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Sample records for two-dimensional gas chromatographymass

  1. [Analysis of aromatic hydrocarbons in cracking products of jet fuel by comprehensive two-dimensional gas chromatography-mass spectrometry].

    Science.gov (United States)

    Li, Haijing; Zhang, Xiangwen

    2017-08-08

    As coking precursors, aromatic hydrocarbons have an effect on the cracking stability of fuels. A method for identifying and quantitating aromatics in the supercritical cracking products of jet fuel was established by comprehensive two-dimensional gas chromatography coupled with mass spectrometry (GC×GC-MS). The effects of main chromatographic conditions such as initial oven temperature and modulation period on the separation of supercritical cracking products were studied. The method has good separation ability for polycyclic aromatic hydrocarbons (PAH) isomers. A total of 27 aromatics, including monocyclic aromatic hydrocarbons, bicyclic aromatic hydrocarbons, tricyclic aromatic hydrocarbons, tetracyclic aromatic hydrocarbons, etc., were identified based on standard mass spectra, the retention times of standards and literature reports. Moreover, the corresponding quantitative determination was achieved by external standard method of GC×GC-FID. The results showed that the contents of aromatics increased with the increase of gas yield. When gas yield reached 22%, the bicyclic aromatic hydrocarbons began to produce, and their contents increased exponentially with the increase of gas yield. Compared with the traditional GC-MS, the method has better separation and qualitative ability, and can be applied to the separation of complex samples and qualitative and quantitative analyses of cracking products.

  2. Discriminating Brazilian crude oils using comprehensive two-dimensional gas chromatography-mass spectrometry and multiway principal component analysis.

    Science.gov (United States)

    Prata, Paloma S; Alexandrino, Guilherme L; Mogollón, Noroska Gabriela S; Augusto, Fabio

    2016-11-11

    The geochemical characterization of petroleum is an essential task to develop new strategies and technologies when analyzing the commercial potential of crude oils for exploitation. Due to the chemical complexity of these samples, the use of modern analytical techniques along with multivariate exploratory data analysis approaches is an interesting strategy to extract relevant geochemical characteristics about the oils. In this work, important geochemical information obtained from crude oils from different production basins were obtained analyzing the maltene fraction of the oils by comprehensive two-dimensional gas chromatography coupled to quadrupole mass spectrometry (GC×GC-QMS), and performing multiway principal component analysis (MPCA) of the chromatographic data. The results showed that four MPC explained 93.57% of the data variance, expressing mainly the differences on the profiles of the saturated hydrocarbon fraction of the oils (C 13 -C 18 and C 19 -C 30 n-alkanes and the pristane/phytane ratio). The MPC1 grouped the samples severely biodegraded oils, while the type of the depositional paleoenvironments of the oils and its oxidation conditions (as well as their thermal maturity) could be inferred analysing others relevant MPC. Additionally, considerations about the source of the oil samples was also possible based on the overall distribution of relevant biomarkers such as the phenanthrene derivatives, tri-, tetra- and pentacyclic terpanes. Copyright © 2016 Elsevier B.V. All rights reserved.

  3. Chemical characterisation of two Australian-grown strawberry varieties by using comprehensive two-dimensional gas chromatography-mass spectrometry.

    Science.gov (United States)

    Samykanno, Kavitha; Pang, Edwin; Marriott, Philip J

    2013-12-01

    The volatile compositions of two strawberry varieties ('Albion' and 'Juliette') grown in Australia were analysed with comprehensive two-dimensional gas chromatography (GC×GC) combined with time-of-flight mass spectrometry (ToFMS). A suitable data processing method was created that should be sufficiently robust to compare sample chromatograms within a harvest season as well as between seasons with relative ease. Ninety-four compounds were tentatively or positively identified between the two varieties of which 20 have apparently not been previously reported to be components of strawberry volatiles. It was determined that Albion and Juliette have comparable total soluble solids content close to 11°Brix. However, since Juliette exhibited a lower titratable acidity content than Albion, it consequently has a slightly larger sugar/acid ratio. The presence of 2,5-dimethyl-4-hydroxy-(2H)-furan-3-one (furaneol) was detected only in Juliette and this variety also had a higher area percentage of 2,5-dimethyl-4-methoxy-(2H)-furan-3-one (mesifuran), according to the sampling protocol. These experimental results offer possible explanations as to why Juliette is perceived to have a sweeter flavour than Albion. Copyright © 2013 Elsevier Ltd. All rights reserved.

  4. Identification of odorants in wood of Calocedrus decurrens (Torr.) Florin by aroma extract dilution analysis and two-dimensional gas chromatography-mass spectrometry/olfactometry.

    Science.gov (United States)

    Schreiner, Linda; Loos, Helene M; Buettner, Andrea

    2017-06-01

    General emissions of volatile organic compounds from wood are well investigated, but only limited information is available on the odor-active substances contained therein. To close this gap, we aimed at specifically elucidating the odorous constituents of wood from incense cedar [Calocedrus decurrens (Torr.) Florin]; this material is commonly used for the production of a range of products such as pencils and interior accessories. Targeted odorant analysis requires specialized techniques combining modern odorant analytical tools with human-sensory evaluation. Following this concept, the odor profile of the wood sample was first evaluated by human-sensory analyses. Then, the most potent wood odorants were characterized by means of gas chromatography-olfactometry and ranked according to their odor potency via aroma extract dilution analysis. With use of this approach, more than 60 odorous substances were detected, and the 22 most potent odorants were successfully identified by gas chromatography-mass spectrometry/olfactometry and two-dimensional gas chromatography-mass spectrometry/olfactometry. Among the main odorants found were a series of terpenes, several degradation products of fatty acids, and a number of odorants with a phenolic core moiety. Five odorants are reported here for the first time as wood odorants, such as γ-octalactone and 3-phenylpropanoic acid; thymoquinone was demonstrated for the first time to have a pencil-like odor quality.

  5. Multivariate analytical figures of merit as a metric for evaluation of quantitative measurements using comprehensive two-dimensional gas chromatography-mass spectrometry.

    Science.gov (United States)

    Eftekhari, Ali; Parastar, Hadi

    2016-09-30

    The present contribution is devoted to develop multivariate analytical figures of merit (AFOMs) as a new metric for evaluation of quantitative measurements using comprehensive two-dimensional gas chromatography-mass spectrometry (GC×GC-MS). In this regard, new definition of sensitivity (SEN) is extended to GC×GC-MS data and then, other multivariate AFOMs including analytical SEN (γ), selectivity (SEL) and limit of detection (LOD) are calculated. Also, two frequently used second- and third-order calibration algorithms of multivariate curve resolution-alternating least squares (MCR-ALS) as representative of multi-set methods and parallel factor analysis (PARAFAC) as representative of multi-way methods are discussed to exploit pure component profiles and to calculate multivariate AFOMs. Different GC×GC-MS data sets with different number of components along with various levels of artifacts are simulated and analyzed. Noise, elution time shifts in both chromatographic dimensions, peak overlap and interferences are considered as the main artifacts in this work. Additionally, a new strategy is developed to estimate the noise level using variance-covariance matrix of residuals which is very important to calculate multivariate AFOMs. Finally, determination of polycyclic aromatic hydrocarbons (PAHs) in aromatic fraction of heavy fuel oil (HFO) analyzed by GC×GC-MS is considered as real case to confirm applicability of the proposed metric in real samples. It should be pointed out that the proposed strategy in this work can be used for other types of comprehensive two-dimensional chromatographic (CTDC) techniques like comprehensive two dimensional liquid chromatography (LC×LC). Copyright © 2016 Elsevier B.V. All rights reserved.

  6. Quantitative analysis of fragrance in selectable one dimensional or two dimensional gas chromatography-mass spectrometry with simultaneous detection of multiple detectors in single injection.

    Science.gov (United States)

    Tan, Hui Peng; Wan, Tow Shi; Min, Christina Liew Shu; Osborne, Murray; Ng, Khim Hui

    2014-03-14

    A selectable one-dimensional ((1)D) or two-dimensional ((2)D) gas chromatography-mass spectrometry (GC-MS) system coupled with flame ionization detector (FID) and olfactory detection port (ODP) was employed in this study to analyze perfume oil and fragrance in shower gel. A split/splitless (SSL) injector and a programmable temperature vaporization (PTV) injector are connected via a 2-way splitter of capillary flow technology (CFT) in this selectable (1)D/(2)D GC-MS/FID/ODP system to facilitate liquid sample injections and thermal desorption (TD) for stir bar sorptive extraction (SBSE) technique, respectively. The dual-linked injectors set-up enable the use of two different injector ports (one at a time) in single sequence run without having to relocate the (1)D capillary column from one inlet to another. Target analytes were separated in (1)D GC-MS/FID/ODP and followed by further separation of co-elution mixture from (1)D in (2)D GC-MS/FID/ODP in single injection without any instrumental reconfiguration. A (1)D/(2)D quantitative analysis method was developed and validated for its repeatability - tR; calculated linear retention indices (LRI); response ratio in both MS and FID signal, limit of detection (LOD), limit of quantitation (LOQ), as well as linearity over a concentration range. The method was successfully applied in quantitative analysis of perfume solution at different concentration level (RSD≤0.01%, n=5) and shower gel spiked with perfume at different dosages (RSD≤0.04%, n=5) with good recovery (96-103% for SSL injection; 94-107% for stir bar sorptive extraction-thermal desorption (SBSE-TD). Copyright © 2014 Elsevier B.V. All rights reserved.

  7. Development and validation of a comprehensive two-dimensional gas chromatography-mass spectrometry method for the analysis of phytosterol oxidation products in human plasma

    NARCIS (Netherlands)

    Menéndez-Carreño, M.; Steenbergen, H.; Janssen, H.-G.

    2012-01-01

    Phytosterol oxidation products (POPs) have been suggested to exert adverse biological effects similar to, although less severe than, their cholesterol counterparts. For that reason, their analysis in human plasma is highly relevant. Comprehensive two-dimensional gas chromatography (GC×GC) coupled

  8. Offline coupling of high-speed counter-current chromatography and gas chromatography/mass spectrometry generates a two-dimensional plot of toxaphene components.

    Science.gov (United States)

    Kapp, Thomas; Vetter, Walter

    2009-11-20

    High-speed counter-current chromatography (HSCCC), a separation technique based solely on the partitioning of solutes between two immiscible liquid phases, was applied for the fractionation of technical toxaphene, an organochlorine pesticide which consists of a complex mixture of structurally closely related compounds. A solvent system (n-hexane/methanol/water 34:24:1, v/v/v) was developed which allowed to separate compounds of technical toxaphene (CTTs) with excellent retention of the stationary phase (S(f) = 88%). Subsequent analysis of all HSCCC fractions by gas chromatography coupled to electron-capture negative ion mass spectrometry (GC/ECNI-MS) provided a wealth of information regarding separation characteristics of HSCCC and the composition of technical toxaphene. The visualization of the large amount of data obtained from the offline two-dimensional HSCCC-GC/ECNI-MS experiment was facilitated by the creation of a two-dimensional (2D) contour plot. The contour plot not only provided an excellent overview of the HSCCC separation progress, it also illustrated the differences in selectivity between HSCCC and GC. The results of this proof-of-concept study showed that the 2D chromatographic approach involving HSCCC facilitated the separation of CTTs that coelute in unidimensional GC. Furthermore, the creation of 2D contour plots may provide a useful means of enhancing data visualization for other offline two-dimensional separations.

  9. Impurity profiling of a chemical weapon precursor for possible forensic signatures by comprehensive two-dimensional gas chromatography/mass spectrometry and chemometrics.

    Science.gov (United States)

    Hoggard, Jamin C; Wahl, Jon H; Synovec, Robert E; Mong, Gary M; Fraga, Carlos G

    2010-01-15

    In this report we present the feasibility of using analytical and chemometric methodologies to reveal and exploit the chemical impurity profiles from commercial dimethyl methylphosphonate (DMMP) samples to illustrate the type of forensic information that may be obtained from chemical-attack evidence. Using DMMP as a model compound of a toxicant that may be used in a chemical attack, we used comprehensive two-dimensional gas chromatography/time-of-flight mass spectrometry (GC x GC/TOF-MS) to detect and identify trace organic impurities in six samples of commercially acquired DMMP. The GC x GC/TOF-MS data was analyzed to produce impurity profiles for all six DMMP samples using 29 analyte impurities. The use of PARAFAC for the mathematical resolution of overlapped GC x GC peaks ensured clean spectra for the identification of many of the detected analytes by spectral library matching. The use of statistical pairwise comparison revealed that there were trace impurities that were quantitatively similar and different among five of the six DMMP samples. Two of the DMMP samples were revealed to have identical impurity profiles by this approach. The use of nonnegative matrix factorization indicated that there were five distinct DMMP sample types as illustrated by the clustering of the multiple DMMP analyses into five distinct clusters in the scores plots. The two indistinguishable DMMP samples were confirmed by their chemical supplier to be from the same bulk source. Sample information from the other chemical suppliers supported the idea that the other four DMMP samples were likely from different bulk sources. These results demonstrate that the matching of synthesized products from the same source is possible using impurity profiling. In addition, the identified impurities common to all six DMMP samples provide strong evidence that basic route information can be obtained from impurity profiles. Finally, impurities that may be unique to the sole bulk manufacturer of DMMP were

  10. Comprehensive lipidomic analysis of human plasma using multidimensional liquid- and gas-phase separations: Two-dimensional liquid chromatography-mass spectrometry vs. liquid chromatography-trapped-ion-mobility-mass spectrometry.

    Science.gov (United States)

    Baglai, Anna; Gargano, Andrea F G; Jordens, Jan; Mengerink, Ynze; Honing, Maarten; van der Wal, Sjoerd; Schoenmakers, Peter J

    2017-12-29

    Recent advancements in separation science have resulted in the commercialization of multidimensional separation systems that provide higher peak capacities and, hence, enable a more-detailed characterization of complex mixtures. In particular, two powerful analytical tools are increasingly used by analytical scientists, namely online comprehensive two-dimensional liquid chromatography (LC×LC, having a second-dimension separation in the liquid phase) and liquid chromatography-ion mobility-spectrometry (LC-IMS, second dimension separation in the gas phase). The goal of the current study was a general assessment of the liquid-chromatography-trapped-ion-mobility-mass spectrometry (LC-TIMS-MS) and comprehensive two-dimensional liquid chromatography-mass spectrometry (LC×LC-MS) platforms for untargeted lipid mapping in human plasma. For the first time trapped-ion-mobility spectrometry (TIMS) was employed for the separation of the major lipid classes and ion-mobility-derived collision-cross-section values were determined for a number of lipid standards. The general effects of a number of influencing parameters have been inspected and possible directions for improvements are discussed. We aimed to provide a general indication and practical guidelines for the analyst to choose an efficient multidimensional separation platform according to the particular requirements of the application. Analysis time, orthogonality, peak capacity, and an indicative measure for the resolving power are discussed as main characteristics for multidimensional separation systems. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Target analysis of tert-butyldimethylsilyl derivatives of nerve agent hydrolysis products by selectable one-dimensional or two-dimensional gas chromatography-mass spectrometry.

    Science.gov (United States)

    Seto, Yasuo; Tachikawa, Masumi; Kanamori-Kataoka, Mieko; Sasamoto, Kikuo; Ochiai, Nobuo

    2017-06-09

    A target analysis method for the sensitive and discriminative determination of the nerve agent hydrolysis products alkyl methylphosphonic acids as their tert-butyldimethylsilyl (TBDMS) derivatives was developed using a combination of selectable one- and two-dimensional ( 1 D/ 2 D) GC-MS, and applied to the analysis of samples with significant interfering matrices. After sample drying, the alkylmethylphosphonic acids and methylphosphonic acid (MPA) were converted to TBDMS derivatives by addition of N-methyl-N-(tert-butyldimethylsilyl)trifluoroacetamide with heating, and subjected to 1 D/ 2 D GC-MS. The apparatus consisted of an initial low thermal mass DB-5 column and a second DB-17 column together with an electron ionization quadrupole mass spectrometer, offering simple and flexible switching between one- and two-dimensional GC-MS analysis in a single GC-MS system. Using 1 D/ 2 D GC-MS, analytes that do not co-elute with matrix components can be separated using 1 D GC mode alone. Only those parts of the chromatogram that are negatively affected by the co-elution of matrix components need to be transferred and separated with 2 D GC. Quantitation can be performed by a combination of both separations and mass spectrometric detection. The TBDMS derivatives of ethyl-, isopropyl-, isobutyl-, pinacolyl-, and cyclohexyl-MPA (cHMPA) and MPA itself were well separated within 3min and determined in 1 D GC-MS mode with detection limits of around 10ng/ml of reaction mixture (except for the cHMPA derivative, whose mass spectrum contained noisy background peaks). In 2 D-GC-MS mode, where each 0.04min elution window from the 1 D GC was subjected to heart-cut (H/C) and transferred to the second column after back-flushing the first column, the peak for the cHMPA TBDMS derivative was isolated and afforded a clean mass spectrum within 6min. The recoveries of all the derivatives on 2 D GC from 1 D GC were estimated to be over 66%, and the detection limits were around 10ng/ml of

  12. Comprehensive two-dimensional gas chromatography-mass spectrometry analysis of volatile constituents in Thai vetiver root oils obtained by using different extraction methods.

    Science.gov (United States)

    Pripdeevech, Patcharee; Wongpornchai, Sugunya; Marriott, Philip J

    2010-01-01

    Vetiver root oil is known as one of the finest fixatives used in perfumery. This highly complex oil contains more than 200 components, which are mainly sesquiterpene hydrocarbons and their oxygenated derivatives. Since conventional GC-MS has limitation in terms of separation efficiency, the comprehensive two-dimensional GC-MS (GC x GC-MS) was proposed in this study as an alternative technique for the analysis of vetiver oil constituents. To evaluate efficiency of the hyphenated GC x GC-MS technique in terms of separation power and sensitivity prior to identification and quantitation of the volatile constituents in a variety of vetiver root oil samples. METHODOLOGY. Dried roots of Vetiveria zizanioides were subjected to extraction using various conditions of four different methods; simultaneous steam distillation, supercritical fluid, microwave-assisted, and Soxhlet extraction. Volatile components in all vetiver root oil samples were separated and identified by GC-MS and GC x GC-MS. The relative contents of volatile constituents in each vetiver oil sample were calculated using the peak volume normalization method. Different techniques of extraction had diverse effects on yield, physical and chemical properties of the vetiver root oils obtained. Overall, 64 volatile constituents were identified by GC-MS. Among the 245 well-resolved individual components obtained by GC x GC-MS, the additional identification of 43 more volatiles was achieved. In comparison with GC-MS, GC x GC-MS showed greater ability to differentiate the quality of essential oils obtained from diverse extraction conditions in terms of their volatile compositions and contents.

  13. Determination of benzenic and halogenated volatile organic compounds in animal-derived food products by one-dimensional and comprehensive two-dimensional gas chromatography-mass spectrometry.

    Science.gov (United States)

    Ratel, Jérémy; Engel, Erwan

    2009-11-06

    Animal-derived products are particularly vulnerable to contamination by volatile organic compounds (VOCs). These lipophilic substances, which are generated by an increasing number of sources, are easily transferred to the atmosphere, water, soil, and plants. They are ingested by livestock and become trapped in the fat fraction of edible animal tissues. The aim of this work was to determine the occurrence, risk for human health and entryways of benzenic and halogenated VOCs (BHVOCs) in meat products, milks and sea foods using gas chromatography- mass spectrometry (GC-MS) techniques. In the first part, the occurrence and levels of the BHVOCs in animal products were studied. One muscle and three fat tissues were analysed by GC-Quad/MS in 16 lambs. Of 52 BHVOCs identified, 46 were found in the three fat tissues and 29 in all four tissues, confirming that VOCs are widely disseminated in the body. Twenty-six BHVOCs were quantified in fat tissues, and risk for consumer health was assessed for six of these compounds regulated by the US Environmental Protection Agency (EPA). The BHVOC content was found to be consistent with previous reports and was below the maximum contaminant levels set by the EPA. In the second part, the performance of GCxGC-TOF/MS for comprehensively detecting BHVOCs and showing their entryways in animal-derived food chains was assessed. Meat, milk and oysters were analysed by GC-Quad/MS and GCxGC-TOF/MS. For all these products, at least a 7-fold increase in the contaminants detected was achieved with the GCxGC-TOF/MS technique. The results showed that the production surroundings, through animal feeding or geographical location, were key determinants of BHVOC composition in the animal products.

  14. Parallel comprehensive two-dimensional gas chromatography.

    Science.gov (United States)

    Yan, DanDan; Tedone, Laura; Koutoulis, Anthony; Whittock, Simon P; Shellie, Robert A

    2017-11-17

    We introduce an information rich analytical approach called parallel comprehensive two-dimensional gas chromatography (2GC×2GC). This parallel chromatography approach splits injected samples into two independent two-dimensional column ensembles and provides two GC×GC separations by using contra-directional thermal modulation. The first-dimension ( 1 D) and second-dimension ( 2 D) columns are connected using planar three-port microchannel devices, which are supplied with supplementary flow via two pressure controller modules. Precise carrier gas flow control at the junction of the 1 D and 2 D columns permits independent control of flow conditions in each separation column. The 2GC×2GC approach provides two entirely independent GC×GC separations for each injection. Analysis of hop (Humulus lupulus L.) essential oils is used to demonstrate the capability of the approach. The analytical performance of each GC×GC separation in the 2GC×2GC experiment is comparable to individual GC×GC separation with matching column configurations. The peak capacity of 2GC×2GC is about 2 times than that of single GC×GC system. The dual 2D chromatograms produced by this single detector system provide complementary separations and additional identification information by harnessing different selectivity provided by the four separation columns. Copyright © 2017 Elsevier B.V. All rights reserved.

  15. One- and two-dimensional gas chromatography-mass spectrometry and high performance liquid chromatography-diode-array detector fingerprints of complex substances: a comparison of classification performance of similar, complex Rhizoma Curcumae samples with the aid of chemometrics.

    Science.gov (United States)

    Ni, Yongnian; Mei, Minghua; Kokot, Serge

    2012-01-27

    Many complex natural or synthetic products are analysed either by the GC-MS (gas chromatography-mass spectrometry) or HPLC-DAD (high performance liquid chromatography-diode-array detector) technique, each of which produces a one-dimensional fingerprint for a given sample. This may be used for classification of different batches of a product. GC-MS and HPLC-DAD analyses of complex, similar substances represented by the three common types of the TCM (traditional Chinese medicine), Rhizoma Curcumae were analysed in the form of one- and two-dimensional matrices firstly with the use of PCA (Principal component analysis), which showed a reasonable separation of the samples for each technique. However, the separation patterns were rather different for each analytical method, and PCA of the combined data matrix showed improved discrimination of the three types of object; close associations between the GC-MS and HPLC-DAD variables were observed. LDA (linear discriminant analysis), BP-ANN (back propagation-artificial neural networks) and LS-SVM (least squares-support vector machine) chemometrics methods were then applied to classify the training and prediction sets. For one-dimensional matrices, all training models indicated that several samples would be misclassified; the same was observed for each prediction set. However, by comparison, in the analysis of the combined matrix, all models gave 100% classification with the training set, and the LS-SVM calibration also produced a 100% result for prediction, with the BP-ANN calibration closely behind. This has important implications for comparing complex substances such as the TCMs because clearly the one-dimensional data matrices alone produce inferior results for training and prediction as compared to the combined data matrix models. Thus, product samples may be misclassified with the use of the one-dimensional data because of insufficient information. Copyright © 2011 Elsevier B.V. All rights reserved.

  16. Spin dynamics in a two-dimensional quantum gas

    DEFF Research Database (Denmark)

    Pedersen, Poul Lindholm; Gajdacz, Miroslav; Deuretzbacher, Frank

    2014-01-01

    We have investigated spin dynamics in a two-dimensional quantum gas. Through spin-changing collisions, two clouds with opposite spin orientations are spontaneously created in a Bose-Einstein condensate. After ballistic expansion, both clouds acquire ring-shaped density distributions with superimp......We have investigated spin dynamics in a two-dimensional quantum gas. Through spin-changing collisions, two clouds with opposite spin orientations are spontaneously created in a Bose-Einstein condensate. After ballistic expansion, both clouds acquire ring-shaped density distributions...... with nonlocal Einstein-Podolsky-Rosen entanglement....

  17. Magnetoelectronic transport of the two-dimensional electron gas in ...

    Indian Academy of Sciences (India)

    Home; Journals; Pramana – Journal of Physics; Volume 72; Issue 2 ... CdSe quantum wells; 2D electron gas; magneto-electronic transport. Abstract. Hall mobility and magnetoresistance coefficient for the two-dimensional (2D) electron transport parallel to the heterojunction interfaces in a single quantum well of CdSe are ...

  18. Zero sound in a two-dimensional dipolar Fermi gas

    NARCIS (Netherlands)

    Lu, Z.K.; Matveenko, S.I.; Shlyapnikov, G.V.

    2013-01-01

    We study zero sound in a weakly interacting two-dimensional (2D) gas of single-component fermionic dipoles (polar molecules or atoms with a large magnetic moment) tilted with respect to the plane of their translational motion. It is shown that the propagation of zero sound is provided by both

  19. Stable corrugated state of the two-dimensional electron gas

    International Nuclear Information System (INIS)

    Mendez-Moreno, R.M.; Moreno, M.; Ortiz, M.A.

    1991-01-01

    A corrugated and stable ground state is found for the two-dimensional electron gas in both the normal paramagnetic and the fully polarized phases. The self-consistent Hartree-Fock method is used with a modulated set of trial wave functions within the deformable jellium model. The results for high metallic densities reproduce the usual noncorrugated ferromagnetic electron-gas behavior. A transition to a paramagnetic corrugated state for values of r s ∼6.5 is predicted. At lower densities r s ∼30, a second transition to a corrugated ferromagnetic phase is suggested

  20. Coherent Response of Two Dimensional Electron Gas probed by Two Dimensional Fourier Transform Spectroscopy

    Science.gov (United States)

    Paul, Jagannath

    Advent of ultrashort lasers made it possible to probe various scattering phenomena in materials that occur in a time scale on the order of few femtoseconds to several tens of picoseconds. Nonlinear optical spectroscopy techniques, such as pump-probe, transient four wave mixing (TFWM), etc., are very common to study the carrier dynamics in various material systems. In time domain, the transient FWM uses several ultrashort pulses separated by time delays to obtain the information of dephasing and population relaxation times, which are very important parameters that govern the carrier dynamics of materials. A recently developed multidimensional nonlinear optical spectroscopy is an enhanced version of TFWM which keeps track of two time delays simultaneously and correlate them in the frequency domain with the aid of Fourier transform in a two dimensional map. Using this technique, the nonlinear complex signal field is characterized both in amplitude and phase. Furthermore, this technique allows us to identify the coupling between resonances which are rather difficult to interpret from time domain measurements. This work focuses on the study of the coherent response of a two dimensional electron gas formed in a modulation doped GaAs/AlGaAs quantum well both at zero and at high magnetic fields. In modulation doped quantum wells, the excitons are formed as a result of the inter- actions of the charged holes with the electrons at the Fermi edge in the conduction band, leading to the formation of Mahan excitons, which is also referred to as Fermi edge singularity (FES). Polarization and temperature dependent rephasing 2DFT spectra in combination with TI-FWM measurements, provides insight into the dephasing mechanism of the heavy hole (HH) Mahan exciton. In addition to that strong quantum coherence between the HH and LH Mahan excitons is observed, which is rather surprising at this high doping concentration. The binding energy of Mahan excitons is expected to be greatly

  1. Statistical thermodynamics of a two-dimensional relativistic gas.

    Science.gov (United States)

    Montakhab, Afshin; Ghodrat, Malihe; Barati, Mahmood

    2009-03-01

    In this paper we study a fully relativistic model of a two-dimensional hard-disk gas. This model avoids the general problems associated with relativistic particle collisions and is therefore an ideal system to study relativistic effects in statistical thermodynamics. We study this model using molecular-dynamics simulation, concentrating on the velocity distribution functions. We obtain results for x and y components of velocity in the rest frame (Gamma) as well as the moving frame (Gamma;{'}) . Our results confirm that Jüttner distribution is the correct generalization of Maxwell-Boltzmann distribution. We obtain the same "temperature" parameter beta for both frames consistent with a recent study of a limited one-dimensional model. We also address the controversial topic of temperature transformation. We show that while local thermal equilibrium holds in the moving frame, relying on statistical methods such as distribution functions or equipartition theorem are ultimately inconclusive in deciding on a correct temperature transformation law (if any).

  2. Micromachined two dimensional resistor arrays for determination of gas parameters

    NARCIS (Netherlands)

    van Baar, J.J.J.; Verwey, Willem B.; Dijkstra, Mindert; Dijkstra, Marcel; Wiegerink, Remco J.; Lammerink, Theodorus S.J.; Krijnen, Gijsbertus J.M.; Elwenspoek, Michael Curt

    A resistive sensor array is presented for two dimensional temperature distribution measurements in a micromachined flow channel. This allows simultaneous measurement of flow velocity and fluid parameters, like thermal conductivity, diffusion coefficient and viscosity. More general advantages of

  3. Magnetoelectronic transport of the two-dimensional electron gas in ...

    Indian Academy of Sciences (India)

    Abstract. Hall mobility and magnetoresistance coefficient for the two-dimensional (2D) electron transport parallel to the heterojunction interfaces in a single quantum well of. CdSe are calculated with a numerical iterative technique in the framework of Fermi–Dirac statistics. Lattice scatterings due to polar-mode longitudinal ...

  4. Carrier transport in multi-terminal superconductor/two-dimensional electron gas Josephson junctions

    NARCIS (Netherlands)

    Guzenko, V.A.; Schäpers, Th.; Müller, R.P.; Golubov, Alexandre Avraamovitch; Brinkman, Alexander; Crecelius, G.; Kaluza, A.; Lüth, H.

    2001-01-01

    The critical current in a superconductor/two-dimensional electron gas junction/superconductor junction is controlled by an injection current. In case of a carrier injection from one contact to the semiconductor through the two-dimensional electron gas region of the junction to an ohmic contact at

  5. A microstrip gas avalanche chamber with two-dimensional readout

    International Nuclear Information System (INIS)

    Angelini, F.; Bellazzini, R.; Brez, A.; Massai, M.M.; Spandre, G.; Torquati, M.R.

    1989-01-01

    A microstrip gas avalanche chamber with a 200 μm anode pitch has been built and successfully tested in our laboratory. A gas gain of 10 4 and an energy resolution of 18% (FWHM) at 6 keV have been measured using a gas mixture of argon-CO 2 at atmospheric pressure. A preliminary measurement of the positional sensitivity indicates that a spatial resolution of 50 μm can be obtained. (orig.)

  6. Induced superconductivity in high-mobility two-dimensional electron gas in gallium arsenide heterostructures.

    Science.gov (United States)

    Wan, Zhong; Kazakov, Aleksandr; Manfra, Michael J; Pfeiffer, Loren N; West, Ken W; Rokhinson, Leonid P

    2015-06-11

    Search for Majorana fermions renewed interest in semiconductor-superconductor interfaces, while a quest for higher-order non-Abelian excitations demands formation of superconducting contacts to materials with fractionalized excitations, such as a two-dimensional electron gas in a fractional quantum Hall regime. Here we report induced superconductivity in high-mobility two-dimensional electron gas in gallium arsenide heterostructures and development of highly transparent semiconductor-superconductor ohmic contacts. Supercurrent with characteristic temperature dependence of a ballistic junction has been observed across 0.6 μm, a regime previously achieved only in point contacts but essential to the formation of well separated non-Abelian states. High critical fields (>16 T) in NbN contacts enables investigation of an interplay between superconductivity and strongly correlated states in a two-dimensional electron gas at high magnetic fields.

  7. Magnetoresistance of a two-dimensional electron gas in a random magnetic field

    DEFF Research Database (Denmark)

    Smith, Anders; Taboryski, Rafael Jozef; Hansen, Luise Theil

    1994-01-01

    We report magnetoresistance measurements on a two-dimensional electron gas made from a high-mobility GaAs/AlxGa1-xAs heterostructure, where the externally applied magnetic field was expelled from regions of the semiconductor by means of superconducting lead grains randomly distributed on the surf......We report magnetoresistance measurements on a two-dimensional electron gas made from a high-mobility GaAs/AlxGa1-xAs heterostructure, where the externally applied magnetic field was expelled from regions of the semiconductor by means of superconducting lead grains randomly distributed...

  8. Impact of comprehensive two-dimensional gas chromatography with mass spectrometry on food analysis.

    Science.gov (United States)

    Tranchida, Peter Q; Purcaro, Giorgia; Maimone, Mariarosa; Mondello, Luigi

    2016-01-01

    Comprehensive two-dimensional gas chromatography with mass spectrometry has been on the separation-science scene for about 15 years. This three-dimensional method has made a great positive impact on various fields of research, and among these that related to food analysis is certainly at the forefront. The present critical review is based on the use of comprehensive two-dimensional gas chromatography with mass spectrometry in the untargeted (general qualitative profiling and fingerprinting) and targeted analysis of food volatiles; attention is focused not only on its potential in such applications, but also on how recent advances in comprehensive two-dimensional gas chromatography with mass spectrometry will potentially be important for food analysis. Additionally, emphasis is devoted to the many instances in which straightforward gas chromatography with mass spectrometry is a sufficiently-powerful analytical tool. Finally, possible future scenarios in the comprehensive two-dimensional gas chromatography with mass spectrometry food analysis field are discussed. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Nonlocality, Correlations, and Magnetotransport in a Spatially Modulated Two-Dimensional Electron Gas

    Science.gov (United States)

    Raichev, O. E.

    2018-04-01

    It is shown that the classical commensurability phenomena in weakly modulated two-dimensional electron systems is a manifestation of the intrinsic properties of the correlation functions describing a homogeneous electron gas in a magnetic field. The theory demonstrates the importance for consideration of nonlocal response and removes the gap between classical and quantum approaches to magnetotransport in such systems.

  10. Direct Measurement of the Band Structure of a Buried Two-Dimensional Electron Gas

    DEFF Research Database (Denmark)

    Miwa, Jill; Hofmann, Philip; Simmons, Michelle Y.

    2013-01-01

    We directly measure the band structure of a buried two dimensional electron gas (2DEG) using angle resolved photoemission spectroscopy. The buried 2DEG forms 2 nm beneath the surface of p-type silicon, because of a dense delta-type layer of phosphorus n-type dopants which have been placed there...

  11. Model of two-dimensional electron gas formation at ferroelectric interfaces

    Energy Technology Data Exchange (ETDEWEB)

    Aguado-Puente, P.; Bristowe, N. C.; Yin, B.; Shirasawa, R.; Ghosez, Philippe; Littlewood, P. B.; Artacho, Emilio

    2015-07-01

    The formation of a two-dimensional electron gas at oxide interfaces as a consequence of polar discontinuities has generated an enormous amount of activity due to the variety of interesting effects it gives rise to. Here, we study under what circumstances similar processes can also take place underneath ferroelectric thin films. We use a simple Landau model to demonstrate that in the absence of extrinsic screening mechanisms, a monodomain phase can be stabilized in ferroelectric films by means of an electronic reconstruction. Unlike in the LaAlO3/SrTiO3 heterostructure, the emergence with thickness of the free charge at the interface is discontinuous. This prediction is confirmed by performing first-principles simulations of free-standing slabs of PbTiO3. The model is also used to predict the response of the system to an applied electric field, demonstrating that the two-dimensional electron gas can be switched on and off discontinuously and in a nonvolatile fashion. Furthermore, the reversal of the polarization can be used to switch between a two-dimensional electron gas and a two-dimensional hole gas, which should, in principle, have very different transport properties. We discuss the possible formation of polarization domains and how such configuration competes with the spontaneous accumulation of free charge at the interfaces.

  12. Magnetization of a two-dimensional electron gas with a spin-orbit interaction

    International Nuclear Information System (INIS)

    Hatano, Naomichi; Shirasaki, Ryoen; Nakamura, Hiroaki

    2006-04-01

    We argue that a two-dimensional electron gas with a spin-orbit interaction is magnetized when a voltage is applied with the Fermi level tuned to be in the energy gap. The magnetization is an indication of spin-carrying currents due to the spin-orbit interaction. (author)

  13. Model for ballistic spin-transport in ferromagnet/two-dimensional electron gas/ferromagnet structures

    NARCIS (Netherlands)

    Schapers, T; Nitta, J; Heersche, HB; Takayanagi, H

    The spin dependent conductance of a ferromagnet/two-dimensional electron gas ferromagnet structure is theoretically examined in the ballistic transport regime. It is shown that the spin signal can be improved considerably by making use of the spin filtering effect of a barrier at the ferromagnet

  14. Spin-polarized transport in a two-dimensional electron gas with interdigital-ferromagnetic contacts

    DEFF Research Database (Denmark)

    Hu, C.-M.; Nitta, Junsaku; Jensen, Ane

    2001-01-01

    Ferromagnetic contacts on a high-mobility, two-dimensional electron gas (2DEG) in a narrow gap semiconductor with strong spin-orbit interaction are used to investigate spin-polarized electron transport. We demonstrate the use of magnetized contacts to preferentially inject and detect specific spi...

  15. Pixel-based analysis of comprehensive two-dimensional gas chromatograms (color plots) of petroleum

    DEFF Research Database (Denmark)

    Furbo, Søren; Hansen, Asger B.; Skov, Thomas

    2014-01-01

    We demonstrate how to process comprehensive two-dimensional gas chromatograms (GC × GC chromatograms) to remove nonsample information (artifacts), including background and retention time shifts. We also demonstrate how this, combined with further reduction of the influence of irrelevant informati...

  16. Analysis of host-cell proteins in biotherapeutic proteins by comprehensive online two-dimensional liquid chromatography/mass spectrometry

    OpenAIRE

    Doneanu, Catalin E; Xenopoulos, Alex; Fadgen, Keith; Murphy, Jim; Skilton, St. John; Prentice, Holly; Stapels, Martha; Chen, Weibin

    2012-01-01

    Assays for identification and quantification of host-cell proteins (HCPs) in biotherapeutic proteins over 5 orders of magnitude in concentration are presented. The HCP assays consist of two types: HCP identification using comprehensive online two-dimensional liquid chromatography coupled with high resolution mass spectrometry (2D-LC/MS), followed by high-throughput HCP quantification by liquid chromatography, multiple reaction monitoring (LC-MRM). The former is described as a “discovery” assa...

