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Sample records for thermal ionisation mass

  1. U-series dating using thermal ionisation mass spectrometry (TIMS)

    Energy Technology Data Exchange (ETDEWEB)

    McCulloch, M.T. [Australian National University, Canberra, ACT (Australia). Research School of Earth Science

    1999-11-01

    U-series dating is based on the decay of the two long-lived isotopes{sup 238}U({tau}{sub 1/2}=4.47 x 10{sup 9} years) and {sup 235}U ({tau}{sub 1/2} 0.7 x 10{sup 9} years). {sup 238}U and its intermediate daughter isotopes {sup 234}U ({tau}{sub 1/2} = 245.4 ka) and {sup 230}Th ({tau}{sub 1/2} = 75.4 ka) have been the main focus of recently developed mass spectrometric techniques (Edwards et al., 1987) while the other less frequently used decay chain is based on the decay {sup 235}U to {sup 231}Pa ({tau}{sub 1/2} = 32.8 ka). Both the {sup 238}U and {sup 235}U decay chains terminate at the stable isotopes {sup 206}Pb and {sup 207}Pb respectively. Thermal ionization mass spectrometry (TIMS) has a number of inherent advantages, mainly the ability to measure isotopic ratios at high precision on relatively small samples. In spite of these now obvious advantages, it is only since the mid-1980`s when Chen et al., (1986) made the first precise measurements of {sup 234}U and {sup 232}Th in seawater followed by Edwards et al., (1987) who made combined {sup 234}U-{sup 230}Th measurements, was the full potential of mass spectrometric methods first realised. Several examples are given to illustrate various aspects of TIMS U-series 9 refs., 3 figs.

  2. High throughput volatile fatty acid skin metabolite profiling by thermal desorption secondary electrospray ionisation mass spectrometry.

    Science.gov (United States)

    Martin, Helen J; Reynolds, James C; Riazanskaia, Svetlana; Thomas, C L Paul

    2014-09-07

    The non-invasive nature of volatile organic compound (VOC) sampling from skin makes this a priority in the development of new screening and diagnostic assays. Evaluation of recent literature highlights the tension between the analytical utility of ambient ionisation approaches for skin profiling and the practicality of undertaking larger campaigns (higher statistical power), or undertaking research in remote locations. This study describes how VOC may be sampled from skin and recovered from a polydimethylsilicone sampling coupon and analysed by thermal desorption (TD) interfaced to secondary electrospray ionisation (SESI) time-of-flight mass spectrometry (MS) for the high throughput screening of volatile fatty acids (VFAs) from human skin. Analysis times were reduced by 79% compared to gas chromatography-mass spectrometry methods (GC-MS) and limits of detection in the range 300 to 900 pg cm(-2) for VFA skin concentrations were obtained. Using body odour as a surrogate model for clinical testing 10 Filipino participants, 5 high and 5 low odour, were sampled in Manilla and the samples returned to the UK and screened by TD-SESI-MS and TD-GC-MS for malodour precursors with greater than >95% agreement between the two analytical techniques. Eight additional VFAs were also identified by both techniques with chains 4 to 15 carbons long being observed. TD-SESI-MS appears to have significant potential for the high throughput targeted screening of volatile biomarkers in human skin.

  3. Measurement of small ion beams by thermal ionisation mass spectrometry using new 10(13) Ohm resistors.

    Science.gov (United States)

    Koornneef, J M; Bouman, C; Schwieters, J B; Davies, G R

    2014-03-28

    We tested 5 newly manufactured - prototype - 10(13)Ohm resistors in the feedback loop of Faraday cup amplifiers to measure small ion beams by Thermal Ionisation Mass Spectrometry (TIMS). The high Ohmic resistors installed in the TRITON Plus at the VU University Amsterdam theoretically have 10 times lower noise levels relative to the default 10(11)Ohm resistors. To investigate the precision and accuracy of analyses using these new amplifiers we measured Sr and Nd isotopes of reference standards at a range of ion currents (3.2×10(-16) to 1×10(-12) A, corresponding to intensities of 32 μV to 100 mV on a default 10(11)Ohm amplifier) and on small amounts of material (100 and 10 pg). Internal precision and external reproducibility for Sr and Nd isotope ratios are both better when collected on 10(13) compared 10(12)Ohm resistors and to the default 10(11)Ohm resistors. At an (87)Sr ion current of 3×10(-14) A (3 mV on a 10(11)Ohm amplifier) the internal precision (2 SE) of (87)Sr/(86)Sr is 5 times better for 10(13)Ohm resistors compared to 10(11)Ohm resistors. The external reproducibility (2 SD) at this beam intensity is 9 times better. Multiple 100 and 10 pg Sr standards, ran to exhaustion, yielded low (87)Sr/(86)Sr compared to the long term average (e.g. 10 pg average=0.710083±164 (n=11) instead of 0.710244±12, n=73). The average off-set for 10 pg standards can be explained by a loading blank contribution of 1.3 pg. In contrast, Nd data on 100 pg and 10 pg samples are accurate suggesting that Nd loading blanks do not compromise the data. The external reproducibility of (143)Nd/(144)Nd on 100 pg samples is 125 ppm and 3.3‰ on 10 pg samples (2 RSD=relative standard deviation, n=10). Thus, variability in Nd and Sr isotope ratios in the 4th decimal place, e.g. (143)Nd/(144)Nd 0.5110-0.5119 or (87)Sr/(86)Sr 0.7100-0.7109, can be resolved in 10 to 100 pg samples provided that the procedural blanks and chemical separation are optimal. For measurements in the beam

  4. Simultaneous determination of picogram per gram concentrations of Ba, Pb and Pb isotopes in Greenland ice by thermal ionisation mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Jimi, Salah I.; Rosman, Kevin J.R.; Candelone, Jean-Pierre; Burn, Laurie J. [Curtin University of Technology, Department of Imaging and Applied Physics, Perth (Australia); Hong, Sungmin [Polar Research Centre, Korean Ocean Research and Development Institute, Ansan, P.O. Box 29, Seoul (Korea); Boutron, Claude F. [Domaine Universitaire, Laboratoire de Glaciologie et Geophysique du l' Environnement, 54 rue Moliere, Saint Martin d' Heres (France); UFR de Mecanique, Universite Joseph Fourier de Grenoble (Institut Universitaire de France), Domaine Universitaire, Grenoble (France)

    2008-01-15

    A technique has been developed to simultaneously measure picogram per gram concentrations of Ba and Pb by isotope dilution mass spectrometry, as well as Pb isotopic ratios in polar ice by thermal ionisation mass spectrometry. BaPO{sup +}{sub 2} and Pb{sup +} ions were employed for these determinations. A calibrated mixture of enriched {sup 205}Pb and {sup 137}Ba was added to the samples providing an accuracy of better than approximately 2% for Pb/Ba element ratio determinations. Interference by molecular ions in the Pb mass spectrum occurred only at {sup 204}Pb and {sup 205}Pb, but these contributions were negligible in terms of precisions expected on picogram-sized Pb samples. The technique is illustrated with measurements on Greenland firn, using a drill-core section that includes the Laki volcanic eruption of 1783-1784. The data show deviations from the element concentrations indicating volatile metal enrichments, but the Pb isotopic signature of the Laki lava could not be identified. (orig.)

  5. 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

  6. {sup 226}Ra measurement by thermal ionisation mass spectrometry: Use of {sup 226}Ra and {sup 14}C for groundwater dating

    Energy Technology Data Exchange (ETDEWEB)

    Dever, L. [Universite Paris-SUD, Orsay, (France). Lab d`Hydrologie et Geochemie Isotopique; Hillaire-Marcel, C. [Geotop, Universite du Quebec a Montreal, Montreal (Canada)

    1997-10-01

    Recent developments in thermal ionisation mass spectrometry (TIMS) and in chemical separation Ra and Ba allow to analyse {sup 226}Ra on smaller water samples (<200 ml) than with conventional counting techniques (10{sup 3} litres). The sampling has been realised on the Chalk aquifer of the Paris basin. The water samples have been collected in the unsaturated zone using in situ filtering devices and in the unconfined and confined parts of the aquifer in the boreholes used for public water supply. {sup 226}Ra contents vary from 0.064{+-}0.02 dpm/kg (n=6) in the unsaturated zone to 0.119{+-}0.069 dpm/kg (n=7) in the unconfined aquifer and 0.319{+-}0.057 dpm/kg (n=9) in the confined aquifer. For all the samples the {sup 226}Ra/{sup 238}U activity ratios are much lower than the secular equilibrium. This points out that the two isotopes have different input function in the water during the mineralisation of the solution. The good correlation (r{sup 2}=0.9) between the {sup 226}Ra and Sr indicates that dissolution of Chalk is the dominant mechanism of mineralisation in {sup 226}Ra of the solution. In the Chalk the mineralisation of the water occurs in the first metres of the unsaturated zone, during the water percolation the water rock interaction takes place through dissolution and precipitation of calcite in a non steady state. According to his distribution coefficient Sr is then a better tracer of dissolution/precipitation process than Ba. Using a geochemical model based on {sup 226}Ra/Sr and Sr/Ca ratios an `age` of the water could be determined. With {sup 226}Ra half life of 1620 years we obtain `ages` varying from 150 years to 1950 years in the unconfined aquifer. For the confined part of the aquifer where the redox condition is different it is necessary to use a geochemical model based on the U concentration in the water, the {sup 226}Ra gives in such case ages varying from 1.8ka to 12.8ka. The radiocarbon ages obtained through usual chemical and/or isotopic models

  7. Isotope Dilution - Thermal Ionisation Mass Spectrometric Analysis for Tin in a Fly Ash Material; Analisis de Estano en una Ceniza de Combustion mediante Espectrometria de Masas de Ionizacion Termica con Dilucion Isotopica

    Energy Technology Data Exchange (ETDEWEB)

    Hernandez, C.; Fernandez, M.; Quejido, A. L.

    2006-07-01

    Isotope dilution-thermal ionisation mass spectrometry (ID-TIMS) analysis has been applied to the determination of tin in a fly ash sample supplied by the EC Joint Research Centre (Ispra, Italy). The proposed procedure includes the silica gel/phosphoric acid technique for tin thermal ionisation activation and a strict heating protocol for isotope ratio measurements. Instrumental mass discrimination factor has been previously determined measuring a natural tin standard solution. Spike solutions has been prepared from 112Sn-enriched metal and quantified by reverse isotope dilution analysis. Two sample aliquots were spiked and tin was extracted with 4,5 M HCI during 25 min ultrasound exposure time. Due to the complex matrix of this fly ash material, a two-step purification stage using ion-exchange chromatography was required prior TIMS analysis. Obtained results for the two sample-spike blends (10,10 + - 0,55 y 10,50 + - 0,64 imolg-1) are comprarable, both value and uncertainty. Also a good reproducibility is observed between measurements. The proposed ID-TIMS procedure, as a primary method and due to the lack of fly ash reference material certified for tin content, can be used to validate more routine methodologies applied to tin determination in this kind of materials. (Author) 75 refs.

  8. Electrospray Ionisation Mass Spectrometry: Principles and Clinical Applications

    Science.gov (United States)

    Ho, CS; Lam, CWK; Chan, MHM; Cheung, RCK; Law, LK; Lit, LCW; Ng, KF; Suen, MWM; Tai, HL

    2003-01-01

    This mini-review provides a general understanding of electrospray ionisation mass spectrometry (ESI-MS) which has become an increasingly important technique in the clinical laboratory for structural study or quantitative measurement of metabolites in a complex biological sample. The first part of the review explains the electrospray ionisation process, design of mass spectrometers with separation capability, characteristics of the mass spectrum, and practical considerations in quantitative analysis. The second part then focuses on some clinical applications. The capability of ESI-tandem-MS in measuring bio-molecules sharing similar molecular structures makes it particularly useful in screening for inborn errors of amino acid, fatty acid, purine, pyrimidine metabolism and diagnosis of galactosaemia and peroxisomal disorders. Electrospray ionisation is also efficient in generating cluster ions for structural elucidation of macromolecules. This has fostered a new and improved approach (vs electrophoresis) for identification and quantification of haemoglobin variants. With the understanding of glycohaemoglobin structure, an IFCC reference method for glycohaemoglobin assay has been established using ESI-MS. It represents a significant advancement for the standardisation of HbA1c in diabetic monitoring. With its other applications such as in therapeutic drug monitoring, ESI-MS will continue to exert an important influence in the future development and organisation of the clinical laboratory service. PMID:18568044

  9. Ambient ionisation mass spectrometry for the characterisation of polymers and polymer additives: a review.

    Science.gov (United States)

    Paine, Martin R L; Barker, Philip J; Blanksby, Stephen J

    2014-01-15

    The purpose of this review is to showcase the present capabilities of ambient sampling and ionisation technologies for the analysis of polymers and polymer additives by mass spectrometry (MS) while simultaneously highlighting their advantages and limitations in a critical fashion. To qualify as an ambient ionisation technique, the method must be able to probe the surface of solid or liquid samples while operating in an open environment, allowing a variety of sample sizes, shapes, and substrate materials to be analysed. The main sections of this review will be guided by the underlying principle governing the desorption/extraction step of the analysis; liquid extraction, laser ablation, or thermal desorption, and the major component investigated, either the polymer itself or exogenous compounds (additives and contaminants) present within or on the polymer substrate. The review will conclude by summarising some of the challenges these technologies still face and possible directions that would further enhance the utility of ambient ionisation mass spectrometry as a tool for polymer analysis. Copyright © 2013 Elsevier B.V. All rights reserved.

  10. Characterisation of bacteria by matrix-assisted laser desorption/ionisation and electrospray mass spectrometry

    NARCIS (Netherlands)

    Baar, B.L.M. van

    2000-01-01

    Chemical analysis for the characterisation of micro-organisms is rapidly evolving, after the recent advent of new ionisation methods in mass spectrometry (MS): electrospray (ES) and matrix-assisted laser desorption/ionisation (MALDI). These methods allow quick characterisation of micro-organisms,

  11. Photo-ionisation mass spectrometry as detection method for gas chromatography. Optical selectivity and multidimensional comprehensive separations.

    Science.gov (United States)

    Zimmermann, Ralf; Welthagen, Werner; Gröger, Thomas

    2008-03-14

    Mass spectrometry (MS) with soft ionisation techniques (i.e. ionisation without fragmentation of the analyte molecules) for gaseous samples exhibits interesting analytical properties for direct analysis applications (i.e. direct inlet mass spectrometric on-line monitoring) as well as mass spectrometric detection method for gas chromatography (GC-MS). Commonly either chemical ionisation (CI) or field ionisation (FI) is applied as soft ionisation technology for GC-MS. An interesting alternative to the CI and FI technologies methods are photo-ionisation (PI) methods. PI overcomes some of the limitations of CI and FI and furthermore add some unique analytical properties. The resonance enhanced multi-photon ionisation (REMPI) method uses intense UV-laser pulses (wavelength range approximately 350-193 nm) for highly selective, sensitive and soft ionisation of predominately aromatic compounds. The single photon ionisation (SPI) method utilises VUV light (from lamps or laser sources, wavelengths range approximately 150-110 nm) can be used for a universal soft ionisation of organic molecules. In this article the historical development as well as the current status and concepts of gas chromatography hyphenated to photo-ionisation mass spectrometry are reviewed.

  12. Bioaerosol detection by aerosol TOF-mass spectrometry: Application of matrix assisted laser desorption/ionisation

    NARCIS (Netherlands)

    Wuijckhuijse, A.L. van; Stowers, M.A.; Kientz, Ch.E.; Marijnissen, J.C.M.; Scarlett, B.

    2000-01-01

    In previous publications the use of an aerosol time of flight mass spectrometer was reported for the on-line measurements of aerosols (Weiss 1997, Kievit 1995). The apparatus is capable of measuring the size as well as the chemical composition, by the use of Laser Desorption/Ionisation (LDI), of an

  13. Use of matrix-assisted laser desorption/ionisation mass spectrometry in cancer research.

    Science.gov (United States)

    Bateson, Hannah; Saleem, Saira; Loadman, Paul M; Sutton, Chris W

    2011-01-01

    Cancer significantly affects millions of people worldwide. It is possible to use proteomic techniques to aid in detection, monitoring of treatment and progression, as well as gaining an increased understanding of cancer. Matrix-assisted laser desorption/ionisation (MALDI) mass spectrometry can be utilised to detect the presence of proteins and peptides within various samples from the body, including blood, biological fluids and tumour tissue. This review aims to introduce MALDI mass spectrometry and discuss a range of applications in the field of cancer research, from quantitative to qualitative methods. Also described is MALDI imaging mass spectrometry which differs from typical sample preparation methods, as analytes are ionised directly from the tissue. Finally, presented is a brief summary of the status of biomarker discovery using blood/serum and biological fluids samples, and the implications in the clinic. Copyright © 2011 Elsevier Inc. All rights reserved.

  14. Development of lithium attachment mass spectrometry - knudsen effusion and chemical ionisation mass spectrometry (KEMS, CIMS).

    Science.gov (United States)

    Booth, A Murray; Bannan, Thomas J; Benyezzar, Med; Bacak, Asan; Alfarra, M Rami; Topping, David; Percival, Carl J

    2017-10-07

    Lithium ion attachment mass spectrometry provides a non-specific, non-fragmenting, sensitive and robust method for the detection of volatile species in the gas phase. The design, manufacture and results of lithium based ion attachment ionisation sources for two different mass spectrometry systems are presented. In this study trace gas analysis is investigated using a modified Chemical Ionization Mass Spectrometer (CIMS) and vapour pressure measurements are made using a modified Knudsen Effusion Mass Spectrometer (KEMS). In the Li+ CIMS, where the Li+ ionization acts a soft and unselective ionization source, limits of detection of 0.2 ppt for formic acid, 15 ppt for nitric acid and 120 ppt for ammonia were achieved, allowing for ambient measurements of such species at atmospherically relevant concentrations. In the first application of Lithium ion attachment in ultra-high vacuum (UHV), vapor pressures of various atmospherically relevant species were measured with the adapted KEMS, giving measured values equivalent to previous results from electron impact KEMS. In the Li+ KEMS vapour pressures <10-3 mbar can be measured without any fragmentation, as is seen with the initial electron impact (EI) set up, allowing the vapor pressure of individual components within mixtures to be determined.

  15. Comparison of quantification methods for the analysis of polychlorinated alkanes using electron capture negative ionisation mass spectrometry

    NARCIS (Netherlands)

    Rusina, T.; Korytar, P.; Boer, de J.

    2011-01-01

    Four quantification methods for short-chain chlorinated paraffins (SCCPs) or polychlorinated alkanes (PCAs) using gas chromatography electron capture negative ionisation low resolution mass spectrometry (GC-ECNI-LRMS) were investigated. The method based on visual comparison of congener group

  16. Matrix-assisted laser desorption/ionisation mass spectrometry of transfer ribonucleic acids isolated from yeast.

    Science.gov (United States)

    Gruic-Sovulj, I; Lüdemann, H C; Hillenkamp, F; Weygand-Durasevic, I; Kucan, Z; Peter-Katalinic, J

    1997-01-01

    tRNATyr and tRNASer purified from bulk brewer's yeast tRNA were subjected to analysis by matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry. Choosing a mixture of 2,4,6- and 2,3,4-trihydroxy-acetophenone and diammonium citrate as matrix a mass resolution of up to 220 (FWHM) was achieved in the linear mode of operation. Cation adduct suppression by addition of cation exchange beads and a chelating agent (CDTA) is shown to substantially improve mass resolution for this class of molecules. PMID:9108172

  17. Matrix-free mass spectrometric imaging using laser desorption ionisation Fourier transform ion cyclotron resonance mass spectrometry

    Science.gov (United States)

    Goodwin, Richard J A; Pitt, Andrew R; Harrison, David; Weidt, Stefan K; Langridge-Smith, Pat R R; Barrett, Michael P; Logan Mackay, C

    2011-01-01

    Mass spectrometry imaging (MSI) is a powerful tool in metabolomics and proteomics for the spatial localization and identification of pharmaceuticals, metabolites, lipids, peptides and proteins in biological tissues. However, sample preparation remains a crucial variable in obtaining the most accurate distributions. Common washing steps used to remove salts, and solvent-based matrix application, allow analyte spreading to occur. Solvent-free matrix applications can reduce this risk, but increase the possibility of ionisation bias due to matrix adhesion to tissue sections. We report here the use of matrix-free MSI using laser desorption ionisation performed on a 12 T Fourier transform ion cyclotron resonance (FTICR) mass spectrometer. We used unprocessed tissue with no post-processing following thaw-mounting on matrix-assisted laser desorption ionisation (MALDI) indium-tin oxide (ITO) target plates. The identification and distribution of a range of phospholipids in mouse brain and kidney sections are presented and compared with previously published MALDI time-of-flight (TOF) MSI distributions. Copyright © 2011 John Wiley & Sons, Ltd. PMID:21416534

  18. Chemical profile of mango (Mangifera indica L.) using electrospray ionisation mass spectrometry (ESI-MS).

    Science.gov (United States)

    Oliveira, Bruno G; Costa, Helber B; Ventura, José A; Kondratyuk, Tamara P; Barroso, Maria E S; Correia, Radigya M; Pimentel, Elisângela F; Pinto, Fernanda E; Endringer, Denise C; Romão, Wanderson

    2016-08-01

    Mangifera indica L., mango fruit, is consumed as a dietary supplement with purported health benefits; it is widely used in the food industry. Herein, the chemical profile of the Ubá mango at four distinct maturation stages was evaluated during the process of growth and maturity using negative-ion mode electrospray ionisation Fourier transform ion cyclotron resonance mass spectrometry (ESI(-)FT-ICR MS) and physicochemical characterisation analysis (total titratable acidity (TA), total soluble solids (TSS), TSS/TA ratio, and total polyphenolic content). Primary (organic acids and sugars) and secondary metabolites (polyphenolic compounds) were mostly identified in the third maturation stage, thus indicating the best stage for harvesting and consuming the fruit. In addition, the potential cancer chemoprevention of the secondary metabolites (phenolic extracts obtained from mango samples) was evaluated using the induction of quinone reductase activity, concluding that fruit polyphenols have the potential for cancer chemoprevention. Copyright © 2016 Elsevier Ltd. All rights reserved.

  19. Ionisation in turbulent magnetic molecular clouds. I. Effect on density and mass-to-flux ratio structures

    Science.gov (United States)

    Bailey, Nicole D.; Basu, Shantanu; Caselli, Paola

    2017-05-01

    Context. Previous studies show that the physical structures and kinematics of a region depend significantly on the ionisation fraction. These studies have only considered these effects in non-ideal magnetohydrodynamic simulations with microturbulence. The next logical step is to explore the effects of turbulence on ionised magnetic molecular clouds and then compare model predictions with observations to assess the importance of turbulence in the dynamical evolution of molecular clouds. Aims: In this paper, we extend our previous studies of the effect of ionisation fractions on star formation to clouds that include both non-ideal magnetohydrodynamics and turbulence. We aim to quantify the importance of a treatment of the ionisation fraction in turbulent magnetised media and investigate the effect of the turbulence on shaping the clouds and filaments before star formation sets in. In particular, here we investigate how the structure, mass and width of filamentary structures depend on the amount of turbulence in ionised media and the initial mass-to-flux ratio. Methods: To determine the effects of turbulence and mass-to-flux ratio on the evolution of non-ideal magnetised clouds with varying ionisation profiles, we have run two sets of simulations. The first set assumes different initial turbulent Mach values for a fixed initial mass-to-flux ratio. The second set assumes different initial mass-to-flux ratio values for a fixed initial turbulent Mach number. Both sets explore the effect of using one of two ionisation profiles: step-like (SL) or cosmic ray only (CR-only). We compare the resulting density and mass-to-flux ratio structures both qualitatively and quantitatively via filament and core masses and filament fitting techniques (Gaussian and Plummer profiles). Results: We find that even with almost no turbulence, filamentary structure still exists although at lower density contours. Comparison of simulations shows that for turbulent Mach numbers above 2, there is

  20. High-resolution mass spectrometric analysis of myo-inositol hexakisphosphate using electrospray ionisation Orbitrap.

    Science.gov (United States)

    McIntyre, Catherine A; Arthur, Christopher J; Evershed, Richard P

    2017-10-30

    The phosphorus storage compound in grains, phytic acid, or myo-inositol hexakisphosphate (IP6), is important for nutrition and human health, and is reportedly the most abundant organic phosphorus compound in soils. Methods for its determination have traditionally relied on complexation with iron and precipitation, acid digestion and measurement of phosphate concentration, or 31 P NMR spectroscopy. Direct determination of phytic acid (and its homologues) using mass spectrometry has, as yet, found limited application to environmental or other complex matrices. The behaviour of phytic acid in electrospray ionisation high-resolution mass spectrometry (ESI-HRMS) and its fragmentation, both in-source and via collision-induced dissociation, have not been studied so far. The negative ion mass spectrometry and tandem mass spectrometry (MS/MS) of IP6, and the lower inositol pentakisphosphate (IP5), using an ESI-Orbitrap mass spectrometer is described. The purity of the compounds was investigated using anion-exchange chromatography. IP6 is highly anionic, forming multiply charged ions and sodium adduct ions, which readily undergo dissociation in the ESI source. MS/MS analysis of the phytic acid [M-2H]2- ion and fragment ions and comparison with the full MS of the IP5 reference standard, and the MS/MS spectrum of the pentakisphosphate [M-2H]2- ion, confirm the fragmentation pattern of inositol phosphates in ESI. Further evidence for dissociation in the ion source is shown by the effect of increasing the source voltage on the mass spectrum of phytic acid. The ESI-HRMS of inositol phosphates is unusual and highly characteristic. The study of the full mass spectrum of IP6 in ESI-HRMS mode indicates the detection of the compound in environmental matrices using this technique is preferable to the use of multiple reaction monitoring (MRM). © 2017 The Authors. Rapid Communications in Mass Spectrometry Published by John Wiley & Sons Ltd.

  1. High‐resolution mass spectrometric analysis of myo‐inositol hexakisphosphate using electrospray ionisation Orbitrap

    Science.gov (United States)

    McIntyre, Catherine A.; Arthur, Christopher J.

    2017-01-01

    Rationale The phosphorus storage compound in grains, phytic acid, or myo‐inositol hexakisphosphate (IP6), is important for nutrition and human health, and is reportedly the most abundant organic phosphorus compound in soils. Methods for its determination have traditionally relied on complexation with iron and precipitation, acid digestion and measurement of phosphate concentration, or 31P NMR spectroscopy. Direct determination of phytic acid (and its homologues) using mass spectrometry has, as yet, found limited application to environmental or other complex matrices. The behaviour of phytic acid in electrospray ionisation high‐resolution mass spectrometry (ESI‐HRMS) and its fragmentation, both in‐source and via collision‐induced dissociation, have not been studied so far. Methods The negative ion mass spectrometry and tandem mass spectrometry (MS/MS) of IP6, and the lower inositol pentakisphosphate (IP5), using an ESI‐Orbitrap mass spectrometer is described. The purity of the compounds was investigated using anion‐exchange chromatography. Results IP6 is highly anionic, forming multiply charged ions and sodium adduct ions, which readily undergo dissociation in the ESI source. MS/MS analysis of the phytic acid [M−2H]2− ion and fragment ions and comparison with the full MS of the IP5 reference standard, and the MS/MS spectrum of the pentakisphosphate [M−2H]2− ion, confirm the fragmentation pattern of inositol phosphates in ESI. Further evidence for dissociation in the ion source is shown by the effect of increasing the source voltage on the mass spectrum of phytic acid. Conclusions The ESI‐HRMS of inositol phosphates is unusual and highly characteristic. The study of the full mass spectrum of IP6 in ESI‐HRMS mode indicates the detection of the compound in environmental matrices using this technique is preferable to the use of multiple reaction monitoring (MRM). PMID:28696018

  2. Eddy covariance flux measurements of ammonia by high temperature chemical ionisation mass spectrometry

    Directory of Open Access Journals (Sweden)

    J. Sintermann

    2011-03-01

    Full Text Available A system for fast ammonia (NH3 measurements with chemical ionisation mass spectrometry (CIMS based on a commercial Proton Transfer Reaction-Mass Spectrometer (PTR-MS is presented. It uses electron transfer reaction as ionisation pathway and features a drift tube of polyetheretherketone (PEEK and silica-coated steel. Heating the instrumental inlet and the drift tube to 180 °C enabled an effective time resolution of ~1 s and made it possible to apply the instrument for eddy covariance (EC measurements. EC fluxes of NH3 were measured over two agricultural fields in Oensingen, Switzerland, following fertilisations with cattle slurry. Air was aspirated close to a sonic anemometer at a flow of 100 STP L min−1 and was directed through a 23 m long 1/2" PFA tube heated to 150 °C to an air-conditioned trailer where the gas was sub-sampled from the large bypass stream. This setup minimised damping of fast NH3 concentration changes between the sampling point and the actual measurement. High-frequency attenuation loss of the NH3 fluxes of 20 to 40% was quantified and corrected for using an empirical ogive method. The instrumental NH3 background signal showed a minor interference with H2O which was characterised in the laboratory. The resulting correction of the NH3 flux after slurry spreading was less than 1‰. The flux detection limit of the EC system was about 5 ng m−2 s−1 while the accuracy of individual flux measurements was estimated 16% for the high-flux regime during these experiments. The NH3 emissions after broad spreading of the slurry showed an initial maximum of 150 μg m−2 s−1 with a fast decline in the following hours.

  3. Liquid chromatography-mass spectrometry for C60 fullerene analysis: optimisation and comparison of three ionisation techniques.

    Science.gov (United States)

    Li, Ling; Huhtala, Sami; Sillanpää, Markus; Sainio, Pirjo

    2012-06-01

    The increasing use and production of nanomaterials have led to growing concern over the release of new pollutants to the environment. Fullerenes have been a subject of intense research, both because of their unique chemistry and because of technological applications. The development of analytical methods to quantify the fullerenes in complex sample matrices is a crucial step in the study of their occurrence and exposure, and thus in risk assessment. This paper reports the development and optimisation of a method combining liquid chromatography with ion-trap mass spectrometry (LC-ITMS) for analysis of the fullerene C(60). Under the optimised chromatogram conditions, a C(18) analytical column had good selectivity for fullerenes C(60) and C(70), with retention times of 3.0 and 4.1 min, respectively. Mass spectrometric detection was tested and optimised using three common ionisation techniques-atmospheric-pressure chemical ionisation (APCI), atmospheric-pressure photoionisation (APPI), and electrospray ionisation (ESI). The molecular ion was most abundant for C (60) (-) (m/z=720) in APCI and APPI, whereas adduct ions were formed with the molecular ion in ESI. Finally, the performance of the three ionisation techniques examined was compared by use of five validation criteria. The instrument detection limit (8 ng mL(-1)), quantification limit (27 ng mL(-1)), detection sensitivity (90.2 ng mL(-1)), linear range (8-1,000 ng mL(-1)), and repeatability (15 %) of APPI make it the most promising ionisation technique for fullerene C(60) analysis.

  4. CF3+ and CF2H+: new reagents for n-alkane determination in chemical ionisation reaction mass spectrometry.

    Science.gov (United States)

    Blake, Robert S; Ouheda, Saleh A; Evans, Corey J; Monks, Paul S

    2016-11-28

    Alkanes provide a particular analytical challenge to commonly used chemical ionisation methods such as proton-transfer from water owing to their basicity. It is demonstrated that the fluorocarbon ions CF3+ and CF2H+, generated from CF4, as reagents provide an effective means of detecting light n-alkanes in the range C2-C6 using direct chemical ionisation mass spectrometry. The present work assesses the applicability of the reagents in Chemical Ionisation Mass Spectrometric (CI-TOF-MS) environments with factors such as high moisture content, operating pressures of 1-10 Torr, accelerating electric fields (E/N) and long-lived intermediate complex formation. Of the commonly used chemical ionisation reagents, H3O+ and NO+ only react with hexane and higher while O2+ reacts with all the target samples, but creates significant fragmentation. By contrast, CF3+ and CF2H+ acting together were found to produce little or no fragmentation. In dry conditions with E/N = 100 Td or higher the relative intensity of CF2H+ to CF3+ was mostly less than 1% but always less than 3%, making CF3+ the main reagent ion. Using O2+ in a parallel series of experiments, a substantially greater degree of fragmentation was observed. The detection sensitivities of the alkanes with CF3+ and CF2H+, while relatively low, were found to be better than those observed with O2+. Experiments using alkane mixtures in the ppm range have shown the ionisation technique based on CF3+ and CF2H+ to be particularly useful for measurements of alkane/air mixtures found in polluted environments. As a demonstration of the technique's effectiveness in complex mixtures, the detection of n-alkanes in a smoker's breath is demonstrated.

  5. Hyphenation of atmospheric pressure chemical ionisation mass spectrometry to supercritical fluid chromatography for polar car lubricant additives analysis.

    Science.gov (United States)

    Lavison-Bompard, Gwenaelle; Thiébaut, Didier; Beziau, Jean-François; Carrazé, Bernadette; Valette, Pascale; Duteurtre, Xavier; Tabet, Jean-Claude

    2009-01-30

    Car lubricant additives are added to mineral or synthetic base stocks to improve viscosity and resistance to oxidation of the lubricant and to limit wear of engines. As they belong to various chemical classes and are added to a very complex medium, the base stock, their detailed chromatographic analysis is very difficult and time consuming. In a previous paper, it was demonstrated that supercritical fluid chromatography (SFC) allows the elution of common low-molecular-weight additives. Since their total resolution could not be achieved owing to the limited peak capacity of packed columns, the hyphenation of selective and informative detection methods such as atomic emission detection (AED) was required. Further to results obtained in SFC-AED, this work describes the hyphenation of SFC to atmospheric pressure chemical ionisation ion trap mass spectrometry (MS). SFC-MS hyphenation is detailed: temperature, flow rates of gas and mobile phase introduced in the source, position of the restrictor, ionisation additives and conditions of autotune are studied. Car lubricant monitoring requires negative and positive ionisation modes with or without the addition of ionisation auxiliary solvent according to the nature of additives. Moreover, when sensitivity is of major concern for a selected additive, the autotuning routine of the MS has to be performed in conditions as close as possible to analytical conditions, i.e. under subcritical conditions. Unambiguous identification and structure elucidation of several additives in formulated car lubricants are also presented.

  6. Quick elucidation of cyclodepsipeptide sequence from sacoglossan Elysia grandifolia using electrospray ionisation-tandem mass spectrometry.

    Science.gov (United States)

    Tilvi, Supriya; Devi, Prabha; Majik, Mahesh S

    2017-06-01

    Butanol fraction of sacoglossan Elysia grandifolia was investigated for identifying peptides using electrospray ionisation-tandem mass spectrometry (ESI-MS/MS). Without prior isolation, the structural determination is achieved on the basis of mass fragmentation pattern and comparison with the previously established data. The ESI-MS of the fraction in the positive ion mode gave clusters of singly and doubly charged molecular ion peaks. The ESI-MS spectrum showed peaks for the presence of the peptides kahalalides F, G, R and S reported earlier. In addition, it also showed molecular ion peaks at m/z 1557.8 [M+H]+ and doubly charged ions at m/z 779.4 [M+2H]2+, 790.4 [M+Na]2+ and 796.4 [M+K]2+. The MS/MS at m/z 779.4 [M+2H]+2 at collision energy 40 V obtained series of b and y fragment ions. The MS/MS spectrum showed identical fragment ion y6 at m/z 643 which revealed that cyclic part is identical with kahalalide F, R and S. Careful examination of the fragment ions b1 to b7 with their corresponding y fragment ions y12 to y6, respectively and by comparison of MS/MS pattern of kahalalide S, established that proline can be replaced by tyrosine amino acid residue. The mass difference between b4 ( m/z 511) and b5 ( m/z 674) is equal to 163 which is equivalent to mass residue of tyrosine. Their y fragment ions also quickly helped in fixing the puzzle. This resulted in the identification of the peptide sequence cyclo-[Val-(5-MeHex-Val-Thr-Val-Val-Tyr-Lys-Ile)Thr-Ile-Val-Phe-Dhb)] for the new cyclodepsipeptide, kahalalide Z3. Thus, ESI-MS/MS has set a trend in quick identification of new marine molecules.

  7. Characterisation of tryptic peptides of phosphorylated tyrosine hydroxylase by high-pressure liquid chromatography electrospray ionisation mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Graham, Mark E. [Molecular Structure and Detection Group, School of Environmental and Life Sciences, University of Newcastle, Callaghan, NSW 2308 (Australia); Dickson, Phillip W. [School of Biomedical Science, University of Newcastle, Callaghan, NSW 2308 (Australia); Dunkley, Peter R. [School of Biomedical Science, University of Newcastle, Callaghan, NSW 2308 (Australia); Nagy-Felsobuki, Ellak I. von [Molecular Structure and Detection Group, School of Environmental and Life Sciences, University of Newcastle, Callaghan, NSW 2308 (Australia)]. E-mail: ellak@newcastle.edu.au

    2005-03-01

    Tyrosine hydroxylase (TH) is involved in the biosynthesis of catecholamines and is activated by phosphorylation. Phosphorylated TH was analysed using high-pressure liquid chromatography combined with electrospray mass spectrometry (HPLC ESI-MS). Two mass scanning methods were used to detect tryptic cleavage products of TH. In the positive electrospray ionisation mode (ESI+), the peptides that contain the phosphorylation sites of TH were identified. In the alternative method, a phosphopeptide was detected in the negative electrospray ionisation mode (ESI-) using single ion monitoring in combination with a sequential ESI+ switching experiment. A raised baseline interfered with detection of hydrophilic peptides in ESI-, with the signal-to-noise ratio indicating that the method was operating near the limit of detection for a conventional electrospray source. The switching method improved the certainty of identification of phosphopeptides.

  8. Artificially-aged cachaça samples characterised by direct infusion electrospray ionisation mass spectrometry.

    Science.gov (United States)

    de Souza, Patterson P; Resende, Ana M M; Augusti, Daniella V; Badotti, Fernanda; Gomes, Fátima de Cássia O; Catharino, Rodrigo R; Eberlin, Marcos N; Augusti, Rodinei

    2014-01-15

    Direct infusion electrospray ionisation mass spectrometry in the negative ion mode [ESI(-)-MS] was employed to evaluate the authenticity of aged cachaças, a traditional and valuable Brazilian alcoholic beverage prepared from the distillation of brewed sugarcane juice and aged in barrels made of common woods. Counterfeit samples were prepared by adding dyes, sawdust or essences to a freshly-distiled, much less valuable sample (white cachaça) to simulate the 1-2years long natural ageing in wooden barrels. A simple visual inspection revealed remarkable differences between the ESI(-)-MS of the authentic samples (aged in oak or amburana casks) and the artificially-aged counterfeit samples. A set of diagnostic ions were detectable in the ESI(-)-MS of the authentic samples aged in oak (m/z 197, 241, 301 and 307) and amburana (m/z 271 and 377/379). This fast and direct methodology seems useful as a routine procedure to monitor this highly profitable and common counterfeit practice. Copyright © 2013 Elsevier Ltd. All rights reserved.

  9. A real time metabolomic profiling approach to detecting fish fraud using rapid evaporative ionisation mass spectrometry.

    Science.gov (United States)

    Black, Connor; Chevallier, Olivier P; Haughey, Simon A; Balog, Julia; Stead, Sara; Pringle, Steven D; Riina, Maria V; Martucci, Francesca; Acutis, Pier L; Morris, Mike; Nikolopoulos, Dimitrios S; Takats, Zoltan; Elliott, Christopher T

    2017-01-01

    Fish fraud detection is mainly carried out using a genomic profiling approach requiring long and complex sample preparations and assay running times. Rapid evaporative ionisation mass spectrometry (REIMS) can circumvent these issues without sacrificing a loss in the quality of results. To demonstrate that REIMS can be used as a fast profiling technique capable of achieving accurate species identification without the need for any sample preparation. Additionally, we wanted to demonstrate that other aspects of fish fraud other than speciation are detectable using REIMS. 478 samples of five different white fish species were subjected to REIMS analysis using an electrosurgical knife. Each sample was cut 8-12 times with each one lasting 3-5 s and chemometric models were generated based on the mass range m/z 600-950 of each sample. The identification of 99 validation samples provided a 98.99% correct classification in which species identification was obtained near-instantaneously (≈ 2 s) unlike any other form of food fraud analysis. Significant time comparisons between REIMS and polymerase chain reaction (PCR) were observed when analysing 6 mislabelled samples demonstrating how REIMS can be used as a complimentary technique to detect fish fraud. Additionally, we have demonstrated that the catch method of fish products is capable of detection using REIMS, a concept never previously reported. REIMS has been proven to be an innovative technique to help aid the detection of fish fraud and has the potential to be utilised by fisheries to conduct their own quality control (QC) checks for fast accurate results.

  10. Metabolite signal identification in accurate mass metabolomics data with MZedDB, an interactive m/z annotation tool utilising predicted ionisation behaviour 'rules'.

    Science.gov (United States)

    Draper, John; Enot, David P; Parker, David; Beckmann, Manfred; Snowdon, Stuart; Lin, Wanchang; Zubair, Hassan

    2009-07-21

    Metabolomics experiments using Mass Spectrometry (MS) technology measure the mass to charge ratio (m/z) and intensity of ionised molecules in crude extracts of complex biological samples to generate high dimensional metabolite 'fingerprint' or metabolite 'profile' data. High resolution MS instruments perform routinely with a mass accuracy of ionised. In reality the annotation process is confounded by the fact that many ionisation products will be not only molecular isotopes but also salt/solvent adducts and neutral loss fragments of original metabolites. This report describes an annotation strategy that will allow searching based on all potential ionisation products predicted to form during electrospray ionisation (ESI). Metabolite 'structures' harvested from publicly accessible databases were converted into a common format to generate a comprehensive archive in MZedDB. 'Rules' were derived from chemical information that allowed MZedDB to generate a list of adducts and neutral loss fragments putatively able to form for each structure and calculate, on the fly, the exact molecular weight of every potential ionisation product to provide targets for annotation searches based on accurate mass. We demonstrate that data matrices representing populations of ionisation products generated from different biological matrices contain a large proportion (sometimes > 50%) of molecular isotopes, salt adducts and neutral loss fragments. Correlation analysis of ESI-MS data features confirmed the predicted relationships of m/z signals. An integrated isotope enumerator in MZedDB allowed verification of exact isotopic pattern distributions to corroborate experimental data. We conclude that although ultra-high accurate mass instruments provide major insight into the chemical diversity of biological extracts, the facile annotation of a large proportion of signals is not possible by simple, automated query of current databases using computed molecular formulae. Parameterising MZedDB to

  11. Spectrometre de masse a ionisation Penning selective: Elimination des corrections necessaires a la determination du rapport isotopique de l'hydrogene

    Science.gov (United States)

    Letarte, Sylvain

    Dans le but d'ameliorer la precision avec laquelle le rapport isotopique de l'hydrogene peut etre determine, un spectrometre de masse a ionisation Penning a ete construit pour provoquer l'ionisation selective de l'hydrogene moleculaire et de l'hydrure de deuterium a partir d'un melange gazeux. L'utilisation d'atomes dans des etats d'excitation metastable s'est averee une solution adequate pour reponde a cette attente. L'emploi de l'helium, a l'interieur d'une source d'atomes metastables construit specifiquement pour ce travail, ne permet pas d'obtenir un spectre de masse compose uniquement des deux molecules d'interet. L'ionisation de ces dernieres provient de deux processus distincts, soient l'ionisation Penning et l'ionisation par bombardement electronique. Contrairement a l'helium, il a ete demontre que le neon metastable est un candidat ideal pour produire l'ionisation selective de type Penning. Le nombre d'ions produits est directement proportionnel au courant de la decharge electrique et de la pression d'operation de la source d'atomes metastables. Ces resultats demontrent le potentiel d'un tel spectrometre de masse pour ameliorer la precision a laquelle le rapport isotopique peut etre determine comparativement aux autres techniques existantes.

  12. LA SPECTROSCOPIE DE MASSE PAR IONISATION CHIMIQUE AVEC LA DIETHYLAMINE COMME GAZ REACTANT DES IRIDOIDES GLUCOSIDIQUES DE TYPE C-9

    Directory of Open Access Journals (Sweden)

    H SAADI

    2000-12-01

    Full Text Available Ce travail s’intéresse à l’étude de la spectrométrie de masse par ionisation chimique de quelques composés des iridoïdes glucosidiques de type C-9 extraits des plantes de l’espèce Euplantago en utilisant la diéthylamine comme gaz réactant. Nous avons appliqué la même technique que précédemment à deux d’entre eux se trouvant en abondance dans ce type de plantes, après leur acétylation.

  13. Rapid Evaporative Ionisation Mass Spectrometry (REIMS) Provides Accurate Direct from Culture Species Identification within the Genus Candida.

    Science.gov (United States)

    Cameron, Simon J S; Bolt, Frances; Perdones-Montero, Alvaro; Rickards, Tony; Hardiman, Kate; Abdolrasouli, Alireza; Burke, Adam; Bodai, Zsolt; Karancsi, Tamas; Simon, Daniel; Schaffer, Richard; Rebec, Monica; Balog, Julia; Takáts, Zoltan

    2016-11-14

    Members of the genus Candida, such as C. albicans and C. parapsilosis, are important human pathogens. Other members of this genus, previously believed to carry minimal disease risk, are increasingly recognised as important human pathogens, particularly because of variations in susceptibilities to widely used anti-fungal agents. Thus, rapid and accurate identification of clinical Candida isolates is fundamental in ensuring timely and effective treatments are delivered. Rapid Evaporative Ionisation Mass Spectrometry (REIMS) has previously been shown to provide a high-throughput platform for the rapid and accurate identification of bacterial and fungal isolates. In comparison to commercially available matrix assisted laser desorption ionisation time of flight mass spectrometry (MALDI-ToF), REIMS based methods require no preparative steps nor time-consuming cell extractions. Here, we report on the ability of REIMS-based analysis to rapidly and accurately identify 153 clinical Candida isolates to species level. Both handheld bipolar REIMS and high-throughput REIMS platforms showed high levels of species classification accuracy, with 96% and 100% of isolates classified correctly to species level respectively. In addition, significantly different (FDR corrected P value < 0.05) lipids within the 600 to 1000 m/z mass range were identified, which could act as species-specific biomarkers in complex microbial communities.

  14. Characterisation of nicotine and related compounds using electrospray ionisation with ion trap mass spectrometry and with quadrupole time-of-flight mass spectrometry and their detection by liquid chromatography/electrospray ionisation mass spectrometry.

    Science.gov (United States)

    Smyth, Thomas J; Ramachandran, V N; McGuigan, Alex; Hopps, Jason; Smyth, W Franklin

    2007-01-01

    Electrospray ionisation ion trap mass spectrometry (ESI-MS(n)) has been used to study the fragmentation patterns of nicotine and nine of its related compounds. From this study certain characteristic fragmentations are apparent with generally the pyrrolidine or piperidine ring being subject to chemical modifications. The structures of the product ions proposed for the ESI-MS(n) study have been supported by results from electrospray ionisation quadrupole time-of-flight mass spectrometry (ESI-QTOF-MS). Compounds with pyrrolidine and piperidine rings that possess an unsubstituted N atom have been shown to lose NH(3) at the MS(2) stage. Those compounds with N-methyl groups lose CH(3)NH(2) at the MS(2) stage. The loss of NH(3) or CH(3)NH(2) leaves the corresponding rings opened and this is followed by ring closure at the pyridine-2 carbon atom. Mono-N-oxides fragment in a similar way but the di-N-oxide can also fragment by cleavage of the bond between the pyridine and pyrrolidine rings. Cotinine also can undergo cleavage of this bond between the rings. This data therefore provides useful information on how substituents and the nature of the non-pyridine ring can affect the fragmentation patterns of nicotine and its related compounds. This information can be used in the characterisation of these compounds by liquid chromatography/electrospray ionization mass spectrometry (LC/ESI-MS) which results in the separation of nicotine and its related compounds with limits of detection (LODs) ranging from 15 to 105 ng/mL. The use of LC/ESI-MS to study nicotine-containing samples resulted in the simultaneous and unambiguous identification of seven of the compounds discussed in this paper: cotinine identified at retention time 12.5 min (with its [M+H](+) ion at m/z 177), nornicotine 16.0 min (m/z 149), anatabine 18.0 min (m/z 161), myosmine 18.5 min (m/z 147), anabasine 20.4 min (m/z 163), nicotine 22.2 min (m/z 163), and nicotyrine 31.4 min (m/z 159). For quality control of nicotine

  15. Using aromatic polyamines with high proton affinity as "proton sponge" dopants for electrospray ionisation mass spectrometry.

    Science.gov (United States)

    Wirth, Marisa A; Rüger, Christopher P; Sklorz, Martin; Zimmermann, Ralf

    2017-04-01

    Proton sponges are polyamines with high proton affinity that enable gentle deprotonation of even mildly acidic compounds. In this study, the concept of proton sponges as signal enhancing dopants for electrospray ionisation is presented for the first time. 1,8-Bis(dimethylamino)naphthalene (DMAN) and 1,8-bis(tetramethylguanidino)naphthalene (TMGN) were chosen as dopants, using methanol and acetonitrile/methanol as solvents. Individual standard compounds, compound mixtures and a diesel fuel as a complex sample matrix were investigated. Both proton sponges enhanced signal intensities in electrospray ionisation negative mode, but TMGN decomposed rapidly in methanolic solution. Significantly higher signals were only achieved using the acetonitrile/methanol mixture. On average a more than 10-fold higher signal intensity was measured with 10-3 mol l-1 DMAN concentration. A stronger signal increase of alcohol functionalities was observed compared to acid functionalities. All compound classes which were detected in the diesel fuel (CH- and CHOx-class) received roughly 100-fold higher signal intensities when using DMAN as a dopant. Furthermore, the number of detected compounds as well as the double bond equivalent of the detected compounds increased. The compound class distribution shifted when adding DMAN and the formerly dominant CHO2-, CHO3-, and CHO4- classes received similar relative intensities as formerly less accessible classes. The findings depict DMAN as a promising additive for electrospray ionisation negative analysis of at least mildly acidic compounds, even within complex sample material.

  16. (S)-(-)-N-(pentafluorobenzylcarbamoyl)prolyl chloride: a chiral derivatisation reagent designed for gas chromatography/negative ion chemical ionisation mass spectrometry of amino compounds.

    Science.gov (United States)

    Leis, Hans J; Windischhofer, Werner

    2012-03-30

    The synthesis of a novel chiral derivatisation reagent, (S)-(-)-N-(pentafluorobenzylcarbamoyl)prolyl chloride is described which is preferably useful for negative-ion chemical ionisation mass spectrometry. Preparation of the reagent followed a general strategy used to prepare enantioselective reagents based on the N-substitution of L-proline. Pentafluorobenzyl chloroformate smoothly reacted with L-proline to give the desired derivatisation reagent after conversion into the acyl chloride. The product was sufficiently pure to be used in the following steps without any additional purification. The reagent was tested against selected chiral and non-chiral analytical targets. Chromatographic enantioseparation was at least equal to the commonly used (S)-(-)-N-(heptafluorobutyryl)prolyl derivatives. The derivatives exhibit excellent mass spectral properties under negative ion chemical ionisation, i.e. reduced fragmentation and thus high ion current for the targeted m/z during analysis. With electron ionisation, the fragmentation that occurs is mainly directed by the introduced group. Enantioseparation with gas chromatography/negative-ion chemical ionisation mass spectrometry of the derivatives was demonstrated for the enantiomers of amphetamine, α-aminocaprylic acid methyl ester and threo-methylphenidate. The new derivatisation reagent shows highly improved mass spectral properties for negative-ion chemical ionisation mass spectrometry and is thus suitable for sensitive chiral detection of amino compounds. The reagent extends the applicability of dissociative resonance electron capture using pentafluorobenzyl derivatives to chiral analysis. Copyright © 2012 John Wiley & Sons, Ltd.

  17. STRAPS v1.0: evaluating a methodology for predicting electron impact ionisation mass spectra for the aerosol mass spectrometer

    Science.gov (United States)

    Topping, David O.; Allan, James; Rami Alfarra, M.; Aumont, Bernard

    2017-06-01

    Our ability to model the chemical and thermodynamic processes that lead to secondary organic aerosol (SOA) formation is thought to be hampered by the complexity of the system. While there are fundamental models now available that can simulate the tens of thousands of reactions thought to take place, validation against experiments is highly challenging. Techniques capable of identifying individual molecules such as chromatography are generally only capable of quantifying a subset of the material present, making it unsuitable for a carbon budget analysis. Integrative analytical methods such as the Aerosol Mass Spectrometer (AMS) are capable of quantifying all mass, but because of their inability to isolate individual molecules, comparisons have been limited to simple data products such as total organic mass and the O : C ratio. More detailed comparisons could be made if more of the mass spectral information could be used, but because a discrete inversion of AMS data is not possible, this activity requires a system of predicting mass spectra based on molecular composition. In this proof-of-concept study, the ability to train supervised methods to predict electron impact ionisation (EI) mass spectra for the AMS is evaluated. Supervised Training Regression for the Arbitrary Prediction of Spectra (STRAPS) is not built from first principles. A methodology is constructed whereby the presence of specific mass-to-charge ratio (m/z) channels is fitted as a function of molecular structure before the relative peak height for each channel is similarly fitted using a range of regression methods. The widely used AMS mass spectral database is used as a basis for this, using unit mass resolution spectra of laboratory standards. Key to the fitting process is choice of structural information, or molecular fingerprint. Our approach relies on using supervised methods to automatically optimise the relationship between spectral characteristics and these molecular fingerprints. Therefore

  18. STRAPS v1.0: evaluating a methodology for predicting electron impact ionisation mass spectra for the aerosol mass spectrometer

    Directory of Open Access Journals (Sweden)

    D. O. Topping

    2017-06-01

    Full Text Available Our ability to model the chemical and thermodynamic processes that lead to secondary organic aerosol (SOA formation is thought to be hampered by the complexity of the system. While there are fundamental models now available that can simulate the tens of thousands of reactions thought to take place, validation against experiments is highly challenging. Techniques capable of identifying individual molecules such as chromatography are generally only capable of quantifying a subset of the material present, making it unsuitable for a carbon budget analysis. Integrative analytical methods such as the Aerosol Mass Spectrometer (AMS are capable of quantifying all mass, but because of their inability to isolate individual molecules, comparisons have been limited to simple data products such as total organic mass and the O : C ratio. More detailed comparisons could be made if more of the mass spectral information could be used, but because a discrete inversion of AMS data is not possible, this activity requires a system of predicting mass spectra based on molecular composition. In this proof-of-concept study, the ability to train supervised methods to predict electron impact ionisation (EI mass spectra for the AMS is evaluated. Supervised Training Regression for the Arbitrary Prediction of Spectra (STRAPS is not built from first principles. A methodology is constructed whereby the presence of specific mass-to-charge ratio (m∕z channels is fitted as a function of molecular structure before the relative peak height for each channel is similarly fitted using a range of regression methods. The widely used AMS mass spectral database is used as a basis for this, using unit mass resolution spectra of laboratory standards. Key to the fitting process is choice of structural information, or molecular fingerprint. Our approach relies on using supervised methods to automatically optimise the relationship between spectral characteristics and these molecular

  19. Matrix-assisted laser desorption/ionisation mass spectrometry imaging and its development for plant protein imaging

    Science.gov (United States)

    2011-01-01

    Matrix-Assisted Laser Desorption/Ionisation (MALDI) mass spectrometry imaging (MSI) uses the power of high mass resolution time of flight (ToF) mass spectrometry coupled to the raster of lasers shots across the cut surface of tissues to provide new insights into the spatial distribution of biomolecules within biological tissues. The history of this technique in animals and plants is considered and the potential for analysis of proteins by this technique in plants is discussed. Protein biomarker identification from MALDI-MSI is a challenge and a number of different approaches to address this bottleneck are discussed. The technical considerations needed for MALDI-MSI are reviewed and these are presented alongside examples from our own work and a protocol for MALDI-MSI of proteins in plant samples. PMID:21726462

  20. Surface analysis using a new plasma assisted desorption/ionisation source for mass spectrometry in ambient air

    Science.gov (United States)

    Bowfield, A.; Barrett, D. A.; Alexander, M. R.; Ortori, C. A.; Rutten, F. M.; Salter, T. L.; Gilmore, I. S.; Bradley, J. W.

    2012-06-01

    The authors report on a modified micro-plasma assisted desorption/ionisation (PADI) device which creates plasma through the breakdown of ambient air rather than utilising an independent noble gas flow. This new micro-PADI device is used as an ion source for ambient mass spectrometry to analyse species released from the surfaces of polytetrafluoroethylene, and generic ibuprofen and paracetamol tablets through remote activation of the surface by the plasma. The mass spectra from these surfaces compare favourably to those produced by a PADI device constructed using an earlier design and confirm that the new ion source is an effective device which can be used to achieve ambient mass spectrometry with improved spatial resolution.

  1. Solvent separating secondary metabolites directly from biosynthetic tissue for surface-assisted laser desorption ionisation mass spectrometry.

    Science.gov (United States)

    Rudd, David; Benkendorff, Kirsten; Voelcker, Nicolas H

    2015-03-16

    Marine bioactive metabolites are often heterogeneously expressed in tissues both spatially and over time. Therefore, traditional solvent extraction methods benefit from an understanding of the in situ sites of biosynthesis and storage to deal with heterogeneity and maximize yield. Recently, surface-assisted mass spectrometry (MS) methods namely nanostructure-assisted laser desorption ionisation (NALDI) and desorption ionisation on porous silicon (DIOS) surfaces have been developed to enable the direct detection of low molecular weight metabolites. Since direct tissue NALDI-MS or DIOS-MS produce complex spectra due to the wide variety of other metabolites and fragments present in the low mass range, we report here the use of "on surface" solvent separation directly from mollusc tissue onto nanostructured surfaces for MS analysis, as a mechanism for simplifying data annotation and detecting possible artefacts from compound delocalization during the preparative steps. Water, ethanol, chloroform and hexane selectively extracted a range of choline esters, brominated indoles and lipids from Dicathais orbita hypobranchial tissue imprints. These compounds could be quantified on the nanostructured surfaces by comparison to standard curves generated from the pure compounds. Surface-assisted MS could have broad utility for detecting a broad range of secondary metabolites in complex marine tissue samples.

  2. The use of dicationic ion-pairing compounds to enhance the ambient detection of surface lipids in positive ionization mode using desorption electrospray ionisation mass spectrometry.

    Science.gov (United States)

    Rao, Wei; Mitchell, Daniel; Licence, Peter; Barrett, David A

    2014-03-30

    Lipids are typically analysed in negative ionisation mode in desorption electrospray ionisation mass spectrometry (DESI-MS), which can result in reduced sensitivity. In this study we examine the use of dicationic compounds as reactive DESI-MS agents to detect a range of lipid standards from the surface in positive ionisation mode. Nine dicationic compounds were tested for their ability to detect seven representative lipid species (palmitoleic acid, linoleic acid, phosphatidic acid (34:1), phosphoethanolamine (34:2), phosphatidylglycerol (34:1), phosphatidylserine (36:1), and phosphoinositol (34:2)) with a 2D DESI source on hydrophobic surfaces. Two different solvent systems (methanol/chloroform (1:1) and methanol) were tested with each dicationic compound, with the DESI-MS analysis performed in the positive ionisation mode. Most of the dications tested were able to form stable ion-pairs with the negatively charged lipid species when analysed from the surface with DESI-MS, and were detected readily in positive ionisation electrospray mode as singly charged species. The optimal solvent system was found to be methanol. The dicationic compound [C6(C1Pyrr)2][Br]2 was found to enhance the detection of palmitoleic acid (638%), linoleic acid (304%) and phosphoethanolamine (269%) compared with the negative ionisation mode. We demonstrate the first successful application of dicationic compounds in DESI-MS for the ambient surface detection of model lipids in positive electrospray ionisation mode. Dicationic compounds could potentially be used as reactive DESI-MS agents to improve the ambient detection of a number of negatively charged analytes. © 2014 The Authors. Rapid Communications in Mass Spectrometry published by John Wiley & Sons, Ltd.

  3. Ambient ionisation mass spectrometry for lipid profiling and structural analysis of mammalian oocytes, preimplantation embryos and stem cells.

    Science.gov (United States)

    Ferreira, Christina R; Jarmusch, Alan K; Pirro, Valentina; Alfaro, Clint M; González-Serrano, Andres F; Niemann, Heiner; Wheeler, Matthew B; Rabel, Rathnaweera A C; Hallett, Judy E; Houser, Rebecca; Kaufman, Annemarie; Cooks, R Graham

    2015-05-01

    Lipids play fundamental roles in mammalian embryo preimplantation development and cell fate. Triacylglycerol accumulates in oocytes and blastomeres as lipid droplets, phospholipids influence membrane functional properties, and essential fatty acid metabolism is important for maintaining the stemness of cells cultured in vitro. The growing impact that lipids have in the field of developmental biology makes analytical approaches to analyse structural information of great interest. This paper describes the concept and presents the results of lipid profiling by mass spectrometry (MS) of oocytes and preimplantation embryos, with special focus on ambient ionisation. Based on our previous experience with oocytes and embryos, we aim to convey that ambient MS is also valuable for stem cell differentiation analysis. Ambient ionisation MS allows the detection of a wide range of lipid classes (e.g. free fatty acids, cholesterol esters, phospholipids) in single oocytes, embryos and cell pellets, which are informative of in vitro culture impact, developmental and differentiation stages. Background on MS principles, the importance of underused MS scan modes for structural analysis of lipids, and statistical approaches used for data analysis are covered. We envisage that MS alone or in combination with other techniques will have a profound impact on the understanding of lipid metabolism, particularly in early embryo development and cell differentiation research.

  4. Determination of potato glycoalkaloids using high-pressure liquid chromatography-electrospray ionisation/mass spectrometry.

    Science.gov (United States)

    Matsuda, Fumio; Morino, Keiko; Miyazawa, Haruna; Miyashita, Masahiro; Miyagawa, Hisashi

    2004-01-01

    A method for quantifying two toxic glycoalkaloids, alpha-solanine and alpha-chaconine, in potato (Solanum tuberosum) tuber tissue was developed using HPLC-electrospray ionisation (ESI)/MS. Potato samples were extracted with 5% aqueous acetic acid, and the extracts were subjected directly to HPLC-ESI/MS after filtration. By determining the intensities of the protonated molecules of alpha-solanine (m/z 868) and alpha-chaconine (m/z 852) using selected ion monitoring (positive ion mode), a sensitive assay was attained with detection limits of 38 and 14 ppb for the two glycoalkaloids, respectively. The high sensitivity and selectivity of MS detection effectively reduced the time of analysis thus enabling a high throughput assay of glycoalkaloids in potato tubers.

  5. Determination of food emulsifiers in commercial additives and food products by liquid chromatography/atmospheric-pressure chemical ionisation mass spectrometry.

    Science.gov (United States)

    Suman, M; Silva, G; Catellani, D; Bersellini, U; Caffarra, V; Careri, M

    2009-05-01

    A new, reliable liquid chromatography/atmospheric-pressure chemical ionisation mass spectrometry (LC-APCI-MS) method was developed for the quantitative determination of food emulsifiers composed of mono- and diacylglycerols of fatty acids (E471 series) in complex food matrices. These additives are extremely interesting for the food industry because of their useful properties. Indeed, they improve the manufacture of products by acting as foams and creams stabilisers, crumb-softeners, or antistaling agents. The proposed method also allows us to qualitatively characterise new food emulsifiers composed of other acid esters of mono- and diacylglycerols (E472 series). The validation of the method was performed on blank minicake spiked samples for detection limits (reaching ppm levels), linearity, recovery, precision, and accuracy. The method was then successfully applied to commercial additives containing mixtures of emulsifiers, as well as to food products such as margarines and minicakes.

  6. Identification of barley and rye varieties using matrix- assisted laser desorption/ionisation time-of-flight mass spectrometry with neural networks

    DEFF Research Database (Denmark)

    Bloch, H.A.; Petersen, Marianne Kjerstine; Sperotto, Maria Maddalena

    2001-01-01

    developed, which combines analysis of alcohol-soluble wheat proteins (gliadins) using matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry with neural networks. Here we have applied the same method for the identification of both barley (Hordeum vulgare L.) and rye (Secale cereale L...

  7. Laser post-ionisation combined with a high resolving power orbitrap mass spectrometer for enhanced MALDI-MS imaging of lipids.

    Science.gov (United States)

    Ellis, S R; Soltwisch, J; Paine, M R L; Dreisewerd, K; Heeren, R M A

    2017-06-29

    Coupling laser post-ionisation with a high resolving power MALDI Orbitrap mass spectrometer has realised an up to ∼100-fold increase in the sensitivity and enhanced the chemical coverage for MALDI-MS imaging of lipids relative to conventional MALDI. This could constitute a major breakthrough for biomedical research.

  8. The Spatial Distribution of Alkaloids in Psychotria prunifolia (Kunth) Steyerm and Palicourea coriacea (Cham.) K. Schum Leaves Analysed by Desorption Electrospray Ionisation Mass Spectrometry Imaging

    DEFF Research Database (Denmark)

    Kato, Lucilia; Moraes, Aline Pereira; de Oliveira, Cecília Maria Alves

    2018-01-01

    INTRODUCTION: Species of the genera Psychotria and Palicourea are sources of indole alkaloids, however, the distribution of alkaloids within the plants is not known. Analysing the spatial distribution using desorption electrospray ionisation mass spectrometry imaging (DESI-MSI) has become attract...

  9. Ion suppression in the determination of clenbuterol in urine by solid-phase extraction atmospheric pressure chemical ionisation ion-trap mass spectrometry

    NARCIS (Netherlands)

    van Hout, M.W.J.; Niederlander, H.A G; de Zeeuw, R.A.; de Jong, G.J.

    2003-01-01

    Ion suppression effects were observed during the determination of clenbuterol in urine with solid-phase extraction/multiple-stage ion-trap mass spectrometry (SPE/MS3), despite the use of atmospheric pressure chemical ionisation. During SPE, a polymeric stationary phase (polydivinylbenzene) was

  10. Characterisation of chemical components for identifying historical Chinese textile dyes by ultra high performance liquid chromatography – photodiode array – electrospray ionisation mass spectrometer

    NARCIS (Netherlands)

    Han, J.; Wanrooij, J.; van Bommel, M.; Quye, A.

    2017-01-01

    This research makes the first attempt to apply Ultra High Performance Liquid Chromatography (UHPLC) coupled to both Photodiode Array detection (PDA) and Electrospray Ionisation Mass Spectrometer (ESI–MS) to the chemical characterisation of common textile dyes in ancient China. Three different

  11. Can laser-ionisation time-of-flight mass spectrometry be a promising alternative to laser ablation/inductively-coupled plasma mass spectrometry and glow discharge mass spectrometry for the elemental analysis of solids?

    NARCIS (Netherlands)

    Sysoev, AA; Sysoev, AA

    2002-01-01

    At the beginning of the age of laser-ionisation mass spectrometry (LIMS) increasing numbers of publications were observed. However, later the method began to run into obstacles associated with poor reproducibility of analysis and large variations in elemental sensitivities so that the wide interest

  12. Thermally and optically stimulated luminescence of AlN-Y2O3 ceramics after ionising irradiation

    DEFF Research Database (Denmark)

    Trinkler, L.; Bos, A.J.J.; Winkelman, A.J.M.

    1999-01-01

    Thermally (TL) and optically stimulated luminescence (OSL) were studied in AlN-Y2O3 ceramics after irradiation with ionising radiation. The extremely high TL sensitivity (approximately 60 times the sensitivity of LiF:Mg,Tl (TLD-100)) makes AlN-Y2O3 ceramics attractive as a TLD material. However...... on spectral properties and thermal evolution of OSL are also presented. The stimulation spectrum covers the spectral range from green to infrared light. A combination of thermal and optical stimulation allowed a correlation to be found between parameters of OSL and TL after the same irradiation dose...

  13. The characterisation of shellac resin by flow injection and liquid chromatography coupled with electrospray ionisation and mass spectrometry.

    Science.gov (United States)

    Tamburini, Diego; Dyer, Joanne; Bonaduce, Ilaria

    2017-11-01

    A strategy based on electrospray ionisation (ESI) in negative mode coupled with quadrupole-time of flight (Q-ToF) detection techniques was adopted to characterise some samples of shellac resin. Flow injection analysis (FIA) was used to investigate the distribution of the components of the resin. Eight groups of compounds with increasing masses were detected and assigned to free acids, esters and polyesters with up to eight units. High pressure liquid chromatography (HPLC) enabled the compounds to be chromatographically separated. Accurate molecular masses and tandem mass (MS/MS) spectra interpretation were used to characterise the different compounds, assigning and/or suggesting molecular structures. In some cases, highly detailed information about the ester linkages was provided by the MS/MS spectra, enabling the different isomers to be distinguished. Oxidation products were also identified in the samples and differences were observed in terms of hydrolysis and oxidation. In addition to providing the first characterisation of shellac by HPLC-ESI-Q-ToF and an atlas of MS/MS spectra of shellac components, this work demonstrates the suitability of the proposed strategy for characterising the resin, and provides the identification of previously unknown degradation products and minor components. This represents a significant step forward in the chemical knowledge of this material.

  14. A comparative study of matrix- and nano-assisted laser desorption/ionisation time-of-flight mass spectrometry of isolated and synthetic lignin.

    Science.gov (United States)

    Yoshioka, Koichi; Ando, Daisuke; Watanabe, Takashi

    2012-01-01

    Lignin is the second most abundant biopolymer next to cellulose. However, because of the complexity of the heterogeneous macromolecules, it is difficult to elucidate the polymeric structures of lignin by conventional analytical methods. To obtain the detailed structures of lignin, we comparatively applied nano-assisted laser desorption/ionisation time-of-flight mass spectrometry (NALDI-TOF MS) and matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry (MALDI-TOF MS). Synthetic lignin from coniferyl alcohol and an isolated lignin from Pinus densiflora were subjected to NALDI- and MALDI-TOF MS. We first obtained NALDI-TOF MS of synthetic and isolated lignin. Mass increments of 178 and 196 Da were observed in NALDI- and MALDI-TOF mass spectra of the synthetic and isolated lignin. The mass intervals indicated that radical coupling forming β-O-4 bonds is the major pathway. Peaks in the low molecular mass region between m/z 500 and 800 were observed more extensively using NALDI-TOF MS than MALDI-TOF MS, which enabled detailed analysis of the interunit linkages in lignin. Owing to the ionisation profile differentiation from MALDI-TOF MS, NALDI-TOF MS is useful for the structural analysis of lignin. Copyright © 2011 John Wiley & Sons, Ltd.

  15. Headspace analysis of new psychoactive substances using a Selective Reagent Ionisation-Time of Flight-Mass Spectrometer

    Science.gov (United States)

    Acton, W. Joe; Lanza, Matteo; Agarwal, Bishu; Jürschik, Simone; Sulzer, Philipp; Breiev, Kostiantyn; Jordan, Alfons; Hartungen, Eugen; Hanel, Gernot; Märk, Lukas; Mayhew, Chris A.; Märk, Tilmann D.

    2014-01-01

    The rapid expansion in the number and use of new psychoactive substances presents a significant analytical challenge because highly sensitive instrumentation capable of detecting a broad range of chemical compounds in real-time with a low rate of false positives is required. A Selective Reagent Ionisation-Time of Flight-Mass Spectrometry (SRI-ToF-MS) instrument is capable of meeting all of these requirements. With its high mass resolution (up to m/Δm of 8000), the application of variations in reduced electric field strength (E/N) and use of different reagent ions, the ambiguity of a nominal (monoisotopic) m/z is reduced and hence the identification of chemicals in a complex chemical environment with a high level of confidence is enabled. In this study we report the use of a SRI-ToF-MS instrument to investigate the reactions of H3O+, O2+, NO+ and Kr+ with 10 readily available (at the time of purchase) new psychoactive substances, namely 4-fluoroamphetamine, methiopropamine, ethcathinone, 4-methylethcathinone, N-ethylbuphedrone, ethylphenidate, 5-MeO-DALT, dimethocaine, 5-(2-aminopropyl)benzofuran and nitracaine. In particular, the dependence of product ion branching ratios on the reduced electric field strength for all reagent ions was investigated and is reported here. The results reported represent a significant amount of new data which will be of use for the development of drug detection techniques suitable for real world scenarios. PMID:25844048

  16. Rapid assignment of malting barley varieties by matrix-assisted laser desorption-ionisation - Time-of-flight mass spectrometry.

    Science.gov (United States)

    Šedo, Ondrej; Kořán, Michal; Jakešová, Michaela; Mikulíková, Renata; Boháč, Michal; Zdráhal, Zbyněk

    2016-09-01

    A method for discriminating malting barley varieties based on direct matrix-assisted laser desorption-ionisation - time-of-flight mass spectrometry (MALDI-TOF MS) fingerprinting of proteins was developed. Signals corresponding to hordeins were obtained by simple mixing of powdered barley grain with a MALDI matrix solution containing 12.5mgmL(-1) of ferulic acid in an acetonitrile:water:formic acid 50:33:17 v/v/v mixture. Compared to previous attempts at MALDI-TOF mass spectrometric analysis of barley proteins, the extraction and fractionation steps were practically omitted, resulting in a significant reduction in analytical time and costs. The discriminatory power was examined on twenty malting barley varieties and the practicability of the method was tested on sixty barley samples acquired from Pilsner Urquell Brewery. The method is proposed as a rapid tool for variety assignment and purity determination of malting barley that may replace gel electrophoresis currently used for this purpose. Copyright © 2016 Elsevier Ltd. All rights reserved.

  17. Determination of the plant growth regulator chlormequat in food by liquid chromatography-electrospray ionisation tandem mass spectrometry.

    Science.gov (United States)

    Hau, J; Riediker, S; Varga, N; Stadler, R H

    2000-05-05

    A confirmatory method for the determination of trace levels of chlormequat in a variety of different food matrices was developed. It entails a single clean-up step over a solid-phase cation exchange resin and subsequent liquid chromatography-electrospray ionisation tandem mass spectrometry using a stable isotopically labelled internal standard. Mass spectral acquisition was done in selected reaction monitoring mode, selecting the transitions from both the 35Cl and the 37Cl isotope of chlormequat. Recoveries after extraction and clean-up, determined with radio-labelled chlormequat and averaged over the spiking range (16-65 microg kg(-1)) in four different commodities, were within 88-96%, with a coefficient of variation better than 8%. The method can be applied to pears, pear juice concentrates, fruit purées, and cereal products, with typical limits of detection for chlormequat estimated at 2-5 microg kg(-1). A survey of different food commodities revealed that chlormequat was detectable--albeit at very low levels--in many of the food samples analysed, with the highest concentration recorded in pears purchased in Switzerland and of South African origin (5.5 mg kg(-1)). Measurements were also conducted on two LC-MS instruments and demonstrate the versatility and robustness of the method and its applicability to instruments of different ion source design.

