical attributes. Soils were a Rhodic Kandiudalf, an Anionic Acrudox and a Typic Humaquept. Soil samples were amended with KH2PO4 at equivalent rates of 0; 1,000; 5,000; 20,000 and 50,000 kg ha-1 of P2O5, which are high from the agricultural point of view, but necessary in order to perform sorption and desorption studies. The experimental design consisted of a completely randomized factorial: 2 soils x 5 phosphorus rates and 3 replicates. For the sorption experiments, five glyphosate solutions were employed (0.42; 0.84; 1.68; 3.36 and 6.72 mg L-1, with a 14C radioactivity of 0.233 kBq mL-1. Four steps of the desorption procedure with CaCl2 0.01 mol L-1 and one extraction with Mehlich 3 were performed only at one concentration (0.84 mol L-1. Soil samples were afterwards biologically oxidized to establish the radioactive balance. Glyphosate competes with phosphorus for specific sorption sites, but this competition becomes important when phosphorus is present at rates higher than 1,000 mg dm-3. Moreover, a small amount of applied glyphosate was extracted (<10%, and the extraction increased with increasing soil phosphorus content.

  5. Time-Dependent Zinc Desorption in Some Calcareous Soils of Iran

    Institute of Scientific and Technical Information of China (English)

    M.BARANIMOTLAGH; M.GHOLAMI

    2013-01-01

    Desorption of zinc (Zn) from soil is an important factor governing Zn concentration in the soil solution and Zn availability to plants.Batch experiments were performed to study the kinetics of Zn desorption by diethylenetriaminepentaacetic acid (DTPA) from 15 calcareous soil samples taken from Golestan Province in northern Iran.Soils were equilibrated with 0.005 mol L-1 DTPA solutions for 0.25 to 192 h.The results showed that the extraction process consisted of rapid extraction in the first 2 h followed by much slower extraction for the remainder of the experiment.Desorption kinetic data was fitted to pseudo-first-order kinetic model.The experimental data were found to deviate from the straight line of the pseudo-first-order plots after 2 h.The model of two first-order reactions was fitted to the kinetic data and allowed to distinguish two pools for Zn:a labile fraction (Q1),quickly extracted with a rate constant k1,and a slowly labile fraction (Q2),more slowly extracted with a rate constant k2.The applicability of pseudo-second-order model in describing the kinetic data of Zn desorption was also evaluated.

  6. Effects of surface coordination on the temperature-programmed desorption of oxalate from goethite

    Energy Technology Data Exchange (ETDEWEB)

    Boily, Jean F.; Szanyi, Janos; Felmy, Andrew R.

    2007-11-15

    The temperature-programmed desorption (TPD) of weakly-bound, hydrogen-bonded and metal-bonded oxalate complexes at the goethite surface was investigated in the 300-900 K range with concerted Fourier Transform Infrared (FTIR) measurements (TPD-FTIR). These reactions took place with the concomitant dehydroxylation reaction of goethite to hematite and decarbonation of bulk-occluded carbonate. The measurements revealed three important stages of desorption. Stage I (300-440 K) corresponds to the desorption of weakly-and/or un-bound oxalate molecules in the goethite powder with a thermal decomposition reaction pathway characteristic of oxalic acid. Stage II (440-520 K) corresponds to a thermally-driven dehydration of hydrogen-bonded surface complexes, leading to a partial desorption via oxalic acid thermal decomposition pathways and to a partial conversion to metal-bonded surface complexes. This latter mechanism led to the increase in FTIR bands characteristic of these complexes. Finally, Stage III (520-660 K) corresponds to the thermal decomposition of the metal-bonded oxalate complex, proceeding through a 2 electron reduction pathway.

  7. A photoluminescence study of indium desorption from strained Ga sub 1-x In sub x As/GaAs

    Energy Technology Data Exchange (ETDEWEB)

    Emeny, M.T.; Whitehouse, C.R. (Royal Signals and Radar Establishment, Great Malvern (UK)); Howard, L.K.; Lambkin, J.D. (Strained Layer Structures Group, Univ. of Surrey, Guildford (UK)); Homewood, K.P. (Dept. of Electronic and Electrical Engineering, Univ. of Surrey, Guildford (UK))

    1991-05-01

    In this paper we present detailed measurements of the thermal desorption rates of indium from strained GaInAs grown off a GaAs substrate. We have made these measurements by monitoring the photoluminescence (PL) of the groundstate emission from strained quantum wells. We show that this method can be an accurate and highly sensitive technique for measuring desorption rates. The measurements have been made as a function of composition and arsenic overpressure. A simple model for the indium incorporation is developed and an activation energy for the desorption process has been obtained. (orig.).

  8. Gender Recognition from Human-Body Images Using Visible-Light and Thermal Camera Videos Based on a Convolutional Neural Network for Image Feature Extraction.

    Science.gov (United States)

    Nguyen, Dat Tien; Kim, Ki Wan; Hong, Hyung Gil; Koo, Ja Hyung; Kim, Min Cheol; Park, Kang Ryoung

    2017-03-20

    Extracting powerful image features plays an important role in computer vision systems. Many methods have previously been proposed to extract image features for various computer vision applications, such as the scale-invariant feature transform (SIFT), speed-up robust feature (SURF), local binary patterns (LBP), histogram of oriented gradients (HOG), and weighted HOG. Recently, the convolutional neural network (CNN) method for image feature extraction and classification in computer vision has been used in various applications. In this research, we propose a new gender recognition method for recognizing males and females in observation scenes of surveillance systems based on feature extraction from visible-light and thermal camera videos through CNN. Experimental results confirm the superiority of our proposed method over state-of-the-art recognition methods for the gender recognition problem using human body images.

  9. Effect of Extractant and Cold-drawing on the Structure and Performance of HDPE Hollow Fiber Membranes Fabricated via Thermally Induced Phase Separation Method

    Institute of Scientific and Technical Information of China (English)

    WANG Jian-li; RUAN Wen-xiang; SONG Yi-lin; JI Jian-bing; YAO Ke-jian

    2006-01-01

    Microporous polyolefin hollow fiber membranes were prepared from high density polyethylene (HDPE)-paraffin solution via thermally induced phase separation (TIPS)method. Effects of extraction and cold-drawing condition on membrane structure and performance were investigated.Five volatile solvents were used as extractant. Dimension of hollow fiber and gas permeation rate of membrane were measured. Microstructure of membrane was examined by Scanning Electronic Microscope (SEM). The results show that the membrane treated by pentane possesses a higher porosity, nitrogen permeability and lower shrinkage than those of membranes extracted by other three extractants. It is also found that thc membrane stretched 133% shows the highest porosity and gas permeability in this study.

  10. Gender Recognition from Human-Body Images Using Visible-Light and Thermal Camera Videos Based on a Convolutional Neural Network for Image Feature Extraction

    Science.gov (United States)

    Nguyen, Dat Tien; Kim, Ki Wan; Hong, Hyung Gil; Koo, Ja Hyung; Kim, Min Cheol; Park, Kang Ryoung

    2017-01-01

    Extracting powerful image features plays an important role in computer vision systems. Many methods have previously been proposed to extract image features for various computer vision applications, such as the scale-invariant feature transform (SIFT), speed-up robust feature (SURF), local binary patterns (LBP), histogram of oriented gradients (HOG), and weighted HOG. Recently, the convolutional neural network (CNN) method for image feature extraction and classification in computer vision has been used in various applications. In this research, we propose a new gender recognition method for recognizing males and females in observation scenes of surveillance systems based on feature extraction from visible-light and thermal camera videos through CNN. Experimental results confirm the superiority of our proposed method over state-of-the-art recognition methods for the gender recognition problem using human body images. PMID:28335510

  11. Recovery of naringin from kinnow (Citrus reticulata Blanco) peels by adsorption–desorption technique using an indigenous resin

    Indian Academy of Sciences (India)

    M LAXMI DEEPAK BHATLU; SATYA VIR SINGH; ASHOK KUMAR VERMA

    2017-01-01

    A process technology has been developed for recovery of naringin from kinnow (citrus) peels,which is a waste. The kinnow peels were boiled with water to extract naringin into water. It was adsorbed on an indigenous macroporous resin, Indion PA-500. Naringin was recovered from the saturated resin by desorption with ethanol as a solvent. The equilibrium and kinetic studies for both adsorption and desorption are presented.The Langmuir isotherm described the adsorption equilibrium data. However, desorption data were best described by the Toth isotherm. Adsorption and desorption kinetic data were found to follow a pseudo-secondorder rate equation and second-order rate equation, respectively. Recovery of naringin was about 49% w/w (based on naringin present in peel-boiled extract). The purity of final products was 91–94% w/w.

  12. Infrared laser desorption/ionization on silicon.

    Science.gov (United States)

    Bhattacharya, Sucharita H; Raiford, Timothy J; Murray, Kermit K

    2002-05-01

    Laser desorption/ionization from a single-crystal silicon surface was performed using a laser operating in the 3-microm region of the mid-infrared. Analyte molecules up to 6 kDa were ionized with no added matrix. As with ultraviolet desorption/ionization from porous silicon (DIOS), IR laser desorption from silicon does not produce matrix ions that can interfere with analysis of low-mass analytes. However, in contrast to UV DIOS, silicon porosity or roughness is not required for ionization using an IR laser. Mass spectra were obtained in the wavelength range between 2.8 and 3.5 microm, which is consistent with energy absorption by a hydrogen-bonded OH group. A mechanism based on desorption of adsorbed solvent molecules is postulated.

  13. Survival of HCl( v=2) in trapping-desorption from MgO(100)

    Science.gov (United States)

    Korolik, M.; Suchan, M. M.; Johnson, M. J.; Arnold, D. W.; Reisler, H.; Wittig, C.

    2000-08-01

    An HCl molecular beam incident on MgO(100) is photoexcited to v=2, J=1 by using a pulsed parametric oscillator. At a translational energy of 0.11 eV, incident HCl is adsorbed. Thermal desorption yields v=2 molecules whose rotational and translational degrees of freedom are equilibrated at the surface temperature. Surface residence times for v=2 might be as long as 1 μs. At 180 K, it is concluded that a large fraction of surface-bound v=2 molecules reenter the gas phase, while at 120 K, deactivation exceeds desorption by an order of magnitude. Deactivation probably takes place at steps.

  14. Adsorption, desorption and bioregeneration in the treatment of 2-chlorophenol with activated carbon.

    Science.gov (United States)

    Aktaş, Ozgür; Ceçen, Ferhan

    2007-03-22

    This study aims to clarify the effect of activated carbon type on the extent of adsorbability, desorbability, and bioregenerability in the treatment of 2-chlorophenol. Four different activated carbon types; thermally activated and chemically activated powdered carbons (PAC), and their granular countertypes (GAC) with similar physical characteristics were used. Thermally activated carbons adsorbed 2-chlorophenol much better than chemically activated ones. However, adsorption was more reversible in the case of chemically activated ones. The use of powdered and granular activated carbon countertypes resulted in comparable adsorption and desorption characteristics. For each activated carbon type, 2-chlorophenol exhibited higher adsorbability and lower desorbability than phenol. Biodegradation of 2-chlorophenol took place very slowly when it was used as the sole carbon source in acclimated and non-acclimated activated sludges. Bioregeneration occurred only via desorption due to an initial concentration gradient and no further desorption took place due to low biodegradability. Bioregeneration of activated carbon loaded with 2-chlorophenol was not a suitable option when 2-chlorophenol was the only carbon source. It is suggested to remove 2-chlorophenol via adsorption onto activated carbon rather than applying biological treatment. Also in such cases, the use of thermally activated carbons with higher adsorption and lower desorption capacities is recommended rather than chemically activated carbons.

  15. Thermal Desorption-Gas Chromatography or Gas Chromatograph-Mass Spectrometry for Analysis of Semi-Volatile Compounds on Atmospheric Particulate Matters%热解析-气相色谱或气相色谱-质谱法分析大气可吸入颗粒物中的半挥发性有机化合物

    Institute of Scientific and Technical Information of China (English)

    孟虎; 赵景红; 段春凤; 郝亮; 关亚风

    2014-01-01

    A thermal desorption ( TD) device was developed and coupled to gas chromatography ( GC) or gas chromatography-mass spectrometry ( GC-MS ) for the qualitative and quantitative analysis of semi-volatile organic compounds on atmospheric particulate matters ( PM ) . The TD was operated by direct heating and placed on the GC injector, leading to high heating rate and easy transfer of analytes to GC without focusing of analytes by cold trap. For establishing the TD-GC method, the materials used for supporting PM samples, temperature and time of thermal desorption, and types of sample injection were investigated for detection of sixteen polycyclic aromatic hydrocarbons ( PAHs) and nine n-alkanes. The limits of detection of the proposed TD-GC method were in the range of 0. 014-0. 093 ng for PAHs, and 0. 016-0. 026 ng for n-alkanes, respectively, with the correlation coefficients of correlation above 0. 9975. The TD-GC method was applied to the determination of trace PAHs and n-alkanes on PM10 samples from three cities. The recoveries were in the range of 95%-135% ( PAHs) and 95%-115% ( n-alkanes) , respectively. Finally, the TD was coupled to GC-MS for comparison of the contents of PAHs and n-alkanes on PMx with different particulate size ( x=10 , 5, 2, 1, 0. 5, 0. 25, 0. 1).%研制了一种热解析装置,并与气相色谱或气相色谱-质谱联用,定性定量分析了大气可吸入颗粒物中的半挥发性有机物。装置为直热式加热,升温速率快;直接安装在色谱进样器上方,无需冷阱聚焦。将热解析装置与气相色谱联用,优化了样品承载体材质、热解析条件和进样模式,并用于16种多环芳烃和9种正构烷烃的检测。结果表明,热解析-气相色谱方法对多环芳烃和正构烷烃的检出限分别为0.014~0.093 ng和0.016~0.026 ng,线性相关系数大于0.9975;用于3个城市PM10中的痕量多环芳烃和正构烷烃的定量测定,回收率分别在95%~135%(多环芳烃)和95%~115%(正构烷

  16. Effects of High Temperature and Thermal Cycling on the Performance of Perovskite Solar Cells: Acceleration of Charge Recombination and Deterioration of Charge Extraction

    KAUST Repository

    Sheikh, Arif D.

    2017-09-18

    In this work, we investigated the effects of high operating temperature and thermal cycling on the photovoltaic performance of perovskite solar cells (PSCs) with a typical mesostructured (m)-TiO2-CH3NH3PbI3-xClx-spiro-OMeTAD architecture. After carrying out temperature-dependent grazing incidence wide-angle X-ray scattering (GIWAXS), in-situ X-ray diffraction (XRD) and optical absorption experiments, thermal durability of PSCs was tested by subjecting the devices to repetitive heating to 70 °C and cooling to room temperature (20 °C). An unexpected regenerative effect was observed after the first thermal cycle; the average power conversion efficiency (PCE) increased by approximately 10 % in reference to the as-prepared device. This increase of PCE was attributed to the heating-induced improvement of crystallinity and p-doping in the hole-transporter, Spiro-OMeTAD, which promotes the efficient extraction of photo-generated carriers. However, further thermal cycles produced a detrimental effect on the photovoltaic performance of PSCs with short-circuit current and fill factor degrading faster than the open-circuit voltage. Similarly, the photovoltaic performance of PSCs degraded at high operation temperatures; both short-circuit current and open-circuit voltage decreased with increasing temperature, but the temperature-dependent trend of fill factor was opposite. Our impedance spectroscopy analysis revealed a monotonous increase of charge transfer resistance and a concurrent decrease of charge recombination resistance with increasing temperature, indicating high recombination of charge carriers. Our results revealed that both thermal cycling and high temperatures produce irreversible detrimental effects on the PSC performance due to the deteriorated interfacial photo-carrier extraction. The present findings suggest that development of robust charge transporters and proper interface engineering are critical for the deployment of perovskite photovoltaics in harsh

  17. Feasibility of desorption atmospheric pressure photoionization and desorption electrospray ionization mass spectrometry to monitor urinary steroid metabolites during pregnancy.

    Science.gov (United States)

    Vaikkinen, Anu; Rejšek, Jan; Vrkoslav, Vladimír; Kauppila, Tiina J; Cvačka, Josef; Kostiainen, Risto

    2015-06-23

    Steroids have important roles in the progress of pregnancy, and their study in maternal urine is a non-invasive method to monitor the steroid metabolome and its possible abnormalities. However, the current screening techniques of choice, namely immunoassays and gas and liquid chromatography-mass spectrometry, do not offer means for the rapid and non-targeted multi-analyte studies of large sample sets. In this study, we explore the feasibility of two ambient mass spectrometry methods in steroid fingerprinting. Urine samples from pregnant women were screened by desorption electrospray ionization (DESI) and desorption atmospheric pressure photoionization (DAPPI) Orbitrap high resolution mass spectrometry (HRMS). The urine samples were processed by solid phase extraction for the DESI measurements and by enzymatic hydrolysis and liquid-liquid-extraction for DAPPI. Consequently, steroid glucuronides and sulfates were detected by negative ion mode DESI-HRMS, and free steroids by positive ion mode DAPPI-HRMS. In DESI, signals of eleven steroid metabolite ions were found to increase as the pregnancy proceeded, and in DAPPI ten steroid ions showed at least an order of magnitude increase during pregnancy. In DESI, the increase was seen for ions corresponding to C18 and C21 steroid glucuronides, while DAPPI detected increased excretion of C19 and C21 steroids. Thus both techniques show promise for the steroid marker screening in pregnancy.

  18. Evaluation of sorption-desorption processes for metalaxyl in natural and artificial soils.

    Science.gov (United States)

    Sukul, Premasis; Lamshöft, Marc; Zühlke, Sebastian; Spiteller, Michael

    2013-01-01

    The main process controlling soil-pesticide interaction is the sorption-desorption as influenced by active soil surfaces. The sorption phenomena can influence translocation, volatility, persistence and bioactivity of a pesticide in soil. The present investigation was conducted on natural and artificial soils in order to enumerate the effect of soil components such as montmorillonite and ferrihydrite on the sorption behaviour of the fungicide metalaxyl and if sorption-desorption of the chiral pesticide affects the enantiomeric ratio. The sorption-desorption characteristics of metalaxyl were investigated by batch equilibration technique in a natural soil, two artificial soils, and in pure montmorillonite and ferrihydrite. After extraction, pesticide residues were analyzed by conventional and chiral chromatography using tandem mass spectrometry. A KdSorp (2.3-6.5) suggests low level sorption of metalaxyl with an appreciable risk of run-off and leaching. Thus, metalaxyl poses a threat to surface and ground water contamination. Furthermore, desorption tests revealed a hysteretic effect (H ≤ 0.8) in natural and artificial soils. Significant amount of metalaxyl was found tightly bound to the adsorbents without desorbing readily after desorption cycle. Desorption of 22-56% of the total amount of the retained metalaxyl was determined. This study reveals that an artificial soil derived from different soil constituents can be used to assess their influence on sorption/desorption processes. The present investigation showed that both montmorillonite and ferrihydrite play a significant role in the sorption of metalaxyl. The sorption doesn't influence the enantiomeric ratio of racemic metalaxyl.

  19. Adsorption and Desorption of Methiopyrsulfuron in Soils

    Institute of Scientific and Technical Information of China (English)

    WU Chun-Xian; WANG Jin-Jun; ZHANG Su-Zhi; ZHANG Zhong-Ming

    2011-01-01

    Methiopyrsulfuron is a new low-rate sulfonylurea herbicide for weed control in wheat; however, there is a lack of published information on its behavior in soils. In this study, methiopyrsulfuron adsorption and desorption were measured in seven soils sampled from Heilongjiang, Shandong, Jiangxi, Sichuan, Anhui, and Chongqing provinces of China using a batch equilibrium method. The Freundlich equation was used to described its adsorption and desorption. Adsorption isotherms were nonlinear with the values of Kf-ads, the Freundlich empirical constant indicative of the adsorption capacity,ranging from 0.75 to 2.46, suggesting that little of this herbicide was adsorbed by any of the seven soils. Soil pH and organic matter content (OM) were the main factors influencing adsorption; adsorption was negatively correlated with pH and positively correlated with OM. Methiopyrsulfuron desorption was hysteretic on the soils with high OM content and low pH.

  20. Ionic Adsorption and Desorption of CNT Nanoropes

    Directory of Open Access Journals (Sweden)

    Jun-Jun Shang

    2016-09-01

    Full Text Available A nanorope is comprised of several carbon nanotubes (CNTs with different chiralities. A molecular dynamic model is built to investigate the ionic adsorption and desorption of the CNT nanoropes. The charge distribution on the nanorope is obtained by using a modified gradient method based on classical electrostatic theory. The electrostatic interactions among charged carbon atoms are calculated by using the Coulomb law. It was found here that the charged nanorope can adsorb heavy metal ions, and the adsorption and desorption can be realized by controlling the strength of applied electric field. The distance between the ions and the nanorope as well as the amount of ions have an effect on the adsorption capacity of the nanorope. The desorption process takes less time than that of adsorption. The study indicates that the CNT nanorope can be used as a core element of devices for sewage treatment.

  1. Long-term tillage effects on soil metolachlor sorption and desorption behavior.

    Science.gov (United States)

    Ding, Guangwei; Novak, Jeffrey M; Herbert, Stephen; Xing, Baoshan

    2002-09-01

    Sorption and desorption are two important processes that influence the amount of pesticides retained by soils. However, the detailed sorption mechanisms as influenced by soil tillage management are unclear. This study examined the sorption and desorption characteristics of metolachlor [2-chloro-N-(2-ethyl-6-methyphenyl)-N-(2-methoxy-1-methylethyl)-acetamide] using the soil samples collected from the long-term conservation tillage (CnT) and conventional tillage (CT) research plots established in 1979 in Darlinton, SC. Humic acid (HA) and humin were extracted from the soils and used in the sorption experiments along with the whole soil samples. The sorption experiments were conducted using a batch-equilibration method. Three sequential desorption rinses were carried out following the sorption experiments. By comparing metolachlor sorption and desorption results we observed hysteresis for all soil samples and their organic matter fractions. Sorption nonlinearity (N) and hysteresis were dependent on the structure and composition of soil organic matter (SOM), e.g., Freundlich isotherm exponents (N) of HA and humin from CnT were higher than those of CT treatment, which may be related to high aromaticity of SOM fractions in CT treatment. Sorption capacity (K'f) was positively correlated with soil organic carbon (SOC) content. These results show that long-term tillage management can greatly affect metolachlor sorption and desorption behavior probably by qualitative differences in the structural characteristics of the humic substances.