  17. De Haas-van Alphen effect of a two-dimensional ultracold atomic gas

    Science.gov (United States)

    Farias, B.; Furtado, C.

    2016-01-01

    In this paper, we show how the ultracold atom analogue of the two-dimensional de Haas-van Alphen effect in electronic condensed matter systems can be induced by optical fields in a neutral atomic system. The interaction between the suitable spatially varying laser fields and tripod-type trapped atoms generates a synthetic magnetic field which leads the particles to organize themselves in Landau levels. Initially, with the atomic gas in a regime of lowest Landau level, we display the oscillatory behaviour of the atomic energy and its derivative with respect to the effective magnetic field (B) as a function of 1/B. Furthermore, we estimate the area of the Fermi circle of the two-dimensional atomic gas.

  18. The static and dynamic screening of power loss of a two-dimensional electron gas

    Science.gov (United States)

    Bennett, C.; Balkan, N.; Tanatar, B.; Celik, H.; Cankurtaran, M.

    1998-07-01

    Experimental results concerning the well-width dependence of the acoustic-phonon-assisted energy relaxation of a two-dimensional electron gas in GaAs/Ga1 - xAlxAs quantum-well structures are compared with theoretical models that involve piezoelectric and deformation-potential scattering and the effects of static and dynamic screening of the electron-acoustic phonon interaction. It is shown that screening only slightly modifies the predictions of the approximate calculations.

  19. Interaction-induced huge magnetoresistance in a high mobility two-dimensional electron gas

    Energy Technology Data Exchange (ETDEWEB)

    Bockhorn, L.; Haug, R. J. [Institut für Festkörperphysik, Leibniz Universität Hannover, D-30167 Hannover (Germany); Gornyi, I. V. [Institut für Nanotechnologie, Karlsruher Institut of Technology, D-76021 Karlsruhe (Germany); Schuh, D. [Institut für Experimentelle und Angewandte Physik, Universität Regensburg, D-93053 Regensburg (Germany); Wegscheider, W. [ETH Zürich (Switzerland)

    2013-12-04

    A strong negative magnetoresistance is observed in a high-mobility two-dimensional electron gas in a GaAs/Al{sub 0.3}Ga{sub 0.7}As quantum well. We discuss that the negative magnetoresistance consists of a small peak induced by a combination of two types of disorder and a huge magnetoresistance explained by the interaction correction to the conductivity for mixed disorder.

  20. Curvature-tuned InAs-based shells containing two-dimensional electron gas

    Energy Technology Data Exchange (ETDEWEB)

    Mutilin, S V; Vorobyova, Ju S; Vorob' ev, A B; Putyato, M A; Prinz, V Ya, E-mail: s.mutilin@gmail.com [AV Rzhanov Institute of Semiconductor Physics, 630090, acad. Lavrentyev ave., 13, Novosibirsk (Russian Federation)

    2011-09-14

    Conducting InAs/AlSb/GaSb shells of curvature radius {approx}10 {mu}m are fabricated on GaSb (1 0 0) substrates. In the InAs quantum well, the shells are shown to contain a two-dimensional electron gas. Controlled tuning of the curvature of the formed shells in excess of three times is demonstrated. The sequence of fabrication steps for forming curvature-tuned InAs-based shells with quantum well is described.

  1. Affinity selection-based two-dimensional chromatography coupled with high-performance liquid chromatography-mass spectrometry for discovering xanthine oxidase inhibitors from Radix Salviae Miltiorrhizae.

    Science.gov (United States)

    Fu, Yu; Mo, Hua-Yan; Gao, Wen; Hong, Jia-Ying; Lu, Jun; Li, Ping; Chen, Jun

    2014-08-01

    Xanthine oxidase (XOD) is a key oxidative enzyme to the pathogenesis of hyperuricemia and certain diseases induced by excessive reactive oxygen species. XOD inhibitors could provide an important therapeutic approach to treat such diseases. A new method using affinity selection-based two-dimensional chromatography coupled with liquid chromatography-mass spectrometry was developed for the online screening of potential XOD inhibitors from Radix Salviae Miltiorrhizae. Based on our previous study, the two-dimensional, turbulent-flow chromatography (TFC) was changed to a mixed-mode anion-exchange/reversed-phase column and one reversed-phase column. The developed method was validated to be selective and sensitive for screening XOD-binding compounds, especially weak acidic ones, in the extracts. Three salvianolic acids were screened from the Radix Salviae Miltiorrhizae extract via the developed method. The XOD inhibitory activities of salvianolic acid C and salvianolic acid A were confirmed, and their inhibitory modes were measured. Salvianolic acid C exhibited potent XOD inhibitory activity with an IC(50) of 9.07 μM. This work demonstrated that the developed online, two-dimensional TFC/LC-MS method was effective in discovering the binding affinity of new compounds from natural extracts for target proteins, even at low concentrations.

  2. Kinetic Theory of a Confined Quasi-Two-Dimensional Gas of Hard Spheres

    Directory of Open Access Journals (Sweden)

    J. Javier Brey

    2017-02-01

    Full Text Available The dynamics of a system of hard spheres enclosed between two parallel plates separated a distance smaller than two particle diameters is described at the level of kinetic theory. The interest focuses on the behavior of the quasi-two-dimensional fluid seen when looking at the system from above or below. In the first part, a collisional model for the effective two-dimensional dynamics is analyzed. Although it is able to describe quite well the homogeneous evolution observed in the experiments, it is shown that it fails to predict the existence of non-equilibrium phase transitions, and in particular, the bimodal regime exhibited by the real system. A critical revision analysis of the model is presented , and as a starting point to get a more accurate description, the Boltzmann equation for the quasi-two-dimensional gas has been derived. In the elastic case, the solutions of the equation verify an H-theorem implying a monotonic tendency to a non-uniform steady state. As an example of application of the kinetic equation, here the evolution equations for the vertical and horizontal temperatures of the system are derived in the homogeneous approximation, and the results compared with molecular dynamics simulation results.

  3. Kinetic theory model for the flow of a simple gas from a two-dimensional nozzle

    Science.gov (United States)

    Riley, B. R.; Scheller, K. W.

    1989-01-01

    A system of nonlinear integral equations equivalent to the Krook kinetic equation for the steady state is the mathematical basis used to develop a computer code to model the flowfields for low-thrust two-dimensional nozzles. The method of characteristics was used to solve numerically by an iteration process the approximated Boltzmann equation for the number density, temperature, and velocity profiles of a simple gas as it exhausts into a vacuum. Results predict backscatter and show the effect of the inside wall boundary layer on the flowfields external to the nozzle.

  4. Spin injection into a two-dimensional electron gas using inter-digital-ferromagnetic contacts

    DEFF Research Database (Denmark)

    Hu, C.M.; Nitta, J.; Jensen, Ane

    2002-01-01

    We present a model that describes the spin injection across a single interface with two electrodes. The spin-injection rate across a typical hybrid junction made of ferromagnet (FM) and a two-dimensional electron gas (2DEG) is found at the percentage level. We perforin spin-injection-detection ex......-injection-detection experiment on devices with two ferromagnetic contacts on a 2DEG confined in an InAs quantum well. A spin-injection rate of 4.5% is estimated from the measured magnetoresistance....

  5. Two dimensional radial gas flows in atmospheric pressure plasma-enhanced chemical vapor deposition

    Science.gov (United States)

    Kim, Gwihyun; Park, Seran; Shin, Hyunsu; Song, Seungho; Oh, Hoon-Jung; Ko, Dae Hong; Choi, Jung-Il; Baik, Seung Jae

    2017-12-01

    Atmospheric pressure (AP) operation of plasma-enhanced chemical vapor deposition (PECVD) is one of promising concepts for high quality and low cost processing. Atmospheric plasma discharge requires narrow gap configuration, which causes an inherent feature of AP PECVD. Two dimensional radial gas flows in AP PECVD induces radial variation of mass-transport and that of substrate temperature. The opposite trend of these variations would be the key consideration in the development of uniform deposition process. Another inherent feature of AP PECVD is confined plasma discharge, from which volume power density concept is derived as a key parameter for the control of deposition rate. We investigated deposition rate as a function of volume power density, gas flux, source gas partial pressure, hydrogen partial pressure, plasma source frequency, and substrate temperature; and derived a design guideline of deposition tool and process development in terms of deposition rate and uniformity.

  6. Shear viscosity and spin-diffusion coefficient of a two-dimensional Fermi gas

    DEFF Research Database (Denmark)

    Bruun, Georg

    2012-01-01

    Using kinetic theory, we calculate the shear viscosity and the spin-diffusion coefficient as well as the associated relaxation times for a two-component Fermi gas in two dimensions, as a function of temperature, coupling strength, polarization, and mass ratio of the two components. It is demonstr......Using kinetic theory, we calculate the shear viscosity and the spin-diffusion coefficient as well as the associated relaxation times for a two-component Fermi gas in two dimensions, as a function of temperature, coupling strength, polarization, and mass ratio of the two components....... It is demonstrated that the minimum value of the viscosity decreases with the mass ratio, since Fermi blocking becomes less efficient. We furthermore analyze recent experimental results for the quadrupole mode of a two-dimensional gas in terms of viscous damping, obtaining a qualitative agreement using no fitting...

  7. Room Temperature Gas Sensing of Two-Dimensional Titanium Carbide (MXene).

    Science.gov (United States)

    Lee, Eunji; VahidMohammadi, Armin; Prorok, Barton C; Yoon, Young Soo; Beidaghi, Majid; Kim, Dong-Joo

    2017-10-25

    Wearable gas sensors have received lots of attention for diagnostic and monitoring applications, and two-dimensional (2D) materials can provide a promising platform for fabricating gas sensors that can operate at room temperature. In the present study, the room temperature gas-sensing performance of Ti 3 C 2 T x nanosheets was investigated. 2D Ti 3 C 2 T x (MXene) sheets were synthesized by removal of Al atoms from Ti 3 AlC 2 (MAX phases) and were integrated on flexible polyimide platforms with a simple solution casting method. The Ti 3 C 2 T x sensors successfully measured ethanol, methanol, acetone, and ammonia gas at room temperature and showed a p-type sensing behavior. The fabricated sensors showed their highest and lowest response toward ammonia and acetone gas, respectively. The limit of detection of acetone gas was theoretically calculated to be about 9.27 ppm, presenting better performance compared to other 2D material-based sensors. The sensing mechanism was proposed in terms of the interactions between the majority charge carriers of Ti 3 C 2 T x and gas species.

  8. Analysis of host-cell proteins in biotherapeutic proteins by comprehensive online two-dimensional liquid chromatography/mass spectrometry.

    Science.gov (United States)

    Doneanu, Catalin E; Xenopoulos, Alex; Fadgen, Keith; Murphy, Jim; Skilton, St John; Prentice, Holly; Stapels, Martha; Chen, Weibin

    2012-01-01

    Assays for identification and quantification of host-cell proteins (HCPs) in biotherapeutic proteins over 5 orders of magnitude in concentration are presented. The HCP assays consist of two types: HCP identification using comprehensive online two-dimensional liquid chromatography coupled with high resolution mass spectrometry (2D-LC/MS), followed by high-throughput HCP quantification by liquid chromatography, multiple reaction monitoring (LC-MRM). The former is described as a "discovery" assay, the latter as a "monitoring" assay. Purified biotherapeutic proteins (e.g., monoclonal antibodies) were digested with trypsin after reduction and alkylation, and the digests were fractionated using reversed-phase (RP) chromatography at high pH (pH 10) by a step gradient in the first dimension, followed by a high-resolution separation at low pH (pH 2.5) in the second dimension. As peptides eluted from the second dimension, a quadrupole time-of-flight mass spectrometer was used to detect the peptides and their fragments simultaneously by alternating the collision cell energy between a low and an elevated energy (MSE methodology). The MSE data was used to identify and quantify the proteins in the mixture using a proven label-free quantification technique ("Hi3" method). The same data set was mined to subsequently develop target peptides and transitions for monitoring the concentration of selected HCPs on a triple quadrupole mass spectrometer in a high-throughput manner (20 min LC-MRM analysis). This analytical methodology was applied to the identification and quantification of low-abundance HCPs in six samples of PTG1, a recombinant chimeric anti-phosphotyrosine monoclonal antibody (mAb). Thirty three HCPs were identified in total from the PTG1 samples among which 21 HCP isoforms were selected for MRM monitoring. The absolute quantification of three selected HCPs was undertaken on two different LC-MRM platforms after spiking isotopically labeled peptides in the samples. Finally

  9. Chemical warfare agent detection in complex environments with comprehensive two-dimensional gas chromatography

    Science.gov (United States)

    Reichenbach, Stephen E.; Ni, Mingtian; Kottapalli, Visweswara; Visvanathan, Arvind; Ledford, Edward B., Jr.; Oostdijk, John; Trap, Henk C.

    2003-08-01

    Comprehensive two-dimensional gas chromatography (GCxGC) is an emerging technology for chemical separation that provides an order-of-magnitude increase in separation capacity over traditional gas chromatography. GCxGC separates chemical species with two capillary columns interfaced by two-stage thermal desorption. Because GCxGC is comprehensive and has high separation capacity, it can perform multiple traditional analytical methods with a single analysis. GCxGC has great potential for a wide variety of environmental sensing applications, including detection of chemical warfare agents (CWA) and other harmful chemicals. This paper demonstrates separation of nerve agents sarin and soman from a matrix of gasoline and diesel fuel. Using a combination of an initial column separating on the basis of boiling point and a second column separating on the basis of polarity, GCxGC clearly separates the nerve agents from the thousands of other chemicals in the sample. The GCxGC data is visualized, processed, and analyzed as a two-dimensional digital image using a software system for GCxGC image processing developed at the University of Nebraska - Lincoln.

  10. Direct observation of two dimensional trace gas distributions with an airborne Imaging DOAS instrument

    Directory of Open Access Journals (Sweden)

    K.-P. Heue

    2008-11-01

    Full Text Available In many investigations of tropospheric chemistry information about the two dimensional distribution of trace gases on a small scale (e.g. tens to hundreds of metres is highly desirable. An airborne instrument based on imaging Differential Optical Absorption Spectroscopy has been built to map the two dimensional distribution of a series of relevant trace gases including NO2, HCHO, C2H2O2, H2O, O4, SO2, and BrO on a scale of 100 m.

    Here we report on the first tests of the novel aircraft instrument over the industrialised South African Highveld, where large variations in NO2 column densities in the immediate vicinity of several sources e.g. power plants or steel works, were measured. The observed patterns in the trace gas distribution are interpreted with respect to flux estimates, and it is seen that the fine resolution of the measurements allows separate sources in close proximity to one another to be distinguished.

  11. Comprehensive two-dimensional gas chromatography for biogas and biomethane analysis.

    Science.gov (United States)

    Hilaire, F; Basset, E; Bayard, R; Gallardo, M; Thiebaut, D; Vial, J

    2017-11-17

    The gas industry is going to be revolutionized by being able to generate bioenergy from biomass. The production of biomethane - a green substitute of natural gas - is growing in Europe and the United-States of America. Biomethane can be injected into the gas grid or used as fuel for vehicles after compression. Due to various biomass inputs (e.g. agricultural wastes, sludges from sewage treatment plants, etc.), production processes (e.g. anaerobic digestion, municipal solid waste (MSW) landfills), seasonal effects and purification processes (e.g. gas scrubbers, pressure swing adsorption, membranes for biogas upgrading), the composition and quality of biogas and biomethane produced is difficult to assess. All previous publications dealing with biogas analysis reported that hundreds of chemicals from ten chemical families do exist in trace amounts in biogas. However, to the best of our knowledge, no study reported a detailed analysis or the implementation of comprehensive two-dimensional gas chromatography (GC×GC) for biogas matrices. This is the reason why the benefit of implementing two-dimensional gas chromatography for the characterization of biogas and biomethane samples was evaluated. In a first step, a standard mixture of 89 compounds belonging to 10 chemical families, representative of those likely to be found, was used to optimize the analytical method. A set consisting of a non-polar and a polar columns, respectively in the first and the second dimension, was used with a modulation period of six seconds. Applied to ten samples of raw biogas, treated biogas and biomethane collected on 4 industrial sites (two MSW landfills, one anaerobic digester on a wastewater treatment plant and one agricultural biogas plant), this analytical method provided a "fingerprint" of the gases composition at the molecular level in all biogas and biomethane samples. Estimated limits of detection (far below the μgNm -3 ) coupled with the resolution of GC×GC allowed the comparison

  12. Terahertz Radiation Heterodyne Detector Using Two-Dimensional Electron Gas in a GaN Heterostructure

    Science.gov (United States)

    Karasik, Boris S.; Gill, John J.; Mehdi, Imran; Crawford, Timothy J.; Sergeev, Andrei V.; Mitin, Vladimir V.

    2012-01-01

    High-resolution submillimeter/terahertz spectroscopy is important for studying atmospheric and interstellar molecular gaseous species. It typically uses heterodyne receivers where an unknown (weak) signal is mixed with a strong signal from the local oscillator (LO) operating at a slightly different frequency. The non-linear mixer devices for this frequency range are unique and are not off-the-shelf commercial products. Three types of THz mixers are commonly used: Schottky diode, superconducting hot-electron bolometer (HEB), and superconductor-insulation-superconductor (SIS) junction. A HEB mixer based on the two-dimensional electron gas (2DEG) formed at the interface of two slightly dissimilar semiconductors was developed. This mixer can operate at temperatures between 100 and 300 K, and thus can be used with just passive radiative cooling available even on small spacecraft.

  13. Ballistic magnetotransport in a suspended two-dimensional electron gas with periodic antidot lattices

    Energy Technology Data Exchange (ETDEWEB)

    Zhdanov, E. Yu., E-mail: zhdanov@isp.nsc.ru; Pogosov, A. G.; Budantsev, M. V.; Pokhabov, D. A.; Bakarov, A. K. [Siberian Branch of the Russian Academy of Sciences, Rzhanov Institute of Semiconductor Physics (Russian Federation)

    2017-01-15

    The magnetoresistance of suspended semiconductor nanostructures with a two-dimensional electron gas structured by periodic square antidot lattices is studied. It is shown that the ballistic regime of electron transport is retained after detaching the sample from the substrate. Direct comparative analysis of commensurability oscillations of magnetoresistance and their temperature dependences in samples before and after suspension is performed. It is found that the temperature dependences are almost identical for non-suspended and suspended samples, whereas significant differences are observed in the nonlinear regime, caused by direct current passage. Commensurability oscillations in the suspended samples are more stable with respect to exposure to direct current, which can be presumably explained by electron–electron interaction enhancement after detaching nanostructures from the high-permittivity substrate.

  14. Automated multivariate analysis of comprehensive two-dimensional gas chromatograms of petroleum

    DEFF Research Database (Denmark)

    Skov, Søren Furbo

    Petroleum is an economically and industrially important resource. Crude oil must be refined before use to ensure suitable properties of the product. Among the processes used in this refining is distillation and desulfurization. In order to optimize these processes, it is essential to understand...... them. Comprehensive two-dimensional gas chromatography (GCGC) is a method for analyzing the volatile parts of a sample. It can separate hundreds or thousands of compounds based on their boiling point, polarity and polarizability. This makes it ideally suited for petroleum analysis. The number...... impossible to find it. For a special class of models, multi-way models, unique solutions often exist, meaning that the underlying phenomena can be found. I have tested this class of models on GCGC data from petroleum and conclude that more work is needed before they can be automated. I demonstrate how...

  15. A compact system for two-dimensional readout of Gas Electron Multiplier detectors

    International Nuclear Information System (INIS)

    Mindur, B; Dąbrowski, W; Fiutowski, T; Wiącek, P; Zielińska, A

    2013-01-01

    There is a growing interest in the use of Gas Electron Multiplier (GEM) and other micro-pattern gas detectors (MPGD) for two-dimensional (2-D) position sensitive measurements of photons or charged particles. A Gas Electron Multiplier Readout Chip (GEMROC) is an Application Specific Integrated Circuit (ASIC) dedicated for 2-D strip readout of GEM detectors. The ASICs deliver the amplitudes and time coordinates of the signals recorded on two sets of orthogonal strips. Timing information is used for finding coincidences of signals on two spatial coordinates while amplitude information is used to find the center of gravity for the cluster of signals belonging to the same detection event. In this paper we present a Field Programmable Gate Array (FPGA) based compact readout system dedicated for these ASICs. The readout system consists of two synchronized FPGA-ADC boards connected to four front-end boards, each one equipped with two GEMROCs. Both FPGAs are connected to a DAQ PC using separate Gigabit Ethernet links. The DAQ PC is equipped with a dedicated C++ based software, which is responsible for configuration of the FPGAs and ASICs settings, storing all the incoming data as well as for on-line/off-line data processing and visualization. The performance of the system is illustrated by test bench measurements.

  16. Photon drag investigations of current relaxation processes in a two-dimensional electron gas

    CERN Document Server

    Graf, S; Kohler, K U; Bachtold, W

    2000-01-01

    We have investigated the photon drag current that is excited by an infrared laser beam in the plane of the two-dimensional electron gas of GaAs/Al/sub 0.35/Ga/sub 0.65/As multiple-quantum-well systems. An analysis of the spectral response, measured with the picosecond infrared pulses of the wavelength-tunable free electron laser source FELIX, is presented for different doping schemes and examined as a function of temperature and intensity. The influence of the subband- selective scattering by a delta doping is explored, which demonstrates that the photon drag spectral response allows the determination of the momentum relaxation time ratio, R= tau /sub 1// tau /sub 2/, of the electrons in the ground and excited subbands. The relaxation time ratio is found to be surprisingly constant over a large temperature range. The variation of the ratio with intensity can be attributed to heating of the electron gas, whose temperature exceeds 1000 K at saturation intensity. (41 refs).

  17. Statistical problem of ideal gas in general two-dimensional regions

    Science.gov (United States)

    Song, Ci; Li, Wen-Du; Mwansa, Pardon; Zhang, Ping

    2015-09-01

    In this paper, based on the conformal mapping method and the perturbation theory, we develop a method to solve the statistical problem within general two-dimensional regions. We consider some examples and the numerical results and fitting results are given. We also give the thermodynamic quantities of the general two-dimensional regions, and compare the thermodynamic quantities of the different regions.

  18. The multi-mode modulator: A versatile fluidic device for two-dimensional gas chromatography.

    Science.gov (United States)

    Seeley, John V; Schimmel, Nicolaas E; Seeley, Stacy K

    2018-02-09

    A fluidic device called the multi-mode modulator (MMM) has been developed for use as a comprehensive two-dimensional gas chromatography (GC x GC) modulator. The MMM can be employed in a wide range of capacities including as a traditional heart-cutting device, a low duty cycle GC x GC modulator, and a full transfer GC x GC modulator. The MMM is capable of producing narrow component pulses (widths modulated components is confined to the interior of a joining capillary. The joining capillary dimensions and the position of the columns within the joining capillary can be optimized for the selected modulation mode. Furthermore, the joining capillary can be replaced easily and inexpensively if it becomes fouled due to sample matrix components or column bleed. The principles of operation of the MMM are described and its efficacy is demonstrated as a heart-cutting device and as a GC x GC modulator. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. Tunneling conductance of a two-dimensional electron gas with Dresselhaus spin-orbit coupling

    International Nuclear Information System (INIS)

    Srisongmuang, B.; Ka-oey, A.

    2012-01-01

    We theoretically studied the spin-dependent charge transport in a two-dimensional electron gas with Dresselhaus spin-orbit coupling (DSOC) and metal junctions. It is shown that the DSOC energy can be directly measured from the tunneling conductance spectrum. We found that spin polarization of the conductance in the propagation direction can be obtained by injecting from the DSOC system. We also considered the effect of the interfacial scattering barrier (both spin-flip and non-spin-flip scattering) on the overall conductance and the spin polarization of the conductance. It is found that the increase of spin-flip scattering can enhance the conductance under certain conditions. Moreover, both types of scattering can increase the spin polarization below the branches crossing of the energy band. - Highlights: → DSOC energy can be directly measured from tunneling conductance spectrum. → Spin polarization of conductance in the propagation direction can be obtained by injecting from DSOC system. → Both types of scattering can increase spin polarization.

  20. Unconventional superconductivity in a two-dimensional repulsive gas of fermions with spin-orbit coupling

    Science.gov (United States)

    Wang, Luyang; Vafek, Oskar

    2014-02-01

    We investigate the superconducting instability of a two-dimensional repulsive Fermi gas with Rashba spin-orbit coupling αR. Using renormalization group approach, we find the superconducting transition temperature as a function of the dimensionless ratio Θ=1}/{2}mαR2/EF where EF = 0 when the smaller Fermi surface shrinks to a (Dirac) point. The general trend is that superconductivity is enhanced as Θ increases, but in an intermediate regime Θ ∼ 0.1, a dome-like behavior appears. At a very small value of Θ, the angular momentum channel jz in which superconductivity occurs is quite high. With increasing Θ, jz decreases with a step of 2 down to jz = 6, after which we find the sequence jz = 6, 4, 6, 2, the last value of which continues to Θ → ∞. In an extended range of Θ, the superconducting gap predominantly resides on the large Fermi surface, while Josephson coupling induces a much smaller gap on the small Fermi surface. Below the superconducting transition temperature, we apply mean field theory to derive the self-consistent equations and find the condensation energies. The state with the lowest condensation energy is an unconventional superconducting state which breaks time-reversal symmetry, and in which singlet and triplet pairings are mixed. In general, these states are topologically nontrivial, and the Chern number of the state with total angular momentum jz is C = 2jz.

  1. Electrical detection of spin transport in Si two-dimensional electron gas systems

    Science.gov (United States)

    Chang, Li-Te; Fischer, Inga Anita; Tang, Jianshi; Wang, Chiu-Yen; Yu, Guoqiang; Fan, Yabin; Murata, Koichi; Nie, Tianxiao; Oehme, Michael; Schulze, Jörg; Wang, Kang L.

    2016-09-01

    Spin transport in a semiconductor-based two-dimensional electron gas (2DEG) system has been attractive in spintronics for more than ten years. The inherent advantages of high-mobility channel and enhanced spin-orbital interaction promise a long spin diffusion length and efficient spin manipulation, which are essential for the application of spintronics devices. However, the difficulty of making high-quality ferromagnetic (FM) contacts to the buried 2DEG channel in the heterostructure systems limits the potential developments in functional devices. In this paper, we experimentally demonstrate electrical detection of spin transport in a high-mobility 2DEG system using FM Mn-germanosilicide (Mn(Si0.7Ge0.3)x) end contacts, which is the first report of spin injection and detection in a 2DEG confined in a Si/SiGe modulation doped quantum well structure (MODQW). The extracted spin diffusion length and lifetime are l sf = 4.5 μm and {τ }{{s}}=16 {{ns}} at 1.9 K respectively. Our results provide a promising approach for spin injection into 2DEG system in the Si-based MODQW, which may lead to innovative spintronic applications such as spin-based transistor, logic, and memory devices.

  2. Comprehensive two-dimensional gas chromatography: A perspective on processes of modulation.

    Science.gov (United States)

    Tranchida, Peter Q

    2018-02-09

    The first comprehensive two-dimensional gas chromatography (GC×GC) experiment was reported about 25 years ago [J. Chromatogr. Sci. 29 (1991) 227-231]; the GC×GC process was made possible by the development of a transfer device, defined as modulator. The process of modulation enables the isolation of effluent segments from the first column, and their re-injection onto the second column, in a continuous and sequential manner throughout the analysis. Over the years, many types of modulation systems have been introduced, each with specific advantages and disadvantages. Cryogenic systems are, at present, the most popular devices and represent the most effective form of modulation. The present contribution is focused on possible future scenarios, with respect to modulation, and as a consequence related to comprehensive GC, in general. The development of new forms of modulation may open the road to a more widespread use of GC×GC technologies. Copyright © 2017 Elsevier B.V. All rights reserved.

  3. A two-dimensional position sensitive gas chamber with scanned charge transfer readout

    Energy Technology Data Exchange (ETDEWEB)

    Gomez, F. E-mail: faustgr@usc.es; Iglesias, A.; Lobato, R.; Mosquera, J.; Pardo, J.; Pena, J.; Pazos, A.; Pombar, M.; Rodriguez, A

    2003-10-21

    We have constructed and tested a two-dimensional position sensitive parallel-plate gas ionization chamber with scanned charge transfer readout. The scan readout method described here is based on the development of a new position-dependent charge transfer technique. It has been implemented by using gate strips perpendicularly oriented to the collector strips. This solution reduces considerably the number of electronic readout channels needed to cover large detector areas. The use of a 25 {mu}m thick kapton etched circuit allows high charge transfer efficiency with a low gating voltage, consequently needing a very simple commutating circuit. The present prototype covers 8x8 cm{sup 2} with a pixel size of 1.27x1.27 mm{sup 2}. Depending on the intended use and beam characteristics a smaller effective pixel is feasible and larger active areas are possible. This detector can be used for X-ray or other continuous beam intensity profile monitoring.

  4. Forensic profiling of sassafras oils based on comprehensive two-dimensional gas chromatography.

    Science.gov (United States)

    Schäffer, M; Gröger, T; Pütz, M; Zimmermann, R

    2013-06-10

    Safrole, the main compound in the essential oil of several plants of the Laurel family (Lauraceae), and its secondary product piperonylmethylketone are the predominantly used precursors for the illicit synthesis of 3,4-methylenedioxymethamphetamine (MDMA) which is, in turn, the most common active ingredient in Ecstasy tablets. Analytical methods with adequate capacity to identify links and origin of precursors, such as safrole, provide valuable information for drug-related police intelligence. Authentic sassafras oil samples from police seizures were subjected to comparative analysis based on their chemical profiles obtained by comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC × GC-TOFMS). The enhanced separation power and increased sensitivity of GC × GC allowed for the detection of minor compounds present in the essential oils which were of particular interest in case of very pure samples whose impurity profiles were not very pronounced. Discrimination of such samples was still possible even in the absence of characteristic main compounds. Copyright © 2013 Elsevier Ireland Ltd. All rights reserved.

  5. Reversed thermo-switchable molecular sieving membranes composed of two-dimensional metal-organic nanosheets for gas separation.

    Science.gov (United States)

    Wang, Xuerui; Chi, Chenglong; Zhang, Kang; Qian, Yuhong; Gupta, Krishna M; Kang, Zixi; Jiang, Jianwen; Zhao, Dan

    2017-02-16

    It is highly desirable to reduce the membrane thickness in order to maximize the throughput and break the trade-off limitation for membrane-based gas separation. Two-dimensional membranes composed of atomic-thick graphene or graphene oxide nanosheets have gas transport pathways that are at least three orders of magnitude higher than the membrane thickness, leading to reduced gas permeation flux and impaired separation throughput. Here we present nm-thick molecular sieving membranes composed of porous two-dimensional metal-organic nanosheets. These membranes possess pore openings parallel to gas concentration gradient allowing high gas permeation flux and high selectivity, which are proven by both experiment and molecular dynamics simulation. Furthermore, the gas transport pathways of these membranes exhibit a reversed thermo-switchable feature, which is attributed to the molecular flexibility of the building metal-organic nanosheets.

  6. Reversed thermo-switchable molecular sieving membranes composed of two-dimensional metal-organic nanosheets for gas separation

    Science.gov (United States)

    Wang, Xuerui; Chi, Chenglong; Zhang, Kang; Qian, Yuhong; Gupta, Krishna M.; Kang, Zixi; Jiang, Jianwen; Zhao, Dan

    2017-02-01

    It is highly desirable to reduce the membrane thickness in order to maximize the throughput and break the trade-off limitation for membrane-based gas separation. Two-dimensional membranes composed of atomic-thick graphene or graphene oxide nanosheets have gas transport pathways that are at least three orders of magnitude higher than the membrane thickness, leading to reduced gas permeation flux and impaired separation throughput. Here we present nm-thick molecular sieving membranes composed of porous two-dimensional metal-organic nanosheets. These membranes possess pore openings parallel to gas concentration gradient allowing high gas permeation flux and high selectivity, which are proven by both experiment and molecular dynamics simulation. Furthermore, the gas transport pathways of these membranes exhibit a reversed thermo-switchable feature, which is attributed to the molecular flexibility of the building metal-organic nanosheets.

  7. Many-body pairing in a two-dimensional Fermi gas

    Energy Technology Data Exchange (ETDEWEB)

    Neidig, Mathias

    2017-05-24

    This thesis reports on experiments conducted in a single layer, quasi two-dimensional, two-component ultracold Fermi gas in the strongly interacting regime. Ultracold gases can be used to simulate key aspects of more complicated systems like for example cuprates which show high-T{sub c} superconductivity. The momentum distribution of a sample of bosonic dimers in a quasi-2D square lattice geometry was measured to obtain the coherence properties. For shallow lattices, sharp peaks in the momentum distribution, indicating coherence, were observed at zero momentum as well as at positive and negative lattice momenta along each axis. For deeper lattices, heating impeded the ability to prepare a Mott-insulator. A spatially resolved radio-frequency spectroscopy was employed for a quasi-2D Fermi gas in the normal phase throughout the BEC-BCS crossover. The interaction induced energy shifts were measured in the strongly interacting region where they can be on the order of the Fermi energy and thus the local resolution is crucial. Furthermore, the onset of pairing in the strongly interacting region was measured as a function of temperature and it was shown that the fraction of free atoms decreases faster than expected from thermal non-interacting theory. At last, the pairing gap was measured using an imbalanced sample. On the BEC side it was found to be in very good agreement with two-body physics as expected. In the strongly interacting regime, however, a deviation from two-body physics indicates that here many-body effects play a role and thus further studies are required.

  8. Evaluation of a microfabricated thermal modulator for comprehensive two-dimensional microscale gas chromatography.

    Science.gov (United States)

    Kim, Sung-Jin; Serrano, Gustavo; Wise, Kensall D; Kurabayashi, Katsuo; Zellers, Edward T

    2011-07-15

    A microfabricated thermal modulator (μTM) designed for ultimate use in a comprehensive two-dimensional microscale gas chromatography (μGC × μGC) system is evaluated. The 2-stage device measures 13 mm (l) × 6 mm (w) × 0.5 mm (h) and consists of two interconnected serpentine etched-Si microchannels suspended from a thin Pyrex cap and wall-coated with PDMS (polydimethylsiloxane). The chip is mounted within a few tens of micrometers of a thermoelectric cooler that maintains both stages at a baseline temperature between -35 and -20 °C in order to focus analytes eluting from an upstream separation column. Each stage is heated to 210 °C sequentially at a rate as high as 2400 °C/s by independent thin-film resistors to inject the analytes in consecutive fractions to a downstream column, and then cooled at a rate as high as -168 °C/s. The average power dissipation is only ∼10 W for heating and 21 W for cooling without using consumable materials. In this study, the outlet of the μTM is connected directly to a flame ionization detector to assess its performance. Following a demonstration of basic operation, the modulated peak amplitude enhancement (PAE) and full-width-at-half-maximum (fwhm) are evaluated for members of a series of n-alkanes (C(6)-C(10)) as a function of the rim and stage temperatures; modulation period, phase, and offset; analyte concentration; and carrier-gas flow rate. A PAE as high as 50 and a fwhm as narrow as 90 ms are achieved for n-octane under optimized conditions.

  9. Thermodynamic-based retention time predictions of endogenous steroids in comprehensive two-dimensional gas chromatography.

    Science.gov (United States)

    Silva, Aline C A; Ebrahimi-Najafadabi, Heshmatollah; McGinitie, Teague M; Casilli, Alessandro; Pereira, Henrique M G; Aquino Neto, Francisco R; Harynuk, James J

    2015-05-01

    This work evaluates the application of a thermodynamic model to comprehensive two-dimensional gas chromatography (GC × GC) coupled with time-of-flight mass spectrometry for anabolic agent investigation. Doping control deals with hundreds of drugs that are prohibited in sports. Drug discovery in biological matrices is a challenging task that requires powerful tools when one is faced with the rapidly changing designer drug landscape. In this work, a thermodynamic model developed for the prediction of both primary and secondary retention times in GC × GC has been applied to trimethylsilylated hydroxyl (O-TMS)- and methoxime-trimethylsilylated carbonyl (MO-TMS)-derivatized endogenous steroids. This model was previously demonstrated on a pneumatically modulated GC × GC system, and is applied for the first time to a thermally modulated GC × GC system. Preliminary one-dimensional experiments allowed the calculation of thermodynamic parameters (ΔH, ΔS, and ΔC p ) which were successfully applied for the prediction of the analytes' interactions with the stationary phases of both the first-dimension column and the second-dimension column. The model was able to predict both first-dimension and second-dimension retention times with high accuracy compared with the GC × GC experimental measurements. Maximum differences of -8.22 s in the first dimension and 0.4 s in the second dimension were encountered for the O-TMS derivatives of 11β-hydroxyandrosterone and 11-ketoetiocholanolone, respectively. For the MO-TMS derivatives, the largest discrepancies were from testosterone (9.65 ) for the first-dimension retention times and 11-keto-etiocholanolone (0.4 s) for the second-dimension retention times.