  18. Desorption electrospray ionisation mass spectrometry: A rapid screening tool for veterinary drug preparations and forensic samples from hormone crime investigations

    Energy Technology Data Exchange (ETDEWEB)

    Nielen, M.W.F. [RIKILT Institute of Food Safety, P.O. Box 230, 6700 AE Wageningen (Netherlands); Wageningen University, Laboratory of Organic Chemistry, Dreijenplein 8, 6703 HB Wageningen (Netherlands)], E-mail: michel.nielen@wur.nl; Hooijerink, H. [RIKILT Institute of Food Safety, P.O. Box 230, 6700 AE Wageningen (Netherlands); Claassen, F.C. [Wageningen University, Laboratory of Organic Chemistry, Dreijenplein 8, 6703 HB Wageningen (Netherlands); Engelen, M.C. van [RIKILT Institute of Food Safety, P.O. Box 230, 6700 AE Wageningen (Netherlands); Beek, T.A. van [Wageningen University, Laboratory of Organic Chemistry, Dreijenplein 8, 6703 HB Wageningen (Netherlands)

    2009-04-01

    Hormone and veterinary drug screening and forensics can benefit from the recent developments in desorption electrospray ionisation (DESI) mass spectrometry (MS). In this work the feasibility of DESI application has been studied. Using a linear ion trap or quadrupole time-of-flight (TOF) MS instrument both full-scan and data-dependent collision-induced dissociation MS{sup n} spectra were acquired in seconds without sample preparation. Preliminary data are presented for the rapid screening of (pro)hormone supplement samples, an illegal steroid cocktail and forensic samples from veterinary drug investigations. The potential of this DESI approach is clearly demonstrated since compounds observed could be independently confirmed by liquid chromatography/TOFMS with accurate mass measurement, and/or proton nuclear magnetic resonance spectroscopy. Specific concerns related to false-positive and false-negative findings due to limitations in quantification and memory-effects are briefly discussed. It is envisaged that DESI will achieve a prominent role in hormone and veterinary drug analysis in the near future.

  19. Rapid and simultaneous determination of polychlorinated biphenyls and their main metabolites (hydroxylated and methyl sulfonyl) by gas chromatography coupled to mass spectrometry: comparison of different ionisation modes.

    Science.gov (United States)

    Castro-Puyana, M; Herrero, L; González, M J; Gómara, B

    2013-07-17

    Instrumental methods based on gas chromatography coupled to mass spectrometry (GC-MS) have been developed and compared using two different MS ionisation modes, electron impact (EI) and electron capture negative ionisation (ECNI), for the fast, quantitative and simultaneous determination of polychlorinated biphenyls (PCBs) and their main metabolites (hydroxylated PCBs, OH-PCBs, and methyl sulfone PCBs, MeSO2-PCBs). Parameters affecting chromatographic separation and MS detection were evaluated in order to achieve the highest selectivity and sensitivity for both operation modes. The analytical characteristics of the developed methods were studied and compared in terms of linear range, limits of detection (LODs), limits of quantification (LOQs), and instrumental precision (repeatability and intermediate precision). Both ionisation methods showed similar precision, being relative standard deviations (RSD, %) lower than 9% and 14% for repeatability and intermediate precision, respectively. However, better LODs (from 0.01 to 0.14 pg injected for the three families of congeners studied) were achieved using ECNI-MS as ionisation mode. The suitability of the developed method was demonstrated through their application to fish liver oil samples. Copyright © 2013 Elsevier B.V. All rights reserved.

  20. Investigation of colloidal graphite as a matrix for matrix-assisted laser desorption/ionisation mass spectrometry of low molecular weight analytes.

    Science.gov (United States)

    Warren, Alexander D; Conway, Ulric; Arthur, Christopher J; Gates, Paul J

    2016-07-01

    The analysis of low molecular weight compounds by matrix-assisted laser desorption/ionisation mass spectrometry is problematic due to the interference and suppression of analyte ionisation by the matrices typically employed - which are themselves low molecular weight compounds. The application of colloidal graphite is demonstrated here as an easy to use matrix that can promote the ionisation of a wide range of analytes including low molecular weight organic compounds, complex natural products and inorganic complexes. Analyte ionisation with colloidal graphite is compared with traditional organic matrices along with various other sources of graphite (e.g. graphite rods and charcoal pencils). Factors such as ease of application, spectra reproducibility, spot longevity, spot-to-spot reproducibility and spot homogeneity (through single spot imaging) are explored. For some analytes, considerable matrix suppression effects are observed resulting in spectra completely devoid of matrix ions. We also report the observation of radical molecular ions [M(-●) ] in the negative ion mode, particularly with some aromatic analytes. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  1. Comparison of electrospray ionisation, atmospheric pressure chemical ionisation and atmospheric pressure photoionisation for the identification of metabolites from labile artemisinin-based anti-malarial drugs using a QTRAP® mass spectrometer.

    Science.gov (United States)

    Louw, Stefan; Njoroge, Mathew; Chigorimbo-Murefu, Nyaradzo; Chibale, Kelly

    2012-10-30

    Artemisinin-based drugs and their metabolites are prone to in-source fragmentation under atmospheric pressure ionisation mass spectrometry (API-MS) conditions. To facilitate correct and efficient identification of all possible drug metabolites using full scan MS analyzer methods, stable [M + NH(4) ](+) ions should be produced in the MS source. Using a high-performance liquid chromatography (HPLC) hybrid triple quadrupole linear ion trap MS system, electrospray ionisation (ESI), atmospheric pressure chemical ionisation (APCI) and atmospheric pressure photoionisation (APPI) methods were developed for the detection of [M + NH(4) ](+) ions of the test compounds dihydroartemisinin, artemisinin, artemether and artesunic acid. The optimised methods employed ammonium formate buffered HPLC mobile phase in combination with moderate source temperatures (100-200 °C) and showed satisfactorily reduced in-source fragmentation. With a full scan MS analyser method for the detection of the in vitro metabolites of the test compounds, the respective performance of the ESI and APCI methods was found to be comparable. ESI generally resulted in less in-source fragmentation. Incorrect assignment of metabolites resulted from strong in-source fragmentation of artemether using the APPI method. The most number of metabolites could be detected using ESI in combination with a selective MS analyser method. ESI and APCI full scan methods proved to be capable of detecting any drug metabolites present in reasonable concentrations, and are useful when employed in addition to selective scan methods that target low level expected metabolites. APPI can be a valuable alternative for detecting expected metabolites due to good signal-to-noise (S/N) ratio. Copyright © 2012 John Wiley & Sons, Ltd.

  2. Simultaneous determination of volatile and non-volatile nitrosamines in processed meat products by liquid chromatography tandem mass spectrometry using atmospheric pressure chemical ionisation and electrospray ionisation.

    Science.gov (United States)

    Herrmann, S S; Duedahl-Olesen, L; Granby, K

    2014-02-21

    A sensitive, selective and generic method has been developed for the simultaneous determination of the contents (μgkg(-1) range) of both volatile nitrosamines (VNA) and non-volatile nitrosamines (NVNA) in processed meat products. The extraction procedure only requires basic laboratory equipment and a small volume of organic solvent. Separation and quantification were performed by the developed LC-(APCI/ESI)MS/MS method. The method was validated using spiked samples of three different processed meat products. Satisfactory recoveries (50-130%) and precisions (2-23%) were obtained for eight VNA and six NVNAs with LODs generally between 0.2 and 1μgkg(-1), though for a few analyte/matrix combinations higher LODs were obtained (3 to 18μgkg(-1)). The validation results show that results obtained for one meat product is not always valid for other meat products. We were not able to obtain satisfactory results for N-nitrosohydroxyproline (NHPRO), N-nitrosodibenzylamine (NDBzA) and N-nitrosodiphenylamine (NDPhA). Application of the APCI interface improved the sensitivity of the method, because of less matrix interference, and gave the method a wider scope, as some NAs were ionisable only by APCI. However, it was only possible to ionize N-nitroso-thiazolidine-4-carboxylic acid (NTCA) and N-nitroso-2-methyl-thiazolidine-4-carboxylic acid (NMTCA) by ESI. The validated method was applied for the analysis of processed meat products and contents of N-nitrosodimethylamine (NDMA), N-nitrosopyrrolidine (NPYR), N-nitrosomethylaniline (NMA), N-nitrosoproline (NPRO), NTCA, and NMTCA were found in one or several nitrite cured meat products, whereas none were detected in non-nitrite cured bacon. Copyright © 2014 Elsevier B.V. All rights reserved.

  3. Online antioxidant activity and ultra-performance LC-electrospray ionisation-quadrupole time-of-fight mass spectrometry for chemical fingerprinting of Indian polyherbal formulations.

    Science.gov (United States)

    Bhandari, Pamita; Kumar, Neeraj; Khan, Shahid M; Bhutani, Kamlesh K

    2016-01-01

    A HPLC-DAD-DPPH method was developed for evaluating the 1, 1-diphenyl-2-picryl hydrazyl free radical scavenging activity of ethylacetate extracts of different polyherbal formulations (draksarista, draksava, lohasava and arvindasava) by using RP-18e column. The ethylacetate extract from polyherbal, 'draksarista' exhibited maximum free radical scavenging activity (99.9 ± 0.38%) followed by draksava (99.8 ± 0.34%), lohasava (98.5 ± 0.30%) and arvindasava (42.3 ± 0.34%) at 100 μg mL(-1). Simultaneously, ultra-performance liquid chromatography coupled with electrospray ionisation-quadrupole time-of-flight mass spectrometry (UPLC-ESI-QTOF-MS) was used to study chemical composition of the ethylacetate extracts of formulations. The characteristic electrospray mass ionisation reveals the dominance of polyphenols and their glycosides in the four polyherbal formulations.

  4. Analysis of triacetone triperoxide complexes with alkali metal ions by electrospray and extractive electrospray ionisation combined with ion mobility spectrometry and mass spectrometry.

    Science.gov (United States)

    Hill, Alex R; Edgar, Mark; Chatzigeorgiou, Maria; Reynolds, James C; Kelly, Paul F; Creaser, Colin S

    2015-01-01

    The complexation of triacetone triperoxide (TATP) with a range of alkali metals has been studied by electrospray ionisation-mass spectrometry yield [M+Cat](+) ions for all of the alkali metals. The formation of [2TATP+Li+LiX](+) (X = Br, Cl) sandwich complexes was also observed. Collision cross- sections for the lithium-containing complexes of TATP were measured by travelling wave ion mobility spectrometry mass spectrometry, and compared well with computationally determined structures. Extractive electrospray ionisation (EESI) using a lithium doped electrospray is demonstrated for the detection of TATP vapours desorbed from a metal surface. The limit of detection for EESI was shown to be 20 ng using the [TATP+Li](+) ion.

  5. Identification of synthetic dyes in early colour photographs using capillary electrophoresis and electrospray ionisation-mass spectrometry.

    Science.gov (United States)

    López-Montes, Ana Ma; Dupont, Anne-Laurence; Desmazières, Bernard; Lavédrine, Bertrand

    2013-09-30

    Capillary electrophoresis with photodiode array detection (CE-PDA) and with electrospray ionisation-mass spectrometry (CE-ESI-MS) was used for the separation and the identification of 23 synthetic organic dyes, among those used in early 20th century colour photographs such as autochromes. Both cationic and anionic dyes could be separated within 15min using a single CE-PDA method. The method was used as the basis to develop a CE-ESI-MS methodology through the optimisation of the relevant ESI and MS parameters. Sheath liquid composition, nebulising gas pressure, drying gas flow rate and drying gas temperature were found to influence the sensitivity of the detection. These parameters were optimised in positive and negative ion modes for cationic dyes and anionic dyes, respectively. The two analyses could be carried out successively on a single sample. In view of the application to cultural heritage objects, the CE-ESI-MS analytical procedure was applied to identify the dyes in a Filmcolor artefact, late version of the autochrome. The results complemented and enhanced current knowledge as four cationic dyes and three anionic dyes were identified. Four additional dyes are proposed as possibly present as traces. Copyright © 2013 Elsevier B.V. All rights reserved.

  6. Neutral and acidic products derived from hydroxyl radical-induced oxidation of arabinotriose assessed by electrospray ionisation mass spectrometry.

    Science.gov (United States)

    Moreira, Ana S P; da Costa, Elisabete V; Evtuguin, Dmitry V; Coimbra, Manuel A; Nunes, Fernando M; Domingues, M Rosário M

    2014-04-01

    The oxidation of α-(1 → 5)-L-arabinotriose (Ara3), an oligosaccharide structurally related to side chains of coffee arabinogalactans, was studied in reaction with hydroxyl radicals generated under conditions of Fenton reaction (Fe(2+)/H2O2). The acidic and neutral oxidation products were separated by ligand exchange/size-exclusion chromatography, subsequently identified by electrospray ionisation mass spectrometry (ESI-MS) and structurally characterised by tandem MS (ESI-MS/MS). In acidic fraction were identified several oxidation products containing an acidic residue at the corresponding reducing end of Ara3, namely arabinonic acid, and erythronic, glyceric and glycolic acids formed by oxidative scission of the furanose ring. In neutral fractions were identified derivatives containing keto, hydroxy and hydroperoxy moieties, as well as derivatives resulting from the ring scission at the reducing end of Ara3. In both acidic and neutral fractions, beyond the trisaccharide derivatives, the corresponding di- and monosaccharide derivatives were identified indicating the occurrence of oxidative depolymerisation. The structural characterisation of these oxidation products by ESI-MS/MS allowed the differentiation of isobaric and isomeric species of acidic and neutral character. The species identified in this study may help in detection of roasting products associated with the free radical-mediated oxidation of coffee arabinogalactans. Copyright © 2014 John Wiley & Sons, Ltd.

  7. Multi-residue analysis of pesticides in traditional Chinese medicines using gas chromatography-negative chemical ionisation tandem mass spectrometry.

    Science.gov (United States)

    Nie, Jing; Miao, Shui; Lehotay, Steven J; Li, Wen-Ting; Zhou, Heng; Mao, Xiu-Hong; Lu, Ji-Wei; Lan, Lan; Ji, Shen

    2015-01-01

    In this study, a residue analysis method for the simultaneous determination of 107 pesticides in traditional Chinese medicines (TCMs), Angelica sinensis, A. dahurica, Leonurus heterophyllus Sweet, Pogostemon cablin and Lonicera japonica Thunb., was developed using gas chromatography coupled with tandem mass spectrometry in negative chemical ionisation mode (GC-NCI-MS/MS). NCI has advantages of high sensitivity and selectivity to chemicals with electron-withdrawing groups, and yields low background interference. For sample preparation, QuEChERS (quick, easy, cheap, effective, rugged and safe) was applied. Due to the unique characteristics of TCMs, the clean-up step was optimised by adjusting amounts of primary secondary amine, C18, graphitised carbon black and silica sorbents. Validation was mainly performed by determining analyte recoveries at four different spiking concentrations of 10, 50, 100 and 200 ng g(-1), with seven replicates at each concentration. Method trueness, precision, linearity of calibration curves, lowest calibrated levels (LCLs) and matrix effects were determined to demonstrate method and instrument performance. Among the 107 pesticides tested, approximately 80% gave recoveries from 80% to 110% and pesticides were 5 ng g(-1), and as low as 0.1 ng g(-1) for dichlofenthion, endosulfan sulphate, flumetralin, isofenphos-methyl, methyl-pentachlorophenyl sulphide and trifluralin. The results indicate that GC-NCI-MS/MS is an excellent technique for quantitative and qualitative analysis of targeted GC-amenable pesticides at ultra-trace levels, especially in complex matrices such as TCMs.

  8. Determination of chlorinated paraffins in sediments from the Firth of Clyde by gas chromatography with electron capture negative ionisation mass spectrometry and carbon skeleton analysis by gas chromatography with flame ionisation detection.

    Science.gov (United States)

    Hussy, Ines; Webster, Lynda; Russell, Marie; Moffat, Colin

    2012-07-01

    Short chain chlorinated paraffins (SCCPs) are a group of persistent organic pollutants (POPs) of increasing concern, but are to date not widely investigated in the environment, largely due to the challenges involved in their quantification. Here, SCCPs were quantified in marine sediments from the Firth of Clyde, Scotland, by gas chromatography with electron capture negative ionisation mass spectrometry (GC-ECNIMS) and through carbon skeleton analysis by gas chromatography with flame ionisation detection (GC-FID), and the analytical challenges encountered are discussed. Concentrations in the sediments ranged from 0.4 to 69 μg kg(-1) when determined by GC-ECNIMS, and from 5.6 to 379 μg kg(-1) when determined by GC-FID. For 8 out of 11 samples, analysis by GC-FID gave higher results than analysis by GC-ECNIMS. Unexpected aspects of the analysis, such as the presence of high concentrations of longer chain chlorinated paraffins in the samples, are also presented. Copyright © 2012 Elsevier Ltd. All rights reserved.

  9. Rapid analysis of formic acid, acetic acid, and furfural in pretreated wheat straw hydrolysates and ethanol in a bioethanol fermentation using atmospheric pressure chemical ionisation mass spectrometry

    Science.gov (United States)

    2011-01-01

    Atmospheric pressure chemical ionisation mass spectrometry (APCI-MS) offers advantages as a rapid analytical technique for the quantification of three biomass degradation products (acetic acid, formic acid and furfural) within pretreated wheat straw hydrolysates and the analysis of ethanol during fermentation. The data we obtained using APCI-MS correlated significantly with high-performance liquid chromatography analysis whilst offering the analyst minimal sample preparation and faster sample throughput. PMID:21896164

  10. Visualisation of abscisic acid and 12-oxo-phytodienoic acid in immature Phaseolus vulgaris L. seeds using desorption electrospray ionisation-imaging mass spectrometry

    OpenAIRE

    Enomoto, Hirofumi; Sensu, Takuya; Sato, Kei; Sato, Futoshi; Paxton, Thanai; Yumoto, Emi; Miyamoto, Koji; Asahina, Masashi; Yokota, Takao; Yamane, Hisakazu

    2017-01-01

    The plant hormone abscisic acid (ABA) and the jasmonic acid related-compound 12-oxo-phytodienoic acid (OPDA) play crucial roles in seed development, dormancy, and germination. However, a lack of suitable techniques for visualising plant hormones has restricted the investigation of their biological mechanisms. In the present study, desorption electrospray ionisation-imaging mass spectrometry (DESI-IMS), a powerful tool for visualising metabolites in biological tissues, was used to visualise AB...

  11. Accounting for matrix effects of pesticide residue liquid chromatography/electrospray ionisation mass spectrometric determination by treatment of background mass spectra with chemometric tools.

    Science.gov (United States)

    Kruve, Anneli; Herodes, Koit; Leito, Ivo

    2011-05-15

    Matrix effect (ME) - ionisation suppression or enhancement - in liquid chromatography/electrospray ionisation mass spectrometry (LC/ESI-MS) is caused by matrix components co-eluting with the analytes. ME has a complex and not fully understood nature. ME is also highly variable from sample to sample making it difficult to compensate for. In this work it was studied whether the background ion signals in scanned mass spectra of the LC effluent at the retention time of the analyte offer some insight into the presence and extent of matrix effect. Matrix effects for six pesticides - thiabendazole, carbendazime, methomyl, aldicarb, imazalil and methiocarb - in garlic and onion samples used in the study varied from 1% (suppression 99%) to 127% (enhancement 27%) depending on the pesticide and sample. Also standards in solvent and solvent blanks were included in the study. The ions most strongly varying from sample to sample - and therefore best describing the changes in sample composition and ME - were selected for quantification according to principal component analysis (PCA) for all six pesticides under study. These ions were used to account for ME via partial least-squares (PLS) regression. The calibration set was constructed from 19 samples and standards and the obtained calibration function was validated with seven samples and standards. The average errors from the test set were from 0.05 to 0.27 mg/kg for carbendazim and imazalil, respectively (the respective average pesticide concentrations were 0.22 and 0.88 mg/kg). The PLS results were significantly more accurate compared to the conventional solvent calibration resulting in average errors from 0.07 to 0.69 mg/kg for carbendazime and methiocarb, respectively. Copyright © 2011 John Wiley & Sons, Ltd.

  12. Identification of Tsetse (Glossina spp.) Using Matrix-Assisted Laser Desorption/Ionisation Time of Flight Mass Spectrometry

    Science.gov (United States)

    Hoppenheit, Antje; Murugaiyan, Jayaseelan; Bauer, Burkhard; Steuber, Stephan; Clausen, Peter-Henning; Roesler, Uwe

    2013-01-01

    Glossina (G.) spp. (Diptera: Glossinidae), known as tsetse flies, are vectors of African trypanosomes that cause sleeping sickness in humans and nagana in domestic livestock. Knowledge on tsetse distribution and accurate species identification help identify potential vector intervention sites. Morphological species identification of tsetse is challenging and sometimes not accurate. The matrix-assisted laser desorption/ionisation time of flight mass spectrometry (MALDI TOF MS) technique, already standardised for microbial identification, could become a standard method for tsetse fly diagnostics. Therefore, a unique spectra reference database was created for five lab-reared species of riverine-, savannah- and forest- type tsetse flies and incorporated with the commercial Biotyper 3.0 database. The standard formic acid/acetonitrile extraction of male and female whole insects and their body parts (head, thorax, abdomen, wings and legs) was used to obtain the flies' proteins. The computed composite correlation index and cluster analysis revealed the suitability of any tsetse body part for a rapid taxonomical identification. Phyloproteomic analysis revealed that the peak patterns of G. brevipalpis differed greatly from the other tsetse. This outcome was comparable to previous theories that they might be considered as a sister group to other tsetse spp. Freshly extracted samples were found to be matched at the species level. However, sex differentiation proved to be less reliable. Similarly processed samples of the common house fly Musca domestica (Diptera: Muscidae; strain: Lei) did not yield any match with the tsetse reference database. The inclusion of additional strains of morphologically defined wild caught flies of known origin and the availability of large-scale mass spectrometry data could facilitate rapid tsetse species identification in the future. PMID:23875040

  13. Identification of Tsetse (Glossina spp. using matrix-assisted laser desorption/ionisation time of flight mass spectrometry.

    Directory of Open Access Journals (Sweden)

    Antje Hoppenheit

    Full Text Available Glossina (G. spp. (Diptera: Glossinidae, known as tsetse flies, are vectors of African trypanosomes that cause sleeping sickness in humans and nagana in domestic livestock. Knowledge on tsetse distribution and accurate species identification help identify potential vector intervention sites. Morphological species identification of tsetse is challenging and sometimes not accurate. The matrix-assisted laser desorption/ionisation time of flight mass spectrometry (MALDI TOF MS technique, already standardised for microbial identification, could become a standard method for tsetse fly diagnostics. Therefore, a unique spectra reference database was created for five lab-reared species of riverine-, savannah- and forest- type tsetse flies and incorporated with the commercial Biotyper 3.0 database. The standard formic acid/acetonitrile extraction of male and female whole insects and their body parts (head, thorax, abdomen, wings and legs was used to obtain the flies' proteins. The computed composite correlation index and cluster analysis revealed the suitability of any tsetse body part for a rapid taxonomical identification. Phyloproteomic analysis revealed that the peak patterns of G. brevipalpis differed greatly from the other tsetse. This outcome was comparable to previous theories that they might be considered as a sister group to other tsetse spp. Freshly extracted samples were found to be matched at the species level. However, sex differentiation proved to be less reliable. Similarly processed samples of the common house fly Musca domestica (Diptera: Muscidae; strain: Lei did not yield any match with the tsetse reference database. The inclusion of additional strains of morphologically defined wild caught flies of known origin and the availability of large-scale mass spectrometry data could facilitate rapid tsetse species identification in the future.

  14. Direct matrix-assisted laser desorption ionisation time-of-flight mass spectrometry identification of mycobacteria from colonies.

    Science.gov (United States)

    Zingue, D; Flaudrops, C; Drancourt, M

    2016-12-01

    Matrix-assisted laser desorption ionisation time-of-flight mass spectrometry (MALDI-TOF-MS) identification of mycobacteria requires a standard acetonitrile/formic acid pre-MALDI-TOF-MS. We prospectively compared this standard protocol with direct deposit with matrix for the identification of mycobacteria cultured on solid media. We first verified that Mycobacterium tuberculosis was killed after it was mixed with matrix. Then, 111 Mycobacterium isolates previously identified by partial rpoB gene sequencing were tested in parallel by the two protocols. An identification score >1.7 was obtained in 86/111 (77.5 %) isolates after protein extraction versus 97/111 (87.4 %) isolates after direct deposit (p = 0.039, Chi-squared test). In a third step, we determined that direct deposit achieved identification for as few as 2.104 M. tuberculosis organisms. In a fourth step, we evaluated direct deposit of one colony for 116 solid medium-cultured clinical isolates finally identified as representative of 12 species (63.8 % M. tuberculosis). For 114/116 (98.3 %) isolates with an identification score >1.2, the MALDI-TOF-MS identification was in complete agreement with the reference rpoB gene sequencing identification. One isolate with a MALDI-TOF-MS identification score of 1.22 for M. fortuitum was identified as M. avium by partial rpoB gene sequencing. One other isolate with a MALDI-TOF-MS identification score of 1.22 for M. tuberculosis was identified as M. tuberculosis by genotyping. All the original MALDI-TOF-MS spectra reported here have been deposited in a public database. Direct deposit of one colony on a MALDI-TOF-MS plate allows for an accurate identification of mycobacteria for an identification score >1.3.

  15. Identification of organic pigments in tattoo inks and permanent make-up using laser desorption ionisation mass spectrometry.

    Science.gov (United States)

    Niederer, Markus; Hauri, Urs; Kroll, Lydia; Hohl, Christopher

    2017-01-01

    Nowadays, about 12% of the European and 20% of the US population are tattooed. Rising concerns regarding consumer safety, led to legal restrictions on tattoo and permanent make-up (PMU) inks. Restrictions also include bans on certain colourants. Both ink types use organic pigments for colour-giving, plus inorganic pigments for white and black and colour tones. Pigments are only sparingly soluble in common solvents and occur as suspended particles in the ink matrix. Their detection and identification therefore pose a major challenge for laboratories involved in monitoring the legal compliance of tattoo inks and PMU. We overcame this challenge by developing a direct laser desorption ionisation time-of-flight mass spectrometry method, which included an easy sample clean up. The method proved to be capable of detecting and identifying organic pigments in almost all of the tested ink samples. Method validation and routine deployment during market surveys showed the method to be fit for purpose. Pigment screening of 396 tattoo inks and 55 PMU taken from the Swiss market between 2009 and 2017 lead to the following conclusions: Pigment variety is much greater in tattoo inks (18) than in PMU (10); four prohibited pigments (Pigment Green 7, Pigment Red 122, Pigment Violet 19 and 23) were found in both ink types; for PMU, these four pigments made up 12% of the pigment findings, compared to 32% for tattoo inks. Therefore, legal compliance of PMU was at a higher level. A comparison of pigments found with those declared on tattoo ink labels clearly showed that banned pigments are rarely declared, but rather masked by listing non present legal pigments and label forging; therefore, highlighting the urgency of widespread market controls.

  16. Analysis of wax ester molecular species by high performance liquid chromatography/atmospheric pressure chemical ionisation mass spectrometry.

    Science.gov (United States)

    Vrkoslav, Vladimír; Urbanová, Klára; Cvacka, Josef

    2010-06-18

    High chromatographic resolution of wax esters (WEs) was achieved by non-aqueous reversed-phase liquid chromatography on a Nova-Pak C18 column by optimising the acetonitrile/ethyl acetate mobile phase gradient. The retention behaviour of WEs was studied in this chromatographic system. The WEs eluted according to their equivalent carbon number (ECN) values; within the group of WEs with the identical ECN, the most unsaturated species tended to elute first. The isobaric WEs with different positions of the ester moiety were separated from each other whenever the lengths of the chains were sufficiently different. The methyl-branched esters eluted at shorter retention times than the straight-chained analogues, and the resolution among methyl-branched WEs depended on the position of the branching. The analytes were detected by atmospheric pressure chemical ionisation mass spectrometry (APCI-MS) using data-dependent scanning. WEs provided simple full-scan spectra with abundant protonated molecules and low-intensity fragments. Collision-induced dissociation (CID) promoted identification of the WE molecular species. The responses of WEs were found to be dependent on the number of double bonds and on the alkyl-chain length; the limits of the detection ranged from 20micromol/L to 200nmol/L. The HPLC/APCI-MS was applied for the analysis of the WEs isolated from honeycomb beeswax, jojoba oil and human hair. Good agreement between reported results and the literature data was achieved, with several novel polyunsaturated WEs also being found. Copyright (c) 2010 Elsevier B.V. All rights reserved.

  17. Chemical analyses of micrometre-sized solids by a miniature laser ablation/ionisation mass spectrometer (LMS)

    Science.gov (United States)

    Tulej, Marek; Wiesendanger, Reto; Neuland, Maike; Meyer, Stefan; Wurz, Peter; Neubeck, Anna; Ivarsson, Magnus; Riedo, Valentine; Moreno-Garcia, Pavel; Riedo, Andreas; Knopp, Gregor

    2017-04-01

    Investigation of elemental and isotope compositions of planetary solids with high spatial resolution are of considerable interest to current space research. Planetary materials are typically highly heterogenous and such studies can deliver detailed chemical information of individual sample components with the sizes down to a few micrometres. The results of such investigations can yield mineralogical surface context including mineralogy of individual grains or the elemental composition of of other objects embedded in the sample surface such as micro-sized fossils. The identification of bio-relevant material can follow by the detection of bio-relevant elements and their isotope fractionation effects [1, 2]. For chemical analysis of heterogenous solid surfaces we have combined a miniature laser ablation mass spectrometer (LMS) (mass resolution (m/Dm) 400-600; dynamic range 105-108) with in situ microscope-camera system (spatial resolution ˜2um, depth 10 um). The microscope helps to find the micrometre-sized solids across the surface sample for the direct mass spectrometric analysis by the LMS instrument. The LMS instrument combines an fs-laser ion source and a miniature reflectron-type time-of-flight mass spectrometer. The mass spectrometric analysis of the selected on the sample surface objects followed after ablation, atomisation and ionisation of the sample by a focussed laser radiation (775 nm, 180 fs, 1 kHz; the spot size of ˜20 um) [4, 5, 6]. Mass spectra of almost all elements (isotopes) present in the investigated location are measured instantaneously. A number of heterogenous rock samples containing micrometre-sized fossils and mineralogical grains were investigated with high selectivity and sensitivity. Chemical analyses of filamentous structures observed in carbonate veins (in harzburgite) and amygdales in pillow basalt lava can be well characterised chemically yielding elemental and isotope composition of these objects [7, 8]. The investigation can be

  18. Investigation of Tobacco Pyrolysis Gases and Puff-by-puff Resolved Cigarette Smoke by Single Photon Ionisation (SPI - Time-of-flight Mass Spectrometry (TOFMS

    Directory of Open Access Journals (Sweden)

    Adam T

    2014-12-01

    Full Text Available The work presented deals with the application of Single Photon Ionisation- Time-of-Flight Mass Spectrometry (SPI-TOFMS for the investigation of tobacco smoke. SPI-TOFMS is a modern analytical technique, which enables the simultaneous analysis of a large number of organic species in complex gas mixtures in real time. The paper is a summary of a PhD thesis (1 and seven research articles, which were recently published in various scientific journals (2-8. Consequently, more detailed information on particular aspects can be found in there.

  19. Identification of N-glycans from Ebola virus glycoproteins by matrix-assisted laser desorption/ionisation time-of-flight and negative ion electrospray tandem mass spectrometry

    Science.gov (United States)

    Ritchie, Gayle; Harvey, David J.; Stroeher, Ute; Feldmann, Friederike; Feldmann, Heinz; Wahl-Jensen, Victoria; Royle, Louise; Dwek, Raymond A.; Rudd, Pauline M.

    2012-01-01

    The larger fragment of the transmembrane glycoprotein (GP1) and the soluble glycoprotein (sGP) of Ebola virus were expressed in human embryonic kidney cells and the secreted products were purified from the supernatant for carbohydrate analysis. The N-glycans were released with PNGase F from within sodium dodecyl sulphate/polyacrylamide gel electrophoresis (SDS-PAGE) gels. Identification of the glycans was made with normal-phase high-performance liquid chromatography (HPLC), matrix-assisted laser desorption/ionisation mass spectrometry, negative ion electrospray ionisation fragmentation mass spectrometry and exoglycosidase digestion. Most glycans were complex bi-, tri-and tetra-antennary compounds with reduced amounts of galactose. No bisected compounds were detected. Triantennary glycans were branched on the 6-antenna; fucose was attached to the core GlcNAc residue. Sialylated glycans were present on sGP but were largely absent from GP1, the larger fragment of the transmembrane glycoprotein. Consistent with this was the generally higher level of processing of carbohydrates found on sGP as evidenced by a higher percentage of galactose and lower levels of high-mannose glycans than were found on GP1. These results confirm and expand previous findings on partial characterisation of the Ebola virus transmembrane glycoprotein. They represent the first detailed data on carbohydrate structures of the Ebola virus sGP. PMID:20131323

  20. Novel characterisation of minor α-linolenic acid isomers in linseed oil by gas chromatography and covalent adduct chemical ionisation tandem mass spectrometry.

    Science.gov (United States)

    Gómez-Cortés, P; Brenna, J T; Lawrence, P; de la Fuente, M A

    2016-06-01

    Discrimination between polyunsaturated fatty acid isomers with three double bonds is a great challenge, due to structural similarities and similar polarities. In this study, we report the identification of four minor geometrical isomers of α-linolenic acid (ALA) present in linseed oil samples: (9E,12Z,15E)-, (9Z,12Z,15E)-, (9Z,12E,15Z)- and (9E,12Z,15Z)-octadeca-9,12,15-trienoic acids, chromatographically resolved by gas chromatography (GC) using a new and highly polar ionic phase column (SLB-IL111). Gas chromatography-electron ionisation mass spectrometry (GC-EIMS) determined that the four unknown compounds were C18:3 n-3 isomers. The positional 9-12-15 C18:3 configuration was achieved by covalent adduct chemical ionisation tandem mass spectrometry (CACI-MS/MS) while geometrical configuration was established with analytical standards based on relative retention. We hypothesised that these isomers are formed during linseed oil deodorisation and postulate preferred and unfavoured isomerisation pathways of ALA. Copyright © 2016 Elsevier Ltd. All rights reserved.

  1. Qualitative analysis of Copaifera oleoresin using comprehensive two-dimensional gas chromatography and gas chromatography with classical and cold electron ionisation mass spectrometry.

    Science.gov (United States)

    Wong, Yong Foo; Uekane, Thais M; Rezende, Claudia M; Bizzo, Humberto R; Marriott, Philip J

    2016-12-16

    Improved separation of both sesquiterpenes and diterpenic acids in Copaifera multijuga Hayne oleoresin, is demonstrated by using comprehensive two-dimensional gas chromatography (GC×GC) coupled to accurate mass time-of-flight mass spectrometry (accTOFMS). GC×GC separation employs polar phases (including ionic liquid phases) as the first dimension (1D) column, combined with a lower polarity 2D phase. Elution temperatures (Te) of diterpenic acids (in methyl ester form, DAME) increased as the 1D McReynolds' polarity value of the column phase decreased. Since Te of sesquiterpene hydrocarbons decreased with increased polarity, the very polar SLB-IL111 1D phase leads to excessive peak broadening in the 2D apolar phase due to increased second dimension retention (2tR). The combination of SLB-IL59 with a nonpolar column phase was selected, providing reasonable separation and low Te for sesquiterpenes and DAME, compared to other tested column sets, without excessive 2tR. Identities of DAME were aided by both soft (30eV) electron ionisation (EI) accurate mass TOFMS analysis and supersonic molecular beam ionisation (cold EI) TOFMS, both which providing less fragmentation and increased relative abundance of molecular ions. The inter-relation between EI energies, emission current, signal-to-noise and mass error for the accurate mass measurement of DAME are reported. These approaches can be used as a basis for conducting of GC×GC with soft EI accurate mass measurement of terpenes, particularly for unknown phytochemicals. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. Proteome analysis of Arabidopsis thaliana by two-dimensional gel electrophoresis and matrix-assisted laser desorption/ionisation-time of flight mass spectrometry.

    Science.gov (United States)

    Giavalisco, Patrick; Nordhoff, Eckhard; Kreitler, Thomas; Klöppel, Klaus-Dieter; Lehrach, Hans; Klose, Joachim; Gobom, Johan

    2005-05-01

    In the present study we show results of a large-scale proteome analysis of the recently sequenced plant Arabidopsis thaliana. On the basis of a previously published sequential protein extraction protocol, we prepared protein extracts from eight different A. thaliana tissues (primary leaf, leaf, stem, silique, seedling, seed, root, and inflorescence) and analysed these by two-dimensional gel electrophoresis. A total of 6000 protein spots, from three of these tissues, namely primary leaf, silique and seedling, were excised and the contained proteins were analysed by matrix assisted laser desorption/ionisation time of flight mass spectrometry peptide mass fingerprinting. This resulted in the identification of the proteins contained in 2943 spots, which were found to be products of 663 different genes. In this report we present and discuss the methodological and biological results of our plant proteome analysis.

  3. Acid-yield measurements of the gas-phase ozonolysis of ethene as a function of humidity using Chemical Ionisation Mass Spectrometry (CIMS

    Directory of Open Access Journals (Sweden)

    K. E. Leather

    2012-01-01

    Full Text Available Gas-phase ethene ozonolysis experiments were conducted at room temperature to determine formic acid yields as a function of relative humidity (RH using the integrated EXTreme RAnge chamber-Chemical Ionisation Mass Spectrometry technique, employing a CH3I ionisation scheme. RHs studied were <1, 11, 21, 27, 30 % and formic acid yields of (0.07±0.01 and (0.41±0.07 were determined at <1 % RH and 30 % RH respectively, showing a strong water dependence. It has been possible to estimate the ratio of the rate coefficient for the reaction of the Criegee biradical, CH2OO with water compared with decomposition. This analysis suggests that the rate of reaction with water ranges between 1×10−12–1×10−15 cm3 molecule−1 s−1 and will therefore dominate its loss with respect to bimolecular processes in the atmosphere. Global model integrations suggest that this reaction between CH2OO and water may dominate the production of HC(OOH in the atmosphere.

  4. Rapid characterisation and identification of compounds in Saposhnikoviae Radix by high-performance liquid chromatography coupled with electrospray ionisation quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Chen, Luxiao; Chen, Xiangyang; Su, Lei; Jiang, Yanyan; Liu, Bin

    2017-08-18

    Saposhnikoviae Radix (SR), the dried root of Saposhnikovia divaricata (Turcz.) Schischk. (Umbelliferae), is commonly used as a traditional Chinese medicine. In this study, a rapid and accurate method was firstly, developed for the qualitative analysis of SR by high-performance liquid chromatography coupled with electrospray ionisation quadrupole time-of-flight mass spectrometry (HPLC-ESI-Q-TOF-MS/MS). A total of 45 compounds were identified or tentatively characterised, including 13 chromones, 28 coumarins and four others. Among them, 16 compounds were identified from SR for the first time. In addition, six chromones reference standards, including two isolated compounds of 3'-O-angeloylhamaudol and norcimifugin from the extraction of SR, were used to study the fragmentation pathways of chromones. The developed method was effective for characterising the compounds of SR, and the results of the study enriched the understanding of the chemical connotation.

  5. Identification of wheat varieties using matrix-assisted laserdesorption/ionisation time-of-flight mass spectrometry and anartificial neural network

    DEFF Research Database (Denmark)

    Bloch, Helle Aagaard; Kesmir, Can; Petersen, Marianne Kjerstine

    1999-01-01

    of this novelmethod with respect to various experimental parameters has been tested. The results can be summarised: (i)With this approach 97% of the wheat varieties can be classified correctly with a corresponding correlationcoefficient of 1.0, (ii) The method is fast since the time of extracting gliadins from flour......A novel tool for variety identification of wheat (Triticum aestivum L.) has been developed: an artificialneural network (ANN) is used to classify the gliadin fraction analysed by matrix-assisted laserdesorption/ionisation time-of-flight mass spectrometry (MALDI-TOFMS). The robustness...... can be reduced to20 min without significant decrease in overall performance, (iii) The storage of flour or extracts understandard conditions does not influence the classification ability (i. e. the generalisation ability) of themethod, and (iv) The classification obtained is not influenced...

  6. Analysis of peptides and protein digests by reversed phase high performance liquid chromatography-electrospray ionisation mass spectrometry using neutral pH elution conditions.

    Science.gov (United States)

    Yang, Yuanzhong; Boysen, Reinhard I; Chowdhury, Jamil; Alam, Asif; Hearn, Milton T W

    2015-05-04

    In this study, the advantages of carrying out the analysis of peptides and tryptic digests of proteins under gradient elution conditions at pH 6.5 by reversed-phase liquid chromatography (RP-HPLC) and in-line electrospray ionisation mass spectrometry (ESI-MS) are documented. For these RP separations, a double endcapped, bidentate anchored n-octadecyl wide pore silica adsorbent was employed in a capillary column format. Compared to the corresponding analysis of the same peptides and protein tryptic digests using low pH elution conditions for their RP-HPLC separation, this alternative approach provides improved selectivity and more efficient separation of these analytes, thus allowing a more sensitive identification of proteins at different abundance levels, i.e. more tryptic peptides from the same protein could be confidently identified, enabling higher sequence coverage of the protein to be obtained. This approach was further evaluated with very complex tryptic digests derived from a human plasma protein sample using an online two-dimensional (2D) strong cation-exchange (SCX)-RP-HPLC-ESI-MS/MS system. Again, at pH 6.5, with mobile phases of different compositions, improved chromatographic selectivities were obtained, concomitant with more sensitive on-line electrospray ionisation tandem mass spectrometric (ESI-MS/MS) analysis. As a consequence, more plasma proteins could be confidently identified, highlighting the potential of these RP-HPLC methods with elution at pH 6.5 to extend further the scope of proteomic investigations. Copyright © 2015 Elsevier B.V. All rights reserved.

  7. Looking into individual coffee beans during the roasting process: direct micro-probe sampling on-line photo-ionisation mass spectrometric analysis of coffee roasting gases.

    Science.gov (United States)

    Hertz-Schünemann, Romy; Streibel, Thorsten; Ehlert, Sven; Zimmermann, Ralf

    2013-09-01

    A micro-probe (μ-probe) gas sampling device for on-line analysis of gases evolving in confined, small objects by single-photon ionisation time-of-flight mass spectrometry (SPI-TOFMS) was developed. The technique is applied for the first time in a feasibility study to record the formation of volatile and flavour compounds during the roasting process within (inside) or in the direct vicinity (outside) of individual coffee beans. A real-time on-line analysis of evolving volatile and semi-volatile organic compounds (VOC and SVOC) as they are formed under the mild pyrolytic conditions of the roasting process was performed. The soft-ionisation mass spectra depict a molecular ion signature, which is well corresponding with the existing knowledge of coffee roasting and evolving compounds. Additionally, thereby it is possible to discriminate between Coffea arabica (Arabica) and Coffea canephora (Robusta). The recognized differences in the roasting gas profiles reflect the differences in the precursor composition of the coffee cultivars very well. Furthermore, a well-known set of marker compounds for Arabica and Robusta, namely the lipids kahweol and cafestol (detected in their dehydrated form at m/z 296 and m/z 298, respectively) were observed. If the variation in time of different compounds is observed, distinctly different evolution behaviours were detected. Here, phenol (m/z 94) and caffeine (m/z 194) are exemplary chosen, whereas phenol shows very sharp emission peaks, caffeine do not have this highly transient behaviour. Finally, the changes of the chemical signature as a function of the roasting time, the influence of sampling position (inside, outside) and cultivar (Arabica, Robusta) is investigated by multivariate statistics (PCA). In summary, this pilot study demonstrates the high potential of the measurement technique to enhance the fundamental knowledge of the formation processes of volatile and semi-volatile flavour compounds inside the individual coffee bean.

  8. Electron ionisation of sulfur dioxide.

    Science.gov (United States)

    Fletcher, James D; Parkes, Michael A; Price, Stephen D

    2013-05-14

    Relative precursor-specific partial ionisation cross sections for the fragment ions formed following electron ionisation of sulfur dioxide (SO2) have been measured for the first time, from 30 to 200 eV, using time-of-flight mass spectrometry coupled with two-dimensional ion coincidence detection. These data quantify the yields of O(2+), O(+), SO(2+), S(+), O2(+), and SO(+) ions, relative to the formation of SO2(+), via single, double, and triple electron ionisation of SO2. Formation of O(2+), following electron-SO2 collisions, has been quantified for the first time. The data allow a first experimental estimate of the triple ionisation potential of SO2 (69.0 ± 3.6 eV), an energy in good agreement with a value derived in this study via computational chemistry. The triple ion combination S(+) + O(+) + O(+) is clearly detected following electron collisions with SO2 at electron energies markedly below the vertical energy for forming SO2(3 +). This observation is accounted for by the operation of a stepwise pathway to the formation of S(+) + 2O(+) which does not involve the formation of a molecular trication.

  9. Direct analysis of pharmaceutical formulations from non-bonded reversed-phase thin-layer chromatography plates by desorption electrospray ionisation ion mobility mass spectrometry.

    Science.gov (United States)

    Harry, Emma L; Reynolds, James C; Bristow, Anthony W T; Wilson, Ian D; Creaser, Colin S

    2009-09-01

    The direct analysis of pharmaceutical formulations and active ingredients from non-bonded reversed-phase thin layer chromatography (RP-TLC) plates by desorption electrospray ionisation (DESI) combined with ion mobility mass spectrometry (IM-MS) is reported. The analysis of formulations containing analgesic (paracetamol), decongestant (ephedrine), opiate (codeine) and stimulant (caffeine) active pharmaceutical ingredients is described, with and without chromatographic development to separate the active ingredients from the excipient formulation. Selectivity was enhanced by combining ion mobility and mass spectrometry to characterise the desorbed gas-phase analyte ions on the basis of mass-to-charge ratio (m/z) and gas-phase ion mobility (drift time). The solvent composition of the DESI spray using a step gradient was varied to optimise the desorption of active pharmaceutical ingredients from the RP-TLC plates. The combined RP-TLC/DESI-IM-MS approach has potential as a rapid and selective technique for pharmaceutical analysis by orthogonal gas-phase electrophoretic and mass-to-charge separation. Copyright (c) 2009 John Wiley & Sons, Ltd.

  10. Usefulness of matrix-assisted laser desorption ionisation-time-of-flight mass spectrometry for identifying clinical Trichosporon isolates.

    Science.gov (United States)

    de Almeida Júnior, J N; Figueiredo, D S Y; Toubas, D; Del Negro, G M B; Motta, A L; Rossi, F; Guitard, J; Morio, F; Bailly, E; Angoulvant, A; Mazier, D; Benard, G; Hennequin, C

    2014-08-01

    Trichosporon spp. have recently emerged as significant human pathogens. Identification of these species is important, both for epidemiological purposes and for therapeutic management, but conventional identification based on biochemical traits is hindered by the lack of updates to the species databases provided by the different commercial systems. In this study, 93 strains, or isolates, belonging to 16 Trichosporon species were subjected to both molecular identification using IGS1 gene sequencing and matrix-assisted laser desorption ionisation-time-of-flight (MALDI-TOF) analysis. Our results confirmed the limits of biochemical systems for identifying Trichosporon species, because only 27 (36%) of the isolates were correctly identified using them. Different protein extraction procedures were evaluated, revealing that incubation for 30 min with 70% formic acid yields the spectra with the highest scores. Among the six different reference spectra databases that were tested, a specific one composed of 18 reference strains plus seven clinical isolates allowed the correct identification of 67 of the 68 clinical isolates (98.5%). Although until recently it has been less widely applied to the basidiomycetous fungi, MALDI-TOF appears to be a valuable tool for identifying clinical Trichosporon isolates at the species level. © 2013 The Authors Clinical Microbiology and Infection © 2013 European Society of Clinical Microbiology and Infectious Diseases.

  11. Analysis of sialyl oligosaccharides by high-performance liquid chromatography-electrospray ionisation-mass spectrometry with differentiation of alpha2-3 and alpha2-6 sialyl linkages.

    Science.gov (United States)

    Pan, Geoffrey Ge; Melton, Laurence D

    2005-06-10

    A method for analysing sialyl oligosaccharides from bovine colostrum using high-performance liquid chromatography-electrospray ionisation-mass spectrometry (HPLC-ESI-MS) is described. Under positive ionisation mode, mass spectra of alpha2-3 and alpha2-6 linkages were different, and the former produced a prominent B2 (or B3 in disialyl lactose) mass fragment. This fragment was absent from mass spectra with alpha2-6 linkages. Two sialyl oligosaccharides, which have not been reported previously, were tentatively identified. One comprises a N-acetyl neuraminic acid (Neu5Ac), two hexoses (Hex), and one N-acetyl hexosamine (HexNAc) residue ((Neu5Ac)1 (Hex)2 (HexNAc)1), and the other comprises one Neu5Ac and one Hex residue ((Neu5Ac)1(Hex)1).

  12. Visualisation of abscisic acid and 12-oxo-phytodienoic acid in immature Phaseolus vulgaris L. seeds using desorption electrospray ionisation-imaging mass spectrometry

    Science.gov (United States)

    Enomoto, Hirofumi; Sensu, Takuya; Sato, Kei; Sato, Futoshi; Paxton, Thanai; Yumoto, Emi; Miyamoto, Koji; Asahina, Masashi; Yokota, Takao; Yamane, Hisakazu

    2017-02-01

    The plant hormone abscisic acid (ABA) and the jasmonic acid related-compound 12-oxo-phytodienoic acid (OPDA) play crucial roles in seed development, dormancy, and germination. However, a lack of suitable techniques for visualising plant hormones has restricted the investigation of their biological mechanisms. In the present study, desorption electrospray ionisation-imaging mass spectrometry (DESI-IMS), a powerful tool for visualising metabolites in biological tissues, was used to visualise ABA and OPDA in immature Phaseolus vulgaris L. seed sections. The mass spectra, peak values and chemical formulae obtained from the analysis of seed sections were consistent with those determined for ABA and OPDA standards, as were the precursor and major fragment ions observed in tandem mass spectrometry (MS/MS) imaging. Furthermore, the precursor and fragment ion images showed similar distribution patterns. In addition, the localisation of ABA and OPDA using DESI-IMS was confirmed using liquid chromatography-MS/MS (LC-MS/MS). The results indicated that ABA was mainly distributed in the radical and cotyledon of the embryo, whereas OPDA was distributed exclusively in external structures, such as the hilum and seed coat. The present study is the first to report the visualisation of plant hormones using IMS, and demonstrates that DESI-IMS is a promising technique for future plant hormone research.

  13. Visualisation of abscisic acid and 12-oxo-phytodienoic acid in immature Phaseolus vulgaris L. seeds using desorption electrospray ionisation-imaging mass spectrometry.

    Science.gov (United States)

    Enomoto, Hirofumi; Sensu, Takuya; Sato, Kei; Sato, Futoshi; Paxton, Thanai; Yumoto, Emi; Miyamoto, Koji; Asahina, Masashi; Yokota, Takao; Yamane, Hisakazu

    2017-02-17

    The plant hormone abscisic acid (ABA) and the jasmonic acid related-compound 12-oxo-phytodienoic acid (OPDA) play crucial roles in seed development, dormancy, and germination. However, a lack of suitable techniques for visualising plant hormones has restricted the investigation of their biological mechanisms. In the present study, desorption electrospray ionisation-imaging mass spectrometry (DESI-IMS), a powerful tool for visualising metabolites in biological tissues, was used to visualise ABA and OPDA in immature Phaseolus vulgaris L. seed sections. The mass spectra, peak values and chemical formulae obtained from the analysis of seed sections were consistent with those determined for ABA and OPDA standards, as were the precursor and major fragment ions observed in tandem mass spectrometry (MS/MS) imaging. Furthermore, the precursor and fragment ion images showed similar distribution patterns. In addition, the localisation of ABA and OPDA using DESI-IMS was confirmed using liquid chromatography-MS/MS (LC-MS/MS). The results indicated that ABA was mainly distributed in the radical and cotyledon of the embryo, whereas OPDA was distributed exclusively in external structures, such as the hilum and seed coat. The present study is the first to report the visualisation of plant hormones using IMS, and demonstrates that DESI-IMS is a promising technique for future plant hormone research.

  14. An atmospheric pressure chemical ionisation liquid chromatographic-tandem mass spectrometry method for the analysis of benzodiazepines in urine.

    Science.gov (United States)

    Dunlop, S; Hayes, K; Leavy, P; Cusack, D; Maguire, R

    2017-10-01

    The objective of this work was to establish an analytical method for the analysis of 7 Benzodiazepines (diazepam, oxazepam, temazepam, nordiazepam, desalkylflurazepam, alprazolam and α-hydroxyalprazolam) in urine specimens taken from drivers suspected of driving under the influence of drugs. The specimen, calibrator and control preparation involved hydrolysis of conjugated benzodiazepines using β-glucuronidase in sodium acetate buffer, with incubation at 60°C for 2h. Specimens were then centrifuged, before being diluted 1 in 5 (total dilution 1 in 10), with 10% acetonitrile in water. Specimens were analysed using a Shimadzu Prominence UPLC coupled to an AB Sciex 4000 QTrap LC-MS-MS. The chromatographic column was a Shim-pack XR ODS 2.2μm. 3.0×50mm column and the mobile phase was a binary gradient system comprising of mobile phase A which was an ammonium formate/formic acid buffer dissolved in water and mobile phase B which was an ammonium formate/formic acid buffer dissolved in Acetonitrile. APCI was selected as the ionisation technique and the MS was operated in MRM mode, monitoring 2 transitions per analyte. The validation of the method is described. The method was found to be linear, accurate and precise (within day and between day) for diazepam, oxazepam, temazepam, nordiazepam, desalkylflurazepam, alprazolam and α-hydroxyalprazolam. The results of 480 cases are reviewed and show that alprazolam use was found in 35% of cases. Use of benzodiazepines resulting in oxazepam, nordiazepam or temazepam were found ca. 70% of cases analysed. Copyright © 2017 Elsevier B.V. All rights reserved.

  15. Concentration dependent Electrospray Ionisation Mass Spectrometry and Tandem Mass Spectrometry (MS/MS ) studies on (E,E)-1-[5-(1,3-benzodioxol-5yl)-1-oxo-2,4-pentadienyl]- piperidine (Piperine) and its analogues.

    Science.gov (United States)

    Khajuria, Ravi K; Sharma, Neha; Koul, Jawahar L; Verma, Mahendra K

    2013-01-01

    Studies on piperine ((M 1 )) and its synthetic analogues (M 2-18 ) by positive electrospray ionisation mass spectrometry were carried out in the flow injection mode of analysis in methanol. The MS experiments on these compounds at concentration 5 ng/μL or above yielded dimeric ionic species [2 M + Na](+) which revealed that piperine and its analogues exhibit clustering of ions when the solutions of these compounds at concentrations 5 ng/μL or above were allowed to move through the electrospray interface of the mass spectrometer. The same clustering of the ions was not observed when the solutions of the same compounds at concentrations below 5 ng/μL were used for similar studies. The formation of the clusters was further confirmed by tandem mass spectrometry (MS/MS) studies wherein the fragmentation of dimeric ionic species [2 M + Na](+) led to the formation of sodium adducted monomeric ionic species [M + Na](+). The MS measurements of these compounds by Atmospheric Pressure Chemical Ionisation (APCI) were on expected lines as there was no clustering of the ions in case of APCI-MS measurements.

  16. A new approach for plasma (xeno)metabolomics based on solid-phase extraction and nanoflow liquid chromatography-nanoelectrospray ionisation mass spectrometry.

    Science.gov (United States)

    David, Arthur; Abdul-Sada, Alaa; Lange, Anke; Tyler, Charles R; Hill, Elizabeth M

    2014-10-24

    Current metabolite profiling methods based on liquid chromatography-mass spectrometry (LC-MS) platforms do not detect many of the components present at trace concentrations in extracts of plasma due to their low ionisation efficiency or to interference from highly abundant compounds. Nanoflow LC-nanospray MS platforms, which are commonly used in proteomics, could overcome these limitations and significantly increase analytical sensitivity and coverage of the plasma (xeno)metabolome (i.e., metabolites and xenobiotics), but require small injection volumes (ionisation-time-of-flight mass spectrometry (nUHPLC-nESI-TOFMS). These methods use phospholipid filtration plates in combination with polymeric or mixed mode exchange solid-phase extraction (SPE). The phospholipid filtration plates removed >94% of the predominant phospholipid/lysophospholipid species from plasma, whilst absolute recoveries of 63 selected (xeno)metabolites from spiked plasma were generally between 60 and 104%. After a further SPE step, recoveries of test compounds were between 50 and 81%. Studies revealed that both the sample preparation methodology and nUHPLC-nESI-TOFMS analyses gave acceptable repeatability. A qualitative comparison of SPE methods revealed that sample concentration by either polymer or mixed mode ion-exchange SPE gave comprehensive metabolite coverage of plasma extracts, but the use of cation exchange SPE significantly increased detection of many cationic compounds in the sample extracts. Method detection limits for steroid, eicosanoid and bile metabolites were <1.0ng/mL plasma and for pharmaceutical contaminants were between 0.01 and 30ng/mL plasma. Comparison of the phospholipid removal/cation exchange SPE and the classical protein precipitation (PPT) sample preparation methodologies revealed that both methods detected the same range of (xeno)metabolites. However, unlike PPT extracts, the SPE preparations allowed direct injection of more concentrated plasma extracts onto the n

  17. Simultaneous determination of 16 brominated flame retardants in food and feed of animal origin by fast gas chromatography coupled to tandem mass spectrometry using atmospheric pressure chemical ionisation.

    Science.gov (United States)

    Bichon, E; Guiffard, I; Vénisseau, A; Lesquin, E; Vaccher, V; Brosseaud, A; Marchand, P; Le Bizec, B

    2016-08-12

    A gas chromatography tandem mass spectrometry method using atmospheric pressure chemical ionisation was developed for the monitoring of 16 brominated flame retardants (7 usually monitored polybromodiphenylethers (PBDEs) and BDE #209 and 8 additional emerging and novel BFRs) in food and feed of animal origin. The developed analytical method has decreased the run time by three compared to conventional strategies, using a 2.5m column length (5% phenyl stationary phase, 0.1mm i.d., 0.1μmf.t.), a pulsed split injection (1:5) with carrier gas helium flow rate at 0.48mLmin(-1) in one run of 20 min. For most BFRs, analytical data were compared with the current analytical strategy relying on GC/EI/HRMS (double sector, R=10000 at 10% valley). Performances in terms of sensitivity were found to meet the Commission recommendation (118/2014/EC) for nBFRs. GC/APCI/MS/MS represents a promising alternative for multi-BFRs analysis in complex matrices, in that it allows the monitoring of a wider list of contaminants in a single injection and a shorter run time. Copyright © 2016 Elsevier B.V. All rights reserved.

  18. Matrix-assisted laser desorption ionisation time-of-flight mass spectrometry rapid detection of carbapenamase activity in Acinetobacter baumannii isolates.

    Science.gov (United States)

    Abouseada, Noha; Raouf, May; El-Attar, Eman; Moez, Pacinte

    2017-01-01

    Carbapenamase-producing Acinetobacter baumannii are an increasing threat in hospitals and Intensive Care Units. Accurate and rapid detection of carbapenamase producers has a great impact on patient improvement and aids in implementation of infection control measures. In this study, we describe the use of matrix-assisted laser desorption ionisation time-of-flight mass spectrometry (MALDI TOF MS) to identify carbapenamase-producing A. baumannii isolates in up to 3 h. Isolates and Methods: A total of 50 A. baumannii isolates (of which 39 were carabapenamase producers) were tested using MALDI TOF MS. Isolates were incubated for 3 h with 0.25 mg/ml up to 2 mg/ml of imipenem (IMP) at 37°C. Supernatants were analysed by MALDI TOF to analyse peaks corresponding to IMP (300 Da) and an IMP metabolite (254 Da) using UltrafleXtreme (Bruker Daltonics, Bremen, Germany). All carbapenamase-producing isolates were evidenced by the disappearance or reduction in intensity of the 300 Da peak of IPM and the appearance of a 254 Da peak of the IPM metabolite. In isolates that did not produce carbapenamase, the IPM 300 Da peak remained intact. MALDI TOF is a promising tool in the field of diagnostic microbiology that has the ability to transfer identification and antimicrobial susceptibility testing time from days to hours.

  19. A novel matrix-assisted laser desorption/ionisation mass spectrometry imaging based methodology for the identification of sexual assault suspects.

    Science.gov (United States)

    Bradshaw, Robert; Wolstenholme, Rosalind; Blackledge, Robert D; Clench, Malcolm R; Ferguson, Leesa S; Francese, Simona

    2011-02-15

    An increase in the use of condoms by sexual offenders has been observed. This is likely to be due both to the risk of sexually transmitted diseases and to prevent the transfer of DNA evidence. In this scenario the detection of condom lubricants at a crime scene could aid in proving corpus delicti. Here we show a novel application of Matrix-Assisted Laser Desorption/Ionisation Mass Spectrometry Imaging (MALDI MSI) for mapping the fingermark ridge pattern simultaneously to the detection of the condom lubricant within the fingermark itself. Two condom brands have been investigated to prove the concept. Condoms were handled producing lubricant-contaminated fingermarks. Images of the ridge pattern were obtained simultaneously to the detection of two lubricants, even several weeks after the fingermark deposition. The results therefore show the potential of MALDI MSI to link the suspect (identification through fingermark ridge pattern) to the crime (detection of condom lubricant) in one analysis. This would enable forensic scientists to provide evidence with stronger support in alleged cases of sexual assault. Copyright © 2011 John Wiley & Sons, Ltd.

  20. Examination of the translocation of sulfonylurea herbicides in sunflower plants by matrix-assisted laser desorption/ionisation mass spectrometry imaging.

    Science.gov (United States)

    Anderson, David M G; Carolan, Vikki A; Crosland, Susan; Sharples, Kate R; Clench, Malcolm R

    2010-11-30

    Pesticides are widely used in agriculture to control weeds, pests and diseases. Successful control is dependent on the compound reaching the target site within the organism after spray or soil application. Conventional methods for determining uptake and movement of herbicides and pesticides include autoradiography, liquid scintillation and chromatographic techniques such as high-performance liquid chromatography (HPLC). Autoradiography using radiolabelled compounds provides the best indication of a compound's movement within the plant system. Autoradiography is an established technique but it relies on the synthesis of radiolabelled compounds. The distribution of four sulfonylurea herbicides in sunflower plants has been studied 24  h after foliar application. The use of matrix-assisted laser desorption/ionisation mass spectrometry imaging (MALDI-MSI) images of protonated molecules and fragment ions (resulting from fragmentation at the urea bond within the sulfonylurea herbicides) has provided evidence for translocation above and below the application point. The translocation of nicosulfuron and azoxystrobin within the same plant system has also been demonstrated following their application to the plant stem. This study provides evidence that MALDI-MSI has great potential as an analytical technique to detect and assess the foliar, root and stem uptake of agrochemicals, and to reveal their distribution through the plant once absorbed and translocated. 2010 John Wiley & Sons, Ltd.

  1. Characterisation of chemical components for identifying historical Chinese textile dyes by ultra high performance liquid chromatography - photodiode array - electrospray ionisation mass spectrometer.

    Science.gov (United States)

    Han, Jing; Wanrooij, Jantien; van Bommel, Maarten; Quye, Anita

    2017-01-06

    This research makes the first attempt to apply Ultra High Performance Liquid Chromatography (UHPLC) coupled to both Photodiode Array detection (PDA) and Electrospray Ionisation Mass Spectrometer (ESI-MS) to the chemical characterisation of common textile dyes in ancient China. Three different extraction methods, respectively involving dimethyl sulfoxide (DMSO)-oxalic acid, DMSO and hydrochloric acid, are unprecedentedly applied together to achieve an in-depth understanding of the chemical composition of these dyes. The first LC-PDA-MS database of the chemical composition of common dyes in ancient China has been established. The phenomena of esterification and isomerisation of the dye constituents of gallnut, gardenia and saffron, and the dye composition of acorn cup dyed silk are clarified for the first time. 6-Hydroxyrubiadin and its glycosides are first reported on a dyed sample with Rubia cordifolia from China. UHPLC-PDA-ESI-MS with a C18 BEH shield column shows significant advantages in the separation and identification of similar dye constituents, particularly in the cases of analysing pagoda bud and turmeric dyed sample extracts. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. A liquid chromatography/electrospray ionisation tandem mass spectrometry method for the simultaneous quantification of salicylic, jasmonic and abscisic acids in Coffea arabica leaves.

    Science.gov (United States)

    de Sá, Marta; Ferreira, João P; Queiroz, Vagner T; Vilas-Boas, Luís; Silva, Maria C; Almeida, Maria H; Guerra-Guimarães, Leonor; Bronze, Maria R

    2014-02-01

    Plants have developed an efficient system of recognition that induces a complex network of signalling molecules such as salicylic acid (SA), jasmonic acid (JA) and abscisic acid (ABA) in case of a pathogenic infection. The use of specific and sensitive methods is mandatory for the analysis of compounds in these complex samples. In this study a liquid chromatography/electrospray ionisation tandem mass spectrometry method was developed and validated for the simultaneous quantification of SA, JA and ABA in Coffea arabica (L.) leaves in order to understand the role of these phytohormones in the signalling network involved in the coffee defence response against Hemileia vastatrix. The results showed that the method was specific, linear (r ≥ 0.99) in the range 0.125-1.00 µg mL⁻¹ for JA and ABA and 0.125-5.00 µg mL⁻¹ for SA, and precise (relative standard deviation ≤11%), and the limit of detection (0.010 µg g⁻¹ fresh weight) was adequate for quantifying these phytohormones in this type of matrix. In comparison with healthy leaves, those infected with H. vastatrix (resistance reaction) displayed an increase in SA level 24 h after inoculation, suggesting the involvement of an SA-dependent pathway in coffee resistance. © 2013 Society of Chemical Industry.

  3. The Spatial Distribution of Alkaloids in Psychotria prunifolia (Kunth) Steyerm and Palicourea coriacea (Cham.) K. Schum Leaves Analysed by Desorption Electrospray Ionisation Mass Spectrometry Imaging.

    Science.gov (United States)

    Kato, Lucilia; Moraes, Aline Pereira; de Oliveira, Cecília Maria Alves; Vaz, Boniek Gontijo; de Almeida Gonçalves, Letícia; E Silva, Elienai Cândida; Janfelt, Christian

    2017-09-06

    Species of the genera Psychotria and Palicourea are sources of indole alkaloids, however, the distribution of alkaloids within the plants is not known. Analysing the spatial distribution using desorption electrospray ionisation mass spectrometry imaging (DESI-MSI) has become attractive due to its simplicity and high selectivity compared to traditional histochemical techniques. To apply DESI-MSI to visualise the alkaloid distribution on the leaf surface of Psychotria prunifolia and Palicourea coriacea and to compare the distributions with HPLC-MS and histochemical analyses. Based upon previous structure elucidation studies, four alkaloids targeted in this study were identified using high resolution mass spectrometry by direct infusion of plant extracts, and their distributions were imaged by DESI-MSI via tissue imprints on a porous Teflon surface. Relative quantitation of the four alkaloids was obtained by HPLC-MS/MS analysis performed using multiple-reaction monitoring (MRM) mode on a triple quadrupole mass spectrometer. Alkaloids showed distinct distributions on the leaf surfaces. Prunifoleine was mainly present in the midrib, while 10-hydroxyisodeppeaninol was concentrated close to the petiole; a uniform distribution of 10-hydroxyantirhine was observed in the whole leaf of Psychotria prunifolia. The imprinted image from the Palicourea coriacea leaf also showed a homogeneous distribution of calycanthine throughout the leaf surface. Different distributions were found for three alkaloids in Psychotria prunifolia, and the distributions found by MSI were in complete accordance with HPLC-MS analysis and histochemical results. The DESI-MSI technique was therefore demonstrated to provide reliable information about the spatial distribution of metabolites in plants. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

  4. Thermal Mass & Dynamic Effects Danish Building Regulation

    DEFF Research Database (Denmark)

    Le Dreau, Jerome; Selman, Ayser Dawod; Heiselberg, Per

    will focus on three main aspects: ♦ Assess the robustness of the monthly calculation method by varying the input parameters (Part 3) ♦ Better take into consideration the thermal mass in the actual tool by updating the utilisation factors used for the calculation of cooling and heating (Part 3) ♦ Find...... a method to evaluate night-time ventilation in the monthly calculation (Part 4)...

  5. The detection of iron protoporphyrin (heme b) in phytoplankton and marine particulate material by electrospray ionisation mass spectrometry – comparison with diode array detection

    Energy Technology Data Exchange (ETDEWEB)

    Gledhill, Martha, E-mail: m.gledhill@geomar.de

    2014-09-02

    Highlights: • Mass spectrometry was applied to the analysis of heme b in biological material. • Optimal conditions involved selective reactant monitoring of the heme b product ion. • The isotopic signature for this iron tetrapyrrole further improved selectivity. • Mass spectrometry and spectrophotometry were compared for heme b analysis. • Combining techniques made a powerful tool for analysis of heme in marine microbes. - Abstract: A mass spectrometric (MS) method for the identification of iron protoporphyrin (IX) (FePTP, heme b) in marine particulate material and phytoplankton is described. Electrospray ionisation of FePTP produced the molecular Fe(III)PTP{sup +} ion (m/z = 616) or the pseudomolecular [Fe(II)PTP + H]{sup +} ion (m/z = 617), depending on the oxidation state of the central iron ion. Collision induced dissociation (CID) in the ion trap mass spectrometer resulted in a single detected product ion (m/z = 557) indicative of loss of ethanoic acid from a carboxylic acid side chain. Widening the isolation width to 616 ± 3 resulted in production of a mass spectrum demonstrating the distinctive isotopic ratio of the iron containing fragment, further increasing the specificity of the analysis. Selective reactant monitoring (SRM) of the fragment ion (m/z = 557) was applied to the detection of FePTP after chromatography of ammoniacal OGP extracts of marine samples. The detection limit for FePTP analysed by SRM after chromatography was 1.2 ± 0.5 fmol. For phytoplankton samples, reasonably good agreement was achieved between results obtained with SRM and those obtained by monitoring absorbance at λ = 400 nm using a diode array detector (DAD). Use of SRM for analysis of particulate material obtained from the high latitude North Atlantic allowed for the analysis of FePTP in the presence of a co-eluting compound that interfered with detection by DAD. Simultaneous collection of mass spectra from m/z = 300 to 1500 resulted in identification of the

  6. Direct analysis of volatile organic compounds in foods by headspace extraction atmospheric pressure chemical ionisation mass spectrometry.

    Science.gov (United States)

    Perez-Hurtado, P; Palmer, E; Owen, T; Aldcroft, C; Allen, M H; Jones, J; Creaser, C S; Lindley, M R; Turner, M A; Reynolds, J C

    2017-11-30

    The rapid screening of volatile organic compounds (VOCs) by direct analysis has potential applications in the areas of food and flavour science. Currently, the technique of choice for VOC analysis is gas chromatography/mass spectrometry (GC/MS). However, the long chromatographic run times and elaborate sample preparation associated with this technique have led a movement towards direct analysis techniques, such as selected ion flow tube mass spectrometry (SIFT-MS), proton transfer reaction mass spectrometry (PTR-MS) and electronic noses. The work presented here describes the design and construction of a Venturi jet-pump-based modification for a compact mass spectrometer which enables the direct introduction of volatiles for qualitative and quantitative analysis. Volatile organic compounds were extracted from the headspace of heated vials into the atmospheric pressure chemical ionization source of a quadrupole mass spectrometer using a Venturi pump. Samples were analysed directly with no prior sample preparation. Principal component analysis (PCA) was used to differentiate between different classes of samples. The interface is shown to be able to routinely detect problem analytes such as fatty acids and biogenic amines without the requirement of a derivatisation step, and is shown to be able to discriminate between four different varieties of cheese with good intra and inter-day reproducibility using an unsupervised PCA model. Quantitative analysis is demonstrated using indole standards with limits of detection and quantification of 0.395 μg/mL and 1.316 μg/mL, respectively. The described methodology can routinely detect highly reactive analytes such as volatile fatty acids and diamines without the need for a derivatisation step or lengthy chromatographic separations. The capability of the system was demonstrated by discriminating between different varieties of cheese and monitoring the spoilage of meats. © 2017 The Authors. Rapid Communications in Mass

  7. Confirmation and 3D profiling of anabolic steroid esters in injection sites using imaging desorption electrospray ionisation (DESI) mass spectrometry

    NARCIS (Netherlands)

    Rijke, de E.; Hooijerink, H.; Sterk, S.S.; Nielen, M.W.F.

    2013-01-01

    In this study, desorption electrospray ionization (DESI) linear ion trap tandem mass spectrometry (MSn) was applied for the confirmation and 3D profiling of anabolic steroid esters in an injection site of bovine muscle. The spatial resolution of the DESI-MSn was demonstrated by scanning hormone

  8. Characterisation of botulinum toxins type A and B, by matrix-assisted laser desorption ionisation and electrospray mass spectrometry

    NARCIS (Netherlands)

    Baar, B.L.M. van; Hulst, A.G.; Jong, A.L. de; Wils, E.R.J.

    2002-01-01

    A method earlier developed for the mass spectrometric (MS) identification of tetanus toxin (TTx) was applied to botulinum toxins type A and B (BTxA and BTxB). Botulinum toxins are extremely neurotoxic bacterial toxins, likely to be used as biological warfare agent. Biologically active BTxA and BTxB

  9. Liquid chromatography-electrospray ionisation-mass spectrometry based method for the determination of estradiol benzoate in hair of cattle

    NARCIS (Netherlands)

    Hooyerink, H.; Lommen, A.; Mulder, P.P.J.; Rhijn, van J.A.; Nielen, M.W.F.

    2005-01-01

    A liquid chromatography (LC)-based method with mass spectrometric (MS/MS) detection was developed for the determination of estradiol benzoate residues in hair of cattle. First hair samples were pulverized with a ball mill followed by treatment with the reducing agent Tris(2-carboxyethyl)phosphine

  10. Thermal conductivity of mass-graded graphene flakes

    OpenAIRE

    Cheh, Jigger; Zhao, Hong

    2011-01-01

    In this letter we study thermal conduction in mass-graded graphene flakes by nonequilibrium molecular dynamics simulations. It is found that mass-graded graphene flakes reveal no thermal rectification effect in thermal conduction process. The dependence of thermal conductivity upon the heat flux and the mass gradient are studied to confirm the generality of the result.The mechanism leading to the absence of thermal rectification effect is also discussed.

  11. The detection of iron protoporphyrin (heme b) in phytoplankton and marine particulate material by electrospray ionisation mass spectrometry - comparison with diode array detection.

    Science.gov (United States)

    Gledhill, Martha

    2014-09-02

    A mass spectrometric (MS) method for the identification of iron protoporphyrin (IX) (FePTP, heme b) in marine particulate material and phytoplankton is described. Electrospray ionisation of FePTP produced the molecular Fe(III)PTP(+) ion (m/z=616) or the pseudomolecular [Fe(II)PTP + H](+) ion (m/z=617), depending on the oxidation state of the central iron ion. Collision induced dissociation (CID) in the ion trap mass spectrometer resulted in a single detected product ion (m/z=557) indicative of loss of ethanoic acid from a carboxylic acid side chain. Widening the isolation width to 616±3 resulted in production of a mass spectrum demonstrating the distinctive isotopic ratio of the iron containing fragment, further increasing the specificity of the analysis. Selective reactant monitoring (SRM) of the fragment ion (m/z=557) was applied to the detection of FePTP after chromatography of ammoniacal OGP extracts of marine samples. The detection limit for FePTP analysed by SRM after chromatography was 1.2±0.5fmol. For phytoplankton samples, reasonably good agreement was achieved between results obtained with SRM and those obtained by monitoring absorbance at λ=400nm using a diode array detector (DAD). Use of SRM for analysis of particulate material obtained from the high latitude North Atlantic allowed for the analysis of FePTP in the presence of a co-eluting compound that interfered with detection by DAD. Simultaneous collection of mass spectra from m/z=300 to 1500 resulted in identification of the pseudomolecular ion for the interfering compound. The CID fragmentation pattern and UV-visible mass spectra indicated that the interfering compound was a previously unidentified chlorin type compound. Comparison of FePTP determined by SRM and DAD on samples where this compound could not be detected showed that results collected using the two methods correlated. The use of both MS and DAD results in a powerful tool for quantifying this important biogenic component of the

  12. Airborne laser-spark for ambient desorption/ionisation.

    Science.gov (United States)

    Bierstedt, Andreas; Riedel, Jens

    A novel direct sampling ionisation scheme for ambient mass spectrometry is presented. Desorption and ionisation are achieved by a quasi-continuous laser induced plasma in air. Since there are no solid or liquid electrodes involved the ion source does not suffer from chemical interferences or fatigue originating from erosive burning or from electrode consumption. The overall plasma maintains electro-neutrality, minimising charge effects and accompanying long term drift of the charged particles trajectories. In the airborne plasma approach the ambient air not only serves as the plasma medium but at the same time also slows down the nascent ions via collisional cooling. Ionisation of the analyte molecules does not occur in the plasma itself but is induced by interaction with nascent ionic fragments, electrons and/or far ultraviolet photons in the plasma vicinity. At each individual air-spark an audible shockwave is formed, providing new reactive species, which expands concentrically and, thus, prevents direct contact of the analyte with the hot region inside the plasma itself. As a consequence the interaction volume between plasma and analyte does not exceed the threshold temperature for thermal dissociation or fragmentation. Experimentally this indirect ionisation scheme is demonstrated to be widely unspecific to the chemical nature of the analyte and to hardly result in any fragmentation of the studied molecules. A vast ensemble of different test analytes including polar and non-polar hydrocarbons, sugars, low mass active ingredients of pharmaceuticals as well as natural biomolecules in food samples directly out of their complex matrices could be shown to yield easily accessible yet meaningful spectra. Since the plasma medium is humid air, the chemical reaction mechanism of the ionisation is likely to be similar to other ambient ionisation techniques. Wir stellen hier eine neue Ionisationsmethode für die Umgebungsionisation (ambient ionisation) vor. Sowohl die

  13. Diagnostic performance of matrix-assisted laser desorption ionisation time-of-flight mass spectrometry in blood bacterial infections: a systematic review and meta-analysis.