  2. Effect of Dissolved Organic Matter on Chlorotoluron Sorption and Desorption in Soils

    Institute of Scientific and Technical Information of China (English)

    YANG Hong; WU Xin; ZHOU Li-Xiang; YANG Zhi-Min

    2005-01-01

    A batch equilibrium techniques was used to examine the effect of dissolved organic matter (DOM) extracted from both non-treated sludge (NTS) and heat-expanded sludge (HES) on the sorption and desorption of chlorotoluron (3-(3-chloro-p-tolyl)-1,1-dimethylurea) in two types of soils, a yellow fluvo-aquic and a red soil from China. Without DOM,sorption of chlorotoluron was significantly greater (P < 0.05) in the red soil than in the yellow fluvo-aquic soil. However,with DOM the effect was dependent on the soil type and nature of DOM. Chlorotoluron sorption was lower in the yellow fluvo-aquic soil than in the red soil, suggesting that with the same DOM levels the yellow fluvo-aquic soil had a lower sorption capacity for this herbicide. Application of DOM from both NTS and HES led to a general decrease in sorption to the soils and an increase in desorption from the soils. Desorption of chlorotoluron also significantly increased (P < 0.05)with an increase in the DOM concentration. Additionally, for sorption and desorption, at each DOM treatment level the NTS treatments were significantly lower (P < 0.05) than the HES treatments. This implied that non-treated sludge had a greater effect on the sorption and desorption of chlorotoluron than heat-expanded sludge.

  3. Water desorption from nanostructured graphite surfaces.

    Science.gov (United States)

    Clemens, Anna; Hellberg, Lars; Grönbeck, Henrik; Chakarov, Dinko

    2013-12-21

    Water interaction with nanostructured graphite surfaces is strongly dependent on the surface morphology. In this work, temperature programmed desorption (TPD) in combination with quadrupole mass spectrometry (QMS) has been used to study water ice desorption from a nanostructured graphite surface. This model surface was fabricated by hole-mask colloidal lithography (HCL) along with oxygen plasma etching and consists of a rough carbon surface covered by well defined structures of highly oriented pyrolytic graphite (HOPG). The results are compared with those from pristine HOPG and a rough (oxygen plasma etched) carbon surface without graphite nanostructures. The samples were characterized using scanning electron microscopy (SEM) and atomic force microscopy (AFM). The TPD experiments were conducted for H2O coverages obtained after exposures between 0.2 and 55 langmuir (L) and reveal a complex desorption behaviour. The spectra from the nanostructured surface show additional, coverage dependent desorption peaks. They are assigned to water bound in two-dimensional (2D) and three-dimensional (3D) hydrogen-bonded networks, defect-bound water, and to water intercalated into the graphite structures. The intercalation is more pronounced for the nanostructured graphite surface in comparison to HOPG surfaces because of a higher concentration of intersheet openings. From the TPD spectra, the desorption energies for water bound in 2D and 3D (multilayer) networks were determined to be 0.32 ± 0.06 and 0.41 ± 0.03 eV per molecule, respectively. An upper limit for the desorption energy for defect-bound water was estimated to be 1 eV per molecule.

  4. 5th International Workshop on Desorption Induced by Electronic Transitions

    CERN Document Server

    Jennison, Dwight R; Stechel, Ellen B; DIET V; Desorption induced by electronic transitions

    1993-01-01

    This volume in the Springer Series on Surface Sciences presents a recent account of advances in the ever-broadening field of electron-and photon-stimulated sur­ face processes. As in previous volumes, these advances are presented as the proceedings of the International Workshop on Desorption Induced by Electronic Transitions; the fifth workshop (DIET V) was held in Taos, New Mexico, April 1-4, 1992. It will be abundantly clear to the reader that "DIET" is not restricted to desorption, but has for several years included photochemistry, non-thermal surface modification, exciton self-trapping, and many other phenomena that are induced by electron or photon bombardment. However, most stimulated surface processes do share a common physics: initial electronic excitation, localization of the excitation, and conversion of electronic energy into nuclear kinetic energy. It is the rich variation of this theme which makes the field so interesting and fruitful. We have divided the book into eleven parts in orde...

  5. Development of a thermal desorption modulator for gas chromatography

    NARCIS (Netherlands)

    Geus, H.J.; Boer, de J.; Brinkman, U.A.Th.

    1997-01-01

    The separation space in gas chromatography can be enhanced dramatically by the comprehensive coupling of two independent separation dimensions. An interface between the two columns must accumulate analytes eluting from the first dimension, focus them and at the appropriate moment transfer them to th

  6. Electronic Desorption of gas from metals

    Energy Technology Data Exchange (ETDEWEB)

    Molvik, A W; Kollmus, H; Mahner, E; Covo, M K; Bender, M; Bieniosek, F M; Kramer, A; Kwan, J; Prost, L; Seidl, P A; Westenskow, G

    2006-11-02

    During heavy ion operation in several particle accelerators world-wide, dynamic pressure rises of orders of magnitude were triggered by lost beam ions that bombarded the vacuum chamber walls. This ion-induced molecular desorption, observed at CERN, GSI, and BNL, can seriously limit the ion beam lifetime and intensity of the accelerator. From dedicated test stand experiments we have discovered that heavy-ion induced gas desorption scales with the electronic energy loss (dE{sub e}/dx) of the ions slowing down in matter; but it varies only little with the ion impact angle, unlike electronic sputtering.

  7. Pain Modulation by Lignans (Phyllanthin and Hypophyllanthin) and Tannin (Corilagin) Rich Extracts of Phyllanthus amarus in Carrageenan-induced Thermal and Mechanical Chronic Muscle Hyperalgesia.

    Science.gov (United States)

    Chopade, Atul R; Sayyad, F J

    2015-08-01

    The current study was aimed at evaluating the antihyperalgesic effects of lignans (phyllanthin and hypophyllanthin) and tannin (corilagin) rich three standardized extracts of Phyllanthus amarus in a model of chronic musculoskeletal inflammatory pain. Three percent carrageenan injected in the gastrocnemius muscle produced hyperalgesia to mechanical and heat stimuli ipsilaterally, which spreads to the contralateral side within 7 to 9 days. To investigate the effects on chronic thermal and mechanical hypersensitivity, three extracts of P. amarus in three doses (100, 200, and 400 mg/kg) were administered to animals intraperitoneally from 14th day to 22nd day after intramuscular injection of carrageenan. It was observed that intraperitoneal administrations of Phyllanthus extracts showed antihyperalgesic activity, as they elevated thermal and mechanical threshold, which was supported by histopathological observations along with reduction in prostaglandin E2 (PGE2) concentration. In conclusion, we strongly suggest that the observed antihyperalgesic and antiinflammatory effects of P. amarus in current pain model are mediated via spinal or supraspinal neuronal mechanisms, mainly by inhibition of PGE2. Modulation of chronic muscular inflammation may be due to presence of phytoconstituents like phyllanthin, hypophyllanthin, and corilagin, which offers a promising means for treatment of chronic muscle pain.

  8. Effects of water re-saturation conditions and associated extractives leaching on thermal softening of wet wood

    OpenAIRE

    BREMAUD, Iris; Bardet, Sandrine; Gril, Joseph; Perré, Patrick

    2014-01-01

    International audience; Thermal softening, or thermo-activated viscoelasticity, is involved in several industrial and/or traditional craftsmanship techniques processing of wood. More fundamentally, it represents a very useful probe of chemical differences and/or of physical histories of wood samples [1,2,3,4,5]. Thermal softening of wet (= water-saturated) wood occurs at much lower temperature than that of completely (anhydrous) dried wood [6,7]. Softening of oven-dry wood happens at temperat...

  9. Flash Thermal Conditioning of Olive Pastes during the Oil Mechanical Extraction Process: Cultivar Impact on the Phenolic and Volatile Composition of Virgin Olive Oil.

    Science.gov (United States)

    Veneziani, Gianluca; Esposto, Sonia; Taticchi, Agnese; Selvaggini, Roberto; Urbani, Stefania; Di Maio, Ilona; Sordini, Beatrice; Servili, Maurizio

    2015-07-08

    The concentration of phenolic and volatile compounds in virgin olive oil (VOO) is closely related to the different operative conditions applied to the mechanical extraction process of the olive oil. However, the great qualitative and quantitative variability of these compounds indicates an important role played by genetic and agronomic aspects. A heat exchanger was placed in front of a traditional, covered malaxer to study the impact of flash thermal conditioning (FTC) of olive paste on the quality of VOO, which is highly influenced by phenolic release and aroma generation. The VOO flash thermal conditioning of five major Italian cultivars showed a higher concentration of phenols (range of increase percentage, 9.9-37.3%) compared to the control trials, whereas the FTC treatment featured a differentiated impact on the volatile fractions, associated with the genetic origins of the olives.

  10. Flash thermal conditioning of olive pastes during the olive oil mechanical extraction process: impact on the structural modifications of pastes and oil quality.

    Science.gov (United States)

    Esposto, Sonia; Veneziani, Gianluca; Taticchi, Agnese; Selvaggini, Roberto; Urbani, Stefania; Di Maio, Ilona; Sordini, Beatrice; Minnocci, Antonio; Sebastiani, Luca; Servili, Maurizio

    2013-05-22

    The quality of virgin olive oil (VOO) is strictly related to the concentrations of phenolic and volatile compounds, which are strongly affected by the operative conditions of the VOO mechanical extraction process. The aim of this work is to study the impact of a new technology such as flash thermal conditioning (FTC) on olive paste structural modification and on VOO quality. The evaluation of olive paste structure modification by cryo-scanning electron microscopy (cryo-SEM) showed that the application of FTC after crushing produces significant differences in terms of the breaking of the parenchyma cells and aggregation of oil droplets in comparison to the crushed pastes. The virgin olive oil flash thermal conditioning (VOO-FTC) featured a higher concentration of volatile compounds compared to that in the control, particularly of all saturated and unsaturated aldehydes and esters, whereas the phenolic concentration was higher in VOO obtained from the traditional process (VOO-C).

  11. Thermal and electrostatic simulations of the diagnostic calorimeter for the source for production of ion of deuterium extracted from RF plasma beam.

    Science.gov (United States)

    Serianni, G; Dalla Palma, M; De Muri, M; Fasolo, D; Pasqualotto, R; Pomaro, N; Rizzolo, A; Tollin, M

    2012-02-01

    To study and optimise negative ion production for the ITER neutral beam injectors, a test facility is under construction in Padova with the aim of testing beam characteristics and to verify the source proper operation. The instrumented calorimeter STRIKE (short-time retractable instrumented kalorimeter experiment) is being developed to characterise the SPIDER (Source for Production of Ion of Deuterium Extracted from RF plasma) beam during short operations. The paper presents an investigation of the response of STRIKE measurement systems. It results that biasing is necessary to cope with the influence of secondary electrons on current measurements; moreover, despite the discretisation of the recorded thermal patterns introduced by the pixels of thermal cameras, a sufficient spatial resolution is expected.

  12. Quantum theory of laser-stimulated desorption

    Science.gov (United States)

    Slutsky, M. S.; George, T. F.

    1978-01-01

    A quantum theory of laser-stimulated desorption (LSDE) is presented and critically analyzed. It is shown how LSDE depends on laser-pulse characteristics and surface-lattice dynamics. Predictions of the theory for a Debye model of the lattice dynamics are compared to recent experimental results.

  13. A microsystems enabled field desorption source.

    Energy Technology Data Exchange (ETDEWEB)

    Hertz, Kristin L.; Resnick, Paul James; Schwoebel, Paul R. (University of New Mexico, Albuquerque, NM); Holland, Christopher E. (SRI International, Menlo Park, CA); Chichester, David L. (Idaho National Laboratory, Idaho Falls, ID)

    2010-07-01

    Technologies that have been developed for microelectromechanical systems (MEMS) have been applied to the fabrication of field desorption arrays. These techniques include the use of thick films for enhanced dielectric stand-off, as well as an integrated gate electrode. The increased complexity of MEMS fabrication provides enhanced design flexibility over traditional methods.

  14. Product desorption limitations in selective photocatalytic oxidation

    NARCIS (Netherlands)

    Renckens, T.J.A.; Almeida, A.R.; Damen, M.R.; Kreutzer, M.T.; Mul, G.

    2010-01-01

    The rate of photocatalytic processes can be significantly improved if strongly bound products rapidly desorb to free up active sites. This paper deals with the rate of desorption of cyclohexanone, the product of the liquid-phase photo-oxidation of cyclohexane. Dynamic step-response and pulse-respons

  15. 热降解辅助表面解吸常压化学电离质谱对阿莫西林的分析%Analysis of amoxicillin by surface desorption atmospheric pressure chemical ionization mass spectrometry aided with thermal degradation

    Institute of Scientific and Technical Information of China (English)

    陈荣; 邓慧宇; 石俊

    2012-01-01

    To establish a novel approach to the high throughput screening of amoxicillin by direct surface desorption atmospheric pressure chemical ionization -mass spectrometry aided with thermal degradation(TD -SDAP-CI - MS). Methods; Water in the air act as the reactive reagent responsible for the generation of ions in the positive corona discharge. The rapid screening effectiveness of the combination of TD and SDAPGI was demonstrated by application to comparing the total ion current mass spectrum of degradation ingredient ions to ion current mass spectrum of amoxicillin capsules which were observed in full scan mass spectrometry (MS) mode. Collision -induced dissociation of protonated molecules gave characteristic product - ion mass spectra and provided further identification of amoxicillin degradation ingredients. Results: The high throughput screening of amoxicillin was realized by mass spectrum without sample pretreatment and separation step. Conclusions: A single sample analysis is completed in less than 30 seconds. The data show TD - SDAPCI - MS is a convenient tool for high throughtout screening of unstable amoxicillin.%目的:建立一种阿莫西林热降解辅助表面解吸常压化学电离质谱(TD - SDAPCI - MS)快速检测新方法.方法:利用阿莫西林抗生素的易降解并产生特定降解产物的特性,以潮湿空气作为试剂,通过电晕放电产生大量试剂离子,对阿莫西林抗生素总离子流质谱图与特征降解产物离子流图进行比对.并通过串联质谱对阿莫西林抗生素产生的特征降解产物进行了确认.结果:无需样品预处理,实现一级质谱法对阿莫西林抗生素的高通量筛选.结论:单个样品检测不超过30 s,可实现不稳定抗生素阿莫西林的高通量筛选.

  16. 吸附-热解吸法与气相色谱-质谱法联用测定蚊香烟雾中的有机化合物%Determination of Organic Compounds in the Smog of Mosquito-Repellent Incense by Adsorption-Thermal Desorption-GC/MS

    Institute of Scientific and Technical Information of China (English)

    刘秀华; 钟志京; 孟丹; 丁兰岚; 田军华

    2012-01-01

    利用吸附-热解吸法与气相色谱-质谱法联用,对两种固体蚊香烟气中的有机成分进行定性和半定量分析.在两种固体蚊香烟气中共检测出52种挥发性成分,包括酚类、醇类、醛类以及脂肪烃和芳香烃等多种化合物,其中的部分化合物对人体有毒害作用.蚊香A烟气中含量较多的成分为右旋烯丙菊酯(30.06%)、1,6-脱水-β-D-吡喃葡萄糖(19.4%)和甘菊环(13.9%)等;蚊香B烟气中含量较多的成分为1,6-脱水-β-D-吡喃葡萄糖(24.4%)、甘菊环(14.4%)和正十四烷(5.91%)等.%The organic components in the smog of mosquito-repellent incense were analyzed qualitatively and semi-quantitatively by adsorption-thermal desorption with gas chromatog-raphy-mass spectrometry. 52 kinds of compounds are identified in two kinds of solid mosquito-repellent incenses, including phenolic compounds, alcohols, aldehydes, aliphatic hydrocarbons, aromatic hydrocarbons and so on. Some compounds are poisonous to people's health. The principal components in the smog of mosquito-repellent incense A are allethrin (30.06%), l,6-Anhydro-β-D-glucopyranose(19. 4%), azulene(13. 9%) , while the principal components are 1,6-Anhydro-β-D-glucopyranose(24. 4%), azulene(14. 4%), tetrade-cane(5. 91%) for the mosquito-repellent incense B.

  17. Thermal stability of oils added with avocado (Persea americana cv. Hass) or olive (Olea europaea cv. Arbequina) leaf extracts during the French potatoes frying.

    Science.gov (United States)

    Jiménez, Paula; García, Paula; Bustamante, Andrés; Barriga, Andrés; Robert, Paz

    2017-04-15

    Effect of the addition of avocado (Persea americana cv. Hass) or olive (Olea europaea cv. Arbequina) hydroalcoholic leaf extracts (AHE and OHE, respectively) on thermal stability of canola oil (CO) and high oleic sunflower oil (HOSO) during French potatoes frying at 180°C was studied. The extracts were characterized by the total phenolic content, phenol chromatographic profiles and antioxidant activity. B-type trimer procyanidins were the major phenolic compounds identified in AHE. OHE showed higher phenol content, antioxidant activity regarding AHE. CO+OHE and HOSO+OHE decreased the formation of polar compounds and showed an anti-polymeric effect with respect to oils without extracts, whereas AHE extract showed a prooxidant effect on HOSO. Therefore, OHE showed an antioxidant effect on HOSO and CO under the studied conditions. In addition, all systems (CO+AHE, HOSO+AHE, CO+OHE and HOSO+OHE) increased the retention of tocopherols. These results demonstrate the potential utility of OHE as natural antioxidant for oils. Copyright © 2016 Elsevier Ltd. All rights reserved.

  18. Ultrafast Desorption by Impulsive Vibrational Excitation (DIVE). Applications in laser surgery, mass spectrometry and towards ultimate limits in biodiagnosis

    Energy Technology Data Exchange (ETDEWEB)

    Ren, Ling

    2015-07-15

    The prospects for minimally invasive surgery, spatial imaging with mass spectrometry and rapid high throughput biodiagnosis require new means of tissue incision and biomolecule extraction with conserved molecular structure. Towards this aim, a laser ablation process is utilized in this dissertation, which is capable of performing precise tissue incision with minimal collateral damage and extracting intact biological entities with conserved biological functions. The method is based on the recently developed Picosecond Infrared Laser (PIRL) designed to excite selectively the water vibrational modes under the condition of ultrafast Desorption by Impulsive Vibrational Excitation (DIVE). The basic concept is that the selectively excited water molecules act as propellant to ablate whole biological complexes into the plume, faster than any thermal deleterious effect or fragmentation that would mask molecular identities.The PIRL ablation under DIVE condition is applied for the first time to six types of ocular tissues, rendering precise and minimally invasive incisions in a well-controlled and reproducible way. An eminent demonstration is the contact-free and applanation-free corneal trephination with the PIRL. Mass spectrometry and other analytical techniques show that great abundance of proteins with various molecular weights are extracted from the tissue by the PIRL ablation, and that fragmentation or other chemical alternation does not occur to the proteins in the ablation plume. With various microscope imaging and biochemical analysis methods, nano-scale single protein molecules, viruses and cells in the ablation plume are found to be morphologically and functionally identical to their corresponding controls. The PIRL ablation provides a new means to push the frontiers of laser surgery in ophthalmology and can be applied to resolve chemical activities in situ and in vivo. The most important finding is the conserved nature of the extracted biological entities

  19. Comparison of two methods for extraction of volatiles from marine PL emulsions

    DEFF Research Database (Denmark)

    Lu, Henna Fung Sieng; Nielsen, Nina Skall; Jacobsen, Charlotte

    2013-01-01

    analysis. However, the CAR/PDMS‐SPME technique was efficient for lipid oxidation analysis in emulsions of less complex headspace. The SPME method extracted volatiles of lower molecular weights more efficient than the DHS method. On the other hand, DHS Tenax GR appeared to be more efficient in extracting......The dynamic headspace (DHS) thermal desorption principle using Tenax GR tube, as well as the solid phase micro‐extraction (SPME) tool with carboxen/polydimethylsiloxane 50/30 µm CAR/PDMS SPME fiber, both coupled to GC/MS were implemented for the isolation and identification of both lipid...... and Strecker derived volatiles in marine phospholipids (PL) emulsions. Comparison of volatile extraction efficiency was made between the methods. For marine PL emulsions with a highly complex composition of volatiles headspace, a fiber saturation problem was encountered when using CAR/PDMS‐SPME for volatiles...

  20. A novel dispersive micro solid phase extraction using zein nanoparticles as the sorbent combined with headspace solid phase micro-extraction to determine chlorophenols in water and honey samples by GC-ECD.

    Science.gov (United States)

    Farhadi, Khalil; Matin, Amir Abbas; Amanzadeh, Hatam; Biparva, Pourya; Tajik, Hossein; Farshid, Amir Abbas; Pirkharrati, Hossein

    2014-10-01

    This study presents a new technique, dispersive micro solid phase extraction (DMSPE) combined with headspace solid phase micro-extraction (HS-SPME) for extraction and determination of chlorophenols (CPs) in water and honey samples using a Gas Chromatography-Electron Capture Detector (GC-ECD). Zein nanoparticles were made by liquid-liquid dispersion and applied for the first time as the sorbent phase in DMSPE. In the proposed DMSPE-HS-SPME method, 1% w/v of ethanolic zein solution was added to an aqueous sample and then a dose of the in-situ generated zein nanoparticles was applied to a pre-concentration of target analytes. Thermal desorption of analytes was performed after the isolating sorbent phase, and then HS-SPME was applied for enrichment prior to introducing to gas chromatography. All the important parameters influencing efficiency of the extraction process such effects of salt, pH, sorbent concentration, temperature, sorbent solution volume in DMSPE procedure, extraction temperature, extraction time, desorption temperature and time in the HS-SPME procedure were investigated and optimized. Results showed that under optimum extraction conditions, detection limits (signal to noise ratio=3) were in the range of 0.08-0.6 ng mL(-1) and evaluations for relative standard deviations (RSDs %) were between 6.62% and 8.36%.