  10. Comprehensive two-dimensional gas chromatographic separations with a microfabricated thermal modulator.

    Science.gov (United States)

    Serrano, Gustavo; Paul, Dibyadeep; Kim, Sung-Jin; Kurabayashi, Katsuo; Zellers, Edward T

    2012-08-21

    Rapid, comprehensive two-dimensional gas chromatographic (GC × GC) separations by use of a microfabricated midpoint thermal modulator (μTM) are demonstrated, and the effects of various μTM design and operating parameters on performance are characterized. The two-stage μTM chip consists of two interconnected spiral etched-Si microchannels (4.2 and 2.8 cm long) with a cross section of 250 × 140 μm(2), an anodically bonded Pyrex cap, and a cross-linked wall coating of poly(dimethylsiloxane) (PDMS). Integrated heaters provide rapid, sequential heating of each μTM stage, while a proximate, underlying thermoelectric cooler provides continual cooling. The first-dimension column used for GC × GC separations was a 6 m long, 250 μm i.d. capillary with a PDMS stationary phase, and the second-dimension column was a 0.5 m long, 100 μm i.d. capillary with a poly(ethylene glycol) phase. Using sets of five to seven volatile test compounds (boiling point ≤174 °C), the effects of the minimum (T(min)) and maximum (T(max)) modulation temperature, stage heating lag/offset (O(s)), modulation period (P(M)), and volumetric flow rate (F) on the quality of the separations were evaluated with respect to several performance metrics. Best results were obtained with a T(min) = -20 °C, T(max) = 210 °C, O(s) = 600 ms, P(M) = 6 s, and F = 0.9 mL/min. Replicate modulated peak areas and retention times were reproducible to <5%. A structured nine-component GC × GC chromatogram was produced, and a 21 component separation was achieved in <3 min. The potential for creating portable μGC × μGC systems is discussed.

  11. Second dimension column ensemble pressure tuning in comprehensive two-dimensional gas chromatography.

    Science.gov (United States)

    Sharif, Khan M; Kulsing, Chadin; Junior, Ademario I da Silva; Marriott, Philip J

    2018-02-09

    A pressure tunable (PT) coupled column ensemble has been implemented for the second dimension ( 2 D) separation in comprehensive two dimensional gas chromatography (GC×PTGC). This process requires two columns to be connected by a pressure junction, as a replacement for a single narrow bore, short column in 2 D. Various 2 D 1 and 2 D 2 columns may be selected to provide complementary selectivity (polarity) compared to the 1 D column. The tunable residence time arising from differential pressure drop in each 2 D column results in a tunable fractional contribution of each column in the 2 D separation. A sample mixture comprising different chemical classes, including alkanes and alcohols, is used to identify the feasibility and extent of selectivity tuning possible in GC×PTGC. The column length is also varied due to the imposed challenge of wraparound in the PT coupled column system as pressures are adjusted in the 2 D separation. Different experimental parameters, stationary phase materials and column lengths have been applied to investigate and understand the separation behaviour of the 2 D PT coupled column GC×GC system. Results are discussed considering analyte retention time, peak width, linear velocity and the contribution of each 2 D column. A specific and unexpected example of GC×GC separation was demonstrated where the peak positions of polar and apolar compounds could almost swap their 2 D retention position by application of PT. Kerosene was analysed as an example of complex sample analysis by GC×PTGC system. This process is shown to be a practical approach for altering different stationary phase selectivities in a single 2 D arrangement in GC×GC. Copyright © 2017 Elsevier B.V. All rights reserved.

  12. Collective modes of a two-dimensional spin-1/2 Fermi gas in a harmonic trap

    DEFF Research Database (Denmark)

    Baur, Stefan; Vogt, Enrico; Köhl, Michael

    2013-01-01

    We derive analytical expressions for the frequency and damping of the lowest collective modes of a two-dimensional Fermi gas using kinetic theory. For strong coupling, we furthermore show that pairing correlations overcompensate the effects of Pauli blocking on the collision rate for a large range...

  13. Attempt to unravel the composition of toxaphene by comprehensive two-dimensional gas chromatography with selective detection

    NARCIS (Netherlands)

    Korytar, P.; Stee, van L.L.P.; Leonards, P.E.G.; Boer, de J.; Brinkman, U.A.Th.

    2003-01-01

    Comprehensive two-dimensional gas chromatography (GCxGC) coupled with micro electron-capture and time-of-flight mass spectrometric (TOF-MS) detection has been used to analyse technical toxaphene. An HP-1xHT-8 column combination yielded highly structured chromatograms and revealed a complex mixture

  14. Characterization of lipids in complex samples using comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry

    NARCIS (Netherlands)

    Jover, E.; Adahchour, M.; Bayona, J.M.; Vreuls, R.J.J.; Brinkman, U.A.T.

    2005-01-01

    Most lipids are a complex mixture of classes of compounds such as fatty acids, fatty alcohols, diols, sterols and hydroxy acids. In this study, the suitability of comprehensive two-dimensional gas chromatography coupled to a time-of-light mass spectrometer is studied for lipid characterization in

  15. Local Ion Signatures (LIS) for the examination of comprehensive two-dimensional gas chromatography applied to fire debris analysis

    NARCIS (Netherlands)

    Lopatka, Martin; Sampat, Andjoe A.; Jonkers, Steffan; Adutwum, Lawrence A.; Mol, Hans G.J.; Weg, van der Guido; Harynuk, James J.; Schoenmakers, Peter J.; Asten, van Arian; Sjerps, Marjan J.; Vivó-Truyols, Gabriel

    2017-01-01

    Forensic examination of fire debris evidence is a notoriously difficult analytical task due to the complexity and variability of sample composition. The use of comprehensive two-dimensional gas chromatography with mass spectrometry detection (GC × GC–MS) allows the coupling of orthogonal

  16. Specialized Gas Chromatography--Mass Spectrometry Systems for Clinical Chemistry.

    Science.gov (United States)

    Gochman, Nathan; And Others

    1979-01-01

    A discussion of the basic design and characteristics of gas chromatography-mass spectrometry systems used in clinical chemistry. A comparison of three specific systems: the Vitek Olfax IIA, Hewlett-Packard HP5992, and Du Pont DP-102 are included. (BB)

  17. Note: Interpolation for evaluation of a two-dimensional spatial profile of plasma densities at low gas pressures

    International Nuclear Information System (INIS)

    Oh, Se-Jin; Kim, Young-Chul; Chung, Chin-Wook

    2011-01-01

    An interpolation algorithm for the evaluation of the spatial profile of plasma densities in a cylindrical reactor was developed for low gas pressures. The algorithm is based on a collisionless two-dimensional fluid model. Contrary to the collisional case, i.e., diffusion fluid model, the fitting algorithm depends on the aspect ratio of the cylindrical reactor. The spatial density profile of the collisionless fitting algorithm is presented in two-dimensional images and compared with the results of the diffusion fluid model.

  18. Oxygen speciation in upgraded fast pyrolysis bio-oils by comprehensive two-dimensional gas chromatography.

    Science.gov (United States)

    Omais, Badaoui; Crepier, Julien; Charon, Nadège; Courtiade, Marion; Quignard, Alain; Thiébaut, Didier

    2013-04-21

    Biomass fast pyrolysis is considered as a promising route to produce liquid for the transportation field from a renewable resource. However, the derived bio-oils are mainly oxygenated (45-50%w/w O on a wet basis) and contain almost no hydrocarbons. Therefore, upgrading is necessary to obtain a liquid with lower oxygen content and characterization of oxygenated compounds in these products is essential to assist conversion reactions. For this purpose, comprehensive two-dimensional gas chromatography (GC × GC) can be investigated. Oxygen speciation in such matrices is hampered by the large diversity of oxygenated families and the complexity of the hydrocarbon matrix. Moreover, response factors must be taken into account for oxygenate quantification as the Flame Ionisation Detector (FID) response varies when a molecule contains heteroatoms. To conclude, no distillation cuts were accessible and the analysis had to cover a large range of boiling points (30-630 °C). To take up this analytical challenge, a thorough optimization approach was developed. In fact, four GC × GC column sets were investigated to separate oxygenated compounds from the hydrocarbon matrix. Both model mixtures and the upgraded biomass flash pyrolysis oil were injected using GC × GC-FID to reach a suitable chromatographic separation. The advantages and drawbacks of each column combination for oxygen speciation in upgraded bio-oils are highlighted in this study. Among the four sets, an original polar × semi-polar column combination was selected and enabled the identification by GC × GC-ToF/MS of more than 40 compounds belonging to eight chemical families: ketones, furans, alcohols, phenols, carboxylic acids, guaiacols, anisols, and esters. For quantification purpose, the GC × GC-FID chromatogram was divided into more than 60 blobs corresponding to the previously identified analyte and hydrocarbon zones. A database associating each blob to a molecule and its specific response factor (determined

  19. Interpreting comprehensive two-dimensional gas chromatography using peak topography maps with application to petroleum forensics.

    Science.gov (United States)

    Ghasemi Damavandi, Hamidreza; Sen Gupta, Ananya; Nelson, Robert K; Reddy, Christopher M

    2016-01-01

    Comprehensive two-dimensional gas chromatography [Formula: see text] provides high-resolution separations across hundreds of compounds in a complex mixture, thus unlocking unprecedented information for intricate quantitative interpretation. We exploit this compound diversity across the [Formula: see text] topography to provide quantitative compound-cognizant interpretation beyond target compound analysis with petroleum forensics as a practical application. We focus on the [Formula: see text] topography of biomarker hydrocarbons, hopanes and steranes, as they are generally recalcitrant to weathering. We introduce peak topography maps (PTM) and topography partitioning techniques that consider a notably broader and more diverse range of target and non-target biomarker compounds compared to traditional approaches that consider approximately 20 biomarker ratios. Specifically, we consider a range of 33-154 target and non-target biomarkers with highest-to-lowest peak ratio within an injection ranging from 4.86 to 19.6 (precise numbers depend on biomarker diversity of individual injections). We also provide a robust quantitative measure for directly determining "match" between samples, without necessitating training data sets. We validate our methods across 34 [Formula: see text] injections from a diverse portfolio of petroleum sources, and provide quantitative comparison of performance against established statistical methods such as principal components analysis (PCA). Our data set includes a wide range of samples collected following the 2010 Deepwater Horizon disaster that released approximately 160 million gallons of crude oil from the Macondo well (MW). Samples that were clearly collected following this disaster exhibit statistically significant match [Formula: see text] using PTM-based interpretation against other closely related sources. PTM-based interpretation also provides higher differentiation between closely correlated but distinct sources than obtained using

  20. Doppler Velocimetry of Current Driven Spin Helices in a Two-Dimensional Electron Gas

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Luyi [Univ. of California, Berkeley, CA (United States)

    2013-05-17

    Spins in semiconductors provide a pathway towards the development of spin-based electronics. The appeal of spin logic devices lies in the fact that the spin current is even under time reversal symmetry, yielding non-dissipative coupling to the electric field. To exploit the energy-saving potential of spin current it is essential to be able to control it. While recent demonstrations of electrical-gate control in spin-transistor configurations show great promise, operation at room temperature remains elusive. Further progress requires a deeper understanding of the propagation of spin polarization, particularly in the high mobility semiconductors used for devices. This dissertation presents the demonstration and application of a powerful new optical technique, Doppler spin velocimetry, for probing the motion of spin polarization at the level of 1 nm on a picosecond time scale. We discuss experiments in which this technique is used to measure the motion of spin helices in high mobility n-GaAs quantum wells as a function of temperature, in-plane electric field, and photoinduced spin polarization amplitude. We find that the spin helix velocity changes sign as a function of wave vector and is zero at the wave vector that yields the largest spin lifetime. This observation is quite striking, but can be explained by the random walk model that we have developed. We discover that coherent spin precession within a propagating spin density wave is lost at temperatures near 150 K. This finding is critical to understanding why room temperature operation of devices based on electrical gate control of spin current has so far remained elusive. We report that, at all temperatures, electron spin polarization co-propagates with the high-mobility electron sea, even when this requires an unusual form of separation of spin density from photoinjected electron density. Furthermore, although the spin packet co-propagates with the two-dimensional electron gas, spin diffusion is strongly

  1. Hot-Electron Gallium Nitride Two Dimensional Electron Gas Nano-bolometers For Advanced THz Spectroscopy

    Science.gov (United States)

    Ramaswamy, Rahul

    Two-dimensional electron gas (2DEG) in semiconductor heterostructures was identified as a promising medium for hot-electron bolometers (HEB) in the early 90s. Up until now all research based on 2DEG HEBs is done using high mobility AlGaAs/GaAs heterostructures. These systems have demonstrated very good performance, but only in the sub terahertz (THz) range. However, above ˜0.5 THz the performance of AlGaAs/GaAs detectors drastically deteriorates. It is currently understood, that detectors fabricated from standard AlGaAs/GaAs heterostructures do not allow for reasonable coupling to THz radiation while maintaining high conversion efficiency. In this work we have developed 2DEG HEBs based on disordered Gallium Nitride (GaN) semiconductor, that operate at frequencies beyond 1THz at room temperature. We observe strong free carrier absorption at THz frequencies in our disordered 2DEG film due to Drude absorption. We show the design and fabrication procedures of novel micro-bolometers having ultra-low heat capacities. In this work the mechanism of 2DEG response to THz radiation is clearly identified as bolometric effect through our direct detection measurements. With optimal doping and detector geometry, impedances of 10--100 O have been achieved, which allow integration of these devices with standard THz antennas. We also demonstrate performance of the antennas used in this work in effectively coupling THz radiation to the micro-bolometers through polarization dependence and far field measurements. Finally heterodyne mixing due to hot electrons in the 2DEG micro-bolometer has been performed at sub terahertz frequencies and a mixing bandwidth greater than 3GHz has been achieved. This indicates that the characteristic cooling time in our detectors is fast, less than 50ps. Due to the ultra-low heat capacity; these detectors can be used in a heterodyne system with a quantum cascade laser (QCL) as a local oscillator (LO) which typically provides output powers in the micro

  2. Strongly anisotropic spin-orbit splitting in a two-dimensional electron gas

    DEFF Research Database (Denmark)

    Michiardi, Matteo; Bianchi, Marco; Dendzik, Maciej

    2015-01-01

    Near-surface two-dimensional electron gases on the topological insulator Bi$_2$Te$_2$Se are induced by electron doping and studied by angle-resolved photoemission spectroscopy. A pronounced spin-orbit splitting is observed for these states. The $k$-dependent splitting is strongly anisotropic...

  3. Comprehensive two-dimensional gas chromatography for fast characterization of oil contamination

    International Nuclear Information System (INIS)

    Van De Weghe, H.; Vanermen, G.; Gemoets, J.; Lookman, R.; Bertels, D.

    2005-01-01

    Most analytical methods for the characterization of oil contamination rely on gas chromatography. Capillary GC offers a high separation power (peak capacity typically 100 - 500), and by using a boiling point column a volatility based distribution is obtained. However, petrochemical mixtures like mineral oil easily contain more then 5000 compounds, and capillary GC does not succeed in separating such mixtures up to the level of individual components. Analytical results are therefore limited to a classification into boiling point (or equivalent-carbon) fractions. Recent methods refined the classification by fractionation in aromatic and aliphatic hydrocarbons prior to GC-analysis (TPH method, Weisman 1998), and by incorporating water solubility (TTE and OK method, for a detailed description we refer to the Consoil 2005 lecture by R. Lookman 'Oil characterization: assessment of composition, degradation and remediation potential of total petroleum hydrocarbons in soil'). However, besides analytical difficulties and time consuming protocols related with these methods, the resulting classification still remains coarse and the various groups are not univocally chemically identified. Recently, comprehensive two-dimensional GC (GCXGC) was introduced. This technique combines two GC-columns with different separation mechanisms. The two columns are connected by a modulator, a device that traps, focuses and re-injects the peaks that elute from the first column into the second column. Each peak from the first column (representing a number of overlapping peaks) is further separated on the second column. The very high separation power of GCXGC (peak capacity 2000 - 10000) is ideal for the analysis of complex mixtures like mineral oil. Another important feature is the generation of structured chromatograms. Isomers appear as distinct groups in the chromatogram as a result of their similar interaction with the 2D-column phase. For chemical identification comprehensive GC can be

  4. Tunable bilayer two-dimensional electron gas in LaAlO3/SrTiO3 superlattices

    International Nuclear Information System (INIS)

    Ma, H. J. Harsan; Annadi, A.; Zeng, S. W.; Ariando; Huang, Z.; Lü, W. M.; Wong, L. M.; Wang, S. J.; Venkatesan, T.

    2014-01-01

    We report magnetotransport properties of double heterointerfaces in LaAlO 3 /SrTiO 3 /LaAlO 3 /SrTiO 3 (001) (LAO/STO/LAO/STO). A strong nonlinearity in the Hall resistivity is found when the temperature is below 80 K. This effect is attributed to multichannel conduction of interfacial charges generated in double heterostructures of LAO/STO where two-dimensional electron gas (2DEG) is produced. The multichannel conduction is confirmed by back gating modulation of Hall effect. Our result suggests the possibility to achieve coupled bilayer 2DEG layers in LAO/STO superlattices.

  5. Giant Andreev Backscattering through a Quantum Point Contact Coupled via a Disordered Two-Dimensional Electron Gas to Superconductors

    International Nuclear Information System (INIS)

    den Hartog, S.G.; van Wees, B.J.; Klapwijk, T.M.; Nazarov, Y.V.; Borghs, G.

    1997-01-01

    We have investigated the superconducting-phase-modulated reduction in the resistance of a ballistic quantum point contact (QPC) connected via a disordered two-dimensional electron gas (2DEG) to superconductors. We show that this reduction is caused by coherent Andreev backscattering of holes through the QPC, which increases monotonically by reducing the bias voltage to zero. In contrast, the magnitude of the phase-dependent resistance of the disordered 2DEG displays a nonmonotonic reentrant behavior versus bias voltage. copyright 1997 The American Physical Society

  6. A new model for two-dimensional numerical simulation of pseudo-2D gas-solids fluidized beds

    Energy Technology Data Exchange (ETDEWEB)

    Li, Tingwen; Zhang, Yongmin

    2013-10-11

    Pseudo-two dimensional (pseudo-2D) fluidized beds, for which the thickness of the system is much smaller than the other two dimensions, is widely used to perform fundamental studies on bubble behavior, solids mixing, or clustering phenomenon in different gas-solids fluidization systems. The abundant data from such experimental systems are very useful for numerical model development and validation. However, it has been reported that two-dimensional (2D) computational fluid dynamic (CFD) simulations of pseudo-2D gas-solids fluidized beds usually predict poor quantitative agreement with the experimental data, especially for the solids velocity field. In this paper, a new model is proposed to improve the 2D numerical simulations of pseudo-2D gas-solids fluidized beds by properly accounting for the frictional effect of the front and back walls. Two previously reported pseudo-2D experimental systems were simulated with this model. Compared to the traditional 2D simulations, significant improvements in the numerical predictions have been observed and the predicted results are in better agreement with the available experimental data.

  7. Study of pressure vessels for micro-strip-gas-counters as two-dimensional neutron position sensitive detectors

    International Nuclear Information System (INIS)

    Yamagishi, Hideshi; Kaneko, Junichi

    2001-01-01

    The development of two-dimensional position sensitive neutron detectors that have performances of a fast response and a very small space-resolution are required for various neutron scattering experiments using high-intensity pulse-neutron sources in a high-intensity proton accelerator facility. We put forward the development of a micro-strip gas counter (MSGC) filled with helium-3 gas as the two-dimensional position sensitive neutron detector. The MSGC requests a pressure vessel that withstands gas pressure of 5-10 atm. For obtainment of a small neutron-attenuation, the pressure vessel requires a neutron-window that is made thin wall and has small cross sections of absorption and scattering for low energy neutrons. We have studied and compared three kinds of neutron-windows for manufacturing the pressure vessel. After the study, we were able to design the pressure vessel with neutron-window thickness of 2 mm on conditions that are a window area of 100 x 100 mm, material of aluminum and inner pressure of 10 atm. (author)

  8. Subnanometer Two-Dimensional Graphene Oxide Channels for Ultrafast Gas Sieving.

    Science.gov (United States)

    Shen, Jie; Liu, Gongping; Huang, Kang; Chu, Zhenyu; Jin, Wanqin; Xu, Nanping

    2016-03-22

    Two-dimensional (2D) materials with atomic thickness and extraordinary physicochemical properties exhibit unique mass transport behaviors, enabling them as emerging nanobuilding blocks for separation membranes. Engineering 2D materials into membrane with subnanometer apertures for precise molecular sieving remains a great challenge. Here, we report rational-designing external forces to precisely manipulate nanoarchitecture of graphene oxide (GO)-assembled 2D channels with interlayer height of ∼0.4 nm for fast transporting and selective sieving gases. The external forces are synergistic to direct the GO nanosheets stacking so as to realize delicate size-tailoring of in-plane slit-like pores and plane-to-plane interlayer-galleries. The 2D channels endow GO membrane with excellent molecular-sieving characteristics that offer 2-3 orders of magnitude higher H2 permeability and 3-fold enhancement in H2/CO2 selectivity compared with commercial membranes. Formation mechanism of 2D channels is proposed on the basis of the driving forces, nanostructures, and transport behaviors.

  9. Coupled two-dimensional edge plasma and neutral gas modeling of tokamak scrape-off-layers

    International Nuclear Information System (INIS)

    Maingi, R.

    1992-08-01

    The objective of this study is to devise a detailed description of the tokamak scrape-off-layer (SOL), which includes the best available models of both the plasma and neutral species and the strong coupling between the two in many SOL regimes. A good estimate of both particle flux and heat flux profiles at the limiter/divertor target plates is desired. Peak heat flux is one of the limiting factors in determining the survival probability of plasma-facing-components at high power levels. Plate particle flux affects the neutral flux to the pump, which determines the particle exhaust rate. A technique which couples a two-dimensional (2-D) plasma and a 2-D neutral transport code has been developed (coupled code technique), but this procedure requires large amounts of computer time. Relevant physics has been added to an existing two-neutral-species model which takes the SOL plasma/neutral coupling into account in a simple manner (molecular physics model), and this model is compared with the coupled code technique mentioned above. The molecular physics model is benchmarked against experimental data from a divertor tokamak (DIII-D), and a similar model (single-species model) is benchmarked against data from a pump-limiter tokamak (Tore Supra). The models are then used to examine two key issues: free-streaming-limits (ion energy conduction and momentum flux) and the effects of the non-orthogonal geometry of magnetic flux surfaces and target plates on edge plasma parameter profiles

  10. Gas dynamics of H II regions. II. Two-dimensional axisymmetric calculations

    International Nuclear Information System (INIS)

    Bodenheimer, P.; Tenorio-Tagle, G.; Yorke, H.W.

    1979-01-01

    The evolution of H II regions is calculated with a two-dimensional hydrodynamic numerical procedure under the assumption that the exciting star is born within a cool molecular cloud whose density is about 10 3 particles cm -3 . As the ionization of the cloud's edge is completed, a large pressure gradient is set up and ionized cloud material expands into the ionized low-density (1 particle cm -3 ) intercloud medium, with velocities larger than 30 km s -1 .The calculations are made under the simplifying assumptions that (i) within the H II region, ionization equilibrium holds at all times, (ii) the ionization front is a discontinuity, thus its detailed structure is not calculated, (iii) the temperature of each region (H II region, neutral cloud, and intercloud medium) is constant in time, (iv) all ionizing photons come radially from the exciting star. Four cases are calculated and compared with observations: (1) the edge of the cloud is overrun by a supersonic ionization front, (2) the initial Stroemgren sphere surrounding the star lies deep inside the cloud, thus the cloud's edge is ionized by a subsonic ionization front, (3) the ionization front breaks through two opposite faces of the same cloud simultaneously, (4) the flow encounters an isolated globule of density 10 3 particles cm -3 shortly after emerging from the molecular cloud.The phenomena here considered show how evolving H II regions are an important input of kinetic energy to the interstellar medium

  11. A low noise ASIC for two dimensional neutron gas detector with performance of high spatial resolution (Contract research)

    International Nuclear Information System (INIS)

    Yamagishi, Hideshi; Toh, Kentaro; Nakamura, Tatsuya; Sakasai, Kaoru; Soyama, Kazuhiko

    2012-02-01

    An ASD-ASIC (Amplifier-Shaper-Discriminator ASIC) with fast response and low noise performances has been designed for two-dimensional position sensitive neutron gas detectors (InSPaD). The InSPaD is a 2D neutron detector system with 3 He gas and provides a high spatial resolution by making distinction between proton and triton particles generated in the gas chamber. The new ASD-ASIC is required to have very low noise, a wide dynamic range, good output linearity and high counting rate. The new ASD-ASIC has been designed by using CMOS and consisted of 64-channel ASDs, a 16-channel multiplexer with LVTTL drivers and sum amplifier system for summing all analog signals. The performances were evaluated by the Spice simulation. It was confirmed that the new ASD-ASIC had very low noise performance, wide dynamic range and fast signal processing functions. (author)

  12. Second sound in a two-dimensional Bose gas: From the weakly to the strongly interacting regime

    Science.gov (United States)

    Ota, Miki; Stringari, Sandro

    2018-03-01

    Using Landau's theory of two-fluid hydrodynamics, we investigate first and second sounds propagating in a two-dimensional (2D) Bose gas. We study the temperature and interaction dependence of both sound modes and show that their behavior exhibits a deep qualitative change as the gas evolves from the weakly interacting to the strongly interacting regime. Special emphasis is placed on the jump of both sounds at the Berezinskii-Kosterlitz-Thouless transition, caused by the discontinuity of the superfluid density. We find that the excitation of second sound through a density perturbation becomes weaker and weaker as the interaction strength increases as a consequence of the decrease in the thermal expansion coefficient. Our results could be relevant for future experiments on the propagation of sound on the Bose-Einstein condensate (BEC) side of the BCS-BEC crossover of a 2D superfluid Fermi gas.

  13. Ballistic and diffusive dynamics in a two-dimensional ideal gas of macroscopic chaotic Faraday waves.

    Science.gov (United States)

    Welch, Kyle J; Hastings-Hauss, Isaac; Parthasarathy, Raghuveer; Corwin, Eric I

    2014-04-01

    We have constructed a macroscopic driven system of chaotic Faraday waves whose statistical mechanics, we find, are surprisingly simple, mimicking those of a thermal gas. We use real-time tracking of a single floating probe, energy equipartition, and the Stokes-Einstein relation to define and measure a pseudotemperature and diffusion constant and then self-consistently determine a coefficient of viscous friction for a test particle in this pseudothermal gas. Because of its simplicity, this system can serve as a model for direct experimental investigation of nonequilibrium statistical mechanics, much as the ideal gas epitomizes equilibrium statistical mechanics.

  14. A two-dimensional Fermi gas in the BEC-BCS crossover

    Energy Technology Data Exchange (ETDEWEB)

    Ries, Martin Gerhard

    2016-01-21

    This thesis reports on the preparation of a 2D Fermi gas in the BEC-BCS crossover and the observation of the BKT transition into a quasi long-range ordered superfluid phase. The pair momentum distribution of the gas is probed by means of a matter-wave focusing technique which relies on time-of-flight evolution in a weak harmonic potential. This distribution holds the coherence properties of the gas. The quasi long-range ordered phase manifests itself as a sharp low-momentum peak. The temperature where it forms is identified as the transition temperature. By tuning the temperature and the interaction strength, the phase diagram of the 2D Fermi gas in the BEC-BCS crossover is mapped out. The phase coherence is investigated in a self-interference experiment. Furthermore, algebraic decay of correlations is observed in the trap average of the first order correlation function, which is obtained from the Fourier transform of the pair momentum distribution. This is in qualitative agreement with predictions of homogeneous theory for the superfluid phase in a 2D gas. The presented results provide a foundation for future experimental and theoretical studies of strongly correlated 2D Fermi gases. They might thus help to elucidate complex systems such as the electron gas in high-T{sub c} superconductors.

  15. Analysis of cave atmospheres by comprehensive two-dimensional gas chromatography (GC×GC with flame ionization detection (FID

    Directory of Open Access Journals (Sweden)

    Ryan C. Blase

    2015-03-01

    Full Text Available In this paper, we describe a simple method for sampling, pre-concentrating, and separating volatile and semi-volatile components from two different cave atmospheres. Sampling is performed by capturing a volume of cave atmosphere in a Tedlar bag or Suma canister for sample storage and transport back to the laboratory. Loading a portion of the sample on a multi-bed sorption trap allows for sample pre-concentration prior to separation and detection of components on a comprehensive two-dimensional gas chromatograph (GC×GC. Comparison of two Texas caves reveals the power of comprehensive two-dimensional gas chromatography (GC×GC for volatile separation and detection, and to our knowledge marks the first use of GC×GC for the analysis of cave atmospheres. Analysis of the results revealed 138 and 146 chromatographic signals over an S/N threshold of 500 and direct comparison of the two samples revealed 50 identical chromatographic signals. This study is a first step toward demonstrating the ability of GC×GC to separate the complex volatiles and semi-volatiles in the cave atmosphere as a fingerprinting tool.

  16. Manifestly Hermitian semiclassical expansion for the one-particle density matrix of a two-dimensional Fermi gas

    Science.gov (United States)

    Bencheikh, K.; van Zyl, B. P.; Berkane, K.

    2016-08-01

    The semiclassical ℏ expansion of the one-particle density matrix for a two-dimensional Fermi gas is calculated within the Wigner transform method of B. Grammaticos and A. Voros [Ann. Phys. (N.Y.) 123, 359 (1979), 10.1016/0003-4916(79)90343-9], originally developed in the context of nuclear physics. The method of Grammaticos and Voros has the virtue of preserving both the Hermiticity and idempotency of the density matrix to all orders in the ℏ expansion. As a topical application, we use our semiclassical expansion to go beyond the local-density approximation for the construction of the total dipole-dipole interaction energy functional of a two-dimensional, spin-polarized dipolar Fermi gas. We find a finite, second-order gradient correction to the Hartree-Fock energy, which takes the form ɛ (∇ρ ) 2/√{ρ } , with ɛ being small (|ɛ |≪1 ) and negative. We test the quality of the corrected energy by comparing it with the exact results available for harmonic confinement. Even for small particle numbers, the gradient correction to the dipole-dipole energy provides a significant improvement over the local-density approximation.

  17. Low cost, robust, in-house hardware for heart cutting two-dimensional gas chromatography

    CSIR Research Space (South Africa)

    Apps, P

    2006-06-01

    Full Text Available Natural materials are so complex that no single column can separate all of the components. Heart cutting 2-D GC (GC-GC) using a Deans switch provides maximum separation, but the requisite gas flow configurations have earned a reputation for being...

  18. Quantum spin-glass transition in the two-dimensional electron gas

    Indian Academy of Sciences (India)

    Home; Journals; Pramana – Journal of Physics; Volume 58; Issue 2 ... Spin glasses; quantum phase transition; ferromagnetism; electron gas. ... We argue that a quantum transition involving the destruction of the spin-glass order in an applied in-plane magnetic field offers a natural explanation of some features of recent ...

  19. Two dimensional laser induced fluorescence in the gas phase: a spectroscopic tool for studying molecular spectroscopy and dynamics

    Science.gov (United States)

    Gascooke, Jason R.; Lawrance, Warren D.

    2017-11-01

    Two dimensional laser induced fluorescence (2D-LIF) extends the usual laser induced fluorescence technique by adding a second dimension, the wavelength at which excited states emit, thereby significantly enhancing the information that can be extracted. It allows overlapping absorption features, whether they arise from within the same molecule or from different molecules in a mixture, to be associated with their appropriate "parent" state and/or molecule. While the first gas phase version of the technique was published a decade ago, the technique is in its infancy, having been exploited by only a few groups to date. However, its potential in gas phase spectroscopy and dynamics is significant. In this article we provide an overview of the technique and illustrate its potential with examples, with a focus on those utilising high resolution in the dispersed fluorescence dimension.

  20. The statistical mechanics of the classical two-dimensional Coulomb gas is exactly solved

    International Nuclear Information System (INIS)

    Samaj, L

    2003-01-01

    The model under consideration is a classical 2D Coulomb gas of pointlike positive and negative unit charges, interacting via a logarithmic potential. In the whole stability range of temperatures, the equilibrium statistical mechanics of this fluid model is exactly solvable via an equivalence with the integrable 2D sine-Gordon field theory. The exact solution includes the bulk thermodynamics, special cases of the surface thermodynamics and the large-distance asymptotic behaviour of the two-body correlation functions

  1. Joint approximate diagonalization of eigenmatrices as a high-throughput approach for analysis of hyphenated and comprehensive two-dimensional gas chromatographic data.

    Science.gov (United States)

    Zarghani, Maryam; Parastar, Hadi

    2017-11-17

    The objective of the present work is development of joint approximate diagonalization of eigenmatrices (JADE) as a member of independent component analysis (ICA) family, for the analysis of gas chromatography-mass spectrometry (GC-MS) and comprehensive two-dimensional gas chromatography-mass spectrometry (GC×GC-MS) data to address incomplete separation problem occurred during the analysis of complex sample matrices. In this regard, simulated GC-MS and GC×GC-MS data sets with different number of components, different degree of overlap and noise were evaluated. In the case of simultaneous analysis of multiple samples, column-wise augmentation for GC-MS and column-wise super-augmentation for GC×GC-MS was used before JADE analysis. The performance of JADE was evaluated in terms of statistical parameters of lack of fit (LOF), mutual information (MI) and Amari index as well as analytical figures of merit (AFOMs) obtained from calibration curves. In addition, the area of feasible solutions (AFSs) was calculated by two different approaches of MCR-BANDs and polygon inflation algorithm (FACPACK). Furthermore, JADE performance was compared with multivariate curve resolution-alternating least squares (MCR-ALS) and other ICA algorithms of mean-field ICA (MFICA) and mutual information least dependent component analysis (MILCA). In all cases, JADE could successfully resolve the elution and spectral profiles in GC-MS and GC×GC-MS data with acceptable statistical and calibration parameters and their solutions were in AFSs. To check the applicability of JADE in real cases, JADE was used for resolution and quantification of phenanthrene and anthracene in aromatic fraction of heavy fuel oil (HFO) analyzed by GC×GC-MS. Surprisingly, pure elution and spectral profiles of target compounds were properly resolved in the presence of baseline and interferences using JADE. Once more, the performance of JADE was compared with MCR-ALS in real case. On this matter, the mutual information

  2. A high density two-dimensional electron gas in an oxide heterostructure on Si (001)

    Energy Technology Data Exchange (ETDEWEB)

    Jin, E. N.; Kornblum, L.; Kumah, D. P.; Zou, K.; Walker, F. J. [Center for Research on Interface Structures and Phenomena and Department of Applied Physics, Yale University, New Haven, Connecticut 06511 (United States); Broadbridge, C. C. [Center for Research on Interface Structures and Phenomena and Department of Applied Physics, Yale University, New Haven, Connecticut 06511 (United States); Department of Physics, Southern Connecticut State University, 501 Crescent Street, New Haven, Connecticut 06515 (United States); Ngai, J. H. [Department of Physics, The University of Texas at Arlington, Arlington, Texas 76019 (United States); Ahn, C. H. [Center for Research on Interface Structures and Phenomena and Department of Applied Physics, Yale University, New Haven, Connecticut 06511 (United States); Department of Mechanical Engineering and Materials Science, Yale University, New Haven, Connecticut 06511 (United States)

    2014-11-01

    We present the growth and characterization of layered heterostructures comprised of LaTiO{sub 3} and SrTiO{sub 3} epitaxially grown on Si (001). Magnetotransport measurements show that the sheet carrier densities of the heterostructures scale with the number of LaTiO{sub 3}/SrTiO{sub 3} interfaces, consistent with the presence of an interfacial 2-dimensional electron gas (2DEG) at each interface. Sheet carrier densities of 8.9 × 10{sup 14} cm{sup −2} per interface are observed. Integration of such high density oxide 2DEGs on silicon provides a bridge between the exceptional properties and functionalities of oxide 2DEGs and microelectronic technologies.

  3. Two dimensional numerical simulation of gas discharges: comparison between particle-in-cell and FCT techniques

    Energy Technology Data Exchange (ETDEWEB)

    Soria-Hoyo, C; Castellanos, A [Departamento de Electronica y Electromagnetismo, Facultad de Fisica, Universidad de Sevilla, Avda. Reina Mercedes s/n, 41012 Sevilla (Spain); Pontiga, F [Departamento de Fisica Aplicada II, EUAT, Universidad de Sevilla, Avda. Reina Mercedes s/n, 41012 Sevilla (Spain)], E-mail: cshoyo@us.es

    2008-10-21

    Two different numerical techniques have been applied to the numerical integration of equations modelling gas discharges: a finite-difference flux corrected transport (FD-FCT) technique and a particle-in-cell (PIC) technique. The PIC technique here implemented has been specifically designed for the simulation of 2D electrical discharges using cylindrical coordinates. The development and propagation of a streamer between two parallel electrodes has been used as a convenient test to compare the performance of both techniques. In particular, the phase velocity of the cathode directed streamer has been used to check the internal consistency of the numerical simulations. The results obtained from the two techniques are in reasonable agreement with each other, and both techniques have proved their ability to follow the high gradients of charge density and electric field present in this type of problems. Moreover, the streamer velocities predicted by the simulation are in accordance with the typical experimental values.

  4. Tomography for two-dimensional gas temperature distribution based on TDLAS

    Science.gov (United States)

    Luo, Can; Wang, Yunchu; Xing, Fei

    2018-03-01

    Based on tunable diode laser absorption spectroscopy (TDLAS), the tomography is used to reconstruct the combustion gas temperature distribution. The effects of number of rays, number of grids, and spacing of rays on the temperature reconstruction results for parallel ray are researched. The reconstruction quality is proportional to the ray number. The quality tends to be smoother when the ray number exceeds a certain value. The best quality is achieved when η is between 0.5 and 1. A virtual ray method combined with the reconstruction algorithms is tested. It is found that virtual ray method is effective to improve the accuracy of reconstruction results, compared with the original method. The linear interpolation method and cubic spline interpolation method, are used to improve the calculation accuracy of virtual ray absorption value. According to the calculation results, cubic spline interpolation is better. Moreover, the temperature distribution of a TBCC combustion chamber is used to validate those conclusions.