    Science.gov (United States)

    Scott, Jamie S; Sterling, Sarah A; To, Harrison; Seals, Samantha R; Jones, Alan E

    2016-07-01

    Matrix-assisted laser desorption ionisation time-of-flight mass spectrometry (MALDI-TOF MS) has shown promise in decreasing time to identification of causative organisms compared to traditional methods; however, the utility of MALDI-TOF MS in a heterogeneous clinical setting is uncertain. To perform a systematic review on the operational performance of the Bruker MALDI-TOF MS system and evaluate published cut-off values compared to traditional blood cultures. A comprehensive literature search was performed. Studies were included if they performed direct MALDI-TOF MS analysis of blood culture specimens in human patients with suspected bacterial infections using the Bruker Biotyper software. Sensitivities and specificities of the combined studies were estimated using a hierarchical random effects linear model (REML) incorporating cut-off scores of ≥1.7 and ≥2.0. Fifty publications were identified, with 11 studies included after final review. The estimated sensitivity utilising a cut-off of ≥2.0 from the combined studies was 74.6% (95% CI = 67.9-89.3%), with an estimated specificity of 88.0% (95% CI = 74.8-94.7%). When assessing a cut-off of ≥1.7, the combined sensitivity increases to 92.8% (95% CI = 87.4-96.0%), but the estimated specificity decreased to 81.2% (95% CI = 61.9-96.6%). In this analysis, MALDI-TOF MS showed acceptable sensitivity and specificity in bacterial speciation with the current recommended cut-off point compared to blood cultures; however, lowering the cut-off point from ≥2.0 to ≥1.7 would increase the sensitivity of the test without significant detrimental effect on the specificity, which could improve clinician confidence in their results.

  14. Fractionation and analysis of lipopolysaccharide-derived oligosaccharides by zwitterionic-type hydrophilic interaction liquid chromatography coupled with electrospray ionisation mass spectrometry.

    Science.gov (United States)

    Man-Kupisinska, Aleksandra; Bobko, Ewelina; Gozdziewicz, Tomasz K; Maciejewska, Anna; Jachymek, Wojciech; Lugowski, Czeslaw; Lukasiewicz, Jolanta

    2016-06-02

    Lipopolysaccharide (LPS, endotoxin) is a main surface antigen and virulence factor of Gram-negative bacteria. Regardless of the source of LPS, this molecule, isolated from the smooth forms of bacteria, is characterised by a general structural layout encompassing three regions: (i) an O-specific polysaccharide (O-PS) - a polymer of repeating oligosaccharide units, (ii) core oligosaccharide (OS), and (iii) the lipid A anchoring LPS in the outer membrane of the cell envelope of Gram-negative bacteria. Structural analysis usually requires degradation of LPS and further efficient separation of various poly- and oligosaccharide glycoforms. The hydrophilic interaction liquid chromatography (HILIC) was shown as an efficient technique for separation of labelled or native neutral and acidic glycans, glycopeptides, sialylated glycans, glycosylated and nonglycosylated peptides. Herein we adopted ZIC(®) (zwitterionic stationary phase covalently attached to porous silica)-HILIC technology in combination with electrospray ionisation mass spectrometry to separate different LPS-derived oligosaccharides. As a result three effective procedures have been developed: (i) to separate different core oligosaccharides of Escherichia coli R1 LOS, (ii) to separate RU-[Hep]-Kdo oligosaccharides from core OS glycoforms of Hafnia alvei PCM 1200 LPS, and (iii) to separate Hep and Kdo-containing mono, di-, tri- and tetrasaccharides of H. alvei PCM 1200 LPS. Moreover, some of developed analytical procedures were scaled to semi-preparative protocols and used to obtain highly-purified fractions of the interest in larger quantities required for future evaluation, analysis, and biological applications. Copyright © 2016 Elsevier Ltd. All rights reserved.

  15. A versatile cost-effective method for the analysis of fresh frozen tissue sections via matrix-assisted laser desorption/ionisation imaging mass spectrometry.

    Science.gov (United States)

    O'Rourke, Matthew B; Raymond, Benjamin B A; Djordjevic, Steven P; Padula, Matthew P

    2015-04-15

    There are currently multiple methods available for the preparation of fresh frozen tissue samples for analysis via matrix-assisted laser desorption/ionisation time-of-flight (MALDI-TOF) imaging mass spectrometry (IMS). Although these methods report excellent results, many are expensive automated approaches. With no published attempt to standardise less expensive manual processes, our work aims to provide a robust and repeatable method of sample preparation for MALDI-TOF-IMS that is applicable to a variety of tissue types, well explained, simple and cost effective. Fresh frozen tissue was sectioned at 12 µm and mounted onto liquid nitrocellulose coated slides, washed in a graded alcohol series and then mounted into a modified sublimation apparatus. Matrix is deposited onto the slide to achieve a desired coating of 0.2 mg/cm(2). Once coated, the slide is mounted into a custom-built vapor chamber and recrystallised with 50% acetonitrile (ACN), 0.1% trifluoroacetic acid (TFA) for 1 h at 37°C. The slide is then analysed using MALDI-IMS. We have successfully implemented this method for a host of tissue samples, including brain, liver, kidney and heart, with no variation in relative spectra or processing method required. When the protocol is followed correctly, sublimations and recrystallisations are highly predictable with limited variation between samples and a very low failure rate. Additional apparatuses can be easily constructed by following the included instructions, that perform as per specifications with no variation. We believe that we have described a complete protocol for MALDI-IMS that is easy to use and highly reproducible. The lack of expensive commercially available equipment makes this process very cheap with a relatively low initial outlay and our hope is that more laboratories will begin IMS-based avenues of research based on the work we have performed. Copyright © 2015 John Wiley & Sons, Ltd.

  16. Identification of organic pigments in tattoo inks and permanent make-up using laser desorption ionisation mass spectrometry [version 2; referees: 2 approved

    Directory of Open Access Journals (Sweden)

    Markus Niederer

    2018-01-01

    Full Text Available Nowadays, about 12% of the European and 20% of the US population are tattooed. Rising concerns regarding consumer safety, led to legal restrictions on tattoo and permanent make-up (PMU inks. Restrictions also include bans on certain colourants. Both ink types use organic pigments for colour-giving, plus inorganic pigments for white and black and colour tones. Pigments are only sparingly soluble in common solvents and occur as suspended particles in the ink matrix. Their detection and identification therefore pose a major challenge for laboratories involved in monitoring the legal compliance of tattoo inks and PMU. We overcame this challenge by developing a direct laser desorption ionisation time-of-flight mass spectrometry method, which included an easy sample clean up. The method proved to be capable of detecting and identifying organic pigments in almost all of the tested ink samples. Method validation and routine deployment during market surveys showed the method to be fit for purpose. Pigment screening of 396 tattoo inks and 55 PMU taken from the Swiss market between 2009 and 2017 lead to the following conclusions: Pigment variety is much greater in tattoo inks (18 than in PMU (10; four prohibited pigments (Pigment Green 7, Pigment Red 122, Pigment Violet 19 and 23 were found in both ink types; for PMU, these four pigments made up 12% of the pigment findings, compared to 32% for tattoo inks. Therefore, legal compliance of PMU was at a higher level. A comparison of pigments found with those declared on tattoo ink labels clearly showed that banned pigments are rarely declared, but rather masked by listing non present legal pigments and label forging; therefore, highlighting the urgency of widespread market controls.

  17. Matrix-assisted laser desorption/ionisation-time of flight mass spectrometry: rapid identification of bacteria isolated from patients with cystic fibrosis.

    Science.gov (United States)

    Baillie, S; Ireland, K; Warwick, S; Wareham, D; Wilks, M

    2013-01-01

    Despite extensive research into the diagnosis and management of cystic fibrosis (CF) over the past decades, sufferers still have a median life expectancy of less than 37 years. Respiratory tract infections have a significant role in increasing the morbidity and mortality of patients with CF via a progressive decline in lung function. Rapid identification of organisms recovered from CF sputum is necessary for effective management of respiratory tract infections; however, standard techniques of identification are slow, technically demanding and expensive. The aim of this study is to asses the suitability of matrix-assisted laser desorption/ionisation-time of flight mass spectrometry (MALDI-TOF MS) in identifying bacteria isolated from the respiratory tract of patients with CF, and is assessed by testing the accuracy of MALDI-TOF MS in identifying samples from a reference collection of rare CF strains in conjunction with comparing MALDI-TOF MS and standard techniques in identifying clinical isolates from sputum samples of CF patients. MALDI-TOF MS accurately identified 100% of isolates from the reference collection of rare CF pathogens (EuroCare CF collection). The isolate identification given by MALDI-TOF MS agreed with that given by standard techniques for 479/481 (99.6%) clinical isolates obtained from respiratory samples provided by patients with CE In two (0.4%) of 481 samples there was a discrepancy in identification between MALDI-TOF MS and standard techniques. One organism was identified as Pseudomonas aeruginosa by MALDI-TOF but could only be identified by the laboratory's standard methods as of the Pseudomonas genus. The second organism was identified as P. beteli by MALDI-TOF MS and Stenotrophomonas maltophilia by standard methods. This study shows that MALDI-TOF MS is superior to standard techniques in providing cheap, rapid and accurate identification of CF sputum isolates.

  18. Investigation of pyrrolizidine alkaloids including their respective N-oxides in selected food products available in Hong Kong by liquid chromatography electrospray ionisation mass spectrometry.

    Science.gov (United States)

    Chung, Stephen W C; Lam, Aaron C H

    2017-07-01

    This study determined the levels of pyrrolizidine alkaloids (PAs), including their respective N-oxides, in foodstuffs available in Hong Kong by liquid chromatography-electrospray ionisation tandem mass spectrometry. A total of 234 samples (48 food items) were collected randomly from a local market and analysed. About 50% of samples were found to contain detectable amount of PAs. Amongst the 48 food items, PAs were not detected in 11 food items, including barley flour, beef, cattle liver, pork, pig liver, chicken meat, chicken liver, milk, non-fermented tea, Melissa tea and linden tea. For those found to contain detectable PAs, the summed PA content ranged up to 11,000 µg kg-1. The highest sum of PA content among the 37 food items calculated with lower bound was cumin seed, then followed by oregano, tarragon and herbs de Provence with ranges of 2.5-11,000, 1.5-5100, 8.0-3300 and 18-1300 µg kg-1 respectively. Among the samples, the highest sum of PA content was detected in a cumin seed sample (11,000 µg kg-1), followed by an oregano (5100 µg kg-1), a tarragon (3300 µg kg-1) and a herbs de Provence (1300 µg kg-1). In general, the results of this study agreed well with other published results in peer-reviewed journals, except that the total PAs in honey and specific tea infusion in this study were comparatively lower.

  19. Use of matrix-assisted laser desorption/ionisation-time of flight mass spectrometry analyser in a diagnostic microbiology laboratory in a developing country

    Directory of Open Access Journals (Sweden)

    Atang Bulane

    2017-02-01

    Full Text Available Background: Rapid and accurate identification of pathogens is of utmost importance for management of patients. Current identification relies on conventional phenotypic methods which are time consuming. Matrix-assisted laser desorption/ionisation-time of flight mass spectrometry (MALDI-TOF MS is based on proteomic profiling and allows for rapid identification of pathogens.Objective: We compared MALDI-TOF MS against two commercial systems, MicroScan Walkaway and VITEK 2 MS.Methods: Over a three-month period from July 2013 to September 2013, a total of 227 bacteria and yeasts were collected from an academic microbiology laboratory (N = 121; 87 Gramnegatives, seven Gram-positives, 27 yeasts and other laboratories (N = 106; 35 Gram-negatives, 34 Gram-positives, 37 yeasts. Sixty-five positive blood cultures were initially processed with Bruker Sepsityper kit for direct identification.Results: From the 65 blood culture bottles, four grew more than one bacterial pathogen and MALDI-TOF MS identified only one isolate. The blood cultures yielded 21 Gram-negatives, 43 Gram-positives and one Candida. There were 21 Escherirchia coli isolates which were reported by the MALDI-TOF MS as E. coli/Shigella. Of the total 292 isolates, discrepant results were found for one bacterial and three yeast isolates. Discrepant results were resolved by testing with the API system with MALDI-TOF MS showing 100% correlation.Conclusion: The MALDI-TOF MS proved to be very useful for rapid and reliable identification of bacteria and yeasts directly from blood cultures and after culture of other specimens. The difference in time to identification was significant for all isolates. However, for positive blood cultures with minimal sample preparation time there was a massive difference in turn-around time with great appreciation by clinicians.

  20. Positron impact ionisation studies

    CERN Document Server

    Kara, V

    1999-01-01

    impact ionisation of H. The total ionisation cross section (sigma sub T sup +), including contributions from both direct ionisation and Ps formation, was measured by extracting ions randomly. The Ps formation cross section (sigma sub P sub s) of H was then determined from these measurements by subtraction of sigma sub i sup + data. Two recent theoretical calculations, generally considered to be the most reliable thus far, are found to be in agreement with the results for sigma sub P sub s over the entire energy range investigated. The present measurements also differentiate between two prior conflicting measurements of sigma sub P sub s , thus providing a degree of consensus amongst experimental data. In this work, a magnetically confined e beam was crossed with a gas jet to study ionisation of Ne, Kr and Xe atoms. Ions produced in the overlap of the beams were detected in coincidence with the scattered projectile, so as to discriminate against ionisation events involving positronium (Ps) formation. The singl...

  1. Identification of prenylated pterocarpans and other isoflavonoids in Rhizopus spp. elicited soya bean seedlings by electrospray ionisation mass spectrometry.

    Science.gov (United States)

    Simons, Rudy; Vincken, Jean-Paul; Bohin, Maxime C; Kuijpers, Tomas F M; Verbruggen, Marian A; Gruppen, Harry

    2011-01-15

    Phytoalexins from soya are mainly characterised as prenylated pterocarpans, the glyceollins. Extracts of non-soaked and soaked soya beans, as well as that of soya seedlings, grown in the presence of Rhizopus microsporus var. oryzae, were screened for the presence of prenylated flavonoids with a liquid chromatography/mass spectrometry (LC/MS)-based screening method. The glyceollins I-III and glyceollidins I-II, belonging to the isoflavonoid subclass of the pterocarpans, were tentatively assigned. The formation of these prenylated pterocarpans was accompanied by that of other prenylated isoflavonoids of the subclasses of the isoflavones and the coumestans. It was estimated that approx. 40% of the total isoflavonoid content in Rhizopus-challenged soya bean seedlings were prenylated pterocarpans, whereas 7% comprised prenylated isoflavones and prenylated coumestans. The site of prenylation (A-ring or B-ring) of the prenylated isoflavones was tentatively annotated using positive-ion mode MS by comparing the (1,3) A(+) retro-Diels-Alder (RDA) fragments of prenylated and non-prenylated isoflavones. Furthermore, the fragmentation pathways of the five pterocarpans in negative-ion (NI) mode were proposed, which involved the cleavage of the C-ring and/or D-ring. The absence of the ring-closed prenyl (pyran or furan) gave exclusively -H(2) O(x,y) RDA fragments, whereas its presence gave predominantly the common RDA fragments. Copyright © 2010 John Wiley & Sons, Ltd.

  2. Fast gas chromatographic residue analysis in animal feed using split injection and atmospheric pressure chemical ionisation tandem mass spectrometry.

    Science.gov (United States)

    Tienstra, M; Portolés, T; Hernández, F; Mol, J G J

    2015-11-27

    Significant speed improvement for instrumental runtime would make GC–MS much more attractive for determination of pesticides and contaminants and as complementary technique to LC–MS. This was the trigger to develop a fast method (time between injections less than 10 min) for the determination of pesticides and PCBs that are not (or less) amenable to LC–MS. A key factor in achieving shorter analysis time was the use of split injection (1:10) which allowed the use of a much higher initial GC oven temperature. A shorter column (15 m), higher temperature ramp, and higher carrier gas flow rate (6 mL/min) further contributed to analysis-time reduction. Chromatographic resolution was slightly compromised but still well fit-for-purpose. Due to the high sensitivity of the technique used (GC–APCI-triple quadrupole MS/MS), quantification and identification were still possible down to the 10 μg/kg level, which was demonstrated by successful validation of the method for complex feed matrices according to EU guidelines. Other advantages of the method included a better compatibility of acetonitrile extracts (e.g. QuEChERS) with GC, and a reduced transfer of co-extractants into the GC column and mass spectrometer.

  3. Rapid identification of Burkholderia mallei and Burkholderia pseudomallei by intact cell Matrix-assisted Laser Desorption/Ionisation mass spectrometric typing

    Science.gov (United States)

    2012-01-01

    Background Burkholderia (B.) pseudomallei and B. mallei are genetically closely related species. B. pseudomallei causes melioidosis in humans and animals, whereas B. mallei is the causative agent of glanders in equines and rarely also in humans. Both agents have been classified by the CDC as priority category B biological agents. Rapid identification is crucial, because both agents are intrinsically resistant to many antibiotics. Matrix-assisted laser desorption/ionisation mass spectrometry (MALDI-TOF MS) has the potential of rapid and reliable identification of pathogens, but is limited by the availability of a database containing validated reference spectra. The aim of this study was to evaluate the use of MALDI-TOF MS for the rapid and reliable identification and differentiation of B. pseudomallei and B. mallei and to build up a reliable reference database for both organisms. Results A collection of ten B. pseudomallei and seventeen B. mallei strains was used to generate a library of reference spectra. Samples of both species could be identified by MALDI-TOF MS, if a dedicated subset of the reference spectra library was used. In comparison with samples representing B. mallei, higher genetic diversity among B. pseudomallei was reflected in the higher average Eucledian distances between the mass spectra and a broader range of identification score values obtained with commercial software for the identification of microorganisms. The type strain of B. pseudomallei (ATCC 23343) was isolated decades ago and is outstanding in the spectrum-based dendrograms probably due to massive methylations as indicated by two intensive series of mass increments of 14 Da specifically and reproducibly found in the spectra of this strain. Conclusions Handling of pathogens under BSL 3 conditions is dangerous and cumbersome but can be minimized by inactivation of bacteria with ethanol, subsequent protein extraction under BSL 1 conditions and MALDI-TOF MS analysis being faster than

  4. Rapid identification of Burkholderia mallei and Burkholderia pseudomallei by intact cell Matrix-assisted Laser Desorption/Ionisation mass spectrometric typing.

    Science.gov (United States)

    Karger, Axel; Stock, Rüdiger; Ziller, Mario; Elschner, Mandy C; Bettin, Barbara; Melzer, Falk; Maier, Thomas; Kostrzewa, Markus; Scholz, Holger C; Neubauer, Heinrich; Tomaso, Herbert

    2012-10-10

    Burkholderia (B.) pseudomallei and B. mallei are genetically closely related species. B. pseudomallei causes melioidosis in humans and animals, whereas B. mallei is the causative agent of glanders in equines and rarely also in humans. Both agents have been classified by the CDC as priority category B biological agents. Rapid identification is crucial, because both agents are intrinsically resistant to many antibiotics. Matrix-assisted laser desorption/ionisation mass spectrometry (MALDI-TOF MS) has the potential of rapid and reliable identification of pathogens, but is limited by the availability of a database containing validated reference spectra. The aim of this study was to evaluate the use of MALDI-TOF MS for the rapid and reliable identification and differentiation of B. pseudomallei and B. mallei and to build up a reliable reference database for both organisms. A collection of ten B. pseudomallei and seventeen B. mallei strains was used to generate a library of reference spectra. Samples of both species could be identified by MALDI-TOF MS, if a dedicated subset of the reference spectra library was used. In comparison with samples representing B. mallei, higher genetic diversity among B. pseudomallei was reflected in the higher average Eucledian distances between the mass spectra and a broader range of identification score values obtained with commercial software for the identification of microorganisms. The type strain of B. pseudomallei (ATCC 23343) was isolated decades ago and is outstanding in the spectrum-based dendrograms probably due to massive methylations as indicated by two intensive series of mass increments of 14 Da specifically and reproducibly found in the spectra of this strain. Handling of pathogens under BSL 3 conditions is dangerous and cumbersome but can be minimized by inactivation of bacteria with ethanol, subsequent protein extraction under BSL 1 conditions and MALDI-TOF MS analysis being faster than nucleic amplification methods. Our

  5. Rapid identification of Burkholderia mallei and Burkholderia pseudomallei by intact cell Matrix-assisted Laser Desorption/Ionisation mass spectrometric typing

    Directory of Open Access Journals (Sweden)

    Karger Axel

    2012-10-01

    Full Text Available Abstract Background Burkholderia (B. pseudomallei and B. mallei are genetically closely related species. B. pseudomallei causes melioidosis in humans and animals, whereas B. mallei is the causative agent of glanders in equines and rarely also in humans. Both agents have been classified by the CDC as priority category B biological agents. Rapid identification is crucial, because both agents are intrinsically resistant to many antibiotics. Matrix-assisted laser desorption/ionisation mass spectrometry (MALDI-TOF MS has the potential of rapid and reliable identification of pathogens, but is limited by the availability of a database containing validated reference spectra. The aim of this study was to evaluate the use of MALDI-TOF MS for the rapid and reliable identification and differentiation of B. pseudomallei and B. mallei and to build up a reliable reference database for both organisms. Results A collection of ten B. pseudomallei and seventeen B. mallei strains was used to generate a library of reference spectra. Samples of both species could be identified by MALDI-TOF MS, if a dedicated subset of the reference spectra library was used. In comparison with samples representing B. mallei, higher genetic diversity among B. pseudomallei was reflected in the higher average Eucledian distances between the mass spectra and a broader range of identification score values obtained with commercial software for the identification of microorganisms. The type strain of B. pseudomallei (ATCC 23343 was isolated decades ago and is outstanding in the spectrum-based dendrograms probably due to massive methylations as indicated by two intensive series of mass increments of 14 Da specifically and reproducibly found in the spectra of this strain. Conclusions Handling of pathogens under BSL 3 conditions is dangerous and cumbersome but can be minimized by inactivation of bacteria with ethanol, subsequent protein extraction under BSL 1 conditions and MALDI-TOF MS

  6. Rapid evaporative ionisation mass spectrometry of electrosurgical vapours for the identification of breast pathology: towards an intelligent knife for breast cancer surgery.

    Science.gov (United States)

    St John, Edward R; Balog, Julia; McKenzie, James S; Rossi, Merja; Covington, April; Muirhead, Laura; Bodai, Zsolt; Rosini, Francesca; Speller, Abigail V M; Shousha, Sami; Ramakrishnan, Rathi; Darzi, Ara; Takats, Zoltan; Leff, Daniel R

    2017-05-23

    Re-operation for positive resection margins following breast-conserving surgery occurs frequently (average = 20-25%), is cost-inefficient, and leads to physical and psychological morbidity. Current margin assessment techniques are slow and labour intensive. Rapid evaporative ionisation mass spectrometry (REIMS) rapidly identifies dissected tissues by determination of tissue structural lipid profiles through on-line chemical analysis of electrosurgical aerosol toward real-time margin assessment. Electrosurgical aerosol produced from ex-vivo and in-vivo breast samples was aspirated into a mass spectrometer (MS) using a monopolar hand-piece. Tissue identification results obtained by multivariate statistical analysis of MS data were validated by histopathology. Ex-vivo classification models were constructed from a mass spectral database of normal and tumour breast samples. Univariate and tandem MS analysis of significant peaks was conducted to identify biochemical differences between normal and cancerous tissues. An ex-vivo classification model was used in combination with bespoke recognition software, as an intelligent knife (iKnife), to predict the diagnosis for an ex-vivo validation set. Intraoperative REIMS data were acquired during breast surgery and time-synchronized to operative videos. A classification model using histologically validated spectral data acquired from 932 sampling points in normal tissue and 226 in tumour tissue provided 93.4% sensitivity and 94.9% specificity. Tandem MS identified 63 phospholipids and 6 triglyceride species responsible for 24 spectral differences between tissue types. iKnife recognition accuracy with 260 newly acquired fresh and frozen breast tissue specimens (normal n = 161, tumour n = 99) provided sensitivity of 90.9% and specificity of 98.8%. The ex-vivo and intra-operative method produced visually comparable high intensity spectra. iKnife interpretation of intra-operative electrosurgical vapours, including data

  7. Comprehensive chemical comparison of fuel composition and aerosol particles emitted from a ship diesel engine by gas chromatography atmospheric pressure chemical ionisation ultra-high resolution mass spectrometry with improved data processing routines.

    Science.gov (United States)

    Rüger, Christopher P; Schwemer, Theo; Sklorz, Martin; O'Connor, Peter B; Barrow, Mark P; Zimmermann, Ralf

    2017-02-01

    The analysis of petrochemical materials and particulate matter originating from combustion sources remains a challenging task for instrumental analytical techniques. A detailed chemical characterisation is essential for addressing health and environmental effects. Sophisticated instrumentation, such as mass spectrometry coupled with chromatographic separation, is capable of a comprehensive characterisation, but needs advanced data processing methods. In this study, we present an improved data processing routine for the mass chromatogram obtained from gas chromatography hyphenated to atmospheric pressure chemical ionisation and ultra high resolution mass spectrometry. The focus of the investigation was the primary combustion aerosol samples, i.e. particulate matter extracts, as well as the corresponding fossil fuels fed to the engine. We demonstrate that utilisation of the entire transient and chromatographic information results in advantages including minimisation of ionisation artefacts and a reliable peak assignment. A comprehensive comparison of the aerosol and the feed fuel was performed by applying intensity weighted average values, compound class distribution and principle component analysis. Certain differences between the aerosol generated with the two feed fuels, diesel fuel and heavy fuel oil, as well as between the aerosol and the feed were revealed. For the aerosol from heavy fuel oil, oxidised species from the CHN and CHS class precursors of the feed were predominant, whereas the CHOx class is predominant in the combustion aerosol from light fuel oil. Furthermore, the complexity of the aerosol increases significantly compared to the feed and incorporating a higher chemical space. Coupling of atmospheric pressure chemical ionisation to gas chromatography was found to be a useful additional approach for characterisation of a combustion aerosol, especially with an automated utilisation of the information from the ultra-high resolution mass spectrometer

  8. Sensitive monitoring of monoterpene metabolites in human urine using two-step derivatisation and positive chemical ionisation-tandem mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Schmidt, Lukas [Institute and Outpatient Clinic of Occupational, Social and Environmental Medicine, University of Erlangen-Nuremberg, Schillerstrasse 25/29, 91054 Erlangen (Germany); Belov, Vladimir N. [Max Planck Institute for Biophysical Chemistry, Facility for Synthetic Chemistry, Am Fassberg 11, 37077 Göttingen (Germany); Göen, Thomas, E-mail: Thomas.Goeen@ipasum.med.uni-erlangen.de [Institute and Outpatient Clinic of Occupational, Social and Environmental Medicine, University of Erlangen-Nuremberg, Schillerstrasse 25/29, 91054 Erlangen (Germany)

    2013-09-02

    Highlights: •Sensitive monitoring of 10 metabolites of (R)-limonene, α-pinene, and Δ{sup 3}-carene in human urine samples. •Fast and simple sample preparation and derivatisation procedure using two-step silylation for unreactive tertiary hydroxyl groups. •Synthesis of reference substances and isotopically labelled internal standards of (R)-limonene, α-pinene, and Δ{sup 3}-carene metabolites. •Study on (R)-limonene, α-pinene, and Δ{sup 3}-carene metabolite background exposure of 36 occupationally unexposed volunteers. -- Abstract: A gas chromatographic–positive chemical ionisation-tandem mass spectrometric (GC–PCI-MS/MS) method for the simultaneous determination of 10 oxidative metabolites of the monoterpenoid hydrocarbons α-pinene, (R)-limonene, and Δ{sup 3}-carene ((+)-3-carene) in human urine was developed and tested for the monoterpene biomonitoring of the general population (n = 36). The method involves enzymatic cleavage of the glucuronides followed by solid-supported liquid–liquid extraction and derivatisation using a two-step reaction with N,O-bis(trimethylsilyl)-trifluoroacetamide and N-(trimethylsilyl)imidazole. The method proved to be both sensitive and reliable with detection limits ranging from 0.1 to 0.3 μg L{sup −1}. In contrast to the frequent and distinct quantities of (1S,2S,4R)-limonene-1,2-diol, the (1R,2R,4R)-stereoisomer could not be detected. The expected metabolite of (+)-3-carene, 3-caren-10-ol was not detected in any of the samples. All other metabolites were detected in almost all urine samples. The procedure enables for the first time the analysis of trace levels of a broad spectrum of mono- and bicyclic monoterpenoid metabolites (alcohols, diols, and carboxylic acids) in human urine. This analytical procedure is a powerful tool for population studies as well as for the discovery of human metabolism and toxicokinetics of monoterpenes.

  9. Determination of N-nitrosamines in processed meats by liquid extraction combined with gas chromatography-methanol chemical ionisation/mass spectrometry.

    Science.gov (United States)

    Scheeren, Marina Bergoli; Sabik, Hassan; Gariépy, Claude; Terra, Nelcindo Nascimento; Arul, Joseph

    2015-01-01

    A simple, accessible and reproducible method was developed and validated as an alternative for the determination of nine volatile N-nitrosamines (NAs) in meat products, using a low volume of organic solvent and without requiring specific apparatus, offering the possibility of practical implementation in routine laboratories. The NAs were extracted with dichloromethane followed by a clean-up with phosphate buffer solution (pH 7.0). The extracts were analysed by gas chromatography-chemical ionisation/mass spectrometry (GC-CI/MS) in positive-ion mode using methanol as reagent. Limits of detection and quantification, recovery and reproducibility were determined for all NAs (N-nitrosodimethylamine, N-nitrosomethylethylamine, N-nitrosodiethylamine, N-nitrosopyrrolidine, N-nitrosodipropylamine, N-nitrosomorpholine, N-nitrosopiperidine, N-nitrosodibutylamine and N-nitrosodiphenylamine). Satisfactory sensitivity and selectivity were obtained even without concentrating the extract by solvent evaporation, avoiding the loss of the nine NAs studied. Limits of detection ranged from 0.15 to 0.37 µg kg(-1), whereas limits of quantification ranged from 0.50 to 1.24 µg kg(-1). Recoveries calculated in cooked ham that had been spiked at 10 and 100 µg kg(-1) were found to be between 70% and 114% with an average relative standard deviation of 13.2%. The method was successfully used to analyse five samples of processed meat products on the day of purchase and 7 days later (after storage at 4°C). The most abundant NAs found in the analysed products were N-nitrosodipropylamine and N-nitrosopiperidine, which ranged from 1.75 to 34.75 µg kg(-1) and from 1.50 to 4.26 µg kg(-1), respectively. In general, an increase in the level of NAs was observed after the storage period. The proposed method may therefore be a useful tool for food safety control once it allows assessing the profile and the dietary intake of NAs in food over time.

  10. The use of enzyme-coupled magnetic nanoparticles for studying the spectra of unusual substrates of mushroom tyrosinase by direct surface-assisted laser desorption/ionisation and high-resolution electrospray ionisation quadrupole-quadrupole-time-of-flight mass spectrometry.

    Science.gov (United States)

    Salwiński, Aleksander; Da Silva, David; Delépée, Raphaël; Maunit, Benoît

    2014-09-30

    Tyrosinase-coupled magnetic particles (EMPs) were used to demonstrate that resorcinol-containing tyrosinase inhibitors are oxidised by tyrosinase only in the presence of the enzyme's classic substrate. This shows the potential for the application of EMPs as a non-organic matrix for monitoring enzymatic conversion of a novel substrate family directly on-the-spot, principally due to minimal enzyme requirement per analysis. Tyrosinase was covalently coupled to core-shell-type silica-coated iron oxide magnetic nanoparticles (EMPs) that were applied as non-organic SALDI matrix suitable for studying low-mass compounds using a classic matrix-assisted laser desorption/ionisation time-of-flight (MALDI-TOF) mass spectrometer. Because of the dual function of the EMPs - enzyme host and non-organic matrix - we describe this ionisation method as Enzyme-coupled Nanoparticles-Assisted LDI-MS (ENALDI-MS). Supplementary studies of the enzymatic conversion of glabridin and 3-(2,4-dihydroxyphenyl)propionic acid (DHPA) were conducted by high-resolution electrospray ionisation quadrupole-quadrupole-time-of-flight mass spectrometry (ESI-QqTOF-MS). The initial experiment involving EMPs as non-organic matrix (ENALDI-MS) showed enzymatic conversion of glabridin, a strong tyrosinase inhibitor, only in the presence of L-Tyr, the classic tyrosinase substrate. These findings were evaluated by ESI-QqTOF-MS proving that glabridin and DHPA are converted into the corresponding quinones by tyrosinase only in the presence of the auxiliary monophenol or o-diphenol substrates (L-Tyr and catechin, respectively) capable of regenerating the active site of tyrosinase. EMPs were shown to be useful as a non-organic matrix to monitor enzymatic conversion of the novel tyrosinase substrate family directly on-the-spot with a minimal enzyme consumption (6.5 pmol/spot). Results obtained by ENALDI-MS were fully confirmed by ESI-QqTOF-MS demonstrating that resorcinol-containing tyrosinase inhibitors may be oxidised

  11. Determination and separation of bisphenol A, phthalate metabolites and structural isomers of parabens in human urine with conventional high-pressure liquid chromatography combined with electrospray ionisation tandem mass spectrometry.

    Science.gov (United States)

    Myridakis, Antonis; Balaska, Eirini; Gkaitatzi, Christina; Kouvarakis, Antonis; Stephanou, Euripides G

    2015-03-01

    Phthalates, bisphenol A (BPA) and parabens (PBs), organic chemicals widely used in everyday products, are considered to be endocrine disruptors. We propose a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the determination of seven phthalate metabolites, six PBs and BPA in human urine. All three categories of the above endocrine disruptors were simultaneously extracted from 1 mL of human urine using solid phase extraction. In addition, with a conventional reversed phase LC column, we achieved for the first time the separation of three pairs of structural isomers, namely iso-/n-butyl paraben, propyl paraben and monobutyl phthalate. LC-MS/MS was operated and tested in both electrospray ionisation (ESI) and atmospheric pressure chemical ionisation (APCI). ESI was selected for the analysis due to its superior stability and repeatability. The method limit of detection (mLOD), achieved for a single set of high-performance LC conditions, ranged from 0.01 to 0.84 ng/mL for phthalate metabolites, from 0.06 to 0.24 ng/mL for PBs and was 2.01 ng/mL for BPA. Derivatisation of BPA with dansyl chloride lowered its mLOD to 0.007 ng/mL. Blank contamination was non-detectable. The present method was successfully applied for the analysis of the above-mentioned compounds in 80 male human urine samples.

  12. Real-time analysis of aromatics in combustion engine exhaust by resonance-enhanced multiphoton ionisation time-of-flight mass spectrometry (REMPI-TOF-MS): a robust tool for chassis dynamometer testing

    Energy Technology Data Exchange (ETDEWEB)

    Adam, T.W. [European Commission Joint Research Centre, Institute for Environment and Sustainability, Transport and Air Quality Unit, Ispra, VA (Italy); Clairotte, M.; Manfredi, U.; Carriero, M.; Martini, G.; Krasenbrink, A.; Astorga, C. [European Commission Joint Research Centre, Institute for Environment and Sustainability, Transport and Air Quality Unit, Ispra, VA (Italy); European Commission Joint Research Centre, Institute for Energy and Transport, Sustainable Transport Unit, Ispra, Varese (Italy); Streibel, T.; Pommeres, A.; Sklorz, M. [University of Rostock, Analytical Chemistry/Joint Mass Spectrometry Centre, Institute of Chemistry, Rostock (Germany); Elsasser, M.; Zimmermann, R. [Cooperation Group Complex Molecular Systems (CMA)/Joint Mass Spectrometry Centre (JMSC), Neuherberg (Germany); University of Rostock, Analytical Chemistry/Joint Mass Spectrometry Centre, Institute of Chemistry, Rostock (Germany)

    2012-07-15

    Resonance-enhanced multiphoton ionisation time-of-flight mass spectrometry (REMPI-TOF-MS) is a robust method for real-time analysis of monocyclic and polycyclic aromatic hydrocarbons in complex emissions. A mobile system has been developed which enables direct analysis on site. In this paper, we utilize a multicomponent calibration scheme based on the analytes' photo-ionisation cross-sections relative to a calibrated species. This allows semi-quantification of a great number of components by only calibrating one compound of choice, here toluene. The cross-sections were determined by injecting nebulised solutions of aromatic compounds into the TOF-MS ion source with the help of a HPLC pump. Then, REMPI-TOF-MS was implemented at various chassis dynamometers and test cells and the exhaust of the following vehicles and engines investigated: a compression ignition light-duty (LD) passenger car, a compression ignition LD van, two spark ignition LD passenger cars, 2 two-stroke mopeds, and a two-stroke engine of a string gas trimmer. The quantitative time profiles of benzene are shown. The results indicate that two-stroke engines are a significant source for toxic and cancerogenic compounds. Air pollution and health effects caused by gardening equipment might still be underestimated. (orig.)

  13. The Effect of Thermal Mass on Annual Heat Load and Thermal Comfort in Cold Climate Construction

    DEFF Research Database (Denmark)

    Stevens, Vanessa; Kotol, Martin; Grunau, Bruno

    2016-01-01

    Thermal mass in building construction refers to a building material's ability to absorb and release heat based on changing environmental conditions. In building design, materials with high thermal mass used in climates with a diurnal temperature swing around the interior set-point temperature have...... been shown to reduce the annual heating demand. However, few studies exist regarding the effects of thermal mass in cold climates. The purpose of this research is to determine the effect of high thermal mass on the annual heat demand and thermal comfort in a typical Alaskan residence using energy...... that while increased thermal mass does have advantages in all climates, such as a decrease in summer overheating, it is not an effective strategy for decreasing annual heat demand in typical residential buildings in Alaska. (C) 2015 American Society of Civil Engineers....

  14. Isotopic abundance measurements of K and Ca using a wide-dispersion multi-collector mass spectrometer and low-fractionation ionisation techniques

    Science.gov (United States)

    Fletcher, I. R.; Maggi, A. L.; Rosman, K. J. R.; McNaughton, N. J.

    1997-04-01

    Procedures have been established for routine high-precision isotopic analyses of all aspects of the K-Ca isotopic system, for virtually any natural sample, using a set of 40K + 43Ca + 46Ca spikes and a VG354 (Multi-II) mass spectrometer. Loading samples as KI and CaI2 on triple (or double) filament arrays results in reduced mass fractionation, approximately as expected from Rayleigh distillation theory. For K, this improves the fractionation (or 41K anomaly) detection limit to ~0.8[per mille sign]/amu for single analyses. For Ca, the reduced fractionation renders data insensitive to the choice of fractionation law used for internal corrections. The 2[sigma] reproducibility of normalised 40Ca/44Ca data (expressed as [epsilon]Ca) is ~4, approximately twice the theoretical limits, but for measurements of natural fractionation ([delta]44/42Ca) it is ~0.4[per mille sign], about five times theoretical. These measurement procedures yield an atomic weight for the Ca standard which is consistent with the IUPAC value, and provide strong support for a reduced uncertainty (by a factor of two). A value of 40.078 ± 0.002 would include all known isotopic fractionations in natural and commercial materials. Analyses of four Nerita marine mollusc samples from a wide geographic (and water temperature) range failed to detect any thermally controlled Ca isotope fractionation ([delta]44/42Ca) corresponding to the observed [delta]18O variations.

  15. Thermal /Soret/ diffusion effects on interfacial mass transport rates

    Science.gov (United States)

    Rosner, D. E.

    1980-01-01

    It is shown that thermal (Soret) diffusion significantly alters convective mass transport rates and important transition temperatures in highly nonisothermal flow systems involving the transport of 'heavy' species (vapors or particles). Introduction of the Soret transport term is shown to result in mass transfer effects similar to those of 'suction' and a homogeneous chemical 'sink'. It is pointed out that this analogy provides a simple method of correlating and predicting thermal diffusion effects in the abovementioned systems.

  16. Convective Concrete : Additive Manufacturing to facilitate activation of thermal mass

    NARCIS (Netherlands)

    de Witte, D.; de Klijn-Chevalerias, M.L.; Loonen, R.C.G.M.; Hensen, JLM; Knaack, U.; Zimmermann, G

    2017-01-01

    This paper reports on the research-driven design process of an innovative thermal mass concept: Convective Concrete. The goal is to improve building energy efficiency and comfort levels by addressing some of the shortcomings of conventional building slabs with high thermal storage capacity. Such

  17. Matrix-assisted laser desorption/ionisation time-of-flight (MALDI-TOF) mass spectrometry as a tool for rapid diagnosis of potentially toxigenic Corynebacterium species in the laboratory management of diphtheria-associated bacteria.

    Science.gov (United States)

    Konrad, R; Berger, A; Huber, I; Boschert, V; Hörmansdorfer, S; Busch, U; Hogardt, M; Schubert, S; Sing, A

    2010-10-28

    The rapid identification of the potentially toxigenic Corynebacterium species, C. diphtheriae, C. ulcerans and C. pseudotuberculosis is essential for diagnosis and treatment of diphtheria and diphtheria-like diseases. We used matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry (MALDIT-OF MS) in comparison with classical microbiological and molecular methods on 116 Corynebacterium strains. All 90 potentially toxigenic Corynebacterium strains collected by the German National Consiliary Laboratory on Diphtheria in a period of more than ten years were correctly identified by MALDI-TOF MS. We propose an algorithm for fast and reliable diagnosis of diphtheria incorporating MALDI-TOF MS, real-time tox PCR and Elek testing.

  18. Late Periprosthetic Joint Infection due to Staphylococcus lugdunensis Identified by Matrix-Assisted Laser Desorption/Ionisation Time of Flight Mass Spectrometry: A Case Report and Review of the Literature

    Science.gov (United States)

    Szabados, Florian; Anders, Agnes; Kaase, Martin; Marlinghaus, Lennart; Gatermann, Sören G.; Teske, Wolfram; Lichtinger, Thomas

    2011-01-01

    Staphylococcus lugdunensis, member to the group of coagulase-negative staphylococci, is previously thought to be rarely isolated. Recently other staphylococci have been described, which were supposedly related to S. lugdunensis, such as Staphylococcus pseudolugdunensis and Staphylococcus pettenkoferi. To decrease the rate misidentifications, an accurate identification method, such as matrix-assisted laser desorption ionization time of flight mass spectrometry or molecular methods, should be used. S. lugdunensis is usually associated with severe infections similar to those caused by S. aureus. Moreover, it has been described that skin infections due to S. lugdunensis are severely underreported and could be also underreported in periprosthetic joint infections. Ours is the first case of a late periprosthetic infection of the hip due to S. lugdunensis, identified by matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry. A periprosthetic infection due to S. lugdunensis should be treated according to protocols of S. aureus periprosthetic infections, and therefore an accurate species identification is desirable. PMID:21776276

  19. Thermal mass impact on energy performance of a low, medium and heavy mass building in Belgrade

    Directory of Open Access Journals (Sweden)

    Anđelković Bojan V.

    2012-01-01

    Full Text Available Heavy mass materials used in building structures and architecture can significantly affect building energy performance and occupant comfort. The purpose of this study was to investigate if thermal mass can improve the internal environment of a building, resulting in lower energy requirements from the mechanical systems. The study was focused on passive building energy performance and compared annual space heating and cooling energy requirements for an office building in Belgrade with several different applications of thermal mass. A three-dimensional building model was generated to represent a typical office building. Building shape, orientation, glazing to wall ratio, envelope insulation thickness, and indoor design conditions were held constant while location and thickness of building mass (concrete was varied between cases in a series of energy simulations. The results were compared and discussed in terms of the building space heating and cooling energy and demand affected by thermal mass. The simulation results indicated that with addition of thermal mass to the building envelope and structure: 100% of all simulated cases experienced reduced annual space heating energy requirements, 67% of all simulated cases experienced reduced annual space cooling energy requirements, 83% of all simulated cases experienced reduced peak space heating demand and 50% of all simulated cases experienced reduced peak space cooling demand. The study demonstrated that there exists a potential for reducing space heating and cooling energy requirements with heavy mass construction in the analyzed climate region (Belgrade, Serbia.

  20. Screening ionisation and chromatography conditions for quantitative LC/MS methods.

    Science.gov (United States)

    Sillén, Henrik; Magnell, Niklas

    2009-11-01

    To develop an optimal quantitative LC/MS method with high sensitivity, high selectivity and robustness in a limited time period can be very challenging, especially for methods in which many analytes are to be quantified. In this study the relevant options are reviewed and a simple screening strategy of mass spectrometric and chromatographic conditions is presented. The strategy is divided into two stages, mass spectrometric ionisation screening and reversed phase LC column screening. The objective of the first stage is to find out how sensitivity is affected by ionisation technique, ionisation polarity and buffer. The compounds are dissolved in different buffers covering a broad pH range. Thereafter they are injected using flow injection analysis without LC column, evaluating both electrospray and atmospheric pressure chemical ionisation (APCI). In the second stage the buffers yielding the best sensitivity and selectivity in the ionisation screening stage are used as mobile phase buffers to LC column screening with different stationary phases applying a shallow gradient. The aim is to find the combinations of column(s) and buffer(s) that give symmetric peaks, adequate retention and selectivity. Finally the retention is adjusted using isocratic or gradient elution. The strategy provides a simple and practical experimental design that allows fast screening a large range of ionisation and chromatographic conditions especially for multiple compounds. The examples included in this study demonstrate that optimal buffer, ionisation technique, ionisation polarity and column cannot be predicted from compound properties such as structure and pK(a).

  1. Coorbital thermal torques on low-mass protoplanets

    Science.gov (United States)

    Masset, Frédéric S.

    2017-12-01

    Using linear perturbation theory, we investigate the torque exerted on a low-mass planet embedded in a gaseous protoplanetary disc with finite thermal diffusivity. When the planet does not release energy into the ambient disc, the main effect of thermal diffusion is the softening of the enthalpy peak near the planet, which results in the appearance of two cold and dense lobes on either side of the orbit, of size smaller than the thickness of the disc. The lobes exert torques of opposite sign on the planet, each comparable in magnitude to the one-sided Lindblad torque. When the planet is offset from corotation, the lobes are asymmetric and the planet experiences a net torque, the `cold' thermal torque, which has a magnitude that depends on the relative value of the distance to corotation to the size of the lobes {˜ }√{χ /Ω _p}, χ being the thermal diffusivity and Ωp the orbital frequency. We believe that this effect corresponds to the phenomenon named `cold finger' recently reported in numerical simulations, and we argue that it constitutes the dominant mode of migration of sub-Earth-mass objects. When the planet is luminous, the heat released into the ambient disc results in an additional disturbance that takes the form of hot, low-density lobes. They give a torque, named heating torque in previous work, that has an expression similar, but of opposite sign, to the cold thermal torque.

  2. An improved dispersive solid-phase extraction clean-up method for the gas chromatography-negative chemical ionisation tandem mass spectrometric determination of multiclass pesticide residues in edible oils.

    Science.gov (United States)

    Deme, Pragney; Azmeera, Tirupathi; Prabhavathi Devi, B L A; Jonnalagadda, Padmaja R; Prasad, R B N; Vijaya Sarathi, U V R

    2014-01-01

    An improved sample preparation using dispersive solid-phase extraction clean-up was proposed for the trace level determination of 35 multiclass pesticide residues (organochlorine, organophosphorus and synthetic pyrethroids) in edible oils. Quantification of the analytes was carried out by gas chromatography-mass spectrometry in negative chemical ionisation mode (GC-NCI-MS/MS). The limit of detection and limit of quantification of residues were in the range of 0.01-1ng/g and 0.05-2ng/g, respectively. The analytes showed recoveries between 62% and 110%, and the matrix effect was observed to be less than 25% for most of the pesticides. Crude edible oil samples showed endosulfan isomers, p,p'-DDD, α-cypermethrin, chlorpyrifos, and diazinon residues in the range of 0.56-2.14ng/g. However, no pesticide residues in the detection range of the method were observed in refined oils. Copyright © 2013 Elsevier Ltd. All rights reserved.

  3. Comparison of phenotypic methods and matrix-assisted laser desorption ionisation time-of-flight mass spectrometry for the identification of aero-tolerant Actinomyces spp. isolated from soft-tissue infections.

    Science.gov (United States)

    Ng, L S Y; Sim, J H C; Eng, L C; Menon, S; Tan, T Y

    2012-08-01

    Aero-tolerant Actinomyces spp. are an under-recognised cause of cutaneous infections, in part because identification using conventional phenotypic methods is difficult and may be inaccurate. Matrix-assisted laser desorption ionisation time-of-flight mass spectrometry (MALDI-TOF MS) is a promising new technique for bacterial identification, but with limited data on the identification of aero-tolerant Actinomyces spp. This study evaluated the accuracy of a phenotypic biochemical kit, MALDI-TOF MS and genotypic identification methods for the identification of this problematic group of organisms. Thirty aero-tolerant Actinomyces spp. were isolated from soft-tissue infections over a 2-year period. Species identification was performed by 16 s rRNA sequencing and genotypic results were compared with results obtained by API Coryne and MALDI-TOF MS. There was poor agreement between API Coryne and genotypic identification, with only 33% of isolates correctly identified to the species level. MALDI-TOF MS correctly identified 97% of isolates to the species level, with 33% of identifications achieved with high confidence scores. MALDI-TOF MS is a promising new tool for the identification of aero-tolerant Actinomyces spp., but improvement of the database is required in order to increase the confidence level of identification.

  4. Modeling energy flexibility of low energy buildings utilizing thermal mass

    DEFF Research Database (Denmark)

    Foteinaki, Kyriaki; Heller, Alfred; Rode, Carsten

    2016-01-01

    In the future energy system a considerable increase in the penetration of renewable energy is expected, challenging the stability of the system, as both production and consumption will have fluctuating patterns. Hence, the concept of energy flexibility will be necessary in order for the consumption...... to match the production patterns, shifting demand from on-peak hours to off-peak hours. Buildings could act as flexibility suppliers to the energy system, through load shifting potential, provided that the large thermal mass of the building stock could be utilized for energy storage. In the present study...... the load shifting potential of an apartment of a low energy building in Copenhagen is assessed, utilizing the heat storage capacity of the thermal mass when the heating system is switched off for relieving the energy system. It is shown that when using a 4-hour preheating period before switching off...

  5. Characterisation of botulinum toxins type C, D, E, and F by matrix-assisted laser desorption ionisation and electrospray mass spectrometry

    NARCIS (Netherlands)

    Baar, B.L.M. van; Hulst, A.G.; Jong, A.L. de; Wils, E.R.J.

    2004-01-01

    In a follow-up of the earlier characterisation of botulinum toxins type A and B (BTxA and BTxB) by mass spectrometry (MS), types C, D, E, and F (BTxC, BTxD, BTxE, BTxF) were now investigated. Botulinum toxins are extremely neurotoxic bacterial toxins, likely to be used as biological warfare agent.

  6. Genotyping for Glycophorin GYP(B-A-B) Hybrid Genes Using a Single Nucleotide Polymorphism-Based Algorithm by Matrix-Assisted Laser Desorption/Ionisation, Time-of-Flight Mass Spectrometry.

    Science.gov (United States)

    Wei, Ling; Lopez, Genghis H; Ji, Yanli; Condon, Jennifer A; Irwin, Darryl L; Luo, Guangping; Hyland, Catherine A; Flower, Robert L

    2016-10-01

    The genetic basis for five GP(B-A-B) MNS system hybrid glycophorin blood group antigens results from rearrangement between the homologous GYPA and GYPB genes. Each hybrid glycophorin displays a characteristic profile of antigens. Currently, no commercial serological reagents are currently available to serologically type for these antigens. The aim of this study was to develop a single nucleotide polymorphism (SNP) mapping genotyping technique to allow characterisation of various GYP(B-A-B) hybrid alleles. Matrix-assisted laser desorption/ionisation time-of-flight (MALDI-TOF) mass spectrometry (MS) assays were designed to genotype five GYP(B-A-B) hybrid alleles. Eight nucleotide positions were targeted and incorporated into the SNP mapping protocol. The allelic frequencies were calculated using peak areas. Sanger sequencing was performed to resolve a GYP*Hop 3' breakpoint. Observed allelic peak area ratios either coincided with the expected ratio or were skewed (above or below) from the expected ratio with switching occurring at and after the expected break point to generate characteristic mass spectral plots for each hybrid. Sequencing showed that the GYP*Hop crossover in the intron 3 region, for this example, was identical to that for GYP*Bun reference sequence. An analytical algorithm using MALDI-TOF MS genotyping platform defined GYPA inserts for five GYP(B-A-B) hybrids. The SNP mapping technique described here demonstrates proof of concept that this technology is viable for genotyping hybrid glycophorins, GYP(A-B-A), GYP(A-B) and GYP(B-A), and addresses the gap in current typing technologies.

  7. On-line process monitoring of coffee roasting by resonant laser ionisation time-of-flight mass spectrometry: bridging the gap from industrial batch roasting to flavour formation inside an individual coffee bean.

    Science.gov (United States)

    Hertz-Schünemann, R; Dorfner, R; Yeretzian, C; Streibel, T; Zimmermann, R

    2013-12-01

    Resonance-enhanced multiphoton ionisation time-of-flight mass spectrometry (REMPI-TOFMS) enables the fast and sensitive on-line monitoring of volatile organic compounds (VOC) formed during coffee roasting. On the one hand, REMPI-TOFMS was applied to monitor roasting gases of an industrial roaster (1500 kg/h capacity), with the aim of determining the roast degree in real-time from the transient chemical signature of VOCs. On the other hand, a previously developed μ-probe sampling device was used to analyse roasting gases from individual coffee beans. The aim was to explore fundamental processes at the individual bean level and link these to phenomena at the batch level. The pioneering single-bean experiments were conducted in two configurations: (1) VOCs formed inside a bean were sampled in situ, i.e. via a drilled μ-hole, from the interior, using a μ-probe (inside). (2) VOCs were sampled on-line in close vicinity of a single coffee bean's surface (outside). The focus was on VOCs originating from hydrolysis and pyrolytic degradation of chlorogenic acids, like feruloyl quinic acid and caffeoyl quinic acid. The single bean experiments revealed interesting phenomena. First, differences in time-intensity profiles between inside versus outside (time shift of maximum) were observed and tentatively linked to the permeability of the bean's cell walls material. Second, sharp bursts of some VOCs were observed, while others did exhibit smooth release curves. It is believed that these reflect a direct observation of bean popping during roasting. Finally, discrimination between Coffea arabica and Coffea canephora was demonstrated based on high-mass volatile markers, exclusively present in spectra of Coffea arabica. Copyright © 2013 John Wiley & Sons, Ltd.

  8. Negative electrospray ionisation of fluorotelomer alcohols (FTOH) and FTOH-derived acrylate surfactants by liquid chromatography coupled to accurate (tandem) mass spectrometry

    DEFF Research Database (Denmark)

    Trier, Xenia; Christensen, Jan H.; Niessen, Wilfried M. A.

    Fluorotelomer alcohols (FTOHs) are used to synthesize fluorinated surfactants, which form bioaccumulative perfluorinated degradation products, which are toxic to humans and the environment. To facilitate screening for FTOH-derived surfactants by LC-ESI–-MS, we identified product ions of FTOHs, an......, and propose FTOH fragmentation pathways on two MS instruments. By extraction of FTOH basepeak ions from accurate mass spectra, homologues series of peaks showed up in an industrial blend of FTOH-derived fluoroacrylates used in food paper packaging....

  9. Chemical analysis of surfaces by resonance ionization mass spectroscopy associated to ionic pulverization; Analyse chimique de surfaces par spectrometrie d`ionisation resonante associee a la pulverisation ionique

    Energy Technology Data Exchange (ETDEWEB)

    Kern, P.

    1995-12-19

    This work shows that if resonance ionization mass spectroscopy was first applied in isotopic separation, it`s also an analyzing method adapted to the study of semi-conductor materials and thin foils. We have improved this technic: a neodymium laser coupled with a dye laser, a new argon ions gun, a gallium ions gun and a new collection optic for the secondary ions quadrupole spectrometer to allow quantitative and selective measurements. (S.G.). 84 refs.

  10. Characterization of polychlorinated n-alkanes using comprehensive two-dimensional gas chromatography--electron-capture negative ionisation time-of-flight mass spectrometry.

    Science.gov (United States)

    Korytár, P; Parera, J; Leonards, P E G; Santos, F J; de Boer, J; Brinkman, U A Th

    2005-09-09

    Comprehensive two-dimensional gas chromatography with electron-capture negative ionization time-of-flight mass spectrometry (GC x GC-ECNI-TOF-MS) is used to study the composition and characteristics of short-, medium- and long-chain polychlorinated n-alkane (PCA) mixtures. Distinct ordered structures, which enable the highlighting and interpretation of group and sub-group separations are observed when using a DB-1 x 007-65HT column combination. The analysis of a number of, mutually rather different, technical mixtures and 35 individual standard compounds provides information on the role of chlorine substitution (number of substituents as well as their position), the contribution of carbon versus chlorine atoms to analyte volatility, i.e. GC x GC behaviour, and the influence of the chain length of the carbon skeleton. Two dust samples are analyzed to illustrate the practical usefulness of the proposed procedure.

  11. Universal protocol for the rapid automated detection of carbapenem-resistant Gram-negative bacilli directly from blood cultures by matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry (MALDI-TOF/MS).

    Science.gov (United States)

    Oviaño, Marina; Sparbier, Katrin; Barba, Maria José; Kostrzewa, Markus; Bou, Germán

    2016-12-01

    Detection of carbapenemase-producing bacteria directly from blood cultures is a major challenge, as patients with bacteraemia are critically ill. Early detection can be helpful for selection of the most appropriate antibiotic therapy as well as adequate control of outbreaks. In the current study, a novel matrix-assisted laser desorption/ionisation time-of-flight (MALDI-TOF)-based method was developed for the rapid, automated detection of carbapenemase-producing Enterobacteriaceae, Pseudomonas aeruginosa and Acinetobacter baumannii directly from blood cultures. Carbapenemase activity was determined in 30 min by measuring hydrolysis of imipenem (0.31 mg/mL) in blood cultures spiked with a series of 119 previously characterised isolates, 81 of which carried a carbapenemase enzyme (10 blaKPC, 10 blaVIM, 10 blaNDM, 10 blaIMP, 26 blaOXA-48-type, 9 blaOXA-23, 1 blaOXA-237, 3 blaOXA-24 and 2 blaOXA-58). Twenty blood cultures obtained from bacteraemic patients carrying blaOXA-48-producing isolates were also analysed using the same protocol. Analysis was performed using MALDI-TOF Biotyper® Compass software, which automatically provides a result of sensitivity or resistance, calculated as the logRQ or ratio of hydrolysis of the antibiotic. This assay is simple to perform, inexpensive, time saving, universal for Gram-negative bacilli, and highly reliable (overall sensitivity and specificity of 98% and 100%, respectively). Moreover, the protocol could be established as a standardised method in clinical laboratories as it does not require specialised training in mass spectrometry. Copyright © 2016 Elsevier B.V. and International Society of Chemotherapy. All rights reserved.

  12. Determination of dimetridazole, ronidazole and their common metabolite in poultry muscle and eggs by high performance liquid chromatography with UV detection and confirmatory analysis by atmospheric pressure chemical ionisation mass spectrometry.

    Science.gov (United States)

    Sams, M J; Strutt, P R; Barnes, K A; Damant, A P; Rose, M D

    1998-12-01

    A method was developed for the determination of the nitroimidazole compounds dimetridazole (DMZ) and ronidazole (RNZ) and their common metabolite, 2-hydroxymethyl-1-methyl-5-nitroimidazole (2-OH-M). Extracts obtained from a clean-up process using strong cation exchange (SCX) solid phase extraction (SPE) can be analysed either by high performance liquid chromatography with UV detection (HPLC-UV) or by high performance liquid chromatography with atmospheric pressure chemical ionisation mass spectrometry (HPLC-APCI-MS) as a confirmatory method. Up to 20 samples can be extracted in approximately 4 h. The HPLC-UV analysis had a limit of detection of 0.5 microgram kg-1. Validation in chicken muscle fortified at a concentration of 5 micrograms kg-1 gave recoveries of 75% DMZ, 77% RNZ and 81% 2-OH-M with RSDs of 16.4, 11.3 and 14.0%, respectively (n = 17). Validation in egg fortified at the same concentration gave recoveries of 77% DMZ, 80% RNZ and 80% 2-OH-M, with RSDs of 14.9, 22.0 and 18.2%, respectively (n = 18). The limit of detection of the HPLC-APCI-MS method was 0.1 microgram kg-1 for DMZ and RNZ and 0.5 microgram kg-1 for 2-OH-M. This method gave mean recoveries in fortified egg samples of 65% DMZ, 87% RNZ and 75% 2-OH-M with RSDs of 22, 11 and 14%, respectively (n = 10). The ratios of the peak areas of the molecular ion and a fragment ion were monitored as added confirmation of the presence of the analyte. Both the HPLC-UV screening procedure and the HPLC-APCI-MS confirmatory method have subsequently been used for the analysis of several hundred samples as part of UK surveillance programmes.

  13. Probing excited electronic states and ionisation mechanisms of fullerenes

    OpenAIRE

    Johansson, Olof; Campbell, Eleanor E. B.

    2013-01-01

    Fullerenes are interesting model systems for probing the complex, fundamental electron dynamics and ionisation mechanisms of large molecules and nanoparticles. In this Tutorial Review we explain how recent experimental and theoretical advances are providing insight into the interesting phenomenon of thermal electron emission from molecular systems and the properties of hydrogenic, diffuse, excited electronic states, known as superatom molecular orbitals, which are responsible for relatively s...

  14. Quantitative analysis of phenolic compounds in Chinese hawthorn (Crataegus spp.) fruits by high performance liquid chromatography-electrospray ionisation mass spectrometry.

    Science.gov (United States)

    Liu, Pengzhan; Kallio, Heikki; Lü, Deguo; Zhou, Chuansheng; Yang, Baoru

    2011-08-01

    Eleven major phenolic compounds (hyperoside, isoquercitrin, chlorogenic acid, ideain, epicatechin, two procyanidin (PA) dimers, three PA trimers and a PA dimer-hexoside) were quantified in the fruits of 22 cultivars/origins of three species of the Chinese hawthorn (Crataegus spp.) by HPLC-ESI-MS-SIR. Hyperoside (0.1-0.8mg/g dry mass [DM]), isoquercitrin (0.1-0.3mg/g DM), chlorogenic acid (0.2-1.6mg/g DM), epicatechin (0.9-11.7mg/g DM), PA B2 (0.7-12.4mg/g DM), PA dimer II (0.1-1.5mg/g DM), PA trimer I (0.1-2.7mg/g DM), PA trimer II (0.7-6.9mg/g DM), PA trimer III (0.01-1.2mg/g DM) and a PA dimer-hexoside (trace-1.1mg/g DM) were detected in all the samples. Ideain (0.0-0.7mg/g DM) was found in all the samples except Crataegus scabrifolia. Significant correlations between the contents of individual PA aglycons were observed (r>0.9, P<0.01). A strong correlation between flavonols was also shown (r=0.71, P<0.01). Fruits of Crataegus pinnatifida var. major had higher contents of PAs but lower contents of flavonols compared with Crataegus brettschneideri. The fruits of C. scabrifolia contained the highest level of PA dimer-hexoside, which was present in trace amounts in the fruits of C. pinnatifida. Copyright © 2011 Elsevier Ltd. All rights reserved.

  15. Variational approach to thermal masses in compactified models

    Energy Technology Data Exchange (ETDEWEB)

    Dominici, Daniele [Dipartimento di Fisica e Astronomia Università di Firenze and INFN - Sezione di Firenze,Via G. Sansone 1, 50019 Sesto Fiorentino (Italy); Roditi, Itzhak [Centro Brasileiro de Pesquisas Físicas - CBPF/MCT,Rua Dr. Xavier Sigaud 150, 22290-180, Rio de Janeiro, RJ (Brazil)

    2015-08-20

    We investigate by means of a variational approach the effective potential of a 5DU(1) scalar model at finite temperature and compactified on S{sup 1} and S{sup 1}/Z{sub 2} as well as the corresponding 4D model obtained through a trivial dimensional reduction. We are particularly interested in the behavior of the thermal masses of the scalar field with respect to the Wilson line phase and the results obtained are compared with those coming from a one-loop effective potential calculation. We also explore the nature of the phase transition.

  16. Determination of ruthenium in photographic emulsions - Development and comparison of different sample treatments and mass spectrometric methods

    NARCIS (Netherlands)

    Krystek, Petra; Heumann, Klaus G.

    1999-01-01

    Different sample treatment procedures were combined with inductively coupled plasma mass spectrometry (ICP-MS) and negative thermal ionisation mass spectrometry (NTI-MS) for the determination of ruthenium traces in photographic emulsions. Dissolution of the samples in concentrated ammonia solution

  17. Thermal Ionisation and the Saha Equation!

    Indian Academy of Sciences (India)

    populations in two states 1 and 2 whose energies differ by I [2-~ ) are in the ratio N2 I tv, = exp 1- ([2 - ~ ) I kaT). The denominator of the exponent has Boltzmann's constant ka = 1.38 x 10-23 Joules/K, which is just a conversion factor from temperature T to energy kaT For example, the energy required to remove an electron ...

  18. Validation of a modified algorithm for the identification of yeast isolates using matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry (MALDI-TOF MS)

    NARCIS (Netherlands)

    van Herendael, B.H.; Bruynseels, P.; Bensaid, M.; Boekhout, T.; de Baere, T.; Surmont, I.; Mertens, A.H.

    2011-01-01

    Optimising antifungal treatment requires the fast and species-specific identification of yeast isolates. We evaluated a modified protocol for the rapid identification of clinical yeast isolates using matrix-assisted laser desorption/ionisation time-of-flight (MALDI-TOF) technology. First, we

  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. Beam Cooling with ionisation losses

    CERN Document Server

    Rubbia, Carlo; Kadi, Y; Vlachoudis, V

    2006-01-01

    A novel type of particle "cooling", called Ionization Cooling, is applicable to slow (v of the order of 0.1c) ions stored in a small ring. The many traversals through a thin foil enhance the nuclear reaction probability, in a steady configuration in which ionisation losses are recovered at each turn by a RF-cavity. For a uniform target "foil" the longitudinal momentum spread diverges exponentially since faster (slower) particles ionise less (more) than the average. In order to "cool" also longitudinally, a chromaticity has to be introduced with a wedge shaped "foil". Multiple scattering and straggling are then "cooled" in all three dimensions, with a method similar to the one of synchrotron cooling, but valid for low energy ions. Particles then stably circulate in the beam indefinitely, until they undergo for instance nuclear processes in the thin target foil. This new method is under consideration for the nuclear production of a few MeV/A ion beams. Simple reactions, for instance Li 7 + D Li 8 + p, are more ...

  1. Nucleation in an ultra low ionisation environment

    DEFF Research Database (Denmark)

    Enghoff, Martin Andreas Bødker

    In this work we have studied aerosol formation at ultra-low ionisation levels, using the existing deep underground science facility at Boulby mine, UK. At 1100 m depth, with a corresponding factor 106 reduction in cosmic ray muon flux, the Boulby facility is an ideal place to study the role of ions...... in aerosol nucleation. By exposing a controlled volume of air to varying levels of ionising radiation, and with the minimum ionisation level vastly reduced compared to normal surface laboratory conditions, we have provided both a validation of earlier studies of ion-induced nucleation and extended...... the measurements to ionisation levels approximately 3 order of magnitudes lower than any earlier study. Getting this close to zero ionisation allows us to distinguish between the neutral and charged contribution better than previously. The effect is explored over a range of sulphuric acid concentrations....

  2. Development of accurate mass spectrometric routine and reference methods for the determination of trace amounts of iridium and rhodium in photographic emulsionsf

    NARCIS (Netherlands)

    Krystek, Petra; Heumann, Klaus G.

    1999-01-01

    For the determination of trace amounts of iridium and rhodium in photographic emulsions different sample treatment procedures were coupled with inductively coupled plasma mass spectrometry (ICP-MS) and, for iridium, also with negative thermal ionisation isotope dilution mass spectrometry (NTI-IDMS)

  3. Modelling the thermal behaviour of the low-thermal mass liquid chromatography system.

    Science.gov (United States)

    Verstraeten, Matthias; Pursch, Matthias; Eckerle, Patric; Luong, Jim; Desmet, Gert

    2011-04-22

    We report upon the experimental investigation of the heat transfer in low thermal mass LC (LTMLC) systems, used under temperature gradient conditions. The influence of the temperature ramp, the capillary dimensions, the material selection and the chromatographic conditions on the radial temperature gradients formed when applying a temperature ramp were investigated by a numerical model and verified with experimental temperature measurements. It was found that the radial temperature gradients scale linearly with the heating rate, quadratically with the radius of the capillary and inversely to the thermal diffusivity. Because of the thermal radial gradients in the liquid zone inside the capillary lead to radial viscosity and velocity gradients, they form an additional source of dispersion for the solutes. For a temperature ramp of 1 K/s and a strong temperature dependence of the retention of small molecules, the model predicts that narrow-bore columns (i.d. 2.1 mm) can be used. For a temperature ramp of 10 K/s, the maximal inner diameter is of the order of 1 mm before a substantial increase in dispersion occurs. Copyright © 2011 Elsevier B.V. All rights reserved.

  4. Demand Shifting with Thermal Mass in Light and Heavy Mass Commercial Buildings

    Energy Technology Data Exchange (ETDEWEB)

    Xu, Peng; Zagreus, Leah

    2009-05-01

    The potential for utilizing building thermal mass for load shifting and peak demand reduction has been demonstrated in a number of simulation, laboratory, and field studies. This project studied the potential of pre-cooling and demand limiting in a heavy mass and a light mass building in the Bay Area of California. The conclusion of the work to date is that pre-cooling has the potential to improve the demand responsiveness of commercial buildings while maintaining acceptable comfort conditions. Results indicate that pre-cooling increases the depth (kW) and duration (kWh) of the shed capacity of a given building, all other factors being equal. Due to the time necessary for pre-cooling, it is only applicable to day-ahead demand response programs. Pre-cooling can be very effective if the building mass is relatively heavy. The effectiveness of night pre-cooling under hot weather conditions has not been tested. Further work is required to quantify and demonstrate the effectiveness of pre-cooling in different climates. Research is also needed to develop screening tools that can be used to select suitable buildings and customers, identify the most appropriate pre-cooling strategies, and estimate the benefits to the customer and the utility.

  5. Probing excited electronic states and ionisation mechanisms of fullerenes.

    Science.gov (United States)

    Johansson, J Olof; Campbell, Eleanor E B

    2013-07-07

    Fullerenes are interesting model systems for probing the complex, fundamental electron dynamics and ionisation mechanisms of large molecules and nanoparticles. In this Tutorial Review we explain how recent experimental and theoretical advances are providing insight into the interesting phenomenon of thermal electron emission from molecular systems and the properties of hydrogenic, diffuse, excited electronic states, known as superatom molecular orbitals, which are responsible for relatively simple, well-resolved structure in fs laser photoelectron spectra of fullerenes. We focus on the application of velocity map imaging combined with fs laser photoionisation to study angular-resolved photoelectron emission.

  6. Ionisation in the absence of high voltage using supercritical fluid chromatography: a possible route to increased signal.

    Science.gov (United States)

    Thite, Mohini A; Boughtflower, Robert; Caldwell, Jeff; Hitzel, Laure; Holyoak, Clare; Lane, Stephen J; Oakley, Paul; Pullen, Frank S; Richardson, Stefan; Langley, G John

    2008-11-01

    Supercritical fluid chromatography (SFC) is fast becoming a technique of choice for the analysis of a wide range of compounds and has been found to be complementary to high-performance liquid chromatography (HPLC). The combination of SFC and mass spectrometry (MS) affords a very useful tool in the separation and analysis of compounds. In this study the ionisation of samples in the absence of an applied electrospray voltage has been observed when using SFC/MS, with some compounds showing increased sensitivity when all ionisation source high voltage (HV) is removed. In an attempt to understand the mechanism of ionisation, a series of test compounds were analysed using standard electrospray ionisation (ESI) and atmospheric pressure chemical ionisation (APCI) source configurations and also different API source designs. In both cases, data were acquired with the applied high voltage on (normal conditions) or with the high voltage off, i.e. no voltage spray (novo-spray). The standards were analysed with a range of pressure and modifier percentage conditions. To understand the nature of the ionisation process observed, this was compared with three established liquid-to-gas ionisation mechanisms. These were thermospray (TSP), charge residue model (CRM) of ESI and sonic spray ionisation (SSI). Experiments were undertaken in an attempt to explain this ionisation phenomenon and quantify any observed change in sensitivity. The most important point to note is that enhanced ionisation was observed under novo-spray conditions in a SFC/MS configuration, which in certain cases provides a lowering in the overall limit of detection (LOD).

  7. Adsorption of ionisable pesticides in soils.

    Science.gov (United States)

    Kah, M; Brown, C D

    2006-01-01

    Understanding the fate of a pesticide in soil is fundamental to the accurate assessment of its environmental behaviour and vital in ensuring the safe use of new and existing products. Ionisable pesticides comprise a significant proportion of both existing and new active substances registered for use in agriculture worldwide. This group of pesticides includes chemicals that are frequently found in groundwater and surface waters in many different countries. Despite this, approaches to predict the influence of soil properties on the behaviour of ionisable pesticides in soils are poorly developed. Current regulatory assessments frequently default to methods developed for nonionic chemicals, although it is evident that ionisable compounds do not often react like neutral molecules. This review presents the state of knowledge on the adsorption of ionisable pesticides in soils. It first introduces the issues concerning adsorption and the characteristics of this particular kind of chemical. The mechanisms postulated for the adsorption of ionisable pesticides are then described: these are hydrophobic partitioning, ionic exchange, charge transfer, ligand exchange, cation or water bridging, and the formation of bound residues. Relatively little experimental evidence is available, and we are still unable to determine the quantitative contribution of each process in a particular situation. Knowledge is still lacking concerning phenomena occurring at the surfaces of soil particles. Measurements do not allow determination of the operative pH at the surface of soil particles or in microenvironments, and the influence of ionic strength or competition effects is difficult to assess. Subsequently, the review focuses on the influence of soil properties on adsorption and on potential to predict the behaviour of ionisable pesticides in soils. Unlike hydrophobic compounds, adsorption of ionisable pesticides is highly sensitive to variation in pH. This relationship mainly derives from the

  8. A discussion about ionising and non-ionising radiation and the critical issue of mobile phones

    Science.gov (United States)

    Kontomaris, Stylianos-Vasileios; Malamou, Anna

    2018-01-01

    Electromagnetic radiation is one of the most important issues affecting peoples’ lives today. The misunderstanding of students and the general population of the effects of electromagnetic radiation is a problem which must be eliminated. Thus, a discussion about ionising and non-ionising radiation focusing on the crucial issue of radiation emitted by mobile phones is presented.