  1. Sample extraction and injection with a microscale preconcentrator.

    Energy Technology Data Exchange (ETDEWEB)

    Robinson, Alex Lockwood (Advanced Sensor Technologies, Albuquerque, NM); Chan, Helena Kai Lun

    2007-09-01

    This report details the development of a microfabricated preconcentrator that functions as a fully integrated chemical extractor-injector for a microscale gas chromatograph (GC). The device enables parts-per-billion detection and quantitative analysis of volatile organic compounds (VOCs) in indoor air with size and power advantages over macro-scale systems. The 44 mm{sup 3} preconcentrator extracts VOCs using highly adsorptive, granular forms of graphitized carbon black and carbon molecular sieves. The micron-sized silicon cavities have integrated heating and temperature sensing allowing low power, yet rapid heating to thermally desorb the collected VOCs (GC injection). The keys to device construction are a new adsorbent-solvent filling technique and solvent-tolerant wafer-level silicon-gold eutectic bonding technology. The product is the first granular adsorbent preconcentrator integrated at the wafer level. Other advantages include exhaustive VOC extraction and injection peak widths an order of magnitude narrower than predecessor prototypes. A mass transfer model, the first for any microscale preconcentrator, is developed to describe both adsorption and desorption behaviors. The physically intuitive model uses implicit and explicit finite differences to numerically solve the required partial differential equations. The model is applied to the adsorption and desorption of decane at various concentrations to extract Langmuir adsorption isotherm parameters from effluent curve measurements where properties are unknown a priori.

  2. Quantitative Detection of Trace Explosive Vapors by Programmed Temperature Desorption Gas Chromatography-Electron Capture Detector

    OpenAIRE

    2014-01-01

    The direct liquid deposition of solution standards onto sorbent-filled thermal desorption tubes is used for the quantitative analysis of trace explosive vapor samples. The direct liquid deposition method yields a higher fidelity between the analysis of vapor samples and the analysis of solution standards than using separate injection methods for vapors and solutions, i.e., samples collected on vapor collection tubes and standards prepared in solution vials. Additionally, the method can accoun...

  3. Residence time dependent desorption of Staphylococcus epidermidis from hydrophobic and hydrophilic substrata

    NARCIS (Netherlands)

    Boks, Niels P.; Kaper, Hans J.; Norde, Willem; Busscher, Henk J.; van der Mei, Henny C.

    2008-01-01

    Adhesion and desorption are simultaneous events during bacterial adhesion to surfaces. although desorption is far less studied than adhesion. Here, desorption of Staphylococcus epidermidis from substratum surfaces is demonstrated to be residence time dependent. Initial desorption rate coefficients

  4. Residence time dependent desorption of Staphylococcus epidermidis from hydrophobic and hydrophilic substrata

    NARCIS (Netherlands)

    Boks, Niels P.; Kaper, Hans J.; Norde, Willem; Busscher, Henk J.; van der Mei, Henny C.

    2008-01-01

    Adhesion and desorption are simultaneous events during bacterial adhesion to surfaces. although desorption is far less studied than adhesion. Here, desorption of Staphylococcus epidermidis from substratum surfaces is demonstrated to be residence time dependent. Initial desorption rate coefficients w

  5. Characterization of residues from thermal treatment of treated wood and extraction of Cu, Cr, As and Zn

    DEFF Research Database (Denmark)

    Ottosen, Lisbeth M.; Pedersen, Anne Juul; Christensen, Iben Vernegren

    2005-01-01

    , that the charcoal contained a high concentration of Zn, probably from paint. Chemical extraction experiments in HNO were conducted with the charcoal and it was found that the order of extraction (in percentage) was Zn > Cu > As > Cr. A SEM/EDX investigation of the mixed ash from combustion showed the presence...... of small particles with wood structure with elevated Cu and Cr concentrations, but most particles were irregular shaped matrix particles rich in Si, Al and K. Cr was abundant in many different particles including the lignin skeleton of the small, unburned wood pieces, but also inside silica-based matrix...... form in a small layer on the surface of some matrix particles indicating condensation of volatile Cu species. Chemical extraction with inorganic acids showed the order of percentages mobilized as: As > Cu > Cr....

  6. The Effects of Different Extraction Methods on Antioxidant Properties, Chemical Composition, and Thermal Behavior of Black Seed (Nigella sativa L.) Oil

    Science.gov (United States)

    Mohammed, Nameer Khairullah; Abd Manap, Mohd Yazid; Muhialdin, Belal J.; Alhelli, Amaal M.

    2016-01-01

    The Nigella sativa L. popularly referred to as black seeds are widely used as a form of traditional nutrition and medicine. N. sativa seeds were used for the extraction of their oil by way of supercritical fluid extraction (SFE) and cold press (CP) to determine the physicochemical properties, antioxidant activity, and thermal behavior. The GC-MS results showed the primary constituents in the Nigella sativa oil (NSO) were Caryophyllene (17.47%) followed by thymoquinone (TQ) (11.80%), 1,4-Cyclohexadiene (7.17%), longifolene (3.5%), and carvacrol (1.82%). The concentration of TQ was found to be 6.63 mg/mL for oil extracted using SFE and 1.56 mg/mL for oil extracted by CP method. The antioxidant activity measured by DPPH and the IC50 was 1.58 mg/mL and 2.30 mg/mL for SFE oil and cold pressed oil, respectively. The ferric reducing/antioxidant power (FRAP) activity for SFE oil and CP oil was 538.67 mmol/100 mL and 329.00 mmol/100 mL, respectively. The total phenolic content (TPC) of SFE oil was 160.51 mg/100 mL and 94.40 mg/100 mL for CP oil presented as gallic acid equivalents (GAE). This research showed that a high level of natural antioxidants could be derived from NSO extracted by SFE. PMID:27642353

  7. The Effects of Different Extraction Methods on Antioxidant Properties, Chemical Composition, and Thermal Behavior of Black Seed (Nigella sativa L. Oil

    Directory of Open Access Journals (Sweden)

    Nameer Khairullah Mohammed

    2016-01-01

    Full Text Available The Nigella sativa L. popularly referred to as black seeds are widely used as a form of traditional nutrition and medicine. N. sativa seeds were used for the extraction of their oil by way of supercritical fluid extraction (SFE and cold press (CP to determine the physicochemical properties, antioxidant activity, and thermal behavior. The GC-MS results showed the primary constituents in the Nigella sativa oil (NSO were Caryophyllene (17.47% followed by thymoquinone (TQ (11.80%, 1,4-Cyclohexadiene (7.17%, longifolene (3.5%, and carvacrol (1.82%. The concentration of TQ was found to be 6.63 mg/mL for oil extracted using SFE and 1.56 mg/mL for oil extracted by CP method. The antioxidant activity measured by DPPH and the IC50 was 1.58 mg/mL and 2.30 mg/mL for SFE oil and cold pressed oil, respectively. The ferric reducing/antioxidant power (FRAP activity for SFE oil and CP oil was 538.67 mmol/100 mL and 329.00 mmol/100 mL, respectively. The total phenolic content (TPC of SFE oil was 160.51 mg/100 mL and 94.40 mg/100 mL for CP oil presented as gallic acid equivalents (GAE. This research showed that a high level of natural antioxidants could be derived from NSO extracted by SFE.

  8. Investigation of ethyl lactate as a green solvent for desorption of total petroleum hydrocarbons (TPH) from contaminated soil.

    Science.gov (United States)

    Jalilian Ahmadkalaei, Seyedeh Pegah; Gan, Suyin; Ng, Hoon Kiat; Abdul Talib, Suhaimi

    2016-11-01

    Treatment of oil-contaminated soil is a major environmental concern worldwide. The aim of this study is to examine the applicability of a green solvent, ethyl lactate (EL), in desorption of diesel aliphatic fraction within total petroleum hydrocarbons (TPH) in contaminated soil and to determine the associated desorption kinetics. Batch desorption experiments were carried out on artificially contaminated soil at different EL solvent percentages (%). In analysing the diesel range of TPH, TPH was divided into three fractions and the effect of solvent extraction on each fraction was examined. The experimental results demonstrated that EL has a high and fast desorbing power. Pseudo-second order rate equation described the experimental desorption kinetics data well with correlation coefficient values, R (2), between 0.9219 and 0.9999. The effects of EL percentage, initial contamination level of soil and liquid to solid ratio (L/S (v/w)) on initial desorption rate have also been evaluated. The effective desorption performance of ethyl lactate shows its potential as a removal agent for remediation of TPH-contaminated soil worldwide.

  9. Helium Retention and Desorption Behaviour of Reduced Activation Ferritic/Martenstic Steel

    Science.gov (United States)

    Wang, Pinghuai; Nobuta, Yuji; Hino, Tomoaki; Yamauchi, Yuji; Chen, Jiming; Xu, Zengyu; Li, Xiongwei; Liu, Shi

    2009-04-01

    The reduced activation ferritic/martenstic steel CLF-1 prepared by the Southwestern Institute of Physics in China was irradiated by helium ions with an energy of 5 keV at room temperature using an electron cyclotron resonance (ECR) ion irradiation apparatus. After the irradiation, the helium retention and desorption were investigated using a technique of thermal desorption spectroscopy (TDS). The experiment was conducted with both the normal and welded samples. Blisters were observed after the helium ion irradiation, and the surface density of blisters in the welded samples was lower than that in the non-welded samples. Three desorption peaks were observed in both the non-welded and welded samples. These desorption peaks corresponded to those of blister ruptures and the helium release from the inner bubbles and the defects. The amount of helium retained in the welded samples was approximately the same as that in the non-welded samples, which was much less than other reduced activation materials, such as vanadium alloy and SiC/SiC composites.

  10. Direct measurement of desorption and diffusion energies of O and N atoms physisorbed on amorphous surfaces

    CERN Document Server

    Minissale, Marco; Dulieu, François

    2016-01-01

    Physisorbed atoms on the surface of interstellar dust grains play a central role in solid state astrochemistry. Their surface reactivity is one source of the observed molecular complexity in space. In experimental astrophysics, the high reactivity of atoms also constitutes an obstacle to measuring two of the fundamental properties in surface physics, namely desorption and diffusion energies, and so far direct measurements are non-existent for O and N atoms. We investigated the diffusion and desorption processes of O and N atoms on cold surfaces in order to give boundary conditions to astrochemical models. Here we propose a new technique for directly measuring the N- and O-atom mass signals. Including the experimental results in a simple model allows us to almost directly derive the desorption and diffusion barriers of N atoms on amorphous solid water ice (ASW) and O atoms on ASW and oxidized graphite. We find a strong constraint on the values of desorption and thermal diffusion energy barriers. The measured b...

  11. Helium Retention and Desorption Behaviour of Reduced Activation Ferritic/Martenstic Steel

    Institute of Scientific and Technical Information of China (English)

    WANG Pinghuai; NOBUTA Yuji; HINO Tomoaki; YAMAUCHI Yuji; CHEN Zilning; XU Zengyu; LI Xiongwei; LIU Shi

    2009-01-01

    The reduced activation ferritic/martenstic steel CLF-1 prepared by the Southwest-ern Institute of Physics in China was irradiated by helium ions with an energy of 5 keV at room temperature using an electron cyclotron resonance (ECR) ion irradiation apparatus. After the irradiation, the helium retention and desorption were investigated using a technique of thermal desorption spectroscopy (TDS). The experiment was conducted with both the normal and welded samples. Blisters were observed after the helium ion irradiation, and the surface density of blisters in the welded samples was lower than that in the non-welded samples. Three desorption peaks were observed in both the non-welded and welded samples. These desorption peaks corresponded to those of blister ruptures and the helium release from the inner bubbles and the defects. The amount of helium retained in the welded samples was approximately the same as that in the non-welded samples, which was much less than other reduced activation materials, such as vanadium alloy and SiC/SiC composites.

  12. Desorption of Water from Distinct Step Types on a Curved Silver Crystal

    Directory of Open Access Journals (Sweden)

    Jakrapan Janlamool

    2014-07-01

    Full Text Available We have investigated the adsorption of H2O onto the A and B type steps on an Ag single crystal by temperature programmed desorption. For this study, we have used a curved crystal exposing a continuous range of surface structures ranging from [5(111 × (100] via (111 to [5(111 × (110]. LEED and STM studies verify that the curvature of our sample results predominantly from monoatomic steps. The sample thus provides a continuous array of step densities for both step types. Desorption probed by spatially-resolved TPD of multilayers of H2O shows no dependence on the exact substrate structure and thus confirms the absence of thermal gradients during temperature ramps. In the submonolayer regime, we observe a small and linear dependence of the desorption temperature on the A and B step density. We argue that such small differences are only observable by means of a single curved crystal, which thus establishes new experimental benchmarks for theoretical calculation of chemically accurate binding energies. We propose an origin of the observed behavior based on a “two state” desorption model.

  13. Plutonium sorption and desorption behavior on bentonite.

    Science.gov (United States)

    Begg, James D; Zavarin, Mavrik; Tumey, Scott J; Kersting, Annie B

    2015-03-01

    Understanding plutonium (Pu) sorption to, and desorption from, mineral phases is key to understanding its subsurface transport. In this work we study Pu(IV) sorption to industrial grade FEBEX bentonite over the concentration range 10(-7)-10(-16) M to determine if sorption at typical environmental concentrations (≤10(-12) M) is the same as sorption at Pu concentrations used in most laboratory experiments (10(-7)-10(-11) M). Pu(IV) sorption was broadly linear over the 10(-7)-10(-16) M concentration range during the 120 d experimental period; however, it took up to 100 d to reach sorption equilibrium. At concentrations ≥10(-8) M, sorption was likely affected by additional Pu(IV) precipitation/polymerization reactions. The extent of sorption was similar to that previously reported for Pu(IV) sorption to SWy-1 Na-montmorillonite over a narrower range of Pu concentrations (10(-11)-10(-7) M). Sorption experiments with FEBEX bentonite and Pu(V) were also performed across a concentration range of 10(-11)-10(-7) M and over a 10 month period which allowed us to estimate the slow apparent rates of Pu(V) reduction on a smectite-rich clay. Finally, a flow cell experiment with Pu(IV) loaded on FEBEX bentonite demonstrated continued desorption of Pu over a 12 day flow period. Comparison with a desorption experiment performed with SWy-1 montmorillonite showed a strong similarity and suggested the importance of montorillonite phases in controlling Pu sorption/desorption reactions on FEBEX bentonite.

  14. Supercritical Fluid Extraction of a Novel Template from Mesoporous Zirconia and the Effect on Porous Structure

    Institute of Scientific and Technical Information of China (English)

    MA Fu; ZHAO Hongjian

    2013-01-01

    Mesoporous zirconia was synthesized by a new and simple method.Zirconium n-propoxide was used as the zirconium source.A small,inexpensive nonsurfactant,triethanolamine,was used as the template.The template was removed by thermal treatment in air and supercritical fluid extraction using CO2.The structure of the resulting materials was characterized by X-ray diffraction,transmission electron microscopy,and N2 adsorption-desorption analyses.The materials are found to have narrowly distributed average pore diameters and wormhole-like pore channels.However,higher surface area and larger pore volume are exhibited after supercdtical fluid extraction with CO2.The removal of the template by thermal treatment also leads to condensation and mild shrinkage of the zirconia framework.

  15. Preparation of PDMS-coated microspheres by sol-gel method for sorptive extraction of PAHs

    Institute of Scientific and Technical Information of China (English)

    Chang Guang Yang; Xiang Juan Ji; Xiao Zheng Lan

    2008-01-01

    In this paper, a novel SPME mode, PDMS-coated solid glass microspheres (SGMs), were prepared by sol-gel method. Using homemade thermal desorption unit coupled with CGC-FID, six PAHs as model analytes, the performance of the new mode was characterized. The new extractive phase exhibited high thermal stability and satisfactory extraction capability. The detection limits were 0.01-0.045 ng/mL, and the linearity was from 0.5 ng/mL to 96 ng/mL. The R.S.D.s of repeatability for retention time and peak area were all within 0.074% and 6.7%, respectively. The recoveries of the PAHs were 78-127% from the sarnples taken from river water.

  16. Manual for the thermal and hdyraulic design of direct contract spray columns for use in extracting heat from geothermal brines

    Science.gov (United States)

    Jacobs, H. R.

    1985-06-01

    This report outlines the current methods being used in the thermal and hydraulic design of spray column type, direct contact heat exchangers. It provides appropriate referenced equations for both preliminary design and detailed performance. The design methods are primarily empirical and are applicable for use in the design of such units for geothermal application and for application with solar ponds. Methods for design, for both preheater and boiler sections of the primary heat exchangers, for direct contact binary powers plants are included.

  17. Lead sorption-desorption from organic residues.

    Science.gov (United States)

    Duarte Zaragoza, Victor M; Carrillo, Rogelio; Gutierrez Castorena, Carmen M

    2011-01-01

    Sorption and desorption are mechanisms involved in the reduction of metal mobility and bioavailability in organic materials. Metal release from substrates is controlled by desorption. The capacity of coffee husk and pulp residues, vermicompost and cow manure to adsorb Pb2+ was evaluated. The mechanisms involved in the sorption process were also studied. Organic materials retained high concentrations of lead (up to 36,000 mg L(-1)); however, the mechanisms of sorption varied according to the characteristics of each material: degree of decomposition, pH, cation exchange capacity and percentage of organic matter. Vermicompost and manure removed 98% of the Pb from solution. Lead precipitated in manure and vermicompost, forming lead oxide (PbO) and lead ferrite (PbFe4O7). Adsorption isotherms did not fit to the typical Freundlich and Langmuir equations. Not only specific and non-specific adsorption was observed, but also precipitation and coprecipitation. Lead desorption from vermicompost and cow manure was less than 2%. For remediation of Pb-polluted sites, the application of vermicompost and manure is recommended in places with alkaline soils because Pb precipitation can be induced, whereas coffee pulp residue is recommended for acidic soils where Pb is adsorbed.

  18. Experimental characterization of a plume of passive contaminant above a thermal source: capture efficiency of a fume extraction hood.

    Science.gov (United States)

    Devienne, René; Fontaine, Jean Raymond; Kicka, Jérémie; Bonthoux, Francis

    2009-10-01

    Industrial ventilation problems can be linked to the formation of thermal plumes that develop due to natural convection above various heat sources. These plumes, independent of the energy losses and thermal constraints caused, can also be the carrier of polluting products. This article describes an experimental study of the dynamic, thermal, and mass fields that develop from a hot rectangular (0.5 x 1.25 m) horizontal source. The metrology available allows the measurement of not only the local temperatures and velocities but also the concentration of a tracer gas (helium). Mathematical models have been developed enabling representation of the fields concerned; their characterization by isothermal, iso-velocity, or iso-concentration curves; calculation of the flow rate carried by the plume at a given height; calculation of the enthalpy transport; and so on. Moreover, a pollutant capture device has been introduced, and the measurement technique used allows the determination of various efficiencies of practical interest. The ratio of capture flow to free plume flow at a particular height appears to correlate well with the mean efficiencies obtained for distinct source temperatures.

  19. Characterization of Key Aroma Compounds in Raw and Thermally Processed Prawns and Thermally Processed Lobsters by Application of Aroma Extract Dilution Analysis.

    Science.gov (United States)

    Mall, Veronika; Schieberle, Peter

    2016-08-24

    Application of aroma extract dilution analysis (AEDA) to an aroma distillate of blanched prawn meat (Litopenaeus vannamei) (BPM) revealed 40 odorants in the flavor dilution (FD) factor range from 4 to 1024. The highest FD factors were assigned to 2-acetyl-1-pyrroline, 3-(methylthio)propanal, (Z)-1,5-octadien-3-one, trans-4,5-epoxy-(E)-2-decenal, (E)-3-heptenoic acid, and 2-aminoacetophenone. To understand the influence of different processing conditions on odorant formation, fried prawn meat was investigated by means of AEDA in the same way, revealing 31 odorants with FD factors between 4 and 2048. Also, the highest FD factors were determined for 2-acetyl-1-pyrroline, 3-(methylthio)propanal, and (Z)-1,5-octadien-3-one, followed by 4-hydroxy-2,5-dimethyl-3(2H)-furanone, (E)-3-heptenoic acid, and 2-aminoacetophenone. As a source of the typical marine, sea breeze-like odor attribute of the seafood, 2,4,6-tribromoanisole was identified in raw prawn meat as one of the contributors. Additionally, the aroma of blanched prawn meat was compared to that of blanched Norway and American lobster meat, respectively (Nephrops norvegicus and Homarus americanus). Identification experiments revealed the same set of odorants, however, with differing FD factors. In particular, 3-hydroxy-4,5-dimethyl-2(5H)-furanone was found as the key aroma compound in blanched Norway lobster, whereas American lobster contained 3-methylindole with a high FD factor.

  20. Desorption of hydrocarbon chains by association with ionic and nonionic surfactants under flow as a mechanism for enhanced oil recovery.

    Science.gov (United States)

    Terrón-Mejía, Ketzasmin A; López-Rendón, Roberto; Goicochea, Armando Gama

    2017-08-29

    The need to extract oil from wells where it is embedded on the surfaces of rocks has led to the development of new and improved enhanced oil recovery techniques. One of those is the injection of surfactants with water vapor, which promotes desorption of oil that can then be extracted using pumps, as the surfactants encapsulate the oil in foams. However, the mechanisms that lead to the optimal desorption of oil and the best type of surfactants to carry out desorption are not well known yet, which warrants the need to carry out basic research on this topic. In this work, we report non equilibrium dissipative particle dynamics simulations of model surfactants and oil molecules adsorbed on surfaces, with the purpose of studying the efficiency of the surfactants to desorb hydrocarbon chains, that are found adsorbed over flat surfaces. The model surfactants studied correspond to nonionic and cationic surfactants, and the hydrocarbon desorption is studied as a function of surfactant concentration under increasing Poiseuille flow. We obtain various hydrocarbon desorption isotherms for every model of surfactant proposed, under flow. Nonionic surfactants are found to be the most effective to desorb oil and the mechanisms that lead to this phenomenon are presented and discussed.