  5. Two-Dimensional Metal-Organic Framework Nanosheets for Membrane-Based Gas Separation.

    Science.gov (United States)

    Peng, Yuan; Li, Yanshuo; Ban, Yujie; Yang, Weishen

    2017-08-07

    Metal-organic framework (MOF) nanosheets could serve as ideal building blocks of molecular sieve membranes owing to their structural diversity and minimized mass-transfer barrier. To date, discovery of appropriate MOF nanosheets and facile fabrication of high performance MOF nanosheet-based membranes remain as great challenges. A modified soft-physical exfoliation method was used to disintegrate a lamellar amphiprotic MOF into nanosheets with a high aspect ratio. Consequently sub-10 nm-thick ultrathin membranes were successfully prepared, and these demonstrated a remarkable H 2 /CO 2 separation performance, with a separation factor of up to 166 and H 2 permeance of up to 8×10 -7  mol m -2  s -1  Pa -1 at elevated testing temperatures owing to a well-defined size-exclusion effect. This nanosheet-based membrane holds great promise as the next generation of ultrapermeable gas separation membrane. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Flow optimization in one-dimensional and comprehensive two-dimensional gas chromatography.

    Science.gov (United States)

    Blumberg, Leonid M

    2018-02-09

    Theoretical considerations of optimal flow in a GC column under different conditions are outlined from a single perspective, and numerical recommendations are provided. The optimal flow rate in a temperature programmed column is about 30% lower than its isothermal counterpart in the same column with the same carrier gas. A simplified calculation of recommended optimal or near optimal flow rate in a single column under different conditions is summarized in a single equation. In GC × GC, the primary column operates under temperature-programmed conditions while each secondary run is essentially isothermal. As a result, their flow optimization requirements are different. The complementary IDs (internal diameters) corresponding to equal optimal flow rates in both GC × GC columns should relate as 2 d = 0.7  ·1 d. Typical complementary ID pairs are tabulated. If choosing the complementary IDs is not an option, several ways to reconcile the difference in their optimal flow rates are considered. The most typical cases of the column mismatch are identified and their boundary conditions are formulated. The effect of the flow reconciliation in these column pairs on the performance of GC × GC analysis is evaluated. Copyright © 2017 Elsevier B.V. All rights reserved.

  7. Anisotropic Friedel oscillations in a two-dimensional electron gas with a Rashba-Dresselhaus spin-orbit interaction

    Science.gov (United States)

    Kozlov, I. V.; Kolesnichenko, Yu. A.

    2017-07-01

    We present a theoretical study of the spatial distribution of the local density of states (LDOS) and the local magnetization density (LMD) in the vicinity of a magnetic point-defect in a degenerate two-dimensional electron gas with a mixed Rashba-Dresselhaus spin-orbit coupling interaction (SOI). The dependence of the Friedel oscillations, which arise under these conditions, on the ratio of the SOI constants is investigated. We obtain asymptotic expressions for the oscillatory parts of the LDOS and the LMD, that are accurate for large distances from the defect. It is shown, that the Friedel oscillations are significantly anisotropic and contain several harmonics for certain ratios of the SOI constants. Period of the oscillations for directions along the symmetry axes of the Fermi contours are determined. Finally, we introduce a method for determining the values of the two SOI constants by measuring the period of the Friedel oscillations of the LDOS and the LMD for different harmonics.

  8. Current-induced spin polarization in a spin-polarized two-dimensional electron gas with spin-orbit coupling

    International Nuclear Information System (INIS)

    Wang, C.M.; Pang, M.Q.; Liu, S.Y.; Lei, X.L.

    2010-01-01

    The current-induced spin polarization (CISP) is investigated in a combined Rashba-Dresselhaus spin-orbit-coupled two-dimensional electron gas, subjected to a homogeneous out-of-plane magnetization. It is found that, in addition to the usual collision-related in-plane parts of CISP, there are two impurity-density-free contributions, arising from intrinsic and disorder-mediated mechanisms. The intrinsic parts of spin polarization are related to the Berry curvature, analogous with the anomalous and spin Hall effects. For short-range collision, the disorder-mediated spin polarizations completely cancel the intrinsic ones and the total in-plane components of CISP equal those for systems without magnetization. However, for remote disorders, this cancellation does not occur and the total in-plane components of CISP strongly depend on the spin-orbit interaction coefficients and magnetization for both pure Rashba and combined Rashba-Dresselhaus models.

  9. Development of an ultra-fast data-acquisition system for a two-dimensional microstrip gas chamber.

    Science.gov (United States)

    Ochi, A; Tanimori, T; Nishi, Y; Aoki, S; Nishi, Y

    1998-05-01

    A high-performance data-acquisition system has been developed in order to obtain time-resolved sequential images from a two-dimensional microstrip gas chamber (MSGC). This was achieved using fully digital processing with a synchronized pipeline method. Complex logical circuits for processing large numbers of signals are mounted on a small number of complex programmable logic devices. The system is operated with a 10 MHz synchronous clock, and has the capability of handling more than 3 x 10(6) counts s(-1) for asynchronous events. The system was examined using a 5 x 5 cm MSGC and the recently developed 10 x 10 cm MSGC (1024 outputs); the anticipated performances were achieved.

  10. Localization and oscillations of Majorana fermions in a two-dimensional electron gas coupled with d -wave superconductors

    Science.gov (United States)

    Ortiz, L.; Varona, S.; Viyuela, O.; Martin-Delgado, M. A.

    2018-02-01

    We study the localization and oscillation properties of the Majorana fermions that arise in a two-dimensional electron gas (2DEG) with spin-orbit coupling (SOC) and a Zeeman field coupled with a d -wave superconductor. Despite the angular dependence of the d -wave pairing, localization and oscillation properties are found to be similar to the ones seen in conventional s -wave superconductors. In addition, we study a microscopic lattice version of the previous system that can be characterized by a topological invariant. We derive its real space representation that involves nearest and next-to-nearest-neighbors pairing. Finally, we show that the emerging chiral Majorana fermions are indeed robust against static disorder. This analysis has potential applications to quantum simulations and experiments in high-Tc superconductors.

  11. Comprehensive two-dimensional gas chromatography combined to multivariate data analysis for detection of disease-resistant clones of Eucalyptus.

    Science.gov (United States)

    Hantao, Leandro Wang; Toledo, Bruna Regina; Ribeiro, Fabiana Alves de Lima; Pizetta, Marilia; Pierozzi, Caroline Geraldi; Furtado, Edson Luiz; Augusto, Fabio

    2013-11-15

    In this paper it is reported the use of the chromatographic profiles from volatile fractions of plant clones - in this case, hybrids of Eucalyptus grandis×Eucalyptus urophylla - to determine specimens susceptible to rust disease. The analytes were isolated by headspace solid phase microextraction (HS-SPME) and analyzed by comprehensive two-dimensional gas chromatography combined to fast quadrupole mass spectrometry (GC×GC-qMS). Parallel Factor Analysis (PARAFAC) was employed for estimate the correlation between the chromatographic profiles and resistance against Eucalyptus rust, after preliminary variable selection performed by Fisher ratio analysis. The proposed method allowed the differentiation between susceptible and non-susceptible clones and determination of three resistance biomarkers. This approach can be a valuable alternative for the otherwise time-consuming and labor-intensive methods commonly used. © 2013 Elsevier B.V. All rights reserved.

  12. A Study of Two Dimensional Tomography Reconstruction of Temperature and Gas Concentration in a Combustion Field Using TDLAS

    Directory of Open Access Journals (Sweden)

    Pengshuai Sun

    2017-09-01

    Full Text Available Based on tunable diode laser absorption spectroscopy (TDLAS, two-dimensional (2D distribution reconstructions of gas concentration and temperature are realized using an algebraic reconstruction technique (ART. The influence of the beam distribution and grid size on combustion field reconstruction is investigated to attain optimal reconstruction results with a limited number of beams. Under limited optical-path numbers, it shows that a better spatial resolution is attainable only when the laser beam paths are vertical and parallel to the symmetry axis of the combustion field. Furthermore, experiments with 16 beam paths using one and two flat flame combustion fields are carried out in different fuel-air equivalence ratios under room temperature. The results are in agreement with the simulation results, and the time resolution is less than 1 s.

  13. Gas Chromatography-Mass Spectroscopic (GC-MS) Analysis of n ...

    African Journals Online (AJOL)

    tuber-regium (synonym Pleurotus tuber regium) using gas chromatography-mass spectroscopic (GC-. MS) techniques. Methods: The n-hexane extract of the sclerotia ... Soxhlet extraction and analysed using gas chromatography-mass spectroscopic (MS) techniques. ..... Phytochemical composition of Pleurotus tuber regium.

  14. Clinical applications of gas chromatography and gas chromatography-mass spectrometry of steroids

    NARCIS (Netherlands)

    Wolthers, BG; Kraan, GPB

    1999-01-01

    This review article underlines the importance of gas chromatography-mass spectrometry (GC-MS) for determination of steroids in man. The use of steroids labelled with stable isotopes as internal standard and subsequent analysis by GC-MS yields up to now the only reliable measurement of steroids in

  15. Gas Chromatography-Mass Spectroscopy Study of tert-Butylarsine Stability and Purification

    Energy Technology Data Exchange (ETDEWEB)

    Bartram, M.E.; Breiland, W.G.; Bruskas, L.A.; Killeen, K.P.

    1999-07-20

    TBA (tert-butylarsine, H{sub 2}AsC(CH{sub 3}){sub 3}) has been demonstrated to be an effective arsenic precursor for the deposition of compound semiconductors such as GaAs by MOCVD (metal organic chemical vapor deposition). TBA is used as a liquid (bubbler) source in MOCVD and is a less toxic alternative to the more commonly used gaseous arsine (AsH{sub 3}). Materials and device performance using TBA have in many cases equaled or surpassed those using arsine. This includes the first observation of fractional quantum Hall behavior in a two dimensional electron gas structure grown by MOCVD. Despite the beneficial characteristics, the use of TBA in our laboratories has revealed some inconsistent behavior. Small pressure rises have been observed in the TBA bubbler sources when left unused over a period of many days. Measurements of the TBA partial pressure using UV absorption revealed that new absorption peaks could be observed after storage. The features of the absorption profile were insufficient to ascribe to a specific chemical species. Attempts to remove the gaseous impurities with liquid nitrogen freeze-pump-thaw techniques had limited success. Unfortunately, there is no published information on the room temperature decomposition of TBA. In this paper, we present a series of GCMS (gas chromatography-mass spectroscopy) analyses designed to determine the stability of TBA and identify its decomposition products in storage containers. The GCMS is also used to evaluate several methods for in-situ purification of TBA.

  16. Using comprehensive two-dimensional gas chromatography to explore the geochemistry of the Santa Barbara oil seeps

    Energy Technology Data Exchange (ETDEWEB)

    Reddy, Christopher; Nelson, Robert

    2013-03-27

    The development of comprehensive two-dimensional gas chromatography (GC x GC) has expanded the analytical window for studying complex mixtures like oil. Compared to traditional gas chromatography, this technology separates and resolves at least an order of magnitude more compounds, has a much larger signal to noise ratio, and sorts compounds based on their chemical class; hence, providing highly refined inventories of petroleum hydrocarbons in geochemical samples that was previously unattainable. In addition to the increased resolution afforded by GC x GC, the resulting chromatograms have been used to estimate the liquid vapor pressures, aqueous solubilities, octanol-water partition coefficients, and vaporization enthalpies of petroleum hydrocarbons. With these relationships, powerful and incisive analyses of phase-transfer processes affecting petroleum hydrocarbon mixtures in the environment are available. For example, GC x GC retention data has been used to quantitatively deconvolve the effects of phase transfer processes such as water washing and evaporation. In short, the positive attributes of GC x GC-analysis have led to a methodology that has revolutionized the analysis of petroleum hydrocarbons. Overall, this research has opened numerous fields of study on the biogeochemical "genetics" (referred to as petroleomics) of petroleum samples in both subsurface and surface environments. Furthermore, these new findings have already been applied to the behavior of oil at other seeps as well, for petroleum exploration and oil spill studies.

  17. Smart multi-channel two-dimensional micro-gas chromatography for rapid workplace hazardous volatile organic compounds measurement.

    Science.gov (United States)

    Liu, Jing; Seo, Jung Hwan; Li, Yubo; Chen, Di; Kurabayashi, Katsuo; Fan, Xudong

    2013-03-07

    We developed a novel smart multi-channel two-dimensional (2-D) micro-gas chromatography (μGC) architecture that shows promise to significantly improve 2-D μGC performance. In the smart μGC design, a non-destructive on-column gas detector and a flow routing system are installed between the first dimensional separation column and multiple second dimensional separation columns. The effluent from the first dimensional column is monitored in real-time and decision is then made to route the effluent to one of the second dimensional columns for further separation. As compared to the conventional 2-D μGC, the greatest benefit of the smart multi-channel 2-D μGC architecture is the enhanced separation capability of the second dimensional column and hence the overall 2-D GC performance. All the second dimensional columns are independent of each other, and their coating, length, flow rate and temperature can be customized for best separation results. In particular, there is no more constraint on the upper limit of the second dimensional column length and separation time in our architecture. Such flexibility is critical when long second dimensional separation is needed for optimal gas analysis. In addition, the smart μGC is advantageous in terms of elimination of the power intensive thermal modulator, higher peak amplitude enhancement, simplified 2-D chromatogram re-construction and potential scalability to higher dimensional separation. In this paper, we first constructed a complete smart 1 × 2 channel 2-D μGC system, along with an algorithm for automated control/operation of the system. We then characterized and optimized this μGC system, and finally employed it in two important applications that highlight its uniqueness and advantages, i.e., analysis of 31 workplace hazardous volatile organic compounds, and rapid detection and identification of target gas analytes from interference background.

  18. Discrete particle simulation of bubble and slug formation in a two-dimensional gas-fluidised bed: A hard-sphere approach.

    NARCIS (Netherlands)

    Hoomans, B.P.B.; Kuipers, J.A.M.; Briels, Willem J.; van Swaaij, Willibrordus Petrus Maria

    1996-01-01

    A discrete particle model of a gas-fluidised bed has been developed and in this the two-dimensional motion of the individual, spherical particles was directly calculated from the forces acting on them, accounting for the interaction between the particles and the interstitial gas phase. Our collision

  19. Two-dimensional simulation of the development of an inhomogeneous volume discharge in a Ne/Xe/HCl gas mixture

    International Nuclear Information System (INIS)

    Bychkov, Yu. I.; Yampolskaya, S. A.; Yastremskii, A. G.

    2013-01-01

    The kinetic processes accompanying plasma column formation in an inhomogeneous discharge in a Ne/Xe/HCl gas mixture at a pressure of 4 atm were investigated by using a two-dimensional model. Two cathode spots spaced by 0.7 cm were initiated by distorting the cathode surface at local points, which resulted in an increase in the field strength in the cathode region. Three regimes differing in the charging voltage, electric circuit inductance, and electric field strength at the local cathode points were considered. The spatiotemporal distributions of the discharge current; the electron density; and the densities of excited xenon atoms, HCl(v = 0) molecules in the ground state, and HCl(v > 0) molecules in vibrational levels were calculated. The development of the discharge with increasing the electron density from 10 4 to 10 16 cm −3 was analyzed, and three characteristic stages in the evolution of the current distribution were demonstrated. The width of the plasma column was found to depend on the energy deposited in the discharge. The width of the plasma column was found to decrease in inverse proportion to the deposited energy due to spatiotemporal variations in the rates of electron production and loss. The calculated dependences of the cross-sectional area of the plasma column on the energy deposited in the discharge agree with the experimental results.

  20. Detection of an extended human volatome with comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry.

    Science.gov (United States)

    Phillips, Michael; Cataneo, Renee N; Chaturvedi, Anirudh; Kaplan, Peter D; Libardoni, Mark; Mundada, Mayur; Patel, Urvish; Zhang, Xiang

    2013-01-01

    Comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry (GCxGC-TOF MS) has been proposed as a powerful new tool for multidimensional analysis of complex chemical mixtures. We investigated GCxGC-TOF MS as a new method for identifying volatile organic compounds (VOCs) in normal human breath. Samples of alveolar breath VOCs and ambient room air VOC were collected with a breath collection apparatus (BCA) onto separate sorbent traps from 34 normal healthy volunteers (mean age = 40 yr, SD = 17 yr, male/female = 19/15). VOCs were separated on two serial capillary columns separated by a cryogenic modulator, and detected with TOF MS. The first and second dimension columns were non-polar and polar respectively. BCA collection combined with GC×GC-TOF MS analysis identified approximately 2000 different VOCs in samples of human breath, many of which have not been previously reported. The 50 VOCs with the highest alveolar gradients (abundance in breath minus abundance in ambient room air) mostly comprised benzene derivatives, acetone, methylated derivatives of alkanes, and isoprene. Collection and analysis of breath VOCs with the BCA-GC×GC-TOF MS system extended the size of the detectable human volatile metabolome, the volatome, by an order of magnitude compared to previous reports employing one-dimensional GC-MS. The size of the human volatome has been under-estimated in the past due to coelution of VOCs in one-dimensional GC analytical systems.

  1. Durability-enhanced two-dimensional hole gas of C-H diamond surface for complementary power inverter applications.

    Science.gov (United States)

    Kawarada, Hiroshi; Yamada, Tetsuya; Xu, Dechen; Tsuboi, Hidetoshi; Kitabayashi, Yuya; Matsumura, Daisuke; Shibata, Masanobu; Kudo, Takuya; Inaba, Masafumi; Hiraiwa, Atsushi

    2017-02-20

    Complementary power field effect transistors (FETs) based on wide bandgap materials not only provide high-voltage switching capability with the reduction of on-resistance and switching losses, but also enable a smart inverter system by the dramatic simplification of external circuits. However, p-channel power FETs with equivalent performance to those of n-channel FETs are not obtained in any wide bandgap material other than diamond. Here we show that a breakdown voltage of more than 1600 V has been obtained in a diamond metal-oxide-semiconductor (MOS) FET with a p-channel based on a two-dimensional hole gas (2DHG). Atomic layer deposited (ALD) Al 2 O 3 induces the 2DHG ubiquitously on a hydrogen-terminated (C-H) diamond surface and also acts as both gate insulator and passivation layer. The high voltage performance is equivalent to that of state-of-the-art SiC planar n-channel FETs and AlGaN/GaN FETs. The drain current density in the on-state is also comparable to that of these two FETs with similar device size and V B .

  2. Towards chemical profiling of ignitable liquids with comprehensive two-dimensional gas chromatography: Exploring forensic application to neat white spirits.

    Science.gov (United States)

    Sampat, Andjoe A S; Lopatka, Martin; Vivó-Truyols, Gabriel; Schoenmakers, Peter J; van Asten, Arian C

    2016-10-01

    The application of GC×GC-FID and GC×GC-MS for the chemical analysis and profiling of neat white spirit is explored and the benefit of the enhanced peak capacity offered by comprehensive two-dimensional gas chromatography is demonstrated. An extensive sampling exercise was conducted throughout The Netherlands and the production and logistics in terms of bottling and distribution of white spirits were studied. An exploratory approach based on target-peak tables and principal component analysis was employed to study the brand-to-brand differences and production variations over time. Despite the complex chemical composition of white spirit samples this study shows that chemical variation during productions is actually quite limited. Hence care has to be taken with the chemical comparison for forensic purposes. Although some clustering was noticed on brand level, the large scale production process leads to a very consistent composition across stores and brands. However, because of the broad specifications of this commodity product, substantial chemical variation was found over time. This temporal discrimination could be of forensic value when considering white spirits supplies in individual households. Copyright © 2016 Elsevier Ireland Ltd. All rights reserved.

  3. Two-dimensional hydrodynamic lattice-gas simulations of binary immiscible and ternary amphiphilic fluid flow through porous media

    Science.gov (United States)

    Maillet; Coveney

    2000-08-01

    The behavior of two-dimensional binary and ternary amphiphilic fluids under flow conditions is investigated using a hydrodynamic lattice-gas model. After the validation of the model in simple cases (Poiseuille flow, Darcy's law for single component fluids), attention is focused on the properties of binary immiscible fluids in porous media. An extension of Darcy's law which explicitly admits a viscous coupling between the fluids is verified, and evidence of capillary effects is described. The influence of a third component, namely, surfactant, is studied in the same context. Invasion simulations have also been performed. The effect of the applied force on the invasion process is reported. As the forcing level increases, the invasion process becomes faster and the residual oil saturation decreases. The introduction of surfactant in the invading phase during imbibition produces new phenomena, including emulsification and micellization. At very low fluid forcing levels, this leads to the production of a low-resistance gel, which then slows down the progress of the invading fluid. At long times (beyond the water percolation threshold), the concentration of remaining oil within the porous medium is lowered by the action of surfactant, thus enhancing oil recovery. On the other hand, the introduction of surfactant in the invading phase during drainage simulations slows down the invasion process-the invading fluid takes a more tortuous path to invade the porous medium-and reduces the oil recovery (the residual oil saturation increases).

  4. Study on the calculating the second dimension retention index in comprehensive two-dimensional gas chromatography spectrometry

    International Nuclear Information System (INIS)

    Zhao Yaping; Zhang Jun; Wang Bing; Fang Aiqin; Zhang Xiang; Kim, Seong Ho; Bogdanov, Bogdan; McClain, Craig

    2012-01-01

    A method was developed to calculate the second dimension retention index of comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC × GC/TOF MS) data using n-alkanes as reference compounds. The retention times of the C 7 -C 31 alkanes acquired during 24 isothermal experiments cover the 0-6 s retention time area in the second dimension retention time space, which makes it possible to calculate the retention indices of target compounds from the corresponding retention time values without the extension of the retention space of the reference compounds. An empirical function was proposed to show the relationship among the second dimension retention time. the temperature of the second dimension column, and the carbon number of the n-alkanes. The proposed function is able to extend the second dimension retention time beyond the reference n-alkanes by increasing the carbon number. The extension of carbon numbers in reference n-alkanes up to two more carbon atoms introduces less than 10 retention index units (iu) of deviation. The effectiveness of using the proposed method was demonstrated by analyzing a mixture of compound standards in temperature programmed experiments using 6 different initial column temperatures. The standard deviation of the calculated retention index values of the compound standards fluctuated from 1 to 12 iu with a mean standard deviation of 5 iu. (authors)

  5. Comprehensive two-dimensional gas chromatographic profiling and chemometric interpretation of the volatile profiles of sweat in knit fabrics.

    Science.gov (United States)

    de la Mata, A Paulina; McQueen, Rachel H; Nam, Seo Lin; Harynuk, James J

    2017-03-01

    Human axillary sweat is a poorly explored biofluid within the context of metabolomics when compared to other fluids such as blood and urine. In this paper, we explore the volatile organic compounds emitted from two different types of fabric samples (cotton and polyester) which had been worn repeatedly during exercise by participants. Headspace solid-phase microextraction (SPME) and comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC×GC-TOFMS) were employed to profile the (semi)volatile compounds on the fabric. Principal component analysis models were applied to the data to aid in visualizing differences between types of fabrics, wash treatment, and the gender of the subject who had worn the fabric. Statistical tools included with commercial chromatography software (ChromaTOF) and a simple Fisher ratio threshold-based feature selection for model optimization are compared with a custom-written algorithm that uses cluster resolution as an objective function to maximize in a hybrid backward-elimination forward-selection approach for optimizing the chemometric models in an effort to identify some compounds that correlate to differences between fabric types. The custom algorithm is shown to generate better models than the simple Fisher ratio approach. Graphical Abstract A route from samples and questions to data and then answers.

  6. Tuning the conductivity threshold and carrier density of two-dimensional electron gas at oxide interfaces through interface engineering

    Directory of Open Access Journals (Sweden)

    H. J. Harsan Ma

    2015-08-01

    Full Text Available The two-dimensional electron gas (2DEG formed at the perovskite oxides heterostructures is of great interest because of its potential applications in oxides electronics and nanoscale multifunctional devices. A canonical example is the 2DEG at the interface between a polar oxide LaAlO3 (LAO and non-polar SrTiO3 (STO. Here, the LAO polar oxide can be regarded as the modulating or doping layer and is expected to define the electronic properties of 2DEG at the LAO/STO interface. However, to practically implement the 2DEG in electronics and device design, desired properties such as tunable 2D carrier density are necessary. Here, we report the tuning of conductivity threshold, carrier density and electronic properties of 2DEG in LAO/STO heterostructures by insertion of a La0.5Sr0.5TiO3 (LSTO layer of varying thicknesses, and thus modulating the amount of polarization of the oxide over layers. Our experimental result shows an enhancement of carrier density up to a value of about five times higher than that observed at the LAO/STO interface. A complete thickness dependent metal-insulator phase diagram is obtained by varying the thickness of LAO and LSTO providing an estimate for the critical thickness needed for the metallic phase. The observations are discussed in terms of electronic reconstruction induced by polar oxides.

  7. Hysteresis phenomena of the two dimensional electron gas density in lattice-matched InAlN/GaN heterostructures

    Energy Technology Data Exchange (ETDEWEB)

    Sang, Ling; Yang, Xuelin, E-mail: xlyang@pku.edu.cn; Cheng, Jianpeng; Guo, Lei; Hu, Anqi; Xiang, Yong; Yu, Tongjun; Xu, Fujun; Tang, Ning [State Key Laboratory of Artificial Microstructure and Mesoscopic Physics, School of Physics, Peking University, Beijing 100871 (China); Jia, Lifang; He, Zhi [Engineering Research Center for Semiconductor Integrated Technology, Institute of Semiconductors, Chinese Academy of Sciences, P. O. Box 912, Beijing 100083 (China); Wang, Maojun [Institute of Microelectronics, Peking University, Beijing 100871 (China); Wang, Xinqiang; Shen, Bo, E-mail: bshen@pku.edu.cn [State Key Laboratory of Artificial Microstructure and Mesoscopic Physics, School of Physics, Peking University, Beijing 100871 (China); Collaborative Innovation Center of Quantum Matter, Beijing 100871 (China); Ge, Weikun [Department of Physics, Tsinghua University, Beijing 100084 (China)

    2015-08-03

    High-temperature transport properties in high-mobility lattice-matched InAlN/GaN heterostructures have been investigated. An interesting hysteresis phenomenon of the two dimensional electron gas (2DEG) density is observed in the temperature-dependent Hall measurements. After high-temperature thermal cycles treatment, the reduction of the 2DEG density is observed, which is more serious in thinner InAlN barrier samples. This reduction can then be recovered by light illumination. We attribute these behaviors to the shallow trap states with energy level above the Fermi level in the GaN buffer layer. The electrons in the 2DEG are thermal-excited when temperature is increased and then trapped by these shallow trap states in the buffer layer, resulting in the reduction and hysteresis phenomenon of their density. Three trap states are observed in the GaN buffer layer and C{sub Ga} may be one of the candidates responsible for the observed behaviors. Our results provide an alternative approach to assess the quality of InAlN/GaN heterostructures for applications in high-temperature electronic devices.

  8. Analysis of underivatised low volatility compounds by comprehensive two-dimensional gas chromatography with a short primary column.

    Science.gov (United States)

    Novaes, Fábio Junior Moreira; Kulsing, Chadin; Bizzo, Humberto Ribeiro; de Aquino Neto, Francisco Radler; Rezende, Claudia Moraes; Marriott, Philip John

    2018-02-09

    Comprehensive two-dimensional gas chromatography (GC×GC) approaches with cryogenic modulation were developed for the qualitative analysis of selected low volatility compounds in raw coffee bean extracts, without derivatisation. The approaches employed short first ( 1 D) and second ( 2 D) dimension columns, specifically a 1 D 65% phenyl methyl siloxane column (11m) and a 2 D 5% phenyl methyl siloxane column (1m), which allowed elution of high molar mass compounds (e.g.>600Da). Solutes included hydrocarbons, fatty acids, diterpenes, tocopherols, sterols, diterpene esters, and di- and triacylglycerides. An oven temperature program up to 370°C was employed. The effects of experimental conditions were investigated, revealing that the GC×GC results strongly depended on the cryogenic trap T, and oven T program. An appropriate condition was selected and further applied for group type analysis of low volatility compounds in green Arabica coffee beans. Retention indices were compiled for 1D GC analysis and were similar for the composite column data in GC×GC. The elution of some compounds was confirmed by use of authentic standards. The approach allowed direct analysis of coffee extract in ethyl acetate solution, with improved analyte peak capacity (approximately 200 compounds were detected) without prior fractionation or pre-treatment of the sample. This avoided potential hydrolysis of high molar mass conjugate esters as well as degradation of thermally labile compounds such as the derivatives of the diterpenes cafestol and kahweol. Copyright © 2017 Elsevier B.V. All rights reserved.

  9. The Tracing of VOC Composition of Acacia Honey During Ripening Stages by Comprehensive Two-Dimensional Gas Chromatography.

    Science.gov (United States)

    Vyviurska, Olga; Chlebo, Róbert; Pysarevska, Solomiya; Špánik, Ivan

    2016-10-01

    In this study, VOC profiles of acacia flowers and honey samples at different processing stages and related comb wax samples were studied using comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry. It was found that some monoterpene compounds like α-pinene, myrcene, cis-β-ocimene, and 4-terpineol were common for acacia flower and all acacia honey samples, and the presence of verbenone and ocimene was first established in acacia honey. The most enriched VOC profile was obtained for raw honey before cell capping, where the final composition of lactones was achieved. On the contrary, number of alcohols, esters, and variety of terpenes, as well as their concentration in the honey samples decrease through ripening processes. Strained honey was characterized by the absence of camphor, α-bisabolol, and 3-carene, while isophorone and hexanoic acid were identified only in this type of honey. The composition of final VOC profile of honey was also influenced by the age of comb wax. The additional aromatic and lactone compounds, e.g., phenol, 1-phenylethanol, δ-hexalactone, and γ-heptalactone were observed for honey maturated in old dark comb wax. © 2016 Wiley-VHCA AG, Zürich.

  10. Identification of inorganic anions by gas chromatography/mass spectrometry.

    Science.gov (United States)

    Sakayanagi, Masataka; Yamada, Yaeko; Sakabe, Chikako; Watanabe, Kunio; Harigaya, Yoshihiro

    2006-03-10

    Inorganic anions were identified by using gas chromatography/mass spectrometry (GC/MS). Derivatization of the anions was achieved with pentafluorobenzyl p-toluenesulphonate (PFB-Tos) as the reaction reagent and a crown ether as a phase transfer catalyst. When PFB-Br was used as the reaction reagent, the retention time of it was close to those of the derivatized inorganic anions and interfered with the analysis. In contrast, the retention time of PFB-Tos differed greatly from the PFB derivatives of the inorganic anions and the compounds of interest could be detected without interference. Although the PFB derivatives of SO4, S2O3, CO3, ClO4, and ClO3 could not be detected, the derivatives of F, Cl, Br, I, CN, OCN, SCN, N3, NO3, and NO2 were detected using PFB-Tos as the derivatizing reagent. The inorganic anions were detectable within 30 ng approximately, which is of sufficient sensitivity for use in forensic chemistry. Accurate mass number was measured for each PFB derivative by high-resolution mass spectrometry (HRMS) within a measurement error of 2 millimass units (mmu), which allowed determination of the compositional formula from the mass number. In addition, actual analysis was performed successively by our method using trial samples of matrix.

  11. High-temperature two-dimensional gas chromatography of hydrocarbons up to nC60 for analysis of vacuum gas oils.

    Science.gov (United States)

    Dutriez, Thomas; Courtiade, Marion; Thiébaut, Didier; Dulot, Hugues; Bertoncini, Fabrice; Vial, Jérôme; Hennion, Marie-Claire

    2009-04-03

    In a tense energetic context, the characterization of heavy petroleum fractions becomes essential. Conventional comprehensive two-dimensional gas chromatography (2D-GC or GCxGC) is widely used for middle distillates analysis, but only a few applications are devoted to these heavier fractions. In this paper, it is shown how the optimization of GCxGC separation allowed the determination of suitable high-temperature (HT) conditions, adjusting column properties and operating conditions. 2D separations were evaluated using 2D separation criteria and a new concept of 2D asymmetry (As(2D)). New HT conditions allowed the extension of GCxGC range of applications to heavier hydrocarbons, up to nC(60). A first application of high-temperature two-dimensional gas chromatography (HT-2D-GC) to a full vacuum gas oil (VGO) feed stock is described. Comparisons with other standardized methods illustrate the high potential of HT-2D-GC for heavy fractions analysis.

  12. Detection of an extended human volatome with comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry.

    Directory of Open Access Journals (Sweden)

    Michael Phillips

    Full Text Available BACKGROUND: Comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry (GCxGC-TOF MS has been proposed as a powerful new tool for multidimensional analysis of complex chemical mixtures. We investigated GCxGC-TOF MS as a new method for identifying volatile organic compounds (VOCs in normal human breath. METHODS: Samples of alveolar breath VOCs and ambient room air VOC were collected with a breath collection apparatus (BCA onto separate sorbent traps from 34 normal healthy volunteers (mean age = 40 yr, SD = 17 yr, male/female = 19/15. VOCs were separated on two serial capillary columns separated by a cryogenic modulator, and detected with TOF MS. The first and second dimension columns were non-polar and polar respectively. RESULTS: BCA collection combined with GC×GC-TOF MS analysis identified approximately 2000 different VOCs in samples of human breath, many of which have not been previously reported. The 50 VOCs with the highest alveolar gradients (abundance in breath minus abundance in ambient room air mostly comprised benzene derivatives, acetone, methylated derivatives of alkanes, and isoprene. CONCLUSIONS: Collection and analysis of breath VOCs with the BCA-GC×GC-TOF MS system extended the size of the detectable human volatile metabolome, the volatome, by an order of magnitude compared to previous reports employing one-dimensional GC-MS. The size of the human volatome has been under-estimated in the past due to coelution of VOCs in one-dimensional GC analytical systems.

  13. Thermal desorption modulation for comprehensive two-dimensional gas chromatography using a simple and inexpensive segmented-loop fluidic interface.

    Science.gov (United States)

    Mucédola, Vanessa; Vieira, Luis C S; Pierone, Danilo; Gobbi, Angelo L; Poppi, Ronei J; Hantao, Leandro W

    2017-03-01

    In this study, we introduce a modulation strategy for comprehensive two-dimensional gas chromatography (GC×GC) by using a simple and consumable-free modulator. This "Do-It-Yourself" interface comprised a 1.0m×0.25mm segment of MTX-5 metallic column and a low-cost DC power supply. Thermal desorption modulation (TDM) was attained using a dual-stage heater-based modulator in a novel segmented-loop configuration. TDM was achieved by alternating analyte trapping and thermal desorption. Former process relied on analyte partition to sorbent phase, while latter explored direct resistive heating. Introduction of an intermediate delay segment between the two stages mitigated analyte breakthrough, improving peak symmetry and chromatographic efficiency. This feature was critical to acquire reliable GC×GC modulation using such simple heater-based device. The effects of important modulation variables on 2D separations were investigated, including TDM stage length, dimension of delay loop, and outlet pressure. Significant advances and limitations of proposed TDM strategy were carefully determined. Proposed GC×GC prototype by using an in-oven TDM modulator was successfully applied to a series of challenging matrices, including petroleum distillates, biodiesel, and essential oil. This open-hardware, cost-effective modulator was easy to install and operate, as it circumvented the need for sophisticated components (e.g. moving parts and cooling systems). Therefore, our modulator is a compelling alternative to existing GC×GC solutions to operate in resource-limited laboratories. Copyright © 2016 Elsevier B.V. All rights reserved.

  14. Microfabricated thermal modulator for comprehensive two-dimensional micro gas chromatography: design, thermal modeling, and preliminary testing.

    Science.gov (United States)

    Kim, Sung-Jin; Reidy, Shaelah M; Block, Bruce P; Wise, Kensall D; Zellers, Edward T; Kurabayashi, Katsuo

    2010-07-07

    In comprehensive two-dimensional gas chromatography (GC x GC), a modulator is placed at the juncture between two separation columns to focus and re-inject eluting mixture components, thereby enhancing the resolution and the selectivity of analytes. As part of an effort to develop a microGC x microGC prototype, in this report we present the design, fabrication, thermal operation, and initial testing of a two-stage microscale thermal modulator (microTM). The microTM contains two sequential serpentine Pyrex-on-Si microchannels (stages) that cryogenically trap analytes eluting from the first-dimension column and thermally inject them into the second-dimension column in a rapid, programmable manner. For each modulation cycle (typically 5 s for cooling with refrigeration work of 200 J and 100 ms for heating at 10 W), the microTM is kept approximately at -50 degrees C by a solid-state thermoelectric cooling unit placed within a few tens of micrometres of the device, and heated to 250 degrees C at 2800 degrees C s(-1) by integrated resistive microheaters and then cooled back to -50 degrees C at 250 degrees C s(-1). Thermal crosstalk between the two stages is less than 9%. A lumped heat transfer model is used to analyze the device design with respect to the rates of heating and cooling, power dissipation, and inter-stage thermal crosstalk as a function of Pyrex-membrane thickness, air-gap depth, and stage separation distance. Experimental results are in agreement with trends predicted by the model. Preliminary tests using a conventional capillary column interfaced to the microTM demonstrate the capability for enhanced sensitivity and resolution as well as the modulation of a mixture of alkanes.

  15. Two-dimensional Molecular Gas and Ongoing Star Formation around H II Region Sh2-104

    Science.gov (United States)

    Xu, Jin-Long; Xu, Ye; Yu, Naiping; Zhang, Chuan-peng; Liu, Xiao-Lan; Wang, Jun-Jie; Ning, Chang-chun; Ju, Bing-Gang; Zhang, Guo-Yin

    2017-11-01

    We performed a multi-wavelength study toward H II region Sh2-104. New maps of 12CO J = 1 - 0 and 13CO J = 1 - 0 were obtained from the Purple Mountain Observatory 13.7 m radio telescope. Sh2-104 displays a double-ring structure. The outer ring with a radius of 4.4 pc is dominated by 12, 500 μm, 12CO J = 1 - 0, and 13CO J = 1 - 0 emission, while the inner ring with a radius of 2.9 pc is dominated by 22 μm and 21 cm emission. We did not detect CO emission inside the outer ring. The north-east portion of the outer ring is blueshifted, while the south-west portion is redshifted. The present observations have provided evidence that the collected outer ring around Sh2-104 is a two-dimensional structure. From the column density map constructed by the Hi-GAL survey data, we extract 21 clumps. About 90% of all the clumps will form low-mass stars. A power-law fit to the clumps yields M=281 {M}⊙ {(r/{pc})}1.31+/- 0.08. The selected YSOs are associated with the collected material on the edge of Sh2-104. The derived dynamical age of Sh2-104 is 1.6× {10}6 yr. Comparing the Sh2-104 dynamical age with the YSO timescale and the fragmentation time of the molecular ring, we further confirm that the collect-and-collapse process operates in this region, indicating positive feedback from a massive star for surrounding gas.