  9. A Discussion about Ionising and Non-Ionising Radiation and the Critical Issue of Mobile Phones

    Science.gov (United States)

    Kontomaris, Stylianos-Vasileios; Malamou, Anna

    2018-01-01

    Electromagnetic radiation is one of the most important issues affecting peoples' lives today. The misunderstanding of students and the general population of the effects of electromagnetic radiation is a problem which must be eliminated. Thus, a discussion about ionising and non-ionising radiation focusing on the crucial issue of radiation emitted…

  10. The use of recently described ionisation techniques for the rapid analysis of some common drugs and samples of biological origin.

    Science.gov (United States)

    Williams, Jonathan P; Patel, Vibhuti J; Holland, Richard; Scrivens, James H

    2006-01-01

    Three ionisation techniques that require no sample preparation or extraction prior to mass analysis have been used for the rapid analysis of pharmaceutical tablets and ointments. These methods were (i) the novel direct analysis in real time (DART), (ii) desorption electrospray ionisation (DESI), and (iii) desorption atmospheric pressure chemical ionisation (DAPCI). The performance of the three techniques was investigated for a number of common drugs. Significant differences between these approaches were observed. For compounds of moderate to low polarity DAPCI produced more effective ionisation. Accurate DESI and DAPCI tandem mass spectra were obtained and these greatly enhance the selectivity and information content of the experiment. The detection from human skin of the active ingredients from ointments is reported together with the detection of ibuprofen metabolites in human urine. Copyright 2006 John Wiley & Sons, Ltd.

  11. Effect of microstructure of graphite on the nonreductive thermal ion emission in thermal ionization mass spectrometry.

    Science.gov (United States)

    Wei, H Z; Jiang, S Y; Xiao, Y K

    2010-02-25

    The emission behavior of polyatomic ions in the ionization source of thermal ionization mass spectrometry (TIMS) was investigated. The results suggest that the presence of a graphite promoter plays a key role for the formation and stable emission of polyatomic ions, such as M(2)X(+), M(2)BO(2)(+), Cs(2)NO(2)(+), and Cs(2)CNO(+). Our data further implied that the intensity of M(2)X(+) and M(2)BO(2)(+) increases and the emission temperature decreases with increasing cationic and anionic radius. During the boron isotopic measurement using the Cs(2)BO(2)(+)-graphite-PTIMS method, the isobaric interference ion Cs(2)CNO(+) cannot be transformed from nitrate or organic compounds containing an amide group but can be induced by the existence of trace amounts of boron because of its special electron-deficiency property (B(3+)). Characterization on the planar crystalline structure of various graphite samples with SEM, TEM, and Raman spectroscopy confirmed the relationship of the emission capacity of polyatomic ions and the crystal microstructure of graphite and provides direct evidence that graphite with a perfect parallel and equidistant layer orientation shows a beneficial effect on the emission of polyatomic ions in TIMS. The mechanism study on the formation of polyatomic ions opens the possibility to establish high precision methods for isotopic composition analysis of more nonmetal elements with the TIMS technique.

  12. Ionisation D'atomes Par un Laser Carbon Dioxide Intense Par L'effet Tunnel

    Science.gov (United States)

    Xiong, Wei

    Cette these decrit des experiences d'ionisation d'atomes (Xe et K) par un laser CO_2 intense. Des spectrometres de masse et d'energie electronique ont ete developpes pour mesurer le nombre d'ions crees et l'energie des electrons acceleres par le gradient spatial du champ laser. Des details sur ces mesures sont fournis et justifies. On a mesure des energies d'electrons jusqu'a 1000eV, a une intensite de 10^{14} W/cm^2. Les mesures experimentales sont comparees avec deux types de theorie, qui decrivent le processus d'ionisation dans deux limites: l'interaction entre electron et noyau est beaucoup plus forte que celle entre electron et champ laser (processus multiphotonique), ou l'inverse (effect tunnel). Les resultats montrent que la courbe du nombre d'ions crees en fonction de l'intensite n'est pas tres sensible aux details du processus d'ionsisation. Par contre les spectres d'energie des electrons dependent fortement du processus d'ionisation, et on peut en deduire le taux d'ionisation. On trouve que la theorie multiphotonique ne fournit pas une explication satisfaisante aux resultats experimentaux, mais que la theorie de l'effet tunnel s'ajuste bien si on suppose que le seuil d'ionisation peut etre deplace legerement par le champ laser. Le deplacement necessaire du seuil est estime dans cette these, mais une explication theorique reste a trouver.

  13. Vertical profile measurements of lower troposphere ionisation

    OpenAIRE

    Harrison, R. G.; Nicoll, K.A.; Aplin, K. L.

    2014-01-01

    Vertical soundings of the atmospheric ion production rate have been obtained from Geiger counters integrated with conventional meteorological radiosondes. In launches made from Reading (UK) during 2013-2014, the Regener-Pfotzer ionisation maximum was at an altitude equivalent to a pressure of (63.1±2.4) hPa, or, expressed in terms of the local air density, (0.101±0.005) kgm−3. The measured ionisation profiles have been evaluated against the Usoskin-Kovaltsov model and, separately, surface neu...

  14. Resonance enhanced multiphoton ionisation (REMPI) and REMPI-photoelectron spectroscopy of carbonyl sulphide and carbon disulphide

    NARCIS (Netherlands)

    Morgan, R.A.; Buma, W.J.; Baldwin, M.A.; Ascenzi, D.; Orr-Ewing, A.J.; Ashfold, M.N.R.; de Milan, J.B.; Scheper, C.R.; de Lange, C.A.

    1996-01-01

    The results of recent mass-resolved resonance enhanced multiphoton ionisation (REMPI) and REMPI-photoelectron spectroscopy (PES) studies of the sixteen valence electron molecules OCS and CS2 are used to illustrate some of the many opportunities offered by (and a few of the possible limitations

  15. Ionising radiation exposure in the Netherlands

    NARCIS (Netherlands)

    Eleveld H; LSO

    2003-01-01

    The Dutch population is exposed to ionising radiation from various sources, both natural and man-made. This is a review of the radiation exposure for members of the public from all sources for the year 2000. The average annual effective dose per capita is estimated at 2.5 mSv, which is almost the

  16. Impact of Thermal Mass Oriented Measures Over CO2 Emissions Of a Thermally Insulated Lowrise Apartment Building in Izmir, Turkey

    Directory of Open Access Journals (Sweden)

    Mümine Gerçek

    2015-02-01

    Full Text Available Climate change has drawn the attention of many researchers and practitioners to focus on the methods to address the challenges in achieving low-carbon buildings and cities and in future developments. Nevertheless, few studies have explored the impacts of thermal mass applications for the lowest carbon emissions of building operational energy consumption. A comparative study of CO2 emissions due to different wall and floor compositions is presented in accordance with their lifespans for a hot-humid climate site. Aim of this study is to examine the relation between the energy oriented operations and carbon emissions of the building. Firstly, an existing low-rise building in İzmir is selected, then modelled in the dynamic simulation model software DesignBuilder v4 by synchronizing drawings with basic operational principles of the program. Furthermore, various influence factors of building envelope thermal characteristics are selected as follows: type, location, thickness and thermal specifications of materials used by keeping thermal conductivity value constant. At the end, the research presents remarkable influence of thermal mass oriented measures on reducing energy demands and carbon footprints.

  17. Effects of functional group mass variance on vibrational properties and thermal transport in graphene

    Science.gov (United States)

    Lindsay, L.; Kuang, Y.

    2017-03-01

    Intrinsic thermal resistivity critically depends on features of phonon dispersions dictated by harmonic interatomic forces and masses. Here we present the effects of functional group mass variance on vibrational properties and thermal conductivity (κ ) of functionalized graphene from first-principles calculations. We use graphane, a buckled graphene backbone with covalently bonded hydrogen atoms on both sides, as the base material and vary the mass of the hydrogen atoms to simulate the effect of mass variance from other functional groups. We find nonmonotonic behavior of κ with increasing mass of the functional group and an unusual crossover from acoustic-dominated to optic-dominated thermal transport behavior. We connect this crossover to changes in the phonon dispersion with varying mass which suppress acoustic phonon velocities, but also give unusually high velocity optic modes. Further, we show that out-of-plane acoustic vibrations contribute significantly more to thermal transport than in-plane acoustic modes despite breaking of a reflection-symmetry-based scattering selection rule responsible for their large contributions in graphene. This work demonstrates the potential for manipulation and engineering of thermal transport properties in two-dimensional materials toward targeted applications.

  18. Understanding thermal energy and mass transport in major volcanic centers

    Science.gov (United States)

    Hermance, John F.

    1984-04-01

    An understanding of the thermal regions of the earth's interior and their associated dynamic processes is of central importance, not only to basic science but to a number of national priorities including resource and the mitigation of volcanic and earthquake hazards. Major thermal anomalies over large regions of the continent are associated with intraplate rifts and transform faults (e.g., the Salton Trough and the Rio Grande Rift), distributed extensional tectonics (e.g., the Basin and Range Province), and plate margins (e.g., the Cascade Range). However, it is clear that of all classes of volcanic phenomena within the conterminous United States, the major intraplate silicic caldera complexes (e.g., Yellowstone, the Valles Caldera, the Long Valley/Mono Craters volcanic complex) appear to have, according to present estimates, the highest accessible geothermal resource base and the greatest destructive power during major eruptive phases. In addition, the exhumed fossil analogs of these systems are associated with extensive mineralization and economic ore deposits. What is lacking, however, is a predictive scientific theory describing the fundamental physio-chemical processes responsible for the development and longterm sustenance of these major volcanic centers in space and time.

  19. Dedicated Trigger for Highly Ionising Particles at ATLAS

    CERN Document Server

    Katre, Akshay; The ATLAS collaboration

    2015-01-01

    In 2012, a novel strategy was designed to detect signatures of Highly Ionising Particles (HIPs) such as magnetic monopoles, dyons or Q-balls with ATLAS. A dedicated trigger was developed and deployed for proton-proton collisions at a centre of mass energy of 8 TeV. It uses the Transition Radiation Tracker (TRT) system, applying an algorithm distinct from standard tracking ones. The high threshold (HT) readout capability of the TRT is used to distinguish HIPs from other background processes. The trigger requires significantly lower energy depositions in the electromagnetic calorimeters and is thereby capable of probing a larger range of HIP masses and charges. A description of the algorithm for this newly developed trigger is presented, along with a comparitive study of its performance during the 2012 data-taking period with respect to previous efforts.

  20. Thermal Cracking Analysis during Pipe Cooling of Mass Concrete Using Particle Flow Code

    Directory of Open Access Journals (Sweden)

    Liang Li

    2016-01-01

    Full Text Available Pipe cooling systems are among the potentially effective measures to control the temperature of mass concrete. However, if not properly controlled, thermal cracking in concrete, especially near water pipes, might occur, as experienced in many mass concrete structures. In this paper, a new numerical approach to simulate thermal cracking based on particle flow code is used to shed more light onto the process of thermal crack propagation and the effect of thermal cracks on thermal fields. Key details of the simulation, including the procedure of obtaining thermal and mechanical properties of particles, are presented. Importantly, a heat flow boundary based on an analytical solution is proposed and used in particle flow code in two dimensions to simulate the effect of pipe cooling. The simulation results are in good agreement with the monitored temperature data and observations on cored specimens from a real concrete gravity dam, giving confidence to the appropriateness of the adopted simulation. The simulated results also clearly demonstrate why thermal cracks occur and how they propagate, as well as the influence of such cracks on thermal fields.

  1. Thermally modulated nano-trampoline material as smart skin for gas molecular mass detection

    Science.gov (United States)

    Xia, Hua

    2012-06-01

    Conventional multi-component gas analysis is based either on laser spectroscopy, laser and photoacoustic absorption at specific wavelengths, or on gas chromatography by separating the components of a gas mixture primarily due to boiling point (or vapor pressure) differences. This paper will present a new gas molecular mass detection method based on thermally modulated nano-trampoline material as smart skin for gas molecular mass detection by fiber Bragg grating-based gas sensors. Such a nanomaterial and fiber Bragg grating integrated sensing device has been designed to be operated either at high-energy level (highly thermal strained status) or at low-energy level (low thermal strained status). Thermal energy absorption of gas molecular trigs the sensing device transition from high-thermal-energy status to low-thermal- energy status. Experiment has shown that thermal energy variation due to gas molecular thermal energy absorption is dependent upon the gas molecular mass, and can be detected by fiber Bragg resonant wavelength shift with a linear function from 17 kg/kmol to 32 kg/kmol and a sensitivity of 0.025 kg/kmol for a 5 micron-thick nano-trampoline structure and fiber Bragg grating integrated gas sensing device. The laboratory and field validation data have further demonstrated its fast response characteristics and reliability to be online gas analysis instrument for measuring effective gas molecular mass from single-component gas, binary-component gas mixture, and multi-gas mixture. The potential industrial applications include fouling and surge control for gas charge centrifugal compressor ethylene production, gas purity for hydrogen-cooled generator, gasification for syngas production, gasoline/diesel and natural gas fuel quality monitoring for consumer market.

  2. An Update on the Non-Mass-Dependent Isotope Fractionation under Thermal Gradient

    Science.gov (United States)

    Sun, Tao; Niles, Paul; Bao, Huiming; Socki, Richard; Liu, Yun

    2013-01-01

    Mass flow and compositional gradient (elemental and isotope separation) occurs when flu-id(s) or gas(es) in an enclosure is subjected to a thermal gradient, and the phenomenon is named thermal diffusion. Gas phase thermal diffusion has been theoretically and experimentally studied for more than a century, although there has not been a satisfactory theory to date. Nevertheless, for isotopic system, the Chapman-Enskog theory predicts that the mass difference is the only term in the thermal diffusion separation factors that differs one isotope pair to another,with the assumptions that the molecules are spherical and systematic (monoatomic-like structure) and the particle collision is elastic. Our previous report indicates factors may be playing a role because the Non-Mass Dependent (NMD) effect is found for both symmetric and asymmetric, linear and spherical polyatomic molecules over a wide range of temperature (-196C to +237C). The observed NMD phenomenon in the simple thermal-diffusion experiments demands quantitative validation and theoretical explanation. Besides the pressure and temperature dependency illustrated in our previous reports, efforts are made in this study to address issues such as the role of convection or molecular structure and whether it is a transient, non-equilibrium effect only.

  3. Food ionisation. Realities and perspectives; L'ionisation alimentaire. Realites et perspectives

    Energy Technology Data Exchange (ETDEWEB)

    Bonnet, G

    1994-06-01

    The ionisation of food is a treatment using a certain type of energy. the radiations used in the industrial treatments are limited to three sources. The gamma radiations, the x radiations and the electrons beams emitted with accelerators. The physical treatments by ionizing radiations have for aim to cleanse and to increase the conservation time of food. Now, the applications in agriculture and food industry, are still marginal. The industrial using ionisation are these ones that did not find any alternative decontamination method. The barriers are more scientific or technical or economical than a question of regulation or behaviour. (N.C.)

  4. On computations for thermal radiation in MHD channel flow with heat and mass transfer.

    Science.gov (United States)

    Hayat, T; Awais, M; Alsaedi, A; Safdar, Ambreen

    2014-01-01

    This study examines the simultaneous effects of heat and mass transfer on the three-dimensional boundary layer flow of viscous fluid between two infinite parallel plates. Magnetohydrodynamic (MHD) and thermal radiation effects are present. The governing problems are first modeled and then solved by homotopy analysis method (HAM). Influence of several embedded parameters on the velocity, concentration and temperature fields are described.

  5. Thermal Inertia Variations from Recent Gully and Mass Wasting Activity in Gasa Crater, Mars

    Science.gov (United States)

    Harrison, T. N.; Tornabene, L. L.; Osinski, G. R.; Conway, S. J.

    2016-12-01

    Gasa Crater is the most active gully site observed on Mars to date, making it of particular interest for studying the process(es) behind gully formation and activity. In this study, we investigate whether differences in thermal inertia across different segments of gully systems, combined with morphological and colour observations with HiRISE, can provide some constraints of the physical characteristics associated with recent activity within gullies in Gasa Crater. We also investigate thermophysical differences between slopes in Gasa dominated by gully activity compared to those predominantly modified by dry mass wasting processes. As thermal inertia (TI) can be used as a proxy for grain size and/or induration, utilizing this dataset can help us to better understand the mass movement processes occurring on the slopes within Gasa. We find that Gasa exhibits clear variations in thermal inertia across its walls, controlled by the material properties and the types of dominant mass movement processes occurring on each wall. Analysis of 64 individual gully fan segments show that the average TI values of the youngest apron deposits are systematically 20-40 thermal inertia units (TIU, J m-2 K-1 s-1/2) higher than the older underlying/surrounding deposits. Talus aprons from mass wasting on the southern walls have thermal inertia values 60-80 TIU higher than gully aprons. The highest TI values in the crater correspond with bedrock exposures in the crater walls, particularly along the southwestern (non-gullied) wall and within the gully alcoves of the pole-facing walls. Analysis of thermal inertia differences could aid in selecting or refining sites for gully activity monitoring by the Mars Reconnaissance Orbiter (MRO) CTX and HiRISE cameras and the CaSSIS camera aboard ESA's ExoMars Trace Gas Orbiter. The results of this study also suggest that repeated THEMIS day/night IR imaging coordinated with MRO and ExoMars observations could be used for surface change detection.

  6. A comparative study of primary secondary amino (PSA) and multi-walled carbon nanotubes (MWCNTs) as QuEChERS absorbents for the rapid determination of diazepam and its major metabolites in fish samples by high-performance liquid chromatography-electrospray ionisation-tandem mass spectrometry.

    Science.gov (United States)

    Li, Jincheng; Zhang, Jing; Liu, Huan; Wu, Lidong

    2016-01-30

    A simple and fast modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) method is presented for the determination of diazepam and its three major metabolites, nordiazepam, temazepam and oxazepam (benzodiazepines) in fish samples by liquid chromatography-electrospray ionisation-tandem mass spectrometry. Muscle tissues were extracted with acetonitrile, and then cleaned with primary secondary amino (PSA) adsorbents. The cleanup effect of PSA was compared with that of multi-walled carbon nanotubes (MWCNTs) in term of extraction efficiency. The better results were obtained when PSA was used. The chromatography separation was achieved within 5.0 min on a C18 column. The limit of detection was 0.5 µg kg(-1) and the limit of quantification was 2.5 µg kg(-1). Average recoveries of diazepam and its main metabolites were in the range of 88.5-110.1%, with a relative standard deviation lower than 10.0%. The proposed method for fish samples gives good recoveries, linearity, precision and accuracy. © 2015 Society of Chemical Industry.

  7. On the Effective Thermal Conductivity of Frost Considering Mass Diffusion and Eddy Convection

    Science.gov (United States)

    Kandula, Max

    2010-01-01

    A physical model for the effective thermal conductivity of water frost is proposed for application to the full range of frost density. The proposed model builds on the Zehner-Schlunder one-dimensional formulation for porous media appropriate for solid-to-fluid thermal conductivity ratios less than about 1000. By superposing the effects of mass diffusion and eddy convection on stagnant conduction in the fluid, the total effective thermal conductivity of frost is shown to be satisfactorily described. It is shown that the effects of vapor diffusion and eddy convection on the frost conductivity are of the same order. The results also point out that idealization of the frost structure by cylindrical inclusions offers a better representation of the effective conductivity of frost as compared to spherical inclusions. Satisfactory agreement between the theory and the measurements for the effective thermal conductivity of frost is demonstrated for a wide range of frost density and frost temperature.

  8. Experimental and Numerical Studies of Controlling Thermal Cracks in Mass Concrete Foundation by Circulating Water

    Directory of Open Access Journals (Sweden)

    Wenchao Liu

    2016-04-01

    Full Text Available This paper summarizes an engineering experience of solving the problem of thermal cracking in mass concrete by using a large project, Zhongguancun No.1 (Beijing, China, as an example. A new method is presented for controlling temperature cracks in the mass concrete of a foundation. The method involves controlled cycles of water circulating between the surface of mass concrete foundation and the atmospheric environment. The temperature gradient between the surface and the core of the mass concrete is controlled at a relatively stable state. Water collected from the well-points used for dewatering and from rainfall is used as the source for circulating water. Mass concrete of a foundation slab is experimentally investigated through field temperature monitoring. Numerical analyses are performed by developing a finite element model of the foundation with and without water circulation. The calculation parameters are proposed based on the experiment, and finite element analysis software MIDAS/CIVIL is used to calculate the 3D temperature field of the mass concrete during the entire process of heat of hydration. The numerical results are in good agreement with the measured results. The proposed method provides an alternative practical basis for preventing thermal cracks in mass concrete.

  9. Thermal transport in a 2D stressed nanostructure with mass gradient

    Directory of Open Access Journals (Sweden)

    R. Barreto

    2015-05-01

    Full Text Available Inspired by some recent molecular dynamics (MD simulations and experiments on suspended graphene nanoribbons, we study a simplified model where the atoms are disposed in a rectangular lattice coupled by nearest neighbor interactions which are quadratic in the interatomic distance. The system has a mechanical strain, and the border atoms are coupled to Langevin thermal baths. Atom masses vary linearly in the longitudinal direction, modeling an isotope or doping distribution. This asymmetry and tension modify thermal properties. Although the atomic interaction is quadratic, the potential is anharmonic in the coordinates. By direct MD simulations and solving Fokker-Planck equations at low temperatures, we can better understand the role of anharmonicities in thermal rectification. We observe an increasing thermal current with an increasing applied mechanical tension. The temperatures and thermal currents vary along the transverse direction. This effect can be useful to establish which parts of the system are more sensitive to thermal damage. We also study thermal rectification as a function of strain and system size. Received: 20 Novembre 2014, Accepted: 17 April 2015; Edited by: C. A. Condat, G. J. Sibona; DOI: http://dx.doi.org/10.4279/PIP.070008 Cite as: R Barreto, M F Carusela, A Mancardo Viotti, A G Monastra, Papers in Physics 7, 070008 (2015

  10. Turbulent heat and mass transfers across a thermally stratified air-water interface

    Science.gov (United States)

    Papadimitrakis, Y. A.; Hsu, Y.-H. L.; Wu, J.

    1986-01-01

    Rates of heat and mass transfer across an air-water interface were measured in a wind-wave research facility, under various wind and thermal stability conditions (unless otherwise noted, mass refers to water vapor). Heat fluxes were obtained from both the eddy correlation and the profile method, under unstable, neutral, and stable conditions. Mass fluxes were obtained only under unstable stratification from the profile and global method. Under unstable conditions the turbulent Prandtl and Schmidt numbers remain fairly constant and equal to 0.74, whereas the rate of mass transfer varies linearly with bulk Richardson number. Under stable conditions the turbulent Prandtl number rises steadily to a value of 1.4 for a bulk Richardson number of about 0.016. Results of heat and mass transfer, expressed in the form of bulk aerodynamic coefficients with friction velocity as a parameter, are also compared with field data.

  11. Transition dynamics in two-photon ionisation

    Science.gov (United States)

    Vacher, Morgane; Gaillac, Romain; Maquet, Alfred; Taïeb, Richard; Caillat, Jérémie

    2017-11-01

    We review various aspects of photoemission dynamics in the case of two-photon ionisation. We first recall the definition of a transition phase specific to two-photon transitions. Numerical experiments on model atoms are used to show how the group delay associated with the transition phase is actually representative of the early dynamics of the detected photoelectron wave packets. Then we address the question of measuring these transition delays using a standard interferometric technique of experimental attosecond physics, so-called rabbit. Finally, we outline different reinterpretations of rabbit giving access to the more fundamental scattering dynamics affecting any photoemission processes.

  12. Impact of thermal energy storage properties on solar dynamic space power conversion system mass

    Science.gov (United States)

    Juhasz, Albert J.; Coles-Hamilton, Carolyn E.; Lacy, Dovie E.

    1987-01-01

    A 16 parameter solar concentrator/heat receiver mass model is used in conjunction with Stirling and Brayton Power Conversion System (PCS) performance and mass computer codes to determine the effect of thermal energy storage (TES) material property changes on overall PCS mass as a function of steady state electrical power output. Included in the PCS mass model are component masses as a function of thermal power for: concentrator, heat receiver, heat exchangers (source unless integral with heat receiver, heat sink, regenerator), heat engine units with optional parallel redundancy, power conditioning and control (PC and C), PC and C radiator, main radiator, and structure. Critical TES properties are: melting temperature, heat of fusion, density of the liquid phase, and the ratio of solid-to-liquid density. Preliminary results indicate that even though overall system efficiency increases with TES melting temperature up to 1400 K for concentrator surface accuracies of 1 mrad or better, reductions in the overall system mass beyond that achievable with lithium fluoride (LiF) can be accomplished only if the heat of fusion is at least 800 kJ/kg and the liquid density is comparable to that of LiF (1800 kg/cu m).

  13. Behavioural responses to thermal conditions affect seasonal mass change in a heat-sensitive northern ungulate.

    Directory of Open Access Journals (Sweden)

    Floris M van Beest

    Full Text Available BACKGROUND: Empirical tests that link temperature-mediated changes in behaviour (activity and resource selection to individual fitness or condition are currently lacking for endotherms yet may be critical to understanding the effect of climate change on population dynamics. Moose (Alces alces are thought to suffer from heat stress in all seasons so provide a good biological model to test whether exposure to non-optimal ambient temperatures influence seasonal changes in body mass. Seasonal mass change is an important fitness correlate of large herbivores and affects reproductive success of female moose. METHODOLOGY/PRINCIPAL FINDINGS: Using GPS-collared adult female moose from two populations in southern Norway we quantified individual differences in seasonal activity budget and resource selection patterns as a function of seasonal temperatures thought to induce heat stress in moose. Individual body mass was recorded in early and late winter, and autumn to calculate seasonal mass changes (n = 52 over winter, n = 47 over summer. We found large individual differences in temperature-dependent resource selection patterns as well as within and between season variability in thermoregulatory strategies. As expected, individuals using an optimal strategy, selecting young successional forest (foraging habitat at low ambient temperatures and mature coniferous forest (thermal shelter during thermally stressful conditions, lost less mass in winter and gained more mass in summer. CONCLUSIONS/SIGNIFICANCE: This study provides evidence that behavioural responses to temperature have important consequences for seasonal mass change in moose living in the south of their distribution in Norway, and may be a contributing factor to recently observed declines in moose demographic performance. Although the mechanisms that underlie the observed temperature mediated habitat-fitness relationship remain to be tested, physiological state and individual variation in

  14. Students' Conceptions of Ionisation Energy: A Cross-Cultural Study

    Science.gov (United States)

    Tan, Kim Chwee Daniel; Taber, Keith S.; Liu, Xiufeng; Coll, Richard K.; Lorenzo, Mercedes; Li, Jia; Goh, Ngoh Khang; Chia, Lian Sai

    2008-01-01

    Previous studies have indicated that A-level students in the UK and Singapore have difficulty learning the topic of ionisation energy. A two-tier multiple-choice instrument developed in Singapore in an earlier study, the Ionisation Energy Diagnostic Instrument, was administered to A-level students in the UK, advanced placement high school students…

  15. An analysis of a charring ablator with thermal nonequilibrium, chemical kinetics, and mass transfer

    Science.gov (United States)

    Clark, R. K.

    1973-01-01

    The differential equations governing the transient response of a one-dimensional ablative thermal protection system are presented for thermal nonequilibrium between the pyrolysis gases and the char layer and with finite rate chemical reactions occurring. The system consists of three layers (the char layer, the uncharred layer, and an optical insulation layer) with concentrated heat sinks at the back surface and between the second and third layers. The equations are solved numerically by using a modified implicit finite difference scheme to obtain solutions for the thickness of the charred and uncharred layers, surface recession and pyrolysis rates, solid temperatures, porosity profiles, and profiles of pyrolysis-gas temperature, pressure, composition, and flow rate. Good agreement is obtained between numerical results and exact solutions for a number of simplified cases. The complete numerical analysis is used to obtain solutions for an ablative system subjected to a constant heating environment. Effects of thermal, chemical, and mass transfer processes are shown.

  16. Thermodynamic analysis of human heat and mass transfer and their impact on thermal comfort

    OpenAIRE

    Prek, Matjaž

    2015-01-01

    In this paper a thermodynamic analysis of human heat and mass transfer based on the 2nd law of thermodynamics in presented. For modelling purposes the two-node human thermal model was used. This model was improved in order to establish the exergy consumption within the human body as a consequence of heat and mass transfer and/or conversion. It is shown that the human body's exergy consumption in relation to selected human parameters exhibit a minimal value at certain combinations of environme...

  17. Relativistic mass and charge of photons in thermal plasmas through electromagnetic field quantization.

    Science.gov (United States)

    Asenjo, Felipe A; Muñoz, Víctor; Valdivia, J Alejandro

    2010-05-01

    An effective photon mass and equivalent photon charge are calculated for plasmas with finite temperature, by using a second covariant quantization of the electromagnetic field, which is based on a nonlinear magnetofluid unification field formalism. Relativistic effects are considered both in the fluid bulk motion and in the thermal motion. The effective relativistic photon mass is found for transverse and longitudinal photons, while the equivalent relativistic photon charge is obtained for purely transverse photons. Both quantum quantities are the relativistic generalization, at finite temperature, of previous results [Mendonça, et al., Phys. Rev. E 62, 2989 (2000)]. The dependence with temperature is studied in both cases.

  18. Thermal diffusion effects on free convection and mass transfer flow for an infinite vertical plate

    CERN Document Server

    Abdel-Khalek, M M

    2003-01-01

    A theoretical study is performed to examine the effects of thermal diffusion on free convection and mass transfer flow for an infinite vertical plate. The governing equations for the fluid flow and the heat transfer are solved subject to the relevant boundary conditions. A perturbation technique is used to obtain expressions for the velocity field and skin friction. An analysis of the effects of the parameters on the concentration, velocity and temperature profiles as well as skin friction and the rate of mass and heat transfer is done with the aid of graphs.

  19. Thermal Dilepton Radiation at Intermediate Masses at the CERN-SpS

    CERN Document Server

    Rapp, R

    2000-01-01

    We investigate the significance of thermal dilepton radiation in the intermediate-mass region in heavy-ion reactions at CERN-SpS energies. Within a thermal fireball model for the space-time evolution, the radiation from hot matter is found to dominate over hard 'background' processes (Drell-Yan and open charm) up to invariant masses of about 2 GeV, with a rather moderate fraction emerging from early stages with temperatures $T\\simeq 175-200$ MeV associated with deconfined matter. Further including a schematic acceptance for the NA50 experiment we find good agreement with the observed enhancement in the region 1.5 GeV~$

  20. Reducing Residential Peak Electricity Demand with Mechanical Pre-Cooling of Building Thermal Mass

    Energy Technology Data Exchange (ETDEWEB)

    Turner, Will [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States); Walker, Iain [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States); Roux, Jordan [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)

    2014-08-01

    This study uses an advanced airflow, energy and humidity modelling tool to evaluate the potential for residential mechanical pre-cooling of building thermal mass to shift electricity loads away from the peak electricity demand period. The focus of this study is residential buildings with low thermal mass, such as timber-frame houses typical to the US. Simulations were performed for homes in 12 US DOE climate zones. The results show that the effectiveness of mechanical pre-cooling is highly dependent on climate zone and the selected pre-cooling strategy. The expected energy trade-off between cooling peak energy savings and increased off-peak energy use is also shown.

  1. Lighter touch keeps in the heat. [Advantages of low-thermal-mass insulation

    Energy Technology Data Exchange (ETDEWEB)

    Pipes, A.

    1979-04-01

    Low-thermal-mass insulation of ceramic fibers and light refractory materials is more suitable to applications with intermittent processes and lower-temperature melting and retreating, where the heat-retention requirements do not require traditional furnace design. Old furnaces can be retrofitted by replacing bricks with insulation or by veneering. Insulating materials include ceramic, alumina, and quartz fibers, and microtherm in the form of blocks, blankets and other shapes. 4 figures. (DCK)

  2. Investigation of naproxen drug using mass spectrometry, thermal analyses and semi-empirical molecular orbital calculation

    Directory of Open Access Journals (Sweden)

    M.A. Zayed

    2017-03-01

    Full Text Available Naproxen (C14H14O3 is a non-steroidal anti-inflammatory drug (NSAID. It is important to investigate its structure to know the active groups and weak bonds responsible for medical activity. In the present study, naproxen was investigated by mass spectrometry (MS, thermal analysis (TA measurements (TG/DTG and DTA and confirmed by semi empirical molecular orbital (MO calculation, using PM3 procedure. These calculations included, bond length, bond order, bond strain, partial charge distribution, ionization energy and heat of formation (ΔHf. The mass spectra and thermal analysis fragmentation pathways were proposed and compared to select the most suitable scheme representing the correct fragmentation pathway of the drug in both techniques. The PM3 procedure reveals that the primary cleavage site of the charged molecule is the rupture of the COOH group (lowest bond order and high strain which followed by CH3 loss of the methoxy group. Thermal analysis of the neutral drug reveals a high response to the temperature variation with very fast rate. It decomposed in several sequential steps in the temperature range 80–400 °C. These mass losses appear as two endothermic and one exothermic peaks which required energy values of 255.42, 10.67 and 371.49 J g−1 respectively. The initial thermal ruptures are similar to that obtained by mass spectral fragmentation (COOH rupture. It was followed by the loss of the methyl group and finally by ethylene loss. Therefore, comparison between MS and TA helps in selection of the proper pathway representing its fragmentation. This comparison is successfully confirmed by MO-calculation.

  3. Demand Shifting With Thermal Mass in Large Commercial Buildings:Field Tests, Simulation and Audits

    Energy Technology Data Exchange (ETDEWEB)

    Xu, Peng; Haves, Philip; Piette, Mary Ann; Zagreus, Leah

    2005-09-01

    The principle of pre-cooling and demand limiting is to pre-cool buildings at night or in the morning during off-peak hours, storing cooling in the building thermal mass and thereby reducing cooling loads and reducing or shedding related electrical demand during the peak periods. Cost savings are achieved by reducing on-peak energy and demand charges. The potential for utilizing building thermal mass for load shifting and peak demand reduction has been demonstrated in a number of simulation, laboratory, and field studies (Braun 1990, Ruud et al. 1990, Conniff 1991, Andresen and Brandemuehl 1992, Mahajan et al. 1993, Morris et al. 1994, Keeney and Braun 1997, Becker and Paciuk 2002, Xu et al. 2003). This technology appears to have significant potential for demand reduction if applied within an overall demand response program. The primary goal associated with this research is to develop information and tools necessary to assess the viability of and, where appropriate, implement demand response programs involving building thermal mass in buildings throughout California. The project involves evaluating the technology readiness, overall demand reduction potential, and customer acceptance for different classes of buildings. This information can be used along with estimates of the impact of the strategies on energy use to design appropriate incentives for customers.

  4. Effectiveness of indirect evaporative cooling and thermal mass in a hot arid climate

    Energy Technology Data Exchange (ETDEWEB)

    Krueger, Eduardo [Programa de Pos-Graduacao em Tecnologia/Programa de Pos-Graduacao em Engenharia Civil, Departamento de Construcao Civil, Universidade Tecnologica Federal do Parana - UTFPR, Av. Sete de Setembro, 3165. Curitiba PR, CEP. 80230-901 (Brazil); Gonzalez Cruz, Eduardo [Instituto de Investigaciones de la Facultad de Arquitectura y Diseno (IFAD), Universidad del Zulia, Nucleo Tecnico de LUZ, Av. Goajira (16) con Calle 67, Maracaibo, CP 4011-A-526 (Venezuela); Givoni, Baruch [Department of Architecture, School of Arts and Architecture, UCLA, Los Angeles CA, USA, and Ben Gurion University (Israel)

    2010-06-15

    In this paper, we compare results of a long-term temperature monitoring in a building with high thermal mass to indoor temperature predictions of a second building that uses an indirect evaporative cooling system as a means of passive cooling (Vivienda Bioclimatica Prototipo -VBP-1), for the climatic conditions of Sde Boqer, Negev region of Israel (local latitude 30 52'N, longitude 34 46'E, approximately 480 m above sea level). The high-mass building was monitored from January through September 2006 and belongs to a student dormitory complex located at the Sde Boqer Campus of Ben-Gurion University. VBP-1 was designed and built in Maracaibo, Venezuela (latitude 10 34'N, longitude 71 44'W, elevation 66 m above sea level) and had its indoor air temperatures, below and above a shaded roof pond, as well as the pond temperature monitored from February to September 2006. Formulas were developed for the VBP-1, based on part of the whole monitoring period, which represent the measured daily indoor maximum, average and minimum temperatures. The formulas were then validated against measurements taken independently in different time periods. The developed formulas were here used for estimating the building's thermal and energy performance at the climate of Sde Boqer, allowing a comparison of two different strategies: indirect evaporative cooling and the use of thermal mass. (author)

  5. Chemistry of Aliphatic Unconjugated Nitramines. Part 7. Interrelations between the Thermal, Photochemical and Mass Spectral Fragmentation of RDX,

    Science.gov (United States)

    The mass spectral fragmentation of RDX and HMX has been described in terms of their metastable transitions, mass measurements and ionization...efficiency curves. The ring migration of an NO2 group is noted. The known interrelation between the thermal, photochemical and mass spectral fragmentation of

  6. Modeling of thermal mass energy storage in buildings with phase change materials

    Science.gov (United States)

    Delcroix, Benoit

    Building thermal mass is a key parameter defining the ability of a building to mitigate inside temperature variations and to maintain a better thermal comfort. Increasing the thermal mass of a lightweight building can be achieved by using Phase Change Materials (PCMs). These materials offer a high energy storage capacity (using latent energy) and a nearly constant temperature phase change. They can be integrated conveniently in net-zero energy buildings. The current interest for these buildings and for better power demand management strategies requires accurate transient simulation of heavy and highly insulated slabs or walls with short time-steps (lower than or equal to 5 minutes). This represents a challenge for codes that were mainly developed for yearly energy load calculations with a time-step of 1 hour. It is the case of the TRNSYS building model (called Type 56) which presents limitations when modeling heavy and highly insulated slabs with short time-steps. These limitations come from the method used by TRNSYS for modeling conduction heat transfer through walls which is known as the Conduction Transfer Function (CTF) method. In particular, problems have been identified in the generation of CTF coefficients used to model the walls thermal response. This method is also unable to define layers with variable thermophysical properties, as displayed by PCMs. PCM modeling is further hindered by the limited information provided by manufacturers: physical properties are often incomplete or incorrect. Finally, current models are unable to represent the whole complexity of PCM thermal behavior: they rarely include different properties for melting and solidification (hysteresis); they sometimes take into account variable thermal conductivity; but they never model subcooling effects. All these challenges are tackled in this thesis and solutions are proposed. The first part (chapter 4) focuses on improving the CTF method in TRNSYS through state-space modeling

  7. Energy efficiency and comfort conditions in passive solar buildings: Effect of thermal mass at equatorial high altitudes

    Science.gov (United States)

    Ogoli, David Mwale

    This dissertation is based on the philosophy that architectural design should not just be a function of aesthetics, but also of energy-efficiency, advanced technologies and passive solar strategies. A lot of published literature is silent regarding buildings in equatorial highland regions. This dissertation is part of the body of knowledge that attempts to provide a study of energy in buildings using thermal mass. The objectives were to establish (1) effect of equatorial high-altitude climate on thermal mass, (2) effect of thermal mass on moderating indoor temperatures, (3) effect of thermal mass in reducing heating and cooling energy, and (4) the amount of time lag and decrement factor of thermal mass. Evidence to analyze the effect of thermal mass issues came from three sources. First, experimental physical models involving four houses were parametrically conducted in Nairobi, Kenya. Second, energy computations were made using variations in thermal mass for determining annual energy usage and costs. Third, the data gathered were observed, evaluated, and compared with currently published research. The findings showed that: (1) Equatorial high-altitude climates that have diurnal temperature ranging about 10--15°C allow thermal mass to moderate indoor temperatures; (2) Several equations were established that indicate that indoor mean radiant temperatures can be predicted from outdoor temperatures; (3) Thermal mass can reduce annual energy for heating and cooling by about 71%; (4) Time lag and decrement of 200mm thick stone and concrete thermal mass can be predicted by a new formula; (5) All windows on a building should be shaded. East and west windows when shaded save 51% of the cooling energy. North and south windows when fully shaded account for a further 26% of the cooling energy; (6) Insulation on the outside of a wall reduces energy use by about 19.6% below the levels with insulation on the inside. The basic premise of this dissertation is that decisions that

  8. A novel method for the analysis of the substitution pattern of O-methyl-[alpha]- and [beta]-1,4-glucans by means of electrospray ionisation-mass spectrometry/collision induced dissociation

    Science.gov (United States)

    Adden, Roland; Mischnick, Petra

    2005-03-01

    The substitution pattern of O-methyl amylose and O-methyl cellulose was analysed after per-O-methylation (Me-d3), and partial hydrolysis by subsequent ESI-MS/CID of the sodium (MS2) and the lithium adducts (MS3). Based on previous studies about the influence of regioselective O-methylation on the fragmentation pathways of malto- and cello-oligosaccharides, we could calculate the contribution of a certain methyl pattern to a distinct signal in the reproducible ESI-MS2 daughter spectrum. Signal intensities obtained from each O-methyl-O-methyl-d3 disaccharide were distributed on the corresponding methyl patterns and accumulated for all peaks of the mother mass spectrum. Data from ESI-MS2 were not sufficient for disaccharides bearing methyl and deuteromethyl groups in the combination 2 and 4, 3 and 3, or 4 and 2. Further independent information was obtained by ESI-MS3 of the lithium adducts. Monomer composition of methyl celluloses and methyl amyloses obtained by this novel approach were in very good agreement with reference data from GLC of the partially methylated glucitol acetates after complete hydrolysis, reduction and acetylation.

  9. Direct extraction of urinary analytes from undeveloped reversed-phase thin layer chromatography plates using a solvent gradient combined with on-line electrospray ionisation ion mobility-mass spectrometry.

    Science.gov (United States)

    Devenport, Neil A; Reynolds, James C; Weston, Daniel J; Wilson, Ian D; Creaser, Colin S

    2012-08-07

    The direct extraction of urinary analytes deposited on reversed-phase thin-layer chromatography (RP-TLC) plates is demonstrated using a solvent gradient extraction procedure without prior chromatographic development. The surface sample probe TLC-MS interface used for the gradient extraction is compared to direct loop injection into the electrospray ion source for biofluid profiling. The gradient elution is shown to enhance ion intensities, as urinary salts are eluted in aqueous formic acid in the early part of the gradient reducing ion suppression. The retention of urinary components on the C18 RP-TLC plate was confirmed by monitoring analyte responses with, and without, an aqueous wash phase prior to the solvent gradient extraction. The use of gradient elution allows fractionation of the complex biological matrix as a result of differential retention of urine components on the undeveloped RP-TLC plate. The direct gradient analysis of TLC plates has also been combined with ion mobility-mass spectrometry to further resolve the complex urinary profile and identify co-eluting compounds.

  10. Dedicated Trigger for Highly Ionising Particles at ATLAS

    CERN Document Server

    Katre, Akshay; The ATLAS collaboration

    2015-01-01

    In 2012, a novel strategy was designed to detect signatures of Highly Ionising Particles (HIPs) such as magnetic monopoles, dyons or Qballs with the ATLAS trigger system. With proton-proton collisions at a centre of mass enegy of 8 TeV, the trigger was designed to have unique properties as a tracker for HIPs. It uses only the Transition Radiation Tracker (TRT) system, applying an algorithm distinct from standard tracking ones. The unique high threshold readout capability of the TRT is used at the location where HIPs in the detector are looked for. In particular the number and the fraction of TRT high threshold hits is used to distinguish HIPs from background processes. The trigger requires significantly lower energy depositions in the electro-magnetic calorimeters as a seed unlike previously used trigger algorithms for such searches. Thus the new trigger is capable of probing a large range of HIP masses and charges. We will give a description of the algorithms for this newly developed trigger for HIP searches...

  11. Determination of Coefficient of Thermal Expansion (CTE) of 20MPa Mass Concrete Using Granite Aggregate

    Science.gov (United States)

    Chee Siang, GO

    2017-07-01

    Experimental test was carried out to determine the coefficient of thermal expansion (CTE) value of 20MPa mass concrete using granite aggregate. The CTE value was established using procedure proposed by Kada et al. 2002 in determining the magnitude of early-ages CTE through laboratory test which is a rather accurate way by eliminating any possible superimposed effect of others early-age thermal deformation shrinkages such as autogenous, carbonation, plastic and drying shrinkage. This was done by submitting granite concrete block samples instrumented with ST4 vibrating wire extensometers to thermal shocks. The response of the concrete samples to this shock results in a nearly instantaneous deformation, which are measured by the sensor. These deformations, as well as the temperature signal, are used to calculate the CTE. By repeating heat cycles, the variation in the early-ages of concrete CTE over time was monitored and assessed for a period of upto 7 days. The developed CTE value facilitating the verification and validation of actual maximum permissible critical temperature differential limit (rather than arbitrarily follow published value) of cracking potential. For thick sections, internal restraint is dominant and this is governed by differentials mainly. Of the required physical properties for thermal modelling, CTE is of paramount importance that with given appropriate internal restraint factor the condition of cracking due to internal restraint is governs by equation, ΔTmax= 3.663ɛctu / αc. Thus, it can be appreciated that an increase in CTE will lower the maximum allowable differential for cracking avoidance in mass concrete while an increase of tensile strain capacity will increase the maximum allowable temperature differential.

  12. Evaluation of Background Ionising Radiation Levels in Benue State ...

    African Journals Online (AJOL)

    Evaluation of Background Ionising Radiation Levels in Benue State University Teaching Hospital Makurdi North Central Nigeria. H Mohammad, J T Iortile, J E Ekediwe, L Alumuku, E A Okon, D M Chia, E Ejeh, F U Ugbo ...

  13. The core mass growth and stellar lifetime of thermally pulsing asymptotic giant branch stars

    Energy Technology Data Exchange (ETDEWEB)

    Kalirai, Jason S.; Tremblay, Pier-Emmanuel [Space Telescope Science Institute, 3700 San Martin Drive, Baltimore, MD 21218 (United States); Marigo, Paola, E-mail: jkalirai@stsci.edu, E-mail: paola.marigo@unipd.it, E-mail: ptremblay@lsw.uni-heidelberg.de [Department of Physics and Astronomy, University of Padova, Vicolo dell' Osservatorio 3, I-35122 Padova (Italy)

    2014-02-10

    We establish new constraints on the intermediate-mass range of the initial-final mass relation, and apply the results to study the evolution of stars on the thermally pulsing asymptotic giant branch (TP-AGB). These constraints derive from newly discovered (bright) white dwarfs in the nearby Hyades and Praesepe star clusters, including a total of 18 high signal-to-noise ratio measurements with progenitor masses of M {sub initial} = 2.8-3.8 M {sub ☉}. We also include a new analysis of existing white dwarfs in the older NGC 6819 and NGC 7789 star clusters, M {sub initial} = 1.6 and 2.0 M {sub ☉}. Over this range of initial masses, stellar evolutionary models for metallicity Z {sub initial} = 0.02 predict the maximum growth of the core of TP-AGB stars. By comparing the newly measured remnant masses to the robust prediction of the core mass at the first thermal pulse on the AGB (i.e., from stellar interior models), we establish several findings. First, we show that the stellar core mass on the AGB grows rapidly from 10% to 30% for stars with M {sub initial} = 1.6 to 2.0 M {sub ☉}. At larger masses, the core-mass growth decreases steadily to ∼10% at M {sub initial} = 3.4 M {sub ☉}, after which there is a small hint of a upturn out to M {sub initial} = 3.8 M {sub ☉}. These observations are in excellent agreement with predictions from the latest TP-AGB evolutionary models in Marigo et al. We also compare to models with varying efficiencies of the third dredge-up and mass loss, and demonstrate that the process governing the growth of the core is largely the stellar wind, while the third dredge-up plays a secondary, but non-negligible role. Based on the new white dwarf measurements, we perform an exploratory calibration of the most popular mass-loss prescriptions in the literature, as well as of the third dredge-up efficiency as a function of the stellar mass. Finally, we estimate the lifetime and the integrated luminosity of stars on the TP-AGB to peak at t

  14. Unconventional thermal transport enhancement with large atom mass: a comparative study of 2D transition dichalcogenides

    Science.gov (United States)

    Wang, Huimin; Qin, Guangzhao; Li, Guojian; Wang, Qiang; Hu, Ming

    2018-01-01

    2D layered transition dichalcogenides have attracted tremendous attention for their excellent properties and multifarious applications. In particular, NbSe2 and TaSe2 are the canonical systems to study superconductivity and charge density waves. Here, we perform a comparative study of the thermal transport properties of 2D NbSe2 and TaSe2 for both 1T and 2H phases based on first-principles calculations. Usually, the lattice thermal conductivity ({{κ }L} ) is smaller with larger average atom mass. However, it is contrary for the comparison between TaSe2 and NbSe2, despite the heavier Ta than Nb. The abnormally larger {{κ }L} of TaSe2 originates from the weakened phonon–phonon scattering due to the combination of large phonon bandgap and bunching of the acoustic phonon branches, which is caused by the larger mass difference. On one hand, the large bandgap hinders the acoustic–optical phonon scattering. On the other hand, the bunching of the acoustic phonon branches hampers Umklapp process by weakening the high frequency acoustic–acoustic phonon scattering. The special characteristics of phonon transport are further conformed by mode level analysis and scattering channels of phonon–phonon scattering. Moreover, lower κ L of 1T phase for both Nb and Ta selenides compared to 2H phase are also reported, which stems from the stronger anharmonicity.

  15. Investigation of diazepam drug using thermal analyses, mass spectrometry and semi-empirical MO calculation

    Science.gov (United States)

    Zayed, M. A.; Fahmey, M. A.; Hawash, M. F.

    2005-03-01

    In the present work diazepam (Dz) drug was investigated using thermal analyses (TA) measurements (TG/DTG) in comparison with EI mass spectral (MS) fragmentation at 70 and 20 eV. Semi-empirical MO calculations, MNDO procedure, have been carried out on diazepam both as neutral molecule and the corresponding positively charged molecular ion. These include molecular geometry, bond order, charge distribution, heats of formation and ionization energy. Thermogravimetric and kinetic analysis, reveal a high response of the drug to the temperature variation with very fast rate. It is completely decomposed in the temperature range between 204 and 340 °C with average kinetic energy (KE) at 164.69 kJ mol -1. On the other hand, diazepam can easily fragmented at low energy after ionization by electron energy at 9.56 eV. The losses of CO gas molecules followed by chlorine gas from the entity of diazepam (both neutral and charged molecular ion) as the best selected pathway were observed in both mass spectra (MS) and thermal analyses (TA). MNDO calculation was applied to declare both TA and MS observations.

  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. Optimisation of secondary electrospray ionisation (SESI) for the trace determination of gas-phase volatile organic compounds.

    Science.gov (United States)

    Dillon, Leonard A; Stone, Victoria N; Croasdell, Laura A; Fielden, Peter R; Goddard, Nicholas J; Thomas, C L Paul

    2010-02-01

    An electrospray ionisation triple quadrupole mass spectrometer (Varian 1200 L) was modified to accept nitrogen samples containing low concentrations of volatile organic compounds. Six candidate probe compounds, methyl decanoate, octan-3-one, 2-ethylhexanoic acid, 1,4-diaminobutane, dimethyl methylphosphonate, and 2,3-butanediol, at concentrations below 50 ppb(v) were generated with permeation tubes in a test atmosphere generator. The concept of using a set of molecular probes to evaluate gas-phase electrospray ionisation of volatile analytes was assessed and the feasibility of adopting a unified ionisation approach for gas and liquid contamination of exobiotic environments established. 450 experiments were run in a five-replicate, fifteen-level, three-factor, central-composite-design with exponential dilution for each of the six probe compounds studied. The three factors studied were ionisation voltage, drying-gas flow and nebulising-gas flow. Parametric modelling by regression analysis enabled the differences in the ionisation behaviours of the probe compounds to be described by the optimisation models. Regression coefficients were in the range 0.91 to 0.99, indicating satisfactory levels of precision in the optimisation models. A wide range in ionisation efficiency was observed, with different optimised conditions required for the probe compounds. It was evident that no one factor appeared to dominate the response and the different factors produced different effects on the responses for the different molecules. 1,4-Butanediamine and dimethyl methylphosphonate required significantly lower ionisation voltages (1.2 kV) than the other four, which achieved optimised sensitivity towards the maximum voltage used in this design (5 to 6 kV). Drying-gas flow rates were found to be more important than nebulising-gas flow rates. However, variations in the constant term B(0) in the optimisation models indicated that other factors, not included in this study, were also likely

  18. Marine heatwave causes unprecedented regional mass bleaching of thermally resistant corals in northwestern Australia.

    Science.gov (United States)

    Le Nohaïc, Morane; Ross, Claire L; Cornwall, Christopher E; Comeau, Steeve; Lowe, Ryan; McCulloch, Malcolm T; Schoepf, Verena

    2017-11-03

    In 2015/16, a marine heatwave associated with a record El Niño led to the third global mass bleaching event documented to date. This event impacted coral reefs around the world, including in Western Australia (WA), although WA reefs had largely escaped bleaching during previous strong El Niño years. Coral health surveys were conducted during the austral summer of 2016 in four bioregions along the WA coast (~17 degrees of latitude), ranging from tropical to temperate locations. Here we report the first El Niño-related regional-scale mass bleaching event in WA. The heatwave primarily affected the macrotidal Kimberley region in northwest WA (~16°S), where 4.5-9.3 degree heating weeks (DHW) resulted in 56.6-80.6% bleaching, demonstrating that even heat-tolerant corals from naturally extreme, thermally variable reef environments are threatened by heatwaves. Some heat stress (2.4 DHW) and bleaching (coral communities at Ningaloo Reef (23°9'S) and Bremer Bay (34°25'S) were not impacted. The only other major mass bleaching in WA occurred during a strong La Niña event in 2010/11 and primarily affected reefs along the central-to-southern coast. This suggests that WA reefs are now at risk of severe bleaching during both El Niño and La Niña years.

  19. 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.

  20. Excitation and Ionisation dynamics in high-frequency plasmas

    Science.gov (United States)

    O'Connell, D.

    2008-07-01

    Non-thermal low temperature plasmas are widely used for technological applications. Increased demands on plasma technology have resulted in the development of various discharge concepts based on different power coupling mechanisms. Despite this, power dissipation mechanisms in these discharges are not yet fully understood. Of particular interest are low pressure radio-frequency (rf) discharges. The limited understanding of these discharges is predominantly due to the complexity of the underlying mechanisms and difficult diagnostic access to important parameters. Optical measurements are a powerful diagnostic tool offering high spatial and temporal resolution. Optical emission spectroscopy (OES) provides non-intrusive access, to the physics of the plasma, with comparatively simple experimental requirements. Improved advances in technology and modern diagnostics now allow deeper insight into fundamental mechanisms. In low pressure rf discharges insight into the electron dynamics within the rf cycle can yield vital information. This requires high temporal resolution on a nano-second time scale. The optical emission from rf discharges exhibits temporal variations within the rf cycle. These variations are particularly strong, in for example capacitively coupled plasmas (CCPs), but also easily observable in inductively coupled plasmas (ICPs), and can be exploited for insight into power dissipation. Interesting kinetic and non-linear coupling effects are revealed in capacitive systems. The electron dynamics exhibits a complex spatio-temporal structure. Excitation and ionisation, and, therefore, plasma sustainment is dominated through directed energetic electrons created through the dynamics of the plasma boundary sheath. In the relatively simple case of an asymmetric capacitively coupled rf plasma the complexity of the power dissipation is exposed and various mode transitions can be clearly observed and investigated. At higher pressure secondary electrons dominate the

  1. Mass spectrometry characterization of the thermal decomposition/digestion (TDD) at cysteine in peptides and proteins in the condensed phase.

    Science.gov (United States)

    Basile, Franco; Zhang, Shaofeng; Kandar, Sujit Kumar; Lu, Liang

    2011-11-01

    We report on the characterization by mass spectrometry (MS) of a rapid, reagentless and site-specific cleavage at the N-terminus of the amino acid cysteine (C) in peptides and proteins induced by the thermal decomposition at 220-250 °C for 10 s in solid samples. This thermally induced cleavage at C occurs under the same conditions and simultaneously to our previously reported thermally induced site-specific cleavage at the C-terminus of aspartic acid (D) (Zhang, S.; Basile, F. J. Proteome Res. 2007, 6, (5), 1700-1704). The C cleavage proceeds through cleavage of the nitrogen and α-carbon bond (N-terminus) of cysteine and produces modifications at the cleavage site with an amidation (-1 Da) of the N-terminal thermal decomposition product and a -32 Da mass change of the C-terminal thermal decomposition product, the latter yielding either an alanine or β-alanine residue at the N-terminus site. These modifications were confirmed by off-line thermal decomposition electrospray ionization (ESI)-MS, tandem MS (MS/MS) analyses and accurate mass measurements of standard peptides. Molecular oxygen was found to be required for the thermal decomposition and cleavage at C as it induced an initial cysteine thiol side chain oxidation to sulfinic acid. Similar to the thermally induced D cleavage, missed cleavages at C were also observed. The combined thermally induced digestion process at D and C, termed thermal decomposition/digestion (TDD), was observed on several model proteins tested under ambient conditions and the site-specificity of the method confirmed by MS/MS.

  2. Thermal erosion of cratonic lithosphere as a potential trigger for mass-extinction

    Science.gov (United States)

    Pilet, Sebastien; Guex, Jean; Muntener, Othmar; Bartolini, Annachiara; Spangenberg, Jorge; Schoene, Blair; Schaltegger, Urs

    2016-04-01

    The temporal coincidence between large igneous provinces (LIPs) and mass extinctions has led many to pose a causal relationship between the two. However, there is still no consensus on a mechanistic model that explains how magmatism leads to the turnover of terrestrial and marine plants, invertebrates and vertebrates. Here, we present a synthesis of stratigraphic constraints on the Triassic-Jurassic (T-J) and Pliensbachian-Toarcian (Pl-To) boundaries combined with geochronological data in order to establish the sequence of events that initiate two of the major mass extinctions recorded in Earth's history. This synthesis demonstrates that these biotic crises are both associated with rapid change from an initial cool period to greenhouse conditions. The initial regressive events recorded at T-J and Pl-To boundaries seem difficult to reconcile either with large initial CO2 degassing associated with plume activity or by volatile-release (CO2, CH4, Cl2) from deep sedimentary reservoirs during contact metamorphism associated to dykes and sills intrusion because massive CO2 degassing is expected to produce super greenhouse conditions. We evaluate, here, an alternative suggesting that the initial cooling could be due to gas release during the initial thermal erosion of the cratonic lithosphere due to emplacement of the CAMP and Karoo-Ferrar volcanic provinces. Petrological constraints on primary magmas indicate that the mantle is hotter and melts more extensively to produce LIP lavas than for current oceanic islands basalts. However, available data suggest that the Karoo and CAMP areas were underlain by thick lithosphere (>200 km) prior to continental break up. The presence of thick lithosphere excludes significant melting of the asthenospheric mantle without initial stage of thermal erosion of the cratonic lithosphere. This initial step of thermal erosion / thermal heating of the cratonic lithosphere is critical to understand the volatile budget associated with LIPs while

  3. Separation Techniques for Uranium and Plutonium at Trace Levels for the Thermal Ionization Mass Spectrometric Determination

    Energy Technology Data Exchange (ETDEWEB)

    Suh, M. Y.; Han, S. H.; Kim, J. G.; Park, Y. J.; Kim, W. H

    2005-12-15

    This report describes the state of the art and the progress of the chemical separation and purification techniques required for the thermal ionization mass spectrometric determination of uranium and plutonium in environmental samples at trace or ultratrace levels. Various techniques, such as precipitation, solvent extraction, extraction chromatography, and ion exchange chromatography, for separation of uranium and plutonium were evaluated. Sample preparation methods and dissolution techniques for environmental samples were also discussed. Especially, both extraction chromatographic and anion exchange chromatographic procedures for uranium and plutonium in environmental samples, such as soil, sediment, plant, seawater, urine, and bone ash were reviewed in detail in order to propose some suitable methods for the separation and purification of uranium and plutonium from the safeguards environmental or swipe samples. A survey of the IAEA strengthened safeguards system, the clean room facility of IAEA's NWAL(Network of Analytical Laboratories), and the analytical techniques for safeguards environmental samples was also discussed here.

  4. Resonant multiphoton ionisation probe of the photodissociation dynamics of ammonia.

    Science.gov (United States)

    Smith, Adam D; Watts, Hannah M; Jager, Edward; Horke, Daniel A; Springate, Emma; Alexander, Oliver; Cacho, Cephise; Chapman, Richard T; Minns, Russell S

    2016-10-12

    The dissociation dynamics of the Ã-state of ammonia have been studied using a resonant multiphoton ionisation probe in a photoelectron spectroscopy experiment. The use of a resonant intermediate in the multiphoton ionisation process changes the ionisation propensity, allowing access to different ion states when compared with equivalent single photon ionisation experiments. Ionisation through the E' 1A1' Rydberg intermediate means we maintain overlap with the ion state for an extended period, allowing us to monitor the excited state population for several hundred femtoseconds. The vibrational states in the photoelectron spectrum show two distinct timescales, 200 fs and 320 fs, that we assign to the non-adiabatic and adiabatic dissociation processes respectively. The different timescales derive from differences in the wavepacket trajectories for the two dissociation pathways that resonantly excite different vibrational states in the intermediate Rydberg state. The timescales are similar to those obtained from time resolved ion kinetic energy release measurements, suggesting we can measure the different trajectories taken out to the region of conical intersection.

  5. Utilizing Thermal Mass in Refrigerated Display Cases to Reduce Peak Demand

    Energy Technology Data Exchange (ETDEWEB)

    Fricke, Brian A [ORNL; Kuruganti, Teja [ORNL; Nutaro, James J [ORNL; Fugate, David L [ORNL; Sanyal, Jibonananda [ORNL

    2016-01-01

    The potential to store energy within refrigerated food products presents convenience store and supermarket operators with an opportunity to participate in utility sponsored demand response programs, whereby electricity usage can be shifted or reduced during peak periods. To determine the feasibility of reducing peak demand by shifting the refrigeration load to off-peak times, experimental and analytical analyses were performed. Simulated product, consisting of one-pint containers filled with a 50% ethylene glycol and 50% water solution, were stored in a medium-temperature vertical open refrigerated display case. Product temperature rise as a function of time was determined by turning off the refrigeration to the display case, while product temperature pull-down time was subsequently determined by turning on the refrigeration to the display case. It was found that the thermal mass of the product in a medium-temperature display case was such that during a 2.5 hour period with no refrigeration, the average product temperature increased by 5.5 C. In addition, it took approximately 3.5 hours for the product to recover to its initial temperature after the refrigeration was turned on. Transient heat conduction analyses for one-dimensional objects is in good agreement with the experimental results obtained in this study. From the analysis, it appears that the thermal mass of the stored product in refrigerated display cases is sufficient to allow product temperatures to safely drift for a significant time under reduced refrigeration system operation. Thus, strategies for shifting refrigeration system electrical demand can be developed. The use of an advanced refrigeration system controller that can respond to utility signals can enable demand shifting with minimal impact.

  6. Thermal desorption gas chromatography with mass spectrometry study of outgassing from polymethacrylimide foam (Rohacell®).

    Science.gov (United States)

    Carrasco-Correa, Enrique J; Herrero-Martínez, José M; Consuegra, Lina; Ramis-Ramos, Guillermo; Sanz, Rafael Mata; Martínez, Benito Gimeno; Esbert, Vicente E Boria; García-Baquero, David Raboso

    2015-09-01

    Polymethacrylimide foams are used as light structural materials in outer-space devices; however, the foam closed cells contain volatile compounds that are outgassed even at low temperatures. These compounds ignite as plasmas under outer-space radiation and the intense radio-frequency fields used in communications. Since plasmas may cause spacecraft fatal events, the conditions in which they are ignited should be investigated. Therefore, qualitative and quantitative knowledge about polymethacrylimide foam outgassing should be established. Using thermogravimetric analysis, weight losses reached 3% at ca. 200°C. Thermal desorption gas chromatography with mass spectrometry detection was used to study the offgassed compounds. Using successive 4 min heating cycles at 125°C, each one corresponding to an injection, significant amounts of nitrogen (25.3%), water (2.6%), isobutylene (11.3%), tert-butanol (2.9%), 1-propanol (11.9%), hexane (25.3%), propyl methacrylate (1.4%), higher hydrocarbons (11.3%), fatty acids (2.2%) and their esters (1.3%), and other compounds were outgassed. Other compounds were observed during the main stage of thermal destruction (220-280°C). A similar study at 175°C revealed the extreme difficulty in fully outgassing polar compounds from polymethacrylimide foams by baking and showed the different compositions of the offgassed atmosphere that can be expected in the long term. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Mass spectrometric comparison of swift heavy ion-induced and anaerobic thermal degradation of polymers

    Science.gov (United States)

    Lima, V.; Hossain, U. H.; Walbert, T.; Seidl, T.; Ensinger, W.

    2018-03-01

    The study of polymers irradiated by highly energetic ions and the resulting radiation-induced degradation is of major importance for space and particle accelerator applications. The mechanism of ion-induced molecular fragmentation of polyethylene, polyethyleneimine and polyamide was investigated by means of mass spectrometry and infrared spectroscopy. The results show that the introduction of nitrogen and oxygen into the polymer influences the stability rendering aliphatic polymers with heteroatoms less stable. A comparison to thermal decomposition data from literature reveals that ion-induced degradation is different in its bond fracture mechanism. While thermal degradation starts at the weakest bond, which is usually the carbon-heteroatom bond, energetic ion irradiation leads in the first step to scission of all types of bonds creating smaller molecular fragments. This is due to the localized extreme energy input under non-equilibrium conditions when the ions transfer kinetic energy onto electrons. These findings are of relevance for the choice of polymers for long-term application in both space and accelerator facilities.

  8. Performance of thermal deposition and mass flux condition on bioconvection nanoparticles containing gyrotactic microorganisms

    Science.gov (United States)

    Iqbal, Z.; Ahmad, Bilal

    2017-11-01

    This is an attempt to investigate the influence of thermal radiation on the movement of motile gyrotactic microorganisms submerged in a water-based nanofluid flow over a nonlinear stretching sheet. The mathematical modeling of this physical problem leads to a system of nonlinear coupled partial differential equations. The problem is tackled by converting nonlinear partial differential equations into the system of highly nonlinear ordinary differential equations. The resulting nonlinear equations of momentum, energy, concentration of nanoparticles and motile gyrotactic microorganisms along with the mass flux condition are solved numerically by means of a shooting algorithm. The effects of the involved physical parameters of interest are discussed graphically. The values of the skin friction coefficient, Nusselt number, Sherwood number and local density number of motile microorganisms are tabulated for detailed analysis on the flow pattern at the stretching surface. It is concluded that the nanofluid temperature is an increasing function of the thermal radiation and the Biot number parameter. An opposite trend is observed for the local Nusselt number. The association with the preceding results in limiting sense is shown as well. A tremendous agreement of the current study in a restrictive manner is achieved as well. In addition, flow configurations through stream functions are presented and deliberated significantly.

  9. Asymmetric resonance response analysis of a thermally excited silicon microcantilever for mass-sensitive nanoparticle detection

    Science.gov (United States)

    Bertke, Maik; Hamdana, Gerry; Wu, Wenze; Wasisto, Hutomo Suryo; Peiner, Erwin

    2017-06-01

    The asymmetric resonance responses of a thermally actuated silicon microcantilever of a portable, cantilever-based nanoparticle detector (Cantor) is analysed. For airborne nanoparticle concentration measurements, the cantilever is excited in its first in-plane bending mode by an integrated p-type heating actuator. The mass-sensitive nanoparticle (NP) detection is based on the resonance frequency (f0) shifting due to the deposition of NPs. A homemade phase-locked loop (PLL) circuit is developed for tracking of f0. For deflection sensing the cantilever contains an integrated piezo-resistive Wheatstone bridge (WB). A new fitting function based on the Fano resonance is proposed for analysing the asymmetric resonance curves including a method for calculating the quality factor Q from the fitting parameters. To obtain a better understanding, we introduce an electrical equivalent circuit diagram (ECD) comprising a series resonant circuit (SRC) for the cantilever resonator and voltage sources for the parasitics, which enables us to simulate the asymmetric resonance response and discuss the possible causes. Furthermore, we compare the frequency response of the on-chip thermal excitation with an external excitation using an in-plane piezo actuator revealing parasitic heating of the WB as the origin of the asymmetry. Moreover, we are able to model the phase component of the sensor output using the ECD. Knowing and understanding the phase response is crucial to the design of the PLL and thus the next generation of Cantor.

  10. Investigation of the impact of using thermal mass with the net zero energy town house in Toronto using TRNSYS

    Energy Technology Data Exchange (ETDEWEB)

    Siddiqui, O.; Fung, A.; Tse, H.; Zhang, D. [Ryerson Polytechnic Univ., Toronto, ON (Canada). Dept. of Mechanical and Industrial Engineering

    2008-07-01

    Since buildings in Canada account for 30 per cent of the country's total energy consumption, it has become necessary to find ways to reduce the overall energy use in buildings. Heating and cooling loads in buildings can be effectively reduced by using the thermal mass incorporated into the building envelope, particularly in climates where a large daily temperature fluctuations exist. Thermal mass is defined as any building material that has a high heat storage capacity that can be integrated into the structural fabric of the building to use the passive solar energy for heating or cooling purposes. Concrete slabs, bricks and ceramic blocks are some of the commonly used materials. This study analyzed the impact of using thermal mass with a highly insulated building envelope such as that used in Low Energy or Net Zero housing. In particular, TRNSYS was used to simulate a Net Zero Energy Town House located in Toronto, in which a ground source heat pump was integrated with an infloor radiant heating system. The simulation revealed that for colder climates such as in Canada, thermal mass can replace some of the insulation while still providing excellent results in terms of the reductions in daily indoor temperature fluctuations. The impact of thermal mass during the winter was more significant when compared with summer, possibly because of the unique construction and orientation of the Net Zero Energy House. The optimum thickness of the concrete slab was determined to be 6 inches for the winter season and 4 inches for summer. The optimum location for the thermal mass was found to be right next to the gypsum wallboard that forms the interior part of the wall. 12 refs., 1 tab., 11 figs.

  11. The RF System for the International Muon Ionisation Cooling Experiment

    CERN Document Server

    Ronald, K.; Dick, A.J.; Speirs, D.C.; Moss, A.; Grant, A.; White, C.; Griffiths, S.; Stanley, T.; Li, D.; DeMello, A.J.; Virostek, S.; Moretti, A.; Pasquinelli, R.; Peterson, D.; Schultz, R.; Volk, J.; Popovic, M.; Torun, Y.; Hanlet, P.; Alsari, S.; Long, K.; Pasternak, J.; Hunt, C.; Summers, D.; Luo, T.; Smith, P.J.

    2014-01-01

    The International Muon Ionisation Cooling Experiment (MICE) is designed to demonstrate the effectiveness of ionisation cooling to reduce the phase space footprint of a charged particle beam, principally to allow the subsequent acceleration of muons for next generation colliders and/or neutrino factories. The experiment (and indeed any subsequent accelerator cooling channel based on the same principles) poses certain unusual requirements on its RF system, whilst the precision measurement of the ionisation cooling process demands special diagnostics. This paper shall outline the key features of the RF system, including the low level RF control, the power amplifier chain, distribution network, cavities, tuners and couplers, many parts of which are required to operate in a high magnetic field environment. The RF diagnostics which, in conjunction with the other MICE diagnostics, shall allow detailed knowledge of the amplitude and phase of the acceleration field during the transit of each individual muon will also ...

  12. The effectiveness of photocatalytic ionisation disinfection of filter materials.

    Science.gov (United States)

    Pietrzak, Katarzyna; Gutarowska, Beata

    2013-01-01

    The purpose of this study was to determine the effectiveness of photocatalytic ionisation as a disinfection method for filter materials contaminated by microorganisms, and to assess how air relative humidity (RH), time and microbe type influence the effectiveness of this disinfection. In the quantitative analysis of a used car air filter, bacterial contamination equalled 1.2 x 10(5) cfu/cm2, fungal contamination was 3.8 x 10(6) cfu/cm2, and the isolated microorganisms were Aspergillus niger, Bacillus megaterium, Cladosporium herbarum, Cryptococcus laurenti, Micrococcus sp., Rhodotorula glutinis and Staphylococcus cohnii. In the model experiment, three isolates (C. herbarum, R. glutinis, S. cohnii) and 3 ATCC species (A. niger, E. coli, S. aureus) were used for photocatalytic ionisation disinfection. The conditions of effective photocatalytic ionisation disinfection (R > or = 99.9%) were established as 2-3 h at RH = 77% (bacteria) and 6-24 h at RH = 53% (fungi). RH has an influence on the effectiveness of the photocatalytic disinfection process; the highest effectiveness was obtained for bacteria at RH = 77%, with results 5% higher than for RH = 49%. The studies show that the sensitivity of microorganisms to photocatalytic ionisation disinfection is ordered as follows: Gram-positive bacteria (S. cohnii, S. aureus), Gram-negative bacteria (E. coli), yeasts (R. glutinis), and moulds (C. herbarum, A. niger). Of all the mathematical models used for the description of death dynamics after photocatalytic ionisation disinfection, the Chick-Watson model is the most useful, but for more resistant microorganisms, the delayed Chick-Watson model is highly recommended. It therefore seems, that the presented disinfection method of photocatalytic ionisation can be successfully used to clean filtration materials.

  13. [Bipolar ionisation of indoor air through ion generators mountable into inflow ventilation and conditioning].

    Science.gov (United States)

    Dudarev, A A; Spichkin, G L; Denisikhina, D M; Burtsev, S I

    2010-01-01

    Experimental studies and digital modelling of artificial indoor air ionisation through bipolar ionisers mountable into inflow ventilation and conditioning proved possible creation of continuous even bipolar ion background in indoor air, similar to the natural one.

  14. Thermal Emission of Alkali Metal Ions from Al30-Pillared Montmorillonite Studied by Mass Spectrometric Method.

    Science.gov (United States)

    Motalov, V B; Karasev, N S; Ovchinnikov, N L; Butman, M F

    2017-01-01

    The thermal emission of alkali metal ions from Al 30 -pillared montmorillonite in comparison with its natural form was studied by mass spectrometry in the temperature range 770-930 K. The measurements were carried out on a magnetic mass spectrometer MI-1201. For natural montmorillonite, the densities of the emission currents ( j ) decrease in the mass spectrum in the following sequence (T = 805 K, A/cm 2 ): K + (4.55 · 10 -14 ), Cs + (9.72 · 10 -15 ), Rb + (1.13 · 10 -15 ), Na + (1.75 · 10 -16 ), Li + (3.37 · 10 -17 ). For Al 30 -pillared montmorillonite, thermionic emission undergoes temperature-time changes. In the low-temperature section of the investigated range (770-805 K), the value of j increases substantially for all ions in comparison with natural montmorillonite (T = 805 K, A/cm 2 ): Cs + (6.47 · 10 -13 ), K + (9.44 · 10 -14 ), Na + (3.34 · 10 -15 ), Rb + (1.77 · 10 -15 ), and Li + (4.59 · 10 -16 ). A reversible anomaly is observed in the temperature range 805-832 K: with increasing temperature, the value of j of alkaline ions falls abruptly. This effect increases with increasing ionic radius of M + . After a long heating-up period, this anomaly disappears and the ln j - 1/ T dependence acquires a classical linear form. The results are interpreted from the point of view of the dependence of the efficiency of thermionic emission on the phase transformations of pillars.