  1. Plasma Desorption Mass Spectrometry analysis of HCOOH ice

    Energy Technology Data Exchange (ETDEWEB)

    Andrade, D.P.P.; Rocco, M.L.M. [Departamento de Fisico-Quimica, Instituto de Quimica, Universidade Federal do Rio de Janeiro, Cidade Universitaria, Ilha do Fundao, 21949-900 Rio de Janeiro, RJ (Brazil); Boechat-Roberty, H.M. [Observatorio do Valongo, Universidade Federal do Rio de Janeiro, Ladeira Pedro Antonio, 43, Centro, Rio de Janeiro, RJ (Brazil); Iza, P.; Martinez, R. [Departamento de Fisica, Pontificia Universidade Catolica do Rio de Janeiro, 22543-900 Rio de Janeiro (Brazil); Homem, M.G.P. [Laboratorio Nacional de Luz Sincrotron (LNLS), Box 6192, 13084-971 Campinas, SP (Brazil); Silveira, E.F. da [Departamento de Fisica, Pontificia Universidade Catolica do Rio de Janeiro, 22543-900 Rio de Janeiro (Brazil)], E-mail: enio@vdg.fis.puc-rio.br

    2007-03-15

    Planetary magnetospheres, in which outer planet satellites orbit, are bombarded by energetic particles inducing chemical and physical changes in their icy surfaces. The existing condensed gases react to form new products, which then undergo thermal evolution from the natural day/night cycles of these satellites. Plasma irradiation of ice causes phase changes, e.g., water ice from crystalline to amorphous over short timescales. When ice is recrystallized by heating, the surface layers retain some disorder, which promote reactions among adsorbed molecules such as H{sub 2}O, CO{sub 2}, CH{sub 2}CO, HCOOH and theirs radiolysis products. In this work, chemical reactions involving formic acid condensed at 56 K are analyzed by using Plasma Desorption Mass Spectrometry-time-of-flight ({sup 252}Cf-PDMS-TOF). Mass spectra of positive and negative desorbed ions were obtained, giving information on the structure and abundance of the molecules on the ice; the expected cations and anions generated by the HCOOH dissociation have been observed. Furthermore, several series of cluster ions were also detected, all exhibiting the structure X{sub n}Y{sub m}R{sup {+-}}, where X and Y are the neutral ice molecules, such as HCOOH or H{sub 2}O, and R{sup {+-}} is either an atomic or a molecular ion, such as H{sup +}, H{sub 3}O{sup +} or COOH{sup -}. In general, the desorption yields of the observed positive and negative ions are characterized by a decreasing exponential function as the emitted ion mass increases; however, the (HCOOH){sub n}OH{sup -} series presents its maximum at n = 8.

  2. Role of desorption kinetics in the rhamnolipid-enhanced biodegradation of polycyclic aromatic hydrocarbons.

    Science.gov (United States)

    Congiu, Eleonora; Ortega-Calvo, José-Julio

    2014-09-16

    The main aim of this study was to investigate the effect of a rhamnolipid biosurfactant on biodegradation of (14)C-labeled phenanthrene and pyrene under desorption-limiting conditions. The rhamnolipid caused a significant solubilization and enhanced biodegradation of PAHs sorbed to soils. The enhancement was, however, negatively influenced by experimental conditions that caused an enrichment of slow desorption fractions. These conditions included aging, a higher organic matter content in soil, and previous extraction with Tenax to remove the labile-desorbing chemical. The decline in bioavailability caused by aging on sorbed (14)C-pyrene was partially reversed by rhamnolipids, which enhanced mineralization of the aged compound, although not so efficiently like with the unaged chemical. This loss in biosurfactant efficiency in promoting biodegradation can be explained by intra-aggregate diffusion of the pollutant during aging. We suggest that rhamnolipid can enhance biodegradation of soil-sorbed PAHs by micellar solubilization, which increase the cell exposure to the chemicals in the aqueous phase, and partitioning into soil organic matter, thus enhancing the kinetics of slow desorption. Our study show that rhamnolipid can constitute a valid alternative to chemical surfactants in promoting the biodegradation of slow desorption PAHs, which constitutes a major bottleneck in bioremediation.

  3. Interactions on external MOF surfaces: desorption of water and ethanol from CuBDC nanosheets.

    Science.gov (United States)

    Elder, Alexander C; Aleksandrov, Alexandr B; Nair, Sankar; Orlando, Thomas M

    2017-09-06

    The external surfaces of metal-organic framework (MOF) materials are difficult to experimentally isolate due to the high porosities of these materials. MOF surface surrogates in the form of copper benzenedicarboxylate (CuBDC) nanosheets were synthesized using a bottom-up approach and the surface interactions of water and ethanol were investigated by temperature programmed desorption (TPD). A method of analysis of diffusion-influenced TPD was developed to measure the kinetic desorption properties of these porous materials. This approach also allows the extraction of diffusion coefficients from TPD data. Water desorbs from CuBDC nanosheets with activation energies of 44±2 kJ/mol at edge sites and 58 ± 1 kJ/mol at internal and surface sites. Ethanol desorbs with activation energies of 58 ± 1 kJ/mol at internal sites and 66 ± 0.4 kJ/mol at external surface sites. Co-adsorption of water and ethanol was also investigated. The presence of ethanol was found to inhibit the desorption of water that results in a water desorption process with an activation energy of 68 ± 0.7.

  4. Manual for the thermal and hydraulic design of direct contact spray columns for use in extracting heat from geothermal brines

    Energy Technology Data Exchange (ETDEWEB)

    Jacobs, H.R.

    1985-06-01

    This report outlines the current methods being used in the thermal and hydraulic design of spray column type, direct contact heat exchangers. It provides appropriate referenced equations for both preliminary design and detailed performance. The design methods are primarily empirical and are applicable for us in the design of such units for geothermal application and for application with solar ponds. Methods for design, for both preheater and boiler sections of the primary heat exchangers, for direct contact binary powers plants are included. 23 refs., 8 figs.

  5. New Activated Carbon with High Thermal Conductivity and Its Microwave Regeneration Performance

    Institute of Scientific and Technical Information of China (English)

    GU Xuexian; SU Zhanjun; XI Hongxia

    2016-01-01

    Using a walnut shell as a carbon source and ZnCl2 as an activating agent, we resolved the temperature gradient problems of activated carbon in the microwave desorption process. An appropriate amount of silicon carbide was added to prepare the composite activated carbon with high thermal conductivity while developing VOC adsorption-microwave regeneration technology. The experimental results show that the coefficient of thermal conductivity of SiC-AC is three times as much as those of AC and SY-6. When microwave power was 480 W in its microwave desorption , the temperature of the bed thermal desorption was 10℃ to 30℃below that of normal activated carbon prepared in our laboratory. The toluene desorption activation energy was 16.05 kJ∙mol-1, which was 15% less than the desorption activation energy of commercial activated carbon. This study testified that the process could maintain its high adsorption and regeneration desorption performances.

  6. STUDIES ON INOSINE EXTRACTION BY ION EXCHANGE METHOD

    Institute of Scientific and Technical Information of China (English)

    HuangXiwen; ShiFang; 等

    1998-01-01

    The adsorption characteristics of inosine from fermentation solution on anion exchange resin under the condition of different pH,resin type are investigated.Besides,the desorption conditions are studied under different temperature.The adsorption and desorption mechanism are described to obtain the optimum technological condition of inosine extraction.

  7. Evidence for a CO Desorption Front in the Outer AS 209 Disk

    Science.gov (United States)

    Huang, Jane; Öberg, Karin I.; Andrews, Sean M.

    2016-05-01

    Millimeter observations of CO isotopologues are often used to make inferences about protoplanetary disk gas density and temperature structures. The accuracy of these estimates depends on our understanding of CO freezeout and desorption from dust grains. Most models of these processes indicate that CO column density decreases monotonically with distance from the central star due to a decrease in gas density and freezeout beyond the CO snowline. We present ALMA Cycle 2 observations of 12CO, 13CO, and C18O J=2-1 emission that instead suggest CO enhancement in the outer disk of T Tauri star AS 209. Most notably, the C18O emission consists of a central peak and a ring at a radius of ˜ 1\\prime \\prime (120 au), well outside the expected CO snowline. We propose that the ring arises from the onset of CO desorption near the edge of the millimeter dust disk. CO desorption exterior to a CO snowline may occur via non-thermal processes involving cosmic rays or high-energy photons, or via a radial thermal inversion arising from dust migration.

  8. Evidence for a CO desorption front in the outer AS 209 disk

    CERN Document Server

    Huang, Jane; Andrews, Sean M

    2016-01-01

    Millimeter observations of CO isotopologues are often used to make inferences about protoplanetary disk gas density and temperature structures. The accuracy of these estimates depends on our understanding of CO freezeout and desorption from dust grains. Most models of these processes indicate that CO column density decreases monotonically with distance from the central star due to a decrease in gas density and freezeout beyond the CO snowline. We present ALMA Cycle 2 observations of $^{12}$CO, $^{13}$CO, and C$^{18}$O $J=2-1$ emission that instead suggest CO enhancement in the outer disk of T Tauri star AS 209. Most notably, the C$^{18}$O emission consists of a central peak and a ring at a radius of $\\sim1''$ (120 AU), well outside the expected CO snowline. We propose that the ring arises from the onset of CO desorption near the edge of the millimeter dust disk. CO desorption exterior to a CO snowline may occur via non-thermal processes involving cosmic rays or high-energy photons, or via a radial thermal inv...

  9. Optical breathing of nano-porous antireflective coatings through adsorption and desorption of water.

    Science.gov (United States)

    Nielsen, Karsten H; Kittel, Thomas; Wondraczek, Katrin; Wondraczek, Lothar

    2014-10-13

    We report on the direct consequences of reversible water adsorption on the optical performance of silica-based nanoporous antireflective (AR) coatings as they are applied on glass in photovoltaic and solar thermal energy conversion systems. In situ UV-VIS transmission spectroscopy and path length measurements through high-resolution interferometric microscopy were conducted on model films during exposure to different levels of humidity and temperature. We show that water adsorption in the pores of the film results in a notable increase of the effective refractive index of the coating. As a consequence, the AR effect is strongly reduced. The temperature regime in which the major part of the water can be driven-out rapidly lies in the range of 55°C and 135°C. Such thermal desorption was found to increase the overall transmission of a coated glass by ~ 1%-point. As the activation energy of isothermal desorption, we find a value of about 18 kJ/mol. Within the experimental range of our data, the sorption and desorption process is fully reversible, resulting in optical breathing of the film. Nanoporous AR films with closed pore structure or high hydrophobicity may be of advantage for maintaining AR performance under air exposure.

  10. Optical breathing of nano-porous antireflective coatings through adsorption and desorption of water

    Science.gov (United States)

    Nielsen, Karsten H.; Kittel, Thomas; Wondraczek, Katrin; Wondraczek, Lothar

    2014-10-01

    We report on the direct consequences of reversible water adsorption on the optical performance of silica-based nanoporous antireflective (AR) coatings as they are applied on glass in photovoltaic and solar thermal energy conversion systems. In situ UV-VIS transmission spectroscopy and path length measurements through high-resolution interferometric microscopy were conducted on model films during exposure to different levels of humidity and temperature. We show that water adsorption in the pores of the film results in a notable increase of the effective refractive index of the coating. As a consequence, the AR effect is strongly reduced. The temperature regime in which the major part of the water can be driven-out rapidly lies in the range of 55°C and 135°C. Such thermal desorption was found to increase the overall transmission of a coated glass by ~ 1%-point. As the activation energy of isothermal desorption, we find a value of about 18 kJ/mol. Within the experimental range of our data, the sorption and desorption process is fully reversible, resulting in optical breathing of the film. Nanoporous AR films with closed pore structure or high hydrophobicity may be of advantage for maintaining AR performance under air exposure.

  11. Polypyrrole-magnetite dispersive micro-solid-phase extraction combined with ultraviolet-visible spectrophotometry for the determination of rhodamine 6G and crystal violet in textile wastewater.

    Science.gov (United States)

    Kamaruddin, Amirah Farhan; Sanagi, Mohd Marsin; Wan Ibrahim, Wan Aini; Md Shukri, Dyia S; Abdul Keyon, Aemi S

    2017-08-29

    Polypyrrole-magnetite dispersive micro-solid-phase extraction method combined with ultraviolet-visible spectrophotometry was developed for the determination of selected cationic dyes in textile wastewater. Polypyrrole-magnetite was used as adsorbent due to its thermal stability, magnetic properties, and ability to adsorb Rhodamine 6G and crystal violet. Dispersive micro-solid-phase extraction parameters were optimized, including sample pH, adsorbent amount, extraction time, and desorption solvent. The optimum polypyrrole-magnetite dispersive micro-solid phase-extraction conditions were sample pH 8, 60 mg polypyrrole-magnetite adsorbent, 5 min of extraction time, and acetonitrile as the desorption solvent. Under the optimized conditions, the polypyrrole-magnetite dispersive micro-solid-phase extraction with ultraviolet-visible method showed good linearity in the range of 0.05-7 mg/L (R(2)  > 0.9980). The method also showed a good limit of detection for the dyes (0.05 mg/L) and good analyte recoveries (97.4-111.3%) with relative standard deviations extraction and determination of dyes at trace concentration levels. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Kinetic Monte Carlo simulations of temperature programed desorption of O/Rh(111).

    Science.gov (United States)

    Franz, T; Mittendorfer, F

    2010-05-21

    We present a kinetic Monte Carlo simulation based on ab initio calculations for the thermal desorption of oxygen from a Rh(111) surface. Several models have been used for the parametrization of the interaction between the adsorbed atoms. We find that models based on a parametrization with only pairwise interactions have a relatively large error in the predicted adsorption energies. This error can be significantly reduced by including three- and four-body interactions. In addition, we find that a significant amount of atoms adsorb in a second adsorption site - the hcp-hollow site - at an elevated temperature. Consequently, only a many-body multisite model of the oxygen interactions yields appropriate desorption spectra for the full coverage range, while more simple models only capture the correct shape in the low-coverage case. Our parametrization allows us to predict the adsorption energies of an arbitrary configuration of adsorbates with a mean average error of less than 6 meV/atom.

  13. Large Scale Nanoparticle Screening for Small Molecule Analysis in Laser Desorption Ionization Mass Spectrometry.

    Science.gov (United States)

    Yagnik, Gargey B; Hansen, Rebecca L; Korte, Andrew R; Reichert, Malinda D; Vela, Javier; Lee, Young Jin

    2016-09-20

    Nanoparticles (NPs) have been suggested as efficient matrixes for small molecule profiling and imaging by laser-desorption ionization mass spectrometry (LDI-MS), but so far there has been no systematic study comparing different NPs in the analysis of various classes of small molecules. Here, we present a large scale screening of 13 NPs for the analysis of two dozen small metabolite molecules. Many NPs showed much higher LDI efficiency than organic matrixes in positive mode and some NPs showed comparable efficiencies for selected analytes in negative mode. Our results suggest that a thermally driven desorption process is a key factor for metal oxide NPs, but chemical interactions are also very important, especially for other NPs. The screening results provide a useful guideline for the selection of NPs in the LDI-MS analysis of small molecules.

  14. Kinetics of hydrogen desorption from MgH2 and AlH3 hydrides

    Science.gov (United States)

    Terent'ev, P. B.; Gerasimov, E. G.; Mushnikov, N. V.; Uimin, M. A.; Maikov, V. V.; Gaviko, V. S.; Golovatenko, V. D.

    2015-12-01

    Kinetic parameters of the process of thermal decomposition of the MgH2 hydride (obtained by the method of the mechanoactivation of magnesium in a hydrogen atmosphere) and of the commercial AlH3 hydride have been studied upon the rapid heating in the range of temperatures of 150-510°C at hydrogen pressures of 0-2 atm. The time dependences of the amount of hydrogen released by the metal hydrides at different temperatures and pressures have been determined. It has been shown that the activation energies of the hydrogen desorption are 135 kJ/mol for MgH2 and 107 kJ/mol for AlH3. The maximum rates of hydrogen desorption from the investigated metal hydrides have been established, and the temperatures and initial pressures that ensure the maximum rate and maximum volume of the hydrogen release have been determined.

  15. Experimental study on effects of CBM temperature-rising desorption

    Institute of Scientific and Technical Information of China (English)

    MA Dong-min; LIN Ya-bing

    2012-01-01

    To study the effects of CBM (coal bed methane) temperature-rising desorption,isothermal adsorption/desorption experiments on three ranks (anthracite,coking coal and lignite) of coal at different temperatures were designed based on the traditional CBM decompression desorption.The experimental results indicate that temperature-rising desorption is more effective in high-rank coal,and ever-increasing temperature of high-rank coal reservoir can reduce the negative effects of coal matrix shrinkage in the process of production and improve the permeability of the coal reservoir as well.It is also revealed that the technique of temperature-rising desorption applied in higher-rank coal reservoir can enhance CBM recovery ratio.This study provided theoretical support for the application of temperature-rising desorption technique in practical discharging and mining projects,which can effectively tackle the gas production bottleneck problem.

  16. The effect of selective desorption mechanisms during interstellar ice formation

    CERN Document Server

    Kalvans, Juris

    2015-01-01

    Major components of ices on interstellar grains in molecular clouds - water and carbon oxides - occur at various optical depths. This implies that selective desorption mechanisms are at work. An astrochemical model of a contracting low-mass molecular cloud core is presented. Ice was treated as consisting of the surface and three subsurface layers (sublayers). Photodesorption, reactive desorption, and indirect reactive desorption were investigated. The latter manifests itself through desorption from H+H reaction on grains. Desorption of shallow subsurface species was included. Modeling results suggest the existence of a "photon-dominated ice" during the early phases of core contraction. Subsurface ice is chemically processed by interstellar photons, which produces complex organic molecules. Desorption from the subsurface layer results in high COM gas-phase abundances at Av = 2.4...10mag. This may contribute towards an explanation for COM observations in dark cores. It was found that photodesorption mostly gove...

  17. Nonisothermal desorption of droplets of complex compositions

    Directory of Open Access Journals (Sweden)

    Nakoryakov Vladimir E.

    2012-01-01

    Full Text Available This paper presents the process of nonstationary evaporation of aqueous solutions of LiBr-H2O, CaCl2-H2O, NaCl-H2O droplets on a horizontal heating surface. The following typical stages of heat and mass transfer depending on wall temperature have been considered: evaporation below boiling temperature and nucleate boiling. The significant decrease in desorption intensity with a rise of initial mass concentration of salt has been observed. Formation of a surface crystallization front at evaporation of a droplet has been detected. We have developed the experimental method for direct measurements of the mass of evaporating droplet.

  18. Displacement desorption test of coalbed methane and its mechanism exploring

    Institute of Scientific and Technical Information of China (English)

    ZHANG Suian; HUO Yongzhong; YE Jianping; TANG Shuheng; MA Dongmin

    2005-01-01

    Through the test of CH4 displaced by CO2 using the coal sample as the adsorbent, this paper has found the coalbed methane (CBM) displacement desorption phenomenon under the natural conditions and CBM mining conditions. With the help of the adsorption theory of the modern physical chemistry and interfacial chemistry, the CBM competitive adsorption and displacement desorption mechanism are intensively discussed, and a new path for studying the CBM desorption mechanism in the CBM exploitation process is explored.

  19. A Transformational Journey: Compositional Changes in Organic Matter during Desorption from Sediments

    Science.gov (United States)

    Matiasek, S. J.; Pellerin, B. A.; Spencer, R.; Bergamaschi, B. A.; Hernes, P.

    2016-12-01

    The release of organic matter (OM) from suspended particles via desorption is a critical component of OM cycling since dissolved OM (DOM) fuels aquatic ecosystems and is a precursor for disinfection by-products formation. This study assessed the elemental and molecular composition of DOM desorbed abiotically from sediments and soils of an irrigated agricultural watershed of northern California. Relative to mineral-bound OM, the released DOM was nitrogen-poor (lower carbon:nitrogen ratios) and depleted in amino acids and lignin phenols (lower carbon-normalized yields). Water-extracted DOM appeared substantially more degraded than its parent particulate OM with increased molar contributions of acidic amino acids, non-protein amino acids, and acidic lignin phenols, all molecular indicators of a more extensively processed OM pool. Desorption processes also significantly altered lignin compositional ratios which help distinguish vascular-plant sources of DOM. Specific optical parameters, including spectral slope, specific UV absorbance at 254 nm (SUVA254), and fluorescence index (FI), did not constitute useful proxies for the desorbed DOM pool, while absorption coefficients and fluorescence peak intensities were strongly correlated with extracted DOM concentrations and composition. This study highlights the profound impact of desorption on DOM composition which, if unaccounted for, could lead to misinterpretations of common biomarkers and optical proxies used to predict DOM sources and reactivity. Our findings suggest that sediments contribute a biogeochemically distinct source of DOM to surface waters, with potential impacts on aquatic health and drinking water quality.

  20. Kinetic isotope effect for H2 and D2 quantum molecular sieving in adsorption/desorption on porous carbon materials.

    Science.gov (United States)

    Zhao, Xuebo; Villar-Rodil, Silvia; Fletcher, Ashleigh J; Thomas, K Mark

    2006-05-25

    Adsorption and desorption of H(2) and D(2) from porous carbon materials, such as activated carbon at 77 K, are usually fully reversible with very rapid adsorption/desorption kinetics. The adsorption and desorption of H(2) and D(2) at 77 K on a carbon molecular sieve (Takeda 3A), where the kinetic selectivity was incorporated by carbon deposition, and a carbon, where the pore structure was modified by thermal annealing to give similar pore structure characteristics to the carbon molecular sieve substrate, were studied. The D(2) adsorption and desorption kinetics were significantly faster (up to x1.9) than the corresponding H(2) kinetics for specific pressure increments/decrements. This represents the first experimental observation of kinetic isotope quantum molecular sieving in porous materials due to the larger zero-point energy for the lighter H(2), resulting in slower adsorption/desorption kinetics compared with the heavier D(2). The results are discussed in terms of the adsorption mechanism.