  16. Organophosphorus pesticide and ester analysis by using comprehensive two-dimensional gas chromatography with flame photometric detection.

    Science.gov (United States)

    Liu, Xiangping; Li, Dengkun; Li, Jiequan; Rose, Gavin; Marriott, Philip J

    2013-12-15

    Thirty-seven phosphorus (P)-containing compounds comprising organophosphorus pesticides and organophosphate esters were analyzed by using comprehensive two-dimensional gas chromatography with flame photometric detection in P mode (GC × GC-FPD(P)), with a non-polar/moderately polar column set. A suitable modulation temperature and period was chosen based on experimental observation. A number of co-eluting peak pairs on the (1)D column were well separated in 2D space. Excellent FPD(P) detection selectivity, responding to compounds containing the P atom, produces clear 2D GC × GC plots with little interference from complex hydrocarbon matrices. Limits of detection (LOD) were within the range of 0.0021-0.048 μmol L(-1), and linear calibration correlation coefficients (R(2)) for all 37 P-compounds were at least 0.998. The P-compounds were spiked in 2% diesel and good reproducibility for their response areas and retention times was obtained. Spiked recoveries were 88%-157% for 5 μg L(-1) and 80%-138% for 10 μg L(-1) spiked levels. Both (1)tR and (2)tR shifts were noted when the content of diesel was in excess of 5% in the matrix. Soil samples were analyzed by using the developed method; some P-compounds were positively detected. In general, this study shows that GC × GC-FPD(P) is an accurate, sensitive and simple method for P-compound analysis in complicated environmental samples. Copyright © 2013 Elsevier B.V. All rights reserved.

  17. Quantitative analysis of essential oils in perfume using multivariate curve resolution combined with comprehensive two-dimensional gas chromatography.

    Science.gov (United States)

    de Godoy, Luiz Antonio Fonseca; Hantao, Leandro Wang; Pedroso, Marcio Pozzobon; Poppi, Ronei Jesus; Augusto, Fabio

    2011-08-05

    The use of multivariate curve resolution (MCR) to build multivariate quantitative models using data obtained from comprehensive two-dimensional gas chromatography with flame ionization detection (GC×GC-FID) is presented and evaluated. The MCR algorithm presents some important features, such as second order advantage and the recovery of the instrumental response for each pure component after optimization by an alternating least squares (ALS) procedure. A model to quantify the essential oil of rosemary was built using a calibration set containing only known concentrations of the essential oil and cereal alcohol as solvent. A calibration curve correlating the concentration of the essential oil of rosemary and the instrumental response obtained from the MCR-ALS algorithm was obtained, and this calibration model was applied to predict the concentration of the oil in complex samples (mixtures of the essential oil, pineapple essence and commercial perfume). The values of the root mean square error of prediction (RMSEP) and of the root mean square error of the percentage deviation (RMSPD) obtained were 0.4% (v/v) and 7.2%, respectively. Additionally, a second model was built and used to evaluate the accuracy of the method. A model to quantify the essential oil of lemon grass was built and its concentration was predicted in the validation set and real perfume samples. The RMSEP and RMSPD obtained were 0.5% (v/v) and 6.9%, respectively, and the concentration of the essential oil of lemon grass in perfume agreed to the value informed by the manufacturer. The result indicates that the MCR algorithm is adequate to resolve the target chromatogram from the complex sample and to build multivariate models of GC×GC-FID data. Copyright © 2011 Elsevier B.V. All rights reserved.

  18. Identification and classification of components in flash pyrolysis oil and hydrodeoxygenated oils by two-dimensional gas chromatography and time-of-flight mass spectrometry

    NARCIS (Netherlands)

    Marsman, J. H.; Wildschut, J.; Evers, P.; Heeres, H. J.; Koning de, S.

    2008-01-01

    Hydrodeoxygenated pyrolysis oils (HDO) are considered promising renewable liquid energy carriers. To gain insights in the various reaction pathways taking place during the hydrodeoxygenation reaction of pyrolysis oil, two-dimensional gas chromatography with time-of-flight mass spectrometric analyses

  19. Characterisation of volatile components of Pinotage wines using comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GC x GC–TOFMS)

    NARCIS (Netherlands)

    Weldegergis, B.T.; Villiers, de A.; McNeish, C.; Seethapathy, S.; Mostafa, A.; Górecki, T.; Crouch, A.M.

    2011-01-01

    As part of the ongoing research into the chemical composition of the uniquely South African wine cultivar Pinotage, the volatile composition of nine young wines of this cultivar was investigated using comprehensive two-dimensional gas chromatography (GC × GC) in combination with time-of-flight mass

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

    NARCIS (Netherlands)

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

    2005-01-01

    Comprehensive two-dimensional gas chromatography with electron-capture negative ionization time-of-flight mass spectrometry (GC × 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

  1. Comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry in the identification of organic compounds in atmospheric aerosols from coniferous forest

    NARCIS (Netherlands)

    Kallio, M.; Jussila, M.; Rissanen, T.; Anttila, P.; Hartonen, K.; Reissell, A.; Vreuls, R.J.J.; Adahchour, M.; Hyotylainen, T.

    2006-01-01

    Comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GC × GC-TOF-MS) was applied in the identification of organic compounds in atmospheric aerosols from coniferous forest. The samples were collected at Hyytiälä, Finland, as part of the QUEST campaign, in

  2. Spin-orbit interaction in a two-dimensional electron gas in a InAs/AlSb quantum well with gate-controlled electron density

    NARCIS (Netherlands)

    Heida, J.P.; Wees, B.J. van; Kuipers, J.J.; Klapwijk, T.M.; Borghs, G.

    1998-01-01

    We present experiments on the tuning of the spin-orbit interaction in a two-dimensional electron gas in an asymmetric InAs/AlSb quantum well using a gate. The observed dependence of the spin splitting energy on the electron density can be attributed solely to the change in the Fermi wave vector. The

  3. Comprehensive two-dimensional gas chromatography using partial modulation via a pulsed flow valve with a short modulation period.

    Science.gov (United States)

    Freye, Chris E; Bahaghighat, H Daniel; Synovec, Robert E

    2018-01-15

    Partial modulation via a pulsed flow valve for comprehensive two-dimensional (2D) gas chromatography (GC × GC) is demonstrated, producing narrow peak widths, 2 W b , on the secondary separation dimension, 2 D, coupled with short modulation periods, P M , thus producing a high peak capacity on the 2 D dimension, 2 n c . The GC × GC modulator is a pulse flow valve that injects a pulse of carrier gas at the specified P M , at the connection between the primary, 1 D, column and the 2 D column. Using a commercially available pulse flow valve, this injection technique performs a combination of vacancy chromatography and frontal analysis, whereby each pulse disturbance in the analyte concentration profile as it exits the 1 D column results in data that is readily converted into a 2 D separation. A three-step process converts the raw data into a format analogous to a GC × GC separation, incorporating signal differentiation, baseline correction and conversion to a GC × GC chromatogram representation. A 115-component test mixture with a wide range of boiling points (36-372°C) of nine compound classes is demonstrated using modulation periods of P M = 50, 100, 250, and 500ms, respectively. For the test mixture with a P M of 250ms, peak shapes on 2 D are symmetric with apparent 2 W b ranging from 12 to 45ms producing a 2 n c of ~ 10. Based on the average peak width of 0.93s on the 1 D separation for a time window of 400s, the 1 D peak capacity is 1 n c ∼ 430. Thus, the ideal 2D peak capacity n c,2D is 4300 or a peak capacity production of 650 peaks/min using the P M of 250ms. Additionally, for a P M of 50, 100 and 500ms, the 2 n c are 4, 7, and 12, respectively. Retention times on 2 D, 2 t R , are reproducible having standard deviations less than 1ms. Finally, the processed data is shown to be quantitative, with an average RSD of 4.7% for test analytes. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. AlGaAs/GaAs two-dimensional electron gas structures studied by photo reflectance spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Guillen Cervantes, A; Rivera Alvarez, Z; Hernandez, F; Huerta, J. [Instituto Politecnico Nacional, Mexico, D.F. (Mexico); Mendez Garcia, V. H.; Lastras Martinez, A.; Zamora, L.; Saucedo, N. [Universidad Autonoma de San Luis Potosi, San Luis Potosi (Mexico); Melendez Lira, M; Lopez, M [Instituto Politecnico Nacional, Mexico, D.F. (Mexico)

    2001-12-01

    Al{sub x} Ga{sub 1}-x As/GaAs two-dimensional electron gas (2-DEG) heterostructures were fabricated by molecular beam epitaxy in three different laboratories. The samples were characterized by room temperature Photo reflectance (PR) spectroscopy and measurements at 77 K. Internal electric fields were detected by the presence of Franz-Keldysh (FK) oscillations in the PR spectra. >From a FK analysis we obtained the GaAs band-gap energy and the built-in electric field strength in each sample. On the other hand, in the energy region corresponding to Al{sub x} Ga{sub 1}-x As a broad PR signal was registered typical of a highly doped material. Using the third derivative theory we obtained the Al{sub x} Ga{sub 1}-x As band-gap energy, and from this value the Al concentration in the samples. Results showed that the sample with highest electron mobility exhibited the lowest internal electric field strength. [Spanish] Se fabricaron heteroestructuras del tipo Al{sub x} Ga{sub 1}-x As/GaAs con un gas de electrones en dos dimensiones por medio de epitaxia de haces moleculares en tres laboratorios diferentes. Las muestras se caracterizaron por fotorreflectancia (FR) a temperatura ambiente y por mediciones del efecto mayor a 77 K. Campos electricos internos se detectaron por la presencia de oscilaciones Franz-Leldysh (FK) en los espectros de FR. Del analisis de las oscilaciones FK obtuvimos la energia de la brecha prohibida del GaAs y la intensidad del campo electrico interno en cada muestra. Por otra parte, en la region de energia correspondiente al Al{sub x} Ga{sub 1}-x As observamos una senal de FR ancha, tipica de un material altamente impurificado. Usando la teoria de la tercera derivada, obtuvimos el valor de la brecha de energia del Al{sub x}Ga{sub 1}-xAs, y de este valor la concentracion de Al en las muestras. Los resultados mostraron que la estructura con el valor de movilidad electronica mas alto tiene la intensidad de campo electrico interno mas baja.

  5. Organophosphorus pesticide and ester analysis by using comprehensive two-dimensional gas chromatography with flame photometric detection

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Xiangping; Li, Dengkun; Li, Jiequan [Nanjing Centre for Disease Control and Prevention, Zizhulin Street, Gulou 210003, Nanjing (China); Rose, Gavin [Department of Environment and Primary Industries, Macleod Centre, Ernest Jones Drive, Macleod, Vic 3085 (Australia); Marriott, Philip J., E-mail: philip.marriott@monash.edu [Australian Centre for Research on Separation Science, School of Chemistry, Monash University, Wellington Road, Clayton 3800 (Australia)

    2013-12-15

    Highlights: • GC × GC-FPD(P-mode) was applied to detection of 37 phosphorus (P)-containing compounds. • The method improves resolution of P-compounds that coelute in the first dimension. • P-compounds are analyzed with excellent sensitivity supported by cryogenic modulation. • The FPD(P-mode) selectivity allows analysis in high hydrocarbon (H/C) matrix. • Soil samples and spiked chemical weapon compounds in H/C matrix are readily screened. -- Abstract: Thirty-seven phosphorus (P)-containing compounds comprising organophosphorus pesticides and organophosphate esters were analyzed by using comprehensive two-dimensional gas chromatography with flame photometric detection in P mode (GC × GC-FPD(P)), with a non-polar/moderately polar column set. A suitable modulation temperature and period was chosen based on experimental observation. A number of co-eluting peak pairs on the {sup 1}D column were well separated in 2D space. Excellent FPD(P) detection selectivity, responding to compounds containing the P atom, produces clear 2D GC × GC plots with little interference from complex hydrocarbon matrices. Limits of detection (LOD) were within the range of 0.0021–0.048 μmol L{sup −1}, and linear calibration correlation coefficients (R{sup 2}) for all 37 P-compounds were at least 0.998. The P-compounds were spiked in 2% diesel and good reproducibility for their response areas and retention times was obtained. Spiked recoveries were 88%–157% for 5 μg L{sup −1} and 80%–138% for 10 μg L{sup −1} spiked levels. Both {sup 1}t{sub R} and {sup 2}t{sub R} shifts were noted when the content of diesel was in excess of 5% in the matrix. Soil samples were analyzed by using the developed method; some P-compounds were positively detected. In general, this study shows that GC × GC-FPD(P) is an accurate, sensitive and simple method for P-compound analysis in complicated environmental samples.

  6. Chemical discrimination in turbulent gas mixtures with MOX sensors validated by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Fonollosa, Jordi; Rodríguez-Luján, Irene; Trincavelli, Marco; Vergara, Alexander; Huerta, Ramón

    2014-10-16

    Chemical detection systems based on chemo-resistive sensors usually include a gas chamber to control the sample air flow and to minimize turbulence. However, such a kind of experimental setup does not reproduce the gas concentration fluctuations observed in natural environments and destroys the spatio-temporal information contained in gas plumes. Aiming at reproducing more realistic environments, we utilize a wind tunnel with two independent gas sources that get naturally mixed along a turbulent flow. For the first time, chemo-resistive gas sensors are exposed to dynamic gas mixtures generated with several concentration levels at the sources. Moreover, the ground truth of gas concentrations at the sensor location was estimated by means of gas chromatography-mass spectrometry. We used a support vector machine as a tool to show that chemo-resistive transduction can be utilized to reliably identify chemical components in dynamic turbulent mixtures, as long as sufficient gas concentration coverage is used. We show that in open sampling systems, training the classifiers only on high concentrations of gases produces less effective classification and that it is important to calibrate the classification method with data at low gas concentrations to achieve optimal performance.

  7. Fast, high peak capacity separations in comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry.

    Science.gov (United States)

    Fitz, Brian D; Wilson, Ryan B; Parsons, Brendon A; Hoggard, Jamin C; Synovec, Robert E

    2012-11-30

    Peak capacity production is substantially improved for two-dimensional gas chromatography coupled with time-of-flight mass spectrometry (GC×GC-TOFMS) and applied to the fast separation of a 28 component liquid test mixture, and two complex vapor samples (a 65 component volatile organic compound test mixture, and the headspace of warm ground coffee beans). A high peak capacity is achieved in a short separation time by selecting appropriate experimental conditions based on theoretical modeling of on-column band broadening, and by reducing the off-column band broadening by applying a narrow, concentrated injection pulse onto the primary column using high-speed cryo-focusing injection (HSCFI), referred to as thermal injection. A long, relatively narrow open tubular capillary column (20 m, 100 μm inner diameter (i.d.) with a 0.4 μm film thickness to benefit column capacity) was used as the primary column. The initial flow rate was 2 ml/min (60 cm/s average linear flow velocity) which is slightly below the optimal average linear gas velocity of 83 cm/s, due to the flow rate constraint of the TOFMS vacuum system. The oven temperature programming rate was 30°C/min. The secondary column (1.8m, 100 μm i.d. with a 0.1 μm film thickness) provided a relatively high peak capacity separation, concurrent with a significantly shorter modulation period, P(M), than commonly applied with the commercial instrument. With this GC×GC-TOFMS instrumental platform, compounds in the 28 component liquid test mixture provided a ∼7 min separation (with a ∼6.5 min separation time window), producing average peak widths of ∼600 ms full width half maximum (FWHM), resulting in a peak capacity on the primary column of ∼400 peaks (at unit resolution). Using a secondary column with a 500 ms P(M), average peak widths of ∼20 ms FWHM were achieved, thus providing a peak capacity of 15 peaks on the second dimension. Overall, an ideal orthogonal GC×GC peak capacity of ∼6000 peaks (at unit

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1992-07-01

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

  9. Voltage- and Light-Controlled Spin Properties of a Two-Dimensional Hole Gas in p-Type GaAs/AlAs Resonant Tunneling Diodes

    Science.gov (United States)

    Galeti, H. V. A.; Galvão Gobato, Y.; Brasil, M. J. S. P.; Taylor, D.; Henini, M.

    2018-03-01

    We have investigated the spin properties of a two-dimensional hole gas (2DHG) formed at the contact layer of a p-type GaAs/AlAs resonant tunneling diode (RTD). We have measured the polarized-resolved photoluminescence of the RTD as a function of bias voltage, laser intensity and external magnetic field up to 15T. By tuning the voltage and the laser intensity, we are able to change the spin-splitting from the 2DHG from almost 0 meV to 5 meV and its polarization degree from - 40% to + 50% at 15T. These results are attributed to changes of the local electric field applied to the two-dimensional gas which affects the valence band and the hole Rashba spin-orbit effect.

  10. Two-dimensional liquid fraction measurement in horizontal wavy liquid-gas geometry using X-ray radiography

    International Nuclear Information System (INIS)

    Maxym A Rychkov; Hyun Sun Park; Roberta C Hansson; Bal Raj Sehgal

    2005-01-01

    facility is located inside reinforced concrete containment (3.8 m x 3.8 m x 3.9 m) with a wall thickness of 0.6 m. The visualization system of continuous high-speed X-ray radiography consists of an X-ray source tube, an X-ray converter with image intensifier and a high-speed video camera. The X-ray source tube can be varied its power and current up to 320 keV and 22 mA, respectively. The X-ray converter and image intensifier equipped with a view window of 170 mm and powered by a high voltage power supplier. The high-speed camera can record images at the maximum frame rate of 100,000 fps for up to 1 seconds at the maximum frame rate. By installing the water tank with different water levels and evaluating the grey level, which is proportional to the intensity of the X-ray beam, we determine the two-dimensional interface structure. In this paper, the results obtained from the different shapes of the interface are studied and results are recorded and analysed. The methodology to the liquid fraction measurement using X-ray radiography is discussed. The liquid-gas interfacial areas are evaluated from the measurement of liquid fractions. (authors)

  11. Evaluation of quantitative sulfur speciation in gas oils by Fourier transform ion cyclotron resonance mass spectrometry: validation by comprehensive two-dimensional gas chromatography.

    Science.gov (United States)

    Muller, Hendrik; Adam, Frederick M; Panda, Saroj K; Al-Jawad, Hanadi H; Al-Hajji, Adnan A

    2012-05-01

    Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS) has been applied for the quantitative speciation of sulfur containing compounds in gas oil (GO). For this purpose, ionization and mass spectrometric parameters have been studied and optimized with a set of standard compounds and GO samples. Comprehensive two-dimensional gas chromatography (GCxGC) was used as the reference method. To allow a quantitative comparison between FT-ICR MS and GCxGC results for GO samples, FT-ICR MS parameters were optimized and data obtained by both techniques were standardized. Response factors were established for two ionization modes: atmospheric pressure photo ionization (APPI) and electrospray after selective derivatization of sulfur compounds (MeESI). To test the validity of the developed MS methods, a third GO was analyzed and response factors were applied. Comparison with GCxGC results showed good agreement for sulfur families (deviation within 5% and 15% for MeESI and APPI data, respectively). Abundances of individual isomer groups match within 40% in most cases. These results principally demonstrate the suitability of FT-ICR MS for a quantitative analysis of sulfur compounds (by DBE and carbon number distribution pattern) in petroleum middle distillates. This approach has the potential to be extended to higher- and non-boiling petroleum fractions where quantitative speciation is presently not available.

  12. Comparison of an Electronic Nose Based on Ultrafast Gas Chromatography, Comprehensive Two-Dimensional Gas Chromatography, and Sensory Evaluation for an Analysis of Type of Whisky

    Directory of Open Access Journals (Sweden)

    Paulina Wiśniewska

    2017-01-01

    Full Text Available Whisky is one of the most popular alcoholic beverages. There are many types of whisky, for example, Scotch, Irish, and American whisky (called bourbon. The whisky market is highly diversified, and, because of this, it is important to have a method which would enable rapid quality evaluation and authentication of the type of whisky. The aim of this work was to compare 3 methods: an electronic nose based on the technology of ultrafast gas chromatography (Fast-GC, comprehensive two-dimensional gas chromatography (GC × GC, and sensory evaluation. The selected whisky brands included 6 blended whiskies from Scotland, 4 blended whiskies from Ireland, and 4 bourbons produced in the USA. For data analysis, peak heights of chromatograms were used. The panelists who took part in sensory evaluations included 4 women and 4 men. The obtained data were analyzed by 2 chemometric methods: partial least squares discriminant analysis (PLS-DA and discrimination function analysis (DFA. E-nose and GC × GC allowed for differentiation between whiskies by type. Sensory analysis did not allow for differentiation between whiskies by type, but it allowed giving consumer preferences.

  13. Magnetic and Nematic Orders of the Two-Dimensional Electron Gas at Oxide (111) Surfaces and Interfaces

    Science.gov (United States)

    Boudjada, Nazim; Wachtel, Gideon; Paramekanti, Arun

    2018-02-01

    Recent experiments have explored two-dimensional electron gases (2DEGs) at oxide (111) surfaces and interfaces, finding evidence for hexagonal symmetry breaking in SrTiO3 at low temperature. We discuss many-body instabilities of such (111) 2DEGs, incorporating multiorbital interactions in the t2 g manifold which can induce diverse magnetic and orbital orders. Such broken symmetries may partly account for the observed nematicity, cooperating or competing with phonon mechanisms. We present an effective field theory for the interplay of magnetism and nematic charge order, and discuss implications of the nematicity for transport and superconductivity in (111) 2DEGs.

  14. Drude weight and optical conductivity of a two-dimensional heavy-hole gas with k-cubic spin-orbit interactions

    Energy Technology Data Exchange (ETDEWEB)

    Mawrie, Alestin; Ghosh, Tarun Kanti [Department of Physics, Indian Institute of Technology-Kanpur, Kanpur 208 016 (India)

    2016-01-28

    We present a detailed theoretical study on zero-frequency Drude weight and optical conductivity of a two-dimensional heavy-hole gas (2DHG) with k-cubic Rashba and Dresselhaus spin-orbit interactions. The presence of k-cubic spin-orbit couplings strongly modifies the Drude weight in comparison to the electron gas with k-linear spin-orbit couplings. For large hole density and strong k-cubic spin-orbit couplings, the density dependence of Drude weight deviates from the linear behavior. We establish a relation between optical conductivity and the Berry connection. Unlike two-dimensional electron gas with k-linear spin-orbit couplings, we explicitly show that the optical conductivity does not vanish even for equal strength of the two spin-orbit couplings. We attribute this fact to the non-zero Berry phase for equal strength of k-cubic spin-orbit couplings. The least photon energy needed to set in the optical transition in hole gas is one order of magnitude smaller than that of electron gas. Types of two van Hove singularities appear in the optical spectrum are also discussed.

  15. Thomas-Fermi-von Weizsäcker theory for a harmonically trapped, two-dimensional, spin-polarized dipolar Fermi gas

    Science.gov (United States)

    van Zyl, B. P.; Zaremba, E.; Pisarski, P.

    2013-04-01

    We systematically develop a density functional description for the equilibrium properties of a two-dimensional, harmonically trapped, spin-polarized dipolar Fermi gas based on the Thomas-Fermi-von Weizsäcker approximation. We pay particular attention to the construction of the two-dimensional kinetic energy functional, where corrections beyond the local density approximation must be motivated with care. We also present an intuitive derivation of the interaction energy functional associated with the dipolar interactions and provide physical insight into why it can be represented as a local functional. Finally, a simple and highly efficient self-consistent numerical procedure is developed to determine the equilibrium density of the system for a range of dipole interaction strengths.

  16. Incorporation of Gas Chromatography-Mass Spectrometry into the Undergraduate Organic Chemistry Laboratory Curriculum

    Science.gov (United States)

    Giarikos, Dimitrios G.; Patel, Sagir; Lister, Andrew; Razeghifard, Reza

    2013-01-01

    Gas chromatography-mass spectrometry (GC-MS) is a powerful analytical tool for detection, identification, and quantification of many volatile organic compounds. However, many colleges and universities have not fully incorporated this technique into undergraduate teaching laboratories despite its wide application and ease of use in organic…

  17. Gas Chromatography/mass Spectrometry Analysis of Exhaled Leukotrienes in Asthmatic Patients

    Czech Academy of Sciences Publication Activity Database

    Čáp, P.; Chládek, J.; Pehal, F.; Malý, Marek; Petrů, V.; Barnes, P.J.; Montuschi, P.

    2004-01-01

    Roč. 59, č. 6 (2004), s. 465-470 ISSN 0040-6376 Source of funding: V - iné verejné zdroje Keywords : asthma * breath condensate * gas chromatography/mass spectrometry * leukotrienes Subject RIV: BB - Applied Statistics, Operational Research Impact factor: 5.040, year: 2004

  18. Gas chromatography-mass spectrometry (GC-MS) analysis of extractives of naturally durable wood

    Science.gov (United States)

    G.T. Kirker; A.B. Blodgett; S.T. Lebow; C.A. Clausen

    2011-01-01

    A preliminary study to evaluate naturally durable wood species in an above ground field trial using Gas Chromatography-Mass Spectrometry (GC-MS) detected differences in fatty acid extractives between species and within the same species over time. Fatty acids were extracted with chloroform: methanol mixture then methylated with sodium methoxide and fractionated using...

  19. Ion counting method and it's operational characteristics in gas chromatography-mass spectrometry

    International Nuclear Information System (INIS)

    Fujii, Toshihiro

    1976-01-01

    Ion counting method with continuous channel electron multiplier which affords the direct detection of very small ion currents and it's operational characteristics were studied in gas chromatography-mass spectrometry. Then this method was applied to the single ion detection technique of GC-MS. A detection limit was measured, using various standard samples of low level concentration. (auth.)

  20. Identification of Synthetic Polymers and Copolymers by Analytical Pyrolysis-Gas Chromatography/Mass Spectrometry

    Science.gov (United States)

    Kusch, Peter

    2014-01-01

    An experiment for the identification of synthetic polymers and copolymers by analytical pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) was developed and performed in the polymer analysis courses for third-year undergraduate students of chemistry with material sciences, and for first-year postgraduate students of polymer sciences. In…

  1. Suppression of the two-dimensional electron gas in LaGaO3/SrTiO3 by cation intermixing

    KAUST Repository

    Nazir, S.

    2013-12-03

    Cation intermixing at the n-type polar LaGaO 3 /SrTiO 3 (001) interface is investigated by first principles calculations. Ti"Ga, Sr"La, and SrTi"LaGa intermixing are studied in comparison to each other, with a focus on the interface stability. We demonstrate in which cases intermixing is energetically favorable as compared to a clean interface. A depopulation of the Ti 3d xy orbitals under cation intermixing is found, reflecting a complete suppression of the two-dimensional electron gas present at the clean interface.

  2. Direct Imaging of Charge Density Modulation in Switchable Two-Dimensional Electron Gas at the Oxide Hetero-Interfaces by Using Electron Bean Inline Holography

    Science.gov (United States)

    2015-08-16

    Switchable Two-Dimensional Electron Gas at the Oxide Hetero-Interfaces by Using Electron Bean Inline Holography 5a. CONTRACT NUMBER FA2386-13-1-4136...directly imaged the charge carrier densities and spatial distributions at the (001) LaAlO3/SrTiO3 heterointerfaces by in-situ TEM holography . The new...Hetero-Interfaces by Using Electron Bean Inline Holography 5a. CONTRACT NUMBER FA2386-13-1-4136 5b. GRANT NUMBER 5c. PROGRAM ELEMENT NUMBER 61102F

  3. Anisotropic scattering effect of the inclined misfit dislocation on the two-dimensional electron gas in Al(In)GaN/GaN heterostructures

    International Nuclear Information System (INIS)

    Jin, Dong-Dong; Wang, Lian-shan; Yang, Shao-Yan; Li, Hui-jie; Zhang, Heng; Wang, Jian-xia; Xiang, Ruo-fei; Wei, Hong-yuan; Jiao, Chun-mei; Liu, Xiang-Lin; Zhu, Qin-Sheng; Wang, Zhan-Guo; Zhang, Liu-Wan

    2014-01-01

    In this paper, a theory is developed to study the anisotropic scattering effect of the inclined misfit dislocation on the two-dimensional electron gas in Al(In)GaN/GaN heterostructures. The inclined misfit dislocation, which differs from the well-known vertical threading dislocation, has a remarkable tilt angle from the vertical. The predicted electron mobility shows a remarkable anisotropy. It has a maximum mobility value along the direction perpendicular to the projection of the inclined dislocation line, and a minimum mobility value along the direction parallel to the projection. The degree of the anisotropic scattering effect will be even greater with the increase of the tilt angle

  4. Substantiation of buried two dimensional hole gas (2DHG) existence in GaN-on-Si epitaxial heterostructure

    Science.gov (United States)

    Sun, Jinming; Longobardi, Giorgia; Udrea, Florin; Zhu, Congyong; Camuso, Gianluca; Yang, Shu; Garg, Reenu; Imam, Mohamed; Charles, Alain

    2017-04-01

    Gallium Nitride on Silicon (GaN-on-Si) devices feature a relatively thick epi buffer layer to release the stress related to the lattice constant mismatch between GaN and Si. The buffer layer is formed by several AlGaN-based transition layers with different Al contents. This work addresses the fundamental question of whether two-dimensional hole gases (2DHGs) exist at those interfaces where the theory predicts a high concentration of a negative fixed charge as a consequence of the discontinuity in polarization between the layers. In this study, we demonstrate that the presence of such 2DHGs is consistent with the measured vertical Capacitance-Votage Profiling (CV) and Technology Caomputer-Aided Design (TCAD) simulation in the whole range of measurable frequencies (10 mHz-1 MHz). N-type compensating background donor included in the epi structure in the simulation deck proves to be crucial to explain the depletion region extension consistent with the CV experimental data. For the standard range of frequencies (1 kHz-1 MHz), there was no indication of the presence of 2DHGs. A set of ultra-low frequency (10 mHz-10 Hz) measurements performed were able to reveal the existence of 2DHGs. The outcome of these ultra-low frequency experiments was matched with TCAD simulations which validated our theory.

  5. Chemometrics comparison of gas chromatography with mass spectrometry and comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry Daphnia magna metabolic profiles exposed to salinity.

    Science.gov (United States)

    Parastar, Hadi; Garreta-Lara, Elba; Campos, Bruno; Barata, Carlos; Lacorte, Silvia; Tauler, Roma

    2018-02-27

    The performances of gas chromatography with mass spectrometry and of comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry are examined through the comparison of Daphnia magna metabolic profiles. Gas chromatography with mass spectrometry and comprehensive two-dimensional gas chromatography with mass spectrometry were used to compare the concentration changes of metabolites under saline conditions. In this regard, a chemometric strategy based on wavelet compression and multivariate curve resolution-alternating least squares is used to compare the performances of gas chromatography with mass spectrometry and comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry for the untargeted metabolic profiling of Daphnia magna in control and salinity-exposed samples. Examination of the results confirmed the outperformance of comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry over gas chromatography with mass spectrometry for the detection of metabolites in D. magna samples. The peak areas of multivariate curve resolution-alternating least squares resolved elution profiles in every sample analyzed by comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry were arranged in a new data matrix that was then modeled by partial least squares discriminant analysis. The control and salt-exposed daphnids samples were discriminated and the most relevant metabolites were estimated using variable importance in projection and selectivity ratio values. Salinity de-regulated 18 metabolites from metabolic pathways involved in protein translation, transmembrane cell transport, carbon metabolism, secondary metabolism, glycolysis, and osmoregulation. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Heart-cutting two-dimensional gas chromatography-isotope ratio mass spectrometry analysis of monoaromatic hydrocarbons in complex groundwater and gas-phase samples.

    Science.gov (United States)

    Ponsin, Violaine; Buscheck, Timothy E; Hunkeler, Daniel

    2017-04-07

    Compound-specific isotope analysis (CSIA) is increasingly used to evaluate the origin and fate of petroleum hydrocarbons in the environment. However, as samples often contain a complex mixture of compounds and the method requires a full chromatographic separation, it can be challenging to obtain accurate and precise isotope values. In this study, in order to develop a method to analyze carbon isotopes in benzene, toluene, ethylbenzene, and xylenes (BTEX) in complex environmental samples, a two-dimensional heart-cutting gas chromatograph (GC) was hyphenated to an isotope ratio mass spectrometer (IRMS). The focus was placed on benzene and toluene, which are the main compounds of concern in contaminated sites. A full separation for BTEX was successfully achieved using a 60m polar column in the first dimension and a 30m non-polar column in the second dimension. Accuracy and precision of carbon isotope measurements of standards were not impacted by the new setup compared to classic one-dimensional (1D) GC-C-IRMS. For benzene and toluene, precision remained very good (≤0.2‰) for concentrations comprised between 5 and 20μg/L. A high matrix load did not influence the precision and accuracy of isotope measurements. The method was tested on several samples from two different field sites. For all samples tested, full chromatographic baseline resolution was achieved for benzene and toluene. Spatial variability of isotopes values linked to biodegradation was evidenced for one field site. This new 2D-GC-C-IRMS method will broaden the spectrum of samples suitable for isotope analysis and will be therefore able to give new insights into attenuation processes of BTEX in contaminated sites or source fingerprinting. Copyright © 2017 Elsevier B.V. All rights reserved.

  7. Two-dimensional errors

    International Nuclear Information System (INIS)

    Anon.

    1991-01-01

    This chapter addresses the extension of previous work in one-dimensional (linear) error theory to two-dimensional error analysis. The topics of the chapter include the definition of two-dimensional error, the probability ellipse, the probability circle, elliptical (circular) error evaluation, the application to position accuracy, and the use of control systems (points) in measurements

  8. Microbial metabolomics with gas chromatography/mass spectrometry

    NARCIS (Netherlands)

    Koek, M.M.; Muilwijk, B.; Werf, M.J. van der; Hankemeier, T.

    2006-01-01

    An analytical method was set up suitable for the analysis of microbial metabolomes, consisting of an oximation and silylation derivatization reaction and subsequent analysis by gas chromatography coupled to mass spectrometry. Microbial matrixes contain many compounds that potentially interfere with

  9. Magnetic two-dimensional electron gas at the manganite-buffered LaAlO3/SrTiO3 interface

    DEFF Research Database (Denmark)

    R. Zhang, H.; Zhang, Y.; Zhang, H.

    2017-01-01

    Fabrication of highly mobile spin-polarized two-dimensional electron gas (2DEG) is crucially important for both fundamental and applied research. Usually, spin polarization appears below 10 K for the 2DEG of LaAlO3/SrTiO3 interface, stemming from the magnetic ordering of Ti3+ ions with the mediat......Fabrication of highly mobile spin-polarized two-dimensional electron gas (2DEG) is crucially important for both fundamental and applied research. Usually, spin polarization appears below 10 K for the 2DEG of LaAlO3/SrTiO3 interface, stemming from the magnetic ordering of Ti3+ ions...... with the mediation of itinerant electrons. Herein, we report a magnetic 2DEG at a La7/8Sr1/8MnO3-buffered LaAlO3/SrTiO3 interface, which simultaneously shows electrically tunable anomalous Hall effect and high conductivity. The spin-polarized temperature for the 2DEG is promoted to 30 K while the mobility remains...... high. The magnetism likely results from a gradient manganese interdiffusion into SrTiO3. The present work demonstrates the great potential of manganite-buffered LaAlO3/SrTiO3 interfaces for spintronic applications....

  10. A two-dimensional microscale model of gas exchange during photosynthesis in maize (Zea mays L.) leaves

    NARCIS (Netherlands)

    Retta, Moges; Ho, Quang Tri; Yin, Xinyou; Verboven, Pieter; Berghuijs, Herman N.C.; Struik, Paul C.; Nicolaï, Bart M.

    2016-01-01

    CO2 exchange in leaves of maize (Zea mays L.) was examined using a microscale model of combined gas diffusion and C4 photosynthesis kinetics at the leaf tissue level. Based on a generalized scheme of photosynthesis in NADP-malic enzyme type C4 plants, the model

  11. Identification and quantification of alkene-based drilling fluids in crude oils by comprehensive two-dimensional gas chromatography with flame ionization detection.

    Science.gov (United States)

    Reddy, Christopher M; Nelson, Robert K; Sylva, Sean P; Xu, Li; Peacock, Emily A; Raghuraman, Bhavani; Mullins, Oliver C

    2007-04-27

    Comprehensive two-dimensional gas chromatography with flame ionization detection (GC x GC-FID) was used to measure alkene-based drilling fluids in crude oils. Compared to one-dimensional gas chromatography, GC x GC-FID is more robust for detecting alkenes due to the increased resolution afforded by second dimension separations. Using GC x GC-FID to analyze four oil samples from one reservoir contaminated with the same drilling fluid, C(15), C(16), C(17), C(18) and C(20) alkenes were identified. The drilling fluid that contaminated these samples also differed from another commercially obtained fluid, which only contained C(16) and C(18) alkenes. These results should motivate the petroleum industry to consider GC x GC-FID for measuring drilling fluids.

  12. Flow-modulated comprehensive two-dimensional gas chromatography combined with a vacuum ultraviolet detector for the analysis of complex mixtures.

    Science.gov (United States)

    Zoccali, Mariosimone; Schug, Kevin A; Walsh, Phillip; Smuts, Jonathan; Mondello, Luigi

    2017-05-12

    The present paper is focused on the use of a vacuum ultraviolet absorption spectrometer (VUV) for gas chromatography (GC), within the context of flow modulated comprehensive two-dimensional gas chromatography (FM GC×GC). The features of the VUV detector were evaluated through the analysis of petrochemical and fatty acids samples. Besides responding in a predictable fashion via Beer's law principles, the detector provides additional spectroscopic information for qualitative analysis. Virtually all chemical species absorb and have unique gas phase absorption features in the 120-240nm wavelength range monitored. The VUV detector can acquire up to 90 full range absorption spectra per second, allowing its coupling with comprehensive two-dimensional gas chromatography. This recent form of detection can address specific limitations related to mass spectrometry (e.g., identification of isobaric and isomeric species with very similar mass spectra or labile chemical compounds), and it is also able to deconvolute co-eluting peaks. Moreover, it is possible to exploit a pseudo-absolute quantitation of analytes based on pre-recorded absorption cross-sections for target analytes, without the need for traditional calibration. Using this and the other features of the detector, particular attention was devoted to the suitability of the FM GC×GC-VUV system toward qualitative and quantitative analysis of bio-diesel fuel and different kinds of fatty acids. Satisfactory results were obtained in terms of tailing factor (1.1), asymmetry factor (1.1), and similarity (average value 97%), for the FAMEs mixtures analysis. Copyright © 2017 Elsevier B.V. All rights reserved.