  15. Laser-modified electron scattering from a slowly ionising atom

    Science.gov (United States)

    Fiordilino, E.; Mittleman, M. H.

    1983-01-01

    When an electron scatters from an atom in the presence of a laser field which is resonant with an atomic transition, off-shell effects enter into the cross section. These only become significant at higher laser intensities where the atom may also be ionised by the laser. Cross-sections are obtained for electron-atom scattering in which these off-shell effects appear and in which the slow ionisation of the atom by the laser is included. Experiments are suggested in which simplifications can occur and which still retain these 'exotic' effects.

  16. Binary-Encounter-Bethe ionisation cross sections for simulation of DNA damage by the direct effect of ionising radiation.

    Science.gov (United States)

    Plante, I; Cucinotta, F A

    2015-09-01

    DNA damage is of crucial importance in the understanding of the effects of ionising radiation. To refine existing DNA damage models, an approach using the Binary-Encounter-Bethe (BEB) cross sections was developed. The differential cross sections for ionisation of the molecular orbitals of the DNA bases, sugars and phosphates are calculated using the electron binding energy, the mean kinetic energy and the occupancy number of each orbital as parameters. The resulting cross section has an analytic form which is quite convenient to use for Monte-Carlo codes that randomly sample the energy loss occurring during an ionisation event. We also describe an algorithm to simulate the interactions of electrons with DNA in the radiation transport code RITRACKS using the integrated BEB cross section for the bases, sugar and phosphates. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  17. Thermal erosion of cratonic lithosphere as a potential trigger for mass-extinction

    Science.gov (United States)

    Pilet, S.; Müntener, O.; Jean, G.; Schoene, B.; Schaltegger, U.

    2016-12-01

    The temporal coincidence between LIPs and mass extinctions has led many to pose a causal relationship between the two. However, there is still no consensus on a mechanistic model that explains how magmatism leads to the turnover of terrestrial and marine plants, invertebrates and vertebrates. Here, we present a synthesis of stratigraphic constraints on the Triassic-Jurassic and Pliensbachian-Toarcian boundaries combined with geochronological data demonstrating that these biotic crises are both associated with rapid change from an initial cool period to greenhouse conditions. As current hypothesis for LIPs seems unable to produce these successive climatic changes, we evaluate an alternative suggesting that the initial cooling could be due to gas release during the initial thermal erosion of the cratonic lithosphere due to emplacement of the CAMP and Karoo-Ferrar volcanic provinces. Karoo and CAMP areas were underlain by thick lithosphere (>200 km) prior to continental break up. Even in presence of abnormal potential mantle temperature, the presence of thick lithosphere excludes significant melting of the asthenospheric mantle without initial stage of thermal erosion of the cratonic lithosphere. Various studies on Kaapvaal craton have shown that sulfide minerals are enclosed in the basal part of the cratonic lithosphere. We argue that initial gas emission was dominated by sulfur liberated from sulfide-bearing cratonic lithosphere causing global cooling and eustatic regression, which was followed by warming/transgression associated with the progressive increase of CO2 in the atmosphere associated to LIPs emission. We suggest that the nature of the underlying lithosphere during large LIP eruption exerts an important control on the consequences at the Earth's surface. This model offers an explanation for why LIPs erupted through oceanic lithosphere are not associated with climatic and biotic crises comparable to LIPs emitted through cratonic lithosphere.

  18. Essentials of iron, chromium, and calcium isotope analysis of natural materials by thermal ionization mass spectrometry

    Science.gov (United States)

    Fantle, M.S.; Bullen, T.D.

    2009-01-01

    The use of isotopes to understand the behavior of metals in geological, hydrological, and biological systems has rapidly expanded in recent years. One of the mass spectrometric techniques used to analyze metal isotopes is thermal ionization mass spectrometry, or TIMS. While TIMS has been a useful analytical technique for the measurement of isotopic composition for decades and TIMS instruments are widely distributed, there are significant difficulties associated with using TIMS to analyze isotopes of the lighter alkaline earth elements and transition metals. Overcoming these difficulties to produce relatively long-lived and stable ion beams from microgram-sized samples is a non-trivial task. We focus here on TIMS analysis of three geologically and environmentally important elements (Fe, Cr, and Ca) and present an in-depth look at several key aspects that we feel have the greatest potential to trouble new users. Our discussion includes accessible descriptions of different analytical approaches and issues, including filament loading procedures, collector cup configurations, peak shapes and interferences, and the use of isotopic double spikes and related error estimation. Building on previous work, we present quantitative simulations, applied specifically in this study to Fe and Ca, that explore the effects of (1) time-variable evaporation of isotopically homogeneous spots from a filament and (2) interferences on the isotope ratios derived from a double spike subtraction routine. We discuss how and to what extent interferences at spike masses, as well as at other measured masses, affect the double spike-subtracted isotope ratio of interest (44Ca/40Ca in the case presented, though a similar analysis can be used to evaluate 56Fe/54Fe and 53Cr/52Cr). The conclusions of these simulations are neither intuitive nor immediately obvious, making this examination useful for those who are developing new methodologies. While all simulations are carried out in the context of a

  19. Structure investigation of codeine drug using mass spectrometry, thermal analyses and semi-emperical molecular orbital (MO) calculations

    Science.gov (United States)

    Zayed, M. A.; Hawash, M. F.; Fahmey, M. A.

    2006-05-01

    Codeine is an analgesic with uses similar to morphine, but it has a mild sedative effect. It is preferable used as phosphate form and it is often administrated by mouth with aspirin or paracetamol. Therefore, it is important to investigate its structure to know the active groups and weak bonds responsible for its medical activity. Consequently in the present work, codeine was investigated by mass spectrometry and thermal analyses (TG, DTG and DTA) and confirming by semi-empirical MO-calculation (PM3 method) in the neutral and positively charged forms of the drug. Some results of studying the d-block element complexes of codeine were used to declare the relationship between drug structure and its chemical reactivity in vitro system. The mass spectra and thermal analyses fragmentation pathways were proposed and compared to each other to select the most suitable scheme representing the correct fragmentation of this drug. From EI mass spectra, the main primary cleavage site of the charged drug molecule is that due to β-cleavage to nitrogen atom in its skeleton. It occurs in two parallel mechanisms with the same possibility, i.e. no difference in appearance activation energy between them. In the neutral drug form the primary site cleavage is that occurs in the ether ring. Thermal analyses of the neutral form of the drug revealed the high response of the drug to the temperature variation with very fast rate. It decomposed in several sequential steps in the temperature range 200-600 °C. The initial thermal fragments are very similar to that obtained by mass spectrometric fragmentation. Therefore, comparison between mass and thermal helps in selection of the proper pathway representing the fragmentation of this drug. This comparison successfully confirmed by MOC. These calculations give the bond order, charge distribution, heat of formation and possible hybridization of some atoms in different position of the drug skeleton. This helps the successful choice of the weakest

  20. A longitudinal thermal actuation principle for mass detection using a resonant micro -cantilever in a fluid medium

    DEFF Research Database (Denmark)

    Grigorov, Alexander; Davis, Zachary James; Rasmussen, Peter

    2004-01-01

    from existing thermal actuation configurations as the actuation acts on the base of the cantilever device, as opposed to the whole length of the device, separating cantilever and actuator. This allows much bigger freedom in optimizing separately the dimensions of cantilever and actuator. Optimizing...... the mass sensitivity of the device depends on the relative and absolute dimensions of the cantilever, by limiting fluid damping, displaced mass and cantilever mass. The ability to detect resonance shifts depends on the resonant amplitude, which can be optimized by varying the actuator dimensions and shape...

  1. Laser diode thermal desorption mass spectrometry for the analysis of quinolone antibiotic residues in aquacultured seafood.

    Science.gov (United States)

    Lohne, Jack J; Andersen, Wendy C; Clark, Susan B; Turnipseed, Sherri B; Madson, Mark R

    2012-12-30

    Veterinary drug residue analysis of meat and seafood products is an important part of national regulatory agency food safety programs to ensure that consumers are not exposed to potentially dangerous substances. Complex tissue matrices often require lengthy extraction and analysis procedures to identify improper animal drug treatment. Direct and rapid analysis mass spectrometry techniques have the potential to increase regulatory sample analysis speed by eliminating liquid chromatographic separation. Flumequine, oxolinic acid, and nalidixic acid were extracted from catfish, shrimp, and salmon using acidified acetonitrile. Extracts were concentrated, dried onto metal sample wells, then rapidly desorbed (6 s) with an infrared diode laser for analysis by laser diode thermal desorption atmospheric pressure chemical ionization with tandem mass spectrometry (LDTD-MS/MS). Analysis was conducted in selected reaction monitoring mode using piromidic acid as internal standard. Six-point calibration curves for each compound in extracted matrix were linear with r(2) correlation greater than 0.99. The method was validated by analyzing 23 negative samples and 116 fortified samples at concentrations of 10, 20, 50, 100, and 600 ng/g. Average recoveries of fortified samples were greater than 77% with method detection levels ranging from 2 to 7 /g. Three product ion transitions were acquired per analyte to identify each residue. A rapid method for quinolone analysis in fish muscle was developed using LDTD-MS/MS. The total analysis time was less than 30 s per sample; quinolone residues were detected below 10 ng/g and in most cases residue identity was confirmed. This represents the first application of LDTD to tissue extract analysis. Published 2012. This article is a US Government work and is in the public domain in the USA. Published 2012. This article is a US Government work and is in the public domain in the USA.

  2. Evaluation of injection methods for fast, high peak capacity separations with low thermal mass gas chromatography.

    Science.gov (United States)

    Fitz, Brian D; Mannion, Brandyn C; To, Khang; Hoac, Trinh; Synovec, Robert E

    2015-05-01

    Low thermal mass gas chromatography (LTM-GC) was evaluated for rapid, high peak capacity separations with three injection methods: liquid, headspace solid phase micro-extraction (HS-SPME), and direct vapor. An Agilent LTM equipped with a short microbore capillary column was operated at a column heating rate of 250 °C/min to produce a 60s separation. Two sets of experiments were conducted in parallel to characterize the instrumental platform. First, the three injection methods were performed in conjunction with in-house built high-speed cryo-focusing injection (HSCFI) to cryogenically trap and re-inject the analytes onto the LTM-GC column in a narrower band. Next, the three injection methods were performed natively with LTM-GC. Using HSCFI, the peak capacity of a separation of 50 nl of a 73 component liquid test mixture was 270, which was 23% higher than without HSCFI. Similar peak capacity gains were obtained when using the HSCFI with HS-SPME (25%), and even greater with vapor injection (56%). For the 100 μl vapor sample injected without HSCFI, the preconcentration factor, defined as the ratio of the maximum concentration of the detected analyte peak relative to the analyte concentration injected with the syringe, was determined to be 11 for the earliest eluting peak (most volatile analyte). In contrast, the preconcentration factor for the earliest eluting peak using HSCFI was 103. Therefore, LTM-GC is demonstrated to natively provide in situ analyte trapping, although not to as great an extent as with HSCFI. We also report the use of LTM-GC applied with time-of-flight mass spectrometry (TOFMS) detection for rapid, high peak capacity separations from SPME sampled banana peel headspace. Copyright © 2015 Elsevier B.V. All rights reserved.

  3. Risques spécifiques du CERN : rayonnements ionisants

    CERN Multimedia

    CERN; Daniel Boileau

    1991-01-01

    Précautions - Instructions - Dosimètres - Différentes zones - Accès règlementés - Dangers particuliers - Panneaux d'information - Stockage de matériaux - Règles de transport - Rayonnements ionisants - Lasers.

  4. Connecting stars and ionised gas with integral-field spectroscopy

    NARCIS (Netherlands)

    McDermid, Richard M.; Emsellem, Eric; Shapiro, Kristen L.; Bacon, Roland; Bureau, Martin; Cappellari, Michele; Davies, Roger L.; de Zeeuw, Tim; Falcon-Barroso, Jesus; Krajnovic, Davor; Kuntschner, Harald; Peletier, Reynier F.; Sarzi, Marc; van de Ven, Glenn

    Using integral-field spectroscopy, the SAURON survey has shown that early-type galaxies, once thought to be essentially devoid of gas, commonly show ionised gas emission. This emission is found with a rich variety of distributions and kinematics, ranging from very uniform disks or rings, and

  5. Unbiased metal oxide semiconductor ionising radiation dosemeter

    Energy Technology Data Exchange (ETDEWEB)

    Kumurdjian, N.; Sarrabayrouse, G.J.

    1995-12-31

    To assess the application of MOS devices as low dose rate dosemeters, the sensitivity is the major factor although little studies have been performed on that subject. It is studied here, as well as thermal stability and linearity of the response curve. Other advantages are specified such as large measurable dose range, low cost, small size, possibility of integration. (D.L.). 21 refs.

  6. Separation and Analysis of Boron Isotope in High Plant by Thermal Ionization Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Qingcai Xu

    2015-01-01

    Full Text Available Knowledge of boron and its isotope in plants is useful to better understand the transposition and translocation of boron within plant, the geochemical behavior in the interface between soil and plant, and the biogeochemical cycle of boron. It is critical to develop a useful method to separate boron from the plant for the geochemical application of boron and its isotope. A method was developed for the extraction of boron in plant sample, whose isotope was determined by thermal ionization mass spectrometry. The results indicated that this method of dry ashing coupled with two-step ion-exchange chromatography is powerful for the separation of boron in plant sample with large amounts of organic matters completely. The ratios of boron isotope composition in those plant tissue samples ranged from -19.45‰ to +28.13‰ (total range: 47.58‰ with a mean value of 2.61±11.76‰ SD. The stem and root isotopic compositions were lower than those in flower and leaf. The molecular mechanism of boron isotope may be responsible for the observed variation of boron isotopic composition and are considered as a useful tool for the better understanding of boron cycling process in the environment and for the signature of living systems.

  7. Demand Shifting with Thermal Mass in Large Commercial Buildings in a California Hot Climate Zone

    Energy Technology Data Exchange (ETDEWEB)

    Xu, Peng; Yin, Rongxin; Brown, Carrie; Kim, DongEun

    2009-06-01

    The potential for using building thermal mass for load shifting and peak energy demand reduction has been demonstrated in a number of simulation, laboratory, and field studies. Previous Lawrence Berkeley National Laboratory research has demonstrated that the approach is very effective in cool and moderately warm climate conditions (California Climate Zones 2-4). However, this method had not been tested in hotter climate zones. This project studied the potential of pre-cooling the building early in the morning and increasing temperature setpoints during peak hours to reduce cooling-related demand in two typical office buildings in hotter California climates ? one in Visalia (CEC Climate Zone 13) and the other in San Bernardino (CEC Climate Zone 10). The conclusion of the work to date is that pre-cooling in hotter climates has similar potential to that seen previously in cool and moderate climates. All other factors being equal, results to date indicate that pre-cooling increases the depth (kW) and duration (kWh) of the possible demand shed of a given building. The effectiveness of night pre-cooling in typical office building under hot weather conditions is very limited. However, night pre-cooling is helpful for office buildings with an undersized HVAC system. Further work is required to duplicate the tests in other typical buildings and in other hot climate zones and prove that pre-cooling is truly effective.

  8. A new approach to the correlation of boundary layer mass transfer rates with thermal diffusion and/or variable properties

    Science.gov (United States)

    Srivastava, R.; Rosner, D. E.

    1979-01-01

    A rational approach to the correlation of boundary layer mass transport rates, applicable to many commonly encountered laminar flow conditions with thermal diffusion and/or variable properties, is outlined. The correlation scheme builds upon already available constant property blowing/suction solutions by introducing appropriate correction factors to account for the additional ('pseudo' blowing and source) effects identified with variable properties and thermal diffusion. Applications of the scheme to the particular laminar boundary layer mass transfer problems considered herein (alkali and transition metal compound vapor transport) indicates satisfactory accuracy up to effective blowing factors equivalent to about one third of the 'blow off' value. As a useful by-product of the variable property correlation, we extend the heat-mass transfer analogy, for a wide range of Lewis numbers, to include variable property effects.

  9. High-precision measurements of seawater Pb isotope compositions by double spike thermal ionization mass spectrometry.

    Science.gov (United States)

    Paul, Maxence; Bridgestock, Luke; Rehkämper, Mark; van DeFlierdt, Tina; Weiss, Dominik

    2015-03-10

    A new method for the determination of seawater Pb isotope compositions and concentrations was developed, which combines and optimizes previously published protocols for the separation and isotopic analysis of this element. For isotopic analysis, the procedure involves initial separation of Pb from 1 to 2L of seawater by co-precipitation with Mg hydroxide and further purification by a two stage anion exchange procedure. The Pb isotope measurements are subsequently carried out by thermal ionization mass spectrometry using a (207)Pb-(204)Pb double spike for correction of instrumental mass fractionation. These methods are associated with a total procedural Pb blank of 28±21 pg (1sd) and typical Pb recoveries of 40-60%. The Pb concentrations are determined by isotope dilution (ID) on 50 mL of seawater, using a simplified version of above methods. Analyses of multiple aliquots of six seawater samples yield a reproducibility of about ±1 to ±10% (1sd) for Pb concentrations of between 7 and 50 pmol/kg, where precision was primarily limited by the uncertainty of the blank correction (12±4 pg; 1sd). For the Pb isotope analyses, typical reproducibilities (±2sd) of 700-1500 ppm and 1000-2000 ppm were achieved for (207)Pb/(206)Pb, (208)Pb/(206)Pb and (206)Pb/(204)Pb, (207)Pb/(204)Pb, (208)Pb/(204)Pb, respectively. These results are superior to literature data that were obtained using plasma source mass spectrometry and they are at least a factor of five more precise for ratios involving the minor (204)Pb isotope. Both Pb concentration and isotope data, furthermore, show good agreement with published results for two seawater intercomparison samples of the GEOTRACES program. Finally, the new methods were applied to a seawater depth profile from the eastern South Atlantic. Both Pb contents and isotope compositions display a smooth evolution with depth, and no obvious outliers. Compared to previous Pb isotope data for seawater, the (206)Pb/(204)Pb ratios are well correlated

  10. Coincidence angular correlation in electron impact single or double ionisation of atoms and molecules

    Energy Technology Data Exchange (ETDEWEB)

    Casagrande, E M Staicu [Laboratoire des Collisions Atomiques et Moleculaires (UMR 862), Bat. 351, Universite de Paris-Sud XI, 91405 Orsay Cedex (France); Naja, A [Laboratoire des Collisions Atomiques et Moleculaires (UMR 862), Bat. 351, Universite de Paris-Sud XI, 91405 Orsay Cedex (France); Ren, X G [Laboratoire des Collisions Atomiques et Moleculaires (UMR 862), Bat. 351, Universite de Paris-Sud XI, 91405 Orsay Cedex (France); Nekkab, M [Laboratoire de Physique Quantique et Systemes Dynamiques, Universite Ferhat Abbas, Setif (Algeria); Catoire, F [Laboratoire des Collisions Atomiques et Moleculaires (UMR 862), Bat. 351, Universite de Paris-Sud XI, 91405 Orsay Cedex (France); Mezdari, F [Laboratoire des Collisions Atomiques et Moleculaires (UMR 862), Bat. 351, Universite de Paris-Sud XI, 91405 Orsay Cedex (France); Lahmam-Bennani, A [Laboratoire des Collisions Atomiques et Moleculaires (UMR 862), Bat. 351, Universite de Paris-Sud XI, 91405 Orsay Cedex (France); Madison, D [Department of Physics, University of Missoun-Rolla, Rolla, Missouri 65409 (United States); Chuluunbaatar, O [Joint Institute for Nuclear research, Dubna, Moscow region 141980 (Russian Federation); Joulakian, B [Universite Paul Verlaine-Metz, Laboratoire de Physique Moleculaire et des Collisions (FR 2843), Institut de Physique, 1 rue Arago, 57078 Metz Cedex 3 (France)

    2007-11-15

    Experimental results obtained with our multi parameter multi-coincidence spectrometer are presented for the (e,3e) double ionisation of Ar and (e,2e) single ionisation of small molecules. The (e,3e) measurements are discussed in terms of competition between the two double ionisation processes present under the chosen kinematics, and qualitative conclusions are given. The results for the ionisation of H{sub 2} and the outer orbital of N{sub 2} are compared with the predictions of the most elaborate available theoretical models for description of the molecular ionisation process. Overall reasonable agreement is observed and tentative interpretations for the discrepancies are discussed.

  11. Evolution of thermally pulsing asymptotic giant branch stars. IV. Constraining mass loss and lifetimes of low mass, low metallicity AGB stars

    Energy Technology Data Exchange (ETDEWEB)

    Rosenfield, Philip; Dalcanton, Julianne J.; Weisz, Daniel; Williams, Benjamin F. [Department of Astronomy, University of Washington, Box 351580, Seattle, WA 98195 (United States); Marigo, Paola [Department of Physics and Astronomy G. Galilei, University of Padova, Vicolo dell' Osservatorio 3, I-35122 Padova (Italy); Girardi, Léo; Gullieuszik, Marco [Osservatorio Astronomico di Padova—INAF, Vicolo dell' Osservatorio 5, I-35122 Padova (Italy); Bressan, Alessandro [Astrophysics Sector, SISSA, Via Bonomea 265, I-34136 Trieste (Italy); Dolphin, Andrew [Raytheon Company, 1151 East Hermans Road, Tucson, AZ 85756 (United States); Aringer, Bernhard [Department of Astrophysics, University of Vienna, Turkenschanzstraße 17, A-1180 Wien (Austria)

    2014-07-20

    The evolution and lifetimes of thermally pulsating asymptotic giant branch (TP-AGB) stars suffer from significant uncertainties. In this work, we analyze the numbers and luminosity functions of TP-AGB stars in six quiescent, low metallicity ([Fe/H] ≲ –0.86) galaxies taken from the ACS Nearby Galaxy Survey Treasury sample, using Hubble Space Telescope (HST) photometry in both optical and near-infrared filters. The galaxies contain over 1000 TP-AGB stars (at least 60 per field). We compare the observed TP-AGB luminosity functions and relative numbers of TP-AGB and red giant branch (RGB) stars, N{sub TP-AGB}/N{sub RGB}, to models generated from different suites of TP-AGB evolutionary tracks after adopting star formation histories derived from the HST deep optical observations. We test various mass-loss prescriptions that differ in their treatments of mass loss before the onset of dust-driven winds (pre-dust). These comparisons confirm that pre-dust mass loss is important, since models that neglect pre-dust mass loss fail to explain the observed N{sub TP-AGB}/N{sub RGB} ratio or the luminosity functions. In contrast, models with more efficient pre-dust mass loss produce results consistent with observations. We find that for [Fe/H] ≲ –0.86, lower mass TP-AGB stars (M ≲ 1 M{sub ☉}) must have lifetimes of ∼0.5 Myr and higher masses (M ≲ 3 M{sub ☉}) must have lifetimes ≲ 1.2 Myr. In addition, assuming our best-fitting mass-loss prescription, we show that the third dredge-up has no significant effect on TP-AGB lifetimes in this mass and metallicity range.

  12. Kinematic and Thermal Structure at the onset of high-mass star formation

    Science.gov (United States)

    Bihr, Simon; Beuther, Henrik

    2015-08-01

    Even though high-mass stars are crucial for understanding a diversity of processes within our galaxy and beyond, their formation and initial conditions are still poorly constrained. We want to understand the kinematic and thermal properties of young massive gas clumps prior to and at the earliest evolutionary stages. Do we find signatures of gravitational collapse? Do we find temperature gradients in the vicinity or absence of infrared emission sources? Do we find coherent velocity structures toward the centre of the dense and cold gas clumps?To determine kinematics and gas temperatures, we used ammonia, because it is known to be a good tracer and thermometer of dense gas. We observed the NH3 (1,1) and (2,2) lines within seven very young high-mass star-forming regions comprised of infrared dark clouds (IRDCs), along with ISO-selected far-infrared emission sources (ISOSS) with the VLA and the Effelsberg 100m telescope. The molecular line data allows us to study velocity structures, linewidths, and gas temperatures at high spatial resolution of 3-5'', corresponding to ~0.05pc at a typical source distance of 2.5kpc. We find on average cold gas clumps with temperatures in the range between 10K and 30K. The observations do not reveal a clear correlation between infrared emission peaks and ammonia temperature peaks. Several infrared emission sources show ammonia temperature peaks up to 30K, whereas other infrared emission sources show no enhanced kinetic gas temperature in their surrounding. We report an upper limit for the linewidth of ~1.3km/s, at the spectral resolution limit of our VLA observation. This indicates a relatively low level of turbulence on the scale of the observations. Velocity gradients are present in almost all regions with typical velocity differences of 1 to 2km/s and gradients of 5 to 10km/s/pc. These velocity gradients are smooth in most cases, but there is one exceptional source (ISOSS23053), for which we find several velocity components with a

  13. Effect of molar ratio on thermal mass loss kinetics of poly({epsilon}-caprolactone-b-propylene adipate) copolymers

    Energy Technology Data Exchange (ETDEWEB)

    Nanaki, Stavroula G. [Laboratory of Polymer Chemistry and Technology, Department of Chemistry, Aristotle University of Thessaloniki, GR-541 24, Thessaloniki, Macedonia (Greece); Chrissafis, K. [Solid State Physics Section, Physics Department, Aristotle University of Thessaloniki, GR-541 24, Thessaloniki, Macedonia (Greece); Bikiaris, Dimitrios N., E-mail: dbic@chem.auth.gr [Laboratory of Polymer Chemistry and Technology, Department of Chemistry, Aristotle University of Thessaloniki, GR-541 24, Thessaloniki, Macedonia (Greece)

    2011-04-20

    Research highlights: {yields} Thermal decomposition behaviour of PCL-b-PPAd block copolymers was estimated. {yields} The prepared copolymers have higher thermal stability than neat polymers. {yields} In copolymers the evaporation of PPAd short blocks and formed {epsilon}-CL is delayed. {yields} This is because copolymers degrade with a different mechanism than neat polymers. - Abstract: Poly({epsilon}-caprolactone-b-propylene adipate) copolymers were synthesized using a combination of polycondensation and ring opening polymerisation. GPC was used for molecular weight determination. {sup 1}H-NMR and {sup 13}C-NMR spectroscopy was also used for copolymer characterization and composition, which was found similar to the feeding ratio. DSC study was used in order to define T{sub g}, T{sub m} and {Delta}H{sub m} values of neat polymers and copolymers. Mass loss upon heating kinetics of neat polymers and their copolymers were studied by using thermogravimetric analysis (TGA). It was found that copolymers have almost the same thermal stability as PCL, which is the most stable part. The influence of PPAd in copolymers can mainly be seen at the beginning of mass loss where a small overlapped peak can be observed. The kinetic parameters of mass loss upon heating of all polyesters were calculated while the activation energies were estimated using the Ozawa, Flynn and Wall (OFW) and Friedman methods. Mass loss upon heating was found to be described by two mechanisms that follow each other. The first mechanism is attributed to a small mass loss, while the second mechanism is attributed to the main mass loss as in autocatalysis n{sup th}-order (reaction model Cn) or n{sup th} order (reaction model Fn).

  14. A miniaturised 3D printed polypropylene reactor for online reaction analysis by mass spectrometry

    OpenAIRE

    Scotti, Gianmario; Nilsson, Sofia Märta Elisabeth; Haapala, Markus Juhani; Pöhö, Päivi Anneli; Boije af Gennäs, Per Gustav; Yli-Kauhaluoma, Jari Tapani; Kotiaho, Ahti Antti Tapio

    2017-01-01

    A miniaturised polypropylene reactor was fabricated by 3D printing using fused deposition modeling. A stainless steel nanoelectrospray ionisation capillary and a magnetic stir bar were integrated into the reactor during the printing process. The integrated nanoelectrospray ionisation capillary allows direct sampling of a reaction solution without external pumping. It also allows ionisation of the analytes. Therefore, very rapid online mass spectrometric chemical reaction monitoring is possibl...

  15. Ionised gas structure of 100 kpc in an over-dense region of the galaxy group COSMOS-Gr30 at z 0.7

    Science.gov (United States)

    Epinat, B.; Contini, T.; Finley, H.; Boogaard, L. A.; Guérou, A.; Brinchmann, J.; Carton, D.; Michel-Dansac, L.; Bacon, R.; Cantalupo, S.; Carollo, M.; Hamer, S.; Kollatschny, W.; Krajnović, D.; Marino, R. A.; Richard, J.; Soucail, G.; Weilbacher, P. M.; Wisotzki, L.

    2018-01-01

    We report the discovery of a 104 kpc2 gaseous structure detected in [O II]λλ3727, 3729 in an over-dense region of the COSMOS-Gr30 galaxy group at z 0.725 with deep MUSE Guaranteed Time Observations. We estimate the total amount of diffuse ionised gas to be of the order of ( 5 ± 3) × 1010 M⊙ and explore its physical properties to understand its origin and the source(s) of the ionisation. The MUSE data allow the identification of a dozen group members that are embedded in this structure through emission and absorption lines. We extracted spectra from small apertures defined for both the diffuse ionised gas and the galaxies. We investigated the kinematics and ionisation properties of the various galaxies and extended gas regions through line diagnostics (R23, O32, and [O III]/Hβ) that are available within the MUSE wavelength range. We compared these diagnostics to photo-ionisation models and shock models. The structure is divided into two kinematically distinct sub-structures. The most extended sub-structure of ionised gas is likely rotating around a massive galaxy and displays filamentary patterns that link some galaxies. The second sub-structure links another massive galaxy that hosts an active galactic nucleus (AGN) to a low-mass galaxy, but it also extends orthogonally to the AGN host disc over 35 kpc. This extent is likely ionised by the AGN itself. The location of small diffuse regions in the R23 vs. O32 diagram is compatible with photo-ionisation. However, the location of three of these regions in this diagram (low O32, high R23) can also be explained by shocks, which is supported by their high velocity dispersions. One edge-on galaxy shares the same properties and may be a source of shocks. Regardless of the hypothesis, the extended gas seems to be non-primordial. We favour a scenario where the gas has been extracted from galaxies by tidal forces and AGN triggered by interactions between at least the two sub-structures. Based on observations made with

  16. THE INFLUENCE OF SALTS UPON THE IONISATION OF EGG ALBUMIN

    Science.gov (United States)

    Sørensen, S. P. L.; Linderstrøm-Lang, K.; Lund, Ellen

    1927-01-01

    Introduction. A description is given of the principle followed in the experimental determination of the ionisation of egg albumin, its capacity to combine with acids and bases. Egg albumin is regarded as an ampholyte, and in accordance with J. N. Brønsted's definition of acids and bases, ampholytes are considered as substances capable of both taking up and giving off hydrogen ions. The theoretical treatment of the capacity of ampholytes to combine with acids (and bases) has been carried out on this basis. Section A. Several experimental series are noted, comprising the determination of the activity coefficient of the hydrogen ion (fH) in ammonium chloride solutions of different concentration. Section B. The general method of experimental determination of the ionisation (capacity to combine with adds and bases) of egg albumin in ammonium chloride and potassium chloride solutions is briefly described, and the results of the experiments are compared. Section C. 1). In a brief theoretical survey we have suggested that distinction should be made between isoelectric and isoionic reaction of an ampholyte, the former defined as the hydrogen ion activity (value of paH) at which the mean valency of the ampholyte is 0, the latter as the hydrogen ion activity at which the quantity of acid or base combined with the ampholyte is 0; or, as we prefer to express it, the hydrogen ion activity at which the specific hydrogen ionisation of the ampholyte is 0. If the ampholyte does not combine with other ions than the hydrogen ion, then isoelectric and isoionic reaction coincide. Isoionic reaction is determined by acid-combining experiments. The principle of this determination is briefly described. A theoretical investigation of the alteration with salt concentration of both isoelectric (isoionic) reaction and the shape and direction of the ionisation curves is made, with regard to ampholytes capable only of combining with hydrogen ions, on the basis of the Debye-Hückel formulæ and

  17. THE INFLUENCE OF SALTS UPON THE IONISATION OF EGG ALBUMIN.

    Science.gov (United States)

    Sørensen, S P; Linderstrøm-Lang, K; Lund, E

    1927-03-07

    Introduction. A description is given of the principle followed in the experimental determination of the ionisation of egg albumin, its capacity to combine with acids and bases. Egg albumin is regarded as an ampholyte, and in accordance with J. N. Brønsted's definition of acids and bases, ampholytes are considered as substances capable of both taking up and giving off hydrogen ions. The theoretical treatment of the capacity of ampholytes to combine with acids (and bases) has been carried out on this basis. Section A. Several experimental series are noted, comprising the determination of the activity coefficient of the hydrogen ion (fH) in ammonium chloride solutions of different concentration. Section B. The general method of experimental determination of the ionisation (capacity to combine with adds and bases) of egg albumin in ammonium chloride and potassium chloride solutions is briefly described, and the results of the experiments are compared. Section C. 1). In a brief theoretical survey we have suggested that distinction should be made between isoelectric and isoionic reaction of an ampholyte, the former defined as the hydrogen ion activity (value of paH) at which the mean valency of the ampholyte is 0, the latter as the hydrogen ion activity at which the quantity of acid or base combined with the ampholyte is 0; or, as we prefer to express it, the hydrogen ion activity at which the specific hydrogen ionisation of the ampholyte is 0. If the ampholyte does not combine with other ions than the hydrogen ion, then isoelectric and isoionic reaction coincide. Isoionic reaction is determined by acid-combining experiments. The principle of this determination is briefly described. A theoretical investigation of the alteration with salt concentration of both isoelectric (isoionic) reaction and the shape and direction of the ionisation curves is made, with regard to ampholytes capable only of combining with hydrogen ions, on the basis of the Debye-Hückel formulae and

  18. Fully kinetic simulations of magnetic reconnection in partially ionised gases

    Science.gov (United States)

    Innocenti, M. E.; Jiang, W.; Lapenta, G.; Markidis, S.

    2016-12-01

    Magnetic reconnection has been explored for decades as a way to convert magnetic energy into kinetic energy and heat and to accelerate particles in environments as different as the solar surface, planetary magnetospheres, the solar wind, accretion disks, laboratory plasmas. When studying reconnection via simulations, it is usually assumed that the plasma is fully ionised, as it is indeed the case in many of the above-mentioned cases. There are, however, exceptions, the most notable being the lower solar atmosphere. Small ionisation fractions are registered also in the warm neutral interstellar medium, in dense interstellar clouds, in protostellar and protoplanetary accreditation disks, in tokamak edge plasmas and in ad-hoc laboratory experiments [1]. We study here how magnetic reconnection is modified by the presence of a neutral background, i.e. when the majority of the gas is not ionised. The ionised plasma is simulated with the fully kinetic Particle-In-Cell (PIC) code iPic3D [2]. Collisions with the neutral background are introduced via a Monte Carlo plug-in. The standard Monte Carlo procedure [3] is employed to account for elastic, excitation and ionization electron-neutral collisions, as well as for elastic scattering and charge exchange ion-neutral collisions. Collisions with the background introduce resistivity in an otherwise collisionless plasma and modifications of the particle distribution functions: particles (and ions at a faster rate) tend to thermalise to the background. To pinpoint the consequences of this, we compare reconnection simulations with and without background. References [1] E E Lawrence et al. Physical review letters, 110(1):015001, 2013. [2] S Markidis et al. Mathematics and Computers in Simulation, 80(7):1509-1519, 2010. [3] K Nanbu. IEEE Transactions on plasma science, 28(3):971-990, 2000.

  19. IEC standards for individual monitoring of ionising radiation.

    Science.gov (United States)

    Voytchev, M; Ambrosi, P; Behrens, R; Chiaro, P

    2011-03-01

    This paper presents IEC/SC 45B 'Radiation protection instrumentation' and its standards for individual monitoring of ionising radiation: IEC 61526 Ed. 3 for active personal dosemeters and IEC 62387-1 for passive integrating dosimetry systems. The transposition of these standards as CENELEC (European) standards is also discussed together with the collaboration between IEC/SC 45B and ISO/TC 85/SC 2.

  20. Impact ionisation measurement and modelling of long wavelength avalanche photodiodes

    CERN Document Server

    Ng, J S

    2003-01-01

    Impact ionisation coefficients are measured in In sub 0 sub . sub 5 sub 3 Ga sub 0 sub . sub 4 sub 7 As and excess noise characteristics are measured in sub-micron ln sub 0 sub . sub 5 sub 2 Al sub 0 sub . sub 4 sub 8 As. Photomultiplication measurements performed on a series of In sub 0 sub . sub 5 sub 3 Ga sub 0 sub . sub 4 sub 7 As p-i-n diodes are reported. Taking careful account of factors which could give rise to erroneous results at low fields, ln sub 0 sub . sub 5 sub 3 Ga sub 0 sub . sub 4 sub 7 As ionisation coefficients are deduced at room temperature as a function of electric field. The results confirm the low field ionisation behaviour of alpha and the conventional field dependence of beta. Excess avalanche noise factors of In sub 0 sub . sub 5 sub 2 Al sub 0 sub . sub 4 sub 8 As p-i-n diodes, with i-region thicknesses ranging from 1.0 mu m to 0.1 mu m, are reported. The results indicate effective beta/alpha values lying between 0.15 and 0.23, comparable with or lower than the values reported in ...

  1. KINETIC SIMULATIONS OF THERMOLUMINESCENCE DOSE RESPONSE: LONG OVERDUE CONFRONTATION WITH THE EFFECTS OF IONISATION DENSITY.

    Science.gov (United States)

    Horowitz, Y S; Eliyahu, I; Oster, L

    2016-12-01

    The reader will time-travel through almost seven decades of kinetic models and mathematical simulations of thermoluminescence (TL) characteristics based on the band-gap theory of the solid state. From post-World-War II, ideas concerning electron trapping mechanisms to the highly idealised one trap-one recombination (OTOR) model first elaborated in 1956 but still in 'high gear' today. The review caresses but purposely avoids in-depth discussion of the endless stream of papers discussing the intricacies of glow peak shapes arising from first-order, second-order, mixed-order and general-order kinetics predominantly based on non-interacting systems, and then on to the more physically realistic scenarios that have attempted to analyse complex systems involving ever greater numbers of interacting trapping centres, luminescent centres and non-luminescent centres. The review emphasises the difficulty the band-gap models have in the simulation of dose response linear/supralinear behaviour and especially the dependence of the supralinearity on ionisation density. The significance of the non-observation of filling-rate supralinearity in the absorption stage is emphasised since it removes from consideration the possibility of TL supralinearity arising from irradiation stage supralinearity. The importance of the simultaneous action of both localised and delocalised transitions has gradually penetrated the mindset of the community of kinetic researchers, but most simulations have concentrated on the shape of glow peaks and the extraction of the glow peak parameters, E (the thermal activation energy) and s (the attempt-to-escape frequency). The simulation of linear/supralinear dose response and its dependence on ionisation density have been largely avoided until recently due to the fundamental schism between the effects of ionisation density and some basic assumptions of the band-gap model. The review finishes with an in-depth presentation and discussion of the most recent

  2. On ionising radiation and breast cancer risk

    Energy Technology Data Exchange (ETDEWEB)

    Mattson, Anders

    1999-05-01

    A cohort of 3,090 women with clinical diagnosis of benign breast disease (BBD) was studied. Of these, 1,216 were treated with radiation therapy during 1925-54 (median age 40 years). The mean dose to the breasts was 5.8 Gy (range 0-50 Gy). Among other organs the lung received the highest scattered dose (0.75 Gy; range 0.004-8.98 Gy) and the rectum the lowest (0.008 Gy; range 0-0.06 Gy). A pooled analysis of eight breast cancer incidence cohorts was done, including: tumour registry data on breast cancer incidence among women in the Life Span Study cohort of atomic bomb survivors; women in Massachusetts who received repeated chest fluoroscopic during lung collapse treatment for tuberculosis; women who received x-ray therapy for acute post-partum mastitis; women who were irradiated in infancy for enlarged thymus glands ; two Swedish cohorts of women who received radiation treatments during infancy for skin hemangioma; and the BBD cohort. Together the cohorts included almost 78,000 women (-35,000 were exposed), around 1.8 million woman-years and 1500 cases. The breast cancer incidence rate as a function of breast dose was analysed using linear-quadratic Poisson regression models. Cell-killing effects and other modifying effects were incorporated through additional log-linear terms. Additive (EAR) and multiplicative (ERR) models were compared in estimating the age-at-exposure patterns and time related excess. The carcinogenic risks associated with radiation in mammographic mass screening is evaluated. Assessment was made in terms of breast cancer mortality and years of life. Effects were related to rates not influenced by a mammographic mass screening program and based on a hypothetical cohort of 100,000 40-year old women with no history of breast cancer being followed to 100 years of age. Two radiation risk assumptions were compared. The dose-response relationship is linear with little support in data for an upward curvature at low to medium doses. The competing effect

  3. Direct analysis of anabolic steroids in urine using Leidenfrost phenomenon assisted thermal desorption-dielectric barrier discharge ionization mass spectrometry.

    Science.gov (United States)

    Saha, Subhrakanti; Mandal, Mridul Kanti; Nonami, Hiroshi; Hiraoka, Kenzo

    2014-08-11

    Rapid detection of trace level anabolic steroids in urine is highly desirable to monitor the consumption of performance enhancing anabolic steroids by athletes. The present article describes a novel strategy for identifying the trace anabolic steroids in urine using Leidenfrost phenomenon assisted thermal desorption (LPTD) coupled to dielectric barrier discharge (DBD) ionization mass spectrometry. Using this method the steroid molecules are enriched within a liquid droplet during the thermal desorption process and desorbed all-together at the last moment of droplet evaporation in a short time domain. The desorbed molecules were ionized using a dielectric barrier discharge ion-source in front of the mass spectrometer inlet at open atmosphere. This process facilitates the sensitivity enhancement with several orders of magnitude compared to the thermal desorption at a lower temperature. The limits of detection (LODs) of various steroid molecules were found to be in the range of 0.05-0.1 ng mL(-1) for standard solutions and around two orders of magnitude higher for synthetic urine samples. The detection limits of urinary anabolic steroids could be lowered by using a simple and rapid dichloromethane extraction technique. The analytical figures of merit of this technique were evaluated at open atmosphere using suitable internal standards. The technique is simple and rapid for high sensitivity and high throughput screening of anabolic steroids in urine. Copyright © 2014 Elsevier B.V. All rights reserved.

  4. Plasmonic Thermal Decomposition/Digestion of Proteins: A Rapid On-Surface Protein Digestion Technique for Mass Spectrometry Imaging.

    Science.gov (United States)

    Zhou, Rong; Basile, Franco

    2017-09-05

    A method based on plasmon surface resonance absorption and heating was developed to perform a rapid on-surface protein thermal decomposition and digestion suitable for imaging mass spectrometry (MS) and/or profiling. This photothermal process or plasmonic thermal decomposition/digestion (plasmonic-TDD) method incorporates a continuous wave (CW) laser excitation and gold nanoparticles (Au-NPs) to induce known thermal decomposition reactions that cleave peptides and proteins specifically at the C-terminus of aspartic acid and at the N-terminus of cysteine. These thermal decomposition reactions are induced by heating a solid protein sample to temperatures between 200 and 270 °C for a short period of time (10-50 s per 200 μm segment) and are reagentless and solventless, and thus are devoid of sample product delocalization. In the plasmonic-TDD setup the sample is coated with Au-NPs and irradiated with 532 nm laser radiation to induce thermoplasmonic heating and bring about site-specific thermal decomposition on solid peptide/protein samples. In this manner the Au-NPs act as nanoheaters that result in a highly localized thermal decomposition and digestion of the protein sample that is independent of the absorption properties of the protein, making the method universally applicable to all types of proteinaceous samples (e.g., tissues or protein arrays). Several experimental variables were optimized to maximize product yield, and they include heating time, laser intensity, size of Au-NPs, and surface coverage of Au-NPs. Using optimized parameters, proof-of-principle experiments confirmed the ability of the plasmonic-TDD method to induce both C-cleavage and D-cleavage on several peptide standards and the protein lysozyme by detecting their thermal decomposition products with matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS). The high spatial specificity of the plasmonic-TDD method was demonstrated by using a mask to digest designated sections of

  5. Effects of thermal mass, window size, and night-time ventilation on peak indoor air temperature in the warm-humid climate of Ghana

    National Research Council Canada - National Science Library

    Amos-Abanyie, S; Akuffo, F O; Kutin-Sanwu, V

    2013-01-01

    Most office buildings in the warm-humid sub-Saharan countries experience high cooling load because of the predominant use of sandcrete blocks which are of low thermal mass in construction and extensive use of glazing...

  6. Effects of Thermal Mass, Window Size, and Night-Time Ventilation on Peak Indoor Air Temperature in the Warm-Humid Climate of Ghana

    National Research Council Canada - National Science Library

    Amos-Abanyie, S; Akuffo, F. O; Kutin-Sanwu, V

    2013-01-01

    Most office buildings in the warm-humid sub-Saharan countries experience high cooling load because of the predominant use of sandcrete blocks which are of low thermal mass in construction and extensive use of glazing...

  7. Significant Enhancement of Thermal Conductivity in Nanofibrillated Cellulose Films with Low Mass Fraction of Nanodiamond.

    Science.gov (United States)

    Song, Na; Cui, Siqi; Hou, Xingshuang; Ding, Peng; Shi, Liyi

    2017-11-10

    High thermal conductive nanofibrillated cellulose (NFC) hybrid films based on nanodiamond (ND) were fabricated by a facile vacuum filtration technique. In this issue, the thermal conductivity (TC) on the in-plane direction of the NFC/ND hybrid film had a significant enhancement of 775.2% at a comparatively low ND content (0.5 wt %). The NFC not only helps ND to disperse in the aqueous medium stably but also plays a positive role in the formation of the hierarchical structure. ND could form a thermal conductive pathway in the hierarchical structures under the intermolecular hydrogen bonds. Moreover, the hybrid films composed of zero-dimensional ND and one-dimensional NFC exhibit remarkable mechanical properties and optical transparency. The NFC/ND hybrid films possessing superior TC, mechanical properties, and optical transparency can open applications for portable electronic equipment as a lateral heat spreader.

  8. Thermal analysis of the cold mass of the 2T solenoid for the PANDA detector at FAIR

    CERN Document Server

    Rolando, G; Dudarev, A; Pais Da Silva, H; Vodopyanov, A; Schmitt, L

    2015-01-01

    The superconducting solenoid of the PANDA experiment at the Facility for Antiproton and Ion Research (FAIR) in Darmstadt (Germany) is designed to provide a magnetic field of 2 T over a length of about 4 m in a bore of 1.9 m. To allow a warm target feed pipe oriented transversely to the solenoid axis and penetrating through the cryostat and solenoid cold mass, the magnet is split into 3 inter-connected coils fitted in a common support cylinder. During normal operation, cooling of the cold mass to the working temperature of 4.5 K will be achieved through the circulation by natural convection of two-phase helium in cooling pipes attached to the Al-alloy support cylinder. Pure aluminium strips acting as heat drains and glued to the inner surface of the three coils and thermally bonded to the cooling pipes allow minimizing the temperature gradient across the 6-layers coils. In this paper the thermal design of the cold mass during normal operation and current ramps up and down is validated using an analytical appro...

  9. Thermal winds in stellar mass black hole and neutron star binary systems

    Science.gov (United States)

    Done, Chris; Tomaru, Ryota; Takahashi, Tadayuki

    2018-01-01

    Black hole binaries show equatorial disc winds at high luminosities, which apparently disappear during the spectral transition to the low/hard state. This is also where the radio jet appears, motivating speculation that both wind and jet are driven by different configurations of the same magnetic field. However, these systems must also have thermal winds, as the outer disc is clearly irradiated. We develop a predictive model of the absorption features from thermal winds, based on pioneering work of Begelman, McKee & Shields. We couple this to a realistic model of the irradiating spectrum as a function of luminosity to predict the entire wind evolution during outbursts. We show that the column density of the thermal wind scales roughly with luminosity, and does not shut off at the spectral transition, though its visibility will be affected by the abrupt change in ionizing spectrum. We re-analyse the data from H1743-322, which most constrains the difference in wind across the spectral transition, and show that these are consistent with the thermal wind models. We include simple corrections for radiation pressure, which allows stronger winds to be launched from smaller radii. These winds become optically thick around Eddington, which may even explain the exceptional wind seen in one observation of GRO J1655-40. These data can instead be fit by magnetic wind models, but similar winds are not seen in this or other systems at similar luminosities. Hence, we conclude that the majority (perhaps all) of current data can be explained by thermal or thermal-radiative winds.

  10. Transformation of chlorinated paraffins to olefins during metal work and thermal exposure - Deconvolution of mass spectra and kinetics.

    Science.gov (United States)

    Schinkel, Lena; Lehner, Sandro; Knobloch, Marco; Lienemann, Peter; Bogdal, Christian; McNeill, Kristopher; Heeb, Norbert V

    2018-03-01

    Chlorinated paraffins (CPs) are high production volume chemicals widely used as additives in metal working fluids. Thereby, CPs are exposed to hot metal surfaces which may induce degradation processes. We hypothesized that the elimination of hydrochloric acid would transform CPs into chlorinated olefins (COs). Mass spectrometry is widely used to detect CPs, mostly in the selected ion monitoring mode (SIM) evaluating 2-3 ions at mass resolutions R drilling indeed induced HCl-losses. CO proportions in exposed mixtures of chlorotridecanes increased. Thermal exposure of chlorotridecanes at 160, 180, 200 and 220 °C also induced dehydrohalogenation reactions and CO proportions also increased. Deconvolution of respective mass spectra is needed to study the CP transformation kinetics without bias from CO interferences. Apparent first-order rate constants (k app ) increased up to 0.17, 0.29 and 0.46 h -1 for penta-, hexa- and heptachloro-tridecanes exposed at 220 °C. Respective half-life times (τ 1/2 ) decreased from 4.0 to 2.4 and 1.5 h. Thus, higher chlorinated paraffins degrade faster than lower chlorinated ones. In conclusion, exposure of CPs during metal drilling and thermal treatment induced HCl losses and CO formation. It is expected that CPs and COs are co-released from such processes. Full-scan mass spectra and subsequent deconvolution of interfered signals is a promising approach to tackle the CP/CO problem, in case of insufficient mass resolution. Copyright © 2017 Elsevier Ltd. All rights reserved.

  11. Effect of thermal acclimation on organ mass, tissue respiration, and allometry in Leichhardtian river prawns Macrobrachium tolmerum (Riek, 1951).

    Science.gov (United States)

    Crispin, Taryn S; White, Craig R

    2013-01-01

    Changes to an animal's abiotic environment-and consequent changes in the allometry of metabolic rate in the whole animal and its constituent parts-has considerable potential to reveal important patterns in both intraspecific and interindividual variation of metabolic rates. This study demonstrates that, after 6 wk of thermal acclimation at replicate treatments of 16°, 21°, and 25°C, standard metabolic rate (SMR) scales allometrically in Leichhardtian river prawns Macrobrachium tolmerum ([Formula: see text]) and that the scaling exponent and normalization constant of the relationship between SMR and body mass is not significantly different among acclimation treatments when measured at 21°C. There is, however, significant variation among individuals in whole-animal metabolic rate. We hypothesized that these observations may arise because of changes in the metabolic rate and allometry of metabolic rate or mass of organ tissues within the animal. To investigate this hypothesis, rates of oxygen consumption in a range of tissues (gills, gonads, hepatopancreas, chelae muscle, tail muscle) were measured at 21°C and related to the body mass (M) and whole-animal SMR of individual prawns. We demonstrate that thermal acclimation had no effect on organ and tissue mass, that most organ and tissue (gills, gonads, hepatopancreas) respiration rates do not change with acclimation temperature, and that residual variation in the allometry of M. tolmerum SMR is not explained by differences in organ and tissue mass and respiration rates. These results suggest that body size and ambient temperature may independently affect metabolic rate in this species. Both chelae and tail muscle, however, exhibited a reduction in respiration rate in animals acclimated to 25° relative to those acclimated to 16° and 21°C. This reduction in respiration rates of muscle at higher temperatures is evidence of a tissue-specific acclimation response that was not detectable at the whole-animal level.

  12. Investigating the thermal decomposition of starch and cellulose in model systems and toasted bread using domino tandem mass spectrometry.

    Science.gov (United States)

    Golon, Agnieszka; González, Francisco Javier; Dávalos, Juan Z; Kuhnert, Nikolai

    2013-01-23

    Many dietary products containing polysaccharides, mostly starch and cellulose, are processed by thermal treatment. Similarly to the formation of caramel from mono- and disaccharides, the chemical structure of the carbohydrates is dramatically altered by heat treatment. This contribution investigates the products of thermal decomposition of pure starch and cellulose as model systems followed by an investigation of bread obtained at comparable conditions using a combination of modern mass spectrometry techniques. From both starch and cellulose, dehydrated oligomers of glucose and dehydrated glucose have been predominately observed, with oligomers of more than four glucose moieties dominating. Moreover, disproportionation and oligomers with up to six carbohydrates units are formed through unselective glycosidic bond breakage. MALDI-MS data confirm the presence of the majority of products in toasted bread.

  13. NUMERICAL STUDY OF MICROPOLAR FLUID FLOW HEAT AND MASS TRANSFER OVER VERTICAL PLATE: EFFECTS OF THERMAL RADIATION AND MAGNETIC FIELD

    Directory of Open Access Journals (Sweden)

    REDHA ALOUAOUI

    2015-06-01

    Full Text Available In this paper, we examine the thermal radiation effect on heat and mass transfer in steady laminar boundary layer flow of an incompressible viscous micropolar fluid over a vertical flat plate, with the presence of a magnetic field. Rosseland approximation is applied to describe the radiative heat flux in the energy equation. The resulting similarity equations are solved numerically. Many results are obtained and representative set is displayed graphically to illustrate the influence of the various parameters on different profiles. The conclusion is drawn that the flow field, temperature, concentration and microrotation  as well as the skin friction coefficient and the both  local Nusselt and Sherwood numbers  are significantly influenced by Magnetic parameter, material parameter  and thermal radiation parameter.

  14. Characterisation of covalent copper and manganese organometallic complexes with Schiff bases by ionspray mass spectrometry

    NARCIS (Netherlands)

    Raffaelli, A.; Minutolo, F.; Feringa, B.L.; Salvadori, P.

    1998-01-01

    Copper and manganese complexes containing Schiff bases as ligands, having potential interest in homogeneous catalysis, have been characterised by mass spectrometry using ionspray ionisation. Single stage mass spectrometry allowed us to confirm the molecular weight of complexes in all cases,

  15. Thermoluminescent properties of CVD diamond: applications to ionising radiation dosimetry; Proprietes thermoluminescentes du diamant CVD: applications a la dosimetrie des rayonnements ionisants

    Energy Technology Data Exchange (ETDEWEB)

    Petitfils, A

    2007-09-15

    Remarkable properties of synthetic diamond (human soft tissue equivalence, chemical stability, non-toxicity) make this material suitable for medical application as thermoluminescent dosimeter (TLD). This work highlights the interest of this material as radiotherapy TLD. In the first stage of this work, we looked after thermoluminescent (TL) and dosimetric properties of polycrystalline diamond made by Chemically Vapor Deposited (CVD) synthesis. Dosimetric characteristics are satisfactory as TLD for medical application. Luminescence thermal quenching on diamond has been investigated. This phenomenon leads to a decrease of dosimetric TL peak sensitivity when the heating rate increases. The second part of this work analyses the use of synthetic diamond as TLD in radiotherapy. Dose profiles, depth dose distributions and the cartography of an electron beam obtained with our samples are in very good agreement with results from an ionisation chamber. It is clearly shown that CVD) diamond is of interest to check beams of treatment accelerators. The use of these samples in a control of treatment with Intensity Modulated Radiation Therapy underlines good response of synthetic diamond in high dose gradient areas. These results indicate that CVD diamond is a promising material for radiotherapy dosimetry. (author)

  16. Determination of iodine at ppt level in a nitric acid medium by inductively coupled plasma sector field mass spectrometry: influence of the chemical forms; Etude de la determination de traces d'iode en solution par spectrometrie de masse a secteur magnetique utilisant un plasma a couplage inductif comme source d'ionisation: influence de la forme chimique

    Energy Technology Data Exchange (ETDEWEB)

    Langlois, B

    2001-07-01

    Inductively Coupled Plasma Sector Field Mass Spectrometry (ICP/SFMS) was used to determine several chemical forms of iodine, at ppt level, in a nitric acid media. Ascorbic acid was added as a reducing agent in order to maintain iodine as iodide. In a preliminary approach, the influence of the chemical form was studied by comparing inorganic iodine (NaI) and organic iodine (CH3I). Different signal responses were observed. With a conventional sample introduction system, sensitivities obtained for iodo-methane could differ by a factor of 5. This was not caused by a problem of atomization or by a change in the ionization efficiency of the iodo-compound into the plasma. The low volatilization temperature of iodo-methane (315.5 K) seemed to be the main explanation of this phenomena. Actually, nebulization resulted in the volatilization of a 2% nitric acid solution containing iodo-methane. As a result, the transport efficiency of iodo-methane between the nebulizer and the torch was approaching 100%. A Direct Injection High Efficiency Nebulizer (DIHEN) allowed us to minimize the behavior difference between the two iodine species, but the sensitivity ratio was inverted and still differed by 20 - 40%. Moreover, the association of a guard electrode and the direct injection system was studied in order to apply these equipments to the determination of iodine. This association allowed us to improve the sensitivity by a factor of 10 and to minimize memory effects, when compared with a conventional system. Further studies indicated that signal responses obtained with different iodine-containing species, except for iodo-methane, were found to be similar. (author)

  17. Rapid characterization of chemical compounds in liquid and solid states using thermal desorption electrospray ionization mass spectrometry.

    Science.gov (United States)

    Huang, Min-Zong; Zhou, Chi-Chang; Liu, De-Lin; Jhang, Siou-Sian; Cheng, Sy-Chyi; Shiea, Jentaie

    2013-10-01

    Rapid characterization of thermally stable chemical compounds in solid or liquid states is achieved through thermal desorption electrospray ionization mass spectrometry (TD-ESI/MS). A feature of this technique is that sampling, desorption, ionization, and mass spectrometric detection are four separate events with respect to time and location. A metal probe was used to sample analytes in their solid or liquid states. The probe was then inserted in a preheated oven to thermally desorb the analytes on the probe. The desorbed analytes were carried by a nitrogen gas stream into an ESI plume, where analyte ions were formed via interactions with charged solvent species generated in the ESI plume. The analyte ions were subsequently detected by a mass analyzer attached to the TD-ESI source. Quantification of acetaminophen in aqueous solutions using TD-ESI/MS was also performed in which a linear response for acetaminophen was obtained between 25 and 500 ppb (R(2) = 0.9978). The standard deviation for a reproducibility test for ten liquid samples was 9.6%. Since sample preparation for TD-ESI/MS is unnecessary, a typical analysis can be completed in less than 10 s. Analytes such as the active ingredients in over-the-counter drugs were rapidly characterized regardless of the different physical properties of said drugs, which included liquid eye drops, viscous cold syrup solution, ointment cream, and a drug tablet. This approach was also used to detect trace chemical compounds in illicit drugs and explosives, in which samples were obtained from the surfaces of a cell phone, piece of luggage made from hard plastic, business card, and wooden desk.

  18. The effect of mass ratio of electrolyte and electrodes on the thermal stabilities of electrodes used in lithium ion battery

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Qingsong, E-mail: pinew@ustc.edu.cn [State Key Laboratory of Fire Science, University of Science and Technology of China, Hefei 230026 (China); Ping, Ping [State Key Laboratory of Fire Science, University of Science and Technology of China, Hefei 230026 (China); Sun, Jinhua, E-mail: sunjh@ustc.edu.cn [State Key Laboratory of Fire Science, University of Science and Technology of China, Hefei 230026 (China); Chen, Chunhua [Department of Materials Science and Engineering, University of Science and Technology of China, Hefei 230026 (China)

    2011-04-20

    Research highlights: {yields} Mass ratio effect of electrolyte and electrodes is investigated. {yields} The electrode reacts with electrolyte more than one exothermic peaks. {yields} The heat generation increases with the electrolyte content increasing. {yields} The reaction thermodynamics and kinetics are obtained. - Abstract: The mass ratio between electrode and electrolyte in lithium-ion battery plays a key role for the battery thermal stability. Its effect on the thermal stability of their coexisting system was studied using C80 micro-calorimeter. For the Li{sub 0.5}CoO{sub 2}-LiPF{sub 6}/ethylene carbonate (EC) + diethyl carbonate (DEC) coexisting system, when the mass ratios of Li{sub 0.5}CoO{sub 2}-LiPF{sub 6}/EC + DEC are 2:1, 1:1, 1:2 and 1:3, one, two, three and four main exothermic peaks are detected with total heat generation of -1043.8 J g{sup -1}, -1052.6 J g{sup -1}, -1178.5 J g{sup -1} and -1684.5 J g{sup -1}, respectively. For the Li{sub x}C{sub 6}-LiPF{sub 6}/EC + DEC coexisting system, the thermal behavior trend is similar, and the heat generation increases with the electrolyte content increasing, however, and the onset temperature are very close to each others. The heating rate also influence the heat generation rate for the two coexisting system, too far or too low heating rate could results in varies heat generation.

  19. Comparison of Three Infrared Thermal Detection Systems and Self Report for Mass Fever Screening

    Centers for Disease Control (CDC) Podcasts

    2010-10-20

    In this podcast, CDC's Dr. Nicole Cohen describes research that examined the usefulness of thermal scanners for detecting fever in large groups of people in public settings, such as hospitals and airports.  Created: 10/20/2010 by National Center for Emerging and Zoonotic Infectious Diseases (NCEZID).   Date Released: 10/20/2010.

  20. THE EFFECT OF SALTS ON THE IONISATION OF GELATIN

    Science.gov (United States)

    Thimann, Kenneth V.

    1930-01-01

    The effect of the addition of sodium chloride to gelatin solutions is shown from the Donnan relationship to increase the ionisation of the gelatin, the increase produced in acid solutions reaching a maximum at about 1/1000 molar salt concentration. This effect is attributed to the formation of complex ions. From the similar action of calcium and copper chlorides the effective combining power of gelatin for complex positive ion formation is deduced. The bearing of complex ion formation on the zwitter-ionic structure and solubility phenomena of proteins is pointed out. PMID:19872582

  1. Threshold law for positron-atom impact ionisation

    Science.gov (United States)

    Temkin, A.

    1982-01-01

    The threshold law for ionisation of atoms by positron impact is adduced in analogy with our approach to the electron-atom ionization. It is concluded the Coulomb-dipole region of the potential gives the essential part of the interaction in both cases and leads to the same kind of result: a modulated linear law. An additional process which enters positron ionization is positronium formation in the continuum, but that will not dominate the threshold yield. The result is in sharp contrast to the positron threshold law as recently derived by Klar on the basis of a Wannier-type analysis.

  2. Ionisation constants of inorganic acids and bases in aqueous solution

    CERN Document Server

    Perrin, D D

    2013-01-01

    Ionisation Constants of Inorganic Acids and Bases in Aqueous Solution, Second Edition provides a compilation of tables that summarize relevant data recorded in the literature up to the end of 1980 for the ionization constants of inorganic acids and bases in aqueous solution. This book includes references to acidity functions for strong acids and bases, as well as details about the formation of polynuclear species. This text then explains the details of each column of the tables, wherein column 1 gives the name of the substance and the negative logarithm of the ionization constant and column 2

  3. Measuremental analysis of thermal performance of direct gain houses in Kanto district. Effects of thermal mass and caves; Kanto chiho ni tatsu direct gain jutaku no netsuseino jissoku. Netsuyoryo to hisashi no koka

    Energy Technology Data Exchange (ETDEWEB)

    Inoue, K.; Sunaga, N.; Muro, K. [Tokyo Metropolitan University, Tokyo (Japan)

    1996-10-27

    The thermal performance of direct gain passive solar houses was measured. Mr. M`s two-storied RC residence with double glazing windows and thermal storage floors, walls and ceilings of brick or concrete was provided for measurement. Its double eaves of the south window and both SE and SW overhanging exterior walls play a role in sunshade. Mr. I`s two-storied wooden residence with thermal storage RC floors and brick walls, and no eaves of the south window and no overhanging exterior walls was also provided. The summer and winter measurement results were in complete contrast between the residences. In summer, large thermal mass and eaves of Mr. M`s residence were effective, while in winter, small thermal mass and no eaves of Mr. I`s residence were effective. The following ideas are important in design from the viewpoint of indoor thermal environment: a movable sunshade for taking in solar radiation as much as possible in winter, well-balanced arrangement of thermal storage parts with suitable thermal mass corresponding to movement of the sun, a large screen door for cross ventilation in summer, and a night insulation shutter for reducing heat loss in winter. 2 refs., 10 figs., 1 tab.

  4. Polymeric spatial resolution test patterns for mass spectrometry imaging using nano-thermal analysis with atomic force microscopy.

    Science.gov (United States)

    Tai, Tamin; Kertesz, Vilmos; Lin, Ming-Wei; Srijanto, Bernadeta R; Hensley, Dale K; Xiao, Kai; Van Berkel, Gary J

    2017-07-30

    As the spatial resolution of mass spectrometry imaging technologies has begun to reach into the nanometer regime, finding readily available or easily made resolution reference materials has become particularly challenging for molecular imaging purposes. This paper describes the fabrication, characterization and use of vertical line array polymeric spatial resolution test patterns for nano-thermal analysis/atomic force microscopy/mass spectrometry chemical imaging. Test patterns of varied line width (0.7 or 1.0 μm) and spacing (0.7 or 1.0 μm) were created in an ~1-μm-thick poly(methyl methacrylate) thin film using electron beam lithography. The patterns were characterized by scanning electron microscopy, energy-dispersive X-ray spectroscopy, atomic force microscopy topography and nano-thermal analysis/mass spectrometry imaging. The efficacy of these polymeric test patterns for the advancement of chemical imaging techniques was illustrated by their use to judge the spatial resolution improvement achieved by heating the ionization interface of the current instrument platform. The spatial resolution of the mass spectral chemical images was estimated to be 1.4 μm, based on the ability to statistically distinguish 0.7-μm-wide lines separated by 0.7-μm-wide spacings in those images when the interface cross was heated to 200°C. This work illustrates that e-beam lithography is a viable method to create spatial resolution test patterns in a thin film of high molecular weight polymer to allow unbiased judgment of intra-laboratory advancement and/or inter-laboratory comparison of instrument advances in nano-thermal analysis/atomic force microscopy/mass spectrometry chemical imaging. Published in 2017. This article is a U.S. Government work and is in the public domain in the USA. Published in 2017. This article is a U.S. Government work and is in the public domain in the USA.

  5. Thermal requirements for surviving a mass rescue incident in the Arctic: project update

    Energy Technology Data Exchange (ETDEWEB)

    Boileau, Renee [National Research Council Canada: Institute for Ocean Technology, St. John' s, Newfoundland and Labrador (Canada)], email: renee.boileau@nrc-cnrc.gc.ca; DuCharme, Michel B. [Defence Research and Development Canada, Quebec, Quebec (Canada)], email: michel.ducharme@drdc-rddc.gc.ca.gc.ca; Cheung, Stephen [Brock University Department of Physical Education and Kinesiology, St. Catherines, Ontario (Canada)], email: stephen.cheung@brocku.ca; Mak, Lawrence [National Research Council Canada: Institute for Ocean Technology St. John' s, Newfoundland and Labrador (Canada)], email: lawrence.mak@nrc-cnrc.gc.ca

    2010-07-01

    Recently the number of tourists travelling though the Arctic has risen to over 1.5 million per year, increasing the risk of accidents in these extreme conditions. With such harsh conditions, it could take several days for the rescue to arrive on site; however there are no standards specifying the thermal insulation properties that equipment should have. The aim of this paper is to assess the thermal protection afforded by the equipment available and to assess human endurance. A 3 year study was carried out with experiments being performed in simulated Arctic conditions. This study is intended to assess the likelihood of survival for victims in the Arctic with the use of equipment currently available and to identify the principal risks. Subsequent to this assessment, survival prediction tools are expected to be improved based upon the knowledge gained in this study and recommendations made for better equipment to improve the likelihood of survival in accidents in the Arctic Seas.

  6. Controlling ionisation and fragmentation processes in CO2 via inelastic electron recollisions

    Directory of Open Access Journals (Sweden)

    Frasinski L. J.

    2013-03-01

    Full Text Available The angular dependence of nonsequential double ionisation and dissociation induced by laser driven inelastic electron rescattering was investigated experimentally in aligned CO2. A clear dependence on the recollision angle was found demonstrating quantum control of ionisation and dissociation processes in the strong field regime.

  7. Concurrent topology optimization for minimization of total mass considering load-carrying capabilities and thermal insulation simultaneously

    Science.gov (United States)

    Long, Kai; Wang, Xuan; Gu, Xianguang

    2017-09-01

    The present work introduces a novel concurrent optimization formulation to meet the requirements of lightweight design and various constraints simultaneously. Nodal displacement of macrostructure and effective thermal conductivity of microstructure are regarded as the constraint functions, which means taking into account both the load-carrying capabilities and the thermal insulation properties. The effective properties of porous material derived from numerical homogenization are used for macrostructural analysis. Meanwhile, displacement vectors of macrostructures from original and adjoint load cases are used for sensitivity analysis of the microstructure. Design variables in the form of reciprocal functions of relative densities are introduced and used for linearization of the constraint function. The objective function of total mass is approximately expressed by the second order Taylor series expansion. Then, the proposed concurrent optimization problem is solved using a sequential quadratic programming algorithm, by splitting into a series of sub-problems in the form of the quadratic program. Finally, several numerical examples are presented to validate the effectiveness of the proposed optimization method. The various effects including initial designs, prescribed limits of nodal displacement, and effective thermal conductivity on optimized designs are also investigated. An amount of optimized macrostructures and their corresponding microstructures are achieved.

  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. Copyright © 2014 Elsevier B.V. All rights reserved.

  9. Thin-layer chromatography and mass spectrometry coupled using proximal probe thermal desorption with electrospray or atmospheric pressure chemica lionization

    Energy Technology Data Exchange (ETDEWEB)

    Ovchinnikova, Olga S [ORNL; Van Berkel, Gary J [ORNL

    2010-01-01

    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.

  10. Precise measurement of the thermal and stellar 54Fe(n ,γ )55Fe cross sections via accelerator mass spectrometry

    Science.gov (United States)

    Wallner, A.; Buczak, K.; Belgya, T.; Bichler, M.; Coquard, L.; Dillmann, I.; Golser, R.; Käppeler, F.; Karakas, A.; Kutschera, W.; Lederer, C.; Mengoni, A.; Pignatari, M.; Priller, A.; Reifarth, R.; Steier, P.; Szentmiklosi, L.

    2017-08-01

    Accelerator mass spectrometry (AMS) represents a complementary approach for precise measurements of neutron capture cross sections, e.g., for nuclear astrophysics. This technique, completely independent of previous experimental methods, was applied for the measurement of the 54Fe(n ,γ )55Fe reaction. Following a series of irradiations with neutrons from cold and thermal to keV energies, the produced long-lived 55Fe nuclei (t1 /2=2.744 +-0.009 ) yr) were analyzed at the Vienna Environmental Research Accelerator. A reproducibility of about 1% could be achieved for the detection of 55Fe, yielding cross-section uncertainties of less than 3%. Thus, this method produces new and precise data that can serve as anchor points for time-of-flight experiments. We report significantly improved neutron capture cross sections at thermal energy (σth=2.30 ±0.07 b) as well as for a quasi-Maxwellian spectrum of k T =25 keV (σ =30.3 ±1.2 mb) and for En=481 ±53 keV (σ =6.01 ±0.23 mb). The new experimental cross sections have been used to deduce improved Maxwellian-averaged cross sections in the temperature regime of the common s -process scenarios. The astrophysical impact is discussed by using stellar models for low-mass asymptotic giant branch stars.

  11. Mass Dependency of Isotope Fractionation of Gases Under Thermal Gradient and Its Possible Implications for Planetary Atmosphere Escaping Process

    Science.gov (United States)

    Sun, Tao; Niles, Paul; Bao, Huiming; Socki, Richard

    2014-01-01

    Physical processes that unmix elements/isotopes of gas molecules involve phase changes, diffusion (chemical or thermal), effusion and gravitational settling. Some of those play significant roles for the evolution of chemical and isotopic compositions of gases in planetary bodies which lead to better understanding of surface paleoclimatic conditions, e.g. gas bubbles in Antarctic ice, and planetary evolution, e.g. the solar-wind erosion induced gas escaping from exosphere on terrestrial planets.. A mass dependent relationship is always expected for the kinetic isotope fractionations during these simple physical processes, according to the kinetic theory of gases by Chapman, Enskog and others [3-5]. For O-bearing (O16, -O17, -O18) molecules the alpha O-17/ alpha O-18 is expected at 0.5 to 0.515, and for S-bearing (S32,-S33. -S34, -S36) molecules, the alpha S-33/ alpha S-34 is expected at 0.5 to 0.508, where alpha is the isotope fractionation factor associated with unmixing processes. Thus, one isotope pair is generally proxied to yield all the information for the physical history of the gases. However, we recently] reported the violation of mass law for isotope fractionation among isotope pairs of multiple isotope system during gas diffusion or convection under thermal gradient (Thermal Gradient Induced Non-Mass Dependent effect, TGI-NMD). The mechanism(s) that is responsible to such striking observation remains unanswered. In our past studies, we investigated polyatomic molecules, O2 and SF6, and we suggested that nuclear spin effect could be responsible to the observed NMD effect in a way of changing diffusion coefficients of certain molecules, owing to the fact of negligible delta S-36 anomaly for SF6.. On the other hand, our results also showed that for both diffusion and convection under thermal gradient, this NMD effect is increased by lower gas pressure, bigger temperature gradient and lower average temperature, which indicate that the nuclear spin effect may

  12. Electron impact ionisation cross sections of iron oxides

    Science.gov (United States)

    Huber, Stefan E.; Mauracher, Andreas; Sukuba, Ivan; Urban, Jan; Maihom, Thana; Probst, Michael

    2017-12-01

    We report electron impact ionisation cross sections (EICSs) of iron oxide molecules, FexOx and FexOx+1 with x = 1, 2, 3, from the ionisation threshold to 10 keV, obtained with the Deutsch-Märk (DM) and binary-encounter-Bethe (BEB) methods. The maxima of the EICSs range from 3.10 to 9 . 96 × 10-16 cm2 located at 59-72 eV and 5.06 to 14.32 × 10-16 cm2 located at 85-108 eV for the DM and BEB approaches, respectively. The orbital and kinetic energies required for the BEB method are obtained by employing effective core potentials for the inner core electrons in the quantum chemical calculations. The BEB cross sections are 1.4-1.7 times larger than the DM cross sections which can be related to the decreasing population of the Fe 4s orbitals upon addition of oxygen atoms, together with the different methodological foundations of the two methods. Both the DM and BEB cross sections can be fitted excellently to a simple analytical expression used in modelling and simulation codes employed in the framework of nuclear fusion research. Supplementary material in the form of one pdf file available from the Journal web page at http://https://doi.org/10.1140/epjd/e2017-80308-2.

  13. Mass transfer in a 1370 C (2500 F) lithium thermal convection loop

    Science.gov (United States)

    Scheuermann, C. M.