  1. Substrate-Enhanced Micro Laser Desorption Ionization Mass Spectrometry Project

    Data.gov (United States)

    National Aeronautics and Space Administration — Aerodyne Research, Inc. and the University of Massachusetts at Amherst will collaborate to develop laser desorption ionization (LDI) mass spectrometric analysis of...

  2. Testosterone sorption and desorption: Effects of soil particle size

    Energy Technology Data Exchange (ETDEWEB)

    Qi, Yong, E-mail: yqi01@unomaha.edu [Civil Engineering Dept., University of Nebraska-Lincoln at Omaha Campus, Omaha, NE 68182 (United States); Zhang, Tian C. [Civil Engineering Dept., University of Nebraska-Lincoln at Omaha Campus, Omaha, NE 68182 (United States); Ren, Yongzheng [School of Environmental Science and Engineering, Huazhong University of Science and Technology, Wuhan 430074 (China)

    2014-08-30

    Graphical abstract: - Highlights: • Smaller soil particles have higher sorption and lower desorption rates. • The sorption capacity ranks as clay > silt > sand. • Small particles like clays have less potential for desorption. • Colloids (clays) have high potential to facilitate the transport of hormones in soil–water environments. - Abstract: Soils contain a wide range of particles of different diameters with different mobility during rainfall events. Effects of soil particles on sorption and desorption behaviors of steroid hormones have not been investigated. In this study, wet sieve washing and repeated sedimentation methods were used to fractionate the soils into five ranges. The sorption and desorption properties and related mechanisms of testosterone in batch reactors filled with fractionated soil particles were evaluated. Results of sorption and desorption kinetics indicate that small soil particles have higher sorption and lower desorption rates than that of big ones. Thermodynamic results show the sorption processes are spontaneous and exothermal. The sorption capacity ranks as clay > silt > sand, depending mainly on specific surface area and surface functional groups. The urea control test shows that hydrogen bonding contributes to testosterone sorption onto clay and silt but not on sand. Desorption tests indicate sorption is 36–65% irreversible from clay to sand. Clays have highest desorption hysteresis among these five soil fractions, indicating small particles like clays have less potential for desorption. The results provide indirect evidence on the colloid (clay)-facilitated transport of hormones (micro-pollutants) in soil environments.

  3. Extraction of rutin from Tartary buckwheat milling fractions and evaluation of its thermal stability in an instant fried noodle system.

    Science.gov (United States)

    Cho, Yong Jin; Lee, Suyong

    2015-06-01

    Extraction conditions of rutin from buckwheat milling fractions were established and a rutin-enriched material (REM, 31.8g/100g of rutin) was successfully obtained by the ultrasonic-assisted ethanol method (steaming, 16-150 mesh particle size, 70% ethanol, and ultrasonication at 40°C for 30min). When REM was applied to instant fried noodles (1% and 2% by weight of wheat flour) for rutin fortification, the levels of rutin in the noodles were determined to be about 250-500mg/100g which corresponded to the recommended daily dose of rutin. While frying temperatures (150-190°C) and times (1-3min) did not negatively affect the level of rutin in the instant fried noodles, the distinct loss of rutin was observed after cooking. Furthermore, REM did not significantly affect the oil uptake and mechanical property of instant fried noodles. The strong antioxidant activity of rutin in REM contributed to retarding the oxidative deterioration of the noodles during storage. Copyright © 2014 Elsevier Ltd. All rights reserved.

  4. 番泻叶提取物中番泻苷B的热稳定性%Thermal Stability of Sennoside B in Cassia angustifolia Extracts

    Institute of Scientific and Technical Information of China (English)

    陈丹丹; 徐建国; 薛桂蓬; 邢建国

    2013-01-01

    目的:比较不同干燥方法对番泻叶提取物中番泻苷B的影响.方法:以番泻苷B含量为指标,采用单因素试验考察减压浓缩和真空干燥时不同温度的影响;通过正交试验考察进风温度、出风温度及喷速对番泻叶提取物喷雾干燥工艺的影响.结果:番泻叶提取物减压浓缩和真空干燥时最佳温度均为60℃,耗时分别为87 min,58 h;优选的喷雾干燥工艺为进风温度120℃,出风温度55℃,喷速16 mL·min-1.结论:与喷雾干燥相比,真空干燥时番泻苷B含量损失较多;喷雾干燥既节约时间又有利于有效成分的保留,优选的喷雾干燥工艺稳定可行,可用于对热不稳定的番泻叶提取物的干燥.%Objective:To compare effect of different drying methods on the content of sennoside B in Cassia angustifolia extracts. Method:With the content of sennoside B as index, effect of reduced pressure condensing and vacuum drying at different temperatures on the content of sennoside B were investigated by single-factor test; Orthogonal test was used to investigate influence of inlet temperature, outlet temperature and spray velocity on spray drying technology of C. angustifolia extracts. Result:Optimal temperature of reduced pressure concentrating and vacuum drying for C. angustifolia extracts were 60 ℃ , their time-consuming were 87 min, 58 h, respectively; Optimum spray drying technology parameters were as followings:inlet air temperature 120 ℃ , outlet air temperature 55 ℃ , spraying velocity 16 mL · min-1. Conclusion:Loss of sennoside B by vacuum drying was more than spray drying; spray drying was time saving and beneficial to retention of effective ingredients, optimized spray drying process was stable and feasible, and it could be used for drying of C. angustifolia extracts with thermal instability.

  5. Metsulfuron-methyl Molecularly Imprinted Stir Bar Sorptive Extraction Coupled with High Performance Liquid Chromatography for Trace Sulfonylurea Herbicides Analysis in Complex Samples

    Institute of Scientific and Technical Information of China (English)

    XU Zhi-gang; DU Zhuo; LIAN Hai-xian; HU Yu-ling; LI Gong-ke

    2012-01-01

    Metsulfuron-methyl molecularly imprinted polymer(MIP)-coated stir bar was prepared for sorptive extraction of sulfonylurea herbicides in complex samples.The MIP-coating was about 21.3 μm thickness with the relative standard deviation(RSD) of 4.4%(n=10).It was homogeneous and porous with good thermal stability and chemical stability.The extraction capability of the MIP-coating was 2.8 timcs over that of the non-imprinted polymer (NIP)-coating in hexane.The MIP-coating exhibited selective adsorption ability to the template and its analogues.The extraction conditions,including extraction solvent,desorption solvent,extraction time,desorption time and stirring speed,were optimized.A method for the determination of six sulfonylurea herbicides by MIP-coated stir bar sorptive extraction coupled with high performance liquid chromatography(HPLC) was developed.The linear range was 10-200 μg/L and the detection limits were within a range of 2.0-3.3 μg/L.It was also applied to the analysis of sulfonylurea herbicides in spiked river water,soil and rice samples.

  6. UV-Vis diagnostics of the pmma-c 60 composite system and the kinetics of its thermal decomposition

    OpenAIRE

    Bogdanov, A. A.; VOZNYAKOVSKII A.P.; POZDNYAKOV A.O.

    2014-01-01

    The influence of polymer-fullerene interactions and fullerene aggregation on the thermal stability of polymethyl-methacrylate-fullerene C 60 nanocomposite has been studied by means of thermal desorption mass-spectrometry and the UV-Vis absorption spectroscopy.

  7. UV-VIS DIAGNOSTICS OF THE PMMA-C 60 COMPOSITE SYSTEM AND THE KINETICS OF ITS THERMAL DECOMPOSITION

    OpenAIRE

    Bogdanov, A A; VOZNYAKOVSKII A.P.; POZDNYAKOV A.O.

    2014-01-01

    The influence of polymer-fullerene interactions and fullerene aggregation on the thermal stability of polymethyl-methacrylate-fullerene C 60 nanocomposite has been studied by means of thermal desorption mass-spectrometry and the UV-Vis absorption spectroscopy.

  8. CO and N$_2$ desorption energies from water ice

    CERN Document Server

    Fayolle, Edith C; Loomis, Ryan; Bergner, Jennifer; Graninger, Dawn M; Rajappan, Mahesh; Öberg, Karin I

    2015-01-01

    The relative desorption energies of CO and N$_2$ are key to interpretations of observed interstellar CO and N$_2$ abundance patterns, including the well-documented CO and N$_2$H$^+$ anti-correlations in disks, protostars and molecular cloud cores. Based on laboratory experiments on pure CO and N$_2$ ice desorption, the difference between CO and N$_2$ desorption energies is small; the N$_2$-to-CO desorption energy ratio is 0.93$\\pm$0.03. Interstellar ices are not pure, however, and in this study we explore the effect of water ice on the desorption energy ratio of the two molecules. We present temperature programmed desorption experiments of different coverages of $^{13}$CO and $^{15}$N$_2$ on porous and compact amorphous water ices and, for reference, of pure ices. In all experiments, $^{15}$N$_2$ desorption begins a few degrees before the onset of $^{13}$CO desorption. The $^{15}$N$_2$ and $^{13}$CO energy barriers are 770 and 866 K for the pure ices, 1034-1143 K and 1155-1298 K for different sub-monolayer co...

  9. Feasibility of the direct coupling of solid-phase extraction-pipette tips with a programmed-temperature vaporiser for gas chromatographic analysis of drugs in plasma

    NARCIS (Netherlands)

    van Hout, M.W J; van Egmond, W.M A; Franke, J.P.; de Zeeuw, R.A; de Jong, G.J.

    2002-01-01

    Solid-phase extraction-pipette tips (SPE-PTs) were used for micro solid-phase extraction of lidocaine and diazepam from plasma. Off-line extraction was followed by on-line desorption. On-line desorption was carried out by direct coupling of the SPE-PTs with the liner of the programmed-temperature va

  10. Integrated field emission array for ion desorption

    Energy Technology Data Exchange (ETDEWEB)

    Resnick, Paul J; Hertz, Kristin L.; Holland, Christopher; Chichester, David

    2016-08-23

    An integrated field emission array for ion desorption includes an electrically conductive substrate; a dielectric layer lying over the electrically conductive substrate comprising a plurality of laterally separated cavities extending through the dielectric layer; a like plurality of conically-shaped emitter tips on posts, each emitter tip/post disposed concentrically within a laterally separated cavity and electrically contacting the substrate; and a gate electrode structure lying over the dielectric layer, including a like plurality of circular gate apertures, each gate aperture disposed concentrically above an emitter tip/post to provide a like plurality of annular gate electrodes and wherein the lower edge of each annular gate electrode proximate the like emitter tip/post is rounded. Also disclosed herein are methods for fabricating an integrated field emission array.

  11. Methane desorption from a coal-bed

    Energy Technology Data Exchange (ETDEWEB)

    A.D. Alexeev; E.P. Feldman; T.A. Vasilenko [National Academy of Sciences of Ukraine, Donetsk (Ukraine). Donetsk Institute for Physics of Mining Processes

    2007-11-15

    We study the desorption of methane from a coal-bed. A model taking into account both methane diffusion in coal-blocks and its filtration through the system of open pores and cracks is developed. Methane pressure in the coal-bed is found for an arbitrary instant of time. Dependency of the rate of methane release upon the block size, open and closed porosity, viscosity, solubility, bed pressure and temperature is established. We derive the effective coefficient of diffusion of methane in blocks containing closed pores filled with gaseous methane. It is shown that at a hindered diffusion methane is distinctly divided into the 'quick' and the 'slow' one. 25 refs., 5 figs.

  12. Integrated field emission array for ion desorption

    Energy Technology Data Exchange (ETDEWEB)

    Resnick, Paul J; Hertz, Kristin L; Holland, Christopher; Chichester, David; Schwoebel, Paul

    2013-09-17

    An integrated field emission array for ion desorption includes an electrically conductive substrate; a dielectric layer lying over the electrically conductive substrate comprising a plurality of laterally separated cavities extending through the dielectric layer; a like plurality of conically-shaped emitter tips on posts, each emitter tip/post disposed concentrically within a laterally separated cavity and electrically contacting the substrate; and a gate electrode structure lying over the dielectric layer, including a like plurality of circular gate apertures, each gate aperture disposed concentrically above an emitter tip/post to provide a like plurality of annular gate electrodes and wherein the lower edge of each annular gate electrode proximate the like emitter tip/post is rounded. Also disclosed herein are methods for fabricating an integrated field emission array.

  13. Integrated field emission array for ion desorption

    Science.gov (United States)

    Resnick, Paul J; Hertz, Kristin L; Holland, Christopher; Chichester, David; Schwoebel, Paul

    2013-09-17

    An integrated field emission array for ion desorption includes an electrically conductive substrate; a dielectric layer lying over the electrically conductive substrate comprising a plurality of laterally separated cavities extending through the dielectric layer; a like plurality of conically-shaped emitter tips on posts, each emitter tip/post disposed concentrically within a laterally separated cavity and electrically contacting the substrate; and a gate electrode structure lying over the dielectric layer, including a like plurality of circular gate apertures, each gate aperture disposed concentrically above an emitter tip/post to provide a like plurality of annular gate electrodes and wherein the lower edge of each annular gate electrode proximate the like emitter tip/post is rounded. Also disclosed herein are methods for fabricating an integrated field emission array.

  14. Electrical Characteristics and Desorption Kinetics of Soil Boron

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    The status and activities of boron in soils were studied by the approach of electro-ultrafiltration (EUF). The samples of soils, including brown-red soil and calcareous alluvial soil, were collected from Hubei Province of China. The soil samples were incubated in saturated water and then their nutrients were ultrafiltrated with EUF equipment. Filtration and extraction were conducted in accordance with routine process, but fractions in anode and cathode were all collected. Analyses of B, K+, Mg2+, Ca2+, C1- and pH in fractions supposed that boron existed not only in a simple form of borate but also in ion-pair with cations partly in acidic soil,and borate was the primary form existing in the calcareous soil. In studying desorption kinetics with EUF,the boron content of Fractions 2~6 was accumulated, and the accumulative quantities were fit to time factors in three kinetic equations: the zero-order, first-order, and arabolic diffusion equations. Fit degree of the parabolic diffusion equation was the best, followed by the zero-order quation, and the first-order equation was the worst.

  15. The application of thermal methods for determining chemical composition of carbonaceous aerosols: a review.

    Science.gov (United States)

    Chow, Judith C; Yu, Jian Zhen; Watson, John G; Ho, Steven Sai Hang; Bohannan, Theresa L; Hays, Michael D; Fung, Kochy K

    2007-09-01

    Thermal methods of various forms have been used to quantify carbonaceous materials. Thermal/optical carbon analysis provides measurements of organic and elemental carbon concentrations as well as fractions evolving at specific temperatures in ambient and source aerosols. Detection of thermally desorbed organic compounds with thermal desorption-gas chromatography/mass spectrometry (TD-GC/MS) identifies and quantifies over 100 individual organic compounds in particulate matter (PM) samples. The resulting mass spectra contain information that is consistent among, but different between, source emissions even in the absence of association with specific organic compounds. TD-GC/MS is a demonstrated alternative to solvent extraction for many organic compounds and can be applied to samples from existing networks. It is amenable to field-deployable instruments capable of measuring organic aerosol composition in near real-time. In this review, thermal stability of organic compounds is related to chemical structures, providing a basis for understanding thermochemical properties of carbonaceous aerosols. Recent advances in thermal methods applied to determine aerosol chemical compositions are summarized and their potential for uncovering aerosol chemistry are evaluated. Current limitations and future research needs of the thermal methods are included.

  16. Brominated Tyrosine and Polyelectrolyte Multilayer Analysis by Laser Desorption VUV Postionization and Secondary Ion Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    University of Illinois at Chicago; Blaze, Melvin M. T.; Takahashi, Lynelle; Zhou, Jia; Ahmed, Musahid; Gasper, Gerald; Pleticha, F. Douglas; Hanley, Luke

    2011-03-14

    The small molecular analyte 3,5-dibromotyrosine (Br2Y) and chitosan-alginate polyelectrolyte multilayers (PEM) with and without adsorbed Br2Y were analyzed by laser desorption postionization mass spectrometry (LDPI-MS). LDPI-MS using 7.87 eV laser and tunable 8 ? 12.5 eV synchrotron vacuum ultraviolet (VUV) radiation found that desorption of clusters from Br2Y films allowed detection by≤8 eV single photon ionization. Thermal desorption and electronic structure calculations determined the ionization energy of Br2Y to be ~;;8.3?0.1 eV and further indicated that the lower ionization energies of clusters permitted their detection at≤8 eV photon energies. However, single photon ionization could only detect Br2Y adsorbed within PEMs when using either higher photon energies or matrix addition to the sample. All samples were also analyzed by 25 keV Bi3 + secondary ion mass spectrometry (SIMS), with the negative ion spectra showing strong parent ion signal which complemented that observed by LDPI-MS. The negative ion SIMS depended strongly on the high electron affinity of this specific analyte and the analyte?s condensed phase environment.

  17. Desorption and Degradation of Organic Contaminants in Soil by Microwave Radiation

    Science.gov (United States)

    Jeong, S.; Kim, H.

    2011-12-01

    Many military bases located in the down towns of South Korea are asked to move outside of the urban areas due to the growth of the cities. During the past 60 years, many military bases of South Korea have been operated and according to that, parts of the soil have been polluted with organic contaminants such as total petroleum hydrocarbons (TPH), solvents, etc. In the case of South Korea, rapid remediation of the contaminated soil is required for efficient development of land. Thermal desorption is one of the most efficient and rapid remediation methods for polluted soil to clean up, but the fact is it consumes a lot of energy. In this study, desorption and degradation of organic contaminants in soil using microwave radiation is investigated in order to energy efficient and rapid remediation technique development. Polluted soil collected from a military base was remediated in the laboratory using a home made microwave reactor. In order to study uncontaminated soil was also intentionally contaminated with diesel, TCE, and phenanthrene, respectively, for a month and used for experiments. Contaminated soil places within stainless steel reactor and microwave radiates with nitrogen gas. Emitted gas from the reactor was collected with methanol or acetonitrile solution every 3 minute for 15 minutes, and analyzed with GC, HPLC, GC/MS, respectively. The TPH contaminated soil from military base desorbed initially light hydrocarbon (retention time reaction, iron powder, graphite will be added to the contaminated soil and desorption and degradation properties of this soil during microwave radiation will be studied.

  18. Searching out the hydrogen absorption/desorption limiting reaction factors: Strategies allowing to increase kinetics

    Energy Technology Data Exchange (ETDEWEB)

    Zeaiter, Ali, E-mail: ali.zeaiter@femto-st.fr; Chapelle, David; Nardin, Philippe

    2015-10-05

    Highlights: • A macro scale thermodynamic model that simulates the response of a FeTi-X hydride tank is performed, and validated experimentally. • A sensibility study to identify the most influent input variables that can changes very largely the reaction rate. - Abstract: Hydrogen gas has become one of the most promising energy carriers. Main breakthrough concerns hydrogen solid storage, specially based on intermetallic material use. Regarding the raw material abundance and cost, the AB type alloy FeTi is an auspicious candidate to store hydrogen. Its absorption/desorption kinetics is a basic hindrance to common use, compared with more usual hydrides. First, discussions based on literature help us identifying the successive steps leading to metal hydriding, and allow to introduce the physical parameters which drive or limit the reaction. This analysis leads us to suggest strategies in order to increase absorption/desorption kinetics. Attention is then paid to a thermofluidodynamic model, allowing to describe a macroscopic solid storage reactor. Thus, we can achieve a simulation which describes the overall reaction inside the hydrogen reactor and, by varying the sub-mentioned parameters (thermal conductivity, the powder granularity, environment heat exchange…), we attempt to hierarchy the reaction limiting factors. These simulations are correlated to absorption/desorption experiments for which pressure, temperature and hydrogen flow are recorded.

  19. Variable Temperature Infrared Spectroscopy Investigations of Benzoic Acid Desorption from Sodium and Calcium Montmorillonite Clays.

    Science.gov (United States)

    Nickels, Tara M; Ingram, Audrey L; Maraoulaite, Dalia K; White, Robert L

    2015-12-01

    Processes involved in thermal desorption of benzoic acid from sodium and calcium montmorillonite clays are investigated by using variable temperature diffuse reflection Fourier transform infrared spectroscopy (DRIFTS). By monitoring the temperature dependence of infrared absorbance bands while heating samples, subtle changes in molecular vibrations are detected and employed to characterize specific benzoic acid adsorption sites. Abrupt changes in benzoic acid adsorption site properties occur for both clay samples at about 125 °C. Difference spectra absorbance band frequency variations indicate that adsorbed benzoic acid interacts with interlayer cations through water bridges and that these interactions can be disrupted by the presence of organic anions, in particular, benzoate.

  20. Electron- and Photon-stimulated Desorption of Alkali Atoms from Lunar Sample and a Model Mineral Surface

    Science.gov (United States)

    Yakshinskiy, B. V.; Madey, T. E.

    2003-01-01

    We report recent results on an investigation of source mechanisms for the origin of alkali atoms in the tenuous planetary atmospheres, with focus on non-thermal processes (photon stimulated desorption (PSD), electron stimulated desorption (ESD), and ion sputtering). Whereas alkaline earth oxides (MgO, CaO) are far more abundant in lunar samples than alkali oxides (Na2O, K2O), the atmosphere of the Moon contains easily measurable concentrations of Na and K, while Ca and Mg are undetected there; traces of Ca have recently been seen in the Moon's atmosphere (10-3 of Na). The experiments have included ESD, PSD and ion sputtering of alkali atoms from model mineral surface (amorphous SiO2) and from a lunar basalt sample obtained from NASA. The comparison is made between ESD and PSD efficiency of monovalent alkalis (Na, K) and divalent alkaline earths (Ba, Ca).The ultrahigh vacuum measurement scheme for ESD and PSD of Na atoms includes a highly sensitive alkali metal detector based on surface ionization, and a time-of-flight technique. For PSD measurements, a mercury arc light source (filtered and chopped) is used. We find that bombardment of the alkali covered surfaces by ultraviolet photons or by low energy electrons (E>4 eV) causes desorption of hot alkali atoms. This results are consistent with the model developed to explain our previous measurements of sodium desorption from a silica surface and from water ice: electron- or photon-induced charge transfer from the substrate to the ionic adsorbate causes formation of a neutral alkali atom in a repulsive configuration, from which desorption occurs. The two-electron charge transfer to cause desorption of divalent alkaline eath ions is a less likely process.The data support the suggestion that PSD by UV solar photons is a dominant source process for alkalis in the tenuous lunar atmosphere.