  13. Gas Chromatography-Mass Spectrometric Analysis of Nematicidal ...

    African Journals Online (AJOL)

    chromatography (GC) and gas chromaotography-mass spectrometry (GC-MS). The nematicidal activity of the essential oil and its major constituents was determined against second stage juveniles of H. avenae. Results: A total of 33 components of the essential oil were identified. The major constituents were bornyl acetate ...

  14. Two-dimensional perturbations of the accelerated motion of inhomogeneous gas layers and shells in the interstellar medium

    Science.gov (United States)

    Krasnobaev, K. V.; Kotova, G. Yu.; Tagirova, R. R.

    2015-03-01

    The evolution of perturbations in a two-layer spherical shell and a plane layer with a two-step density distribution has been simulated numerically. The clumps formed by instability are shown to have qualitatively different structures, depending on the ratio of the densities in the inner and outer layers of the shell. Inhomogeneities bordered by a dense gas are formed in shells with an outwardly decreasing density. If, however, a denser gas is in the outer layer, then cores surrounded by a more rarefied material appear. These results are used to analyze the expansion of the HII region RCW 82. Since the inhomogeneities observed in the 13CO emission in the outer parts of this region have sharply delineated boundaries, our calculations argue for the model of the expansion of a shell with an outwardly decreasing density. The interaction of an accelerating shell with clumps in front of it has also been investigated. The deformations of a clump during its penetration into the shell and the formation of a groove in the shell gradually fillingwith a cold gas have been revealed. Thereafter, the shell material collapses to form a cumulative jet. As applied to the HII region RCW 82, we conclude that the existence of jets is possible if there are inhomogeneities with a scale of ˜1018 cm in the interstellar medium. The lack of data on such jet flows at the boundary of this region is an additional argument for the model where the inhomogeneous structure of the boundaries is attributable to the development of Rayleigh-Taylor instability.

  15. Determination of Alkyl Methanesulfonates in Doxazosin Mesylate by Gas Chromatography-mass Spectrometer.

    Science.gov (United States)

    Sitaram, C; Rupakula, R B; Reddy, B N; Sastry, C S P

    2011-01-01

    High sensitive rapid gas chromatography-mass spectrometry method for the determination of four carcinogenic alkyl methanesulfonates viz. methyl methanesulfonate, ethyl methanesulfonate, isopropyl methanesulfonate and n-butyl methanesulfonate in doxazosin mesylate has been presented by using selective ion monitoring mode. The optimum separation was achieved between methyl methanesulfonate, ethyl methanesulfonate, isopropyl methanesulfonate and n-butyl methanesulfonate on a DB-5 (30 m×0.32 mm×1.0 μm) capillary column under programming temperature. Acetonitrile, water and ammonia (90:9:1 v/v/v) mixture was used as diluent. Various factors involved in the gas chromatography-mass spectrometry method development are also presented. This method was validated as per International Conference on Harmonization guidelines. The limit of quantitation of methyl methanesulfonate, ethyl methanesulfonate, isopropyl methanesulfonate and n-butyl methanesulfonate is 6 ppm with respect to 30 mg/ml of doxazosin mesylate.

  16. Determination of ketone bodies in blood by headspace gas chromatography-mass spectrometry

    DEFF Research Database (Denmark)

    Holm, Karen Marie Dollerup; Linnet, Kristian; Rasmussen, Brian Schou

    2010-01-01

    A gas chromatography-mass spectrometry (GC-MS) method for determination of ketone bodies (ß-hydroxybutyrate, acetone, and acetoacetate) in blood is presented. The method is based on enzymatic oxidation of D-ß-hydroxybutyrate to acetoacetate, followed by decarboxylation to acetone, which was quant......A gas chromatography-mass spectrometry (GC-MS) method for determination of ketone bodies (ß-hydroxybutyrate, acetone, and acetoacetate) in blood is presented. The method is based on enzymatic oxidation of D-ß-hydroxybutyrate to acetoacetate, followed by decarboxylation to acetone, which...... from 98 to 107%, demonstrating the suitability of the method for measuring ketone bodies over a wide concentration range. The method has been applied to cases in which ketoacidosis was suspected as the cause of death in diabetics or chronic alcoholics, as well as to cases in which another cause...

  17. Bioanalysis of the enantiomers of (+/-)-sarin using automated thermal cold-trap injection combined with two-dimensional gas chromatography.

    Science.gov (United States)

    Spruit, H E; Trap, H C; Langenberg, J P; Benschop, H P

    2001-01-01

    A fully automated multidimensional gas chromatographic system with thermal desorption injection and alkali flame detection was developed for analysis of the enantiomers of the nerve agent (+/-)-sarin. The chiral stationary phase was CP Cyclodex B on which the sarin enantiomers were completely resolved. The absolute detection limit was 2.5 pg per enantiomer. The method is intended to be used for the analysis of the sarin enantiomers in biological samples. For this purpose, sarin was isolated from guinea pig blood via solid-phase extraction. Deuterated sarin was used as internal standard. Stabilization of sarin in the blood sample by acidification and addition of an excess of a competitive organophosphorus compound (neopentyl sarin) appeared to be essential. The absolute recovery of the extraction procedure was 60%, whereas the recovery relative to the internal standard was 100%.

  18. Determination of Alkyl Methanesulfonates in Doxazosin Mesylate by Gas Chromatography-mass Spectrometer

    OpenAIRE

    Sitaram, C.; Rupakula, R. B.; Reddy, B. N.; Sastry, C. S. P

    2011-01-01

    High sensitive rapid gas chromatography-mass spectrometry method for the determination of four carcinogenic alkyl methanesulfonates viz. methyl methanesulfonate, ethyl methanesulfonate, isopropyl methanesulfonate and n-butyl methanesulfonate in doxazosin mesylate has been presented by using selective ion monitoring mode. The optimum separation was achieved between methyl methanesulfonate, ethyl methanesulfonate, isopropyl methanesulfonate and n-butyl methanesulfonate on a DB-5 (30 m×0.32 mm×1...

  19. Determination of Carboxypeptidase Activity in Clinical Pathogens by Gas Chromatography?Mass Spectrometry

    OpenAIRE

    Lough, Fraser; Perry, John D.; Stanforth, Stephen P.; Dean, John R.

    2016-01-01

    ABSTRACT A novel method for the determination of benzoic acid has been employed to identify carboxypeptidase activities in clinically relevant pathogens. Benzoic acid was determined after chemical derivatization by gas chromatography?mass spectrometry (GC?MS). N-Benzoyl amino acid substrates were evaluated for the detection of carboxypeptidase activities in a number of clinical pathogens. Upon enzymatic hydrolysis of these substrates, benzoic acid was produced which was detected by extraction...

  20. Physisorption-Based Charge Transfer in Two-Dimensional SnS2 for Selective and Reversible NO2 Gas Sensing.

    Science.gov (United States)

    Ou, Jian Zhen; Ge, Wanyin; Carey, Benjamin; Daeneke, Torben; Rotbart, Asaf; Shan, Wei; Wang, Yichao; Fu, Zhengqian; Chrimes, Adam F; Wlodarski, Wojtek; Russo, Salvy P; Li, Yong Xiang; Kalantar-Zadeh, Kourosh

    2015-10-27

    Nitrogen dioxide (NO2) is a gas species that plays an important role in certain industrial, farming, and healthcare sectors. However, there are still significant challenges for NO2 sensing at low detection limits, especially in the presence of other interfering gases. The NO2 selectivity of current gas-sensing technologies is significantly traded-off with their sensitivity and reversibility as well as fabrication and operating costs. In this work, we present an important progress for selective and reversible NO2 sensing by demonstrating an economical sensing platform based on the charge transfer between physisorbed NO2 gas molecules and two-dimensional (2D) tin disulfide (SnS2) flakes at low operating temperatures. The device shows high sensitivity and superior selectivity to NO2 at operating temperatures of less than 160 °C, which are well below those of chemisorptive and ion conductive NO2 sensors with much poorer selectivity. At the same time, excellent reversibility of the sensor is demonstrated, which has rarely been observed in other 2D material counterparts. Such impressive features originate from the planar morphology of 2D SnS2 as well as unique physical affinity and favorable electronic band positions of this material that facilitate the NO2 physisorption and charge transfer at parts per billion levels. The 2D SnS2-based sensor provides a real solution for low-cost and selective NO2 gas sensing.

  1. Computer extended asymptotic series for the two-dimensional linear hydrodynamics of a gas centrifuge with sources and sinks

    International Nuclear Information System (INIS)

    Berger, M.H.

    1985-07-01

    We have reformulated the general problem of internal flow in a modern, high-speed gas centrifuge with sources and sinks in such a way as to obtain new simple yet rigorous closed form, analytical solutions. Both symmetric and anti-symmetric drives lead to an ode in place of the usual inhomogeneous Onsager pde. Due to the difficulties of exactly solving this sixth order, inhomogeneous, variable coefficient ode, we appeal to the power of perturbation theory and techniques. Two extreme parameter regimes are easily identifiable, the so-called semi-long bowl and short bowl approximations. However, this paper treats only the former class of problems. It is shown that the long bowl solution for axial drive is the correct leading order terms, just like was found for pure thermal drive. New O(1) results are derived for radial, drag and heat drives in 2-D. Then we formally carry out regular asymptotic, even ordered power series expansions for the flow field to O(epsilon 4 ) on the computer so that our approximations are valid for values of epsilon near unity. In the spirit of Van Dyke one could carry out this expansion process, in theory, to apparently arbitrary order to describe the internal flow for arbitrary but finite decay length ratio. Evidently for asymptotically large x* the flow induced by axial and radial forces are proportional. The corresponding separation theory integral parameters are given in a companion paper

  2. Comprehensive two-dimensional gas chromatography in combination with rapid scanning quadrupole mass spectrometry in perfume analysis.

    Science.gov (United States)

    Mondello, Luigi; Casillia, Alessandro; Tranchida, Peter Quinto; Dugo, Giovanni; Dugo, Paola

    2005-03-04

    Single column gas chromatography (GC) in combination with a flame ionization detector (FID) and/or a mass spectrometer is routinely employed in the determination of perfume profiles. The latter are to be considered medium to highly complex matrices and, as such, can only be partially separated even on long capillaries. Inevitably, several monodimensional peaks are the result of two or more overlapping components, often hindering reliable identification and quantitation. The present investigation is based on the use of a comprehensive GC (GC x GC) method, in vacuum outlet conditions, for the near to complete resolution of a complex perfume sample. A rapid scanning quadrupole mass spectrometry (qMS) system, employed for the assignment of GC x GC peaks, supplied high quality mass spectra. The validity of the three-dimensional (3D) GC x GC-qMS application was measured and compared to that of GC-qMS analysis on the same matrix. Peak identification, in all applications, was achieved through MS spectra library matching and the interactive use of linear retention indices (LRI).

  3. All-optical evaluation of spin-orbit interaction based on diffusive spin motion in a two-dimensional electron gas

    Energy Technology Data Exchange (ETDEWEB)

    Kohda, M. [IBM Research–Zürich, Säumerstrasse 4, CH-8803 Rüschlikon (Switzerland); Department of Materials Science, Tohoku University, 980-8579 Sendai (Japan); Altmann, P.; Salis, G. [IBM Research–Zürich, Säumerstrasse 4, CH-8803 Rüschlikon (Switzerland); Schuh, D.; Ganichev, S. D. [Institute of Experimental and Applied Physics, University of Regensburg, D-93040 Regensburg (Germany); Wegscheider, W. [Solid State Physics Laboratory, ETH Zürich, CH-8093 Zürich (Switzerland)

    2015-10-26

    A method is presented that enables the measurement of spin-orbit coefficients in a diffusive two-dimensional electron gas without the need for processing the sample structure, applying electrical currents or resolving the spatial pattern of the spin mode. It is based on the dependence of the average electron velocity on the spatial distance between local excitation and detection of spin polarization, resulting in a variation of spin precession frequency that in an external magnetic field is linear in the spatial separation. By scanning the relative positions of the exciting and probing spots in a time-resolved Kerr rotation microscope, frequency gradients along the [100] and [010] crystal axes of GaAs/AlGaAs QWs are measured to obtain the Rashba and Dresselhaus spin-orbit coefficients, α and β. This simple method can be applied in a variety of materials with electron diffusion for evaluating spin-orbit coefficients.

  4. Determination of steroids, caffeine and methylparaben in water using solid phase microextraction-comprehensive two dimensional gas chromatography-time of flight mass spectrometry.

    Science.gov (United States)

    Lima Gomes, Paulo C F; Barnes, Brian B; Santos-Neto, Álvaro J; Lancas, Fernando M; Snow, Nicholas H

    2013-07-19

    Analysis of several emerging contaminants (steroids, caffeine and methylparaben) in water using automated solid-phase microextraction with comprehensive two dimensional gas chromatography coupled to time of flight mass spectrometry (SPME-GCxGC-ToF/MS) is presented. Experimental design was used to determine the best SPME extraction conditions and the steroids were not derivatized prior to injection. SPME-GCxGC-ToF/MS provided linear ranges from 0.6 to 1200μgL(-1) and limits of detection and quantitation from 0.02 to 100μgL(-1). A series of river water samples obtained locally were subjected to analysis. SPME-GCxGC-ToF/MS is readily automated, straightforward and competitive with other methods for low level analysis of emerging contaminants. Copyright © 2013 Elsevier B.V. All rights reserved.

  5. Enantioselective comprehensive two-dimensional gas chromatography. A route to elucidate the authenticity and origin of Rosa damascena Miller essential oils.

    Science.gov (United States)

    Krupčík, Ján; Gorovenko, Roman; Špánik, Ivan; Sandra, Pat; Armstrong, Daniel W

    2015-10-01

    The analysis of Bulgarian and Turkish Rosa damascena Miller essential oils was performed by flow-modulated comprehensive two-dimensional gas chromatography using simultaneous detection of the second column effluent by flame ionization and quadrupole mass spectrometric detection. Enantioselective separations were obtained by running the samples on 2,3-di-O-ethyl-6-O-tert-butyldimethylsilyl-β-cyclodextrin column as the first column and on polyethylene glycol as the second column. The determination of enantiomeric or diastereomeric excess of some terpenoic solutes is a possible route for quality or authenticity control as well as for the elucidation of the country of origin. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Spin beam splitter based on Goos-Haenchen shifts in two-dimensional electron gas modulated by ferromagnetic and Schottky metal stripes

    Energy Technology Data Exchange (ETDEWEB)

    Lu, Mao-Wang; Huang, Xin-Hong; Zhang, Gui-Lin; Chen, Sai-Yan [College of Science, Guilin University of Technology, Guilin 541004 (China)

    2012-11-15

    We present a theoretical study on the spin-dependent Goos-Haenchen (GH) effect in a two-dimensional electron gas modulated by ferromagnetic and Schottky metal (SM) stripes. The GH shifts for spin electron beams across this device are calculated with the help of the stationary phase method. It is shown that the GH shift of spin-up beam is significantly different from that of spin-down beam, i.e., this device shows up a considerable spin polarization effect in GH shifts of electron beams. It also is shown that both magnitude and sign of spin polarization of GH shifts are closely related to the stripe width, the magnetic strength and the gated voltage under SM stripe. These interesting properties not only provide an effective method of spin injection for spintronics application, but also give rise to a tunable spin beam splitter. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  7. P-Channel InGaN/GaN heterostructure metal-oxide-semiconductor field effect transistor based on polarization-induced two-dimensional hole gas.

    Science.gov (United States)

    Zhang, Kexiong; Sumiya, Masatomo; Liao, Meiyong; Koide, Yasuo; Sang, Liwen

    2016-03-29

    The concept of p-channel InGaN/GaN heterostructure field effect transistor (FET) using a two-dimensional hole gas (2DHG) induced by polarization effect is demonstrated. The existence of 2DHG near the lower interface of InGaN/GaN heterostructure is verified by theoretical simulation and capacitance-voltage profiling. The metal-oxide-semiconductor FET (MOSFET) with Al2O3 gate dielectric shows a drain-source current density of 0.51 mA/mm at the gate voltage of -2 V and drain bias of -15 V, an ON/OFF ratio of two orders of magnitude and effective hole mobility of 10 cm(2)/Vs at room temperature. The normal operation of MOSFET without freeze-out at 8 K further proves that the p-channel behavior is originated from the polarization-induced 2DHG.

  8. The effect of charged quantum dots on the mobility of a two-dimensional electron gas: How important is the Coulomb scattering?

    International Nuclear Information System (INIS)

    Kurzmann, A.; Beckel, A.; Lorke, A.; Geller, M.; Ludwig, A.; Wieck, A. D.

    2015-01-01

    We have investigated the influence of a layer of charged self-assembled quantum dots (QDs) on the mobility of a nearby two-dimensional electron gas (2DEG). Time-resolved transconductance spectroscopy was used to separate the two contributions of the change in mobility, which are: (i) The electrons in the QDs act as Coulomb scatterers for the electrons in the 2DEG. (ii) The screening ability and, hence, the mobility of the 2DEG decreases when the charge carrier density is reduced by the charged QDs, i.e., the mobility itself depends on the charge carrier concentration. Surprisingly, we find a negligible influence of the Coulomb scattering on the mobility for a 2DEG, separated by a 30 nm tunneling barrier to the layer of QDs. This means that the mobility change is completely caused by depletion, i.e., reduction of the charge carrier density in the 2DEG, which indirectly influences the mobility

  9. Visualizing the BEC-BCS crossover in a two-dimensional Fermi gas: Pairing gaps and dynamical response functions from ab initio computations

    Science.gov (United States)

    Vitali, Ettore; Shi, Hao; Qin, Mingpu; Zhang, Shiwei

    2017-12-01

    Experiments with ultracold atoms provide a highly controllable laboratory setting with many unique opportunities for precision exploration of quantum many-body phenomena. The nature of such systems, with strong interaction and quantum entanglement, makes reliable theoretical calculations challenging. Especially difficult are excitation and dynamical properties, which are often the most directly relevant to experiment. We carry out exact numerical calculations, by Monte Carlo sampling of imaginary-time propagation of Slater determinants, to compute the pairing gap in the two-dimensional Fermi gas from first principles. Applying state-of-the-art analytic continuation techniques, we obtain the spectral function and the density and spin structure factors providing unique tools to visualize the BEC-BCS crossover. These quantities will allow for a direct comparison with experiments.

  10. Temperature dependence of DC transport characteristics for a two-dimensional electron gas in an undoped Si/SiGe heterostructure

    Science.gov (United States)

    Chou, Kuan-Yu; Hsu, Nai-Wen; Su, Yi-Hsin; Chou, Chung-Tao; Chiu, Po-Yuan; Chuang, Yen; Li, Jiun-Yun

    2018-02-01

    We investigate DC characteristics of a two-dimensional electron gas (2DEG) in an undoped Si/SiGe heterostructure and its temperature dependence. An insulated-gate field-effect transistor was fabricated, and transfer characteristics were measured at 4 K-300 K. At low temperatures (T tunneling from the buried channel to the surface channel. Finally, the drain current is saturated again at large gate biases due to parallel conduction of buried and surface channels. By increasing the temperature, an abrupt increase in threshold voltage is observed at T ˜ 45 K and it is speculated that negatively charged impurities at the Al2O3/Si interface are responsible for the threshold voltage shift. At T > 45 K, the current saturation and negative transconductance disappear and the device acts as a normal transistor.

  11. Chemometrics-enhanced one-dimensional/comprehensive two-dimensional gas chromatographic analysis for bioactive terpenoids and phthalides in Chaihu Shugan San essential oils.

    Science.gov (United States)

    He, Min; Yang, Zhi-Yu; Yang, Tian-Biao; Ye, Ying; Nie, Juan; Hu, Yong; Yan, Pan

    2017-05-01

    Chemometrics-enhanced one-dimensional/comprehensive two-dimensional gas chromatographic (GC/GC×GC) technologies, were used to explore the compositions of Chaihu Shugan San essential oils, that were extracted from the herbal formulae by different schemes. We have shown that chemometric resolution using gas chromatographic- mass spectrometry (GC-MS) could be used for the qualitative and quantitative analysis of the majority of Terpenoids or Phthalides from herb formulae and single herbs. A GC×GC system was further optimized to achieve the increased peak capacity and the enhanced signal of the hydro-distillation sample (CSSh). When hardware bottleneck resulted from very complex sample, chemometric tools were once again applied to recover the stained information in the second dimension ( 2 D) matrix data. Heuristic evolving latent projections (HELP) could be used for two dimensional (2D) sub-matrixes Xi at n spectral detection channels, after three dimensional (3D) data splitting. For a real 3D data matrix, alternating trilinear decomposition (ATLD) algorithm could conduct regularization for an iterative trilinear decomposition procedure, by Moore-Penrose pseudoinverse computations based on singular value decomposition. After retention indices (RI) confirmation, 216 target analytes (terpenoids or phthalides) could be elucidated both in CSSh and in supercritical fluid extract (CSSs). Based on the obtained data, some potential quality markers (Q-markers) were identified which may affect the quality of the products. Finally, a "connectivity map" was plotted to describe the unique mechanisms of tradition Chinese medicine (TCM). Copyright © 2017 Elsevier B.V. All rights reserved.

  12. Characterization of Volatile Compounds from Ethnic Agave Alcoholic Beverages by Gas Chromatography-Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Pilar Escalante-Minakata

    2008-01-01

    Full Text Available Ethnic Agave alcoholic beverages such as raicilla, sisal, tequila, mezcal, bacanora, sotol and pulque have been analyzed by gas chromatography and headspace solid-phase microextraction- gas chromatography-mass spectrometry (HS-SPME-GC-MS. There were 105 compounds identified, eleven were classified as major compounds and the others were classified as minor compounds. Seventeen minor compounds could be used as authenticity markers since they were beverage specific. Cluster analysis (CA showed that Agave alcoholic beverages could be distinguished by multivariate analysis of major compounds; however, the analysis of minor compounds provided a better fingerprinting.

  13. Two-Dimensional Numerical Simulations of Ultrasound in Liquids with Gas Bubble Agglomerates: Examples of Bubbly-Liquid-Type Acoustic Metamaterials (BLAMMs

    Directory of Open Access Journals (Sweden)

    Christian Vanhille

    2017-01-01

    Full Text Available This work deals with a theoretical analysis about the possibility of using linear and nonlinear acoustic properties to modify ultrasound by adding gas bubbles of determined sizes in a liquid. We use a two-dimensional numerical model to evaluate the effect that one and several monodisperse bubble populations confined in restricted areas of a liquid have on ultrasound by calculating their nonlinear interaction. The filtering of an input ultrasonic pulse performed by a net of bubbly-liquid cells is analyzed. The generation of a low-frequency component from a single cell impinged by a two-frequency harmonic wave is also studied. These effects rely on the particular dispersive character of attenuation and nonlinearity of such bubbly fluids, which can be extremely high near bubble resonance. They allow us to observe how gas bubbles can change acoustic signals. Variations of the bubbly medium parameters induce alterations of the effects undergone by ultrasound. Results suggest that acoustic signals can be manipulated by bubbles. This capacity to achieve the modification and control of sound with oscillating gas bubbles introduces the concept of bubbly-liquid-based acoustic metamaterials (BLAMMs.

  14. Qualitative gas chromatography-mass spectrometry analyses using amines as chemical ionization reagent gases.

    Science.gov (United States)

    Little, James L; Howard, Adam S

    2013-12-01

    Ammonia is a very useful chemical ionization (CI) reagent gas for the qualitative analyses of compounds by positive ion gas chromatography-mass spectrometry (GCMS). The gas is readily available, inexpensive, and leaves no carbon contamination in the MS source. Compounds of interest to our laboratory typically yield abundant protonated or ammoniated species, which are indicative of a compound's molecular weight. Nevertheless, some labile compounds fragment extensively by substitution and elimination reactions and yield no molecular weight information. In these cases, a CI reagent gas mixture of methylamine in methane prepared dynamically was found to be very useful in obtaining molecular weight data. Likewise, deuterated ammonia and deuterated methylamine are useful CI reagent gases for determining the exchangeable protons in organic compounds. Deuterated methylamine CI reagent gas is conveniently prepared by dynamically mixing small amounts of methylamine with excess deuterated ammonia.

  15. Quantification of carbonate by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Tsikas, Dimitrios; Chobanyan-Jürgens, Kristine

    2010-10-01

    Carbon dioxide and carbonates are widely distributed in nature, are constituents of inorganic and organic matter, and are essential in vegetable and animal organisms. CO(2) is the principal greenhouse gas in the atmosphere. In human blood, CO(2)/HCO(3)(-) is an important buffering system. Quantification of bicarbonate and carbonate in inorganic and organic matter and in biological fluids such as blood or blood plasma by means of the GC-MS technology has been impossible so far, presumably because of the lack of suitable derivatization reactions to produce volatile and thermally stable derivatives. Here, a novel derivatization reaction is described for carbonate that allows for its quantification in aqueous alkaline solutions and alkalinized plasma and urine. Carbonate in acetonic solutions of these matrices (1:4 v/v) and added (13)C-labeled carbonate for use as the internal standard were heated in the presence of the derivatization agent pentafluorobenzyl (PFB) bromide for 60 min and 50 °C. Investigations with (12)CO(3)(2-), (13)CO(3)(2-), (CH(3))(2)CO, and (CD(3))(2)CO in alkaline solutions and GC-MS and GC-MS/MS analyses under negative-ion chemical ionization (NICI) or electron ionization (EI) conditions of toluene extracts of the reactants revealed formation of two minor [i.e., PFB-OCOOH and O=CO(2)-(PFB)(2)] and two major [i.e., CH(3)COCH(2)-C(OH)(OPFB)(2) and CH(3)COCH=C(OPFB)(2)] carbonate derivatives. The latter have different retention times (7.9 and 7.5 min, respectively) but virtually identical EI and NICI mass spectra. It is assumed that CH(3)COCH(2)-C(OH)(OPFB)(2) is formed from the reaction of the carbonate dianion with two molecules of PFB bromide to form the diPFB ester of carbonic acid, which further reacts with one molecule of acetone. Subsequent loss of water finally generates the major derivative CH(3)COCH=C(OPFB)(2). This derivatization reaction was utilized to quantify total CO(2)/HCO(3)(-)/CO(3)(2-) (tCO(2)) in human plasma and urine by GC

  16. Integrable two dimensional supersystems

    International Nuclear Information System (INIS)

    Tripathy, K.C.; Tripathy, L.K.

    1988-08-01

    The integrability of two dimensional time-dependent classical systems is examined in N=2 superspace using Dirac's second class constraints. The invariants involving quadratic powers in velocities for super harmonic oscillator and super Kepler potentials have been derived. (author). 5 refs

  17. Evolution of potent odorants within the volatile metabolome of high-quality hazelnuts (Corylus avellana L.): evaluation by comprehensive two-dimensional gas chromatography coupled with mass spectrometry.

    Science.gov (United States)

    Rosso, Marta Cialiè; Liberto, Erica; Spigolon, Nicola; Fontana, Mauro; Somenzi, Marco; Bicchi, Carlo; Cordero, Chiara

    2018-01-09

    Within the pattern of volatiles released by food products (volatilome), potent odorants are bio-active compounds that trigger aroma perception by activating a complex array of odor receptors (ORs) in the regio olfactoria. Their informative role is fundamental to select optimal post-harvest and storage conditions and preserve food sensory quality. This study addresses the volatile metabolome from high-quality hazelnuts (Corylus avellana L.) from the Ordu region (Turkey) and Tonda Romana from Italy, and investigates its evolution throughout the production chain (post-harvest, industrial storage, roasting) to find functional correlations between technological strategies and product quality. The volatile metabolome is analyzed by headspace solid-phase microextration combined with comprehensive two-dimensional gas chromatography and mass spectrometry. Dedicated pattern recognition, based on 2D data (targeted fingerprinting), is used to mine analytical outputs, while principal component analysis (PCA), Fisher ratio, hierarchical clustering, and analysis of variance are used to find decision makers among the most informative chemicals. Low-temperature drying (18-20 °C) has a decisive effect on quality; it correlates negatively with bacteria and mold metabolic activity, nut viability, and lipid oxidation products (2-methyl-1-propanol, 3-methyl-1-butanol, 2-ethyl-1-hexanol, 2-octanol, 1-octen-3-ol, hexanal, octanal and (E)-2-heptanal). Protective atmosphere storage (99% N 2 -1% O 2 ) effectively limits lipid oxidation for 9-12 months after nut harvest. The combination of optimal drying and storage preserves the aroma potential; after roasting at different shelf-lives, key odorants responsible for malty and buttery (2- and 3-methylbutanal, 2,3-butanedione and 2,3-pentanedione), earthy (methylpyrazine, 2-ethyl-5-methyl pyrazine and 3-ethyl-2,5-dimethyl pyrazine) and caramel-like and musty notes (2,5-dimethyl-4-hydroxy-3(2H)-furanone - furaneol and acetyl pyrrole) show no

  18. Determination of polar pharmaceuticals in sewage water of Greece by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Koutsouba, V; Heberer, Th; Fuhrmann, B; Schmidt-Baumler, K; Tsipi, D; Hiskia, A

    2003-04-01

    Sewage influents and effluents of different urban areas of Greece, were analyzed for polar pharmaceutical residues, used in human medicine. Drugs investigated were the anti-inflammatory drugs diclofenac and ibuprofen, the metabolite of the drugs clofibrates used as blood lipid regulators, clofibric acid and the analgesics phenazone and propyphenazone. Analysis was carried out using capillary gas chromatography-mass spectrometry with selected ion monitoring. The method used was involved solid phase extraction (C(18)) and derivatization with pentafluorobenzyl bromide. Diclofenac was detected in every sewage effluent sample.

  19. Determination of ketone bodies in blood by headspace gas chromatography-mass spectrometry

    DEFF Research Database (Denmark)

    Holm, Karen Marie Dollerup; Linnet, Kristian; Rasmussen, Brian Schou

    2010-01-01

    A gas chromatography-mass spectrometry (GC-MS) method for determination of ketone bodies (ß-hydroxybutyrate, acetone, and acetoacetate) in blood is presented. The method is based on enzymatic oxidation of D-ß-hydroxybutyrate to acetoacetate, followed by decarboxylation to acetone, which...... was quantified by the use of headspace GC-MS using acetone-(13)C(3) as an internal standard. The developed method was found to have intra- and total interday relative standard deviations acetone+acetoacetate levels (~25 to 8300 µM) and D-ß-hydroxybutyrate levels (~30 to 16500 µM). Recovery values varied...

  20. Gas chromatography/mass spectrometry characterization of historical varnishes of ancient Italian lutes and violin.

    Science.gov (United States)

    Echard, J P; Benoit, C; Peris-Vicente, J; Malecki, V; Gimeno-Adelantado, J V; Vaiedelich, S

    2007-02-12

    The organic constituents of historical vanishes from two ancient Italian lutes and a Stradivari violin, kept in the Musée de la musique in Paris, have been characterized using gas chromatography-mass spectrometry. Results have been compared with the chromatograms and mass spectra of recent as well as old naturally aged reference materials. The three historical varnishes analyzed have been shown to be oil varnishes, probably mixtures of linseed oil with resins. Identification of diterpenoids and triterpenoids compounds, and of the resins that may have been ingredients of the varnishes, are discussed in this paper.

  1. Chemical characterization using gas chromatography/mass spectrometry of two extracts from Phyllanthus orbicularis HBK

    International Nuclear Information System (INIS)

    Gutierrez Gaiten, Yamilet Irene; Miranda Martinez, Migdalia; Bello Alarcon, Adonis

    2011-01-01

    The objective of this paper was the chemical characterization of two extracts from Phyllanthus orbicularis HBK through gas chromatography/mass spectrometry. To this end, maceration with N-hexane and ethyl acetate was used to obtain the respective extracts. The study of the hexane extract identified 17 components in which hydrocarbonate structures prevailed, mainly cyclooctacosane. In the ethyl acetate extract, 19 compounds were detected, being the terpenoids the predominant, although the most abundant was sterol g-sitosterol. For the first time, the identified compounds are reported for this species

  2. Analysis of the anthraquinones aloe-emodin and aloin by gas chromatography/mass spectrometry.

    Science.gov (United States)

    ElSohly, Mahmoud A; Gul, Waseem; Murphy, Timothy P

    2004-12-20

    A procedure was developed for the determination of low levels of the anthraquinones aloe-emodin and aloin A (barbalin) in aloe products based on gas chromatography/mass spectrometry (GC/MS) of the trimethyl silyl (TMS) derivatives of these analytes in the presence of Chrysophanol used as internal standard. The method was used to analyze several aloe based commercial products (liquids, gels and solids). Wide variation in the level of these anthraquinones was observed among the different products. The method had a sensitivity of 0.005 ppm of aloe-emodin and 0.05 ppm of aloin.

  3. Determination of cocaine in brazilian paper currency by capillary gas chromatography/mass spectrometry

    Directory of Open Access Journals (Sweden)

    Enrico Di Donato

    2007-01-01

    Full Text Available The presence of illicit drugs such as cocaine and marijuana in US paper currency is very well demonstrated. However, there is no published study describing the presence of cocaine and/or other illicit drugs in Brazilian paper currency. In this study, Brazilian banknotes were collected from nine cities, extracted and analyzed by capillary gas chromatography/mass spectrometry, in order to investigate the presence of cocaine. Bills were extracted with deionized water followed by ethyl acetate. Results showed that 93% of the bills presented cocaine in a concentration range of 2.38-275.10 µg/bill.

  4. Gas chromatography/mass spectrometry and pyrolysis-gas chromatography/mass spectrometry for the chemical characterisation of modern and archaeological figs (Ficus carica).

    Science.gov (United States)

    Ribechini, Erika; Pérez-Arantegui, Josefina; Colombini, Maria Perla

    2011-06-24

    Gas chromatography/mass spectrometry (GC/MS) after alkaline hydrolysis, solvent extraction and trimethylsilylation, and analytical pyrolysis using hexamethyldisilazane (HMDS) for in situ derivatisation followed by gas chromatographic/mass spectrometric analysis (Pyrolysis-silylation-GC/MS) were used to investigate the hydrolysable and soluble constituents, and the polymerised macromolecules of an archaeological fig (Ficus carica) recovered in Zaragoza (Spain), as well as of modern figs. The main aim was to study the compositional alterations undergone by the fig tissues in a particular archaeological environment: the fig was in a vessel and covered by a layer of a mixture of orpiment and gypsum. A comparison between the GC/MS results from modern and archaeological figs revealed that degradative reactions took place, leading to the disappearance/depletion of reactive (unsaturated fatty acids) and sensitive compounds (phytosterols and triterpenes). Py-silylation-GC/MS data provided evidence of a significant degradation of the saccharide and lipid components of the fig tissue, which left a residue enriched in polyphenols and polyesters. Copyright © 2011 Elsevier B.V. All rights reserved.

  5. Scattering times in the two-dimensional electron gas of AlxGa1-xN/AlN/GaN heterostructures

    International Nuclear Information System (INIS)

    Han Xiuxun; Honda, Yoshio; Narita, Tetsuo; Yamaguchi, Masahito; Sawaki, Nobuhiko; Tanaka, Tooru; Guo Qixin; Nishio, Mitsushiro

    2009-01-01

    Low-field Hall and Shubnikov-de Haas (SdH) measurements were performed on two-dimensional electron gas of Al 0.24 Ga 0.76 N/GaN and Al 0.24 Ga 0.76 N/AlN/GaN heterostructures at a low temperature. A dramatic improvement in electron mobility is observed in Al 0.24 Ga 0.76 N/AlN/GaN heterostructures with 1 and 2 nm thick AlN interlayers. A further increase in the AlN thickness degrades the transport behaviour. Transport and quantum scattering times were derived from the corresponding Hall mobility and the oscillatory part of the SdH signal. The ratio of the transport scattering time and the quantum scattering time increases from 3.87 in the heterostructure without the AlN interlayer to 14.34 with the 1 nm AlN interlayer and to 12.45 with the 2 nm AlN interlayer. A modified scattering calculation due to charged dislocation with a finite length suggests that dislocation related long-range scattering event tends to dominate both transport and quantum scattering times when a thin AlN interlayer is introduced.

  6. Effect of asymmetric interface on charge and spin transport across two dimensional electron gas with Dresselhaus spin-orbit coupling/ferromagnet junction

    Science.gov (United States)

    Srisongmuang, B.; Pasanai, K.

    2018-04-01

    We theoretically studied the effect of interfacial scattering on the transport of charge and spin across the junction of a two-dimensional electron gas with Dresselhaus spin-orbit coupling and ferromagnetic material junction, via the conductance (G) and the spin-polarization of the conductance spectra (P) using the scattering method. At the interface, not only were the effects of spin-conserving (Z0) and spin-flip scattering (Zf) considered, but also the interfacial Rashba spin-orbit coupling scattering (ZRSOC) , which was caused by the asymmetry of the interface, was taken into account, and all of them were modeled by the delta potential. It was found that G was suppressed with increasing Z0 , as expected. Interestingly, a particular value of Zf can cause G and P to reach a maximum value. In particular, ZRSOC plays a crucial role to reduce G and P in the metallic limit, but its influence on the tunneling limit was quite weak. On the other hand, the effect of ZRSOC was diminished in the tunneling limit of the magnetic junction.

  7. Identification and classification of components in flash pyrolysis oil and hydrodeoxygenated oils by two-dimensional gas chromatography and time-of-flight mass spectrometry.