    1974-01-01

    Experimental results from a test to evaluate interstitial element mass transfer effects on T-111, ASTAR 811C, and ASTAR 1211C after 5000 hours in flowing lithium at 1370 C (2500 F) are presented. No gross corrosion effects were observed. However, hafnium and nitrogen transfer to cooler regions within the loop were noted. Oxygen was in general removed from test specimens, but there was no evidence to indicate that it was a major factor in the mass transfer process. Carbon and hydrogen transfer were not detected.

  14. Mass transfer across combustion gas thermal boundary layers - Power production and materials processing implications

    Science.gov (United States)

    Rosner, D. E.

    1985-01-01

    The effects of Soret diffusion (for vapors) and thermophoresis (for particles) are illustrated using recent optical experiments and boundary layer computations. Mass transfer rate augmentations of up to a factor of 1000 were observed and predicted for submicron-particle capture by cooled solid surfaces, while mass transfer suppressions of more than 10 to the -10th-fold were predicted for 'overheated' surfaces. It is noted that the results obtained are of interest in connection with such technological applications as fly-ash capture in power generation equipment and glass droplet deposition in optical-waveguide manufacture.

  15. Transferring calibration coefficients from ionisation chambers used for diagnostic radiology to transmission chambers.

    Science.gov (United States)

    Yoshizumi, Maíra T; Caldas, Linda V E

    2012-07-01

    In this work, the response of a double volume transmission ionisation chamber, developed at the Instituto de Pesquisas Energéticas e Nucleares, was compared to that of a commercial transmission chamber. Both ionisation chambers were tested in different X-ray beam qualities using secondary standard ionisation chambers as reference dosimeters. These standard ionisation chambers were a parallel-plate and a cylindrical ionisation chambers, used for diagnostic radiology and mammography beam qualities, respectively. The response of both transmission chambers was compared to that of the secondary standard chambers to obtain coefficients of equivalence. These coefficients allow the transmission chambers to be used as reference equipment. Copyright © 2011 Elsevier Ltd. All rights reserved.

  16. Effect of positive ionisation of inspired air on the response of asthmatic children to exercise.

    Science.gov (United States)

    Lipin, I; Gur, I; Amitai, Y; Amirav, I; Godfrey, S

    1984-01-01

    To evaluate the effect of positive ionisation of inspired air on bronchial reactivity, 12 asthmatic children were twice challenged by exercise in random order. During one test positively ionised air (5-10 X 10(5) ions/cm) was breathed. All challenges were matched in terms of basal lung function and exercise tests were matched in terms of ventilation and respiratory heat loss. Exercise induced asthma was significantly aggravated by exposure to positively ionised air, the postexercise fall in FEV1 (delta FEV1) being 24.7% (SEM and 5.3%) and 35.3% (5%) after the control and ionised air tests respectively (p less than 0.04). It is concluded that positive ionisation aggravates the bronchial response to exercise. PMID:6474386

  17. Chemical separation and mass spectrometry of Cr, Fe, Ni, Zn, and Cu in terrestrial and extraterrestrial materials using thermal ionization mass spectrometry.

    Science.gov (United States)

    Yamakawa, Akane; Yamashita, Katsuyuki; Makishima, Akio; Nakamura, Eizo

    2009-12-01

    A sequential chemical separation technique for Cr, Fe, Ni, Zn, and Cu in terrestrial and extraterrestrial silicate rocks was developed for precise and accurate determination of elemental concentration by the isotope dilution method (ID). The technique uses a combination of cation-anion exchange chromatography and Eichrom nickel specific resin. The method was tested using a variety of matrixes including bulk meteorite (Allende), terrestrial peridotite (JP-1), and basalt (JB-1b). Concentrations of each element was determined by thermal ionization mass spectrometry (TIMS) using W filaments and a Si-B-Al type activator for Cr, Fe, Ni, and Zn and a Re filament and silicic acid-H3PO4 activator for Cu. The method can be used to precisely determine the concentrations of these elements in very small silicate samples, including meteorites, geochemical reference samples, and mineral standards for microprobe analysis. Furthermore, the Cr mass spectrometry procedure developed in this study can be extended to determine the isotopic ratios of 53Cr/52Cr and 54Cr/52Cr with precision of approximately 0.05epsilon and approximately 0.10epsilon (1epsilon = 0.01%), respectively, enabling cosmochemical applications such as high precision Mn-Cr chronology and investigation of nucleosynthetic isotopic anomalies in meteorites.

  18. Effect of Additive of Expanded Polystyrene and Perlite on Some Mechanical Properties and Thermal Conductivity for Mass Concrete

    Directory of Open Access Journals (Sweden)

    Hamid H. Hussein

    2016-07-01

    Full Text Available In  this  research,  the  major  problem  of  mass  concrete  (Differences  in  Temperature  was  studied. Expanded polystyrene and perlite were added in different percentages to investigate the effects on some mechanical properties and thermal conductivity of concrete. Two stages of work were performed.In first stage, reference mix was designed at proportion (1cement: 1.41sand: 2.72gravel with (0.4 water cement  ratio.  Four  tests  were  conducted,  these  tests  including  density,  compressive  strength,  flexural strength and thermal conductivity through exponential equation depending on dry density. In the second stage,  polystyrene  beads  and  perlite  were  added  as  volumetric  ratio  with  (10,  15,  20,  25,  and 30 percentages  to  the  original  size  of  reference mix  and  conducted  the  tests  and  study  their  effects. The results showed a significant improvement in thermal insulation and reduced thermal conductivity (40 , 22 % by using (30 % of polystyrene and perlite respectively. The decreasing in some mechanical properties can be seen and this decreasing did  not have serious effects on the design efficiency of the structure which conformed with the specifications.

  19. 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.

  20. A simplified kinetic and mass transfer modelling of the thermal hydrolysis of vegetable oils

    DEFF Research Database (Denmark)

    Forero-Hernandez, Hector Alexander; Jones, Mark Nicholas; Sarup, Bent

    2017-01-01

    This work presents a combined modelling approach to investigate the kinetics and masstransfer effects on the hydrolysis of vegetable oils under subcritical conditions. The primary purpose of this simplified model is to interpret experimental data collected from typical batch tests and to estimate...... parameters for the proposed model. Due to its heterogeneous nature, the hydrolysis reaction is affected not only by the chemical kinetics but also by the rate of mass transfer between the oil and water as well as their specific contact area in this two phase emulsion. Considering these properties, a model...... was developed and evaluated by comparing the results with experimental data from literature. The model included among others the mass transfer coefficient as a function of operation and process variables, e.g. agitation speed, temperature, pressure, density and viscosity. Thereafter, uncertainty analysis...

  1. The Role of Thermal Convection in Heat and Mass Transport in the Subarctic Snow Cover

    Science.gov (United States)

    1991-10-01

    vapor diffusion have been developed (Bader et al. 1939, Yosida et al. 1955, Giddings and LaChapelle 1962, Yen 1963, de Quervain 1972, Palm and...not agree, other authors (Yosida et al. 1955, Yen 1963, de Quervain 1972, Palm and Tveitereid 1979, Fedoseeva and Fedoseev 1988) concluded that the...for the diffusion model to produce the measured mass transport. Yen (1963), de Quervain (1972), Palm and Tveitereid (1979), and Fedoseeva and Fedoseev

  2. Finnigan ion trap mass spectrometer detection limits and thermal energy analyzer interface status report and present capabilities

    Energy Technology Data Exchange (ETDEWEB)

    Alcaraz, A.; Andresen, B.; Martin, W.

    1990-10-18

    A new Finnigan ion trap mass spectrometer was purchased and installed at LLNL. Over a period of several months the instrument was tested under a variety of conditions utilizing a capillary gas chromatography interface which allowed separated organic compounds to be carried directly into the ion source of the mass spectrometer. This direct interface allowed maximum analytical sensitivity. A variety of critical tests were performed in order to optimize the sensitivity of the system under a variety of analysis conditions. These tests altered the critical time cycles of the ionization, ion trapping, and detection. Various carrier gas pressures were also employed in order to ascertain the overall sensitivity of the instrument. In addition we have also interfaced a thermal energy analyzer (TEA) to the gas chromatograph in order to simultaneously detect volatile nitrogen containing compounds while mass spectral data is being acquired. This is the first application at this laboratory of simultaneous ultra-trace detections while utilizing two orthogonal analytical techniques. In particular, explosive-related compound and/or residues are of interest to the general community in water, soil and gas sampler. In this paper are highlighted a few examples of the analytical power of this new GC-TEA-ITMS technology.

  3. Ionisation Chamber for Measurement of Pulsed Photon Radiation Fields.

    Science.gov (United States)

    Ginzburg, D

    2017-04-28

    The use of pulsed photon radiation in medical, industrial and security sectors has vastly increased during the recent years. The length of pulse from different X-ray flash generators that are commonly used as either portable, battery-operated or fixed systems can be as low as a few femtoseconds. However, the majority of radiation protection instruments, especially various active electronic dosemeters, have limitations when operated in pulsed fields. This study presents measurements that were performed using the dose-integration mode of the RI-02 and Ram Ion survey metres, which are based on ventilated ionisation chamber, when exposed to different pulsed X-ray sources. An intercomparison between the results that were obtained with the survey metres and those that were obtained with thermoluminescence dosemeter, reference passive dosemeter, show good agreement (deviation lies within 10%). © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  4. Dissociative ionisation of adamantane: a combined theoretical and experimental study.

    Science.gov (United States)

    Candian, Alessandra; Bouwman, Jordy; Hemberger, Patrick; Bodi, Andras; Tielens, Alexander G G M

    2017-11-20

    Diamond nanoparticles, or nanodiamonds, are intriguing carbon-based materials which, maybe surprisingly, are the most abundant constituent of presolar grains. While the spectroscopic properties of even quite large diamondoids have already been explored, little is known about their unimolecular fragmentation processes. In this paper we characterise the dissociative ionisation of adamantane (C10H16) - the smallest member of the diamondoid family - utilising imaging Photoelectron Photoion Coincidence (iPEPICO) spectroscopy and Density Functional Theory (DFT) calculations. We have found adamantane to dissociatively photoionise via several parallel channels of which H, C3H7 and C4H8 losses are the most important ones. Calculations confirm the existence of a rate-limiting transition state for the multiple C-loss channels, which is located at 10.55 eV with respect to neutral adamantane. In addition, we found dissociation channels leading to small cationic hydrocarbons, which may be relevant in the interstellar medium.

  5. Studies of Non-Targeted Effects of Ionising Radiation

    Energy Technology Data Exchange (ETDEWEB)

    Oleg V Belyakov; Heli Mononen; Marjo Peraelae [STUK - Radiation and Nuclear Safety Authority, Helsinki (Finland)

    2006-07-01

    The discovery of ionising radiation induced non-targeted effects is important for understanding the dose-response mechanisms relevant to low dose irradiation in vivo. One important question is whether the non-targeted effects relates to a protective mechanism or whether, conversely, it amplifies the number of cells damaged by the isolated radiation tracks of low dose exposures leading to an increased risk of carcinogenesis. One theory supported by the experimental data obtained during this project is that the main functions of the non-targeted effects are to decrease the risk of transformation in a multicellular organism exposed to radiation. Differences in the gene expression profiles, temporal and spatial patterns of key proteins expressed in directly irradiated and bystander cells may determine how the cells ultimately respond to low doses of radiation. Such a mechanism of co-operative response would make the tissue system much more robust. (N.C.)

  6. RF System for the MICE Demonstration of Ionisation Cooling

    Energy Technology Data Exchange (ETDEWEB)

    Ronald, K.; et al.

    2017-04-01

    Muon accelerators offer an attractive option for a range of future particle physics experiments. They can enable high energy (TeV+) high energy lepton colliders whilst mitigating the difficulty of synchrotron losses, and can provide intense beams of neutrinos for fundamental physics experiments investigating the physics of flavor. The method of production of muon beams results in high beam emittance which must be reduced for efficient acceleration. Conventional emittance control schemes take too long, given the very short (2.2 microsecond) rest lifetime of the muon. Ionisation cooling offers a much faster approach to reducing particle emittance, and the international MICE collaboration aims to demonstrate this technique for the first time. This paper will present the MICE RF system and its role in the context of the overall experiment.

  7. An isotopic analysis of ionising radiation as a source of sulphuric acid

    Directory of Open Access Journals (Sweden)

    M. B. Enghoff

    2012-06-01

    Full Text Available Sulphuric acid is an important factor in aerosol nucleation and growth. It has been shown that ions enhance the formation of sulphuric acid aerosols, but the exact mechanism has remained undetermined. Furthermore some studies have found a deficiency in the sulphuric acid budget, suggesting a missing source. In this study the production of sulphuric acid from SO2 through a number of different pathways is investigated. The production methods are standard gas phase oxidation by OH radicals produced by ozone photolysis with UV light, liquid phase oxidation by ozone, and gas phase oxidation initiated by gamma rays. The distributions of stable sulphur isotopes in the products and substrate were measured using isotope ratio mass spectrometry. All methods produced sulphate enriched in 34S and we find an enrichment factor (δ34S of 8.7 ± 0.4‰ (1 standard deviation for the UV-initiated OH reaction. Only UV light (Hg emission at 253.65 nm produced a clear non-mass-dependent excess of 33S. The pattern of isotopic enrichment produced by gamma rays is similar, but not equal, to that produced by aqueous oxidation of SO2 by ozone. This, combined with the relative yields of the experiments, suggests a mechanism in which ionising radiation may lead to hydrated ion clusters that serve as nanoreactors for S(IV to S(VI conversion.

  8. Hydrodynamics and mass transfer deaeration of water on thermal power plants when used natural gas as a desorbing agent

    Science.gov (United States)

    Sharapov, V. I.; Kudryavtseva, E. V.

    2017-11-01

    The technology of low-temperature deaeration of water in thermal power plants was developed. It is proposed to use natural gas supplied to the furnace as desorbing agent in the deaerator instead steam or superheated water. Natural gas has low, often - negative temperature after reducing installs. At the same time, it contains virtually no corrosive gases, oxygen and carbon dioxide, thereby successfully may be used as a stripping agent in water deaeration. The calculation of the energy efficiency of the technology for a typical unit of CHP has shown that achieved a significant annual saving of fuel equivalent in the transition from the traditional method of deaeration of water in the low temperature deaeration. Hydrodynamic and mass transfer indicators were determined for the deaerator thermal power plants using as stripping medium natural gas supplied to the boiler burners. Theoretically required amount and the real specific consumption of natural gas were estimated for deaeration of water standard quality. The calculation of the hydrodynamic characteristics was presented for jet-bubbling atmospheric deaerator with undescended perforated plate when operating on natural gas. The calculation shows the possibility of using commercially available atmospheric deaerators for the application of the new low-temperature water deaeration technology.

  9. Ionising sources in the coma of 67P probed by Rosetta

    Science.gov (United States)

    Heritier, Kevin; Galand, Marina; Henri, Pierre; Eriksson, Anders; Odelstad, Elias; Altwegg, Kathrin; Beth, Arnaud; Broiles, Thomas; Burch, Jim; Carr, Christopher; Cupido, Emanuele; Glassmeier, Karl-Heinz; Nilsson, Hans; Richter, Ingo; Rubin, Martin; Vallieres, Xavier; Vigren, Erik

    2017-04-01

    An ionospheric model has been developed in order to quantify the ion number density in the coma of 67P/Churyumov-Gerasimenko. The model is driven by Rosetta Orbiter Spectrometer for Ion and Neutral Analysis (ROSINA)/Cometary Pressure Sensor (COPS) neutral density and assumes isentropic expansion for the neutral density profile. The two ionisation sources considered are photo-ionisation by solar extreme ultraviolet (EUV) radiation and electron-impact ionisation. The EUV radiation is estimated from fluxes measured by the Thermosphere Ionosphere Mesosphere Energetics and Dynamics (TIMED)/ Solar EUV Experiment (SEE), taking into account the phase shift and the heliocentric distance ratio; between Earth and comet 67P. The electron-impact ionisation production rates are derived from Rosetta Plasma Consortium (RPC)-Ion and Electron Sensor (IES) integrated electron fluxes and corrected for the S/C potential from RPC/LAngmuir Probe (LAP) measurements. Our results are compared with in situ measurements of the plasma density from RPC-Mutual Impedance Probe (MIP) and RPC-LAP. There is a good agreement between the modelled and RPC observed electron densities. The ionospheric model enables to distinguish the relative contributions of the different sources to the total cometary plasma. At high heliocentric distances, electron-impact ionisation becomes the dominant ionisation source and is enhanced over the winter hemisphere. As the solar activity has decreased since the beginning of the mission in 2014, the relative importance of photo-ionisation has decreased as well. However, at low heliocentric distances, photo-ionisation seems to be the most dominant ionising source, in particular through the perihelion period in summer 2015.

  10. Thermal ionization mass spectrometry U-series dating of a hominid site near Nanjing, China

    Science.gov (United States)

    Zhao, Jian-Xin; Hu, Kai; Collerson, Kenneth D.; Xu, Han-Kui

    2001-01-01

    Mass spectrometric U-series dating of speleothems from Tangshan Cave, combined with ecological and paleoclimatic evidence, indicates that Nanjing Man, a typical Homo erectus morphologically correlated with Peking Man at Zhoukoudian, should be at least 580 k.y. old, or more likely lived during the glacial oxygen isotope stage 16 (˜620 ka). Such an age estimate, which is ˜270 ka older than previous electron spin resonance and alpha-counting U-series dates, has significant implications for the evolution of Asian H. erectus. Dentine and enamel samples from the coexisting fossil layer yield significantly younger apparent ages, that of the enamel sample being only less than one-fourth of the minimum age of Nanjing Man. This suggests that U uptake history is far more complex than existing models can handle. As a result, great care must be taken in the interpretation of electron spin resonance and U-series dates of fossil teeth.

  11. Development of FIAT-Based Parametric Thermal Protection System Mass Estimating Relationships for NASA's Multi-Mission Earth Entry Concept

    Science.gov (United States)

    Sepka, Steven A.; Zarchi, Kerry; Maddock, Robert W.; Samareh, Jamshid A.

    2013-01-01

    Part of NASAs In-Space Propulsion Technology (ISPT) program is the development of the tradespace to support the design of a family of multi-mission Earth Entry Vehicles (MMEEV) to meet a wide range of mission requirements. An integrated tool called the Multi Mission System Analysis for Planetary Entry Descent and Landing or M-SAPE tool is being developed as part of Entry Vehicle Technology project under In-Space Technology program. The analysis and design of an Earth Entry Vehicle (EEV) is multidisciplinary in nature, requiring the application many disciplines. Part of M-SAPE's application required the development of parametric mass estimating relationships (MERs) to determine the vehicle's required Thermal Protection System (TPS) for safe Earth entry. For this analysis, the heat shield was assumed to be made of a constant thickness TPS. This resulting MERs will then e used to determine the pre-flight mass of the TPS. Two Mers have been developed for the vehicle forebaody. One MER was developed for PICA and the other consisting of Carbon Phenolic atop an Advanced Carbon-Carbon composition. For the the backshell, MERs have been developed for SIRCA, Acusil II, and LI-900. How these MERs were developed, the resulting equations, model limitations, and model accuracy are discussed in this poster.

  12. Studies on thermal decomposition mechanism of CL-20 by pyrolysis gas chromatography-mass spectrometry (Py-GC/MS)

    Energy Technology Data Exchange (ETDEWEB)

    Naik, N.H.; Gore, G.M. [High Energy Materials Research Laboratory, Sutarwadi, Pune 411021 (India); Gandhe, B.R. [Directorate of Armament, DRDO Bhavan, New Delhi 110011 (India); Sikder, A.K. [High Energy Materials Research Laboratory, Sutarwadi, Pune 411021 (India)], E-mail: ak_sikder@yahoo.com

    2008-11-30

    The thermal decomposition study of CL-20 (hexanitrohexaazaisowurtzitane) using pyrolysis GC/MS was carried out mainly by electron impact (EI) mode. Chemical ionization (CI) mode was used for further confirmation of identified species. Mass spectrum of CL-20 decomposition products predominantly revealed fragments with m/z 81 and 96 corresponding to C{sub 4}H{sub 5}N{sub 2}{sup +} and C{sub 4}H{sub 4}N{sub 2}O{sup +} ions, respectively. The total ion chromatogram (TIC) of CL-20 pyrolysis shows peak within first 2 min due to the presence of low molecular weight gases. Peaks corresponding to several other products were also observed including the atmospheric gases. Cyanogen formation (C{sub 2}N{sub 2}, m/z 52) observed to be enriched at the scan number 300-500. The low molecular mass range decomposition products formed by cleavage of C-N ring structure were found in majority. Additional structural information was sought by employing chemical ionization mode. The data generated during this study was instrumented in determining decomposition pathways of CL-20.

  13. Models of low-mass helium white dwarfs including gravitational settling, thermal and chemical diffusion, and rotational mixing

    Science.gov (United States)

    Istrate, A. G.; Marchant, P.; Tauris, T. M.; Langer, N.; Stancliffe, R. J.; Grassitelli, L.

    2016-10-01

    A large number of extremely low-mass helium white dwarfs (ELM WDs) have been discovered in recent years. The majority of them are found in close binary systems suggesting they are formed either through a common-envelope phase or via stable mass transfer in a low-mass X-ray binary (LMXB) or a cataclysmic variable (CV) system. Here, we investigate the formation of these objects through the LMXB channel with emphasis on the proto-WD evolution in environments with different metallicities. We study for the first time the combined effects of rotational mixing and element diffusion (e.g. gravitational settling, thermal and chemical diffusion) on the evolution of proto-WDs and on the cooling properties of the resulting WDs. We present state-of-the-art binary stellar evolution models computed with MESA for metallicities of Z = 0.02, 0.01, 0.001 and 0.0002, producing WDs with masses between 0.16-0.45 M⊙. Our results confirm that element diffusion plays a significant role in the evolution of proto-WDs that experience hydrogen shell flashes. The occurrence of these flashes produces a clear dichotomy in the cooling timescales of ELM WDs, which has important consequences e.g. for the age determination of binary millisecond pulsars. In addition, we confirm that the threshold mass at which this dichotomy occurs depends on metallicity. Rotational mixing is found to counteract the effect of gravitational settling in the surface layers of young, bloated ELM proto-WDs and therefore plays a key role in determining their surface chemical abundances, I.e. the observed presence of metals in their atmospheres. We predict that these proto-WDs have helium-rich envelopes through a significant part of their lifetime. This is of great importance as helium is a crucial ingredient in the driving of the κ-mechanism suggested for the newly observed ELM proto-WD pulsators. However, we find that the number of hydrogen shell flashes and, as a result, the hydrogen envelope mass at the beginning of

  14. Magnetic headspace adsorptive extraction of chlorobenzenes prior to thermal desorption gas chromatography-mass spectrometry.

    Science.gov (United States)

    Vidal, Lorena; Ahmadi, Mazaher; Fernández, Elena; Madrakian, Tayyebeh; Canals, Antonio

    2017-06-08

    This study presents a new, user-friendly, cost-effective and portable headspace solid-phase extraction technique based on graphene oxide decorated with iron oxide magnetic nanoparticles as sorbent, located on one end of a small neodymium magnet. Hence, the new headspace solid-phase extraction technique has been called Magnetic Headspace Adsorptive Extraction (Mag-HSAE). In order to assess Mag-HSAE technique applicability to model analytes, some chlorobenzenes were extracted from water samples prior to gas chromatography-mass spectrometry determination. A multivariate approach was employed to optimize the experimental parameters affecting Mag-HSAE. The method was evaluated under optimized extraction conditions (i.e., sample volume, 20 mL; extraction time, 30 min; sorbent amount, 10 mg; stirring speed, 1500 rpm, and ionic strength, non-significant), obtaining a linear response from 0.5 to 100 ng L-1 for 1,3-DCB, 1,4-DCB, 1,2-DCB, 1,3,5-TCB, 1,2,4-TCB and 1,2,3-TCB; from 0.5 to 75 ng L-1 for 1,2,4,5-TeCB, and PeCB; and from 1 to 75 ng L-1 for 1,2,3,4-TeCB. The repeatability of the proposed method was evaluated at 10 ng L-1 and 50 ng L-1 spiking levels, and coefficients of variation ranged between 1.5 and 9.5% (n = 5). Limits of detection values were found between 93 and 301 pg L-1. Finally, tap, mineral and effluent water were selected as real water samples to assess method applicability. Relative recoveries varied between 86 and 110% showing negligible matrix effects. Copyright © 2017 Elsevier B.V. All rights reserved.

  15. Thermal desorption mass spectrometric and x-ray photoelectron studies of etched surfaces of polytetrafluoroethylene

    Science.gov (United States)

    Rye, R. R.; Kelber, J. A.

    1987-12-01

    The etching of polytetrafluoroethylene (PTFE) with Na solutions is known to lead to a loss of F, a loss which is correlated with enhanced adhesion. Subsequent heating partially restores surface F with a concurrent loss of adhesion strength. We have combined X-ray photoelectron spectroscopy (XPS) and gas phase mass spectroscopy for in situ measurements of the processes that occur as the fluorocarbon is heated. An array of volatile products, which vary with the specific treatment, desorb from etched PTFE. Among these are: N 2 and low molecular weight fluorocarbons, the amounts of which monotonically decrease with increasing exposure to the etching solution (and probably result from the bulk); species such as CO and CO 2, which in part result from surface impurities; and water and acetone which result from the rinse steps following the etching process. XPS measurements show that etching produces a major loss of surface F and a gain of surface O. The latter probably results from the subsequent rinse steps. Heating produces a substantial recovery in surface F with only a small decrease in the surface O, and the gain in surface F is shown to occur at a higher temperature than the desorption of any species from the surface. Thus, desorption of products from the surface is decoupled, in terms of both the distribution of products and their relative temperatures, from the surface changes as monitored by XPS. This decoupling suggests that the increase in surface F results from diffusion of low molecular weight fluorocarbons from the bulk or a transition region, or from a rearrangement of the sponge-like surface region produced in the etching process.

  16. Medical exposure to ionising radiation and the risk of brain tumours

    DEFF Research Database (Denmark)

    Blettner, Maria; Schlehofer, Brigitte; Samkange-Zeeb, Florence

    2007-01-01

    BACKGROUND: The role of exposure to low doses of ionising radiation in the aetiology of brain tumours has yet to be clarified. The objective of this study was to investigate the association between medically or occupationally related exposure to ionising radiation and brain tumours. METHODS: We...... used self-reported medical and occupational data collected during the German part of a multinational case-control study on mobile phone use and the risk of brain tumours (Interphone study) for the analyses. RESULTS: For any exposure to medical ionising radiation we found odds ratios (ORs) of 0.63 (95...... regions. CONCLUSION: We did not find any significant increased risk of brain tumours for exposure to medical ionising radiation....

  17. Rapid detection of nicotine from breath using desorption ionisation on porous silicon.

    Science.gov (United States)

    Guinan, T M; Abdelmaksoud, H; Voelcker, N H

    2017-05-04

    Desorption ionisation on porous silicon (DIOS) was used for the detection of nicotine from exhaled breath. This result represents proof-of-principle of the ability of DIOS to detect small molecular analytes in breath including biomarkers and illicit drugs.

  18. The Influence of Opacity on Hydrogen Line Emission and Ionisation Balance in High Density Divertor Plasmas

    OpenAIRE

    Behringer, K.

    1997-01-01

    The influence of opacity on hydrogen line emission and ionisation balance in high density divertor plasmas. - Garching bei München : Max-Planck-Inst. für Plasmaphysik, 1997. - 21 S. - (IPP-Report ; 10/5)

  19. Magnetic headspace adsorptive extraction of chlorobenzenes prior to thermal desorption gas chromatography-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Vidal, Lorena, E-mail: lorena.vidal@ua.es [Department of Analytical Chemistry, Nutrition and Food Sciences and University Institute of Materials, University of Alicante, P.O. Box 99, E-03080, Alicante (Spain); Ahmadi, Mazaher [Faculty of Chemistry, Bu-Ali Sina University, Hamedan (Iran, Islamic Republic of); Fernández, Elena [Department of Analytical Chemistry, Nutrition and Food Sciences and University Institute of Materials, University of Alicante, P.O. Box 99, E-03080, Alicante (Spain); Madrakian, Tayyebeh [Faculty of Chemistry, Bu-Ali Sina University, Hamedan (Iran, Islamic Republic of); Canals, Antonio, E-mail: a.canals@ua.es [Department of Analytical Chemistry, Nutrition and Food Sciences and University Institute of Materials, University of Alicante, P.O. Box 99, E-03080, Alicante (Spain)

    2017-06-08

    This study presents a new, user-friendly, cost-effective and portable headspace solid-phase extraction technique based on graphene oxide decorated with iron oxide magnetic nanoparticles as sorbent, located on one end of a small neodymium magnet. Hence, the new headspace solid-phase extraction technique has been called Magnetic Headspace Adsorptive Extraction (Mag-HSAE). In order to assess Mag-HSAE technique applicability to model analytes, some chlorobenzenes were extracted from water samples prior to gas chromatography-mass spectrometry determination. A multivariate approach was employed to optimize the experimental parameters affecting Mag-HSAE. The method was evaluated under optimized extraction conditions (i.e., sample volume, 20 mL; extraction time, 30 min; sorbent amount, 10 mg; stirring speed, 1500 rpm, and ionic strength, non-significant), obtaining a linear response from 0.5 to 100 ng L{sup −1} for 1,3-DCB, 1,4-DCB, 1,2-DCB, 1,3,5-TCB, 1,2,4-TCB and 1,2,3-TCB; from 0.5 to 75 ng L{sup −1} for 1,2,4,5-TeCB, and PeCB; and from 1 to 75 ng L{sup −1} for 1,2,3,4-TeCB. The repeatability of the proposed method was evaluated at 10 ng L{sup −1} and 50 ng L{sup −1} spiking levels, and coefficients of variation ranged between 1.5 and 9.5% (n = 5). Limits of detection values were found between 93 and 301 pg L{sup −1}. Finally, tap, mineral and effluent water were selected as real water samples to assess method applicability. Relative recoveries varied between 86 and 110% showing negligible matrix effects. - Highlights: • A new extraction technique named Magnetic Headspace Adsorptive Extraction is presented. • Graphene oxide/iron oxide composite deposited on a neodymiun magnet as sorbent. • Sorbent of low cost, rapid and simple synthesis, easy manipulation and portability options. • Fast and efficient extraction and sensitive determination of chlorobenzenes in water samples.

  20. Laser sputter neutral mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    King, B.V.; Clarke, M.; Hu, H.; Betz [Newcastle Univ., NSW (Australia). Dept. of Physics

    1993-12-31

    Laser sputter neutral mass spectrometry (LSNMS) is an emerging technique for highly sensitive surface analysis. In this technique a target is bombarded with a pulsed beam of keV ions. The sputtered particles are intercepted by a high intensity pulsed laser beam above the surface and ionised with almost 100% efficiency. The photions may then be mass analysed using a quadrupole or, more commonly, using time of flight (TOF) techniques. In this method photoions are extracted from the ionisation region, accelerated to a known energy E{sub o} and strike a channelplate detector a distance `d` away. The flight time `t` of the photoions is then related to their mass by `d` {radical}m / {radical} 2E{sub o} so measurement of `t` allows mass spectra to be obtained. It is found that LSNMS is an emerging technique of great sensitivity and flexibility, useful for both applied analysis and to investigate basic sputtering processes. 4 refs., 3 figs.

  1. Trace determination of airborne polyfluorinated iodine alkanes using multisorbent thermal desorption/gas chromatography/high resolution mass spectrometry.

    Science.gov (United States)

    Ruan, Ting; Wang, Yawei; Zhang, Qinghua; Ding, Lei; Wang, Pu; Qu, Guangbo; Wang, Chang; Wang, Thanh; Jiang, Guibin

    2010-06-25

    A novel gas chromatography/high resolution mass spectrometry method coupled with multisorbent thermal desorption cartridges has been developed for the determination of volatile neutral polyfluorinated iodine alkanes (PFIs) in airborne samples. It allows, for the first time, simultaneous analysis of four mono-iodized perfluorinated alkanes, three diiodized perfluorinated alkanes and four mono-iodized polyfluorinated telomers in ambient air samples. 3.75 L air sample was passed through a sorbent tube packed with 150 mg of Tenax TA and 200mg of Carbograph 1 TD for analyte adsorption. Important factors during the analysis procedures, such as safe sampling volume, air sampling rate, analyte desorption and transfer strategies, were optimized and good thermal desorption efficiencies were obtained. The method detection limit (MDL) concentration ranged from 0.04 pg/L for 1H,1H,2H,2H-perfluorododecyl iodide to 1.2 pg/L for perfluorohexyl iodide, and instrument response of a seven-point calibration was linear in the range of 10-1000 pg. Travel spike recoveries ranged from 83% to 116%. Small variabilities of less than 36% were obtained near the MDLs and the differences between triplicates were even smaller (2.1-7.3%) at 200 pg spiked level. The method was successfully applied to analyze ambient air samples collected near a point source, and five PFIs were identified (10.8-85.0 pg/L), with none of the analytes detectable at the background site. Copyright 2010. Published by Elsevier B.V.

  2. The Evolutionary Properties and Peculiar Thermal Pulses of Metal-deficient Low-Mass Stars

    Science.gov (United States)

    Cassisi, Santi; Castellani, Vittorio; Tornambe, Amedeo

    1996-03-01

    We investigate the evolutionary behavior of low-mass star models with very low original metal content (log Z = -10, -6, -5) and Y = 0.23. The computations have been extended from the main sequence up to the double shell burning phase. Theoretical isochrones on the H-R diagram are presented for a range of ages spanning 7-15 x 10 yr. Attention has been paid to understand whether, and to what extent, stellar populations in the quoted metallicity range can produce currently observable RR Lyrae variables, the result being that, apart from an intrinsic scarcity of existing stars with such a composition, evolutionary properties are such that a vanishingly small number of RR Lyrae variables is expected to exist. However, if existing, metal-deficient RR Lyrae stars would present pulsational properties not easily distinguishable from those of standard Population II variables. Double shell burning structures are presented with discussion of the dependence of selected evolutionary features on the original metal content and, in particular, the occurrence of unusually strong He shell flashes following the first reignition of He shell burning. The H shell burning along the He intershell accretion phase and the following He shell burning reignition of the M = 0.8 M0, log Z = -10 model are discussed in detail. It is found that, even at the first episode of He shell reignition, the burning grows in so strong a flash that a convective shell develops at once, becoming large enough to interact with the H shell, so that a large amount of fresh protons is suddenly injected into the high-temperature He-burning region. After the third episode of hydrogen ingestion, it has not been possible to follow in detail the development of the instability since a time-dependent treatment of the convection would be required. It is however estimated that during the flash a maximum luminosity of LHe = 2.5' x 108 Lo would have been attained by He burning alone, in contrast with a maximum of LHe = 7.5 x 10

  3. Growth alteration and leaf biochemical responses in Phaseolus vulgaris exposed to different doses of ionising radiation.

    Science.gov (United States)

    Arena, C; De Micco, V; De Maio, A

    2014-01-01

    Ionising radiation may have different effects on plant metabolism, growth and reproduction, depending on radiation dose, plant species, developmental stage and physiological traits. In this study, exposure of dwarf bean plants to different doses of X-rays (0.3, 10, 50, 100 Gy) was investigated with a multidisciplinary approach consisting of morphological, ecophysiological and biochemical analysis. Both mature and young leaves still growing during the X-rays exposure were compared with non-irradiated control leaves. In particular, leaf expansion, leaf anatomy and functional traits, as well as photosynthetic pigment content and Rubisco expression were analysed. Moreover, the activity of poly(ADP-ribose) polymerase (PARP) was also measured as an indicator of radiation-induced DNA damage. Our data showed that leaf growth is affected by high levels of radiation and demonstrate that mature leaves are more radio-resistant than young leaves, which experience severe dose-dependent changes in leaf functional traits. In particular, young leaves exhibited a reduction of area and an increase in specific mass and dry matter content, as well as a decline in Rubisco activity. Moreover, they showed elevated PARP activity and an increase in phenolic compounds in wall cells if compared with mature leaves. Both of these strategies have been interpreted as a way to help developing leaves withstand irradiation. © 2013 German Botanical Society and The Royal Botanical Society of the Netherlands.

  4. Effects of thermal mass, window size, and night-time ventilation on peak indoor air temperature in the warm-humid climate of Ghana.

    Science.gov (United States)

    Amos-Abanyie, S; Akuffo, F O; Kutin-Sanwu, V

    2013-01-01

    Most office buildings in the warm-humid sub-Saharan countries experience high cooling load because of the predominant use of sandcrete blocks which are of low thermal mass in construction and extensive use of glazing. Relatively, low night-time temperatures are not harnessed in cooling buildings because office openings remain closed after work hours. An optimization was performed through a sensitivity analysis-based simulation, using the Energy Plus (E+) simulation software to assess the effects of thermal mass, window size, and night ventilation on peak indoor air temperature (PIAT). An experimental system was designed based on the features of the most promising simulation model, constructed and monitored, and the experimental data used to validate the simulation model. The results show that an optimization of thermal mass and window size coupled with activation of night-time ventilation provides a synergistic effect to obtain reduced peak indoor air temperature. An expression that predicts, indoor maximum temperature has been derived for models of various thermal masses.

  5. Effects of Thermal Mass, Window Size, and Night-Time Ventilation on Peak Indoor Air Temperature in the Warm-Humid Climate of Ghana

    Directory of Open Access Journals (Sweden)

    S. Amos-Abanyie

    2013-01-01

    Full Text Available Most office buildings in the warm-humid sub-Saharan countries experience high cooling load because of the predominant use of sandcrete blocks which are of low thermal mass in construction and extensive use of glazing. Relatively, low night-time temperatures are not harnessed in cooling buildings because office openings remain closed after work hours. An optimization was performed through a sensitivity analysis-based simulation, using the Energy Plus (E+ simulation software to assess the effects of thermal mass, window size, and night ventilation on peak indoor air temperature (PIAT. An experimental system was designed based on the features of the most promising simulation model, constructed and monitored, and the experimental data used to validate the simulation model. The results show that an optimization of thermal mass and window size coupled with activation of night-time ventilation provides a synergistic effect to obtain reduced peak indoor air temperature. An expression that predicts, indoor maximum temperature has been derived for models of various thermal masses.

  6. Thermo-diffusion effect on free convection heat and mass transfer in a thermally linearly stratified non-darcy porous media

    KAUST Repository

    Murthy, P.V.S.N.

    2011-12-26

    Thermo-diffusion effect on free convection heat and mass transfer from a vertical surface embedded in a liquid saturated thermally stratified non - Darcy porous medium has been analyzed using a local non-similar procedure. The wall temperature and concentration are constant and the medium is linearly stratified in the vertical direction with respect to the thermal conditions. The fluid flow, temperature and concentration fields are affected by the complex interactions among the diffusion ratio Le, buoyancy ratio N, thermo-diffusion parameter Sr and stratification parameter ?. Non-linear interactions of all these parameters on the convective transport has been analyzed and variation of heat and mass transfer coefficients with thermo-diffusion parameter in the thermally stratified non-Darcy porous media is presented through computer generated plots.

  7. 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. Copyright © 2016 Elsevier Inc. All rights reserved.

  8. Martian sub-surface ionising radiation: biosignatures and geology

    Directory of Open Access Journals (Sweden)

    J. M. Ward

    2007-07-01

    Full Text Available The surface of Mars, unshielded by thick atmosphere or global magnetic field, is exposed to high levels of cosmic radiation. This ionising radiation field is deleterious to the survival of dormant cells or spores and the persistence of molecular biomarkers in the subsurface, and so its characterisation is of prime astrobiological interest. Here, we present modelling results of the absorbed radiation dose as a function of depth through the Martian subsurface, suitable for calculation of biomarker persistence. A second major implementation of this dose accumulation rate data is in application of the optically stimulated luminescence technique for dating Martian sediments.

    We present calculations of the dose-depth profile in the Martian subsurface for various scenarios: variations of surface composition (dry regolith, ice, layered permafrost, solar minimum and maximum conditions, locations of different elevation (Olympus Mons, Hellas basin, datum altitude, and increasing atmospheric thickness over geological history. We also model the changing composition of the subsurface radiation field with depth compared between Martian locations with different shielding material, determine the relative dose contributions from primaries of different energies, and discuss particle deflection by the crustal magnetic fields.

  9. Topologically frustrated ionisation in a water-ammonia ice mixture.

    Science.gov (United States)

    Liu, C; Mafety, A; Queyroux, J A; Wilson, C W; Zhang, H; Béneut, K; Le Marchand, G; Baptiste, B; Dumas, P; Garbarino, G; Finocchi, F; Loveday, J S; Pietrucci, F; Saitta, A M; Datchi, F; Ninet, S

    2017-10-20

    Water and ammonia are considered major components of the interiors of the giant icy planets and their satellites, which has motivated their exploration under high P-T conditions. Exotic forms of these pure ices have been revealed at extreme (~megabar) pressures, notably symmetric, ionic, and superionic phases. Here we report on an extensive experimental and computational study of the high-pressure properties of the ammonia monohydrate compound forming from an equimolar mixture of water and ammonia. Our experiments demonstrate that relatively mild pressure conditions (7.4 GPa at 300 K) are sufficient to transform ammonia monohydrate from a prototypical hydrogen-bonded crystal into a form where the standard molecular forms of water and ammonia coexist with their ionic counterparts, hydroxide (OH-) and ammonium [Formula: see text] ions. Using ab initio atomistic simulations, we explain this surprising coexistence of neutral/charged species as resulting from a topological frustration between local homonuclear and long-ranged heteronuclear ionisation mechanisms.

  10. Molecular DNA-based detection of ionising radiation in meat.

    Science.gov (United States)

    Şakalar, Ergün

    2017-05-01

    Ionising radiation induces molecular alterations, such as formation of ions, free radicals, and new stable molecules, and cleavage of the chemical bonds of the molecules present in food. Irradiation-treated meat should be labelled to control the process and to ensure free consumer choice. Therefore, sensitive analytical methods are required to detect the irradiation dose. Meat samples were exposed to radiation doses of 0, 0.272, 0.497, 1.063, 3.64, 8.82 and 17.42 kGy in an industrial 60 Co gamma cell. Primers were designed to amplify 998, 498 and 250-base pair (bp) regions of the 18S rRNA gene of nuclear DNA from the irradiated samples. A new DNA-based method was developed to quantify the radiation exposed to the unstored meat and the meat stored at -20 °C for 3 and 6 months. The method was able to detect meat samples stored and unstored with dose limits of 1.063 and 3.64 kGy, respectively. The level of irradiation can be detected using primer pairs that target particularly different-sized sequences for DNA amplification by PCR. This method can be widely used for the analysis of not only meat samples, but also all biological materials containing DNA. © 2016 Society of Chemical Industry. © 2016 Society of Chemical Industry.

  11. Dosimetry of ionising radiation in modern radiation oncology

    Science.gov (United States)

    Kron, Tomas; Lehmann, Joerg; Greer, Peter B.

    2016-07-01

    Dosimetry of ionising radiation is a well-established and mature branch of physical sciences with many applications in medicine and biology. In particular radiotherapy relies on dosimetry for optimisation of cancer treatment and avoidance of severe toxicity for patients. Several novel developments in radiotherapy have introduced new challenges for dosimetry with small and dynamically changing radiation fields being central to many of these applications such as stereotactic ablative body radiotherapy and intensity modulated radiation therapy. There is also an increasing awareness of low doses given to structures not in the target region and the associated risk of secondary cancer induction. Here accurate dosimetry is important not only for treatment optimisation but also for the generation of data that can inform radiation protection approaches in the future. The article introduces some of the challenges and highlights the interdependence of dosimetric calculations and measurements. Dosimetric concepts are explored in the context of six application fields: reference dosimetry, small fields, low dose out of field, in vivo dosimetry, brachytherapy and auditing of radiotherapy practice. Recent developments of dosimeters that can be used for these purposes are discussed using spatial resolution and number of dimensions for measurement as sorting criteria. While dosimetry is ever evolving to address the needs of advancing applications of radiation in medicine two fundamental issues remain: the accuracy of the measurement from a scientific perspective and the importance to link the measurement to a clinically relevant question. This review aims to provide an update on both of these.

  12. Distinguishing chinese star anise from Japanese star anise using thermal desorption-gas chromatography-mass spectrometry.

    Science.gov (United States)

    Howes, Melanie-Jayne R; Kite, Geoffrey C; Simmonds, Monique S J

    2009-07-08

    The volatile compounds from the pericarps of Illicium anisatum L., Illicium brevistylum A.C.Sm., Illicium griffithii Hook.f. & Thomson, Illicium henryi Diels, Illicium lanceolatum A.C.Sm., Illicium majus Hook.f. & Thomson, Illicium micranthum Dunn, and Illicium verum Hook.f. were examined by thermal desorption-gas chromatography-mass spectrometry (TD-GC-MS). The volatiles desorbed from the pericarps of I. verum (Chinese star anise), the species traded for culinary purposes, were generally characterized by a high proportion of (E)-anethole (57.6-77.1%) and the presence of foeniculin; the latter was otherwise only detected in the pericarps of I. lanceolatum. In the pericarps of all other species analyzed, the percentage composition of (E)-anethole was comparatively lower (toxic I. anisatum (Japanese star anise) were characterized by the presence of asaricin, methoxyeugenol, and two other eugenol derivatives, none of which were detected in any of the other species examined. TD-GC-MS enables the direct analysis of the volatile components from the pericarps of Illicium and can assist with differentiating the fruits of I. verum from other species of Illicium, particularly the more toxic I. anisatum.

  13. Quantification of real thermal, catalytic, and hydrodeoxygenated bio-oils via comprehensive two-dimensional gas chromatography with mass spectrometry.

    Science.gov (United States)

    Silva, Raquel V S; Tessarolo, Nathalia S; Pereira, Vinícius B; Ximenes, Vitor L; Mendes, Fábio L; de Almeida, Marlon B B; Azevedo, Débora A

    2017-03-01

    The elucidation of bio-oil composition is important to evaluate the processes of biomass conversion and its upgrading, and to suggest the proper use for each sample. Comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry (GC×GC-TOFMS) is a widely applied analytical approach for bio-oil investigation due to the higher separation and resolution capacity from this technique. This work addresses the issue of analytical performance to assess the comprehensive characterization of real bio-oil samples via GC×GC-TOFMS. The approach was applied to the individual quantification of compounds of real thermal (PWT), catalytic process (CPO), and hydrodeoxygenation process (HDO) bio-oils. Quantification was performed with reliability using the analytical curves of oxygenated and hydrocarbon standards as well as the deuterated internal standards. The limit of quantification was set at 1ngµL-1 for major standards, except for hexanoic acid, which was set at 5ngµL-1. The GC×GC-TOFMS method provided good precision (bio-oil samples. Sugars, furans, and alcohols appear as the major constituents of the PWT, CPO, and HDO samples, respectively. In order to obtain bio-oils with better quality, the catalytic pyrolysis process may be a better option than hydrogenation due to the effective reduction of oxygenated compound concentrations and the lower cost of the process, when hydrogen is not required to promote deoxygenation in the catalytic pyrolysis process. Copyright © 2016 Elsevier B.V. All rights reserved.

  14. Real-time mass spectroscopy analysis of Li-ion battery electrolyte degradation under abusive thermal conditions

    Science.gov (United States)

    Gaulupeau, B.; Delobel, B.; Cahen, S.; Fontana, S.; Hérold, C.

    2017-02-01

    The lithium-ion batteries are widely used in rechargeable electronic devices. The current challenges are to improve the capacity and safety of these systems in view of their development to a larger scale, such as for their application in electric and hybrid vehicles. Lithium-ion batteries use organic solvents because of the wide operating voltage. The corresponding electrolytes are usually based on combinations of linear, cyclic alkyl carbonates and a lithium salt such as LiPF6. It has been reported that in abusive thermal conditions, a catalytic effect of the cathode materials lead to the formation fluoro-organics compounds. In order to understand the degradation phenomenon, the study at 240 °C of the interaction between positive electrode materials (LiCoO2, LiNi1/3Mn1/3Co1/3O2, LiMn2O4 and LiFePO4) and electrolyte in dry and wet conditions has been realized by an original method which consists in analyzing by mass spectrometry in real time the volatile molecules produced. The evolution of specific gases channels coupled to the NMR reveal the formation of rarely discussed species such as 2-fluoroethanol and 1,4-dioxane. Furthermore, it appears that the presence of water or other protic impurities greatly influence their formation.

  15. Measurement of volatile plant compounds in field ambient air by thermal desorption-gas chromatography-mass spectrometry.

    Science.gov (United States)

    Cai, Xiao-Ming; Xu, Xiu-Xiu; Bian, Lei; Luo, Zong-Xiu; Chen, Zong-Mao

    2015-12-01

    Determination of volatile plant compounds in field ambient air is important to understand chemical communication between plants and insects and will aid the development of semiochemicals from plants for pest control. In this study, a thermal desorption-gas chromatography-mass spectrometry (TD-GC-MS) method was developed to measure ultra-trace levels of volatile plant compounds in field ambient air. The desorption parameters of TD, including sorbent tube material, tube desorption temperature, desorption time, and cold trap temperature, were selected and optimized. In GC-MS analysis, the selected ion monitoring mode was used for enhanced sensitivity and selectivity. This method was sufficiently sensitive to detect part-per-trillion levels of volatile plant compounds in field ambient air. Laboratory and field evaluation revealed that the method presented high precision and accuracy. Field studies indicated that the background odor of tea plantations contained some common volatile plant compounds, such as (Z)-3-hexenol, methyl salicylate, and (E)-ocimene, at concentrations ranging from 1 to 3400 ng m(-3). In addition, the background odor in summer was more abundant in quality and quantity than in autumn. Relative to previous methods, the TD-GC-MS method is more sensitive, permitting accurate qualitative and quantitative measurements of volatile plant compounds in field ambient air.

  16. Units for ionisation chamber measurements of {beta} and {gamma} activity; Ensemble de mesure d'activite {beta} et {gamma} par chambre d'ionisation

    Energy Technology Data Exchange (ETDEWEB)

    Engelmann, J.J.; Roquefort, H. [Commissariat a l' Energie Atomique, Saclay (France).Centre d' Etudes Nucleaires

    1960-07-01

    In this paper two methods for ionisation chamber measurements of {beta} and {gamma} activity are discussed. Two ionisation chambers associated with continuous current amplifiers are described: - the first, type C {beta} {gamma} 1, is intended chiefly for measuring the specific activity of {beta}-emitting solutions and the dose rate on the surface of radioactive application systems, - the second, type CCP{gamma} 1, known as a well chamber, serves mainly for measuring the activity of {gamma}-emitting sources or solutions. (author) [French] Dans cet article, nous etudions 2 methodes de mesure d'activite {beta} et {gamma} par chambre d'ionisation. Nous decrirons deux chambres d'ionisation associees a des amplificateurs a courant continu: - l'une, type C {beta} {gamma} 1, permet principalement la mesure de l'activite specifique des solutions emettrices {beta}, et la mesure de dose a la surface d'applicateurs radioactifs; - l'autre, type CCP{gamma} 1, dite chambre a puits, permet principalement la mesure de l'activite de sources ou solutions emettrices {gamma}. (auteur)

  17. THERMAL CONDUCTANCE IN AQUATIC BIRDS IN RELATION TO THE DEGREE OF WATER CONTACT, BODY-MASS, AND BODY-FAT - ENERGETIC IMPLICATIONS OF LIVING IN A STRONG COOLING ENVIRONMENT

    NARCIS (Netherlands)

    DEVRIES, J; VANEERDEN, MR

    1995-01-01

    Thermal conductance of carcasses of 14 aquatic bird species was determined by the warming constant technique. The effect on thermal conductance of body mass, age sex, fat deposits, and the degree of contact with water were studied. Only body mass and the degree of submergence in water had an effect.

  18. Thermophoresis and thermal radiation with heat and mass transfer in a magnetohydrodynamic thin-film second-grade fluid of variable properties past a stretching sheet

    Science.gov (United States)

    Khan, Noor Saeed; Gul, Taza; Islam, Saeed; Khan, Waris

    2017-01-01

    The influences of thermophoresis and thermal radiation of a magnetohydrodynamic two-dimensional thin-film second-grade fluid with heat and mass transfer flow in the presence of viscous dissipation past a stretching sheet are analyzed. The main focus of the study is to discuss the significant roll of the fluid variable properties like thermal conductivity and viscosity under the variation of the thin film. The thermal conductivity varies directly as a linear function of temperature showing the property that expresses the ability of a material to transfer heat, and the viscosity is assumed to vary inversely as a linear function of temperature showing that viscous forces become weak at increasing temperature. Thermophoresis occurs to discuss the mass deposition at the surface of the stretching sheet while thermal radiation occurs, especially, at high temperature. The basic governing equations for the velocity, temperature and concentration of the fluid flow have been transformed to high nonlinear coupled differential equations with physical conditions by invoking suitable similarity transformations. The solution of the problem has been obtained by using HAM (Homotopy Analysis Method). The heat and mass transfer flow behaviors are affected significantly by the thin film. The physical influences of thin film parameter and all other parameters have been studied graphically and illustrated. The residual graphs and residual error table elucidate the authentication of the present work.

  19. Gas chromatographic-mass spectrometric analysis of some potential toxicants amongst volatile compounds emitted during large-scale thermal degradation of poly(acrylonitrile-butadiene-styrene) plastic.

    Science.gov (United States)

    Shapi, M M; Hesso, A

    1991-01-02

    A number of compounds emitted during the thermal degradation of plastics are potentially toxic. This study was aimed at identifying the volatile compounds emitted during large-scale thermal degradation of poly(acrylonitrile-butadiene-styrene). About 5 g of the sample were degraded at between 25 and 470 degrees C in air and nitrogen in a device that can simulate temperature-programmed thermogravimetry. The volatiles were collected in dichloromethane using the solvent trap technique. Some of the 92 compounds identified by gas chromatography-mass spectrometry were found to have no hitherto documented toxicological profiles, even though they are potentially dangerous.

  20. The Ionising Radiations Advisory Committee Open Meeting 10 October 2001

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2001-12-01

    Full text: The Ionising Radiations Advisory Committee (IRAC) held its first open meeting on 10 October 2001 in response to a request from the Health and Safety Commission (HSC) that all its advisory committees should follow the Commission's example and hold such meetings. Some of the other advisory committees have already held open meetings and others are planning to do so shortly. The aim of the meeting was to enable members of the public to meet IRAC members and to find out more about the Committee - how it worked and the type of issues it dealt with. The first two sessions were devoted to short presentations describing IRAC's work and influences, now and in the future, on radiation protection generally. The third session was a discussion forum. The agenda for the meeting and the presentations are posted on the web at: www.hse.gov.uk/foi/iracopen.htm. Each session of presentations was followed by questions of clarification and the third session of the meeting comprised an open forum. Many of the questions raised were not directly relevant to IRAC but, nevertheless, members provided brief responses and referred questions on to others as appropriate. One question had been notified in advance, asking whether members of IRAC agreed that it is now (regrettably) reasonably foreseeable that a loss of containment of radioactive material may occur at a nuclear facility as a result of impact by an aeroplane or by other hostile acts, and that this should be made clear in published guidance on REPPIR. This question was not within IRAC's remit. The Chairman of the Nuclear Safety Advisory Committee offered to take the question to the Committee's next meeting. Issues discussed included: Concerns that exposure to ionising radiation at low levels is more dangerous than is currently reflected in risk estimates. The European Parliament has adopted a resolution calling on the main international bodies, including the International Commission on Radiological

  1. Studies of organic residues from ancient Egyptian mummies using high temperature-gas chromatography-mass spectrometry and sequential thermal desorption-gas chromatography-mass spectrometry and pyrolysis-gas chromatography-mass spectrometry.

    Science.gov (United States)

    Buckley, S A; Stott, A W; Evershed, R P

    1999-04-01

    The techniques of gas chromatography-mass spectrometry (GC-MS) and sequential thermal desorption-gas chromatography-mass spectrometry (TD-GC-MS) and pyrolysis-gas chromatography-mass spectrometry (Py-GC-MS) have been utilised to characterise the constituents of tissue-derived or applied organic material from two Pharaonic Egyptian mummies with a view to identifying embalming practices/substances. The results obtained using TD-GC-MS revealed a series of monocarboxylic acids with the C16:0, C18:1 and C18:0 components dominating in both mummies. The thermal desorption products related to cholesterol, i.e., cholesta-3,5,7-triene and cholesta-3,5-diene (only in Khnum Nakht), were detected in both mummies. Khnum Nakht also contained a number of straight chain alkyl amides (C16-C18) and an alkyl nitrile (C18). Other products included the 2,5-diketopiperazine derivative (DKP) of proline-glycine (pro-gly) which was a major component (7.9%) in Khnum Nakht but only a very minor component in Horemkenesi. Py-GC-MS of samples of both specimens yielded a series of alkene/alkane doublets (Horemkenesi C6-C18, Khnum Nakht C6-C24) which dominated their chromatograms. Series of methyl ketones in the C9-C19 chain length range were also present, with C5-C7 cyclic ketones occurring in Horemkenesi only. These ketones are indicative of covalent bond cleavage, probably of polymerised acyl lipids. Nitrogenous products included nitriles (C9-C18) which were significant in both samples, and amides which were only detected in Khnum Nakht. Also present amongst the pyrolysis products were three steroidal hydrocarbons, cholest-(?)-ene, cholesta-3,5,7-triene and cholesta-3,5-diene. High temperature-GC-MS of trimethylsilylated lipid extracts yielded similar monocarboxylic acids to that obtained using TD-GC-MS, while a series of alpha, omega-dicarboxylic acids and a number of mono- and di-hydroxy carboxylic acids not seen in the thermal desorption or pyrolysis GC-MS analyses were significant

  2. Analysis of the energetic/environmental performances of gas turbine plant: Effect of thermal barrier coatings and mass of cooling air

    Directory of Open Access Journals (Sweden)

    Ion Ion V.

    2009-01-01

    Full Text Available Zirconia stabilized with 8 wt.% Y2O3 is the most common material to be applied in thermal barrier coatings owing to its excellent properties: low thermal conductivity, high toughness and thermal expansion coefficient as ceramic material. Calculation has been made to evaluate the gains of thermal barrier coatings applied on gas turbine blades. The study considers a top ceramic coating Zirconia stabilized with 8 wt.% Y2O3 on a NiCoCrAlY bond coat and Inconel 738LC as substrate. For different thickness and different cooling air flow rates, a thermodynamic analysis has been performed and pollutants emissions (CO, NOx have been estimated to analyze the effect of rising the gas inlet temperature. The effect of thickness and thermal conductivity of top coating and the mass flow rate of cooling air have been analyzed. The model for heat transfer analysis gives the temperature reduction through the wall blade for the considered conditions and the results presented in this contribution are restricted to a two considered limits: (1 maximum allowable temperature for top layer (1200ºC and (2 for blade material (1000ºC. The model can be used to analyze other materials that support higher temperatures helping in the development of new materials for thermal barrier coatings.

  3. Multidimensional gas chromatography using microfluidic switching and low thermal mass gas chromatography for the characterization of targeted volatile organic compounds.

    Science.gov (United States)

    Luong, J; Gras, R; Hawryluk, M; Shellie, R A; Cortes, H J

    2013-05-03

    Volatile organic compounds such as light hydrocarbons, dienes, and aromatic compounds are often encountered in the manufacturing and processing environments of chemical and petrochemical segments. These compounds need to be closely monitored for process optimization, plant maintenance and industrial hygiene purposes. A high throughput analytical approach has been successfully developed and implemented for the accurate measurement of fourteen commonly encountered analytes. The approach incorporates a recently introduced 5-port planar microfluidic device configured for use as a Deans switch for multidimensional gas chromatography. The use of multidimensional gas chromatography allows the elimination of potential chromatographic contaminants with a substantial enhancement of stationary phase selectivity via the use of columns with different separation mechanisms, and the back-flushing of heavier undesired hydrocarbons. A low thermal mass gas chromatographic module was employed in the second dimension of the two-dimensional gas chromatography system and was used to provide independent temperature control, and rapid heating and cooling to meet the high throughput requirements. By successfully combining these concepts, complete analysis of fourteen targeted components can be conducted in less than 120s. Repeatability of retention times for all compounds was found to be less than 0.05% (n=20). Repeatability of area counts at two levels, namely 10ppmv and 1000ppmv over a period of two days was found to be less than 3% (n=20). Apart from methane, which has a detection limit of 0.4ppmv, the rest of the compounds were found to have detection limits of less than 0.2ppmv. Compounds of interest were found to be linear over a range of 500ppbv-3000ppmv with correlation coefficients greater than 0.999. Copyright © 2013 Elsevier B.V. All rights reserved.

  4. Comparison of quantification methods for the analysis of polychlorinated alkanes using electron capture negative ionization mass spectrometry.

    NARCIS (Netherlands)

    Rusina, T.; Korytar, P.; de Boer, J.

    2011-01-01

    Four quantification methods for short-chain chlorinated paraffins (SCCPs) or polychlorinated alkanes (PCAs) using gas chromatography electron capture negative ionisation low resolution mass spectrometry (GC-ECNI-LRMS) were investigated. The method based on visual comparison of congener group

  5. Bayesian analysis of nanodosimetric ionisation distributions due to alpha particles and protons.

    Science.gov (United States)

    De Nardo, L; Ferretti, A; Colautti, P; Grosswendt, B

    2011-02-01

    Track-nanodosimetry has the objective to investigate the stochastic aspect of ionisation events in particle tracks, by evaluating the probability distribution of the number of ionisations produced in a nanometric target volume positioned at distance d from a particle track. Such kind of measurements makes use of electron (or ion) gas detectors with detecting efficiencies non-uniformly distributed inside the target volume. This fact makes the reconstruction of true ionisation distributions, which correspond to an ideal efficiency of 100%, non-trivial. Bayesian unfolding has been applied to ionisation distributions produced by 5.4 MeV alpha particles and 20 MeV protons in cylindrical volumes of propane of 20 nm equivalent size, positioned at different impact parameters with respect to the primary beam. It will be shown that a Bayesian analysis performed by subdividing the target volume in sub-regions of different detection efficiencies is able to provide a good reconstruction of the true nanodosimetric ionisation distributions.

  6. Impact of generalized Fourier's and Fick's laws on MHD 3D second grade nanofluid flow with variable thermal conductivity and convective heat and mass conditions

    Science.gov (United States)

    Ramzan, M.; Bilal, M.; Chung, Jae Dong; Lu, Dian Chen; Farooq, Umer

    2017-09-01

    A mathematical model has been established to study the magnetohydrodynamic second grade nanofluid flow past a bidirectional stretched surface. The flow is induced by Cattaneo-Christov thermal and concentration diffusion fluxes. Novel characteristics of Brownian motion and thermophoresis are accompanied by temperature dependent thermal conductivity and convective heat and mass boundary conditions. Apposite transformations are betrothed to transform a system of nonlinear partial differential equations to nonlinear ordinary differential equations. Analytic solutions of the obtained nonlinear system are obtained via a convergent method. Graphs are plotted to examine how velocity, temperature, and concentration distributions are affected by varied physical involved parameters. Effects of skin friction coefficients along the x- and y-direction versus various parameters are also shown through graphs and are well debated. Our findings show that velocities along both the x and y axes exhibit a decreasing trend for the Hartmann number. Moreover, temperature and concentration distributions are decreasing functions of thermal and concentration relaxation parameters.

  7. Perdeuterated n-alkanes for improved data processing in thermal desorption gas chromatography/mass spectrometry I. Retention indices for identification.

    Science.gov (United States)

    Massold, Emilie

    2007-06-22

    The identification of organic compounds by GC/MS is useful in various areas such as fuel, indoor and outdoor air and flavour and fragrance applications. Multi-compound mixtures often contain isomeric compounds which have similar mass spectra and sometimes cannot be unambiguously identified by library search alone. Retention indices can help with confirmation of identification if they are reproducible. Using perdeuterated n-alkanes as a reference series for calculation of retention indices in GC/MS has a clear benefit because of the distinctive ion trace of m/z 34. Thermal desorption is useful for analysis of volatile organic compounds (VOCs) in air after sampling on appropriate sorbent cartridges. Comparison of indices between three systems, consisting of a thermal desorption unit, a gas chromatograph and a mass spectrometer, showed good agreement for compounds with well-defined peaks, whereas retention times varied.

  8. Non-Darcy free convection flow over a horizontal cylinder in a saturated porous medium with variable viscosity, thermal conductivity and mass diffusivity

    Science.gov (United States)

    Hassanien, I. A.; Rashed, Z. Z.

    2011-04-01

    In this paper, the effects of variable viscosity and thermal conductivity on coupled heat and mass transfer by free convection about a permeable horizontal cylinder embedded in porous media using Ergun mode are studied. The fluid viscosity and thermal conductivity and are assumed to vary as a linear function of temperature while the mass diffusion is assumed to vary as linear function of concentration. The surface of the horizontal cylinder is maintained at a uniform wall temperature and a uniform wall concentration. The transformed governing equations are obtained and solved by using the implicit finite difference method. Numerical results for dimensionless temperature and concentration profiles as well as Nusselt and Sherwood numbers are presented for various values of parameters namely, Ergun number, transpiration parameter, Rayleigh and Lewis numbers and buoyancy ratio parameter.

  9. Group Theoretical Analysis of non-Newtonian Fluid Flow, Heat and Mass Transfer over a Stretching Surface in the Presence of Thermal Radiation

    OpenAIRE

    Muhammad Tufail; Adnan Saeed Butt; Asif Ali

    2016-01-01

    The present article examines the flow, heat and mass transfer of a non-Newtonian fluid known as Casson fluid over a stretching surface in the presence of thermal radiations effects. Lie Group analysis is used to reduce the governing partial differential equations into non-linear ordinary differential equations. These equations are then solved by an analytical technique known as Homotopy Analysis Method (HAM). A comprehensive study of the problem is being made for various parameters i...

  10. The biological effects of ionising radiation on Crustaceans: A review

    Energy Technology Data Exchange (ETDEWEB)

    Fuller, Neil; Lerebours, Adélaïde [Institute of Marine Sciences, School of Biological Sciences, University of Portsmouth, Ferry Road, Portsmouth, Hampshire PO4 9LY (United Kingdom); Smith, Jim T. [School of Earth & Environmental Sciences, University of Portsmouth, Burnaby Building, Burnaby Road, Portsmouth, Hampshire PO1 3QL (United Kingdom); Ford, Alex T., E-mail: alex.ford@port.ac.uk [Institute of Marine Sciences, School of Biological Sciences, University of Portsmouth, Ferry Road, Portsmouth, Hampshire PO4 9LY (United Kingdom)

    2015-10-15

    Highlights: • We comprehensively review the effects of ionising radiation in crustaceans. • Current environmental radioprotection levels found to be inadequate in some cases. • Mutation is shown to be a sensitive endpoint of radiation exposure. • Lowest observed effect dose rate varies by orders of magnitude. - Abstract: Historic approaches to radiation protection are founded on the conjecture that measures to safeguard humans are adequate to protect non-human organisms. This view is disparate with other toxicants wherein well-developed frameworks exist to minimise exposure of biota. Significant data gaps for many organisms, coupled with high profile nuclear incidents such as Chernobyl and Fukushima, have prompted the re-evaluation of our approach toward environmental radioprotection. Elucidating the impacts of radiation on biota has been identified as priority area for future research within both scientific and regulatory communities. The crustaceans are ubiquitous in aquatic ecosystems, comprising greater than 66,000 species of ecological and commercial importance. This paper aims to assess the available literature of radiation-induced effects within this subphylum and identify knowledge gaps. A literature search was conducted pertaining to radiation effects on four endpoints as stipulated by a number of regulatory bodies: mortality, morbidity, reproduction and mutation. A major finding of this review was the paucity of data regarding the effects of environmentally relevant radiation doses on crustacean biology. Extremely few studies utilising chronic exposure durations or wild populations were found across all four endpoints. The dose levels at which effects occur was found to vary by orders of magnitude thus presenting difficulties in developing phyla-specific benchmark values and reference levels for radioprotection. Based on the limited data, mutation was found to be the most sensitive endpoint of radiation exposure, with mortality the least sensitive

  11. Bi-Abundance Ionisation Structure of the Wolf-Rayet Planetary Nebula PB 8

    Science.gov (United States)

    Danehkar, A.

    2018-01-01

    The planetary nebula PB 8 around a [WN/WC]-hybrid central star is one of planetary nebulae with moderate abundance discrepancy factors (ADFs 2-3), which could be an indication of a tiny fraction of metal-rich inclusions embedded in the nebula (bi-abundance). In this work, we have constructed photoionisation models to reproduce the optical and infrared observations of the planetary nebula PB 8 using a non-LTE stellar model atmosphere ionising source. A chemically homogeneous model initially used cannot predict the optical recombination lines. However, a bi-abundance model provides a better fit to most of the observed optical recombination lines from N and O ions. The metal-rich inclusions in the bi-abundance model occupy 5.6% of the total volume of the nebula, and are roughly 1.7 times cooler and denser than the mean values of the surrounding nebula. The N/H and O/H abundance ratios in the metal-rich inclusions are 1.0 and 1.7 dex larger than the diffuse warm nebula, respectively. To reproduce the Spitzer spectral energy distribution of PB 8, dust grains with a dust-to-gas ratio of 0.01 (by mass) were also included. It is found that the presence of metal-rich inclusions can explain the heavy element optical recombination lines, while a dual-dust chemistry with different grain species and discrete grain sizes likely produces the infrared continuum of this planetary nebula. This study demonstrates that the bi-abundance hypothesis, which was examined in a few planetary nebulae with large abundance discrepancies (ADFs > 10), could also be applied to those typical planetary nebulae with moderate abundance discrepancies.

  12. Effect of negative ionisation of inspired air on the response of asthmatic children to exercise and inhaled histamine.

    Science.gov (United States)

    Ben-Dov, I; Amirav, I; Shochina, M; Amitai, I; Bar-Yishay, E; Godfrey, S

    1983-01-01

    To evaluate the effect of negative ionisation of inspired air on bronchial reactivity, 11 asthmatic children were challenged twice by exercise and 10 were challenged twice by histamine inhalation. The children breathed negatively ionised air (4 X 10(5) - 10 X 10(5) ions/cm3) or control room air in random order in a double-blind fashion. All challenges were matched in terms of basal lung function and the exercise tests were matched in terms of ventilation and respiratory heat loss. Exercise-induced asthma was significantly attenuated by exposure to negatively ionised air, the mean postexercise fall in one-second forced expiratory volume (FEV1) being 29% (SE 5%) of the initial value after the control and 21% (3%) after the ionised air test (p less than 0.02). Ten of the 11 subjects developed less exercise-induced asthma while breathing ionised air. Although the median dose of histamine (cumulative breath units) which caused a constant fall in FEV1 for each individual was higher with the ionised air challenge than with the control challenge the difference was not significant. Five of the 10 subjects were less sensitive to histamine and the other five more sensitive when breathing ionised air. It is concluded that negative ionisation of inspired air can modulate the bronchial response to exercise but the effect on the response to histamine is much more variable. PMID:6351332

  13. 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.

  14. Effect of Hall current and thermal radiation on heat and mass transfer of a chemically reacting MHD flow of a micropolar fluid through a porous medium

    Directory of Open Access Journals (Sweden)

    J.I. Oahimire

    2014-07-01

    Full Text Available Heat and mass transfer effects on an unsteady flow of a chemically reacting micropolar fluid over an infinite vertical porous plate through a porous medium in the presence of a transverse magnetic field with Hall effect and thermal radiation are studied. The governing system of partial differential equations is transformed to dimensionless equations using dimensionless variables. The dimensionless equations are then solved analytically using the perturbation technique to obtain the expressions for velocity, microrotation, temperature and concentration. With the help of graphs, the effects of the various important parameters entering into the problem on the velocity, microrotation, temperature and concentration fields within the boundary layer are discussed. Also the effects of the pertinent parameters on the skin friction coefficient and rates of heat and mass transfer in terms of the Nusselt number and Sherwood number are presented numerically in a tabular form. The results show that the observed parameters have a significant influence on the flow, heat and mass transfer.

  15. Determination of clothing evaporative resistance on a sweating thermal manikin in an isothermal condition: heat loss method or mass loss method?

    Science.gov (United States)

    Wang, Faming; Gao, Chuansi; Kuklane, Kalev; Holmér, Ingvar

    2011-08-01

    This paper addresses selection between two calculation options, i.e heat loss option and mass loss option, for thermal manikin measurements on clothing evaporative resistance conducted in an isothermal condition (T(manikin) = T(a) = T(r)). Five vocational clothing ensembles with a thermal insulation range of 1.05-2.58 clo were selected and measured on a sweating thermal manikin 'Tore'. The reasons why the isothermal heat loss method generates a higher evaporative resistance than that of the mass loss method were thoroughly investigated. In addition, an indirect approach was applied to determine the amount of evaporative heat energy taken from the environment. It was found that clothing evaporative resistance values by the heat loss option were 11.2-37.1% greater than those based on the mass loss option. The percentage of evaporative heat loss taken from the environment (H(e,env)) for all test scenarios ranged from 10.9 to 23.8%. The real evaporative cooling efficiency ranged from 0.762 to 0.891, respectively. Furthermore, it is evident that the evaporative heat loss difference introduced by those two options was equal to the heat energy taken from the environment. In order to eliminate the combined effects of dry heat transfer, condensation, and heat pipe on clothing evaporative resistance, it is suggested that manikin measurements on the determination of clothing evaporative resistance should be performed in an isothermal condition. Moreover, the mass loss method should be applied to calculate clothing evaporative resistance. The isothermal heat loss method would appear to overestimate heat stress and thus should be corrected before use.

  16. Fragmentation, auto-modification and post ionisation proton bound dimer ion formation: the differential mobility spectrometry of low molecular weight alcohols.

    Science.gov (United States)

    Ruszkiewicz, D M; Thomas, C L P; Eiceman, G A

    2016-08-07

    Differential mobility spectrometry (DMS) is currently being used for environmental monitoring of space craft atmospheres and has been proposed for the rapid assessment of patients at accident and emergency receptions. Three studies investigated hitherto undescribed complexity in the DMS spectra of methanol, ethanol, propan-1-ol and butan-1-ol product ions formed from a (63)Ni ionisation source. 54 000 DMS spectra obtained over a concentration range of 0.01 mg m(-3)(g) to 1.80 g m(-3)(g) revealed the phenomenon of auto-modification of the product ions. This occurred when the neutral vapour concentration exceeded the level required to induce a neutral-ion collision during the low field portion of the dispersion field waveform. Further, post-ionisation cluster-ion formation or protonated monomer/proton bound dimer inter-conversion within the ion-filter was indicated by apparent shifts in the values of the protonated monomer compensation field maximum; indicative of post-ionisation conversion of the protonated monomer to a proton-bound dimer. APCI-DMS-quadrupole mass spectrometry studies enabled the ion dissociation products from dispersion-field heating to be monitored and product ion fragmentation relationships to be proposed. Methanol was not observed to dissociate, while propan-1-ol and butan-1-ol underwent dissociation reactions consistent with dehydration processes that led ultimately to the generation of what is tentatively assigned as a cyclo-C3H3(+) ion (m/z 39) and hydrated protons. Studies of the interaction of ion filter temperature with dispersion-field heating of product ions isolated dissociation/fragmentation product ions that have not been previously described in DMS. The implications of these combined findings with regard to data sharing and data interpretation were highlighted.