  1. Adsorption-Desorption Characteristics of Chlorimuron-Ethyl in Soils

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    The adsorption-desorption characteristics of chlorimuron-ethyl in soils were investigated to provide the basic data for evaluating the safety in field and the risk to water resource. The adsorption-desorption experiment was conducted by the batch equilibration and HPLC techniques; furthermore, data were analyzed with 5 mathematic models to describe the characteristics and mechanism of adsorption-desorption and translocation of the herbicide in soils. The results showed that the adsorption-desorption isotherms of chlorimuron-ethyl fitted for the Freundlich model well, and the physical reaction presents the main contribution during the adsorption-desorption process. The adsorption values (Kads-f) of chlorimuron-ethyl in 8 types of soil ranged from 0.798 to 6.891. The isotherms of 2# (Jiangxi clay) and 3# (Jiangxi sand loam)soils belong to the S-type curve, while the isotherms of another 6 type soils belong to the L-type isotherm. The results of desorption indicated that the hysteresis phenomena appeared during the desorption process, and the hysteresis coefficients(H) of the herbicides in 8 soils varied from 0.259-0.980. Furthermore, Kads-f and desorption values (Kdes-f) increased with the OM (%) and the clay content increasing, while the values decreased with the soils pH increasing. The H values decreased with the OM and the clay content increasing, and increased with the soils pH increasing. It can be concluded that the low adsorption abilities of chlorimuron-ethyl in test soils and un-reversible adsorption existed in the process, which will induce the great translocation of the herbicide after application in field. It can be transported to ground or groundwater causing risk to environments. The physical and chemical properties of soils, including the OM, the clay content, and the pH of soil were the dominating factors during the adsorption-desorption.

  2. 24-HOUR DIFFUSIVE SAMPLING OF 1,3-BUTADIENE IN AIR ONTO CARBONPAK X SOLID ADSORBENT WITH THEMAL DESORPTION/GC/MS ANALYSIS - FEASIBILITY STUDIES

    Science.gov (United States)

    Diffusive sampling of 1,3-butadiene for 24 hours onto the graphitic adsorbent Carbopack X contained in a stainless steel tube badge (6.3 mm OD, 5 mm ID, and 90 mm in length) with analysis by thermal desorption/GC/MS has been evaluated in controlled tests. A test matrix of 42 tr...

  3. Temperature programmed desorption of weakly bound adsorbates on Au(111)

    Science.gov (United States)

    Engelhart, Daniel P.; Wagner, Roman J. V.; Meling, Artur; Wodtke, Alec M.; Schäfer, Tim

    2016-08-01

    We have performed temperature programmed desorption (TPD) experiments to analyze the desorption kinetics of Ar, Kr, Xe, C2H2, SF6, N2, NO and CO on Au(111). We report desorption activation energies (Edes), which are an excellent proxy for the binding energies. The derived binding energies scale with the polarizability of the molecules, consistent with the conclusion that the surface-adsorbate bonds arise due to dispersion forces. The reported results serve as a benchmark for theories of dispersion force interactions of molecules at metal surfaces.

  4. Hydrogen Desorption from Mg Hydride: An Ab Initio Study

    Directory of Open Access Journals (Sweden)

    Simone Giusepponi

    2012-07-01

    Full Text Available Hydrogen desorption from hydride matrix is still an open field of research. By means of accurate first-principle molecular dynamics (MD simulations an Mg–MgH2 interface is selected, studied and characterized. Electronic structure calculations are used to determine the equilibrium properties and the behavior of the surfaces in terms of structural deformations and total energy considerations. Furthermore, extensive ab-initio molecular dynamics simulations are performed at several temperatures to characterize the desorption process at the interface. The numerical model successfully reproduces the experimental desorption temperature for the hydride.

  5. Effect of Grapefruit Seed Extract on Thermal Inactivation of Listeria monocytogenes during Sous-Vide Processing of Two Marinated Mexican Meat Entrées.

    Science.gov (United States)

    Valenzuela-Melendres, Martin; Peña-Ramos, E Aida; Juneja, Vijay K; Camou, Juan Pedro; Cumplido-Barbeitia, German

    2016-07-01

    D- and z-values for Listeria monocytogenes were obtained for two Mexican meat entrées: pork meat marinated in tomatillo (green tomato) sauce (PTS) and beef marinated in a red chili sauce (BRCS), with addition of 0, 200, and 800 ppm of grapefruit seed extract (GSE). Meat samples inoculated with L. monocytogenes were packaged in sterile bags, immersed in a water bath, and held at 55, 57.5, 60, and 62.5°C for different periods of time. Depending upon the temperature, D-values at 0 ppm of GSE ranged from 26.19 to 2.03 min in BRCS and 26.41 to 0.8 min in PTS. Adding 800 ppm of GSE to BRCS thermally treated at 55 and 62.5°C significantly decreased inactivation time by 35%. A reduction in time of 25.9, 10.6, and 40.1% at 55, 57.5, and 60°C, respectively, was observed in PTS with 800 ppm of GSE. The z-values of L. monocytogenes were not significantly affected by GSE addition; average z-values were 7.25 and 5.09°C for BRCS and PTS, respectively. Estimated thermal lethality for a 7-D log reduction of L. monocytogenes under commercial-size sous-vide conditions at a reference temperature of 55°C was reached at 78 and 71 min for BRCS without and with 800 ppm of GSE, respectively. For PTS, 7-D reduction was attained at 69 and 61 min without and with addition of 800 ppm of GSE, respectively. Supplementing both Mexican meat entrées (BRCS and PTS) with 800 ppm of GSE rendered L. monocytogenes cells more sensitive to the lethal effect of heat. The results of this study will assist the retail food industry in designing acceptance limits on critical control points pertaining to cooking regimes to effectively eliminate L. monocytogenes in BRCS and PTS sous-vide processed Mexican meat entrées.

  6. Determination of synthetic phenolic antioxidants in soft drinks by stir-bar sorptive extraction coupled to gas chromatography-mass spectrometry.

    Science.gov (United States)

    Cacho, Juan Ignacio; Campillo, Natalia; Viñas, Pilar; Hernández-Córdoba, Manuel

    2015-01-01

    The synthetic phenolic antioxidants butylated hydroxyanisole (BHA), butylated hydroxytoluene (BHT) and tert-butyl hydroquinone (TBHQ) were pre-concentrated by stir-bar sorptive extraction and thermally desorbed (SBSE-TD) before analysis by GC-MS. Several parameters affecting the derivatisation step and both SBSE extraction and thermal desorption were carefully optimised. When the analyses of BHA and TBHQ in their acetylated, silylated and underivatised forms were compared, the best results were obtained when the in-situ derivatisation procedure with acetic anhydride was employed. Quantification was carried out using carvacrol as the internal standard, providing quantification limits of between 0.11 and 0.15 ng ml(-1), depending on the compound. Recovery assays for samples spiked at two concentration levels, 1 and 5 ng ml(-1), provided recoveries in the 81-117% range. The proposed method was applied in the analysis canned soft drinks and the analytes were found in five of the 10 samples analysed.

  7. Desorption kinetics of benzene in a sandy soil in the presence of powdered activated carbon.

    Science.gov (United States)

    Choi, J-W; Kim, S-B; Kim, D-J

    2007-02-01

    Desorption kinetics of benzene was investigated with a modified biphasic desorption model in a sandy soil with five different powdered activated carbon (PAC) contents (0, 1, 2, 5, 10% w/w) as sorbents. Sorption experiments followed by series dilution desorption were conducted for each sorbent. Desorption of benzene was successively performed at two stages using deionized water and hexane. Modeling was performed on both desorption isotherm and desorption rate for water-induced desorption to elucidate the presence of sorption-desorption hysteresis and biphasic desorption and if present to quantify the desorption-resistant fraction (q (irr)) and labile fraction (F) of desorption site responsible for rapid process. Desorption isotherms revealed that sorption-desorption exhibited a severe hysteresis with a significant fraction of benzene being irreversibly adsorbed onto both pure sand and PAC, and that desorption-resistant fraction (q (irr)) increased with PAC content. Desorption kinetic modeling showed that desorption of benzene was biphasic with much higher (4-40 times) rate constant for rapid process (k (1)) than that for slow process (k (2)), and that the difference in the rate constant increased with PAC content. The labile fraction (F) of desorption site showed a decreasing tendency with PAC. The experimental results would provide valuable information on remediation methods for soils and groundwater contaminated with BTEX.

  8. Salt Tolerance of Desorption Electrospray Ionization (DESI)

    Energy Technology Data Exchange (ETDEWEB)

    Jackson, Ayanna U. [Purdue University; Talaty, Nari [Purdue University; Cooks, R G [Purdue University; Van Berkel, Gary J [ORNL

    2007-01-01

    Suppression of ion intensity in the presence of high salt matrices is common in most mass spectrometry ionization techniques. Desorption electrospray ionization (DESI) is an ionization method that exhibits salt tolerance, and this is investigated. DESI analysis was performed on three different drug mixtures in the presence of 0, 0.2, 2, 5, 10, and 20% NaCl:KCl weight by volume from seven different surfaces. At physiological concentrations individual drugs in each mixture were observed with each surface. Collision-induced dissociation (CID) was used to provide additional confirmation for select compounds. Multiple stage experiments, to MS5, were performed for select compounds. Even in the absence of added salt, the benzodiazepine containing mixture yielded sodium and potassium adducts of carbamazepine which masked the ions of interest. These adducts were eliminated by adding 0.1% 7M ammonium acetate to the standard methanol:water (1:1) spray solvent. Comparison of the salt tolerance of DESI with that of electrospray ionization (ESI) demonstrated much better signal/noise characteristics for DESI in this study. The salt tolerance of DESI was also studied by performing limit of detection and dynamic range experiments. Even at a salt concentration significantly above physiological concentrations, select surfaces were effective in providing spectra that allowed the ready identification of the compounds of interest. The already high salt tolerance of DESI can be optimized further by appropriate choices of surface and spray solution.

  9. Tailoring the hydrogen desorption thermodynamics of V{sub 2}H by alloying additives

    Energy Technology Data Exchange (ETDEWEB)

    Kumar, Sanjay, E-mail: sanjay.barc@gmail.com [Fusion Reactor Materials Section, BARC, Mumbai (India); Tiwari, G.P. [R.A. Institute of Technology, Vidya Nagri, Nerul 400709, Navi Mumbai (India); Krishnamurthy, N. [Fusion Reactor Materials Section, BARC, Mumbai (India)

    2015-10-05

    Highlights: • Decomposition of VH{sub 2} is three step process. • Electronic structure and H solubility are correlated. • Addition of hydride forming metal enhance the thermal stability of V{sub 2}H. • Lattices strain energy could decrease thermal stability of V{sub 2}H. - Abstract: Vanadium could be a potential candidate for on board hydrogen storage application because of its high gravimetric hydrogen storage capacity (∼3.8 mass%) which is even better then the most widely explored AB{sub 5}, AB{sub 2} & AB intermetallic compounds. Hydrogen absorption of vanadium takes place at ambient temperature and pressure with fast kinetics. The vanadium hydride (VH{sub 2}) releases hydrogen in two steps: (1) VH{sub 2}(γ){sub (s)} ↔ ½ V{sub 2}H(β){sub (s)} and (2) V{sub 2}H(β){sub (s)} ↔ 2V{sub (s)} + ½ H{sub 2(g)}. First step is achievable at the ambient temperature and pressure conditions while, the second step requires high temperature (590 K). Thus only half of the total hydrogen storage capacity is available for use on subsequent absorption–desorption cycles at the ambient temperature. The usable hydrogen storage capacity of VH{sub 2} at ambient conditions could be enhanced by tailoring the thermodynamics and kinetics of second step of hydrogen desorption reaction. This could be possible by selecting suitable alloy additives. The present study deals with the selection criteria of alloy additives based on the electronic consideration to tailor the hydrogen desorption thermodynamics and kinetics of V{sub 2}H.

  10. Microstructure and He desorption behaviors of He charged FeCrNi-based films fabricated by direct current magnetron sputtering

    Energy Technology Data Exchange (ETDEWEB)

    Song, L. [Key Laboratory of Materials Physics, Institute of Solid State Physics, Chinese Academy of Sciences, P.O. Box 1129, Hefei 230031 (China); Wang, X.P., E-mail: xpwang@issp.ac.cn [Key Laboratory of Materials Physics, Institute of Solid State Physics, Chinese Academy of Sciences, P.O. Box 1129, Hefei 230031 (China); Liu, F. [Institute of Plasma Physics, Chinese Academy of Sciences, P.O. Box 1126, Hefei 230031 (China); Gao, Y.X. [Key Laboratory of Materials Physics, Institute of Solid State Physics, Chinese Academy of Sciences, P.O. Box 1129, Hefei 230031 (China); Zhang, T., E-mail: zhangtao@issp.ac.cn [Key Laboratory of Materials Physics, Institute of Solid State Physics, Chinese Academy of Sciences, P.O. Box 1129, Hefei 230031 (China); Luo, G.N. [Institute of Plasma Physics, Chinese Academy of Sciences, P.O. Box 1126, Hefei 230031 (China); Fang, Q.F.; Liu, C.S. [Key Laboratory of Materials Physics, Institute of Solid State Physics, Chinese Academy of Sciences, P.O. Box 1129, Hefei 230031 (China)

    2015-08-31

    He-charged FeCrNi-based films were prepared at different temperatures in a mixed atmosphere of He and Ar by direct-current magnetron sputtering method. X-ray diffraction and energy dispersive spectrometry analysis confirmed the typical austenitic structure of the deposited FeCrNi films and the compositions were in good accordance with 304 stainless steel target. Cross-sectional scanning electron microscopy images revealed the dense columnar nanocrystalline structure of the fabricated FeCrNi films. Nanoindentation measurements showed that the film fabricated at 300 °C exhibited the highest hardness value of 11.5 GPa. He desorption from FeCrNi-based films was traced by thermal desorption spectroscopy; the relatively low He desorption temperature range (150 °C–450 °C) implied that the charged He atoms were mainly located in interstitial sites of FeCrNi-based films. - Highlights: • He-charged columnar nanocrystalline FeCrNi films were prepared by DC magnetron sputtering. • Substrate temperature of 300 °C and He/Ar ratio 1:1 were the best sputtering parameters. • Compact and uniform microstructure obtained at 300 °C resulted in stable, high hardness. • Two He atoms' absorption/desorption mechanisms were revealed by TDS.

  11. Evaluation of stability of allergen extracts for sublingual immunotherapy during transport under unfavourable temperature conditions with an innovative thermal insulating packaging.

    Science.gov (United States)

    Puccinelli, P; Natoli, V; Dell'albani, I; Scurati, S; Incorvaia, C; Barbieri, S; Masieri, S; Frati, F

    2013-10-01

    Many pharmaceutical and biotechnological products are temperature-sensitive and should normally be kept at a controlled temperature, particularly during transport, in order to prevent the loss of their stability and activity. Therefore, stability studies should be performed for temperature-sensitive products, considering product characteristics, typical environmental conditions, and anticipating environmental extremes that may occur during product transport in a specific country. Staloral products for sublingual immunotherapy are temperature sensitive and are labelled for maintenance under refrigerated conditions (2-8°C). Given the peculiar climatic context of Italy and the great temperature fluctuations that may occur during transport, this study was aimed at evaluating the impact of a new engineered thermal insulating packaging for Staloral. In particular, the purpose was to assess whether the new packaging could create a container condition able to preserve the stability and immunological activity of the product during the transport phase throughout Italy. The results showed that the range of temperatures that can affect the product, in the area surrounding the product packaging, may reach a peak of 63°C during transport under the most unfavourable climatic conditions, i.e. in a non-refrigerated van during the summer season, from the site of production in France to the patient's house in Catania, the city with the highest temperatures in Italy. However, the highest temperature reached inside the vaccine did not exceed 45°C over a period of about 2 h. The ELISA inhibition test on samples subjected to the extreme temperature conditions previously defined (45°C) showed an immunological activity higher than 75% of that initially measured and was comparable to those obtained with samples stored at controlled temperature (5°C). This means that, even in the worst case scenario, the structure of the allergen extracts is not influenced and the vaccine potency is

  12. Adsorption and desorption kinetics of carbofuran in acid soils.

    Science.gov (United States)

    Bermúdez-Couso, Alipio; Fernández-Calviño, David; Pateiro-Moure, Miriam; Nóvoa-Muñoz, Juan Carlos; Simal-Gándara, Jesús; Arias-Estévez, Manuel

    2011-06-15

    Carbofuran adsorption and desorption were investigated in batch and stirred flow chamber (SFC) tests. The carbofuran adsorption capacity of the soils was found to be low and strongly dependent on their clay and organic carbon contents. Carbofuran sorption was due mainly (>80%) to fast adsorption processes governed by intraparticle diffusion. The adsorption kinetic constant for the pesticide ranged from 0.047 to 0.195 min(-1) and was highly correlated with constant n in the Freundlich equation (r=0.965, Pcarbofuran desorption to be highly variable and negatively correlated with eCEC and the clay content. The SFC tests showed that soil organic carbon (C) plays a key role in the irreversibility of carbofuran adsorption. Carbofuran desorption increased rapidly at C contents below 4%. The desorption kinetic constant for the compound (0.086-0.195 min(-1)) was generally higher than its adsorption kinetic constant; therefore, carbofuran is more rapidly desorbed than it is adsorbed in soil.

  13. ACTIVATION ENERGY OF DESORPTION OF DIBENZOFURAN ON ACTIVATED CARBONS

    Institute of Scientific and Technical Information of China (English)

    LI Xiang; LI Zhong; XI Hongxia; LUO Lingai

    2004-01-01

    Three kinds of commercial activated carbons, such as Norit RB1, Monolith and Chemviron activated carbons, were used as adsorbents for adsorption of dibenzofuran. The average pore size and specific surface area of these activated carbons were measured. Temperature Programmed Desorption (TPD) experiments were conducted to measure the TPD curves of dibenzofuran on the activated carbons, and then the activation energy for desorption of dibenzofuran on the activated carbons was estimated. The results showed that the Chemviron and the Norit RB1 activated carbon maintained higher specific surface area and larger micropore pore volume in comparison with the Monolith activated carbon, and the activation energy for the desorption of dibenzofuran on these two activated carbons was higher than that on the Monolith activated carbon. The smaller the pore of the activated carbon was, the higher the activated energy of dibenzofuran desorption was.

  14. Thermogravimetric desorption and de novo tests I: method development and validation.

    Science.gov (United States)

    Tsytsik, Palina; Czech, Jan; Carleer, Robert; Reggers, Guy; Buekens, Alfons

    2008-08-01

    Thermogravimetric analysis (TGA) has been combined with evolved gas analysis (EGA) with the purpose of simulating the thermal behaviour of filter dust samples under inert (desorption) and de novo test oxidising conditions. Emphasis is on studying de novo formation of dioxins, surrogates and precursors arising from filter dust derived from thermal processes, such as municipal solid waste incineration and metallurgy. A new method is tested for sampling and analysing dioxin surrogates and precursors in the TGA effluent, which are collected on sampling tubes; the adsorbed compounds are eventually desorbed and quantified by TD-GC-MS. The major sources of error and losses are considered, including potential sorbent artefacts, possible breakthrough of volatiles through sampling tubes, or eventual losses of semi-volatiles due to their incomplete desorption or re-condensation inside the TG Analyser. The method is optimised and validated for di- to hexa-chlorinated benzenes in a range of 10-1000 ppb with average recovery exceeding 85%. The results are compared with data obtained in similar studies, performed by other research groups. As a result, the method provides the means for simulating de novo synthesis of dioxins in fly-ash and facilitates reliable and easy estimation of de novo activity, comparable with results of other studies, in combination with wide flexibility of testing conditions.

  15. Sorption, Desorption and Diffusion of Tc Under Anaerobic Conditions

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    The sorption and diffusion of Tc on granite under anaerobic conditions were investigated. Influencesof pH values, ferrous minerals(reduced iron powder or magnetite), bentonite, concentration of cations andanion (Fe3+, Fe2+ and CO32-) on the distribution coefficient, Kd, were studied. The sorption mechanism of99Tc on granite was analyzed by the desorption method of adding H2O2 into desorption solvent. Based on

  16. Relation Between pH and Desorption of Cu, Cr, Zn, and Pb from Industrially Polluted Soils

    DEFF Research Database (Denmark)

    Ottosen, Lisbeth M.; Hansen, Henrik K.; Jensen, Pernille Erland

    2009-01-01

    Desorption of Cu, Cr, Pb, and Zn from industrially polluted soils as a result of acidification is in focus. The eight soils of the investigation vary greatly in composition and heavy metal concentration/combination. Three soils had elevated concentrations of Cu, Pb, and Zn; regardless of pollution...... level, pollution origin, and soil type, the order for desorption as pH decreased was Zn > Cu > Pb. Turning to a single heavy metal in different soils, there was a huge difference in the pH at which the major desorption started. The variation was most significant for Pb where, e.g., less than 10......% was desorbed at pH 2.5 from one soil, whereas in another soil 60% Pb was desorbed at this pH. Sequential extraction was made and the soils in which a high percentage of Pb was found in the residual phase (adsorbed strongest) was also the soils where less Pb was desorbed at low pH in the desorption experiments...