    Science.gov (United States)

    Marsman, J H; Wildschut, J; Evers, P; de Koning, S; Heeres, H J

    2008-04-18

    Hydrodeoxygenated pyrolysis oils (HDO) are considered promising renewable liquid energy carriers. To gain insights in the various reaction pathways taking place during the hydrodeoxygenation reaction of pyrolysis oil, two-dimensional gas chromatography with time-of-flight mass spectrometric analyses (2D-GC-TOF-MS) was applied on the feedstock and product oil. Chromatographic parameters like injection temperature and column choice of the 1D-(2)D ensemble are discussed. Fractionation of the oils by hexane extraction was applied to show the distribution of analytes over the phases. Some 1000 and 2000 components in the pyrolysis and HDO oil, respectively could be identified and classified. The TOF-MS detection considerably improved the understanding of the molecular distribution over the 1D-(2)D retention time fields in the contour plot, in order to classify the analytes in functional groups. By group-type classification of the main components (>0.3% relative area), it was possible to characterize the oils by 250 and 350 analytes, respectively pyrolysis oil and HDO oil, describing 75% of the chromatographable fraction. The 2D-GC-TOF-MS method showed to be a useful and fast technique to determine the composition of (upgraded) pyrolysis oil and is potentially a very useful tool for exploratory catalyst research and kinetic studies. The 2D-GC-TOF-MS technique is not only useful for the chemical study as such, but also provides the basic knowledge for method transfer to a 2D-GC-FID (flame ionization detector) application.

  8. Chemometrics-assisted effect-directed analysis of crude and refined oil using comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry.

    Science.gov (United States)

    Radović, Jagoš R; Thomas, Kevin V; Parastar, Hadi; Díez, Sergi; Tauler, Romà; Bayona, Josep M

    2014-01-01

    An effect-directed analysis (EDA) of fresh and artificially weathered (evaporated, photooxidized) samples of North Sea crude oil and residual heavy fuel oil is presented. Aliphatic, aromatic, and polar oil fractions were tested for the presence of aryl hydrocarbon receptor (AhR) agonist and androgen receptor (AR) antagonist, demonstrating for the first time the AR antagonist effects in the aromatic and, to a lesser extent, polar fractions. An extension of the typical EDA strategy to include an N-way partial least-squares (N-PLS) model capable of relating the comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry (GC × GC-TOFMS) data set to the bioassay data obtained from normal-phase LC fractions is proposed. The predicted AhR binding effects in the fresh and artificially weathered aromatic oil fractions facilitated the identification of alkyl-substituted three- and four-ring aromatic systems in the active fractions through the weighting of their contributions to the observed effects. A N-PLS chemometric model is demonstrated as a potentially useful strategy for future EDA studies that can streamline the compound identification process and provide additional reduction of samples' complexity. The AhR binding effects of the suspected compounds predicted by N-PLS and identified by GC × GC-TOFMS were confirmed using quantitative structure-activity relationship (QSAR) estimates.

  9. Comprehensive two-dimensional gas chromatography coupled to high resolution time-of-flight mass spectrometry for screening of organohalogenated compounds in cat hair.

    Science.gov (United States)

    Brits, Martin; Gorst-Allman, Peter; Rohwer, Egmont R; De Vos, Jayne; de Boer, Jacob; Weiss, Jana M

    2018-02-09

    The coupling of comprehensive two-dimensional gas chromatography with high-resolution time-of-flight mass spectrometry offers the best separation efficiency combined with accurate mass measurements over a wide mass range. The tremendous power of this screening tool is illustrated by trace qualitative screening analysis of organohalogenated compounds (OHCs) in pet cat hair. Tentative identification was supported by mass spectral database searches and elemental formula prediction from the experimentally determined accurate mass data. This screening approach resulted in the first tentative identification of pentabromoethylbenzene, decabromodiphenyl ethane, hexabromocyclododecane, trisbromoneopentyl alcohol, tris(2-chloroethyl) phosphate and tris(2-chloroisopropyl)phosphate in the South African indoor environment. A total of seventy-two OHCs were identified in the samples and include known flame retardants, such as polybrominated diphenyl ethers, and legacy contaminants such as polychlorinated biphenyls and organochlorine, organophosphorous and pyrethroid pesticides. The results obtained from cat hair indicate that these pets are exposed to complex mixtures of OHCs and the detection of these compounds suggests that non-invasive cat hair samples can be used to model indoor exposure with reference to external deposition of OHCs present in the air and dust surrounding people. Toddlers share the same environment as pet cats and therefore also the same health risks. Copyright © 2017 Elsevier B.V. All rights reserved.

  10. Diamondoid Characterization in Condensate by Comprehensive Two-Dimensional Gas Chromatography with Time-of-Flight Mass Spectrometry: The Junggar Basin of Northwest China

    Science.gov (United States)

    Li, Shuifu; Hu, Shouzhi; Cao, Jian; Wu, Ming; Zhang, Dongmei

    2012-01-01

    Diamondoids in crude oil are useful for assessing the maturity of oil in high maturation. However, they are very difficult to separate and accurately quantify by conventional geochemical methods due to their low abundance in oil. In this paper, we use comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry (GC×GC-TOFMS) to study the compounds in condensates from the Junggar Basin of northwest China and address their geological and geochemical applications. GC×GC-TOFMS improves the resolution and separation efficiency of the compounds. It not only separates the compounds that coelute in conventional GC-MS (e.g., 4, 8-dimethyl-diamantane and trimethyl-diamantane) but also allows the identification of compounds that were not previously detected (e.g., trimethyl-diamantane (15A)). A reversed-phase column system improves the separation capabilities over the normal phase column system. The diamondoid indexes indicate that a representative condensate from Well DX 10 is highly mature with equivalent Ro being approximately 1.5%. PMID:23109861

  11. Analysis of alkyl phosphates in petroleum samples by comprehensive two-dimensional gas chromatography with nitrogen phosphorus detection and post-column Deans switching.

    Science.gov (United States)

    Nizio, Katie D; Harynuk, James J

    2012-08-24

    Alkyl phosphate based gellants used as viscosity builders for fracturing fluids used in the process of hydraulic fracturing have been implicated in numerous refinery-fouling incidents in North America. In response, industry developed an inductively coupled plasma optical emission spectroscopy (ICP-OES) based method for the analysis of total volatile phosphorus in distillate fractions of crude oil; however, this method is plagued by poor precision and a high limit of detection (0.5±1μg phosphorus mL(-1)). Furthermore this method cannot provide speciation information, which is critical for developing an understanding of the challenge of alkyl phosphates at a molecular level. An approach using comprehensive two-dimensional gas chromatography with nitrogen phosphorus detection (GC×GC-NPD) and post-column Deans switching is presented. This method provides qualitative and quantitative profiles of alkyl phosphates in industrial petroleum samples with increased precision and at levels comparable to or below those achievable by ICP-OES. A recovery study in a fracturing fluid sample and a profiling study of alkyl phosphates in four recovered fracturing fluid/crude oil mixtures (flowback) are also presented. Copyright © 2012 Elsevier B.V. All rights reserved.

  12. A new approach to determine vapor pressures of compounds in multicomponent systems by comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry.

    Science.gov (United States)

    Parshintsev, Jevgeni; Lai, Ching Kwan; Hartonen, Kari; Kulmala, Markku; Riekkola, Marja-Liisa

    2014-06-01

    A method is described to determine vapor pressures of compounds in multicomponent systems simultaneously. The method is based on temperature-gradient analysis by comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GCxGC-TOFMS). Vapor pressures are determined with the aid of known vapor pressure values of reference compounds eluting before and after the analytes. Reference compounds with the same functionalities as the analytes are preferred, but when these are not available, the alkane series can be utilized. The number of compounds whose vapor pressures can be determined is limited only by the peak capacity of the chromatographic system. Although the lowest subcooled vapor pressure determined was 0.006 Pa, for tetrahydroaraucarolone in an atmospheric aerosol sample, vapor pressures as low as 10(-6) Pa can be measured with the described set-up. Even lower values can be measured with higher GC temperatures and longer analysis times. Since only a few picograms of compound is required, in a mixture of any complexity, the GCxGC-TOFMS method offers unique sensitivity, rapidity, and comprehensiveness. Copyright © 2014 Elsevier B.V. All rights reserved.

  13. Metabolomics strategy for the mapping of volatile exometabolome from Saccharomyces spp. widely used in the food industry based on comprehensive two-dimensional gas chromatography.

    Science.gov (United States)

    Martins, Cátia; Brandão, Tiago; Almeida, Adelaide; Rocha, Sílvia M

    2017-05-01

    Saccharomyces spp. are widely used in the food and beverages industries. Their cellular excreted metabolites are important for general quality of products and can contribute to product differentiation. This exploratory study presents a metabolomics strategy for the comprehensive mapping of cellular metabolites of two yeast species, Saccharomyces cerevisiae and S. pastorianus (both collected in an industrial context) through a multidimensional chromatography platform. Solid-phase microextraction was used as a sample preparation method. The yeast viability, a specific technological quality parameter, was also assessed. This untargeted analysis allowed the putative identification of 525 analytes, distributed over 14 chemical families, the origin of which may be explained through the pathways network associated with yeasts metabolism. The expression of the different metabolic pathways was similar for both species, event that seems to be yeast genus dependent. Nevertheless, these species showed different growth rates, which led to statistically different metabolites content. This was the first in-depth approach that characterizes the headspace content of S. cerevisiae and S. pastorianus species cultures. The combination of a sample preparation method capable of providing released volatile metabolites directly from yeast culture headspace with comprehensive two-dimensional gas chromatography was successful in uncovering a specific metabolomic pattern for each species. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Comprehensive two-dimensional gas chromatography and three-dimensional fluorometry for detection of volatile and bioactive substances in some berries.

    Science.gov (United States)

    Dymerski, Tomasz; Namieśnik, Jacek; Vearasilp, Kann; Arancibia-Avila, Patricia; Toledo, Fernando; Weisz, Moshe; Katrich, Elena; Gorinstein, Shela

    2015-03-01

    The volatile fractions of Cape gooseberry and blueberry were determined by headspace solid-phase microextraction coupled with comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry (HS-SPME/GC×GC-TOFMS). The highest amount of alcohol (51.8%), ester (32.8%) and carboxylic acid (6.9%) was in blueberry in comparison with gooseberry and oppositely ketones (14.7%), aldehydes (9.9%) and terpenes (8%) were found in gooseberry. The bioactive compounds and antioxidant capacities were higher in blueberries than in gooseberries. Three dimensional fluorescence emission spectrometry (3D-FL) was applied to determine and to compare experimentally found binding parameters of berries extracts with human serum albumin (HSA). The fluorescence quenching of HSA by polyphenols from berries was a result of the formation of a polyphenol-HSA complex. The binding abilities of berries were highly correlated with the bioactivity of polyphenols and volatile substances. The cluster analysis (CA) and linear discriminant analysis (LDA) was applied to differentiate the berries samples according to their type. Copyright © 2014 Elsevier B.V. All rights reserved.

  15. Study of alkyl phosphates in industrial petroleum mixtures by comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry.

    Science.gov (United States)

    Harynuk, James J; Rossé, Aleisha D; McGarvey, G Bryce

    2011-11-01

    Dialkyl phosphate esters used as gellants in some oil well fracturing processes for conventional oil production can result in contamination of the collected crude. Though the exact mechanism is unclear, such compounds form volatile phosphorus that compromises refinery processes. Our initial research involved producing a comprehensive two-dimensional gas chromatographic method (GC × GC) for the detection and quantification of alkyl phosphate esters in petroleum samples, which surpassed the current method employed in sensitivity and speciation capabilities. However, selective detection is required for such analytes in petroleum matrices. This article describes the application of GC × GC with time-of-flight mass spectrometry for selective detection to the analysis of di- and tri-alkyl phosphates in petroleum samples. Features in the electron impact mass spectra of alkyl phosphates are discussed along with the GC × GC retention characteristics of the compounds. Based on these discussions, a preliminary classification and quantification of alkyl phosphate contamination in a suite of industrial samples is then presented.

  16. Temperature dependence of photogalvanic effect in GaAs/AlGaAs two-dimensional electron gas at interband and intersubband excitation

    Science.gov (United States)

    Zeng, X. L.; Yu, J. L.; Cheng, S. Y.; Lai, Y. F.; Chen, Y. H.; Huang, W.

    2017-05-01

    The linear (LPGE) and circular photogalvanic effects (CPGE), induced by interband (532 nm) and intersubband (1064 nm) excitation, have been investigated in a temperature range from 77 to 300 K in GaAs/AlGaAs two-dimensional electron gas. The temperature dependences of the CPGE current induced by Rashba and Dresselhaus spin orbit coupling (SOC) under the interband and intersubband excitation are obtained, respectively. It is revealed that the CPGE and LPGE current induced by the intersubband excitation almost increases with increasing temperature, while that induced by interband excitation nearly decreases with increasing temperatures. These phenomena may be attributed to the different variation trends of photo-induced carrier density and SOC with increasing temperatures between interband and intersubband excitation. The evolutions of the ratio of the Rashba and Dresselhaus SOC (RD ratios) and the anisotropic ratio of linear photogalvanic tensors, corresponding to the interband and intersubband excitations, with temperatures are determined. The power dependence of CPGE and LPGE current induced by intersubband excitation is also investigated. It is found that for the power range from 0 to 275 mW, the CPGE current nearly increases linearly with increasing power, while the LPGE current shows a decreasing generation rate at higher power. This study also provides a method to manipulate the photogalvanic effects by temperatures and by using excitation light of different wavelengths.

  17. Analysis of honeybush tea (Cyclopia spp.) volatiles by comprehensive two-dimensional gas chromatography using a single-stage thermal modulator.

    Science.gov (United States)

    Ntlhokwe, Gaalebalwe; Tredoux, Andreas G J; Górecki, Tadeusz; Edwards, Matthew; Vestner, Jochen; Muller, Magdalena; Erasmus, Lené; Joubert, Elizabeth; Christel Cronje, J; de Villiers, André

    2017-07-01

    The applicability of comprehensive two-dimensional gas chromatography (GC×GC) using a single-stage thermal modulator was explored for the analysis of honeybush tea (Cyclopia spp.) volatile compounds. Headspace solid phase micro-extraction (HS-SPME) was used in combination with GC×GC separation on a non-polar × polar column set with flame ionisation (FID) detection for the analysis of fermented Cyclopia maculata, Cyclopia subternata and Cyclopia genistoides tea infusions of a single harvest season. Method optimisation entailed evaluation of the effects of several experimental parameters on the performance of the modulator, the choice of columns in both dimensions, as well as the HS-SPME extraction fibre. Eighty-four volatile compounds were identified by co-injection of reference standards. Principal component analysis (PCA) showed clear differentiation between the species based on their volatile profiles. Due to the highly reproducible separations obtained using the single-stage thermal modulator, multivariate data analysis was simplified. The results demonstrate both the complexity of honeybush volatile profiles and the potential of GC×GC separation in combination with suitable data analysis techniques for the investigation of the relationship between sensory properties and volatile composition of these products. The developed method therefore offers a fast and inexpensive methodology for the profiling of honeybush tea volatiles. Graphical abstract Surface plot obtained for the GC×GC-FID analysis of honeybush tea volatiles.

  18. Two-dimensional calculus

    CERN Document Server

    Osserman, Robert

    2011-01-01

    The basic component of several-variable calculus, two-dimensional calculus is vital to mastery of the broader field. This extensive treatment of the subject offers the advantage of a thorough integration of linear algebra and materials, which aids readers in the development of geometric intuition. An introductory chapter presents background information on vectors in the plane, plane curves, and functions of two variables. Subsequent chapters address differentiation, transformations, and integration. Each chapter concludes with problem sets, and answers to selected exercises appear at the end o

  19. Characterisation of dense non-aqueous phase liquids of coal tar using comprehensive two-dimensional gas chromatography coupled with time of flight mass spectrometry.

    Science.gov (United States)

    Gauchotte-Lindsay, Caroline; McGregor, Laura; Richards, Phil; Kerr, Stephanie; Glenn, Aliyssa; Thomas, Russell; Kalin, Robert

    2013-04-01

    Comprehensive two-dimensional gas chromatography (GCxGC) is a recently developed analytical technique in which two capillary columns with different stationary phases are placed in series enabling planar resolution of the analytes. The resolution power of GCxGC is one order of magnitude higher than that of one dimension gas chromatography. Because of its high resolution capacity, the use of GCxGC for complex environmental samples such as crude oils, petroleum derivatives and polychlorinated biphenyls mixtures has rapidly grown in recent years. We developed a one-step method for the forensic analysis of coal tar dense non-aqueous phase liquids (DNAPLs) from former manufactured gas plant (FMGP) sites. Coal tar is the by-product of the gasification of coal for heating and lighting and it is composed of thousands of organic and inorganic compounds. Before the boom of natural gases and oils, most towns and cities had one or several manufactured gas plants that have, in many cases, left a devastating environmental print due to coal tar contamination. The fate of coal tar DNAPLs, which can persist in the environment for more than a hundred years, is therefore of crucial interest. The presented analytical method consists of a unique clean-up/ extraction stage by pressurized liquid extraction and a single analysis of its organic chemical composition using GCxGC coupled with time of flight mass spectrometry (TOFMS). The chemical fingerprinting is further improved by derivatisation by N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) of the tar compounds containing -OH functions such as alcohols and carboxylic acids. We present here how, using the logical order of elution in GCxGC-TOFMS system, 1) the identification of never before observed -OH containing compounds is possible and 2) the isomeric selectivity of an oxidation reaction on a DNAPL sample can be revealed. Using samples collected at various FMGP sites, we demonstrate how this GCxGC method enables the simultaneous

  20. Two-dimensional ferroelectrics

    Energy Technology Data Exchange (ETDEWEB)

    Blinov, L M; Fridkin, Vladimir M; Palto, Sergei P [A.V. Shubnikov Institute of Crystallography, Russian Academy of Sciences, Moscow, Russian Federaion (Russian Federation); Bune, A V; Dowben, P A; Ducharme, Stephen [Department of Physics and Astronomy, Behlen Laboratory of Physics, Center for Materials Research and Analysis, University of Nebraska-Linkoln, Linkoln, NE (United States)

    2000-03-31

    The investigation of the finite-size effect in ferroelectric crystals and films has been limited by the experimental conditions. The smallest demonstrated ferroelectric crystals had a diameter of {approx}200 A and the thinnest ferroelectric films were {approx}200 A thick, macroscopic sizes on an atomic scale. Langmuir-Blodgett deposition of films one monolayer at a time has produced high quality ferroelectric films as thin as 10 A, made from polyvinylidene fluoride and its copolymers. These ultrathin films permitted the ultimate investigation of finite-size effects on the atomic thickness scale. Langmuir-Blodgett films also revealed the fundamental two-dimensional character of ferroelectricity in these materials by demonstrating that there is no so-called critical thickness; films as thin as two monolayers (1 nm) are ferroelectric, with a transition temperature near that of the bulk material. The films exhibit all the main properties of ferroelectricity with a first-order ferroelectric-paraelectric phase transition: polarization hysteresis (switching); the jump in spontaneous polarization at the phase transition temperature; thermal hysteresis in the polarization; the increase in the transition temperature with applied field; double hysteresis above the phase transition temperature; and the existence of the ferroelectric critical point. The films also exhibit a new phase transition associated with the two-dimensional layers. (reviews of topical problems)

  1. Determination of gas phase triacetone triperoxide with aspiration ion mobility spectrometry and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Räsänen, Riikka-Marjaana; Nousiainen, Marjaana; Peräkorpi, Kaleva; Sillanpää, Mika; Polari, Lauri; Anttalainen, Osmo; Utriainen, Mikko

    2008-08-08

    Aspiration ion mobility spectrometry (IMS) has been used for the first time to screen 3,3,6,6,9,9-hexamethyl-1,2,4,5,7,8-hexaoxacyclononane explosive, the most commonly known as triacetone triperoxide (TATP). Gaseous TATP was generated from synthesized solid compound, sublimed and directed to a portable chemical detection system comprised of an aspiration-type IMS detector and six semiconductor sensors. Different unknown TATP gas phase concentrations were produced and corresponding IMS and semiconductor responses were measured. The experimental concentrations were determined by gas chromatography-mass spectrometry (GC-MS). The results evidenced that the monitored compound in the gas phase was TATP. In addition, the determined TATP concentrations and corresponding IMS intensities showed that the IMS response values were proportional to the measured TATP concentrations.

  2. Thermal desorption comprehensive two-dimensional gas chromatography coupled to time of flight mass spectrometry for vapour phase mainstream tobacco smoke analysis.

    Science.gov (United States)

    Savareear, Benjamin; Brokl, Michał; Wright, Chris; Focant, Jean-Francois

    2017-11-24

    A thermal desorption comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (TD-GC×GC-TOFMS) method has been developed for the analysis of mainstream tobacco smoke (MTS) vapour phase (VP). The selection process of the sample introduction approach involved comparing the results obtained from three different approaches: a) use of gas sampling bag followed by SPME (Tedlar ® -SPME), b) gas sampling bag followed by TD (Tedlar ® -TD), and c) sampling directly on TD sorbents (Direct-TD). Six different SPME fibers and six different TD sorbent beds were evaluated for the extraction capacities in terms of total number of peaks and related intensities or peak areas. The best results were obtained for the Direct-TD approach using Tenax TA/Carbograph1TD/Carboxen1003 sorbent tubes. The optimisation of TD tube desorption parameters was carried out using a face-centered central composite experimental design and resulted in the use of the Tenax TA/Carbograph 1TD/Carboxen 1003 sorbent with a 7.5min desorption time, a 60mL/min tube desorption flow, and a 250°C tube desorption temperature. The optimised method was applied to the separation of MTS-VP constituents, with 665 analytes detected. The method precision ranged from 1% to 15% for over 99% of identified peak areas and from 0% to 3% and 0% to 1% for both first ( 1 t R ) and second ( 2 t R ) dimension retention times, respectively. The method was applied to the analyses of two cigarette types differing in their filter construction. Principal component analysis (PCA) allowed a clear differentiation of the studied cigarette types (PC1 describing 94% of the explained variance). Supervised Fisher ratio analysis permitted the identification of compounds responsible for the chemical differences between the two sample types. A set of 91 most relevant compounds was selected by applying a Fisher ratio cut-off approach and most of them were selectively removed by one of the cigarette filter types

  3. Comparison of two algorithmic data processing strategies for metabolic fingerprinting by comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry.

    Science.gov (United States)

    Almstetter, Martin F; Appel, Inka J; Dettmer, Katja; Gruber, Michael A; Oefner, Peter J

    2011-09-28

    The alignment algorithm Statistical Compare (SC) developed by LECO Corporation for the processing of comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry (GC×GC-TOFMS) data was validated and compared to the in-house developed retention time correction and data alignment tool INCA (Integrative Normalization and Comparative Analysis) by a spike-in experiment and the comparative metabolic fingerprinting of a wild type versus a double mutant strain of Escherichia coli (E. coli). Starting with the same peak lists generated by LECO's ChromaTOF software, the accuracy of peak alignment and detection of 1.1- to 4-fold changes in metabolite concentration was assessed by spiking 20 standard compounds into an aqueous methanol extract of E. coli. To provide the same quality input signals for both alignment routines, the universal m/z 73 trace of the trimethylsilyl (TMS) group was used as a quantitative measure for all features. The performance of data processing and alignment was evaluated and illustrated by ROC curves. Statistical Compare performed marginally better at the lower fold changes, while INCA did so at the higher fold changes. Using SC, quantitative precision could be improved substantially by exploiting the signal intensities of metabolite-specific unique (U) m/z ion traces rather than the universal m/z 73 trace. A list of 56 features that distinguished the two E. coli strains was obtained by the SC alignment using m/z U with an estimated false discovery rate (FDR) of <0.05. Ultimately, 23 metabolites could be identified, one additional and five less than with INCA due to the failure of SC to extract unitized m/z U's across all fingerprints with suitable spectral intensities for the latter metabolites. Copyright © 2011 Elsevier B.V. All rights reserved.

  4. Evaluation of a single-stage consumable-free modulator for comprehensive two-dimensional gas chromatography: analysis of polychlorinated biphenyls, organochlorine pesticides and chlorobenzenes.

    Science.gov (United States)

    Muscalu, Alina M; Edwards, Matthew; Górecki, Tadeusz; Reiner, Eric J

    2015-04-24

    Comprehensive two-dimensional gas chromatography (GC×GC) has been rapidly growing in popularity. The GC×GC separation is performed by interfacing a modulator between two columns of different selectivities. The modulator periodically traps and then re-injects the analytes eluting from the first column into the second column. The most popular GC×GC systems require consumables such as liquid N2 for the trapping function of the modulator. Although these systems are very effective, their costs are a hindrance to more widespread use. A new, single-stage thermal modulator for GC×GC that requires no consumables has been developed and tested. The device traps analytes using a proprietary stainless steel capillary trap compressed between two ceramic cooling pads. Analytes are thermally desorbed from the trap into the second column via resistive heating. To evaluate this system, a routine accredited method for the analysis of polychlorinated biphenyls, organochlorine pesticides and chlorobenzenes was run using the new modulator and its performance was compared to that of an industry standard modulation system. Within-day repeatability (% RSD ranging from 2% to 13%), between-day reproducibility (% RSD from 3% to 15%), as well as between-trap reproducibility were assessed. The results are very encouraging as negligible shifts in retention times (% RSD from 0.3% to 0.6% in the 1st dimension and 0.8% to 2% in the 2nd dimension) were observed for both within-day and day-to-day comparisons of the studied samples (ANOVA, p=0.9893 for the sediment reference material compared), and the quantitative results were comparable. Routine analysis and quality control applications will benefit from the improved reproducibility as the variances in cold/hot jet flows and temperatures are eliminated. An overview of the device operation and the results from this study are summarized. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. Method translation and full metadata transfer from thermal to differential flow modulated comprehensive two dimensional gas chromatography: Profiling of suspected fragrance allergens.

    Science.gov (United States)

    Cordero, Chiara; Rubiolo, Patrizia; Reichenbach, Stephen E; Carretta, Andrea; Cobelli, Luigi; Giardina, Matthew; Bicchi, Carlo

    2017-01-13

    The possibility to transfer methods from thermal to differential-flow modulated comprehensive two-dimensional gas chromatographic (GC×GC) platforms is of high interest to improve GC×GC flexibility and increase the compatibility of results from different platforms. The principles of method translation are here applied to an original method, developed for a loop-type thermal modulated GC×GC-MS/FID system, suitable for quali-quantitative screening of suspected fragrance allergens. The analysis conditions were translated to a reverse-injection differential flow modulated platform (GC×2GC-MS/FID) with a dual-parallel secondary column and dual detection. The experimental results, for a model mixture of suspected volatile allergens and for raw fragrance mixtures of different composition, confirmed the feasibility of translating methods by preserving 1 D elution order, as well as the relative alignment of resulting 2D peak patterns. A correct translation produced several benefits including an effective transfer of metadata (compound names, MS fragmentation pattern, response factors) by automatic template transformation and matching from the original/reference method to its translated counterpart. The correct translation provided: (a) 2D pattern repeatability, (b) MS fragmentation pattern reliability for identity confirmation, and (c) comparable response factors and quantitation accuracy within a concentration range of three orders of magnitude. The adoption of a narrow bore (i.e. 0.1mm d c ) first-dimension column to operate under close-to-optimal conditions with the differential-flow modulation GC×GC platform was also advantageous in halving the total analysis under the translated conditions. Copyright © 2016 Elsevier B.V. All rights reserved.

  6. Combined untargeted and targeted fingerprinting by comprehensive two-dimensional gas chromatography: revealing fructose-induced changes in mice urinary metabolic signatures.

    Science.gov (United States)

    Bressanello, Davide; Liberto, Erica; Collino, Massimo; Chiazza, Fausto; Mastrocola, Raffaella; Reichenbach, Stephen E; Bicchi, Carlo; Cordero, Chiara

    2018-03-07

    This study exploits the information potential of comprehensive two-dimensional gas chromatography configured with a parallel dual secondary column-dual detection by mass spectrometry and flame ionization (GC×2GC-MS/FID) to study changes in urinary metabolic signatures of mice subjected to high-fructose diets. Samples are taken from mice fed with normal or fructose-enriched diets provided either in aqueous solution or in solid form and analyzed at three stages of the dietary intervention (1, 6, and 12 weeks). Automated Untargeted and Targeted fingerprinting for 2D data elaboration is adopted for the most inclusive data mining of GC×GC patterns. The UT fingerprinting strategy performs a fully automated peak-region features fingerprinting and combines results from pre-targeted compounds and unknowns across the sample-set. The most informative metabolites, with statistically relevant differences between sample groups, are obtained by unsupervised multivariate analysis (MVA) and cross-validated by multi-factor analysis (MFA) with external standard quantitation by GC-MS. Results indicate coherent clustering of mice urine signatures according to dietary manipulation. Notably, the metabolite fingerprints of mice fed with liquid fructose exhibited greater derangement in fructose, glucose, citric, pyruvic, malic, malonic, gluconic, cis-aconitic, succinic and 2-keto glutaric acids, glycine acyl derivatives (N-carboxy glycine, N-butyrylglycine, N-isovaleroylglycine, N-phenylacetylglycine), and hippuric acid. Untargeted fingerprinting indicates some analytes which were not a priori pre-targeted which provide additional insights: N-acetyl glucosamine, N-acetyl glutamine, malonyl glycine, methyl malonyl glycine, and glutaric acid. Visual features fingerprinting is used to track individual variations during experiments, thereby extending the panorama of possible data elaboration tools. Graphical abstract ᅟ.

  7. Tile-based Fisher-ratio software for improved feature selection analysis of comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry data.

    Science.gov (United States)

    Marney, Luke C; Siegler, W Christopher; Parsons, Brendon A; Hoggard, Jamin C; Wright, Bob W; Synovec, Robert E

    2013-10-15

    Comprehensive two-dimensional (2D) gas chromatography coupled with time-of-flight mass spectrometry (GC × GC-TOFMS) is a highly capable instrumental platform that produces complex and information-rich multi-dimensional chemical data. The data can be initially overwhelming, especially when many samples (of various sample classes) are analyzed with multiple injections for each sample. Thus, the data must be analyzed in such a way as to extract the most meaningful information. The pixel-based and peak table-based Fisher ratio algorithmic approaches have been used successfully in the past to reduce the multi-dimensional data down to those chemical compounds that are changing between the sample classes relative to those that are not changing (i.e., chemical feature selection). We report on the initial development of a computationally fast novel tile-based Fisher-ratio software that addresses the challenges due to 2D retention time misalignment without explicitly aligning the data, which is often a shortcoming for both pixel-based and peak table-based algorithmic approaches. Concurrently, the tile-based Fisher-ratio algorithm significantly improves the sensitivity contrast of true positives against a background of potential false positives and noise. In this study, eight compounds, plus one internal standard, were spiked into diesel at various concentrations. The tile-based F-ratio algorithmic approach was able to "discover" all spiked analytes, within the complex diesel sample matrix with thousands of potential false positives, in each possible concentration comparison, even at the lowest absolute spiked analyte concentration ratio of 1.06, the ratio between the concentrations in the spiked diesel sample to the native concentration in diesel. Copyright © 2013 Elsevier B.V. All rights reserved.

  8. Cyclotron resonance spectroscopy of a high-mobility two-dimensional electron gas from 0.4 to 100 K at high filling factors

    Energy Technology Data Exchange (ETDEWEB)

    Curtis, Jeremy A. [Univ. of Alabama, Birmingham, AL (United States); Tokumoto, Takahisa [Univ. of Alabama, Birmingham, AL (United States); Cherian, Judy G. [Florida State Univ., Tallahassee, FL (United States). National High Magnetic Field Lab. (MagLab); Kuno, J. [Rice Univ., Houston, TX (United States); Reno, John L. [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States); McGill, Stephen A. [Florida State Univ., Tallahassee, FL (United States). National High Magnetic Field Lab. (MagLab); Karaiskaj, Denis [Univ. of South Florida, Tampa, FL (United States); Hilton, David J. [Univ. of Alabama, Birmingham, AL (United States)

    2015-10-01

    We have studied the cyclotron mobility of a Landau-quantized two-dimensional electron gas as a function of temperature (0.4 --100 K) at a fixed magnetic field (1.25 T) using terahertz time-domain spectroscopy in a sample with a low frequency mobility of μdc = 3.6 x 106 cm2 V-1 s-1 and a carrier concentration of ns = 2 x 106 cm-2. The low temperature mobility in this sample results from both impurity scattering and acoustic deformation potential scattering, with μ$-1\\atop{CR}$ ≈ (2.1 x 105 cm2 V-1 s-1)-1 + (3.8 x 10-8 V sK-1 cm-2 x T)-1 at low temperatures. Above 50 K, the cyclotron oscillations show a strong reduction in both the oscillation amplitude and lifetime that is dominated by the contribution due to polar optical phonons. These results suggest that electron dephasing times as long as ~ 300 ps are possible even at this high lling factor (v = 6:6) in higher mobility samples (> 107 cm2 V-1 s-1) that have lower impurity concentrations and where the cyclotron mobility at this carrier concentration would be limited by acoustic deformation potential scattering.

  9. Advanced fingerprinting of high-quality cocoa: Challenges in transferring methods from thermal to differential-flow modulated comprehensive two dimensional gas chromatography.

    Science.gov (United States)

    Magagna, Federico; Liberto, Erica; Reichenbach, Stephen E; Tao, Qingping; Carretta, Andrea; Cobelli, Luigi; Giardina, Matthew; Bicchi, Carlo; Cordero, Chiara

    2018-02-09

    The possibility to transfer methods from thermal to differential-flow modulated comprehensive two-dimensional gas chromatographic (GC×GC) platforms opens interesting perspectives for routine analysis of complex samples. Flow modulated platforms avoid the use of cryogenics, thereby simplifying laboratory operations and analyst supervision during intensive analytical sessions. This study evaluates the feasibility of transferring a fingerprinting method capable of classifying and discriminating cocoa samples based on the volatiles fraction composition according to their origin and processing steps. Previously developed principles of GC×GC method translation are applied to an original fingerprinting method, developed for a loop-type thermal modulated GC×GC-MS system, to engineer a method for a reverse-injection differential flow modulated platform (GC×2GC-MS/FID) with a dual-parallel secondary column and dual detection. Effective method translation preserves analytes elution order, 1 D resolution, and 2D pattern coherence. The experimental results confirm the feasibility of translating fingerprinting method conditions while preserving the informative power of 2D peak patterns for sample classification and discrimination. Correct translation enables effective transfer of metadata (e.g., compound names and MS fragmentation patterns) by automatic template transformation and matching from the original/reference method to its translated counterpart. Although the adoption of a narrow bore (i.e. 0.1mm d c ) column in the first-dimension enabled operation under close-to-optimal conditions with the differential-flow modulation platform, due to the dual-parallel columns in the second-dimension, it resulted in lower overall method sensitivity. Nevertheless, fingerprinting accuracy was preserved and most of the key-aroma compounds and technological markers were effectively mapped, thus limiting the loss of fingerprinting information. Copyright © 2017 Elsevier B.V. All rights

  10. Determination of nonylphenol isomers in landfill leachate and municipal wastewater using steam distillation extraction coupled with comprehensive two-dimensional gas chromatography/time-of-flight mass spectrometry.

    Science.gov (United States)

    Zhang, Caixiang; Eganhouse, Robert P; Pontolillo, James; Cozzarelli, Isabelle M; Wang, Yanxin

    2012-03-23

    4-Nonylphenols (4-NPs) are known endocrine disruptors and by-products of the microbial degradation of nonylphenol polyethoxylate surfactants. One of the challenges to understanding the toxic effects of nonylphenols is the large number of isomers that may exist in environmental samples. In order to attribute toxic effects to specific compounds, a method is needed for the separation and quantitation of individual nonylphenol isomers. The pre-concentration methods of solvent sublimation, solid-phase extraction or liquid-liquid extraction prior to chromatographic analysis can be problematic because of co-extraction of thousands of compounds typically found in complex matrices such as municipal wastewater or landfill leachate. In the present study, steam distillation extraction (SDE) was found to be an effective pre-concentration method for extraction of 4-NPs from leachate and wastewater, and comprehensive two-dimensional gas chromatography (GC×GC) coupled with fast mass spectral data acquisition by time-of-flight mass spectrometry (ToFMS) enhanced the resolution and identification of 4-NP isomers. Concentrations of eight 4-NP isomers were determined in leachate from landfill cells of different age and wastewater influent and effluent samples. 4-NP isomers were about 3 times more abundant in leachate from the younger cell than the older one, whereas concentrations in wastewater effluent were either below detection limits or <1% of influent concentrations. 4-NP isomer distribution patterns were found to have been altered following release to the environment. This is believed to reflect isomer-specific degradation and accumulation of 4-NPs in the aquatic environment. Copyright © 2012 Elsevier B.V. All rights reserved.

  11. Quasi-two-dimensional electron gas at the interface of γ-Al2O3/SrTiO3 heterostructures grown by atomic layer deposition

    International Nuclear Information System (INIS)

    Ngo, Thong Q.; McDaniel, Martin D.; Ekerdt, John G.; Goble, Nicholas J.; Gao, Xuan P. A.; Posadas, Agham; Kormondy, Kristy J.; Demkov, Alexander A.; Lu, Sirong; Jordan-Sweet, Jean; Smith, David J.