  17. Exploring Learners' Conceptual Resources: Singapore a Level Students' Explanations in the Topic of Ionisation Energy

    Science.gov (United States)

    Taber, Keith S.; Tan, Kim Chwee Daniel

    2007-01-01

    This paper describes findings from a study to explore Singapore A-level (Grades 11 and 12, 16-19 yr old) students' understanding of ionisation energy, an abstract and complex topic that is featured in school chemistry courses. Previous research had reported that students in the United Kingdom commonly use alternative notions based on the perceived…

  18. Experimental investigation of ionisation track structure of carbon ions at HIL Warsaw.

    Science.gov (United States)

    Bantsar, A; Hilgers, G; Pszona, S; Rabus, H; Szeflinski, Z

    2015-09-01

    In view of the upcoming radiation therapy with carbon ions, the ionisation structure of the carbon ion track at the nanometre scale is of particular interest. Two different nanodosimeters capable of measuring track structure of ionising particles in a gas target equivalent to a nanometric site in condensed matter were involved in the presented experimental investigation, namely the NCBJ Jet Counter and the PTB Ion Counter. At the accelerator facility of the HIL in Warsaw, simulated nanometric volumes were irradiated with carbon ions of 45 and 76 MeV of kinetic energy, corresponding to a range in the tissue of ∼85 µm and ∼190 µm, respectively. The filling gas of both nanodosimeters' ionisation volume was molecular nitrogen N2, and the ionisation cluster size distributions, i.e. the statistical distribution of the number of ionizations produced by one single primary carbon ion in the filling gas, were measured for the two primary particle energies. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  19. Stellar populations, neutral hydrogen, and ionised gas in field early-type galaxies

    NARCIS (Netherlands)

    Serra, P.; Trager, S. C.; Oosterloo, T. A.; Morganti, R.

    Aims. We present a study of the stellar populations of a sample of 39 local, field early-type galaxies whose H I properties are known from interferometric data. Our aim is to understand whether stellar age and chemical composition depend on the H I content of galaxies. We also study their ionised

  20. Calculated ionisation potentials to determine the oxidation of vanillin precursors by lignin peroxidase.

    NARCIS (Netherlands)

    Have, ten R.; Rietjens, I.M.C.M.; Hartmans, S.; Swarts, H.J.; Field, J.A.

    1998-01-01

    In view of the biocatalytic production of vanillin, this research focused on the lignin peroxidase (LiP) catalysed oxidation of naturally occurring phenolic derivatives: O-methyl ethers, O-acetyl esters, and O-glucosyl ethers. The ionisation potential (IP) of a series of model compounds was

  1. The impact of high and low dose ionising radiation on the central nervous system

    Directory of Open Access Journals (Sweden)

    Calina Betlazar

    2016-10-01

    Full Text Available Responses of the central nervous system (CNS to stressors and injuries, such as ionising radiation, are modulated by the concomitant responses of the brains innate immune effector cells, microglia. Exposure to high doses of ionising radiation in brain tissue leads to the expression and release of biochemical mediators of ‘neuroinflammation’, such as pro-inflammatory cytokines and reactive oxygen species (ROS, leading to tissue destruction. Contrastingly, low dose ionising radiation may reduce vulnerability to subsequent exposure of ionising radiation, largely through the stimulation of adaptive responses, such as antioxidant defences. These disparate responses may be reflective of non-linear differential microglial activation at low and high doses, manifesting as an anti-inflammatory or pro-inflammatory functional state. Biomarkers of pathology in the brain, such as the mitochondrial Translocator Protein 18 kDa (TSPO, have facilitated in vivo characterisation of microglial activation and ‘neuroinflammation’ in many pathological states of the CNS, though the exact function of TSPO in these responses remains elusive. Based on the known responsiveness of TSPO expression to a wide range of noxious stimuli, we discuss TSPO as a potential biomarker of radiation-induced effects.

  2. Examining Pre-Service Teachers' Use of Atomic Models in Explaining Subsequent Ionisation Energy Values

    Science.gov (United States)

    Wheeldon, Ruth

    2012-01-01

    Chemistry students' explanations of ionisation energy phenomena often involve a number of non-scientific or inappropriate ideas being used to form causality arguments. Research has attributed this to many science teachers using these ideas themselves (Tan and Taber, in "J Chem Educ" 86(5):623-629, 2009). This research extends this work by…

  3. An ionisation gauge using a channel electron multiplier for pressures below 10$\\^{-12}$

    CERN Document Server

    Blechschmidt, Diether

    1973-01-01

    Since new techniques to achieve pressures of below 10/sup -12/ Torr have been developed, gauges with an appropriate low pressure limit are required. Channeltrons, with their high gain, seem to be the best means to construct gauges with high sensitivity. In this paper a new ionisation gauge using a channeltron has been described. (15 refs).

  4. Design and test of a scintillation dosimeter for dosimetry measurements of high energy radiotherapy beams; Conception et realisation d'un dosimetre a scintillation adapte a la dosimetrie de faisceaux de rayonnements ionisants en faisceaux de rayonnements ionisants en radiotherapie

    Energy Technology Data Exchange (ETDEWEB)

    Fontbonne, J.M

    2002-12-01

    This work describes the design and evaluation of the performances of a scintillation dosimeter developed for the dosimetry of radiation beams used in radiotherapy. The dosimeter consists in a small plastic scintillator producing light which is guided by means of a plastic optical fiber towards photodetectors. In addition to scintillation, high energy ionizing radiations produce Cerenkov light both in the scintillator and the optical fiber. Based on a wavelength analysis, we have developed a deconvolution technique to measure the scintillation light in the presence of Cerenkov light. We stress the advantages that are anticipated from plastic scintillator, in particular concerning tissue or water equivalence (mass stopping power, mass attenuation or mass energy absorption coefficients). We show that detectors based on this material have better characteristics than conventional dosimeters such as ionisation chambers or silicon detectors. The deconvolution technique is exposed, as well as the calibration procedure using an ionisation chamber. We have studied the uncertainty of our dosimeter. The electronics noise, the fiber transmission, the deconvolution technique and the calibration errors give an overall combined experimental uncertainty of about 0,5%. The absolute response of the dosimeter is studied by means of depth dose measurements. We show that absolute uncertainty with photons or electrons beams with energies ranging from 4 MeV to 25 MeV is less than {+-} 1 %. Last, at variance with other devices, our scintillation dosimeter does not need dose correction with depth. (author)

  5. Influence of thermophoresis and Soret-Dufour on magnetohydrodynamic heat and mass transfer over a non-isothermal wedge with thermal radiation and Ohmic dissipation

    Science.gov (United States)

    Pal, Dulal; Mondal, Hiranmoy

    2013-04-01

    The present paper deals with the thermophoresis particle deposition and Soret-Dufour effects on the convective flow, heat and mass transfer characteristics of an incompressible Newtonian electrically conducting fluid having temperature-dependent viscosity over a non-isothermal wedge in the presence of thermal radiation. The governing boundary layer equations are written into a dimensionless form by similarity transformations. The transformed coupled non-linear ordinary differential equations are solved numerically. The effects of various important physical parameters are analyzed in detail. It is found that the skin friction coefficient and the local Sherwood number increase with increase in the values of thermal radiation parameter in the presence of heat generation/absorption whereas reverse effect is seen on the local Nusselt number.

  6. Destruction of Raman biosignatures by ionising radiation and the implications for life detection on Mars.

    Science.gov (United States)

    Dartnell, Lewis R; Page, Kristian; Jorge-Villar, Susana E; Wright, Gary; Munshi, Tasnim; Scowen, Ian J; Ward, John M; Edwards, Howell G M

    2012-04-01

    Raman spectroscopy has proven to be a very effective approach for the detection of microorganisms colonising hostile environments on Earth. The ExoMars rover, due for launch in 2018, will carry a Raman laser spectrometer to analyse samples of the martian subsurface collected by the probe's 2-m drill in a search for similar biosignatures. The martian surface is unprotected from the flux of cosmic rays, an ionising radiation field that will degrade organic molecules and so diminish and distort the detectable Raman signature of potential martian microbial life. This study employs Raman spectroscopy to analyse samples of two model organisms, the cyanobacterium Synechocystis sp. PCC 6803 and the extremely radiation resistant polyextremophile Deinococcus radiodurans, that have been exposed to increasing doses of ionising radiation. The three most prominent peaks in the Raman spectra are from cellular carotenoids: deinoxanthin in D. radiodurans and β-carotene in Synechocystis. The degradative effect of ionising radiation is clearly seen, with significant diminishment of carotenoid spectral peak heights after 15 kGy and complete erasure of Raman biosignatures by 150 kGy of ionising radiation. The Raman signal of carotenoid in D. radiodurans diminishes more rapidly than that of Synechocystis, believed to be due to deinoxanthin acting as a superior scavenger of radiolytically produced reactive oxygen species, and so being destroyed more quickly than the less efficient antioxidant β-carotene. This study highlights the necessity for further experimental work on the manner and rate of degradation of Raman biosignatures by ionising radiation, as this is of prime importance for the successful detection of microbial life in the martian near subsurface.

  7. A semi-analytical model for heat and mass transfer in geothermal reservoirs to estimate fracture surface-are-to-volume ratios and thermal breakthrough using thermally-decaying and diffusing tracers

    Energy Technology Data Exchange (ETDEWEB)

    Reimus, Paul W [Los Alamos National Laboratory

    2010-12-08

    A semi-analytical model was developed to conduct rapid scoping calculations of responses of thermally degrading and diffusing tracers in multi-well tracer tests in enhanced geothermal systems (EGS). The model is based on an existing Laplace transform inversion model for solute transport in dual-porosity media. The heat- and mass-transfer calculations are decoupled and conducted sequentially, taking advantage of the fact that heat transfer between fractures and the rock matrix is much more rapid than mass transfer and therefore mass transfer will effectively occur in a locally isothermal system (although the system will be nonisothermal along fracture flow pathways, which is accounted for by discretizing the flow pathways into multiple segments that have different temperature histories). The model takes advantage of the analogies between heat and mass transfer, solving the same governing equations with k{sub m}/({rho}C{sub p}){sub w} being substituted for {phi}D{sub m} in the equation for fracture transport and k{sub m}/({rho}C{sub p}){sub m} being subsituted for D{sub m} in the equation for matrix transport; where k = thermal conductivity (cal/cm-s-K), {rho} = density (g/cm{sup 3}), C{sub p} = heat capacity (at constant pressure) (cal/g-K), {phi} = matrix porosity, and D = tracer diffusion coefficient (cm{sup 2}/s), with the subscripts w and m referring to water and matrix, respectively. A significant advantage of the model is that it executes in a fraction of second on a single-CPU personal computer, making it very amenable for parameter estimation algorithms that involve repeated runs to find global minima. The combined thermal-mass transport model was used to evaluate the ability to estimate when thermal breakthrough would occur in a multi-well EGS configuration using thermally degrading tracers. Calculations were conducted to evaluate the range of values of Arrhenius parameters, A and E{sub {alpha}} (pre-exponential factor, 1/s, and activation energy, cal

  8. Les méthodesthermiques de production des hydrocarbures. Chapitre 1 : transfert de chaleur et de masse Thermal Methods of Hydrocarbon Production. Chapter 1 : Heat and Mass Transfer

    Directory of Open Access Journals (Sweden)

    Bia P.

    2006-11-01

    Full Text Available Après un rappel général sur le transfert de chaleur et de masse ainsi que sur les lois de conservation dans les milieux continus, on traite de l'adaptation de ces lois au cas des milieux poreux. On donne ensuite des informations quantitatives sur les grandeurs physiques mises en jeu par les phénomènes de transfert en milieu poreux. After making a general review of heat and mass transfer a well as of laws of conservation in continua, this chapter describes how these laws con be adopted to the case of porous media. Quantitative data are then given on the physical magnitudes brought into play by transfer phenomena in porous media.

  9. Tools to discover anionic and nonionic polyfluorinated alkyl surfactants by liquid chromatography electrospray ionisation mass spectrometry

    DEFF Research Database (Denmark)

    Trier, Xenia; Granby, Kit; Christensen, Jan H.

    2011-01-01

    such as [M−H+solvent]− and [(M−H)(M−H+Na)n]− were used to confirm the identity of the precursor ions. In relation to quantification of PFASs, we discuss how their surfactancy influence the ESI processes, challenge their handling in solution and choices of precursor-to-product ions for MSMS of e.......g., structural PFAS isomers. The method has been used to discover PFASs in industrial blends and in extracts from food contact materials....

  10. The effect of thermal processing on the behaviour of peanut allergen peptide targets used in multiple reaction monitoring mass spectrometry experiments.

    Science.gov (United States)

    Sayers, R L; Johnson, P E; Marsh, J T; Barran, P; Brown, H; Mills, E N C

    2016-06-20

    Mass spectrometry-based methods offer an alternative means of determining allergens in foods. Whilst targeted methods are likely to offer the most robust approach for detection and quantification, little is known about how food processing may affect the behaviour of peptide targets. A systematic study has been undertaken to investigate the effects of thermal processing (boiling, roasting, frying) on the behaviour of a suite of peanut peptide targets representing the major clinically-relevant allergens. Initially the effect of thermal processing on protein extractability was investigated and a mass spectrometry-compatible buffer identified comprising 50 mM Tris-HCl, pH 8.8 containing 50 mM dithiothreitol and 0.04% (w/v) acid labile detergent which was able to extract 45-100% of protein from raw, boiled, roasted and fried peanuts using sonication at 60 °C. Eight peptide targets were identified including two peptides from each cupin allergen, Ara h1 and Ara h3 and four peptides from the prolamin superfamily allergens Ara h2, 6 and 7. AQUA peptide standards were synthesised and used to undertake multiple-reaction monitoring experiments, giving assay sensitivities of 0.1-30 amoles of peptide on-column (3 : 1 signal : noise), calculated limits of quantification between 96-1343 amoles of peptide on-column and a linear dynamic range of 4-5 orders of magnitude. Absolute quantification of individual peanut allergens in thermally processed samples showed that peptide targets in the cupin allergens were more prone to processing-induced effects than those from Ara h2, 6 and 7. Targets flanked by arginine residues showed greater thermostability. Identification of processing-stable targets, coupled with more efficient extraction procedures and a wide dynamic range, shows that targeted mass spectrometry methods have great potential as an additional method for quantifying peanut allergens in complex food matrices.

  11. Improved accuracy and precision in δ15 NAIR measurements of explosives, urea, and inorganic nitrates by elemental analyzer/isotope ratio mass spectrometry using thermal decomposition.

    Science.gov (United States)

    Lott, Michael J; Howa, John D; Chesson, Lesley A; Ehleringer, James R

    2015-08-15

    Elemental analyzer systems generate N(2) and CO(2) for elemental composition and isotope ratio measurements. As quantitative conversion of nitrogen in some materials (i.e., nitrate salts and nitro-organic compounds) is difficult, this study tests a recently published method - thermal decomposition without the addition of O(2) - for the analysis of these materials. Elemental analyzer/isotope ratio mass spectrometry (EA/IRMS) was used to compare the traditional combustion method (CM) and the thermal decomposition method (TDM), where additional O(2) is eliminated from the reaction. The comparisons used organic and inorganic materials with oxidized and/or reduced nitrogen and included ureas, nitrate salts, ammonium sulfate, nitro esters, and nitramines. Previous TDM applications were limited to nitrate salts and ammonium sulfate. The measurement precision and accuracy were compared to determine the effectiveness of converting materials containing different fractions of oxidized nitrogen into N(2). The δ(13) C(VPDB) values were not meaningfully different when measured via CM or TDM, allowing for the analysis of multiple elements in one sample. For materials containing oxidized nitrogen, (15) N measurements made using thermal decomposition were more precise than those made using combustion. The precision was similar between the methods for materials containing reduced nitrogen. The %N values were closer to theoretical when measured by TDM than by CM. The δ(15) N(AIR) values of purchased nitrate salts and ureas were nearer to the known values when analyzed using thermal decomposition than using combustion. The thermal decomposition method addresses insufficient recovery of nitrogen during elemental analysis in a variety of organic and inorganic materials. Its implementation requires relatively few changes to the elemental analyzer. Using TDM, it is possible to directly calibrate certain organic materials to international nitrate isotope reference materials without off

  12. Analyses of the wood preservative component N-cyclohexyl-diazeniumdioxide in impregnated pine sapwood by direct thermal desorption-gas chromatography-mass spectrometry.

    Science.gov (United States)

    Jüngel, Peter; de Koning, Sjaak; Brinkman, Udo A Th; Melcher, Eckhard

    2002-04-12

    Investigations concerning the qualitative and quantitative determination of the organic wood preservative component N-cyclohexyl-diazeniumdioxide (HDO) in treated timber were carried out by means of direct thermal desorption-gas chromatography-mass spectrometry (DTD-GC-MS). It could be shown that the identification of HDO in treated pine sapwood (Pinus sylyestris L.) is relatively simple using this analytical technique. Quantification of this active ingredient can be carried out using the peak area of the specific mass fragment m/z 114. A calibration curve with a high correlation coefficient was obtained in the range from 40 to 550 mg HDO per kg timber. Furthermore it can be deduced that the results obtained are characterised by an excellent reproducibility with standard deviations ranging from 5 to 10% in general. For the chosen experimental set up a detection limit of 4 mg HDO per kg treated pine sapwood was calculated, although merely 20% of the active ingredient was desorbed.

  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. Improvement in Thermal-Ionization Mass Spectrometry (TIMS) using Total Flash Evaporation (TFE) method for lanthanides isotope ratio measurements in transmutation targets

    Energy Technology Data Exchange (ETDEWEB)

    Mialle, S.; Gourgiotis, A.; Aubert, M.; Stadelmann, G.; Gautier, C.; Isnard, H. [Commissariat a l' Energie Atomique, CEA Saclay, DEN/DPC/SECR/LANIE, 91191 Gif sur Yvette (France); Chartier, F. [Commissariat a l' Energie Atomique, CEA Saclay, DEN/DPC, 91191 Gif sur Yvette (France)

    2011-07-01

    The experiments involved in the PHENIX french nuclear reactor to obtain precise and accurate data on the total capture cross sections of the heavy isotopes and fission products require isotopic ratios measurements with uncertainty of a few per mil. These accurate isotopic ratio measurements are performed with mass spectrometer equipped with multi-collector system. The major difficulty for the analyses of these actinides and fission products is the low quantity of the initial powder enclosed in steel container (3 to 5 mg) and the very low quantities of products formed (several {mu}g) after irradiation. Specific analytical developments are performed by Thermal Ionization Mass Spectrometry (TIMS) to be able to analyse several nanograms of elements with this technique. A specific method of acquisition named Total Flash Evaporation was adapted in this study in the case of lanthanide measurements for quantity deposited on the filament in the order of 2 ng and applied on irradiated fuel. To validate the analytical approach and discuss about the accuracy of the data, the isotopic ratios obtained by TIMS are compared with other mass spectrometric techniques such as Multiple-Collector Inductively Coupled Plasma Mass Spectrometer (MC-ICPMS). (authors)

  15. Theoretical investigation of the ultrafast dissociation of ionised biomolecules immersed in water: direct and indirect effects.

    Science.gov (United States)

    Gaigeot, M-P; Lopez-Tarifa, P; Martin, F; Alcami, M; Vuilleumier, R; Tavernelli, I; Hervé du Penhoat, M-A; Politis, M-F

    2010-01-01

    Theoretical simulations are particularly well suited to investigate, at a molecular level, direct and indirect effects of ionising radiations in DNA, as in the particular case of irradiation by swift heavy ions such as those used in hadron therapy. In the past recent years, we have developed the modeling at the microscopic level of the early stages of the Coulomb explosion of DNA molecules immersed in liquid water that follows the irradiation by swift heavy ions. To that end, Time-Dependent Density Functional Theory molecular dynamics simulations (TD-DFT MD) have been developed where localised Wannier orbitals are propagated. This latter enables to separate molecular orbitals of each water molecule from the molecular orbitals of the biomolecule. Our main objective is to demonstrate that the double ionisation of one molecule of the liquid sample, either one water molecule from the solvent or the biomolecule, may be in some cases responsible for the formation of an atomic oxygen as a direct consequence of the molecule Coulomb explosion. Our hypothesis is that the molecular double ionisation arising from irradiation by swift heavy ions (about 10% of ionisation events by ions whose velocity is about the third of speed of light), as a primary event, though maybe less probable than other events resulting from the electronic cascading (for instance, electronic excitations, electron attachments), may be systematically more damageable (and more lethal), as supported by experiments that have been carried out in our group in the 1990s (in studies of damages created by K holes in DNA). The chemical reactivity of the produced atomic oxygen with other radicals present in the medium will ultimately lead to chemical products that are harmful to DNA. In the present paper, we review our theoretical methodology in an attempt that the community be familiar with our new approach. Results on the production of atomic oxygen as a result of the double ionisation of water or as a result of

  16. Ratios of colony mass to thermal conductance of tree and man-made nest enclosures of Apis mellifera: implications for survival, clustering, humidity regulation and Varroa destructor

    Science.gov (United States)

    Mitchell, Derek

    2016-05-01

    In the absence of human intervention, the honeybee ( Apis mellifera L.) usually constructs its nest in a tree within a tall, narrow, thick-walled cavity high above the ground (the enclosure); however, most research and apiculture is conducted in the thin-walled, squat wooden enclosures we know as hives. This experimental research, using various hives and thermal models of trees, has found that the heat transfer rate is approximately four to seven times greater in the hives in common use, compared to a typical tree enclosure in winter configuration. This gives a ratio of colony mass to lumped enclosure thermal conductance (MCR) of less than 0.8 kgW-1 K for wooden hives and greater than 5 kgW-1 K for tree enclosures. This result for tree enclosures implies higher levels of humidity in the nest, increased survival of smaller colonies and lower Varroa destructor breeding success. Many honeybee behaviours previously thought to be intrinsic may only be a coping mechanism for human intervention; for example, at an MCR of above 2 kgW-1 K, clustering in a tree enclosure may be an optional, rare, heat conservation behaviour for established colonies, rather than the compulsory, frequent, life-saving behaviour that is in the hives in common use. The implied improved survival in hives with thermal properties of tree nests may help to solve some of the problems honeybees are currently facing in apiculture.

  17. Analysis of the volatile organic matter of engine piston deposits by direct sample introduction thermal desorption gas chromatography/mass spectrometry.

    Science.gov (United States)

    Diaby, M; Kinani, S; Genty, C; Bouchonnet, S; Sablier, M; Le Negrate, A; El Fassi, M

    2009-12-01

    This article establishes an alternative method for the characterization of volatiles organic matter (VOM) contained in deposits of the piston first ring grooves of diesel engines using a ChromatoProbe direct sample introduction (DSI) device coupled to gas chromatography/mass spectrometry (GC/MS) analysis. The addition of an organic solvent during thermal desorption leads to an efficient extraction and a good chromatographic separation of extracted products. The method was optimized investigating the effects of several solvents, the volume added to the solid sample, and temperature programming of the ChromatoProbe DSI device. The best results for thermal desorption were found using toluene as an extraction solvent and heating the programmable temperature injector from room temperature to 300 degrees C with a temperature step of 105 degrees C. With the use of the optimized thermal desorption conditions, several components have been positively identified in the volatile fraction of the deposits: aromatics, antioxidants, and antioxidant degradation products. Moreover, this work highlighted the presence of diesel fuel in the VOM of the piston deposits and gave new facts on the absence of the role of diesel fuel in the deposit formation process. Most importantly, it opens the possibility of quickly performing the analysis of deposits with small amounts of samples while having a good separation of the volatiles.

  18. Ratios of colony mass to thermal conductance of tree and man-made nest enclosures of Apis mellifera: implications for survival, clustering, humidity regulation and Varroa destructor.

    Science.gov (United States)

    Mitchell, Derek

    2016-05-01

    In the absence of human intervention, the honeybee (Apis mellifera L.) usually constructs its nest in a tree within a tall, narrow, thick-walled cavity high above the ground (the enclosure); however, most research and apiculture is conducted in the thin-walled, squat wooden enclosures we know as hives. This experimental research, using various hives and thermal models of trees, has found that the heat transfer rate is approximately four to seven times greater in the hives in common use, compared to a typical tree enclosure in winter configuration. This gives a ratio of colony mass to lumped enclosure thermal conductance (MCR) of less than 0.8 kgW(-1) K for wooden hives and greater than 5 kgW(-1) K for tree enclosures. This result for tree enclosures implies higher levels of humidity in the nest, increased survival of smaller colonies and lower Varroa destructor breeding success. Many honeybee behaviours previously thought to be intrinsic may only be a coping mechanism for human intervention; for example, at an MCR of above 2 kgW(-1) K, clustering in a tree enclosure may be an optional, rare, heat conservation behaviour for established colonies, rather than the compulsory, frequent, life-saving behaviour that is in the hives in common use. The implied improved survival in hives with thermal properties of tree nests may help to solve some of the problems honeybees are currently facing in apiculture.

  19. Identification of volatile butyl rubber thermal-oxidative degradation products by cryofocusing gas chromatography/mass spectrometry (cryo-GC/MS).

    Energy Technology Data Exchange (ETDEWEB)

    Smith, Jonell Nicole; White, Michael Irvin; Bernstein, Robert; Hochrein, James Michael

    2013-02-01

    Chemical structure and physical properties of materials, such as polymers, can be altered as aging progresses, which may result in a material that is ineffective for its envisioned intent. Butyl rubber formulations, starting material, and additives were aged under thermal-oxidative conditions for up to 413 total days at up to 124 ÀC. Samples included: two formulations developed at Kansas City Plant (KCP) (#6 and #10), one commercially available formulation (#21), Laxness bromobutyl 2030 starting material, and two additives (polyethylene AC-617 and Vanax MBM). The low-molecular weight volatile thermal-oxidative degradation products that collected in the headspace over the samples were preconcentrated, separated, and detected using cryofocusing gas chromatography mass spectrometry (cryo-GC/MS). The majority of identified degradation species were alkanes, alkenes, alcohols, ketones, and aldehydes. Observations for Butyl #10 aged in an oxygen-18 enriched atmosphere (18O2) were used to verify when the source of oxygen in the applicable degradation products was from the gaseous environment rather than the polymeric mixture. For comparison purposes, Butyl #10 was also aged under non-oxidative thermal conditions using an argon atmosphere.

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

  1. [Real-time analysis of polyvinyl chloride thermal decomposition/combustion products with single photon ionization/photoelectron ionization online mass spectrometer].

    Science.gov (United States)

    Chen, Wen-Dong; Hou, Ke-Yong; Chen, Ping; Li, Fang-Long; Zhao, Wu-Duo; Cui, Hua-Peng; Hua, Lei; Xie, Yuan-Yuan; Li, Hai-Yang

    2013-01-01

    With the features of a broad range of ionizable compounds, reduced fragments and simple mass spectrum, a homemade magnetic field enhanced photoelectron ionization (MEPEI) source combined with single photon ionization (SPI) for time-of-flight mass spectrometer was built and applied to analyze thermal decomposition/combustion products of polyvinyl chloride (PVC). The combined ion source can be switched very fast between SPI mode and SPI-MEPEI mode for detecting different targeted compounds, and only adjusting the voltage of the electrode in the ionization region to trigger the switch. Among the PVC thermal decomposition/combustion products, HCl and CO2, which ionization energies (12.74 eV, 13.77 eV respectively) were higher than the energy of photon (10.60 eV), were ionized by MEPEI, while alkenes, dichloroethylene, benzene and its homologs, monochlorobenzene, styrene, indane, naphthalene and its homologs were ionized by SPI and MEPEI simultaneously. Spectra of interested products as a function of temperatures indicated that products are formed via two main mechanisms: (1) dechlorination and intramolecular cyclization can lead to the formation of HCl, benzene and naphthalene at 250-370 degrees C; (2) intermolecular crosslinking leads to the formation of alkyl aromatics such as toluene and xylene/ethylbenzene at 380-510 degrees C. The experimental results show that the combined ion source of SPI/ SPI-MEPEI for TOF-MS has broad application prospects in the online analysis field.

  2. Ionisation and dissociation of water induced by swift multicharged ions; Etude de l'ionisation et de la dissociation d'H{sub 2}O induites par collision avec des ions multicharges rapides

    Energy Technology Data Exchange (ETDEWEB)

    Legendre, S

    2006-02-15

    Ionization and dissociation of water molecules and water clusters induced by 11.7 MeV/A Ni{sup 25+} ions were carried out by imaging techniques. Branching ratios, ionisation cross sections and Kinetic Energy Released distributions have been measured together with fragmentation dynamics studies. Multiple ionization represents approximately 30% of the ionizing events. Double ionization produces in significant way atomic oxygen, considered as a possible precursor of the large production of HO{sub 2} radical in liquid water radiolysis by ions of high Linear Energy Transfer. We evidence a strong selectivity of bond breakage in the case of ion-induced HOD fragmentation. Once the molecule doubly ionized, the breakage of the O-H bond is found 6.5 times more probable than that of the O-D bond. A semi-classical calculation simulating the fragmentation dynamics on the potential energy surface of the ground-state of di-cation H{sub 2}O{sup 2+} makes possible to as well reproduce the preferential nature of the breakage of the O-H bond as the position and the shift of the kinetic energy distributions. First results concerning interaction with water clusters are also reported. Measurements in coincidence are carried out giving access to correlation, with the distributions in energy and angle of the emitted fragments. Mass spectrum points fast intra-cluster proton transfer, leading to the emission of protonated clusters. (author)

  3. Effect of the diaphragm of free-air ionisation chamber for X-ray air-kerma measurements.

    Science.gov (United States)

    Kurosawa, Tadahiro; Takata, Nobuhisa; Saito, Norio

    2011-07-01

    Free-air ionisation chambers are widely used at standards laboratories as primary standards for absolute measurements of air kerma in X-ray fields. The area of the diaphragm aperture of a free-air ionisation chambers is an important factor for absolute measurements because it defines the size of the X-ray beam incident on the free-air chamber. In this study, correction factors for the contribution of X rays transmitted through the diaphragm of a free-air ionisation chamber and those scattered from the surface of the diaphragm aperture are obtained by Monte Carlo simulation for two different sized free-air ionisation chambers and for various diaphragm aperture sizes, X-ray energies and source-to-chamber distances.

  4. Simultaneous determination of volatile and non-volatile nitrosamines in processed meat products by liquid chromatography tandem mass spectrometry using atmospheric pressure chemical ionisation and electrospray ionisation

    DEFF Research Database (Denmark)

    Herrmann, Susan Strange; Duedahl-Olesen, Lene; Granby, Kit

    2014-01-01

    A sensitive, selective and generic method has been developed for the simultaneous determination of the contents (μgkg−1 range) of both volatile nitrosamines (VNA) and non-volatile nitrosamines (NVNA) in processed meat products. The extraction procedure only requires basic laboratory equipment...... and a small volume of organic solvent. Separation and quantification were performed by the developed LC–(APCI/ESI)MS/MS method. The method was validated using spiked samples of three different processed meat products. Satisfactory recoveries (50–130%) and precisions (2–23%) were obtained for eight VNA and six...... NVNAs with LODs generally between 0.2 and 1μgkg−1, though for a few analyte/matrix combinations higher LODs were obtained (3 to 18μgkg−1). The validation results show that results obtained for one meat product is not always valid for other meat products. We were not able to obtain satisfactory results...

  5. How do air ions reflect variations in ionising radiation in the lower atmosphere in a boreal forest?

    Directory of Open Access Journals (Sweden)

    X. Chen

    2016-11-01

    Full Text Available Most of the ion production in the atmosphere is attributed to ionising radiation. In the lower atmosphere, ionising radiation consists mainly of the decay emissions of radon and its progeny, gamma radiation of the terrestrial origin as well as photons and elementary particles of cosmic radiation. These types of radiation produce ion pairs via the ionisation of nitrogen and oxygen as well as trace species in the atmosphere, the rate of which is defined as the ionising capacity. Larger air ions are produced out of the initial charge carriers by processes such as clustering or attachment to pre-existing aerosol particles. This study aimed (1 to identify the key factors responsible for the variability in ionising radiation and in the observed air ion concentrations, (2 to reveal the linkage between them and (3 to provide an in-depth analysis into the effects of ionising radiation on air ion formation, based on measurement data collected during 2003–2006 from a boreal forest site in southern Finland. In general, gamma radiation dominated the ion production in the lower atmosphere. Variations in the ionising capacity came from mixing layer dynamics, soil type and moisture content, meteorological conditions, long-distance transportation, snow cover attenuation and precipitation. Slightly similar diurnal patterns to variations in the ionising capacity were observed in air ion concentrations of the cluster size (0.8–1.7 nm in mobility diameters. However, features observed in the 0.8–1 nm ion concentration were in good connection to variations of the ionising capacity. Further, by carefully constraining perturbing variables, a strong dependency of the cluster ion concentration on the ionising capacity was identified, proving the functionality of ionising radiation in air ion production in the lower atmosphere. This relationship, however, was only clearly observed on new particle formation (NPF days, possibly indicating that charges after

  6. Development of a short path thermal desorption-gas chromatography/mass spectrometry method for the determination of polycyclic aromatic hydrocarbons in indoor air.

    Science.gov (United States)

    Li, Yingjie; Xian, Qiming; Li, Li

    2017-05-12

    Polycyclic aromatic hydrocarbons (PAHs) are present in petroleum based products and are combustion by-products of organic matters. Determination of levels of PAHs in the indoor environment is important for assessing human exposure to these chemicals. A new short path thermal desorption (SPTD) gas chromatography/mass spectrometry (GC/MS) method for determining levels of PAHs in indoor air was developed. Thermal desorption (TD) tubes packed with glass beads, Carbopack C, and Carbopack B in sequence, were used for sample collection. Indoor air was sampled using a small portable pump over 7 days at 100ml/min. Target PAHs were thermally released and introduced into the GC/MS for analysis through the SPTD unit. During tube desorption, PAHs were cold trapped (-20°C) at the front end of the GC column. Thermal desorption efficiencies were 100% for PAHs with 2 and 3 rings, and 99-97% for PAHs with 4-6 rings. Relative standard deviation (RSD) values among replicate samples spiked at three different levels were around 10-20%. The detection limit of this method was at or below 0.1μg/m3 except for naphthalene (0.61μg/m3), fluorene (0.28μg/m3) and phenanthrene (0.35μg/m3). This method was applied to measure PAHs in indoor air in nine residential homes. The levels of PAHs in indoor air found in these nine homes are similar to indoor air values reported by others. Copyright © 2017 Elsevier B.V. All rights reserved.

  7. Heat and Mass Transfer in a High-Porous Low-Temperature Thermal Insulation in Real Operating Conditions

    Directory of Open Access Journals (Sweden)

    Polovnikov Vyacheslav Yu.

    2015-01-01

    Full Text Available The results of numerical simulation of heat and mass transfer in a high-porous low-temperature insulation in conditions of insulation freezing, a moisture migration to the front of phase transition and a condensation forming on an outer contour of interaction were obtained. Values of heat leakage were established.

  8. Effect of radiation-induced charge accumulation on build-up cap on the signal current from an ionisation chamber.

    Science.gov (United States)

    Takata, N; Morishita, Y

    2011-04-01

    The signal current from a thimble ionisation chamber with a build-up cap made of an insulator decreases by about 0.41 % after being irradiated for 17 h at an air kerma rate of 41 Gy h(-1) by a collimated (60)Co gamma-ray beam in air. In contrast, the signal current remains constant when the thimble ionisation chamber is irradiated in a water phantom. During irradiation, positive charge is considered to accumulate near the outer surface of the build-up cap where electron equilibrium is not achieved. Secondary electrons travelling in the build-up cap and the chamber wall toward the ionisation volume are decelerated by the electric field generated by the positive charge. Consequently, the signal current decreases with increasing charge accumulation because some secondary electrons are prevented from entering the ionisation volume. In the water phantom, electron equilibrium is established in and around the ionisation chamber and charge does not accumulate. To confirm this hypothesis, the signal current was measured for an ionisation chamber in air with a build-up cap wrapped with Al foil and covered with PMMA tubes. Electron equilibrium was established over the build-up cap because the tubes were thicker than the secondary electron range. The signal current decreased with increasing positive voltage applied to the Al foil. It was estimated from the results that positive charges equivalent to a voltage of over 6 kV applied to the Al foil accumulated during irradiation. The signal current was also measured for an ionisation chamber with a metal build-up cap and for an ionisation chamber with a wall and build-up cap made of conductive plastic.

  9. A micro-gap, air-filled ionisation chamber as a detector for criticality accident dosimetry.

    Science.gov (United States)

    Murawski, Ł; Zielczyński, M; Golnik, N; Gryziński, M A

    2014-10-01

    A micro-gap air-filled ionisation chamber was designed for criticality dosimetry. The special feature of the chamber is its very small gap between electrodes of only 0.3 mm. This prevents ion recombination at high dose rates and minimises the influence of gas on secondary particles spectrum. The electrodes are made of polypropylene because of higher content of hydrogen in this material, when compared with soft tissue. The difference between neutron and gamma sensitivity in such chamber becomes practically negligible. The chamber's envelope contains two specially connected capacitors, one for polarising the electrodes and the other for collecting the ionisation charge. © The Author 2013. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  10. An important step forward in continuous spectroscopic imaging of ionising radiations using ASICs

    CERN Document Server

    Fessler, P; Eberle, H; Raad-Iseli, C D; Hilt, B; Huss, D; Krummenacher, F; Lutz, Jean Robert; Prevot, G; Renouprez, Albert Jean; Sigward, M H; Schwaller, B; Voltolini, C

    1999-01-01

    Characterization results are given for an original ASIC allowing continuous acquisition of ionising radiation images in spectroscopic mode. Ionising radiation imaging in general and spectroscopic imaging in particular must primarily be guided by the attempt to decrease statistical noise, which requires detection systems designed to allow very high counting rates. Any source of dead time must therefore be avoided. Thus, the use of on-line corrections of the inevitable dispersion of characteristics between the large number of electronic channels of the detection system, shall be precluded. Without claiming to achieve ultimate noise levels, the work described is focused on how to prevent good individual acquisition channel noise performance from being totally destroyed by the dispersion between channels without introducing dead times. With this goal, we developed an automatic charge amplifier output voltage offset compensation system which operates regardless of the cause of the offset (detector or electronic). ...

  11. Exploring the Powerful Ionised Wind in the Seyfert Galaxy PG1211+143

    Science.gov (United States)

    Pounds, Ken

    2013-10-01

    Highly-ionised high-speed winds in AGN (UFOs) were first detected with XMM-Newton a decade ago, and are now established as a key factor in the study of SMBH accretion, and in the growth and metal enrichment of their host galaxies. However, information on the ionisation and dynamical structure, and the ultimate fate of UFOs remains very limited. We request a 600ks extended XMM-Newton study of the prototype UFO PG1211+143 in AO-13, to obtain high quality EPIC and RGS spectra, to map the flow structure and variability, while seeking evidence for the anticipated interaction with the ISM and possible conversion of the energetic wind to a momentum-driven flow.

  12. Radon in drinking water: Comparison and evaluation of two ionisation chamber activity measurement methods.

    Science.gov (United States)

    Wiedner, H; Lotter, K; Karner, P; Friedmann, H; Maringer, F J

    2017-06-23

    In this study the radon activity concentration of water samples from the so called "Thermenlinie" are measured using two different techniques: currents measured with an ionisation chamber setup developed by H. Friedmann are compared with results obtained using a commercially available AlphaGUARD. A fit to compensate for measurements made in non-equilibrium state is applied and the detection limit is estimated. Copyright © 2017 Elsevier Ltd. All rights reserved.

  13. Exposure of the French paediatric population to ionising radiation from diagnostic medical procedures in 2010

    Energy Technology Data Exchange (ETDEWEB)

    Etard, Cecile; Aubert, Bernard [Institut de Radioprotection et de Surete Nucleaire, Medical Expertise Unit, Fontenay-aux-Roses (France); Mezzarobba, Myriam [Institut de Radioprotection et de Surete Nucleaire, Laboratory of Epidemiology, Fontenay-aux-Roses (France); Bernier, Marie-Odile [Institut de Radioprotection et de Surete Nucleaire, Laboratory of Epidemiology, Fontenay-aux-Roses (France); Institut de Radioprotection et de Surete Nucleaire, IRSN/PRP-HOM/SRBE/LEPID, Laboratoire d' Epidemiologie, Fontenay-aux-Roses (France)

    2014-12-15

    Medical examination is the main source of artificial radiation exposure. Because children present an increased sensitivity to ionising radiation, radiology practices at a national level in paediatrics should be monitored. This study describes the ionising radiation exposure from diagnostic medical examinations of the French paediatric population in 2010. Data on frequency of examinations were provided by the French National Health Insurance through a representative sample including 107,627 children ages 0-15 years. Effective doses for each type of procedure were obtained from the published French literature. Median and mean effective doses were calculated for the studied population. About a third of the children were exposed to at least one examination using ionising radiation in 2010. Conventional radiology, dental exams, CT scans and nuclear medicine and interventional radiology represent respectively 55.3%, 42.3%, 2.1% and 0.3% of the procedures. Children 10-15 years old and babies from birth to 1 year are the most exposed populations, with respectively 1,098 and 734 examinations per 1,000 children per year. Before 1 year of age, chest and pelvis radiographs are the most common imaging tests, 54% and 32%, respectively. Only 1% of the studied population is exposed to CT scan, with 62% of these children exposed to a head-and-neck procedure. The annual median and mean effective doses were respectively 0.03 mSv and 0.7 mSv for the exposed children. This study gives updated reference data on French paediatric exposure to medical ionising radiation that can be used for public health or epidemiological purposes. Paediatric diagnostic use appears much lower than that of the whole French population as estimated in a previous study. (orig.)

  14. New coplanar (e,2e) experiments for the ionisation of He and Ar atoms

    Energy Technology Data Exchange (ETDEWEB)

    Casagrande, E.M. Staicu [Laboratoire des Collisions Atomiques et Moleculaires (UMR 8625) and Federation Lumiere Matiere (FR 2764), Bat. 351, Universite de Paris-Sud XI, 91405 Orsay Cedex (France)], E-mail: staicu-casagrande@lcam.u-psud.fr; Catoire, F.; Naja, A.; Ren, X.G.; Lahmam-Bennani, A. [Laboratoire des Collisions Atomiques et Moleculaires (UMR 8625) and Federation Lumiere Matiere (FR 2764), Bat. 351, Universite de Paris-Sud XI, 91405 Orsay Cedex (France); Nekkab, M. [Laboratoire de Physique Quantique et Systemes Dynamiques, Universite Ferhat Abbas, Setif (Algeria); Dal Cappello, C. [Laboratoire de Physique Moleculaire et des Collisions and ICPMB (FR 2843), Universite Paul Verlaine-Metz, Institut de Physique, 1 rue Arago, 57078 Metz Cedex 3 (France); Bartschat, K. [Department of Physics and Astronomy, Drake University, Des Moines, IA 5031 (United States); Whelan, C.T. [Department of Physics, College of Sciences, Norfolk, VA 23529-0116 (United States)

    2007-10-15

    We report new coplanar measurements of the (e,2e) TDCS for the ionisation of helium 1s-shell and argon 3p- and 2p-shells. The kinematics employed remained rather unexplored to date, and could be investigated here using an improved version of our multi-angle (e,2e) spectrometer, with increased sensitivity. The results are discussed in the light of state-of-the-art theoretical models.

  15. Desorption Electrospray Ionization Mass Spectrometry (DESI-MS) Analysis of Organophosphorus Chemical Warfare Agents: Rapid Acquisition of Time-Aligned Parallel (TAP) Fragmentation Data

    Science.gov (United States)

    2010-06-01

    Résumé …..... On a appliqué la méthode désorption - ionisation par électronébulisation - spectrométrie de masse (DESI-SM) pour l’analyse...2010-047, R & D pour la défense Canada – Suffield; Juin 2010. Introduction : On a appliqué la méthode désorption – ionisation par...132, 868-875. DRDC Suffield TM 2010-047 29 [26] Williams, J.P. and Scrivens, J.H. (2008). Coupling desorption electrospray ionisation with

  16. Comparison of ionisation measurements in water and polystyrene for electron beam dosimetry.

    Science.gov (United States)

    Bruinvis, I A; Heukelom, S; Mijnheer, B J

    1985-10-01

    For the determination of absorbed dose to water in electron beams, dosimetry protocols advocate ionisation measurements in plastic phantoms instead of water for practical reasons. The chamber readings in polystyrene at the depth of maximum ionisation must be corrected for the difference in physical properties between the two materials. This correction factor was determined for a Farmer 0.6 cm3 graphite-walled chamber in electron beams with mean energies at the phantom surface between 6 and 19 MeV. Experiments with white polystyrene yielded corrections for the measured ionisation ranging from 0.3 to 2.4%. For clear polystyrene, 0.6-1% higher corrections were found. For beams with the same mean energy at the phantom surface, but with different beam-flattening and collimation systems, variations in this correction up to 1.2% were observed. In contrast to recent reports on electrical charge storage in polystyrene due to electron irradiation, our experiments do not show differences in the chamber readings any larger than 0.5%.

  17. Standard test method for determination of uranium or plutonium isotopic composition or concentration by the total evaporation method using a thermal ionization mass spectrometer

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2007-01-01

    1.1 This method describes the determination of the isotopic composition and/or the concentration of uranium and plutonium as nitrate solutions by the thermal ionization mass spectrometric (TIMS) total evaporation method. Purified uranium or plutonium nitrate solutions are loaded onto a degassed metal filament and placed in the mass spectrometer. Under computer control, ion currents are generated by heating of the filament(s). The ion beams are continually measured until the sample is exhausted. The measured ion currents are integrated over the course of the run, and normalized to a reference isotope ion current to yield isotopic ratios. 1.2 In principle, the total evaporation method should yield isotopic ratios that do not require mass bias correction. In practice, some samples may require this bias correction. When compared to the conventional TIMS method, the total evaporation method is approximately two times faster, improves precision from two to four fold, and utilizes smaller sample sizes. 1.3 The tot...

  18. Stable Chlorine Isotopes and Elemental Chlorine by Thermal Ionization Mass Spectrometry and Ion Chromatography; Martian Meteorites, Carbonaceous Chondrites and Standard Rocks

    Science.gov (United States)

    Nakamura, N.; Nyquist, L. E.; Reese, Y.; Shih, C.-Y.; Fujitani, T.; Okano, O.

    2011-01-01

    Recently significantly large mass fractionation of stable chlorine isotopes has been reported for terrestrial and lunar samples [1,2]. In addition, in view of possible early solar system processes [3] and also potential perchlorate-related fluid/microbial activities on the Martian surface [4,5], a large chlorine isotopic fractionation might be expected for some types of planetary materials. Due to analytical difficulties of isotopic and elemental analyses, however, current chlorine analyses for planetary materials are controversial among different laboratories, particularly between IRMS (gas source mass spectrometry) and TIMS (Thermal Ionization Mass Spectrometry) groups [i.e. 1,6,7] for isotopic analyses, as well as between those doing pyrohydrolysis and other groups [i.e. 6,8]. Additional careful investigations of Cl isotope and elemental abundances are required to confirm real chlorine isotope and elemental variations for planetary materials. We have developed a TIMS technique combined with HF-leaching/ion chromatography at NASA JSC that is applicable to analysis of small amounts of meteoritic and planetary materials. We present here results for several standard rocks and meteorites, including Martian meteorites.

  19. Standard test method for isotopic analysis of hydrolyzed uranium hexafluoride and uranyl nitrate solutions by thermal ionization mass spectrometry

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2005-01-01

    1.1 This method applies to the determination of isotopic composition in hydrolyzed nuclear grade uranium hexafluoride. It covers isotopic abundance of 235U between 0.1 and 5.0 % mass fraction, abundance of 234U between 0.0055 and 0.05 % mass fraction, and abundance of 236U between 0.0003 and 0.5 % mass fraction. This test method may be applicable to other isotopic abundance providing that corresponding standards are available. 1.2 This test method can apply to uranyl nitrate solutions. This can be achieved either by transforming the uranyl nitrate solution to a uranyl fluoride solution prior to the deposition on the filaments or directly by depositing the uranyl nitrate solution on the filaments. In the latter case, a calibration with uranyl nitrate standards must be performed. 1.3 This test method can also apply to other nuclear grade matrices (for example, uranium oxides) by providing a chemical transformation to uranyl fluoride or uranyl nitrate solution. 1.4 This standard does not purport to address al...

  20. Thermal radiation and mass transfer effects on unsteady MHD free convection flow past a vertical oscillating plate

    Science.gov (United States)

    Rana, B. M. Jewel; Ahmed, Rubel; Ahmmed, S. F.

    2017-06-01

    Unsteady MHD free convection flow past a vertical porous plate in porous medium with radiation, diffusion thermo, thermal diffusion and heat source are analyzed. The governing non-linear, partial differential equations are transformed into dimensionless by using non-dimensional quantities. Then the resultant dimensionless equations are solved numerically by applying an efficient, accurate and conditionally stable finite difference scheme of explicit type with the help of a computer programming language Compaq Visual Fortran. The stability and convergence analysis has been carried out to establish the effect of velocity, temperature, concentration, skin friction, Nusselt number, Sherwood number, stream lines and isotherms line. Finally, the effects of various parameters are presented graphically and discussed qualitatively.

  1. Analysis of asymmetric resonance response of thermally excited silicon micro-cantilevers for mass-sensitive nanoparticle detection

    Science.gov (United States)

    Bertke, Maik; Hamdana, Gerry; Wu, Wenze; Suryo Wasisto, Hutomo; Uhde, Erik; Peiner, Erwin

    2017-06-01

    In this paper, the asymmetric resonance frequency (f 0) responses of thermally in-plane excited silicon cantilevers for a pocket-sized, cantilever-based airborne nanoparticle detector (Cantor) are analysed. By measuring the shift of f 0 caused by the deposition of nanoparticles (NPs), the cantilevers are used as a microbalance. The cantilever sensors are low cost manufactured from silicon by bulk-micromachining techniques and contain an integrated p-type heating actuator and a sensing piezoresistive Wheatstone bridge. f 0 is tracked by a homemade phase-locked loop (PPL) for real-time measurements. To optimize the sensor performance, a new cantilever geometry was designed, fabricated and characterized by its frequency responses. The most significant characterisation parameters of our application are f 0 and the quality factor (Q), which have high influences on sensitivity and efficiency of the NP detector. Regarding the asymmetric resonance signal, a novel fitting function based on the Fano resonance replacing the conventionally used function of the simple harmonic oscillator and a method to calculate Q by its fitting parameters were developed for a quantitative evaluation. To obtain a better understanding of the resonance behaviours, we analysed the origin of the asymmetric line shapes. Therefore, we compared the frequency response of the on-chip thermal excitation with an external excitation using an in-plane piezo actuator. In correspondence to the Fano effect, we could reconstruct the measured resonance curves by coupling two signals with constant amplitude and the expected signal of the cantilever, respectively. Moreover, the phase of the measurement signal can be analysed by this method, which is important to understand the locking process of the PLL circuit. Besides the frequency analysis, experimental results and calibration measurements with different particle types are presented. Using the described analysis method, decent results to optimize a next

  2. Influence of Hall Current and Thermal Radiation on MHD Convective Heat and Mass Transfer in a Rotating Porous Channel with Chemical Reaction

    Directory of Open Access Journals (Sweden)

    Dulal Pal

    2013-01-01

    Full Text Available A theoretical study is carried out to obtain an analytic solution of heat and mass transfer in a vertical porous channel with rotation and Hall current. A constant suction and injection is applied to the two insulating porous plates. A strong magnetic field is applied in the transverse direction. The entire system rotates with uniform angular velocity Ω about the axis normal to the plates. The governing equations are solved by perturbation technique to obtain the analytical results for velocity, temperature, and concentration fields and shear stresses. The steady and unsteady resultant velocities along with the phase differences for various values of physical parameters are discussed in detail. The effects of rotation, buoyancy force, magnetic field, thermal radiation, and heat generation parameters on resultant velocity, temperature, and concentration fields are analyzed.

  3. Influence of fluctuating thermal and mass diffusion on unsteady MHD buoyancy-driven convection past a vertical surface with chemical reaction and Soret effects

    Science.gov (United States)

    Pal, Dulal; Talukdar, Babulal

    2012-04-01

    The influence of thermal radiation and first-order chemical reaction on unsteady MHD convective flow, heat and mass transfer of a viscous incompressible electrically conducting fluid past a semi-infinite vertical flat plate in the presence of transverse magnetic field under oscillatory suction and heat source in slip-flow regime is studied. The dimensionless governing equations for this investigation are formulated and solved analytically using two-term harmonic and non-harmonic functions. Comparisons with previously published work on special cases of the problem are performed and results are found to be in excellent agreement. A parametric study illustrating the effects of various physical parameters on the fluid velocity, temperature and concentration fields as well as skin-friction coefficient, the Nusselt and Sherwood numbers in terms of amplitude and phase is conducted. The numerical results of this parametric study are presented graphically and in tabular form to highlight the physical aspects of the problem.

  4. Perturbation technique for unsteady MHD mixed convection periodic flow, heat and mass transfer in micropolar fluid with chemical reaction in the presence of thermal radiation

    Science.gov (United States)

    Pal, Dulal; Talukdar, Babulal

    2012-10-01

    An analytical study is presented for the problem of unsteady hydromagnetic heat and mass transfer for a micropolar fluid bounded by semi-infinite vertical permeable plate in the presence of first-order chemical reaction, thermal radiation and heat absorption. A uniform magnetic field acts perpendicularly to the porous surface which absorbs the micropolar fluid with a time-dependent suction velocity. The basic partial differential equations are reduced to a system of nonlinear ordinary differential equations which are solved analytically using perturbation technique. Numerical calculations for the analytical expressions are carried out and the results are shown graphically. The effects of the various dimensionless parameters related to the problem on the velocity, angular velocity, temperature and concentration fields are discussed in detail.

  5. Determination of short-chain branching content in polyethylene by pyrolysis comprehensive multidimensional gas chromatography using low thermal mass column technology.

    Science.gov (United States)

    Eckerle, Patric; Pursch, Matthias; Cortes, Hernan J; Sun, Kefu; Winniford, Bill; Luong, Jim

    2008-10-01

    A research effort was undertaken to utilize the pyrolysis process to create fragments of polyethylene that could be indicative of branching, and allow quantitiation of said short-chain branches by pyrolysis comprehensive 2-D GC (Py-GC x GC). Several strategies for sample introduction and pyrolysis such as the in-column pyrolysis device and the programmed temperature vaporizer (PTV) were studied. The chromatographic separations were executed using low-thermal mass (LTM) comprehensive 2-D GC (GC x GC). A series of polyethylene-co-hexene samples were analyzed and a linear correlation of 1-hexene content with branching peak ratio was found. Correlation coefficients were determined as 0.97 for the measurements performed.

  6. An Investigation of the Complexity of Maillard Reaction Product Profiles from the Thermal Reaction of Amino Acids with Sucrose Using High Resolution Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Agnieszka Golon

    2014-08-01

    Full Text Available Thermal treatment of food changes its chemical composition drastically with the formation of “so-called” Maillard reaction products, being responsible for the sensory properties of food, along with detrimental and beneficial health effects. In this contribution, we will describe the reactivity of several amino acids, including arginine, lysine, aspartic acid, tyrosine, serine and cysteine, with carbohydrates. The analytical strategy employed involves high and ultra-high resolution mass spectrometry followed by chemometric-type data analysis. The different reactivity of amino acids towards carbohydrates has been observed with cysteine and serine, resulting in complex MS spectra with thousands of detectable reaction products. Several compounds have been tentatively identified, including caramelization reaction products, adducts of amino acids with carbohydrates, their dehydration and hydration products, disproportionation products and aromatic compounds based on molecular formula considerations.

  7. Double diffusive magnetohydrodynamic heat and mass transfer of nanofluids over a nonlinear stretching/shrinking sheet with viscous-Ohmic dissipation and thermal radiation

    Directory of Open Access Journals (Sweden)

    Dulal Pal

    2017-03-01

    Full Text Available The study of magnetohydrodynamic (MHD convective heat and mass transfer near a stagnation-point flow over stretching/shrinking sheet of nanofluids is presented in this paper by considering thermal radiation, Ohmic heating, viscous dissipation and heat source/sink parameter effects. Non-similarity method is adopted for the governing basic equations before they are solved numerically using Runge-Kutta-Fehlberg method using shooting technique. The numerical results are validated by comparing the present results with previously published results. The focus of this paper is to study the effects of some selected governing parameters such as Richardson number, radiation parameter, Schimdt number, Eckert number and magnetic parameter on velocity, temperature and concentration profiles as well as on skin-friction coefficient, local Nusselt number and Sherwood number.

  8. Velocity slip effects on heat and mass fluxes of MHD viscous–Ohmic dissipative flow over a stretching sheet with thermal radiation

    Directory of Open Access Journals (Sweden)

    M. Kayalvizhi

    2016-06-01

    Full Text Available In the present article, we discussed the velocity slip effects on the heat and mass fluxes of a viscous electrically conducting fluid flow over a stretching sheet in the presence of viscous dissipation, Ohmic dissipation and thermal radiation. A system of governing nonlinear PDEs is converted into a set of nonlinear ODEs by suitable similarity transformations. The numerical and analytical solutions are presented for the governing non-dimensional ODEs using shooting method and hypergeometric function respectively. The results are discussed for skin friction coefficient, concentration field, non-dimensional wall temperature and non-dimensional wall concentration. The non-dimensional wall concentration increases with slip and magnetic parameters and decreases with Schmidt number. Furthermore, comparisons are found to be good with bench mark solutions.

  9. Effects of Exothermic/Endothermic Chemical Reactions with Arrhenius Activation Energy on MHD Free Convection and Mass Transfer Flow in Presence of Thermal Radiation

    Directory of Open Access Journals (Sweden)

    Kh. Abdul Maleque

    2013-01-01

    Full Text Available A local similarity solution of unsteady MHD natural convection heat and mass transfer boundary layer flow past a flat porous plate within the presence of thermal radiation is investigated. The effects of exothermic and endothermic chemical reactions with Arrhenius activation energy on the velocity, temperature, and concentration are also studied in this paper. The governing partial differential equations are reduced to ordinary differential equations by introducing locally similarity transformation (Maleque (2010. Numerical solutions to the reduced nonlinear similarity equations are then obtained by adopting Runge-Kutta and shooting methods using the Nachtsheim-Swigert iteration technique. The results of the numerical solution are obtained for both steady and unsteady cases then presented graphically in the form of velocity, temperature, and concentration profiles. Comparison has been made for steady flow ( and shows excellent agreement with Bestman (1990, hence encouragement for the use of the present computations.

  10. An Investigation of the Complexity of Maillard Reaction Product Profiles from the Thermal Reaction of Amino Acids with Sucrose Using High Resolution Mass Spectrometry.

    Science.gov (United States)

    Golon, Agnieszka; Kropf, Christian; Vockenroth, Inga; Kuhnert, Nikolai

    2014-08-07

    Thermal treatment of food changes its chemical composition drastically with the formation of "so-called" Maillard reaction products, being responsible for the sensory properties of food, along with detrimental and beneficial health effects. In this contribution, we will describe the reactivity of several amino acids, including arginine, lysine, aspartic acid, tyrosine, serine and cysteine, with carbohydrates. The analytical strategy employed involves high and ultra-high resolution mass spectrometry followed by chemometric-type data analysis. The different reactivity of amino acids towards carbohydrates has been observed with cysteine and serine, resulting in complex MS spectra with thousands of detectable reaction products. Several compounds have been tentatively identified, including caramelization reaction products, adducts of amino acids with carbohydrates, their dehydration and hydration products, disproportionation products and aromatic compounds based on molecular formula considerations.

  11. Ion chromatography electrospray ionization mass spectrometry method development and investigation of lithium hexafluorophosphate-based organic electrolytes and their thermal decomposition products.

    Science.gov (United States)

    Kraft, Vadim; Grützke, Martin; Weber, Waldemar; Winter, Martin; Nowak, Sascha

    2014-08-08

    A method based on the coupling of ion chromatography (IC) and electrospray ionization mass spectrometry (ESI-MS) for the separation and determination of thermal decomposition products of LiPF6-based organic electrolytes is presented. The utilized electrolytes, LP30 and LP50, are commercially available and consist of 1mol/l LiPF6 dissolved in ethylene carbonate/dimethyl carbonate and ethylene carbonate/ethyl methyl carbonate, respectively. For the separation method development three ion chromatographic columns with different capacity and stationary phase were used and compared. Besides the known hydrolysis products of lithium hexafluorophosphate, several new organophosphates were separated and identified with the developed IC-ESI-MS method during aging investigations of the electrolytes. The chemical structures were elucidated with IC-ESI-MS/MS. Copyright © 2014 Elsevier B.V. All rights reserved.

  12. 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....

  13. Born total ionisation cross sections: An algebraic computing program using Maple

    Science.gov (United States)

    Bartlett, Philip L.; Stelbovics, Andris T.

    2003-08-01

    The software described in this paper uses the Maple algebraic computing environment to calculate an analytic form for the matrix element of the plane-wave Born approximation of the electron-impact ionisation of an atomic orbital, with arbitrary orbital and angular momentum quantum numbers. The atomic orbitals are approximated by Hartree-Fock Slater functions, and the ejected electron is modelled by a hydrogenic Coulomb wave, made orthogonal to all occupied orbitals of the target atom. Clenshaw-Curtis integration techniques are then used to calculate the total ionisation cross-section. For improved performance, the numerical integrations are performed using FORTRAN by automatically converting the analytic matrix element for each orbital into a FORTRAN subroutine. The results compare favourably with experimental data for a wide range of elements, including the transition metals, with excellent convergence at high energies. Program summaryTitle of program: BIX Catalogue identifier:ADRZ Program summary URL:http://www.cpc.cs.qub.ac.uk/cpc/summaries/ADRZ Program obtainable from:CPC Program Library, Queen's University of Belfast, N. Ireland Computers: Platform independent Operating systems: Tested on DEC Alpha Unix, Windows NT 4.0 and Windows XP Professional Edition Programming language used: Maple V Release 5.1 and FORTRAN 90 Memory required: 256 MB No. of processors used: 1 No. of bytes in distributed program, including test data, etc.:61754 Distributed format:tar gzip file Keywords: Born approximation, electron-impact ionisation cross-section, Maple, Hartree-Fock Nature of physical problem: Calculates the total electron impact ionisation cross-section for neutral and ionised atomic species using the first-Born approximation. The scattered electron is modelled by a plane wave, and the ejected electron is modelled by a hydrogenic Coulomb wave, which is made orthogonal to all occupied atomic orbitals, and the atomic orbitals are approximated by Hartree-Fock Slater

  14. An initial study on modeling the global thermal and fast reactor fuel cycle mass flow using Vensim

    Energy Technology Data Exchange (ETDEWEB)

    Brinton, Samuel [Kansas State University, Mechanical Engineering, Manhattan, KS 66506 (United States)

    2008-07-01

    This study concentrated on modeling the construction and decommissioning rates of five major facilities comprising the nuclear fuel cycle: (1) current LWRs with a 60-year service life, (2) new LWRs burning MOX fuel, (3) new LWRs to replace units in the current fleet, (4) new FRs to be added to the fleet, and (5) new spent fuel reprocessing facilities. This is a mass flow mode starting from uranium ore and following it to spent forms. The visual dynamic modeling program Vensim was used to create a system of equations and variables to track the mass flows from enrichment, fabrication, burn-up, and the back-end of the fuel cycle. The scenarios considered provide estimates of the uranium ore requirements, quantities of LLW and HLW production, and the number of reprocessing facilities necessary to reduce recently reported levels of spent fuel inventory. Preliminary results indicate that the entire national spent fuel inventory produced in the next 100 years can be reprocessed with a reprocessing plant built every 11 years (small capacity) or even as low as every 23 years (large capacity). (authors)

  15. Modelling the water mass circulation in the Aegean Sea. Part I: wind stresses, thermal and haline fluxes

    Directory of Open Access Journals (Sweden)

    I. A. Valioulis

    Full Text Available The aim of this work is to develop a computer model capable of simulating the water mass circulation in the Aegean Sea. There is historical, phenomenological and recent experimental evidence of important hydrographical features whose causes have been variably identified as the highly complex bathymetry, the extreme seasonal variations in temperature, the considerable fresh water fluxes, and the large gradients in salinity or temperature across neighbouring water masses (Black Sea and Eastern Mediterranean. In the approach taken here, physical processes are introduced into the model one by one. This method reveals the parameters responsible for permanent and seasonal features of the Aegean Sea circulation. In the first part of the work reported herein, wind-induced circulation appears to be seasonally invariant. This yearly pattern is overcome by the inclusion of baroclinicity in the model in the form of surface thermohaline fluxes. The model shows an intricate pattern of sub-basin gyres and locally strong currents, permanent or seasonal, in accord with the experimental evidence.

  16. Modelling the water mass circulation in the Aegean Sea. Part I: wind stresses, thermal and haline fluxes

    Directory of Open Access Journals (Sweden)

    I. A. Valioulis

    1994-07-01

    Full Text Available The aim of this work is to develop a computer model capable of simulating the water mass circulation in the Aegean Sea. There is historical, phenomenological and recent experimental evidence of important hydrographical features whose causes have been variably identified as the highly complex bathymetry, the extreme seasonal variations in temperature, the considerable fresh water fluxes, and the large gradients in salinity or temperature across neighbouring water masses (Black Sea and Eastern Mediterranean. In the approach taken here, physical processes are introduced into the model one by one. This method reveals the parameters responsible for permanent and seasonal features of the Aegean Sea circulation. In the first part of the work reported herein, wind-induced circulation appears to be seasonally invariant. This yearly pattern is overcome by the inclusion of baroclinicity in the model in the form of surface thermohaline fluxes. The model shows an intricate pattern of sub-basin gyres and locally strong currents, permanent or seasonal, in accord with the experimental evidence.

  17. High resolution mass spectrometry in the identification of transformation products and metabolites from β-lactam antibiotics in thermally treated milk.

    Science.gov (United States)

    Junza, A; Montané, A; Barbosa, J; Minguillón, C; Barrón, D

    2014-11-14

    Antibiotics such as β-lactam derivatives (penicillins and cephalosporins) are frequently used in veterinary medicine. The presence of these antibiotics together with their metabolites and/or products produced in subsequent treatments at which milk is submitted (sterilization, pasteurization), may be responsible for bacterial resistance, allergy and/or toxicity on sensitive individuals. In this study, liquid chromatography coupled with high resolution mass spectrometry (LC-HRMS) is used to identify transformation products (TPs) from four β-lactam antibiotics (amoxicillin (AMOX), cephapirin (PIR), ceftiofur (TIO) and penicillin G (PENG)) in thermally treated cow milk. In addition, milk from cows medicated with PENG has also been analogously treated and studied. The detected TPs come mainly from hydrolysis and decarboxylation reactions. Products more strongly degraded respect to parent compounds (of lower molecular weight) were obtained after treating milk at higher temperatures. Products identified in milk from cows medicated with PENG have been classified as TPs when coming from chemical/thermal degradation, and metabolites when resulting from the biological drug metabolism. While TPs are the result of hydrolysis and decarboxylation processes, as already indicated, an enzymatic conjugation with amino acids is suggested to be involved in the formation of metabolites. Copyright © 2014 Elsevier B.V. All rights reserved.

  18. Thermal discomfort with cold extremities in relation to age, gender, and body mass index in a random sample of a Swiss urban population

    Directory of Open Access Journals (Sweden)

    Orgül Selim

    2010-06-01

    Full Text Available Abstract Background The aim of this epidemiological study was to investigate the relationship of thermal discomfort with cold extremities (TDCE to age, gender, and body mass index (BMI in a Swiss urban population. Methods In a random population sample of Basel city, 2,800 subjects aged 20-40 years were asked to complete a questionnaire evaluating the extent of cold extremities. Values of cold extremities were based on questionnaire-derived scores. The correlation of age, gender, and BMI to TDCE was analyzed using multiple regression analysis. Results A total of 1,001 women (72.3% response rate and 809 men (60% response rate returned a completed questionnaire. Statistical analyses revealed the following findings: Younger subjects suffered more intensely from cold extremities than the elderly, and women suffered more than men (particularly younger women. Slimmer subjects suffered significantly more often from cold extremities than subjects with higher BMIs. Conclusions Thermal discomfort with cold extremities (a relevant symptom of primary vascular dysregulation occurs at highest intensity in younger, slimmer women and at lowest intensity in elderly, stouter men.

  19. Determination of short chain chlorinated paraffins in water by stir bar sorptive extraction-thermal desorption-gas chromatography-triple quadrupole tandem mass spectrometry.

    Science.gov (United States)

    Tölgyessy, P; Nagyová, S; Sládkovičová, M

    2017-04-21

    A simple, robust, sensitive and environment friendly method for the determination of short chain chlorinated paraffins (SCCPs) in water using stir bar sorptive extraction (SBSE) coupled to thermal desorption-gas chromatography-triple quadrupole tandem mass spectrometry (TD-GC-QqQ-MS/MS) was developed. SBSE was performed using 100mL of water sample, 20mL of methanol as a modifier, and a commercial sorptive stir bar (with 10mm×0.5mm PDMS layer) during extraction period of 16h. After extraction, the sorptive stir bar was thermally desorbed and online analysed by GC-MS/MS. Method performance was evaluated for MilliQ and surface water spiked samples. For both types of matrices, a linear dynamic range of 0.5-3.0μgL -1 with correlation coefficients >0.999 and relative standard deviations (RSDs) of the relative response factors (RRFs) <12% was established. The limits of quantification (LOQs) of 0.06 and 0.08μgL -1 , and the precision (repeatability) of 6.4 and 7.7% (RSDs) were achieved for MilliQ and surface water, respectively. The method also showed good robustness, recovery and accuracy. The obtained performance characteristics indicate that the method is suitable for screening and monitoring and compliance checking with environmental quality standards (EQS, set by the EU) for SCCPs in surface waters. Copyright © 2017 Elsevier B.V. All rights reserved.

  20. Thermal radiation effects on magnetohydrodynamic free convection heat and mass transfer from a sphere in a variable porosity regime

    KAUST Repository

    Prasad, Vallampati Ramachandra Ramachandra

    2012-02-01

    A mathematical model is presented for multiphysical transport of an optically-dense, electrically-conducting fluid along a permeable isothermal sphere embedded in a variable-porosity medium. A constant, static, magnetic field is applied transverse to the cylinder surface. The non-Darcy effects are simulated via second order Forchheimer drag force term in the momentum boundary layer equation. The surface of the sphere is maintained at a constant temperature and concentration and is permeable, i.e. transpiration into and from the boundary layer regime is possible. The boundary layer conservation equations, which are parabolic in nature, are normalized into non-similar form and then solved numerically with the well-tested, efficient, implicit, stable Keller-box finite difference scheme. Increasing porosity (ε) is found to elevate velocities, i.e. accelerate the flow but decrease temperatures, i.e. cool the boundary layer regime. Increasing Forchheimer inertial drag parameter (Λ) retards the flow considerably but enhances temperatures. Increasing Darcy number accelerates the flow due to a corresponding rise in permeability of the regime and concomitant decrease in Darcian impedance. Thermal radiation is seen to reduce both velocity and temperature in the boundary layer. Local Nusselt number is also found to be enhanced with increasing both porosity and radiation parameters. © 2011 Elsevier B.V.

  1. A comparative STM study of Ru nanoparticles deposited on HOPG by mass-selected gas aggregation versus thermal evaporation

    DEFF Research Database (Denmark)

    Nielsen, Rasmus Munksgård; Murphy, Shane; Strebel, Christian Ejersbo

    2009-01-01

    Scanning tunneling microscopy was used to compare the morphologies of Ru nanoparticles deposited onto highly-oriented graphite surfaces using two different physical vapour deposition methods; (1) pre-formed mass-selected Ru nanoparticles with diameters between 2 nm and 15 nm were soft-landed onto...... HOPG surfaces using a gas-aggregation source and (2) nanoparticles were formed by e-beam evaporation of Ru films onto HOPG. The particles generated by the gas-aggregation source are round in shape with evidence of facets resolved on the larger particles. Annealing these nanoparticles when...... they are supported on unsputtered HOPG resulted in the sintering of smaller nanoparticles, while larger particles remained immobile. Nanoparticles deposited onto sputtered HOPG surfaces were found to be stable against sintering when annealed. The size and shape of nanoparticles deposited by e-beam evaporation depend...

  2. A novel aerosol mass spectrometric approach - Analysis of the organic molecular signature of PM by coupling of thermal EC/OC-carbon analysis to photo-ionization mass spectrometry

    Science.gov (United States)

    Zimmermann, R.; Grabowski, J.; Streibel, T.; Sklorz, M.; Chow, J.

    2012-12-01

    Carbonaceous material in airborne particulate matter (PM) is of increasing interest e.g. due to its adverse health effects and its potential influence on the climate. Its analytical assessment on a molecular level is still very challenging. Hence, analysis of carbonaceous fractions for many studies is often solely carried out by determining sum parameters such as the overall content of organic carbon (OC) and elemental carbon (EC) as well as the total carbon content, TC (sum of OC and EC). The used thermal procedure, however, allows getting additional interesting information: By defining different thermal OC fractions (i.e. temperature steps) also information on the refractory properties of the carbonaceous material is obtained. In this context it is particularly interesting to investigate the release and formation behaviors of the molecular species responsible for the different OC and EC fractions. Thus after initial promising results of pre-studies [1,2] in the current work an EC/OC carbon analyzer (Model DRI 2000) and a homebuilt photo-ionization time-of-flight mass spectrometer (PI-TOFMS) were hyphenated and applied to investigate individual organic compounds especially from the different OC fractions. The carbon analyzer enables the stepwise heating of PM loaded filter samples and provides the sum values of the "carbon" release ("Improve protocol" [2]: OC1 - 120 °C, OC2 - 250°C, OC3 - 450°C OC4 - 550°C). With the on-line coupled PI-TOFMS evolved organic compounds, as released during the thermal program, are detectable in real time. This is possible by MS with soft photo ionization methods (SPI - single photon ionization and REMPI - resonance-enhanced multi photon ionization). Soft ionization suppresses fragmentation upon the ionization step and generates molecular signatures in the MS. The EC/OC-analyzer-PI-TOFMS instrument was applied to several types of PM samples, such as ambient aerosol, emission samples (gasoline/diesel car, wood combustion) or

  3. Characterization of volatile organic compounds from human analogue decomposition using thermal desorption coupled to comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry.

    Science.gov (United States)

    Stadler, Sonja; Stefanuto, Pierre-Hugues; Brokl, Michał; Forbes, Shari L; Focant, Jean-François

    2013-01-15

    Complex processes of decomposition produce a variety of chemicals as soft tissues, and their component parts are broken down. Among others, these decomposition byproducts include volatile organic compounds (VOCs) responsible for the odor of decomposition. Human remains detection (HRD) canines utilize this odor signature to locate human remains during police investigations and recovery missions in the event of a mass disaster. Currently, it is unknown what compounds or combinations of compounds are recognized by the HRD canines. Furthermore, a comprehensive decomposition VOC profile remains elusive. This is likely due to difficulties associated with the nontarget analysis of complex samples. In this study, cadaveric VOCs were collected from the decomposition headspace of pig carcasses and were further analyzed using thermal desorption coupled to comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (TD-GC × GC-TOFMS). Along with an advanced data handling methodology, this approach allowed for enhanced characterization of these complex samples. The additional peak capacity of GC × GC, the spectral deconvolution algorithms applied to unskewed mass spectral data, and the use of a robust data mining strategy generated a characteristic profile of decomposition VOCs across the various stages of soft-tissue decomposition. The profile was comprised of numerous chemical families, particularly alcohols, carboxylic acids, aromatics, and sulfides. Characteristic compounds identified in this study, e.g., 1-butanol, 1-octen-3-ol, 2-and 3-methyl butanoic acid, hexanoic acid, octanal, indole, phenol, benzaldehyde, dimethyl disulfide, and trisulfide, are potential target compounds of decomposition odor. This approach will facilitate the comparison of complex odor profiles and produce a comprehensive VOC profile for decomposition.