  17. STUDY ADSORPTION DESORPTION OF MANGANESE(II USING IMPREGNATED CHITIN-CELLULOSE AS ADSORBENT

    Directory of Open Access Journals (Sweden)

    Aldes Lesbani

    2015-03-01

    Full Text Available Abstract- Study adsorption desorption of manganese(II using impregnated chitin-cellulose as adsorbent has been carried out. Chitin was extracted from snail shell and cellulose isolated from rice straw. Chitin and cellulose were impregnated using thiourea as impregnant agent. Characterization of chitin and cellulose was performed using FTIR spectroscopy, determination of water content, and ash content, while impregnated chitin-cellulose was characterized using FTIR spectrophotometer and X-Ray diffractometer. The adsorption of Mn(II on impregnated chitin-cellulose was studied through determination of adsorption time and the influence of Mn(II concentration, while desorption was carried out sequentially using various reagents. The results shown that chitin and cellulose from extraction processes are has similar FTIR spectrum compared to chitin and cellulose standard. The FTIR spectrum of impregnated chitin-cellulose shows both vibration of chitin and cellulose appeared and indicated successfully impregnate. These results were also equal to XRD pattern analysis. The water and ash contents of chitin are 0.038% and 0.043 while for cellulose are 0.184% and 0.165%, respectively. The adsorption of Mn(II on chitin and cellulose are quite similar kinetically, while adsorption of Mn(II on impregnated chitin-cellulose is higher at the same time with chitin and cellulose. In the low concentration of Mn(II, adsorption phenomena are similar on chitin, cellulose, and impregnated chitin-cellulose. Desorption process of Mn(II on the adsorbents shows sodium etilenediamine tetra acetate able to desorp Mn(II up to 68% higher than other reagents. Keywords: Manganese(II, Chitin, Cellulose, Impregnated Chitin-Cellulose

  18. Sorption and desorption of 1,4-dichlorobenzene on peat

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    Sorption and desorption of 1,4-dichlorobenzene (DCB) on peat (>92% organic matter)display large-scale hysteresis and nonlinearity. The magnitude of desorption hysteresis decreases in the order: untreated Pahokee peat (P)>acid treated peat (FP)>humin (TP). The desorption percentages are lower than 28% of the sorbed 1, 4-DCB after desorbing for 6 days. The sorption and desorption isotherms are well fitted to Freundlich equation, whose parameter 1/n ranges from 0.055 to 0.527. Moreover, the parameter 1/n of the desorption isotherm is significantly lower than that of the sorption isotherm, but the parameter IogK increases on contrary to 1/n. The desorption isotherms are very well fitted to Langmuir equation, whose Qm decreases in the order: TP>FP>P.The apparent partition coefficients (Kp) increase with increasing sorption time or decreasing aqueous equilibrium concentration of DCB. And Kp of P is significantly higher than that of FP or TP.

  19. Calcium lignosulfonate adsorption and desorption on Berea sandstone.

    Science.gov (United States)

    Grigg, Reid B; Bai, Baojun

    2004-11-01

    This paper describes adsorption and desorption studies carried out with calcium lignosulfonate (CLS) on Berea sandstone. Circulation experiments were performed to determine CLS adsorption isotherms and the effects of CLS concentration, temperature, salinity, brine hardness, and injection rate on adsorption density. Flow-through experiments were performed to assess the reversibility of CLS adsorption and the influence of postflush rate, brine concentration, brine hardness, brine pH, and temperature on the desorption process. Results indicate that CLS adsorption isotherms on Berea sandstone follow the Freundlich isotherm law. The results presented in this paper on the effects of CLS adsorption and desorption on Berea sandstone show that: (1) increasing CLS concentration and salinity increases CLS adsorption density; (2) increasing temperature will decrease adsorption density; (3) increasing injection rate of CLS solution will slightly decrease CLS adsorption density; (4) postflush rate and salinity of brine have a large impact on the CLS desorption process; (5) the adsorption and desorption process are not completely reversible; and (5) temperature and pH of the postflush brine have little effect on desorption.

  20. Ultraviolet laser desorption/ionization mass spectrometry of single-core and multi-core polyaromatic hydrocarbons under variable conditions of collisional cooling: insights into the generation of molecular ions, fragments and oligomers.

    Science.gov (United States)

    Gámez, Francisco; Hortal, Ana R; Martínez-Haya, Bruno; Soltwisch, Jens; Dreisewerd, Klaus

    2014-11-01

    The ultraviolet laser desorption/ionization of polyaromatic hydrocarbons (PAHs) has been investigated under different background pressures of an inert gas (up to 1.2 mbar of N2) in the ion source of a hybrid, orthogonal-extracting time-of-flight mass spectrometer (oTOF-MS). The study includes an ensemble of six model PAHs with isolated single polyaromatic cores and four ones with multiple cross-linked aromatic and polyaromatic cores. In combination with a weak ion extraction field, the variation of the buffer gas pressure allowed to control the degree of collisional cooling of the desorbed PAHs and, thus, to modulate their decomposition into fragments. The dominant fragmentation channels observed are related to dehydrogenation of the PAHs, in most cases through the cleavage of even numbers of C-H bonds. Breakage of C-C bonds leading to the fragmentation of rings, side chains and core linkages is also observed, in particular, at low buffer gas pressures. The precise patterns of the combined fragmentation processes vary significantly between the PAHs. The highest abundances of molecular PAH ions and cleanest mass spectra were consistently obtained at the highest buffer gas pressure of 1.2 mbar. The effective quenching of the fragmentation pathways at this elevated pressure improves the sensitivity and data interpretation for analytical applications, although the fragmentation of side chains and of bonds between (poly)aromatic cores is not completely suppressed in all cases. Moreover, these results suggest that the detected fragments are generated through thermal equilibrium processes rather than as a result of rapid photolysis. This assumption is further corroborated by a laser desorption/ionization post-source decay analysis using an axial time-of-flight MS. In line with these findings, covalent oligomers of the PAHs, which are presumably formed by association of two or more dehydrogenated fragments, are detected with higher abundances at the lower buffer gas

  1. Target Plate Material Influence on Fullerene-C60 Laser Desorption/Ionization Efficiency.

    Science.gov (United States)

    Zeegers, Guido P; Günthardt, Barbara F; Zenobi, Renato

    2016-04-01

    Systematic laser desorption/ionization (LDI) experiments of fullerene-C60 on a wide range of target plate materials were conducted to gain insight into the initial ion formation in matrix-assisted laser desorption/ionization (MALDI) mass spectrometry. The positive and negative ion signal intensities of precursor, fragment, and cluster ions were monitored, varying both the laser fluence (0-3.53 Jcm(-2)) and the ion extraction delay time (0-950 ns). The resulting species-specific ion signal intensities are an indication for the ionization mechanisms that contribute to LDI and the time frames in which they operate, providing insight in the (MA)LDI primary ionization. An increasing electrical resistivity of the target plate material increases the fullerene-C60 precursor and fragment anion signal intensity. Inconel 625 and Ti90/Al6/V4, both highly electrically resistive, provide the highest anion signal intensities, exceeding the cation signal intensity by a factor ~1.4 for the latter. We present a mechanism based on transient electrical field strength reduction to explain this trend. Fullerene-C60 cluster anion formation is negligible, which could be due to the high extraction potential. Cluster cations, however, are readily formed, although for high laser fluences, the preferred channel is formation of precursor and fragment cations. Ion signal intensity depends greatly on the choice of substrate material, and careful substrate selection could, therefore, allow for more sensitive (MA)LDI measurements. Graphical Abstract ᅟ.

  2. Target Plate Material Influence on Fullerene-C60 Laser Desorption/Ionization Efficiency

    Science.gov (United States)

    Zeegers, Guido P.; Günthardt, Barbara F.; Zenobi, Renato

    2016-04-01

    Systematic laser desorption/ionization (LDI) experiments of fullerene-C60 on a wide range of target plate materials were conducted to gain insight into the initial ion formation in matrix-assisted laser desorption/ionization (MALDI) mass spectrometry. The positive and negative ion signal intensities of precursor, fragment, and cluster ions were monitored, varying both the laser fluence (0-3.53 Jcm-2) and the ion extraction delay time (0-950 ns). The resulting species-specific ion signal intensities are an indication for the ionization mechanisms that contribute to LDI and the time frames in which they operate, providing insight in the (MA)LDI primary ionization. An increasing electrical resistivity of the target plate material increases the fullerene-C60 precursor and fragment anion signal intensity. Inconel 625 and Ti90/Al6/V4, both highly electrically resistive, provide the highest anion signal intensities, exceeding the cation signal intensity by a factor ~1.4 for the latter. We present a mechanism based on transient electrical field strength reduction to explain this trend. Fullerene-C60 cluster anion formation is negligible, which could be due to the high extraction potential. Cluster cations, however, are readily formed, although for high laser fluences, the preferred channel is formation of precursor and fragment cations. Ion signal intensity depends greatly on the choice of substrate material, and careful substrate selection could, therefore, allow for more sensitive (MA)LDI measurements.

  3. Hard cap espresso extraction-stir bar preconcentration of polychlorinated biphenyls in soil and sediments.

    Science.gov (United States)

    Gallart-Mateu, Daniel; Pastor, Agustín; de la Guardia, Miguel; Armenta, Sergio; Esteve-Turrillas, Francesc A

    2017-02-01

    A Nespresso(©) hard cap espresso machine has been employed for the quantitative extraction of polychlorinated biphenyls (PCBs) from sediments and soils. Sample extraction was performed from five grams of sample in less than 40 s, with 200 mL ethanol 40% (v/v) in water and PCBs were concentrated using stir bar sorptive extraction (SBSE) and determined by thermal desorption-gas chromatography-tandem mass spectrometry (TD-GC-MS-MS). Eleven PCB congeners (28, 52, 77, 80, 81, 101, 118, 138, 153,169, and 180) were determined in soils and sediments with limits of quantification in the 0.03-0.08 ng g(-1) range. Extraction efficiency was established by the analysis of soil samples spiked with the studied PCBs at concentrations from 0.1 to 10.0 ng g(-1), obtaining quantitative recoveries from 81 to 120% and an adequate precision with relative standard deviations lower than 20%. Certified reference materials and natural samples were analyzed by the proposed hard cap espresso extraction and results were compared with those provided by a reference procedure based on pressurized solvent extraction, obtaining statistically comparable results. Therefore, the use of a hard cap espresso machine in tandem with SBSE and TD-GC-MS-MS allowed a simple, sensitive and quantitative determination of PCBs.

  4. Authenticity assessment of beef origin by principal component analysis of matrix-assisted laser desorption/ionization mass spectrometric data.

    Science.gov (United States)

    Zaima, Nobuhiro; Goto-Inoue, Naoko; Hayasaka, Takahiro; Enomoto, Hirofumi; Setou, Mitsutoshi

    2011-06-01

    It has become necessary to assess the authenticity of beef origin because of concerns regarding human health hazards. In this study, we used a metabolomic approach involving matrix-assisted laser desorption/ionization imaging mass spectrometry to assess the authenticity of beef origin. Highly accurate data were obtained for samples of extracted lipids from beef of different origin; the samples were grouped according to their origin. The analysis of extracted lipids in this study ended within 10 min, suggesting this approach can be used as a simple authenticity assessment before a definitive identification by isotope analysis.

  5. Adsorption and desorption dynamics of citric acid anions in soil

    KAUST Repository

    Oburger, E.

    2011-07-26

    The functional role of organic acid anions in soil has been intensively investigated, with special focus on (i) microbial respiration and soil carbon dynamics, (ii) nutrient solubilization or (iii) metal detoxification and reduction of plant metal uptake. Little is known about the interaction dynamics of organic acid anions with the soil matrix and the potential impact of adsorption and desorption processes on the functional significance of these effects. The aim of this study was to characterize experimentally the adsorption and desorption dynamics of organic acid anions in five agricultural soils differing in iron and aluminium oxide contents and using citrate as a model carboxylate. Results showed that both adsorption and desorption processes were fast in all soils, reaching a steady state within approximately 1 hour. However, for a given total soil citrate concentration (ct) the steady state was critically dependent on the starting conditions of the experiment, whether most of the citrate was initially present in solution (cl) or held on the solid phase (cs). Specifically, desorption-led processes resulted in significantly smaller steady-state solution concentrations than adsorption-led processes, indicating that hysteresis occurred. As it is not possible to distinguish between different adsorption and desorption pools in soil experimentally, a new dynamic hysteresis model that relies only on measured soil solution concentrations was developed. The model satisfactorily explained experimental data and was able to predict dynamic adsorption and desorption behaviour. To demonstrate its use, we applied the model to two relevant situations involving exudation and microbial degradation. The study highlighted the complex nature of citrate adsorption and desorption dynamics in soil. We conclude that existing models need to incorporate both temporal and hysteresis components to describe realistically the role and fate of organic acids in soil processes. © 2011 The

  6. The laser desorption/laser ionization mass spectra of some methylated xanthines and the laser desorption of caffeine and theophylline from thin layer chromatography plates

    Science.gov (United States)

    Rogers, Kevin; Milnes, John; Gormally, John

    1993-02-01

    Laser desorption/laser ionization time-of-flight mass spectra of caffeine, theophylline, theobromine and xanthine are reported. These mass spectra are compared with published spectra obtained using electron impact ionization. Mass spectra of caffeine and theophylline obtained by IR laser desorption from thin layer chromatography plates are also described. The laser desorption of materials from thin layer chromatography plates is discussed.

  7. Effects of BaRuO{sub 3} addition on hydrogen desorption in MgH{sub 2}

    Energy Technology Data Exchange (ETDEWEB)

    Baricco, M., E-mail: marcello.baricco@unito.it [Dipartimento di Chimica IFM and NIS, Universita di Torino, Via P. Giuria 9, 10125 Torino (Italy); Rahman, M.W.; Livraghi, S.; Castellero, A. [Dipartimento di Chimica IFM and NIS, Universita di Torino, Via P. Giuria 9, 10125 Torino (Italy); Enzo, S. [Dipartimento di Chimica, Universita di Sassari, Via Vienna, 2, 07100 Sassari (Italy); Giamello, E. [Dipartimento di Chimica IFM and NIS, Universita di Torino, Via P. Giuria 9, 10125 Torino (Italy)

    2012-09-25

    Highlights: Black-Right-Pointing-Pointer Interaction of BaRuO{sub 3} with hydrogen studied. Black-Right-Pointing-Pointer BaRuO{sub 3} is able to release hydrogen after absorption. Black-Right-Pointing-Pointer A distorted rhomohedral phase is formed in BaRuO{sub 3} after hydrogen absorption. Black-Right-Pointing-Pointer A mixture of BaRuO{sub 3} with MgH{sub 2} is able to desorb hydrogen much faster than the parent materials. The interaction of hydrogen with the oxide additive is a crucial aspect for improving the hydrogen desorption rate. - Abstract: Hydrogen storage in MgH{sub 2} is strongly limited by kinetic constraints, so that several additives have been considered in order to improve the rate of hydrogen desorption. The present work is devoted to investigate the effect of BaRuO{sub 3} addition on hydrogen absorption and desorption properties of MgH{sub 2}. BaRuO{sub 3} was prepared by solid-state synthesis of BaO and Ru in oxidizing environment. The interaction of as-prepared BaRuO{sub 3} with hydrogen at room temperature was examined by thermal desorption and X-ray diffraction experiments, showing that BaRuO{sub 3} has the ability to uptake hydrogen in the bulk. The hydrogen interaction is discussed with respect to octahedral ruthenium local environment present in the oxide structure. Addition of 1 mol.% BaRuO{sub 3} to MgH{sub 2} was performed by ball milling. Hydrogen desorption properties were investigated by Sievert and DSC, connected with a H{sub 2} detector. The H{sub 2} desorbed from of the nano-structured materials is lower than the theoretical content in MgH{sub 2}, due to the presence of a non-reactive MgO layer. A remarkable increase of the H{sub 2} desorption kinetics in nano-structured MgH{sub 2} was observed with respect to bare MgH{sub 2}. The activation energy for hydrogen desorption from MgH{sub 2}/BaRuO{sub 3} mixture was estimated by Arrhenius and Kissinger methods and a value around 130 kJ mol{sup -1} and 90 kJ mol{sup -1} was obtained

  8. Effect of organic matter and calcium carbonate on behaviors of cadmium adsorption-desorption on/from purple paddy soils.

    Science.gov (United States)

    Zhao, Xiulan; Jiang, Tao; Du, Bin

    2014-03-01

    Batch experiments and sequential extraction analysis were employed to investigate the effects of soil organic matter and CaCO3 on the adsorption and desorption of cadmium (Cd(2+)) onto and from two purple paddy soils, an acidic purple paddy soil (APPS) and a calcareous purple paddy soil (CPPS). The Cd(2+) adsorption isotherms on both soils could be well-described by the Langmuir and Freundlich equations. CPPS had a higher capacity and a stronger affinity for Cd(2+) adsorption compared with APPS. The adsorption process of Cd(2+) on APPS was dominated by electrostatic attractions, whereas the adsorption mechanism varied depending on the Cd(2+) concentrations in equilibrium solutions on CPPS. At low equilibrium concentrations, the adsorption process was primarily specific adsorption, but nonspecific adsorption dominated at high equilibrium concentrations. Removal of organic matter decreased the amount of Cd(2+) adsorption on both of the soils, slightly affected the Cd(2+) desorption rate and exchangeable Cd (EXC-Cd) in APPS and increased the desorption rate and EXC-Cd in CPPS, suggesting that the effect of organic matter on Cd(2+) adsorption-desorption depends on the soils. CPPS and APPS containing CaCO3 exhibited higher adsorption amounts but lower desorption rates and lower proportions of EXC-Cd than those of their corresponding soils without CaCO3, demonstrating that CaCO3 played an important role in Cd(2+) specific adsorption on soil. The changes in the thermodynamic parameters, including free energy (ΔG(0)), enthalpy (ΔH(0)) and entropy (ΔS(0)), as evaluated by the Van't Hoff equations, indicated that the adsorption was a spontaneous and endothermic process with the primary interaction forces of dipole interactions and hydrogen bonds on APPS, whereas both physical and chemical interactions dominated the adsorption on CPPS.

  9. Quantitative determination of volatile organic compounds (VOC) in milk by multiple dynamic headspace extraction and GC-MS.

    Science.gov (United States)

    Ciccioli, Paolo; Brancaleoni, Enzo; Frattoni, Massimiliano; Fedele, Vincenzo; Claps, Salvatore; Signorelli, Federica

    2004-01-01

    A method for the accurate determination of volatile organic compounds (VOC) in milk samples has been developed and tested. It combines multiple dynamic headspace extraction with GC-MS. Absolute amounts of VOC in the liquid phase are obtained by determining the first order kinetic dependence of the stepwise extraction of the analytes and internal standards from the liquid matrix. Compounds released from milk were collected on a train of traps filled with different solid sorbents to cover all components having a number of carbon atoms ranging from 4 to 15. They were analysed by GC-MS after thermal desorption of VOC from the collecting traps. Quantification of VOC in milk was performed using deuterated compounds as internal standards. The method was used to follow seasonal variations of monoterpenes in goat milk and to detect the impact of air pollution on the quality of milk.

  10. THE EFFECT OF MAGNETITE (Fe3O4CATALYST FROM IRON SANDS ON DESORPTION TEMPERATURE OF MgH2 HYDROGEN STORAGE MATERIAL

    Directory of Open Access Journals (Sweden)

    Maulinda Maulinda

    2016-03-01

    Full Text Available One of the future technologies for a safe hydrogen storage media is  metal hydrides. Currently, Mg-based metal hydride has a safety factor and efficient for vehicle applications. However, the thermodynamic properties of magnesium hydride (MgH2 found a relatively high temperature. High desorption temperatures caused MgH2 high thermodynamic stability resulting desorption enthalpy is also high. In this study, natural mineral (iron ore has been extracted from iron sand into powder of magnetite (Fe3O4 and used as a catalyst in an effort to improve the desorption properties of MgH2. Magnetie has been successfully extracted from iron sand using precipitation method with a purity of 85 % , where the purity of the iron sand before extracted was 81%. Then, MgH2-Fe3O4 was milling using mechanical alloying method with a variety of catalysts and milling time. The observation by XRD showed the material was reduced to nanocrystalline scale. MgH2 phase appears as the main phase. DSC test results showed with the addition of Fe3O4, the desorption temperature can be reduced up to 366oC, compared to pure pure MgH2 reached by 409o C. Furthermore, based on gravimetric test, the hydrogen release occurs at a temperature of 388o C, weight loss  of 0.66 mg during 16 minutes.

  11. Sorption-desorption behavior of polybrominated diphenyl ethers in soils

    Energy Technology Data Exchange (ETDEWEB)

    Olshansky, Yaniv; Polubesova, Tamara [Department of Soil and Water Sciences, Robert H. Smith Faculty of Agriculture, Food and Environment, Hebrew University of Jerusalem, P.O. Box 12, Rehovot 76100 (Israel); Vetter, Walter [Institute of Food Chemistry (170b), University of Hohenheim, Garbenstr. 28, D-70599 Stuttgart (Germany); Chefetz, Benny, E-mail: chefetz@agri.huji.ac.il [Department of Soil and Water Sciences, Robert H. Smith Faculty of Agriculture, Food and Environment, The Hebrew University of Jerusalem, P.O. Box 12, Rehovot 76100 (Israel)

    2011-10-15

    Polybrominated diphenyl ethers (PBDEs) are flame retardants that are commonly found in commercial and household products. These compounds are considered persistent organic pollutants. In this study, we used 4,4'-dibromodiphenyl ether (BDE-15) as a model compound to elucidate the sorption and desorption behavior of PBDEs in soils. The organic carbon-normalized sorption coefficient (K{sub OC}) of BDE-15 was more than three times higher for humin than for bulk soils. However, pronounced desorption hysteresis was obtained mainly for bulk soils. For humin, increasing concentration of sorbed BDE-15 resulted in decreased desorption. Our data illustrate that BDE-15 and probably other PBDEs exhibit high sorption affinity to soils. Moreover, sorption is irreversible and thus PBDEs can potentially accumulate in the topsoil layer. We also suggest that although humin is probably a major sorbent for PBDEs in soils, other humic materials are also responsible for their sequestration. - Highlights: > BDE-15 exhibited pronounced desorption hysteresis. > BDE-15 sowed higher sorption affinity to humin as compared to the bulk soils. > Sequestration of PBDEs depends on soil organic matter constitutes other than humin. - Pronounced desorption hysteresis was observed for BDE-15 in natural soils.

  12. Solid solution barium–strontium chlorides with tunable ammonia desorption properties and superior storage capacity

    Energy Technology Data Exchange (ETDEWEB)

    Bialy, Agata [Amminex Emissions Technology A/S, Gladsaxevej 363, 2860 Soeborg (Denmark); Jensen, Peter B. [Department of Energy Conversion and Storage, Technical University of Denmark, Frederiksborgvej 399, DK-4000 Roskilde (Denmark); Center for Atomic-scale Materials Design, Department of Physics, Technical University of Denmark, Fysikvej 311, DK-2800 Kgs. Lyngby (Denmark); Blanchard, Didier [Department of Energy Conversion and Storage, Technical University of Denmark, Frederiksborgvej 399, DK-4000 Roskilde (Denmark); Vegge, Tejs, E-mail: teve@dtu.dk [Department of Energy Conversion and Storage, Technical University of Denmark, Frederiksborgvej 399, DK-4000 Roskilde (Denmark); Quaade, Ulrich J., E-mail: ujq@amminex.com [Amminex Emissions Technology A/S, Gladsaxevej 363, 2860 Soeborg (Denmark)

    2015-01-15

    Metal halide ammines are very attractive materials for ammonia absorption and storage—applications where the practically accessible or usable gravimetric and volumetric storage densities are of critical importance. Here we present, that by combining advanced computational materials prediction with spray drying and in situ thermogravimetric and structural characterization, we synthesize a range of new, stable barium-strontium chloride solid solutions with superior ammonia storage densities. By tuning the barium/strontium ratio, different crystallographic phases and compositions can be obtained with different ammonia ab- and desorption properties. In particular it is shown, that in the molar range of 35–50% barium and 65–50% strontium, stable materials can be produced with a practically usable ammonia density (both volumetric and gravimetric) that is higher than any of the pure metal halides, and with a practically accessible volumetric ammonia densities in excess of 99% of liquid ammonia. - Graphical abstract: Thermal desorption curves of ammonia from Ba{sub x}Sr{sub (1−x)}Cl{sub 2} mixtures with x equal to 0.125, 0.25 and 0.5 and atomic structure of Sr(NH{sub 3}){sub 8}Cl{sub 2}. - Highlights: • Solid solutions of strontium and barium chloride were synthesized by spray drying. • Adjusting molar ratios led to different crystallographic phases and compositions. • Different molar ratios led to different ammonia ab-/desorption properties. • 35–50 mol% BaCl{sub 2} in SrCl{sub 2} yields higher ammonia density than any other metal halide. • DFT calculations can be used to predict properties of the mixtures.

  13. Laboratory H2O:CO2 ice desorption data: entrapment dependencies and its parameterization with an extended three-phase model

    CERN Document Server

    Fayolle, Edith C; Cuppen, Herma M; Visser, Ruud; Linnartz, Harold; 10.1051/0004-6361/201016121

    2011-01-01

    Ice desorption affects the evolution of the gas-phase chemistry during the protostellar stage, and also determines the chemical composition of comets forming in circumstellar disks. From observations, most volatile species are found in H2O-dominated ices. The aim of this study is first to experimentally determine how entrapment of volatiles in H2O ice depends on ice thickness, mixture ratio and heating rate, and second, to introduce an extended three-phase model (gas, ice surface and ice mantle) to describe ice mixture desorption with a minimum number of free parameters. Thermal H2O:CO2 ice desorption is investigated in temperature programmed desorption experiments of thin (10 - 40 ML) ice mixtures under ultra-high vacuum conditions. Desorption is simultaneously monitored by mass spectrometry and reflection-absorption infrared spectroscopy. The H2O:CO2 experiments are complemented with selected H2O:CO, and H2O:CO2:CO experiments. The results are modeled with rate equations that connect the gas, ice surface an...

  14. Effects of Phosphate Adsorption on Adsorption Desorption and Availability of Cu and Zn Ions in Ultisols and Alfisols

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    Surface charge, secondary adsorption-desorption and form distribution of Cu2+ and Zn2+ in Ultisols and Alfisols having adsorbed phosphate were studied by potentiometric titration, adsorption equilibrium and sequential extraction method, respectively. The soil surface negative charges increased whereas the amount of positive charges decreased with increase of P adsorbed. The soil secondary adsorption capacity for Cu2+and Zn2+ was positively significantly correlated with the amount of P adsorbed by the soils, which could be described by the Langmuir equation. The amounts of Cu2+ and Zn2+ desorption from soils were decreased after P adsorption by the soils and the relationship between them was linear. After the soils adsorbed P,form distribution of Cu2+ and Zn2+ in soils changed remarkably.

  15. Stir bar sorptive extraction coupled to gas chromatography-mass spectrometry for the determination of bisphenols in canned beverages and filling liquids of canned vegetables.

    Science.gov (United States)

    Cacho, J I; Campillo, N; Viñas, P; Hernández-Córdoba, M

    2012-07-20

    This paper describes a method for the simultaneous determination of bisphenol A (BPA), bisphenol F (BPF), bisphenol Z (BPZ) and biphenol (BP), using stir bar sorptive extraction (SBSE) in combination with thermal desorption-gas chromatography-mass spectrometry (TD-GC-MS). Several parameters affecting both extraction and thermal desorption of the SBSE stages were carefully optimized by multivariate designs. SBSE was performed with two derivatization procedures, in situ acetylation and in tube silylation, and the results were compared with those obtained when the analytes were not derivatized. The proposed method, determining the analytes as acyl derivatives, was applied to analyze commercially canned beverages, as well as the filling liquids of canned vegetables, providing detection limits of between 4.7 and 12.5 ng L⁻¹, depending on the compound. The intraday and interday precisions were lower than 6% in terms of relative standard deviation. Recovery studies at two concentration levels, 0.1 and 1 μg L⁻¹, were performed providing recoveries in the 86-122% range. The samples analyzed contained higher concentrations of BPA than of the other analytes.

  16. Femtosecond laser pulse induced desorption: A molecular dynamics simulation

    Energy Technology Data Exchange (ETDEWEB)

    Lončarić, Ivor, E-mail: ivor.loncaric@gmail.com [Centro de Física de Materiales CFM/MPC (CSIC-UPV/EHU), P. Manuel de Lardizabal 5, 20018 San Sebastián (Spain); Alducin, Maite [Centro de Física de Materiales CFM/MPC (CSIC-UPV/EHU), P. Manuel de Lardizabal 5, 20018 San Sebastián (Spain); Donostia International Physics Center DIPC, P. Manuel de Lardizabal 4, 20018 San Sebastián (Spain); Saalfrank, Peter [Institut für Chemie, Universität Potsdam, Karl-Liebknecht-Strasse 24-25, D-14476 Potsdam (Germany); Donostia International Physics Center DIPC, P. Manuel de Lardizabal 4, 20018 San Sebastián (Spain); Juaristi, J. Iñaki [Departamento de Física de Materiales, Facultad de Químicas, Universidad del País Vasco (UPV/EHU), Apartado 1072, 20080 San Sebastián (Spain); Centro de Física de Materiales CFM/MPC (CSIC-UPV/EHU), P. Manuel de Lardizabal 5, 20018 San Sebastián (Spain); Donostia International Physics Center DIPC, P. Manuel de Lardizabal 4, 20018 San Sebastián (Spain)

    2016-09-01

    In recent simulations of femtosecond laser induced desorption of molecular oxygen from the Ag(110) surface, it has been shown that depending on the properties (depth and electronic environment) of the well in which O{sub 2} is adsorbed, the desorption can be either induced dominantly by hot electrons or via excitations of phonons. In this work we explore whether the ratios between the desorption yields from different adsorption wells can be tuned by changing initial surface temperature and laser pulse properties. We show that the initial surface temperature is an important parameter, and that by using low initial surface temperatures the electronically mediated process can be favored. In contrast, laser properties seem to have only a modest influence on the results.

  17. A study of the process of desorption of hexavalent chromium

    Directory of Open Access Journals (Sweden)

    W.B. Amorim

    2003-09-01

    Full Text Available In this work the process of desorption of hexavalent chromium, a toxic metal ion, from the marine algae Sargassum sp, following biosorption experiments 2³ factorial design was studied. A technique was applied to three eluents: HCl, H2SO4 and EDTA. Three factors of importance were evaluated: concentration of eluent, the ratio between mass of biosorbent and volume of eluent (S/L and process time. A statistical analysis of the experimental results showed that the three variables evaluated are significant for all three eluents. The models for chromium desorption were validated, as the results agreed well with the observed values. Through use of the response surface methodology, a factorial design based optimization technique; it was possible to identify the most suitable eluent and the interval of values for the process variables that resulted in the most significant desorption of chromium, which is relevant information for work aiming at process optimization.

  18. Direct scattering, trapping, and desorption in atom-surface collisions.

    Science.gov (United States)

    Fan, Guoqing; Manson, J R

    2008-08-08

    Maxwell is credited as the first to invoke the assumption that an impinging gas beam scatters from a surface with a direct contribution exhibiting little change in state and a trapping-desorption fraction that desorbs in equilibrium [J. C. Maxwell, Phil. Trans. R. Soc. London 170, 231 (1879)]. Here a classical mechanical scattering theory is developed to describe direct scattering, trapping, and subsequent desorption of the incident beam. This theory allows a rigorous test of the Maxwell assumption and determines the conditions under which it is valid. The theory also gives quantitative explanations of important new experimental measurements [K. D. Gibson, N. Isa, and S. J. Sibener, J. Chem. Phys. 119, 13 083 (2003)] for direct and trapping-desorption scattering of Ar atoms by a self-assembled layer of 1-decanethiol on Au(111).

  19. Gas desorption and up-scaling errors in CBM groundwater impact simulations

    Science.gov (United States)

    Herckenrath, D.; Doherty, J.

    2013-12-01

    Coalbed Methane (CBM) is a major energy resource in Australia. Production of CBM requires the extraction of large amounts of groundwater to enable gas desorption from the coalbeds. As CBM raises concerns regarding its impact on adjacent aquifer systems, groundwater models are often required for groundwater impact assessment. Questions arise about the suitability of traditional groundwater flow simulators for CBM groundwater impact quantification as 1) the gas phase is not simulated and 2) up-scaled properties are used that might not reflect coalbed properties appropriately. First, this study aims to quantify the errors incurred by neglecting gas desorption by comparing a CBM reservoir simulator (Eclipse) with an equivalent groundwater flow model (MODFLOW-USG) for a single 1m coal seam. Simulations show the groundwater model significantly overestimates drawdowns during the CBM production stage, as the desorbed gas volume is not accounted for, which impacts storage and the relative permeability of water that are assumed to be constant in the groundwater model. To improve the match between the groundwater model and CBM reservoir simulations, MODFLOW-USG was configured to implement a relationship that was obtained using a pseudo steady-state relationship between drawdown and desaturation derived from Eclipse simulations. A second set of simulations for a sequence of coalbeds was performed to quantify the impact of up-scaling on predicting drawdowns and to validate whether relative permeability curves in the CBM reservoir simulator still have integrity in an up-scaled context. These simulations will help understand how physically representative different up-scaled models are, what errors could be made when regional groundwater modelling is undertaken in a CBM environment and ultimately help decide whether a groundwater flow simulator can be used for CBM groundwater impact assessments. Key words: Coalbed Methane, Up-scaling, Reservoir model, Groundwater model, Dual

  20. Desorption Dynamics, Internal Energies and Imaging of Organic Molecules from Surfaces with Laser Desorption and Vacuum Ultraviolet (VUV) Photoionization

    Energy Technology Data Exchange (ETDEWEB)

    Kostko, Oleg; Takahashi, Lynelle K.; Ahmed, Musahid

    2011-04-05

    There is enormous interest in visualizing the chemical composition of organic material that comprises our world. A convenient method to obtain molecular information with high spatial resolution is imaging mass spectrometry. However, the internal energy deposited within molecules upon transfer to the gas phase from a surface can lead to increased fragmentation and to complications in analysis of mass spectra. Here it is shown that in laser desorption with postionization by tunable vacuum ultraviolet (VUV) radiation, the internal energy gained during laser desorption leads to minimal fragmentation of DNA bases. The internal temperature of laser-desorbed triacontane molecules approaches 670 K, whereas the internal temperature of thymine is 800 K. A synchrotron-based VUV postionization technique for determining translational temperatures reveals that biomolecules have translational temperatures in the range of 216-346 K. The observed low translational temperatures, as well as their decrease with increased desorption laser power is explained by collisional cooling. An example of imaging mass spectrometry on an organic polymer, using laser desorption VUV postionization shows 5 mu m feature details while using a 30 mu m laser spot size and 7 ns duration. Applications of laser desorption postionization to the analysis of cellulose, lignin and humic acids are briefly discussed.

  1. Identification of Scirpus triqueter root exudates and the effects of organic acids on desorption and bioavailability of pyrene and lead in co-contaminated wetland soils.

    Science.gov (United States)

    Hou, Yunyun; Liu, Xiaoyan; Zhang, Xinying; Chen, Xiao; Tao, Kaiyun; Chen, Xueping; Liang, Xia; He, Chiquan

    2015-11-01

    Root exudates (REs) of Scirpus triqueter were extracted from the rhizosphere soil in this study. The components in the REs were identified by GC-MS. Many organic acids, such as hexadecanoic acid, pentadecanoic acid, vanillic acid, octadecanoic acid, citric acid, succinic acid, glutaric acid, and so on, were found. Batch simulated experiments were conducted to evaluate the impacts of different organic acids, such as citric acid, artificial root exudates (ARE), succinic acid, and glutaric acid in REs of S. triqueter on desorption of pyrene (PYR) and lead (Pb) in co-contaminated wetland soils. The desorption amount of PYR and Pb increased with the rise in concentrations of organic acids in the range of 0-50 g·L(-1), within shaking time of 2-24 h. The desorption effects of PYR and Pb in soils with various organic acids treatments decreased in the following order: citric acid > ARE > succinic acid > glutaric acid. The desorption rate of PYR and Pb was higher in co-contaminated soil than in single pollution soil. The impacts of organic acids in REs of S. triqueter on bioavailability of PYR and Pb suggested that organic acids enhanced the bioavailability of PYR and Pb in wetland soil, and the bioavailability effects of organic acids generally followed the same order as that of desorption effects.

  2. Measurements on the gas desorption yield of the oxygen-free copper irradiated with low-energy Xe10+ and O+

    Science.gov (United States)

    Dong, Z. Q.; Li, P.; Yang, J. C.; Yuan, Y. J.; Xie, W. J.; Zheng, W. H.; Liu, X. J.; Chang, J. J.; Luo, C.; Meng, J.; Wang, J. C.; Wang, Y. M.; Yin, Y.; Chai, Z.

    2017-10-01

    Heavy ion beam lost on the accelerator vacuum wall will release quantity of gas molecules and make the vacuum system deteriorate seriously. This phenomenon is called dynamic vacuum effect, observed at CERN, GSI and BNL, leading to the decrease of beam lifetime when increasing beam intensity. Heavy ion-induced gas desorption, which results in dynamic vacuum effect, becomes one of the most important problems for future accelerators proposed to operate with intermediate charge state beams. In order to investigate the mechanism of this effect and find the solution method for the IMP future project High Intensity heavy-ion Accelerator Facility (HIAF), which is designed to extract 1 × 1011 uranium particles with intermediate charge state per cycle, two dedicated experiment setups have been installed at the beam line of the CSR and the 320 kV HV platform respectively. Recently, experiment was performed at the 320 kV HV platform to study effective gas desorption with oxygen-free copper target irradiated with continuous Xe10+ beam and O+ beam in low energy regime. Gas desorption yield in this energy regime was calculated and the link between gas desorption and electronic energy loss in Cu target was proved. These results will be used to support simulations about dynamic vacuum effect and optimizations about efficiency of collimators to be installed in the HIAF main synchrotron BRing, and will also provide guidance for future gas desorption measurements in high energy regime.

  3. Leaf water absorption and desorption functions for three turfgrasses

    Science.gov (United States)

    Liang, Xi; Su, Derong; Yin, Shuxia; Wang, Zhi

    2009-09-01

    SummaryPlant leaf can absorb water when the leaf is in contact with water. This happens when the rainfall is intercepted by plant leaves, where the intercepted part of rain remains on the leaf surface. When the intercepted water is either absorbed or subsequently evaporated into the atmosphere, the plant leaves can dissipate water through the desorption process until the plant is dry or rewatered. In this paper, two symptomatic models in the form of exponential functions for leaf water absorption and leaf water desorption were derived and validated by experimental data using leaves of three turfgrasses (Tall fescue, Perennial ryegrass and Kentucky bluegrass). Both the models and measured data showed that the rate of leaf water absorption was high at the low initial leaf water content and then gradually leveled off toward the saturated leaf water content. The rate of leaf water desorption was high at the high initial leaf water content then decreased drastically over time toward zero. The different plant leaves showed different exponents and other parameters of the functions which indicate the difference of plant species. Both the absorption and desorption rates were relatively higher for the Kentucky bluegrass and lower for the Tall fescue and Perennial ryegrass. The concept of specific leaf area ( SLA) was used to understand the saturated leaf water content ( C s) of the three turfgrasses. Linear relationships were found between C s and SLA. The leaf water absorption and desorption functions are useful for deriving physiological parameters of the plant such as permanent wilting leaf water content, naturally irreducible leaf water content, exponential leaf water absorption coefficient, and exponential leaf desorption coefficient, as well as for evaluating the effects of rainfall interception on plant growth and water use efficiency.

  4. Coverage-dependent adsorption and desorption of oxygen on Pd(100).

    Science.gov (United States)

    den Dunnen, Angela; Jacobse, Leon; Wiegman, Sandra; Berg, Otto T; Juurlink, Ludo B F

    2016-06-28

    We have studied the adsorption and desorption of O2 on Pd(100) by supersonic molecular beam techniques and thermal desorption spectroscopy. Adsorption measurements on the bare surface confirm that O2 initially dissociates for all kinetic energies between 56 and 380 meV and surface temperatures between 100 and 600 K via a direct mechanism. At and below 150 K, continued adsorption leads to a combined O/O2 overlayer. Dissociation of molecularly bound O2 during a subsequent temperature ramp leads to unexpected high atomic oxygen coverages, which are also obtained at high incident energy and high surface temperature. At intermediate temperatures and energies, these high final coverages are not obtained. Our results show that kinetic energy of the gas phase reactant and reaction energy dissipated during O2 dissociation on the cold surface both enable activated nucleation of high-coverage surface structures. We suggest that excitation of local substrate phonons may play a crucial role in oxygen dissociation at any coverage.

  5. Coverage-dependent adsorption and desorption of oxygen on Pd(100)

    Science.gov (United States)

    den Dunnen, Angela; Jacobse, Leon; Wiegman, Sandra; Berg, Otto T.; Juurlink, Ludo B. F.

    2016-06-01

    We have studied the adsorption and desorption of O2 on Pd(100) by supersonic molecular beam techniques and thermal desorption spectroscopy. Adsorption measurements on the bare surface confirm that O2 initially dissociates for all kinetic energies between 56 and 380 meV and surface temperatures between 100 and 600 K via a direct mechanism. At and below 150 K, continued adsorption leads to a combined O/O2 overlayer. Dissociation of molecularly bound O2 during a subsequent temperature ramp leads to unexpected high atomic oxygen coverages, which are also obtained at high incident energy and high surface temperature. At intermediate temperatures and energies, these high final coverages are not obtained. Our results show that kinetic energy of the gas phase reactant and reaction energy dissipated during O2 dissociation on the cold surface both enable activated nucleation of high-coverage surface structures. We suggest that excitation of local substrate phonons may play a crucial role in oxygen dissociation at any coverage.

  6. Determination of Macrolide Antibiotics Using Dispersive Liquid-Liquid Microextraction Followed by Surface-Assisted Laser Desorption/Ionization Mass Spectrometry

    Science.gov (United States)

    Chen, Kuan-Yu; Yang, Thomas C.; Chang, Sarah Y.

    2012-06-01

    A novel method for the determination of macrolide antibiotics using dispersive liquid-liquid microextraction coupled to surface-assisted laser desorption/ionization mass spectrometric detection was developed. Acetone and dichloromethane were used as the disperser solvent and extraction solvent, respectively. A mixture of extraction solvent and disperser solvent were rapidly injected into a 1.0 mL aqueous sample to form a cloudy solution. After the extraction, macrolide antibiotics were detected using surface-assisted laser desorption/ionization mass spectrometry (SALDI/MS) with colloidal silver as the matrix. Under optimum conditions, the limits of detection (LODs) at a signal-to-noise ratio of 3 were 2, 3, 3, and 2 nM for erythromycin (ERY), spiramycin (SPI), tilmicosin (TILM), and tylosin (TYL), respectively. This developed method was successfully applied to the determination of macrolide antibiotics in human urine samples.

  7. Heavy-Ion-Induced Electronic Desorption of Gas from Metals

    CERN Document Server

    Molvik, A W; Mahner, E; Kireeff Covo, M; Bellachioma, M C; Bender, M; Bieniosek, F M; Hedlund, E; Krämer, A; Kwan, J; Malyshev, O B; Prost, L; Seidl, P A; Westenskow, G; Westerberg, L

    2007-01-01

    During heavy-ion operation in several particle accelerators worldwide, dynamic pressure rises of orders of magnitude were triggered by lost beam ions that bombarded the vacuum chamber walls. This ion-induced molecular desorption, observed at CERN, GSI, and BNL, can seriously limit the ion beam lifetime and intensity of the accelerator. From dedicated test stand experiments we have discovered that heavy-ion-induced gas desorption scales with the electronic energy loss (dEe/dx) of the ions slowing down in matter; but it varies only little with the ion impact angle, unlike electronic sputtering.

  8. Desorption of toluene from modified clays using supercritical carbon dioxide

    Directory of Open Access Journals (Sweden)

    Carneiro D. G. P.

    2004-01-01

    Full Text Available The main objective of this work is to study the regeneration capacity of modified clays using supercritical fluid. These modified clays are used as organic compound adsorvents. The experimental step was done using a packed column with the clay contaminated by toluene. The results obtained showed the influence of the density of the supercritical CO2 and of the organic modifier in the desorption process. These data were modeled with first- and second-order models. Better results were obtained using the second-order model. This study makes possible the scale-up of the desorption process for regeneration of solid matrices using supercritical fluids.