  4. Monte Carlo configuration interaction applied to multipole moments, ionisation energies and electron affinities.

    Science.gov (United States)

    Coe, Jeremy P; Taylor, Daniel J; Paterson, Martin J

    2013-05-15

    The method of Monte Carlo configuration interaction (MCCI) (Greer, J. Chem. Phys. 1995a, 103, 1821; Tong, Nolan, Cheng, and Greer, Comp. Phys. Comm. 2000, 142, 132) is applied to the calculation of multipole moments. We look at the ground and excited state dipole moments in carbon monoxide. We then consider the dipole of NO, the quadrupole of N2 and of BH. An octupole of methane is also calculated. We consider experimental geometries and also stretched bonds. We show that these nonvariational quantities may be found to relatively good accuracy when compared with full configuration interaction results, yet using only a small fraction of the full configuration interaction space. MCCI results in the aug-cc-pVDZ basis are seen to generally have reasonably good agreement with experiment. We also investigate the performance of MCCI when applied to ionisation energies and electron affinities of atoms in an aug-cc-pVQZ basis. We compare the MCCI results with full configuration interaction quantum Monte Carlo (Booth and Alavi, J. Chem. Phys. 2010, 132, 174104; Cleland, Booth, and Alavi, J. Chem. Phys. 2011, 134, 024112) and "exact" nonrelativistic results (Booth and Alavi, J. Chem. Phys. 2010, 132, 174104; Cleland, Booth, and Alavi, J. Chem. Phys. 2011, 134, 024112). We show that MCCI could be a useful alternative for the calculation of atomic ionisation energies however electron affinities appear much more challenging for MCCI. Due to the small magnitude of the electron affinities their percentage errors can be high, but with regards to absolute errors MCCI performs similarly for ionisation energies and electron affinities. Copyright © 2013 Wiley Periodicals, Inc.

  5. Dissipative instabilities in a partially ionised prominence plasma slab. II. The effect of compressibility

    Science.gov (United States)

    Mather, J. F.; Ballai, I.; Erdélyi, R.

    2018-02-01

    This study deals with the dissipative instability that appears in a compressible partially ionised plasma slab embedded in a uniform magnetic field, modelling the state of the plasma in solar prominences. In the partially ionised plasma, the dominant dissipative effect is the Cowling resistivity. The regions outside the slab (modelling the solar corona) are fully ionised, and the dominant mechanism of dissipation is viscosity. Analytical solutions to the extended magnetohydrodynamic (MHD) equations are found inside and outside of the slab and solutions are matched at the boundaries of the slab. The dispersion relation is derived and solutions are found analytically in the slender slab limit, while the conditions necessary for the appearance of the instability is investigated numerically for the entire parameter space. Our study is focussed on the effect of the compressibility on the generation and evolution of instabilities. We find that compressibility reduces the threshold of the equilibrium flow, where waves can be unstable, to a level that is comparable to the internal cusp speed, which is of the same order of flow speeds that are currently observed in solar prominences. Our study addresses only the slow waves, as these are the most likely perturbations to become unstable, however the time-scales of the instability are found to be rather large ranging from 105-107 s. It is determined that the instability threshold is further influenced by the concentration of neutrals and the strength of the viscosity of the corona. Interestingly, these two latter aspects have opposite effects. Our numerical analysis shows that the interplay between the equilibrium flow, neutrals and dispersion can change considerably the nature of waves. Despite employing a simple model, our study confirms the necessity of consideration of neutrals when discussing the stability of prominences under solar conditions.

  6. Comparison of low and high dose ionising radiation using topological analysis of gene coexpression networks

    Directory of Open Access Journals (Sweden)

    Ray Monika

    2012-05-01

    Full Text Available Abstract Background The growing use of imaging procedures in medicine has raised concerns about exposure to low-dose ionising radiation (LDIR. While the disastrous effects of high dose ionising radiation (HDIR is well documented, the detrimental effects of LDIR is not well understood and has been a topic of much debate. Since little is known about the effects of LDIR, various kinds of wet-lab and computational analyses are required to advance knowledge in this domain. In this paper we carry out an “upside-down pyramid” form of systems biology analysis of microarray data. We characterised the global genomic response following 10 cGy (low dose and 100 cGy (high dose doses of X-ray ionising radiation at four time points by analysing the topology of gene coexpression networks. This study includes a rich experimental design and state-of-the-art computational systems biology methods of analysis to study the differences in the transcriptional response of skin cells exposed to low and high doses of radiation. Results Using this method we found important genes that have been linked to immune response, cell survival and apoptosis. Furthermore, we also were able to identify genes such as BRCA1, ABCA1, TNFRSF1B, MLLT11 that have been associated with various types of cancers. We were also able to detect many genes known to be associated with various medical conditions. Conclusions Our method of applying network topological differences can aid in identifying the differences among similar (eg: radiation effect yet very different biological conditions (eg: different dose and time to generate testable hypotheses. This is the first study where a network level analysis was performed across two different radiation doses at various time points, thereby illustrating changes in the cellular response over time.

  7. Skin dose measurements using radiochromic films, TLDS and ionisation chamber and comparison with Monte Carlo simulation.

    Science.gov (United States)

    Alashrah, Saleh; Kandaiya, Sivamany; Maalej, Nabil; El-Taher, A

    2014-12-01

    Estimation of the surface dose is very important for patients undergoing radiation therapy. The purpose of this study is to investigate the dose at the surface of a water phantom at a depth of 0.007 cm as recommended by the International Commission on Radiological Protection and International Commission on Radiation Units and Measurement with radiochromic films (RFs), thermoluminescent dosemeters and an ionisation chamber in a 6-MV photon beam. The results were compared with the theoretical calculation using Monte Carlo (MC) simulation software (MCNP5, BEAMnrc and DOSXYZnrc). The RF was calibrated by placing the films at a depth of maximum dose (d(max)) in a solid water phantom and exposing it to doses from 0 to 500 cGy. The films were scanned using a transmission high-resolution HP scanner. The optical density of the film was obtained from the red component of the RGB images using ImageJ software. The per cent surface dose (PSD) and percentage depth dose (PDD) curve were obtained by placing film pieces at the surface and at different depths in the solid water phantom. TLDs were placed at a depth of 10 cm in a solid water phantom for calibration. Then the TLDs were placed at different depths in the water phantom and were exposed to obtain the PDD. The obtained PSD and PDD values were compared with those obtained using a cylindrical ionisation chamber. The PSD was also determined using Monte Carlo simulation of a LINAC 6-MV photon beam. The extrapolation method was used to determine the PSD for all measurements. The PSD was 15.0±3.6% for RF. The TLD measurement of the PSD was 16.0±5.0%. The (0.6 cm(3)) cylindrical ionisation chamber measurement of the PSD was 50.0±3.0%. The theoretical calculation using MCNP5 and DOSXYZnrc yielded a PSD of 15.0±2.0% and 15.7±2.2%. In this study, good agreement between PSD measurements was observed using RF and TLDs with the Monte Carlo calculation. However, the cylindrical chamber measurement yielded an overestimate of the PSD

  8. Migration to new ampoule types for the NPL secondary standard ionisation chambers.

    Science.gov (United States)

    Baker, M; Fenwick, A; Ferreira, K; Keightley, J; Johansson, L; Collins, S

    2014-05-01

    As the pre-calibrated sample containers used for activity assay in the two NPL secondary standards ionisation chambers are being phased out, suitable replacements have been identified. Characterisation checks have been carried out on the new ISO ampoules and a long-term recalibration schedule has been devised. Around 40 calibration factors have been determined so far and comparison of ion chamber responses for the two ampoule types showed variations of up to 7% for low energy photon emitting radionuclides. © 2013 Published by Elsevier Ltd.

  9. First on-line results from the CRIS (Collinear Resonant Ionisation Spectroscopy) beam line at ISOLDE

    Energy Technology Data Exchange (ETDEWEB)

    Procter, T. J., E-mail: thomas.procter@postgrad.manchester.ac.uk; Flanagan, K. T. [University of Manchester (United Kingdom); Collaboration: CRIS Collaboration

    2013-04-15

    The CRIS (Collinear Resonant Ionisation Spectroscopy) experiment at the on-line isotope separator facility, ISOLDE, CERN, has been constructed for high-sensitivity laser spectroscopy measurements on radioactive isotopes. The technique determines the magnetic dipole and electric quadrupole moments, nuclear spin and changes in mean-square charge radii of exotic nuclei via measurement of their hyperfine structures and isotope shifts. In November 2011 the first on-line run was performed using the CRIS beam line, when the hyperfine structure of {sup 207}Fr was successfully measured. This paper will describe the technique and experimental setup of CRIS and present the results from the first on-line experiment.

  10. X-ray imaging of the ionisation cones in NGC 5252

    Science.gov (United States)

    Dadina, M.; Guainazzi, M.; Cappi, M.; Bianchi, S.; Vignali, C.; Malaguti, G.; Comastri, A.

    2010-06-01

    Context. The physical conditions of the gas forming the narrow-line regions (NLR) in active galactic nuclei (AGN) have been extensively studied in the optical band. Recently detailed X-ray studies have shown how the emission in the 0.1-2 keV band detected in Seyfert 2 galaxies is associated to gas lying close to or associated with the NLR. Aims: We take advantage of the spectacular extension (~15”) of the NLR in the type II Seyfert galaxy NGC 5252 and of the complementary characteristics of XMM-Newton and Chandra to investigate the physical conditions of the gas in this galaxy. Methods: The X-ray data from XMM-Newton are used to define the spectral properties of the ionising nuclear source. The Chandra data are used to trace the spatial characteristics of the soft X-ray emission. This information is then compared to the optical HST characteristics of the NLR in NGC 5252. Results: The X-ray spectrum of the nucleus of NGC 5252 is intrinsically flat (Γ~1.4-1.5) and absorbed by neutral gas with a column density NH~1022 cm-2. Below ~1 keV a soft excess is detected. The high-resolution spectrum obtained with the XMM-Newton RGS shows emission lines in the 0.2-1.5 keV range which strongly indicate that the soft X-ray component is essentially due to ionised gas. Moreover, the soft X-ray emission is spatially resolved around the nucleus and well overlaps the images obtained in narrow optical bands centred around the [Oiii] emission line at 5007 Å. The [Oiii]/soft-X flux ratios along the ionisation cones are basically constant. This indicates that the electron density does not significantly deviate from the r-2 law (constant ionisation parameter) moving outward from the nucleus. Conclusions: This result combined with previous optical studies suggests two plausible but different scenarios in the reconstruction of the last ~30 000 years of history of the central AGN. The most promising one is that the source is indeed a “quasar relic” with a steady and inefficient

  11. The potential use of diamond coated tungsten tips as a field ionisation source

    Energy Technology Data Exchange (ETDEWEB)

    Brown, A.; Prawer, S.; Legge, G.J.F.; Kostidis, L.I. [Melbourne Univ., Parkville, VIC (Australia). School of Physics

    1996-12-31

    Tungsten tips are convenient for use in a high brightness gaseous phase field ionisation source. However, the lifetime of these tips is not adequate for practical use. The authors are investigating whether coating tungsten tips with diamond using Chemical Vapor Deposition (CVD) will improve the practicality of using these tips by an improvement in longevity of the source and/or an improvement in brightness due to the effects of the property of negative electron affinity which has been observed on CVD diamond. 1 ref.

  12. Characterisation of the Muon Beams for the Muon Ionisation Cooling Experiment

    CERN Document Server

    Adams, D.; Alekou, A.; Apollonio, M.; Asfandiyarov, R.; Back, J.; Barber, G.; Barclay, P.; de Bari, A.; Bayes, R.; Bayliss, V.; Bertoni, R.; Blackmore, V.J.; Blondel, A.; Blot, S.; Bogomilov, M.; Bonesini, M.; Booth, C.N.; Bowring, D.; Boyd, S.; Bradshaw, T.W.; Bravar, U.; Bross, A.D.; Capponi, M.; Carlisle, T.; Cecchet, G.; Charnley, G.; Cobb, J.H.; Colling, D.; Collomb, N.; Coney, L.; Cooke, P.; Courthold, M.; Cremaldi, L.M.; DeMello, A.; Dick, A.; Dobbs, A.; Dornan, P.; Fayer, S.; Filthaut, F.; Fish, A.; Fitzpatrick, T.; Fletcher, R.; Forrest, D.; Francis, V.; Freemire, B.; Fry, L.; Gallagher, A.; Gamet, R.; Gourlay, S.; Grant, A.; Graulich, J.S.; Griffiths, S.; Hanlet, P.; Hansen, O.M.; Hanson, G.G.; Harrison, P.; Hart, T.L.; Hartnett, T.; Hayler, T.; Heidt, C.; Hills, M.; Hodgson, P.; Iaciofano, A.; Ishimoto, S.; Kafka, G.; Kaplan, D.M.; Karadzhov, Y.; Kim, Y.K.; Kolev, D.; Kuno, Y.; Kyberd, P.; Lau, W.; Leaver, J.; Leonova, M.; Li, D.; Lintern, A.; Littlefield, M.; Long, K.; Lucchini, G.; Luo, T.; Macwaters, C.; Martlew, B.; Martyniak, J.; Middleton, S.; Moretti, A.; Moss, A.; Muir, A.; Mullacrane, I.; Nebrensky, J.J.; Neuffer, D.; Nichols, A.; Nicholson, R.; Nugent, J.C.; Onel, Y.; Orestano, D.; Overton, E.; Owens, P.; Palladino, V.; Palmer, R.B.; Pasternak, J.; Pastore, F.; Pidcott, C.; Popovic, M.; Preece, R.; Prestemon, S.; Rajaram, D.; Ramberger, S.; Rayner, M.A.; Ricciardi, S.; Richards, A.; Roberts, T.J.; Robinson, M.; Rogers, C.; Ronald, K.; Rubinov, P.; Rucinski, R.; Rusinov, I.; Sakamoto, H.; Sanders, D.A.; Santos, E.; Savidge, T.; Smith, P.J.; Snopok, P.; Soler, F.J.P.; Stanley, T.; Summers, D.J.; Takahashi, M.; Tarrant, J.; Taylor, I.; Tortora, L.; Torun, Y.; Tsenov, R.; Tunnell, C.D.; Vankova, G.; Verguilov, V.; Virostek, S.; Vretenar, M.; Walaron, K.; Watson, S.; White, C.; Whyte, C.G.; Wilson, A.; Wisting, H.; Zisman, M.

    2013-01-01

    A novel single-particle technique to measure emittance has been developed and used to characterise seventeen different muon beams for the Muon Ionisation Cooling Experiment (MICE). The muon beams, whose mean momenta vary from 171 to 281 MeV/c, have emittances of approximately 1.5--2.3 \\pi mm-rad horizontally and 0.6--1.0 \\pi mm-rad vertically, a horizontal dispersion of 90--190 mm and momentum spreads of about 25 MeV/c. There is reasonable agreement between the measured parameters of the beams and the results of simulations. The beams are found to meet the requirements of MICE.

  13. Characterisation of the muon beams for the Muon Ionisation Cooling Experiment

    Energy Technology Data Exchange (ETDEWEB)

    Adams, D.; Barclay, P.; Bayliss, V.; Bradshaw, T.W.; Courthold, M.; Francis, V.; Fry, L.; Hayler, T.; Hills, M.; Lintern, A.; Macwaters, C.; Nichols, A.; Preece, R.; Ricciardi, S.; Rogers, C.; Stanley, T.; Tarrant, J.; Watson, S.; Wilson, A. [Harwell Oxford, STFC Rutherford Appleton Laboratory, Didcot (United Kingdom); Adey, D.; Back, J.; Boyd, S.; Harrison, P.; Pidcott, C.; Taylor, I. [University of Warwick, Department of Physics, Coventry (United Kingdom); Alekou, A.; Apollonio, M.; Barber, G.; Colling, D.; Dobbs, A.; Dornan, P.; Fayer, S.; Fish, A.; Hunt, C.; Leaver, J.; Long, K.; Martyniak, J.; Middleton, S.; Pasternak, J.; Richards, A.; Santos, E.; Savidge, T.; Takahashi, M. [Imperial College London, Department of Physics, Blackett Laboratory, London (United Kingdom); Asfandiyarov, R.; Blondel, A.; Graulich, J.S.; Karadzhov, Y.; Verguilov, V.; Wisting, H. [Universite de Geneve, DPNC, Section de Physique, Geneva (Switzerland); De Bari, A.; Cecchet, G. [Sezione INFN Pavia (Italy); Dipartimento di Fisica Nucleare e Teorica, Pavia (Italy); Bayes, R.; Forrest, D.; Nugent, J.C.; Soler, F.J.P.; Walaron, K. [The University of Glasgow, School of Physics and Astronomy, Glasgow (United Kingdom); Bertoni, R.; Bonesini, M.; Lucchini, G. [Sezione INFN Milano Bicocca (Italy); Dipartimento di Fisica G. Occhialini, Milano (Italy); Blackmore, V.J.; Carlisle, T.; Cobb, J.H.; Lau, W.; Rayner, M.A.; Tunnell, C.D. [University of Oxford, Department of Physics, Oxford (United Kingdom); Blot, S.; Kim, Y.K. [University of Chicago, Enrico Fermi Institute, Chicago, IL (United States); Bogomilov, M.; Kolev, D.; Rusinov, I.; Tsenov, R.; Vankova, G. [St. Kliment Ohridski University of Sofia, Department of Atomic Physics, Sofia (Bulgaria); Booth, C.N.; Hodgson, P.; Nicholson, R.; Overton, E.; Robinson, M.; Smith, P.J. [University of Sheffield, Department of Physics and Astronomy, Sheffield (United Kingdom); Bowring, D.; DeMello, A.; Gourlay, S.; Li, D.; Prestemon, S.; Virostek, S.P.; Zisman, M.S. [Lawrence Berkeley National Laboratory, Berkeley, CA (United States); Bravar, U. [University of New Hampshire, Durham, NH (United States); Bross, A.D.; Fitzpatrick, T.; Leonova, M.; Moretti, A.; Neuffer, D.; Popovic, M.; Rubinov, P.; Rucinski, R. [Fermilab, Batavia, IL (United States); Capponi, M.; Iaciofano, A.; Orestano, D.; Pastore, F.; Tortora, L. [Sezione INFN Roma Tre e Dipartimento di Fisica, Roma (Italy); Charnley, G.; Collomb, N.; Gallagher, A.; Grant, A.; Griffiths, S.; Hartnett, T.; Martlew, B.; Moss, A.; Muir, A.; Mullacrane, I.; Owens, P.; White, C. [STFC Daresbury Laboratory, Cheshire (United Kingdom); Coney, L.; Fletcher, R.; Hanson, G.G.; Heidt, C. [University of California, Riverside, CA (United States); Cooke, P.; Gamet, R. [University of Liverpool, Department of Physics, Liverpool (United Kingdom); Cremaldi, L.M.; Hart, T.L.; Luo, T.; Sanders, D.A.; Summers, D.J. [University of Mississippi, Oxford, MS (United States); Dick, A.J.; Ronald, K.; Whyte, C.G. [University of Strathclyde, Department of Physics, Glasgow (United Kingdom); Filthaut, F. [NIKHEF, Amsterdam (Netherlands); Freemire, B.; Hanlet, P.; Kafka, G.; Kaplan, D.M.; Rajaram, D.; Snopok, P.; Torun, Y. [Illinois Institute of Technology, Chicago, IL (United States); Hansen, O.M.; Ramberger, S.; Vretenar, M. [CERN, Geneva (Switzerland); Ishimoto, S. [Institute of Particle and Nuclear Studies, High Energy Accelerator Research Organization (KEK), Tsukuba, Ibaraki (Japan); Kuno, Y.; Sakamoto, H. [Osaka University, Graduate School of Science, Department of Physics, Toyonaka, Osaka (Japan); Kyberd, P.; Littlefield, M.; Nebrensky, J.J. [Brunel University, Uxbridge (United Kingdom); Onel, Y. [University of Iowa, Department of Physics and Astronomy, Iowa City, IA (United States); Palladino, V. [Universita Federico II, Sezione INFN Napoli (Italy); Dipartimento di Fisica, Napoli (Italy); Palmer, R.B. [Brookhaven National Laboratory, Upton, NY (US); Roberts, T.J. [Muons, Inc., Batavia, IL (US); Collaboration: The MICE Collaboration

    2013-10-15

    A novel single-particle technique to measure emittance has been developed and used to characterise seventeen different muon beams for the Muon Ionisation Cooling Experiment (MICE). The muon beams, whose mean momenta vary from 171 to 281 MeV/c, have emittances of approximately 1.2-2.3 {pi} mm-rad horizontally and 0.6-1.0 {pi} mm-rad vertically, a horizontal dispersion of 90-190 mm and momentum spreads of about 25 MeV/c. There is reasonable agreement between the measured parameters of the beams and the results of simulations. The beams are found to meet the requirements of MICE. (orig.)

  14. Characterisation of the muon beams for the Muon Ionisation Cooling Experiment

    Energy Technology Data Exchange (ETDEWEB)

    Adams, D.; et al.,

    2013-10-01

    A novel single-particle technique to measure emittance has been developed and used to characterise seventeen different muon beams for the Muon Ionisation Cooling Experiment (MICE). The muon beams, whose mean momenta vary from 171 to 281 MeV/c, have emittances of approximately 1.5--2.3 \\pi mm-rad horizontally and 0.6--1.0 \\pi mm-rad vertically, a horizontal dispersion of 90--190 mm and momentum spreads of about 25 MeV/c. There is reasonable agreement between the measured parameters of the beams and the results of simulations. The beams are found to meet the requirements of MICE.

  15. The use of IR, magnetism, reflectance, and mass spectra together with thermal analyses in structure investigation of codeine phosphate complexes of d-block elements

    Science.gov (United States)

    Zayed, M. A.; El-shahat, M. F.; Abdullah, S. M.

    2005-06-01

    Codeine is an analgesic with uses similar to morphines, but it is of much less effect, i.e., it had a mild sedative effect; codeine is usually used as the phosphate form (Cod.P) and is often administrated by mouth with aspirin of paracetamol. Due to its serious use, if it is in large dose, attention is paid in this research to the synthesis and stereochemistry of new iron, cobalt, nickel, copper, and zinc complexes of this drug in both solution and the solid states. The spectra of these complexes in solution and the study of their stoichiometry refer to the formation of 1:1 ratio of metal (M) to ligand (L). The steriochemical structures of the solid complexes were studied on the basis of their analytical, spectroscopic, magnetic, and thermal data. Infrared spectra proved the presence of M sbnd O bonds. Magnetic susceptibility and solid reflectance spectral measurements were used to infer the structures. The prepared complexes were found to have the general formulae [ML(OH) x(H 2O) y](H 2O) zH 3PO 4, M: Co(II), Ni(II), and Cu(II), x = 1, y = 0, z = 0; M: Fe(II), x = 1, y = 2, z = 1; Fe(III), x = 2, y = 1, z = 0; Co(III), x = 0, y = 2, z = 1; Zn(II), x = 1, y = 0, z = 3; and L: (Cod.P) of the general formula C 18H 24NO 7P (anhydrate). Octahedral, tetrahedral, and square planer structures were proposed for these complexes depending upon the magnetic and reflectance data and were confirmed by detailed mass and thermal analyses comparative studies.

  16. Determination of Teucrium chamaedrys volatiles by using direct thermal desorption-comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry.

    Science.gov (United States)

    Ozel, Mustafa Z; Göğüş, Fahrettin; Lewis, Alastair C

    2006-05-05

    The direct qualification and quantification of the volatile components of Teucrium chamaedrys was studied using a direct thermal desorption (DTD) technique with comprehensive two-dimensional (2D) gas chromatography-time-of-flight mass spectrometry (GC x GC-TOF/MS). The GC x GC separation chromatographically resolved hundreds of components within this sample, and with the separation coupled with TOF/MS for detection, high probability identifications were made for 68 compounds. The quantitative results were determined through the use of internal standards and the desorption of differing amounts of raw material in the injector. The highest yield of volatile compounds (0.39%, w/w) was obtained at 150 degrees C thermal desorption temperature using 1.0mg of dried sample placed in a glass injector liner when studied over the range 1.0-7.0mg. Lowest yield of 0.33% (w/w) was found for the largest sample size of 7.0mg. Relative standard deviation (RSD) for 10 replicates at each size sample were in the range 3.9-21.6%. The major compounds identified were beta-pinene, germacrene D, alpha-pinene, alpha-farnesene, alpha-gurjunene, gamma-elemene and gamma-cadinene. All identified compounds were quantified using total ion chromatogram (TIC) peak areas. DTD is a promising method for quantitative analysis of complex mixtures, and in particular for quantitative analysis of plant samples, which can yield data without the traditional obligation for costly and time-consuming extraction techniques.

  17. Hydrophilic magnetic ionic liquid for magnetic headspace single-drop microextraction of chlorobenzenes prior to thermal desorption-gas chromatography-mass spectrometry.

    Science.gov (United States)

    Fernández, Elena; Vidal, Lorena; Canals, Antonio

    2017-11-23

    A new, fast, easy to handle, and environmentally friendly magnetic headspace single-drop microextraction (Mag-HS-SDME) based on a magnetic ionic liquid (MIL) as an extractant solvent is presented. A small drop of the MIL 1-ethyl-3-methylimidazolium tetraisothiocyanatocobaltate(II) ([Emim]2[Co(NCS)4]) is located on one end of a small neodymium magnet to extract nine chlorobenzenes (1,2-dichlorobenzene, 1,3-dichlorobenzene, 1,4-dichlorobenzene, 1,2,3-trichlorobenzene, 1,2,4-trichlorobenzene, 1,3,5-trichlorobenzene, 1,2,3,4-tetrachlorobenzene, 1,2,4,5-tetrachlorobenzene, and pentachlorobenzene) as model analytes from water samples prior to thermal desorption-gas chromatography-mass spectrometry determination. A multivariate optimization strategy was employed to optimize experimental parameters affecting Mag-HS-SDME. The method was evaluated under optimized extraction conditions (i.e., sample volume, 20 mL; MIL volume, 1 μL; extraction time, 10 min; stirring speed, 1500 rpm; and ionic strength, 15% NaCl (w/v)), obtaining a linear response from 0.05 to 5 μg L-1 for all analytes. The repeatability of the proposed method was evaluated at 0.7 and 3 μg L-1 spiking levels and coefficients of variation ranged between 3 and 18% (n = 3). Limits of detection were in the order of nanograms per liter ranging from 4 ng L-1 for 1,4-dichlorobenzene and 1,2,3,4-tetrachlorobenzene to 8 ng L-1 for 1,2,4,5-tetrachlorobenzene. Finally, tap water, pond water, and wastewater were selected as real water samples to assess the applicability of the method. Relative recoveries varied between 82 and 114% showing negligible matrix effects. Graphical abstract Magnetic headspace single-drop microextraction followed by thermal desorption-gas chromatography-mass spectrometry.

  18. Improved sample utilization in thermal ionization mass spectrometry isotope ratio measurements: refined development of porous ion emitters for nuclear forensic applications

    Energy Technology Data Exchange (ETDEWEB)

    Baruzzini, Matthew Louis [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

    2017-05-08

    The precise and accurate determination of isotopic composition in nuclear forensic samples is vital for assessing origin, intended use and process history. Thermal ionization mass spectrometry (TIMS) is widely accepted as the gold standard for high performance isotopic measurements and has long served as the workhorse in the isotopic ratio determination of nuclear materials. Nuclear forensic and safeguard specialists have relied heavily on such methods for both routine and atypical e orts. Despite widespread use, TIMS methods for the assay of actinide systems continue to be hindered by poor ionization e ciency, often less than tenths of a percent; the majority of a sample is not measured. This represents a growing challenge in addressing nextgeneration nuclear detection needs by limiting the ability to analyze ultratrace quantities of high priority elements that could potentially provide critical nuclear forensic signatures. Porous ion emitter (PIE) thermal ion sources were developed in response to the growing need for new TIMS ion source strategies for improved ionization e ciency, PIEs have proven to be simple to implement, straightforward approach to boosting ion yield. This work serves to expand the use of PIE techniques for the analysis of trace quantities of plutonium and americium. PIEs exhibited superior plutonium and americium ion yields when compared to direct lament loading and the resin bead technique, one of the most e cient methods for actinide analysis, at similar mass loading levels. Initial attempts at altering PIE composition for the analysis of plutonium proved to enhance sample utilization even further. Preliminary investigations of the instrumental fractionation behavior of plutonium and uranium analyzed via PIE methods were conducted. Data collected during these initial trial indicate that PIEs fractionate in a consistent, reproducible manner; a necessity for high precision isotope ratio measurements. Ultimately, PIEs methods were applied for

  19. A comparison using Faraday cups with 10(13) Ω amplifiers and a secondary electron multiplier to measure Os isotopes by negative thermal ionization mass spectrometry.

    Science.gov (United States)

    Wang, Guiqin; Sun, Tiantian; Xu, Jifeng

    2017-10-15

    According to the Johnson-Nyquist noise equation, the value of electron noise is proportional to the square root of the resistor value. This relationship gives a theoretical improvement of 100 in the signal/noise ratio by going from 10(11) Ω to 10(13) Ω amplifiers for Faraday detection in thermal ionization mass spectrometry (TIMS). We measured Os isotopes using static Faraday cups with 10(13) Ω amplifiers in negative thermal ionization mass spectrometry (NTIMS) and compared the results with those obtained with 10(11) Ω amplifiers and by peak-hopping on a single secondary electron multiplier (SEM). We analysed large loads of Os (1 μg) at a range of intensities of (187) OsO3 (0.02-10 mV) in addition to small loads of Os (5-500 pg) to compare the results of the three methods. Using 10(13) Ω amplifiers, the long-term reproducibility determined from Merck Os was (187) Os/(188) Os = 0.1211 ± 0.0086 and 0.120229 ± 0.000034 at 0.02 mV and 10 mV of (187) OsO3 intensities. Meanwhile, the analysed JMC Os loadings of 5 and 500 pg showed (187) Os/(188) Os = 0.10669 ± 0.00036 and 0.106807 ± 0.000023. In comparison, the values measured by the SEM were (187) Os/(188) Os = 0.10704 ± 0.00056 and 0.10690 ± 0.00013. All errors are in 2 standard deviation (SD). Both the accuracy and the precision determined using the 10(13) Ω amplifiers and the SEM are identical when the Os amounts are within 10-50 pg. However, the former analysis time can be shortened by approximately two-thirds. The SEM measurement is still the most precise method for Os amounts 50 pg. Copyright © 2017 John Wiley & Sons, Ltd.

  20. X-231A demonstration of in-situ remediation of DNAPL compounds in low permeability media by soil fracturing with thermally enhanced mass recovery or reactive barrier destruction

    Energy Technology Data Exchange (ETDEWEB)

    Siegrist, R.L. [Oak Ridge National Lab., TN (United States)]|[Colorado School of Mines, Golden, CO (United States). Environmental Science and Engineering Div.; Lowe, K.S. [Oak Ridge National Lab., Grand Junction, CO (United States). Life Sciences Div.; Murdoch, L.D. [FRx, Inc., Cincinnati, OH (United States)]|[Clemson Univ., SC (United States); Slack, W.W. [FRx, Inc., Cincinnati, OH (United States); Houk, T.C. [Lockheed Martin Energy Systems, Piketon, OH (United States)

    1998-03-01

    The overall goal of the program of activities is to demonstrate robust and cost-effective technologies for in situ remediation of DNAPL compounds in low permeability media (LPM), including adaptations and enhancements of conventional technologies to achieve improved performance for DNAPLs in LPM. The technologies sought should be potential for application at simple, small sites (e.g., gasoline underground storage tanks) as well as at complex, larger sites (e.g., DOE land treatment units). The technologies involved in the X-231A demonstration at Portsmouth Gaseous Diffusion Plant (PORTS) utilized subsurface manipulation of the LPM through soil fracturing with thermally enhanced mass recovery or horizontal barrier in place destruction. To enable field evaluation of these approaches, a set of four test cells was established at the X-231A land treatment unit at the DOE PORTS plant in August 1996 and a series of demonstration field activities occurred through December 1997. The principal objectives of the PORTS X-231A demonstration were to: determine and compare the operational features of hydraulic fractures as an enabling technology for steam and hot air enhanced soil vapor extraction and mass recovery, in situ interception and reductive destruction by zero valent iron, and in situ interception and oxidative destruction by potassium permanganate; determine the interaction of the delivered agents with the LPM matrix adjacent to the fracture and within the fractured zone and assess the beneficial modifications to the transport and/or reaction properties of the LPM deposit; and determine the remediation efficiency achieved by each of the technology strategies.

  1. Correlation of the ionisation response at selected points of IC sensitive regions with SEE sensitivity parameters under pulsed laser irradiation

    Energy Technology Data Exchange (ETDEWEB)

    Gordienko, A V; Mavritskii, O B; Egorov, A N; Pechenkin, A A; Savchenkov, D V [National Research Nuclear University ' ' MEPhI' ' (Russian Federation)

    2014-12-31

    The statistics of the ionisation response amplitude measured at selected points and their surroundings within sensitive regions of integrated circuits (ICs) under focused femtosecond laser irradiation is obtained for samples chosen from large batches of two types of ICs. A correlation between these data and the results of full-chip scanning is found for each type. The criteria for express validation of IC single-event effect (SEE) hardness based on ionisation response measurements at selected points are discussed. (laser applications and other topics in quantum electronics)

  2. On magnetospheric electron impact ionisation and dynamics in Titan's ram-side and polar ionosphere – a Cassini case study

    Directory of Open Access Journals (Sweden)

    K. Agren

    2007-11-01

    Full Text Available We present data from the sixth Cassini flyby of Titan (T5, showing that the magnetosphere of Saturn strongly interacts with the moon's ionosphere and exo-ionosphere. A simple electron ionisation model provides a reasonable agreement with the altitude structure of the ionosphere. Furthermore, we suggest that the dense and cold exo-ionosphere (from the exobase at 1430 km and outward to several Titan radii from the surface can be explained by magnetospheric forcing and other transport processes whereas exospheric ionisation by impacting low energy electrons seems to play a minor role.

  3. Serum ionised calcium and cardiovascular disease in 45-years old men and women followed for 18 years

    DEFF Research Database (Denmark)

    Ogard, Christina Gerlach; Petersen, Janne; Jørgensen, Torben

    2006-01-01

    a health survey in 1981 in Copenhagen had ionised serum calcium and different cardiovascular risk factors measured. The participants were followed until 1999 in The National Hospital Patients Registry and The National Death Registry in Denmark regarding the diagnosis ischemic heart disease (IHD......High level of total serum calcium within the normal range has been associated with increased cardiovascular risk. We wanted to evaluate whether the physiological active ionised form of calcium also was a risk factor for cardiovascular disease (CVD). Methods: A total of 974 participants from...

  4. An experimental and theoretical study of core-valence double ionisation of acetaldehyde (ethanal).

    Science.gov (United States)

    Zagorodskikh, S; Vapa, M; Vahtras, O; Zhaunerchyk, V; Mucke, M; Eland, J H D; Squibb, R J; Linusson, P; Jänkälä, K; Ågren, H; Feifel, R

    2016-01-28

    Core-valence double ionisation spectra of acetaldehyde (ethanal) are presented at photon energies above the carbon and oxygen 1s ionisation edges, measured by a versatile multi-electron coincidence spectroscopy technique. We use this molecule as a testbed for analyzing core-valence spectra by means of quantum chemical calculations of transition energies. These theoretical approaches range from two simple models, one based on orbital energies corrected by core valence interaction and one based on the equivalent core approximation, to a systematic series of quantum chemical electronic structure methods of increasing sophistication. The two simple models are found to provide a fast orbital interpretation of the spectra, in particular in the low energy parts, while the coverage of the full spectrum is best fulfilled by correlated models. CASPT2 is the most sophisticated model applied, but considering precision as well as computational costs, the single and double excitation configuration interaction model seems to provide the best option to analyze core-valence double hole spectra.

  5. A rapid ex vivo tissue model for optimising drug detection and ionisation in MALDI imaging studies.

    Science.gov (United States)

    Huber, K; Aichler, M; Sun, N; Buck, A; Li, Z; Fernandez, I E; Hauck, S M; Zitzelsberger, H; Eickelberg, O; Janssen, K P; Keller, U; Walch, A

    2014-10-01

    The aim of this study was to establish an ex vivo model for a faster optimisation of sample preparation procedures, for example matrix choice, in matrix-assisted laser desorption/ionisation (MALDI) drug imaging studies. The ionisation properties of four drugs, afatinib, erlotinib, irinotecan and pirfenidone, were determined in an ex vivo tissue experiment by spotting decreasing dilution series onto liver sections. Hereby, the drug signals were distinctly detectable using different matrix compounds, which allowed the selection of the optimal matrix for each drug. The analysis of afatinib and erlotinib yielded high drug signals with α-cyano-4-hydroxycinnamic acid matrix, whereas 2,3-dihydroxybenzoic acid was identified as optimal matrix for irinotecan and pirfenidone detection. Our method was validated by a MALDI drug imaging approach of in vivo treated mouse tissue resulting in corresponding findings, indicating the spotting method as an appropriate approach to determine the matrix of choice. The present study shows the accordance between the detection of ex vivo spotted drugs and in vivo administered drugs by MALDI-TOF and MALDI-FT-ICR imaging, which has not been demonstrated so far. Our data suggest the ex vivo tissue spotting method as an easy and reliable model to optimise MALDI imaging measurements and to predict drug detection in tissue sections derived from treated mice prior to the recruitment of laboratory animals, which helps to save animals, time and costs.

  6. Absorbed dose in ion beams: comparison of ionisation- and fluence-based measurements.

    Science.gov (United States)

    Osinga, Julia-Maria; Brons, Stephan; Bartz, James A; Akselrod, Mark S; Jäkel, Oliver; Greilich, Steffen

    2014-10-01

    A direct comparison measurement of fluorescent nuclear track detectors (FNTDs) and a thimble ionisation chamber is presented. Irradiations were performed using monoenergetic protons (142.66 MeV, ϕ=3×10(6) cm(-2)) and carbon ions (270.55 MeV u(-1), ϕ=3 × 10(6) cm(-2)). It was found that absorbed dose to water values as determined by fluence measurements using FNTDs are, in case of protons, in good agreement (2.4 %) with ionisation chamber measurements, if slower protons and Helium secondaries were accounted for by an effective stopping power. For carbon, however, a significant discrepancy of 4.5 % was seen, which could not be explained by fragmentation, uncertainties or experimental design. The results rather suggest a W-value of 32.10 eV ± 2.6 %. Additionally, the abundance of secondary protons expected from Monte-Carlo transport simulation was not observed. © The Author 2014. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  7. Gas chromatography with diode array detection in series with flame ionisation detection.

    Science.gov (United States)

    Gras, Ronda; Luong, Jim; Shellie, Robert A

    2017-06-02

    We introduce a gas chromatography detection approach that uses diode array detection operated in series with flame ionisation detection and demonstrate the utility of the detection approach for determination of volatile organic compounds. Diode array detection brings ultraviolet - visible spectroscopy (over a range of 190-640nm) onto the capillary gas chromatography time-scale, where average peak widths of analytes are on the order of 3-5s. The non-destructive nature of the diode array detector affords serially-coupled flame ionisation detection. This arrangement delivers near-simultaneous selective and universal detection without incurring additional analytical time, and without recourse to column flow splitting. The hyphenated technique is shown to be effective for chromatographic applications spanning an equivalent volatility range from C1 to C7n-paraffin hydrocarbons. The approach introduced herein provides increased sensitivity and selectivity for classes of compounds amenable to electronic spectroscopy such as alkenes, dienes, sulfurs, and aromatic compounds. The approach is demonstrated for direct measurement of carbon disulfide in work place atmospheres with a detection limit of 93pg on column and for the direct measurement of 1,3-butadiene in hydrocarbon matrices and ambient air with a detection of 73pg on column, each in less than 5min. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. Ionisation effects on the permeation of pharmaceutical compounds through silicone membrane.

    Science.gov (United States)

    Waters, L J; Bhuiyan, A K M M H

    2016-05-01

    Silicone membrane is frequently used as an in vitro skin mimic whereby experiments incorporate a range of buffered media which may vary in pH. As a consequence of such variability in pH there is a corresponding variability in the degree of ionisation which in turn, could influence permeation through the mainly hydrophobic-rich membrane structure. This study reports the effect of pH on the permeation of five model compounds (benzoic acid, benzotriazole, ibuprofen, ketoprofen and lidocaine). For the five compounds analysed, each at three distinct percentages of ionisation, it was found that the greater extent of permeation was always for the more 'neutral', i.e. more greatly unionised, species rather than the anionic or cationic species. These findings fit with the theory that the hydrophobic membrane encourages permeation of 'lipid-like' structures, i.e. the more unionised form of compounds. However, results obtained with an Inverse Gas Chromatography Surface Energy Analyser (iGC SEA) indicate the membrane surface to be an electron dense environment. In the knowledge that unionised forms of compounds permeate (rather than the charged species) this negatively charged surface was not anticipated, i.e. the basic membrane surface did not appear to affect permeation. Copyright © 2016 Elsevier B.V. All rights reserved.

  9. Kinematically complete study on electron impact ionisation of aligned hydrogen molecules

    Energy Technology Data Exchange (ETDEWEB)

    Senftleben, Arne

    2009-10-28

    Within the work presented here, single ionisation of spatially aligned hydrogen molecules by 200 eV electrons was studied in a kinematically complete experiment. For the first time, a comprehensive set of fully differential cross sections (FDCS) was obtained for this process on a molecular target. The direction of the internuclear axis was derived from the fragment emission of post-collision dissociation of the residual H{sub 2}{sup +} ion. Therefore, a protonic fragment was detected in coincidence with the two final-state electrons using a dedicated reaction microscope and sophisticated data analysis. For direct ionisation into the ionic ground state, existing theoretical cross sections for aligned molecules were tested. Additionally, we observed molecular frame angular distributions of Auger electrons emitted through dissociative autoionisation of H{sub 2}. Earlier findings of kinematically incomplete experiments were reproduced, but the FDCS reveal structures so far unknown. Furthermore, for random alignment, differential cross sections at two distinct values of the mean internuclear distance were obtained, providing new arguments in the current discussion on the nature of discrepancies observed between atomic and molecular collisions. (orig.)

  10. Modelling the propagation of effects of chronic exposure to ionising radiation from individuals to populations

    Energy Technology Data Exchange (ETDEWEB)

    Alonzo, F. [Laboratory of Environmental Modelling, DEI/SECRE/LME, Institute of Radioprotection and Nuclear Safety (IRSN), Cadarache, Building 159, BP3, 13115 St-Paul-lez-Durance Cedex (France); Laboratory of Radioecology and Ecotoxicology, DEI/SECRE/LRE, Institute of Radioprotection and Nuclear Safety (IRSN), Cadarache Building 186, BP3, 13115 St-Paul-lez-Durance Cedex (France)], E-mail: frederic.alonzo@irsn.fr; Hertel-Aas, T. [Department of Plant and Environmental Sciences, P.O. Box 5003, Norwegian University of Life Sciences, 1432 Aas (Norway); Gilek, M. [School of Life Sciences, Soedertoern University College, 14189 Huddinge (Sweden); Gilbin, R. [Laboratory of Radioecology and Ecotoxicology, DEI/SECRE/LRE, Institute of Radioprotection and Nuclear Safety (IRSN), Cadarache Building 186, BP3, 13115 St-Paul-lez-Durance Cedex (France); Oughton, D.H. [Department of Plant and Environmental Sciences, P.O. Box 5003, Norwegian University of Life Sciences, 1432 Aas (Norway); Garnier-Laplace, J. [Laboratory of Radioecology and Ecotoxicology, DEI/SECRE/LRE, Institute of Radioprotection and Nuclear Safety (IRSN), Cadarache Building 186, BP3, 13115 St-Paul-lez-Durance Cedex (France)

    2008-09-15

    This study evaluated the potential effect of ionising radiation on population growth using simple population models and parameter values derived from chronic exposure experiments in two invertebrate species with contrasting life-history strategies. In the earthworm Eisenia fetida, models predicted increasing delay in population growth with increasing gamma dose rate (up to 0.6 generation times at 11 mGy h{sup -1}). Population extinction was predicted at 43 mGy h{sup -1}. In the microcrustacean Daphnia magna, models predicted increasing delay in population growth with increasing alpha dose rate (up to 0.8 generation times at 15.0 mGy h{sup -1}), only after two successive generations were exposed. The study examined population effects of changes in different individual endpoints (including survival, number of offspring produced and time to first reproduction). Models showed that the two species did not respond equally to equivalent levels of change, the fast growing daphnids being more susceptible to reduction in fecundity or delay in reproduction than the slow growing earthworms. This suggested that susceptibility of a population to ionising radiation cannot be considered independent of the species' life history.

  11. Towards a Symmetric Momentum Distribution in the Muon Ionisation Cooling Experiment

    CERN Document Server

    Hansen, O M; Efthymiopoulos, I

    2013-01-01

    TheMuon Ionisation Cooling Experiment (MICE) is under development at Rutherford Appleton Labratory (UK). It is a proof-of-principle experiment for ionisation cooling, which is a prerequisite for a future Neutrino Factory (NF) or a Muon Collider. The muon beam will have a symmetrical momentum distribution in the cooling channel of theNF [1]. In the MICE beamline pions are captured by a quadrupole triplet, beam momentum is selected by dipole 1 (D1) before the beam traverses the decay solenoid. After the decay solenoid the beam momentum is selected by dipole 2 (D2), the beam is focused in two quadrupole triplets and characterised by time-of-flight (TOF) detectors TOF0 and TOF1 before entering the cooling channel. By doing a so-called D1-scan, where the optics parameters are scaled according to the upstream beam momentum, the purity and momentum distribution of the decay muons are changed. In this paper simulation results from G4Beamline (G4BL) [2] and data from MICE are presented and compared.

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

    Science.gov (United States)

    Kawaguchi, Migaku; Inoue, Koichi; Yoshimura, Mariko; Sakui, Norihiro; Okanouchi, Noriya; Ito, Rie; Yoshimura, Yoshihiro; Nakazawa, Hiroyuki

    2004-07-02

    A method for the simultaneous measurement of trace amounts of phenolic xenoestrogens, such as 2,4-dichlorophenol (2,4-DCP), 4-tert-butyl-phenol (BP), 4-tert-octylphenol (OP), 4-nonylphenol (NP), pentachlorophenol (PCP) and bisphenol A (BPA), in water samples was developed using stir bar sorptive extraction (SBSE) with in situ derivatization followed by thermal desorption (TD)-gas chromatography-mass spectrometry (GC-MS) analysis. The conditions for derivatization with acetic acid anhydride were investigated. A polydimethylsiloxane (PDMS)-coated stir bar and derivatization reagents were added to 10 ml of water sample and stirring was commenced for 10-180 min at room temperature (25 degrees C) in a headspace vial. Then, the extract was analyzed by TD-GC-MS. The optimum time for SBSE with in situ derivatization was 90 min. The detection limits of 2,4-DCP, BP, OP, NP, PCP and BPA were 2, 1, 0.5, 5, 2 and 2 pg ml(-1), respectively. The method showed good linearity over the concentration ranges of 10, 5, 2, 20, 10 and 10-1000 pg ml(-1) for 2,4-DCP, BP, OP, NP, PCP and BPA, respectively, and the correlation coefficients were higher than 0.99. The average recoveries of those compounds in river water samples were equal to or higher than 93.9% (R.S.D. river water samples.

  13. Emission mechanism of polyatomic ions Cs2Cl+ and Cs2BO2(+) in thermal ionization mass spectrometry with various carbon materials.

    Science.gov (United States)

    Wei, Hai-Zhen; Jiang, Shao-Yong; Hemming, Gary N; Yang, Jing-Hong; Xiao, Ying-Kai; Yang, Tao; Yan, Xiong; Yan, Yan

    2011-12-29

    The emission behavior of polyatomic ions Cs(2)Cl(+) and Cs(2)BO(2)(+) in the presence of various carbon materials (Graphite, Carbon, SWNTs, and Fullerenes) in the ionization source of thermal ionization mass spectrometry (TIMS) has been investigated. The emission capacity of various carbon materials are remarkably different as evidenced by the obvious discrepancy in signal intensity of polyatomic ions and accuracy/precision of boron and chlorine isotopic composition determined using Cs(2)Cl(+)-graphite-PTIMS/Cs(2)BO(2)(+)-graphite-PTIMS methods. Combined with morphology and microstructure properties of four selected carbon materials, it could be concluded that the emission behavior of the polyatomic ions strongly depends on the microstructure of the carbon materials used. A surface-induced collision mechanism for formation of such kinds of polyatomic ions in the ionization source of TIMS has been proposed based on the optimized configuration of Cs(2)BO(2)(+) and Cs(2)Cl(+) ions in the gas phase using a molecular dynamics method. The combination of the geometry of the selected carbon materials with the configuration of two polyatomic ions explains the structure effect of carbon materials on the emission behavior of polyatomic ions, where graphite samples with perfect parallels and equidistant layers ensure the capacity of emission to the maximum extent, and fullerenes worsen the emission of polyatomic ions by blocking their pathway. © 2011 American Chemical Society

  14. 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.

  15. Evaluation of three gas chromatography and two direct mass spectrometry techniques for aroma analysis of dried red bell peppers

    NARCIS (Netherlands)

    Ruth, van S.M.; Boscaini, E.; Mayr, D.; Pugh, J.; Posthumus, M.A.

    2003-01-01

    Three gas chromatography methods and two direct mass spectrometry techniques were compared for the analysis of the aroma of rehydrated diced red bell peppers. Gas chromatography methods included systems with olfactometry detection (GC-O), flame ionisation detection (GC-FID) and mass spectrometry

  16. Variety identification of wheat using mass spectrometry with neural networks and the influence of mass spectra processing prior to neural network analysis

    DEFF Research Database (Denmark)

    Sørensen, Helle Aagaard; Sperotto, Maria Maddalena; Petersen, M.

    2002-01-01

    The performance of matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry with neural networks in wheat variety classification is further evaluated.(1) Two principal issues were studied: (a) the number of varieties that could be classified correctly; and (b) various means...

  17. Study and optimization of the ionisation channel in the Edelweiss dark matter direct detection experiment; Etude et optimisation de la voie ionisation dans l'experience Edelweiss de detection directe de la matiere noire

    Energy Technology Data Exchange (ETDEWEB)

    Censier, B

    2006-02-15

    The EDELWEISS experiment is aiming at the detection of Weakly Interactive Massive Particles (WIMPs), today's most favoured candidates for solving the dark matter issue. Background ionising particles are identified thanks to the simultaneous measurement of heat and ionisation in the detectors. The main limitation to this method is coming from the ionisation measurement, charge collection being less efficient in some part of the detectors known as 'dead' areas. The specificity of the measurement is due to the use of very low temperatures and low collection fields. This thesis is dedicated to the study of carrier trapping. It involves time-resolved charge measurements as well as a simulation code adapted to the specific physical conditions. We first present results concerning charge trapping at the free surfaces of the detectors. Our method allows to build a surface-charge in a controlled manner by irradiation with a strong radioactive source. This charge is then characterised with a weaker source which acts as a probe. In a second part of the work, bulk-trapping characteristics are deduced from charge collection efficiency measurements, and by an original method based on event localisation in the detector. The results show that a large proportion of the doping impurities are ionised, as indicated independently by the study of degradation by space-charge build-up. In this last part, near-electrodes areas are found to contain large densities of charged trapping centres, in connection with dead-layer effects. (author)

  18. Ab Initio SCF MO Calculation of Ionisation Energies and Charge Distributions of TCNQ and Its Mono- and Divalent Anions

    NARCIS (Netherlands)

    Jonkman, H.T.; Velde, G.A. van der; Nieuwpoort, W.C.

    1974-01-01

    Ab initio SCF MO calculations using a contracted double zeta basis set of 168 gaussian type functions were performed on TCNQ+, TCNQ, TCNQ- and TCNQ2-. The ionisation potentials obtained from total energy differences are generally 0.25-0.50 eV higher than the corresponding negative orbital energies

  19. Time-dependent hydrogen ionisation in 3D simulations of the solar chromosphere. Methods and first results

    NARCIS (Netherlands)

    Leenaarts, J.; Wedemeyer-Bohm, S.

    2006-01-01

    Context. The hydrogen ionisation degree deviates substantially from statistical equilibrium under the conditions of the solar chromosphere. A realistic description of this atmospheric layer thus must account for time-dependent non-equilibrium effects. Aims. Advancing the realism of numerical

  20. Characterisation of exposure to non-ionising electromagnetic fields in the Spanish INMA birth cohort: Study protocol

    NARCIS (Netherlands)

    M. Gallastegi (Mara); M. Guxens Junyent (Mònica); A. Jiménez-Zabala (Ana); I. Calvente (Irene); M. Fernández (Marta); L. Birks (Laura); B. Struchen (Benjamin); M. Vrijheid (Martine); M. Estarlich (Marisa); M.F. Fernandez (Mariana); M. Torrent (Maties); F. Ballester (Ferran); J.J. Aurrekoetxea (Juan José); J. Ibarluzea (Jesús); D. Guerra (David); J. González (Julián); M. Röösli (Martin); L. Santa-Marina (Loreto)

    2016-01-01

    textabstractBackground: Analysis of the association between exposure to electromagnetic fields of non-ionising radiation (EMF-NIR) and health in children and adolescents is hindered by the limited availability of data, mainly due to the difficulties on the exposure assessment. This study protocol

  1. Brain Radiation Information Data Exchange (BRIDE): Integration of experimental data from low-dose ionising radiation research for pathway discovery

    NARCIS (Netherlands)

    C. Karapiperis (Christos); S.J. Kempf (Stefan J.); R. Quintens (Roel); O. Azimzadeh (Omid); V.L. Vidal (Victoria Linares); S. Pazzaglia; D. Bazyka (Dimitry); P.G. Mastroberardino (Pier); Z.G. Scouras (Zacharias G.); S. Tapio (Soile); M.A. Benotmane (Mohammed Abderrafi); C.A. Ouzounis (Christos A.)

    2016-01-01

    textabstractBackground: The underlying molecular processes representing stress responses to low-dose ionising radiation (LDIR) in mammals are just beginning to be understood. In particular, LDIR effects on the brain and their possible association with neurodegenerative disease are currently being

  2. Multidisciplinary approach to assess the sensitivity of dwarf tomato plants to low-LET ionising radiation

    Science.gov (United States)

    De Micco, Veronica; De Pascale, Stefania; Aronne, Giovanna; Paradiso, Roberta; Vitaglione, Paola; Turano, Mimmo; Arena, Carmen

    Ionising radiation, acting alone or in interaction with microgravity and other environmental constraints, may affect plant at molecular, morpho-structural and physiological level. The intensity of the plant’s response depends on the properties of radiation and on the features of the plant itself. Indeed, different species are characterised by different susceptibility to radiation which may change during the life course. The aim of this research was to study the radiosensitivity to low-LET ionising radiation of plants of dwarf tomato (Solanum lycopersicum L. ‘Microtom’) at two phenological phases (vegetative and reproductive), within the purpose of analysing plants for consideration as candidates for Bioregenerative Life Support Systems (BLSS) in Space. To pursue this objective, plants of the cultivar Microtom were irradiated with different doses of X-rays either at the stage of the second true leaf (VP - vegetative phase) or when at least one flower was blossomed (RP - reproductive phase). Plant’s response to ionising radiation was assessed through a multidisciplinary approach combining genetic analyses, ecophysiological measurements, morpho-anatomical characterisation of leaves and fruits, nutritional analyses of fruits. Growth, molecular and morpho-functional traits were measured during plant development up to fruiting in both VP and RP plant groups, and compared with non-irradiated control plants. Plant growth was monitored weekly recording parameters such as plant height, number of leaves, leaf area, flowering and fruiting rate. Potential DNA alterations were explored through Random Amplified Polymorphic DNA (RAPD) technique. The efficiency of the photosynthetic apparatus was evaluated by determining photosynthetic pigment composition, photochemistry and leaf gas exchanges. Leaf and fruit structure were analysed through light and epi-fluorescence microscopy. Leaf anatomical traits related to photosynthetic efficiency, and to structural radioprotection

  3. Ambient aging of rhenium filaments used in thermal ionization mass spectrometry: Growth of oxo-rhenium crystallites and anti-aging strategies

    Directory of Open Access Journals (Sweden)

    Joseph M. Mannion

    2017-01-01

    Full Text Available Degassing is a common preparation technique for rhenium filaments used for thermal ionization mass spectrometric analysis of actinides, including plutonium. Although optimization studies regarding degassing conditions have been reported, little work has been done to characterize filament aging after degassing. In this study, the effects of filament aging after degassing were explored to determine a “shelf-life” for degassed rhenium filaments, and methods to limit filament aging were investigated. Zone-refined rhenium filaments were degassed by resistance heating under high vacuum before exposure to ambient atmosphere for up to 2 months. After degassing the nucleation and preferential growth of oxo-rhenium crystallites on the surface of polycrystalline rhenium filaments was observed by atomic force microscopy and scanning electron microscopy (SEM. Compositional analysis of the crystallites was conducted using SEM-Raman spectroscopy and SEM energy dispersive X-ray spectroscopy, and grain orientation at the metal surface was investigated by electron back-scatter diffraction mapping. Spectra collected by SEM-Raman suggest crystallites are composed primarily of perrhenic acid. The relative extent of growth and crystallite morphology were found to be grain dependent and affected by the dissolution of carbon into filaments during annealing (often referred to as carbonization or carburization. Crystallites were observed to nucleate in region specific modes and grow over time through transfer of material from the surface. Factors most likely to affect the rates of crystallite growth include rhenium substrate properties such as grain size, orientation, levels of dissolved carbon, and relative abundance of defect sites; as well as environmental factors such as length of exposure to oxygen and relative humidity. Thin (∼180 nm hydrophobic films of poly(vinylbenzyl chloride were found to slow the growth of oxo-rhenium crystallites on the filament

  4. Electron and nuclear dynamics following ionisation of modified bismethylene-adamantane.

    Science.gov (United States)

    Vacher, Morgane; Albertani, Fabio E A; Jenkins, Andrew J; Polyak, Iakov; Bearpark, Michael J; Robb, Michael A

    2016-12-16

    We have simulated the coupled electron and nuclear dynamics using the Ehrenfest method upon valence ionisation of modified bismethylene-adamantane (BMA) molecules where there is an electron transfer between the two π bonds. We have shown that the nuclear motion significantly affects the electron dynamics after a few fs when the electronic states involved are close in energy. We have also demonstrated how the non-stationary electronic wave packet determines the nuclear motion, more precisely the asymmetric stretching of the two π bonds, illustrating "charge-directed reactivity". Taking into account the nuclear wave packet width results in the dephasing of electron dynamics with a half-life of 8 fs; this eventually leads to the equal delocalisation of the hole density over the two methylene groups and thus symmetric bond lengths.

  5. Electrifying atmospheres charging, ionisation and lightning in the solar system and beyond

    CERN Document Server

    Aplin, Karen L

    2013-01-01

    Electrical processes take place in all planetary atmospheres. There is evidence for lightning on Venus, Jupiter, Saturn, Uranus and Neptune, it is possible on Mars and Titan, and cosmic rays ionise every atmosphere, leading to charged droplets and particles. Controversy surrounds the role of atmospheric electricity in physical climate processes on Earth; here, a comparative approach is employed to review the role of electrification in the atmospheres of other planets and their moons. This book reviews the theory, and, where available, measurements, of planetary atmospheric electricity, taken to include ion production and ion-aerosol interactions. The conditions necessary for a global atmospheric electric circuit similar to Earth’s, and the likelihood of meeting these conditions in other planetary atmospheres, are briefly discussed. Atmospheric electrification is more important at planets receiving little solar radiation, increasing the relative significance of electrical forces. Nucleation onto atmospheric ...

  6. Revisiting Bragg's X-ray microscope: scatter based optical transient grating detection of pulsed ionising radiation.

    Science.gov (United States)

    Fullagar, Wilfred K; Paganin, David M; Hall, Chris J

    2011-06-01

    Transient optical gratings for detecting ultrafast signals are routine for temporally resolved photochemical investigations. Many processes can contribute to the formation of such gratings; we indicate use of optically scattering centres that can be formed with highly variable latencies in different materials and devices using ionising radiation. Coherent light scattered by these centres can form the short-wavelength-to-optical-wavelength, incoherent-to-coherent basis of a Bragg X-ray microscope, with inherent scope for optical phasing. Depending on the dynamics of the medium chosen, the way is open to both ultrafast pulsed and integrating measurements. For experiments employing brief pulses, we discuss high-dynamic-range short-wavelength diffraction measurements with real-time optical reconstructions. Applications to optical real-time X-ray phase-retrieval are considered. Copyright © 2010 Elsevier B.V. All rights reserved.

  7. Non-targeted effects of ionising radiation—Implications for low dose risk

    DEFF Research Database (Denmark)

    Kadhim, Munira; Salomaa, Sisko; Wright, Eric

    2013-01-01

    Non-DNA targeted effects of ionising radiation, which include genomic instability, and a variety of bystander effects including abscopal effects and bystander mediated adaptive response, have raised concerns about the magnitude of low-dose radiation risk. Genomic instability, bystander effects an......) Integrated Project funded by the European Union. Here we critically examine the evidence for non-targeted effects, discuss apparently contradictory results and consider implications for low-dose radiation health effects. © 2012 Elsevier B.V. All rights reserved....... and adaptive responses are powered by fundamental, but not clearly understood systems that maintain tissue homeostasis. Despite excellent research in this field by various groups, there are still gaps in our understanding of the likely mechanisms associated with non-DNA targeted effects, particularly...

  8. The study of some thiazinic and indaminic dye syntheses induced by ionising radiation; Etude de quelques syntheses de colorants thianziniques et indaminiques amorcees par les rayonnements ionisants

    Energy Technology Data Exchange (ETDEWEB)

    Balestic, S. [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

    1961-03-15

    With a view to finding some radiochemical reactions applicable on an industrial scale for evaluating the radioactive waste from nuclear reactors, a systematic study was made of the radiochemical synthesis of thiazinic dyes such as methylene blue and Lauths' violet, on which the first tests were carried out in 1954. The first part of the study concerned the identification and the dosage, during radiolysis, of dyes by means of their absorption spectra after separation from the reaction medium by adsorption chromatography or ion-exchange; other radiolysis products such as ammonium chloride and hydrogen peroxide were also identified. During a later stage by systematically varying the physico-chemical parameters it was possible to determine the most favourable conditions for radio-synthesis; the maximum radiochemical yields obtained had the following values: G (Lauths' violet) 1,65; G (Methylene blue) = 1,75. Furthermore, the study of the influence of variously substituted aminated products on the radiochemical yield showed the possibility of synthesising Bindsehedlers green and Wursters blue by radiochemical methods. Finally the discovery of a fundamental intermediate product, Wursters red, together with the kinetic study of the chemical synthesis of methylene blue made it possible to determine the main stages of the reaction mechanism and to decide which of these stages could be attributed to ionising radiations in the case of the radiochemical synthesis. (author) [French] Dans le but de trouver des reactions radiochimiques susceptibles d'une application industrielle pour valoriser les dechets radioactifs provenant des reacteurs nucleaires, il a ete entrepris une etude systematique de la synthese radiochimique des colorants thiazimiques tels que le Bleu de Methylene et le Violet de Lauth dont les premiers essais ont ete effectues par Loiseleur en 1954. La premiere partie de l'etude a porte sur l'identification et le dosage des colorants formes

  9. Surveillance of health care workers exposed to ionising radiation: Rimed pilot study; Etude Rimed rayonnements ionisants en milieu medical. Etude de faisabilite. Rapport final

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2008-07-01

    The project so-called RIMED aimed to set up epidemiological surveillance of health care workers exposed to ionizing radiation. A pilot study was conducted in a sample of hospital personnel to examine the possibility of identifying exposed subjects in order to analyse mortality patterns according to occupational characteristics such as medical departments or occupations in a historical cohort. Seven hospitals participated in this pilot study. Health-care workers who had worn a dosimeter up to December 2003 were to be included in this cohort. The subjects' identification data were obtained from the SISERI (Systeme d'information de la surveillance de l'exposition aux rayonnements ionisants - Ionizing Radiation Exposure Monitoring Information System) database managed by the Institut de radioprotection et de surete nucleaire - Radiation Protection and Nuclear Safety Institute (IRSN). The SISERI system was in a 'pilot' phase in 2004. According to SISERI database, a total of 5126 subjects were found to have worn a dosimeter up to December 2003. The subjects' identification data were completed by the administrative services of the hospitals and occupational physicians searched for subjects' occupational data. Information required for the vital status search was satisfactorily completed only for 38% of the cohort subjects. This pilot study showed that obtaining data from SISERI database completed by hospital administrative data in 2004 led to a database of insufficient quality for epidemiological surveillance. The Institut de veille sanitaire (French Institute of Public Health Surveillance) recommends that transmission by the employers of some specific personal or occupational data of the exposed subjects should be made compulsory. In this way, SISERI system should be able to constitute any database with required quality for epidemiological surveillance of ionizing radiation exposed subjects. (authors)

  10. Measurement of uranium and its isotopes at trace levels in environmental samples using mass spectrometry

    Science.gov (United States)

    Sahoo, S. K.

    2009-06-01

    Actinides have widely entered the environment as a result of nuclear accidents and atmospheric weapon testing. These radionuclides, especially uranium, are outstanding radioactive pollutants, due to their high radiotoxicity and long half-lives. In addition to this, since depleted uranium (DU) has been used in the Balkan conflict in 1999, there has been a concern about the possible consequences of its use for the people and environment. Therefore, accurate, precise and simple determination methods are necessary in order to evaluate the human dose and the concentration and effects of these nuclides in the environment. The principal isotopes of uranium e.g. 235U and 238U are of primordial origin and 234U present in radioactive equilibrium with 238U. 236U occurs in nature at ultra trace concentrations with a 236U: 238U atom ratio of 10-14. Concentrations of uranium in soil samples were determined using inductively coupled plasma mass spectrometry (ICP-MS) and isotope ratios of uranium were measured using a thermal ionisation mass spectrometer. Radioactive dis-equilibrium of 234/238U, depletion of 235/238U and significant evidence of 236U/238U were noticed in soil samples.

  11. At-line gas chromatographic-mass spectrometric analysis of fatty acid profiles of green microalgae using a direct thermal desorption interface

    NARCIS (Netherlands)

    Blokker, P.; Pel, R.; Akoto, L.; Udo, A.; Brinkman, U.A.Th.; Vreuls, R.J.J.

    2002-01-01

    Thermally assisted hydrolysis and methylation¯gas chromatography (THM¯GC) is an important tool to analyse fatty acid in complex matrices. Since THM¯GC has major drawbacks such as isomerisation when applied to fatty acids in natural matrices, a direct thermal desorption (DTD) interface and an

  12. At-line gas chromatographic-mass spectrometric analysis of fatty acid profiles of green microalgae using a direct thermal desorption interface

    NARCIS (Netherlands)

    Blokker, P.; Pel, R.; Akoto, L.; Brinkman, U.A.T.; Vreuls, R.J.J.

    2002-01-01

    Thermally assisted hydrolysis and methylation-gas chromatography (THM-GC) is an important tool to analyse fatty acid in complex matrices. Since THM-GC has major drawbacks such as isomerisation when applied to fatty acids in natural matrices, a direct thermal desorption (DTD) interface and an

  13. Thermal and mass implications of magmatic evolution in the Lassen volcanic region, California, and minimum constraints on basalt influx to the lower crust

    Science.gov (United States)

    Guffanti, M.; Clynne, M.A.; Muffler, L.J.P.

    1996-01-01

    We have analyzed the heat and mass demands of a petrologic model of basaltdriven magmatic evolution in which variously fractionated mafic magmas mix with silicic partial melts of the lower crust. We have formulated steady state heat budgets for two volcanically distinct areas in the Lassen region: the large, late Quaternary, intermediate to silicic Lassen volcanic center and the nearby, coeval, less evolved Caribou volcanic field. At Caribou volcanic field, heat provided by cooling and fractional crystallization of 52 km3 of basalt is more than sufficient to produce 10 km3 of rhyolitic melt by partial melting of lower crust. Net heat added by basalt intrusion at Caribou volcanic field is equivalent to an increase in lower crustal heat flow of ???7 mW m-2, indicating that the field is not a major crustal thermal anomaly. Addition of cumulates from fractionation is offset by removal of erupted partial melts. A minimum basalt influx of 0.3 km3 (km2 Ma)-1 is needed to supply Caribou volcanic field. Our methodology does not fully account for an influx of basalt that remains in the crust as derivative intrusives. On the basis of comparison to deep heat flow, the input of basalt could be ???3 to 7 times the amount we calculate. At Lassen volcanic center, at least 203 km3 of mantle-derived basalt is needed to produce 141 km3 of partial melt and drive the volcanic system. Partial melting mobilizes lower crustal material, augmenting the magmatic volume available for eruption at Lassen volcanic center; thus the erupted volume of 215 km3 exceeds the calculated basalt input of 203 km3. The minimum basalt input of 1.6 km3 (km2 Ma)-1 is >5 times the minimum influx to the Caribou volcanic field. Basalt influx high enough to sustain considerable partial melting, coupled with locally high extension rate, is a crucial factor in development of Lassen volcanic center; in contrast. Caribou volcanic field has failed to develop into a large silicic center primarily because basalt supply

  14. Mass transfer in fuel cells. [electron microscopy of components, thermal decomposition of Teflon, water transport, and surface tension of KOH solutions

    Science.gov (United States)

    Walker, R. D., Jr.

    1973-01-01

    Results of experiments on electron microscopy of fuel cell components, thermal decomposition of Teflon by thermogravimetry, surface area and pore size distribution measurements, water transport in fuel cells, and surface tension of KOH solutions are described.

  15. Numerical and Experimental Investigations of the Flow Field of Ionised Gases with Applications to High-Performance Electronics and Oil Shale Gasification

    OpenAIRE

    Al-Amayreh, Malik

    2013-01-01

    This thesis investigates two new applications of flow field ionised gases. The first application involves coupled electromagnetic and aerothermodynamic phenomena in an electrical contactor chamber. I studied a new blowout technique to control the speed of the flow. With this new blowout technique, the ionised gases can be generated between the electrodes to feed the coils with current. I observed that the recovery time for the case of higher current is less than that of the following low curr...

  16. Risk of cancer from occupational exposure to ionising radiation: retrospective cohort study of workers in France, the United Kingdom, and the United States (INWORKS)

    OpenAIRE

    Richardson, David B.; Cardis, Elisabeth; Daniels, Robert D.; Gillies, Michael; O?Hagan, Jacqueline A; Ghassan B. Hamra; Haylock, Richard; Laurier, Dominique; Leuraud, Klervi; Moissonnier, Monika; Schubauer-Berigan, Mary K; Thierry-Chef, Isabelle; Kesminiene, Ausrele

    2015-01-01

    Study question Is protracted exposure to low doses of ionising radiation associated with an increased risk of solid cancer? Methods In this cohort study, 308?297 workers in the nuclear industry from France, the United Kingdom, and the United States with detailed monitoring data for external exposure to ionising radiation were linked to death registries. Excess relative rate per Gy of radiation dose for mortality from cancer was estimated. Follow-up encompassed 8.2 million person years. Of 66?...

  17. Potential errors in relative dose measurements in kilovoltage photon beams due to polarity effects in plane-parallel ionisation chambers.

    Science.gov (United States)

    Dowdell, S; Tyler, M; McNamara, J; Sloan, K; Ceylan, A; Rinks, A

    2016-11-15

    Plane-parallel ionisation chambers are regularly used to conduct relative dosimetry measurements for therapeutic kilovoltage beams during commissioning and routine quality assurance. This paper presents the first quantification of the polarity effect in kilovoltage photon beams for two types of commercially available plane-parallel ionisation chambers used for such measurements. Measurements were performed at various depths along the central axis in a solid water phantom and for different field sizes at 2 cm depth to determine the polarity effect for PTW Advanced Markus and Roos ionisation chambers (PTW-Freiburg, Germany). Data was acquired for kilovoltage beams between 100 kVp (half-value layer (HVL)  =  2.88 mm Al) and 250 kVp (HVL  =  2.12 mm Cu) and field sizes of 3-15 cm diameter for 30 cm focus-source distance (FSD) and 4  ×  4 cm2-20  ×  20 cm2 for 50 cm FSD. Substantial polarity effects, up to 9.6%, were observed for the Advanced Markus chamber compared to a maximum 0.5% for the Roos chamber. The magnitude of the polarity effect was observed to increase with field size and beam energy but was consistent with depth. The polarity effect is directly influenced by chamber design, with potentially large polarity effects for some plane-parallel ionisation chambers. Depending on the specific chamber used, polarity corrections may be required for output factor measurements of kilovoltage photon beams. Failure to account for polarity effects could lead to an incorrect dose being delivered to the patient.

  18. Interpretation of ionospheric F-region structures in the vicinity of ionisation troughs observed by satellite radio tomography

    OpenAIRE

    Aladjev, G. A.; Evstafiev, O. V.; Mingalev, V. S.; G. I. Mingaleva; E. D. Tereshchenko; Khudukon, B. Z.

    2001-01-01

    Tomographic images of the spatial distribution of electron density in the ionospheric F-region are presented from the Russian-American Tomography Experiment (RATE) in November 1993 as well as from campaigns carried out in northern Scandinavia in November 1995 and in Russia in April 1990. The reconstructions selected display the ionisation troughs above the tomographic chains of receivers during geomagnetically quiet and disturbed periods. Two mathematical models of the high-latitude ionospher...

  19. The stability and generation pattern of thermally formed isocyanic acid (ICA) in air - potential and limitations of proton transfer reaction-mass spectrometry (PTR-MS) for real-time workroom atmosphere measurements.

    Science.gov (United States)

    Jankowski, Mikolaj Jan; Olsen, Raymond; Thomassen, Yngvar; Molander, Paal

    2016-07-13

    Isocyanic acid (ICA) in vapour phase has been reported to be of unstable nature, making the occupational hygienic relevance of ICA questionable. The stability of pure ICA in clean air at different humidity conditions was investigated by Fourier transform-infrared spectrometric (FT-IR) measurements. Furthermore, the stability of ICA in a complex atmosphere representative thermal degradation hot-work procedures were examined by performing parallel measurements by proton transfer reaction-mass spectrometric (PTR-MS) instrumentation and off-line denuder air sampling using di-n-butylamine (as a derivatization agent prior to liquid chromatography mass spectrometric (LC-MS) determination). The apparent half-life of ICA in pure ICA atmospheres was 16 to 4 hours at absolute humidity (AH) in the range 4.2 to 14.6 g m(-3), respectively. In a complex atmosphere at an initial AH of 9.6 g m(-3) the apparent half-life of ICA was 8 hours, as measured with the denuder method. Thus, thermally formed ICA is to be considered as a potential occupational hazard with regard to inhalation. The generation pattern of ICA formed during controlled gradient (100-540 °C) thermal decomposition of different polymers in the presence of air was examined by parallel PTR-MS and denuder air sampling. According to measurement by denuder sampling ICA was the dominant aliphatic isocyanate formed during the thermal decomposition of all polymers. The real-time measurements of the decomposed polymers revealed different ICA generation patterns, with initial appearance of thermally released ICA in the temperature range 200-260 °C. The PTR-MS ICA measurements was however affected by mass overlap from other decomposition products at m/z 44, illustrated by a [ICA]Denuder/[ICA]PTR-MS ratio ranging from 0.04 to 0.90. These findings limits the potential use of PTR-MS for real time measurements of thermally released ICA in field, suggesting parallel sampling with short-term sequential off-line methodology.

  20. Investigation of the ionisation density dependence of the glow curve characteristics of LIF:MG,TI (TLD-100)

    Science.gov (United States)

    Horowitz, Y. S.; Horowitz, A.; Oster, L.; Marino, S.; Datz, H.; Margaliot, M.

    2008-01-01

    The dependence of the shape of the glow curve of LiF:Mg,Ti (TLD-100) on ionisation density was investigated using irradiation with 90Sr/90Y beta rays, 60 and 250 kVp X rays, various heavy-charged particles and 0.2 and 14 MeV neutrons. Special attention is focused on the properties of high-temperature thermoluminescence; specifically, the behaviour of the high-temperature ratio (HTR) of Peaks 7 and 8 as a function of batch and annealing protocol. The correlation of Peaks 7 and 8 with average linear-energy