    2015-01-01

    We report the formation of a quasi-two-dimensional electron gas (2-DEG) at the interface of γ-Al 2 O 3 /TiO 2 -terminated SrTiO 3 (STO) grown by atomic layer deposition (ALD). The ALD growth of Al 2 O 3 on STO(001) single crystal substrates was performed at temperatures in the range of 200–345 °C. Trimethylaluminum and water were used as co-reactants. In situ reflection high energy electron diffraction, ex situ x-ray diffraction, and ex situ cross-sectional transmission electron microscopy were used to determine the crystallinity of the Al 2 O 3 films. As-deposited Al 2 O 3 films grown above 300 °C were crystalline with the γ-Al 2 O 3 phase. In situ x-ray photoelectron spectroscopy was used to characterize the Al 2 O 3 /STO interface, indicating that a Ti 3+ feature in the Ti 2p spectrum of STO was formed after 2–3 ALD cycles of Al 2 O 3 at 345 °C and even after the exposure to trimethylaluminum alone at 300 and 345 °C. The interface quasi-2-DEG is metallic and exhibits mobility values of ∼4 and 3000 cm 2 V −1 s −1 at room temperature and 15 K, respectively. The interfacial conductivity depended on the thickness of the Al 2 O 3 layer. The Ti 3+ signal originated from the near-interfacial region and vanished after annealing in an oxygen environment

  12. Determination of nonylphenol isomers in landfill leachate and municipal wastewater using steam distillation extraction coupled with comprehensive two-dimensional gas chromatography/time-of-flight mass spectrometry

    Science.gov (United States)

    Zhang, Caixiang; Eganhouse, Robert P.; Pontolillo, James; Cozzarelli, Isabelle M.; Wang, Yanxin

    2012-01-01

    4-Nonylphenols (4-NPs) are known endocrine disruptors and by-products of the microbial degradation of nonylphenol polyethoxylate surfactants. One of the challenges to understanding the toxic effects of nonylphenols is the large number of isomers that may exist in environmental samples. In order to attribute toxic effects to specific compounds, a method is needed for the separation and quantitation of individual nonylphenol isomers. The pre-concentration methods of solvent sublimation, solid-phase extraction or liquid–liquid extraction prior to chromatographic analysis can be problematic because of co-extraction of thousands of compounds typically found in complex matrices such as municipal wastewater or landfill leachate. In the present study, steam distillation extraction (SDE) was found to be an effective pre-concentration method for extraction of 4-NPs from leachate and wastewater, and comprehensive two-dimensional gas chromatography (GC × GC) coupled with fast mass spectral data acquisition by time-of-flight mass spectrometry (ToFMS) enhanced the resolution and identification of 4-NP isomers. Concentrations of eight 4-NP isomers were determined in leachate from landfill cells of different age and wastewater influent and effluent samples. 4-NP isomers were about 3 times more abundant in leachate from the younger cell than the older one, whereas concentrations in wastewater effluent were either below detection limits or <1% of influent concentrations. 4-NP isomer distribution patterns were found to have been altered following release to the environment. This is believed to reflect isomer-specific degradation and accumulation of 4-NPs in the aquatic environment.

  13. Automating data analysis for two-dimensional gas chromatography/time-of-flight mass spectrometry non-targeted analysis of comparative samples.

    Science.gov (United States)

    Titaley, Ivan A; Ogba, O Maduka; Chibwe, Leah; Hoh, Eunha; Cheong, Paul H-Y; Simonich, Staci L Massey

    2018-03-16

    Non-targeted analysis of environmental samples, using comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry (GC × GC/ToF-MS), poses significant data analysis challenges due to the large number of possible analytes. Non-targeted data analysis of complex mixtures is prone to human bias and is laborious, particularly for comparative environmental samples such as contaminated soil pre- and post-bioremediation. To address this research bottleneck, we developed OCTpy, a Python™ script that acts as a data reduction filter to automate GC × GC/ToF-MS data analysis from LECO ® ChromaTOF ® software and facilitates selection of analytes of interest based on peak area comparison between comparative samples. We used data from polycyclic aromatic hydrocarbon (PAH) contaminated soil, pre- and post-bioremediation, to assess the effectiveness of OCTpy in facilitating the selection of analytes that have formed or degraded following treatment. Using datasets from the soil extracts pre- and post-bioremediation, OCTpy selected, on average, 18% of the initial suggested analytes generated by the LECO ® ChromaTOF ® software Statistical Compare feature. Based on this list, 63-100% of the candidate analytes identified by a highly trained individual were also selected by OCTpy. This process was accomplished in several minutes per sample, whereas manual data analysis took several hours per sample. OCTpy automates the analysis of complex mixtures of comparative samples, reduces the potential for human error during heavy data handling and decreases data analysis time by at least tenfold. Copyright © 2018 Elsevier B.V. All rights reserved.

  14. Solid phase extraction in combination with comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry for the detailed investigation of volatiles in South African red wines

    NARCIS (Netherlands)

    Weldegergis, B.T.; Crouch, A.M.; Górecki, T.; Villiers, de A.

    2011-01-01

    Comprehensive two-dimensional gas chromatography in combination with time-of-flight mass spectrometry (GC × GC–TOFMS) has been applied for the analysis of volatile compounds in three young South African red wines. In spite of the significant benefits offered by GC × GC–TOFMS for the separation and

  15. A high-mobility two-dimensional electron gas at the spinel/perovskite interface of γ-Al2O3/SrTiO3

    DEFF Research Database (Denmark)

    Chen, Yunzhong; Bovet, N.; Trier, Felix

    2013-01-01

    of magnitude higher than those of hitherto-investigated perovskite-type interfaces are obtained. The spinel/perovskite twodimensional electron gas, where the two-dimensional conduction character is revealed by quantum magnetoresistance oscillations, is found to result from interface-stabilized oxygen vacancies...

  16. Simultaneous analysis of polychlorinated biphenyls and polychlorinated naphthalenes by isotope dilution comprehensive two-dimensional gas chromatography high-resolution time-of-flight mass spectrometry.

    Science.gov (United States)

    Xia, Dan; Gao, Lirong; Zheng, Minghui; Wang, Shasha; Liu, Guorui

    2016-09-21

    Polychlorinated biphenyls (PCBs) and polychlorinated naphthalenes (PCNs) are listed as persistent organic pollutants (POPs) under the Stockholm Convention. Because they have similar physical and chemical properties, they are coeluted and are usually analyzed separately by different gas chromatography high-resolution mass spectrometry (GC-HRMS) methods. In this study, a novel method was developed for simultaneous analysis of six indicator PCBs, 12 dioxin-like PCBs, and 16 PCNs using isotope dilution comprehensive two-dimensional gas chromatography with high-resolution time-of-flight mass spectrometry (GC × GC-HRTOF-MS). The method parameters, including the type of GC column, oven temperature program, and modulation period, were systematically optimized. Complete separation of all target analytes and the matrix was achieved with a DB-XLB column in the first dimension and a BPX-70 column in the second dimension. The isotope dilution method was used for quantification of the PCBs and PCNs by GC × GC-HRTOF-MS. The method showed good linearity from 5 to 500 pg μL(-1) for all the target compounds. The instrumental limit of detection ranged from 0.03 to 0.3 pg μL(-1) for the 18 PCB congeners and from 0.09 to 0.6 pg μL(-1) for the 16 PCN congeners. Repeatability for triplicate injections was always lower than 20%. The method was successfully applied to the determination of 18 PCBs present at 0.9-2054 pg g(-1) and 16 PCNs present at 0.2-15.7 pg g(-1) in three species of fish. The GC × GC-HRTOF-MS results agreed with those obtained by GC-HRMS. The GC × GC-HRTOF-MS method proved to be a sensitive and accurate technique for simultaneous analysis of the selected PCBs and PCNs. With the excellent chromatographic separation offered by GC × GC and accurate mass measurements offered by HRTOF-MS, this method allowed identification of non-target contaminants in the fish samples, including organochlorine pesticides and polycyclic aromatic hydrocarbons

  17. Improving the quality of biomarker candidates in untargeted metabolomics via peak table-based alignment of comprehensive two-dimensional gas chromatography-mass spectrometry data.

    Science.gov (United States)

    Bean, Heather D; Hill, Jane E; Dimandja, Jean-Marie D

    2015-05-15

    The potential of high-resolution analytical technologies like GC×GC/TOF MS in untargeted metabolomics and biomarker discovery has been limited by the development of fully automated software that can efficiently align and extract information from multiple chromatographic data sets. In this work we report the first investigation on a peak-by-peak basis of the chromatographic factors that impact GC×GC data alignment. A representative set of 16 compounds of different chromatographic characteristics were followed through the alignment of 63 GC×GC chromatograms. We found that varying the mass spectral match parameter had a significant influence on the alignment for poorly-resolved peaks, especially those at the extremes of the detector linear range, and no influence on well-chromatographed peaks. Therefore, optimized chromatography is required for proper GC×GC data alignment. Based on these observations, a workflow is presented for the conservative selection of biomarker candidates from untargeted metabolomics analyses. Copyright © 2015 Elsevier B.V. All rights reserved.

  18. Community air monitoring for pesticides-part 2: multiresidue determination of pesticides in air by gas chromatography, gas chromatography-mass spectrometry, and liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Hengel, Matt; Lee, P

    2014-03-01

    Two multiresidue methods were developed to determine pesticides in air collected in California. Pesticides were trapped using XAD-4 resin and extracted with ethyl acetate. Based on an analytical method from the University of California Davis Trace Analytical Laboratory, pesticides were detected by analyzing the extract by gas chromatography-mass spectrometry (GC-MS) to determine chlorothalonil, chlorthal-dimethyl, cycloate, dicloran, dicofol, EPTC, ethalfluralin, iprodione, mefenoxam, metolachlor, PCNB, permethrin, pronamide, simazine, trifluralin, and vinclozolin. A GC with a flame photometric detector was used to determine chlorpyrifos, chlorpyrifos oxon, diazinon, diazinon oxon, dimethoate, dimethoate oxon, fonophos, fonophos oxon, malathion, malathion oxon, naled, and oxydemeton. Trapping efficiencies ranged from 78 to 92 % for low level (0.5 μg) and 37-104 % for high level (50 and 100 μg) recoveries. Little to no degradation of compounds occurred over 31 days; recoveries ranged from 78 to 113 %. In the California Department of Food and Agriculture (CDFA) method, pesticides were detected by analyzing the extract by GC-MS to determine chlorothalonil, chlorpyrifos, cypermethrin, dichlorvos, dicofol, endosulfan 1, endosulfan sulfate, oxyfluorfen, permethrin, propargite, and trifluralin. A liquid chromatograph coupled to a MS was used to determine azinphos-methyl, chloropyrifos oxon, DEF, diazinon, diazinon oxon, dimethoate, dimethoate oxon, diuron, EPTC, malathion, malathion oxon, metolachlor, molinate, norflurazon, oryzalin, phosmet, propanil, simazine and thiobencarb. Trapping efficiencies for compounds determined by the CDFA method ranged from 10 to 113, 22 to 114, and 56 to 132 % for 10, 5, and 2 μg spikes, respectively. Storage tests yielded 70-170 % recovery for up to 28 days. These multiresidue methods represent flexible, sensitive, accurate, and cost-effective ways to determine residues of various pesticides in ambient air.

  19. Pyrolysis-gas chromatography-mass spectrometry of isolated, synthetic and degraded lignins

    Energy Technology Data Exchange (ETDEWEB)

    Saiz-Jimenez, C.; De Leeuw, J.W.

    1984-01-01

    Curie-point pyrolysis-gas chromatography-mass spectrometry was applied to study the chemical structure of sound and fungus degraded, industrial and synthetic lignins. Pyrolysis products reflected in some detail the structural units present in the lignin polymer. Thus, sound spruce lignin yielded trans-isoeugenol coniferaldehyde and trans-coniferyl alcohol as major pyrolysis products. Biodegraded lignin yielded oxidized units, including vanillin, acetoguaiacone, methyl vanillate, propioguaiacone, vanilloyl methyl ketone and vanillic acid as major products. Kraft lignin also showed evidence of oxidation, although not as much as the biodegraded lignin. Major products from this industrial lignin were guaiacol, methylguaiacol, vinylguaiacol and homovanillic acid. Results indicated that synthetic lignin duplicates fairly well the structure of natural lignin. However, coniferylaldehyde and trans-coniferyl alcohol were the dominant products only from the synthetic lignin, indicating the presence of large amounts of coniferyl alcohol and coniferylaldehyde end groups. 21 references.

  20. Verification of chemical composition of commercially available propolis extracts by gas chromatography-mass spectrometry analysis.

    Science.gov (United States)

    Czyżewska, Urszula; Konończuk, Joanna; Teul, Joanna; Drągowski, Paweł; Pawlak-Morka, Renata; Surażyński, Arkadiusz; Miltyk, Wojciech

    2015-05-01

    Propolis is a resin that is collected by honeybees from various plant sources. Due to its pharmacological properties, it is used in commercial production of nutritional supplements in pharmaceutical industry. In this study, gas chromatography-mass spectrometry was applied for quality control analysis of the three commercial specimens containing aqueous-alcoholic extracts of bee propolis. More than 230 constituents were detected in analyzed products, including flavonoids, chalcones, cinnamic acids and their esters, phenylpropenoid glycerides, and phenylpropenoid sesquiterpenoids. An allergenic benzyl cinnamate ester was also identified in all tested samples. This analytical method allows to evaluate biological activity and potential allergenic components of bee glue simultaneously. Studies on chemical composition of propolis samples may provide new approach to quality and safety control analysis in production of propolis supplementary specimens.

  1. Gas chromatography-mass spectrometry identification of photoproducts of hexahydroquinoline derivatives: potential calcium channel antagonists.

    Science.gov (United States)

    Mielcarek, Jadwiga; Matłoka, Agnieszka

    2005-05-05

    Photodegradation products of hexahydroquinoline derivatives (HHQ) have been analysed with gas chromatography-mass spectrometry (GC-MS). The photodegradation was carried out under the conditions recommended in the first version of the document issued by the International Conference on Harmonization (ICH), currently in force in the studies of photochemical stability of drugs and therapeutic substances. The study was performed on the compounds having two chlorine atoms at different positions of the phenyl ring. Photodegradation of dichlorophenyl derivatives of HHQ resulted in formation of one or three photoproducts. The main product of their decomposition was aromatic compound formed as a result of dehydrogenation of the dihydropyridine ring. The most often observed fragmentation pathway of the photoproducts formed was elimination of methyl and methoxy radicals from the ester groups. The fragmentation of the photoproducts containing one chlorine atom at the ortho-position of the phenyl ring occurred through elimination of chlorine radical.

  2. Profiling of plasma metabolites in canine oral melanoma using gas chromatography-mass spectrometry.

    Science.gov (United States)

    Kawabe, Mifumi; Baba, Yuta; Tamai, Reo; Yamamoto, Ryohei; Komori, Masayuki; Mori, Takashi; Takenaka, Shigeo

    2015-08-01

    Malignant melanoma is one of the most common and aggressive tumors in the oral cavity of dog. The tumor has a poor prognosis, and methods for diagnosis and prediction of prognosis after treatment are required. Here, we examined metabolite profiling using gas chromatography-mass spectrometry (GC-MS) for development of a discriminant model for evaluation of prognosis. Metabolite profiles were evaluated in healthy and melanoma plasma samples using orthogonal projection to latent structure using discriminant analysis (OPLS-DA). Cases that were predicted to be healthy using the OPLS discriminant model had no advanced lesions after radiation therapy. These results indicate that metabolite profiling may be useful in diagnosis and prediction of prognosis of canine malignant melanoma.

  3. Gas chromatography-mass spectrometric identification of iodine species arising from photo-chemical vapor generation

    Energy Technology Data Exchange (ETDEWEB)

    Grinberg, Patricia; Mester, Zoltan [Institute for National Measurements Standards, National Research Council Canada, Ottawa, Ontario, K1A 0R6 (Canada); D' Ulivo, Alessandro [Institute for Chemical and Physical Processes, National Research Council, Via G. Moruzzi 1, Pisa, 56124 (Italy); Sturgeon, Ralph E. [Institute for National Measurements Standards, National Research Council Canada, Ottawa, Ontario, K1A 0R6 (Canada)], E-mail: ralph.sturgeon@nrc.ca

    2009-07-15

    Ultraviolet irradiation of aqueous solutions of iodide/iodate ion containing low molecular weight organic acids generates volatile iodine species that are amenable to detection by atomic spectrometry. In the presence of formic, acetic or propionic acids, photo-chemical generation results in the formation of HI, methyl- and ethyl-iodide respectively, the latter two products being directly identified by gas chromatography-mass spectrometry. Deuterium and {sup 13}C-labeled reagents were employed to elucidate the provenance of the alkyl group. Use of {sup 13}CH{sub 3}-COOH produced {sup 13}CH{sub 3}-I; deuterated acetic acid (D{sub 3}C-COOD) resulted in the formation of CD{sub 3}-I. These observations indicate direct transfer of the alkyl group from the carboxylic acid to iodide, consistent with the suggestion that the mechanism of synthesis involves radical induced reactions.

  4. Gas chromatography-mass spectrometric identification of iodine species arising from photo-chemical vapor generation

    Science.gov (United States)

    Grinberg, Patricia; Mester, Zoltan; D'Ulivo, Alessandro; Sturgeon, Ralph E.

    2009-07-01

    Ultraviolet irradiation of aqueous solutions of iodide/iodate ion containing low molecular weight organic acids generates volatile iodine species that are amenable to detection by atomic spectrometry. In the presence of formic, acetic or propionic acids, photo-chemical generation results in the formation of HI, methyl- and ethyl-iodide respectively, the latter two products being directly identified by gas chromatography-mass spectrometry. Deuterium and 13C-labeled reagents were employed to elucidate the provenance of the alkyl group. Use of 13CH 3-COOH produced 13CH 3-I; deuterated acetic acid (D 3C-COOD) resulted in the formation of CD 3-I. These observations indicate direct transfer of the alkyl group from the carboxylic acid to iodide, consistent with the suggestion that the mechanism of synthesis involves radical induced reactions.

  5. Detecting naphthenic acids in waters by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Merlin, Mireya; Guigard, Selma E; Fedorak, Phillip M

    2007-01-26

    Naphthenic acids (general formula C(n)H(2n+Z)O(2)) are water-soluble, toxic compounds found in petroleum and bitumen. Some of the current methods for detecting these acids in waters depend on measuring the presence of the carboxylic acid functional group, and therefore many of these methods also detect naturally occurring carboxylic acids that are not naphthenic acids. We report a procedure that includes liquid-liquid extraction, cleanup, and derivatization to form t-butyldimethylsilyl esters prior to gas chromatography-mass spectrometry (GC-MS) analysis. Using low- and high-resolution MS to detect the ion C(15)H(27)O(2)Si(+) (nominal m/z=267) is an excellent indicator of the presence of naphthenic acids at concentrations > or =10microgL(-1).

  6. Determination of d-limonene in adipose tissue by gas chromatography-mass spectrometry

    Science.gov (United States)

    Miller, Jessica A.; Hakim, Iman A.; Thomson, Cynthia; Thompson, Patricia; Chow, H-H. Sherry

    2008-01-01

    We developed a novel method for analyzing d-limonene levels in adipose tissue. Fat samples were subjected to saponification followed by solvent extraction. d-Limonene in the sample extract was analyzed using gas chromatography-mass spectrometry (GC-MS) with selected ion monitoring. Linear calibration curves were established over the mass range of 79.0-2,529 ng d-limonene per 0.1 grams of adipose tissue. Satisfactory within day precision (RSD 6.7 to 9.6%) and accuracy (% difference of −2.7 to 3.8%) and between day precision (RSD 6.0 to 10.7%) and accuracy (% difference of 1.8 to 2.6%) were achieved. The assay was successfully applied to human fat biopsy samples from a d-limonene feeding trial. PMID:18571481

  7. Determination of Chlorpyrifos in Human Blood by Gas Chromatography-Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Xinhua Dai

    2017-01-01

    Full Text Available Gas chromatography-mass spectrometry method was developed for the qualitative and quantitative analyses of chlorpyrifos in human blood samples. The chlorpyrifos and parathion (internal standard in human blood were extracted with a mixed solvent of hexane and acetonitrile. Chlorpyrifos was well separated from the internal standard. The linear range of chlorpyrifos was 0.01–2 μg/ml in blood. The limit of detection and limit of quantification were estimated at 0.002 and 0.01 μg/ml, respectively. The inter- and intra-day precisions, accuracy, and recovery were assessed to verify this method. The results showed that the developed method is rapid, sensitive, and reliable. It is suitable for the determination of chlorpyrifos in forensic toxicological analysis and clinical diagnosis.

  8. Improvements in bis(cyclopentadienyl)magnesium purity as determined with gas chromatography-mass spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    BARTRAM,MICHAEL E.

    2000-03-08

    Bis(cyclopentadienyl)magnesium (MgCp2) is used commonly as a source for doping nitride materials with magnesium. Increased oxygen incorporation known to accompany the use of MgCp2 makes the purity of this precursor an important consideration in nitride CVD. Gas chromatography-mass spectroscopy (GCMS) methods have now been developed for the identification of volatile impurities in MgCp2. Diethylether, an oxygen containing organic compound (CH{sub 3}CH{sub 2}OCH{sub 2}CH{sub 3}), and additional organic impurities were found in the MgCp2 supplied by three manufacturers. Subsequent refinements in the synthetic processes by these companies have resulted in the availability of MgCp2 free of ether and other organic impurities as determined by GCMS.

  9. Observation of Thermoelectric Voltages from the Two-Dimensional Electron Gas of a HgTe Quantum Well Due to Resonant THz Laser Heating

    Science.gov (United States)

    Pakmehr, Mehdi; McCombe, B. D.; Bruene, C.; Buhmann, H.; Molenkamp, L. W.

    2015-10-01

    HgTe quantum wells (QWs) have shown a number of interesting phenomena, recently the first two-dimensional topological insulating state. We have studied thermoelectric photovoltages of two-dimensional electrons in a 6.1 nm wide HgTe QW induced by cyclotron resonance absorption ( B = 2 to 5 T) of a THz laser beam. We have estimated thermopower coefficients by detailed analysis of the photovoltage signals developed across various contacts of a large Hall bar structure at a bath temperature of 1.6 K. The photovoltage signals are washed out at bath temperature of 18 K.

  10. Determination of polychlorinated terphenyls in aquatic biota and sediment with gas chromatography/mass spectrometry using negative chemical ionization.

    NARCIS (Netherlands)

    Wester, P.G.; de Boer, J.; Brinkman, U.A.T.

    1996-01-01

    Polychlorinated terphenyls (PCTs) have been determined in aquatic biota and sediments by gas chromatography/mass spectrometry using negative chemical ionization. The use of various methods of calculation is discussed. Total PCT concentrations expressed as A (Aroclor) 5442 equivalents ranged from

  11. Gas chromatography-mass spectrometry analysis of effects of dietary fish oil on total fatty acid composition in mouse skin

    OpenAIRE

    Peiru Wang; Min Sun; Jianwei Ren; Zora Djuric; Gary J. Fisher; Xiuli Wang; Yong Li

    2017-01-01

    Altering the fatty acid (FA) composition in the skin by dietary fish oil could provide therapeutic benefits. Although it has been shown that fish oil supplementation enhances EPA (eicosapentaenoic acid) and DHA (docosahexaenoic acid) abundance in the skin, comprehensive skin FA profiling is needed. We established a gas chromatography-mass spectrometry method, which allows precise quantification of FA profile using small (

  12. Molecular analysis of intact preen waxes of Calidris canutus (Aves : Scolopacidae) by gas chromatography/mass spectrometry

    NARCIS (Netherlands)

    Dekker, MHA; Piersma, T; Damste, JSS; Dekker, Marlèn H.A.; Sinninghe Damsté, Jaap S.

    The intact preen wax esters of the red knot Calidris canutus were studied with gas chromatography/mass spectrometry (GC/MS) and GC/MS/MS. In this latter technique, transitions from the molecular ion to fragment ions representing the fatty acid moiety of the wax esters were measured, providing

  13. Introducing Students to Gas Chromatography-Mass Spectrometry Analysis and Determination of Kerosene Components in a Complex Mixture

    Science.gov (United States)

    Pacot, Giselle Mae M.; Lee, Lyn May; Chin, Sung-Tong; Marriott, Philip J.

    2016-01-01

    Gas chromatography-mass spectrometry (GC-MS) and GC-tandem MS (GC-MS/MS) are useful in many separation and characterization procedures. GC-MS is now a common tool in industry and research, and increasingly, GC-MS/MS is applied to the measurement of trace components in complex mixtures. This report describes an upper-level undergraduate experiment…

  14. An Advanced Analytical Chemistry Experiment Using Gas Chromatography-Mass Spectrometry, MATLAB, and Chemometrics to Predict Biodiesel Blend Percent Composition

    Science.gov (United States)

    Pierce, Karisa M.; Schale, Stephen P.; Le, Trang M.; Larson, Joel C.

    2011-01-01

    We present a laboratory experiment for an advanced analytical chemistry course where we first focus on the chemometric technique partial least-squares (PLS) analysis applied to one-dimensional (1D) total-ion-current gas chromatography-mass spectrometry (GC-TIC) separations of biodiesel blends. Then, we focus on n-way PLS (n-PLS) applied to…

  15. Enhancing the chemical selectivity in discovery-based analysis with tandem ionization time-of-flight mass spectrometry detection for comprehensive two-dimensional gas chromatography.

    Science.gov (United States)

    Freye, Chris E; Moore, Nicholas R; Synovec, Robert E

    2018-02-16

    The complementary information provided by tandem ionization time-of-flight mass spectrometry (TI-TOFMS) is investigated for comparative discovery-based analysis, when coupled with comprehensive two-dimensional gas chromatography (GC × GC). The TI conditions implemented were a hard ionization energy (70 eV) concurrently collected with a soft ionization energy (14 eV). Tile-based Fisher ratio (F-ratio) analysis is used to analyze diesel fuel spiked with twelve analytes at a nominal concentration of 50 ppm. F-ratio analysis is a supervised discovery-based technique that compares two different sample classes, in this case spiked and unspiked diesel, to reduce the complex GC × GC-TI-TOFMS data into a hit list of class distinguishing analyte features. Hit lists of the 70 eV and 14 eV data sets, and the single hit list produced when the two data sets are fused together, are all investigated. For the 70 eV hit list, eleven of the twelve analytes were found in the top thirteen hits. For the 14 eV hit list, nine of the twelve analytes were found in the top nine hits, with the other three analytes either not found or well down the hit list. As expected, the F-ratios per m/z used to calculate each average F-ratio per hit were generally smaller fragment ions for the 70 eV data set, while the larger fragment ions were emphasized in the 14 eV data set, supporting the notion that complementary information was provided. The discovery rate was improved when F-ratio analysis was performed on the fused data sets resulted in eleven of the twelve analytes being at the top of the single hit list. Using PARAFAC, analytes that were "discovered" were deconvoluted in order to obtain their identification via match values (MV). Location of the analytes and the "F-ratio spectra" obtained from F-ratio analysis were used to guide the deconvolution. Eight of the twelve analytes where successfully deconvoluted and identified using the in-house library for the 70

  16. Tracking changes in composition and amount of dissolved organic matter throughout drinking water treatment plants by comprehensive two-dimensional gas chromatography-quadrupole mass spectrometry.

    Science.gov (United States)

    Li, Chunmei; Wang, Donghong; Xu, Xiong; Xu, Meijia; Wang, Zijian; Xiao, Ruiyang

    2017-12-31

    Dissolved organic matter (DOM) can affect the performance of water treatment processes and produce undesirable disinfection by-products during disinfection. Several studies have been undertaken on the structural characterization of DOM, but its fate during drinking water treatment processes is still not fully understood. In this work, the nontargeted screening method of comprehensive two-dimensional gas chromatography-quadrupole mass spectrometry (GC×GC-qMS) was used to reveal the detailed changes of different chemical classes of compounds in DOM during conventional and advanced drinking water treatment processes at three drinking water treatment plants in China. The results showed that when the dissolved organic carbon removal was low, shifts in the DOM composition could not be detected with the specific ultraviolet absorbance at 254nm, but the changes were clear in the three-dimensional fluorescence excitation-emission matrix or GC×GC-qMS analyses. Coagulation-sedimentation processes selectively removed 37-59% of the nitrogenous compounds, alcohols and aromatic hydrocarbons but increased the concentrations of halogen-containing compounds by 17-26% because of the contact time with chlorine in this step. Filtration was less efficient at removing DOM but preferentially removed 21-60% of the acids. However, other organic matter would be released from the filter (e.g., nitrogenous compounds, acids, and aromatic hydrocarbons). Biological activated carbon (BAC) treatment removed most of the compounds produced from ozonation, particularly ketones, alcohols, halogen-containing compounds and acids. However, it should be noted that certain highly polar or high molecular weight compounds not identified in this study might be released from the BAC bed. After the whole treatment processes, the concentrations of nitrogenous compounds, alcohols, alkenes, aromatic hydrocarbons and ketones were decreased more by the advanced treatment processes than by the conventional treatment

  17. Simultaneous analysis of polychlorinated biphenyls and polychlorinated naphthalenes by isotope dilution comprehensive two-dimensional gas chromatography high-resolution time-of-flight mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Xia, Dan [State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085 (China); University of Chinese Academy of Sciences, Beijing 100085 (China); Gao, Lirong, E-mail: gaolr@rcees.ac.cn [State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085 (China); Zheng, Minghui; Wang, Shasha; Liu, Guorui [State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085 (China)

    2016-09-21

    Polychlorinated biphenyls (PCBs) and polychlorinated naphthalenes (PCNs) are listed as persistent organic pollutants (POPs) under the Stockholm Convention. Because they have similar physical and chemical properties, they are coeluted and are usually analyzed separately by different gas chromatography high-resolution mass spectrometry (GC-HRMS) methods. In this study, a novel method was developed for simultaneous analysis of six indicator PCBs, 12 dioxin-like PCBs, and 16 PCNs using isotope dilution comprehensive two-dimensional gas chromatography with high-resolution time-of-flight mass spectrometry (GC × GC-HRTOF-MS). The method parameters, including the type of GC column, oven temperature program, and modulation period, were systematically optimized. Complete separation of all target analytes and the matrix was achieved with a DB-XLB column in the first dimension and a BPX-70 column in the second dimension. The isotope dilution method was used for quantification of the PCBs and PCNs by GC × GC-HRTOF-MS. The method showed good linearity from 5 to 500 pg μL{sup −1} for all the target compounds. The instrumental limit of detection ranged from 0.03 to 0.3 pg μL{sup −1} for the 18 PCB congeners and from 0.09 to 0.6 pg μL{sup −1} for the 16 PCN congeners. Repeatability for triplicate injections was always lower than 20%. The method was successfully applied to the determination of 18 PCBs present at 0.9–2054 pg g{sup −1} and 16 PCNs present at 0.2–15.7 pg g{sup −1} in three species of fish. The GC × GC-HRTOF-MS results agreed with those obtained by GC-HRMS. The GC × GC-HRTOF-MS method proved to be a sensitive and accurate technique for simultaneous analysis of the selected PCBs and PCNs. With the excellent chromatographic separation offered by GC × GC and accurate mass measurements offered by HRTOF-MS, this method allowed identification of non-target contaminants in the fish samples, including organochlorine pesticides and

  18. Gas chromatography-mass spectrometry and high-performance liquid chromatographic analyses of thermal degradation products of common plastics.

    Science.gov (United States)

    Pacáková, V; Leclercq, P A

    1991-08-30

    The thermo-oxidation of five commonly used materials, namely low-density polyethylene, retarded polyethylene, paper with a polyethylene foil, a milk package and filled polypropylene, was studied. Capillary gas chromatography and gas chromatography-mass spectrometry were used to analyze the volatile degradation products, while high-performance liquid chromatography was employed to measure polycyclic aromatic hydrocarbons. The results are discussed from the point of view of toxicity of the products.

  19. Urinary metabonomics study in a rat model in response to protein-energy malnutrition by using gas chromatography-mass spectrometry and liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Wu, Zeming; Li, Min; Zhao, Chunxia; Zhou, Jia; Chang, Yuwei; Li, Xiang; Gao, Peng; Lu, Xin; Li, Yousheng; Xu, Guowang

    2010-11-01

    Systematic studies were performed on the biological perturbations in metabolic phenotype responding to protein-energy malnutrition through global metabolic profiling analysis, in combination with pattern recognition. The malnutrition rat model was established through five weeks of strict diet restriction, and the metabonome data obtained from gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-mass spectrometry (LC-MS) were integrated to approximate the comprehensive metabolic signature. Principal component analysis and orthogonal projection to latent structure analysis were used for the classification of metabolic phenotypes and discovery of differentiating metabolites. The perturbations in the urine profiles of malnourished rats were marked by higher levels of creatine, threitol, pyroglutamic acid, gluconic acid and kynurenic acid, as well as decreased levels of succinic acid, cis-aconitic acid, citric acid, isocitric acid, threonic acid, trimethylglycine, N-methylnicotinic acid and uric acid. The alterations in these metabolites were associated with perturbations in energy metabolism, carbohydrate, amino acid, and fatty acid metabolism, purine metabolism, cofactor and vitamin metabolism, in response to protein and energy malnutrition. Our findings show the integration of GC-MS and LC-MS techniques for untargeted metabolic profiling analysis was promising for nutriology.

  20. Development of a technique for mercury speciation and quantification using gas chromatography/mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Barshick, S.A.; Barshick, C.M.; Britt, P.F.; Vance, M.A.; Duckworth, D.C.

    1997-07-01

    One element of concern to DOE is mercury. Mercury was used extensively at the DOE facilities in Oak Ridge, Tennessee from 1950 to 1963 in the process of making lithium deuteride, a component of nuclear weapons. Although both the inorganic and organometallic forms of mercury are toxic to humans, the organic compounds are often more toxic. Since the toxicity of mercury is a function of its chemical form, an understanding of the interactions between commercially discharged mercury, naturally occurring mercury, and the environment in which they are present is vital. In this report, the authors have been investigating gas chromatography/mass spectrometry (GC/MS) for the analysis of both the organometallic and inorganic forms of mercury in the same environmental sample (e.g., solutions, soils, and sludges). Although gas chromatography is the classical technique for analyzing organic molecules, (e.g., organometallic compounds) little has been done on the analysis of inorganic compounds. In a previous publication, the authors described how a solid phase microextraction (SPME) fiber could be used to sample organomercurials from aqueous samples. An alkylation reaction was then carried out to transform chemically mercury nitrate into dimethylmercury; subsequent GC/MS analysis of this compound permitted quantification of the inorganic constituent. Subsequently, several different alkylation reagents have been synthesized that methylate any inorganic mercury compound to methylmercury iodide. Here, the authors report results on alkylation reaction time and the effect of pH on the population of the product.

  1. Oxysterols in cosmetics-Determination by planar solid phase extraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Schrack, S; Hohl, C; Schwack, W

    2016-11-18

    Sterol oxidation products (SOPs) are linked to several toxicological effects. Therefore, investigation of potential dietary uptake sources particularly food of animal origin has been a key issue for these compounds. For the simultaneous determination of oxysterols from cholesterol, phytosterols, dihydrolanosterol and lanosterol in complex cosmetic matrices, planar solid phase extraction (pSPE) was applied as clean-up tool. SOPs were first separated from more non-polar and polar matrix constituents by normal phase thin-layer chromatography and then focussed into one target zone. Zone extraction was performed with the TLC-MS interface, followed by gas chromatography-mass spectrometry analysis. pSPE showed to be effective for cleaning up cosmetic samples as sample extracts were free of interferences, and gas chromatographic columns did not show any signs of overloading. Recoveries were between 86 and 113% with relative standard deviations of below 10% (n=6). Results of our market survey in 2016 showed that some cosmetics with ingredients of plant origin contained phytosterol oxidation products (POPs) in the low ppm range and therefore in line with levels reported for food. In lanolin containing products, total SOPs levels (cholesterol oxidation products (COPs), lanosterol oxidation products (LOPs), dihydrolanosterol oxidation products (DOPs)) being in the low percent range exceeded reported levels for food by several orders of magnitudes. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. [Determination of olive oil content in olive blend oil by headspace gas chromatography-mass spectrometry].

    Science.gov (United States)

    Jiang, Wanfeng; Zhang, Ning; Zhang, Fengyan; Yang, Zhao

    2017-07-08

    A method for the determination of the content of olive oil in olive blend oil by headspace gas chromatography-mass spectrometry (SH-GC/MS) was established. The amount of the sample, the heating temperature, the heating time, the amount of injection, the injection mode and the chromatographic column were optimized. The characteristic compounds of olive oil were found by chemometric method. A sample of 1.0 g was placed in a 20 mL headspace flask, and heated at 180℃ for 2700 s. Then, 1.0 mL headspace gas was taken into the instrument. An HP-88 chromatographic column was used for the separation and the analysis was performed by GC/MS. The results showed that the linear range was 0-100%(olive oil content). The linear correlation coefficient ( r 2 ) was more than 0.995, and the limits of detection were 1.26%-2.13%. The deviations of olive oil contents in the olive blend oil were from -0.65% to 1.02%, with the relative deviations from -1.3% to 6.8% and the relative standard deviations from 1.18% to 4.26% ( n =6). The method is simple, rapid, environment friendly, sensitive and accurate. It is suitable for the determination of the content of olive oil in olive blend oil.

  3. Two-dimensional microstrip detector for neutrons

    Energy Technology Data Exchange (ETDEWEB)

    Oed, A. [Institut Max von Laue - Paul Langevin (ILL), 38 - Grenoble (France)

    1997-04-01

    Because of their robust design, gas microstrip detectors, which were developed at ILL, can be assembled relatively quickly, provided the prefabricated components are available. At the beginning of 1996, orders were received for the construction of three two-dimensional neutron detectors. These detectors have been completed. The detectors are outlined below. (author). 2 refs.

  4. Comparative Analysis of the Volatile Components of Agrimonia eupatoria from Leaves and Roots by Gas Chromatography-Mass Spectrometry and Multivariate Curve Resolution

    Directory of Open Access Journals (Sweden)

    Xiao-Liang Feng

    2013-01-01

    Full Text Available Gas chromatography-mass spectrometry and multivariate curve resolution were applied to the differential analysis of the volatile components in Agrimonia eupatoria specimens from different plant parts. After extracted with water distillation method, the volatile components in Agrimonia eupatoria from leaves and roots were detected by GC-MS. Then the qualitative and quantitative analysis of the volatile components in the main root of Agrimonia eupatoria was completed with the help of subwindow factor analysis resolving two-dimensional original data into mass spectra and chromatograms. 68 of 87 separated constituents in the total ion chromatogram of the volatile components were identified and quantified, accounting for about 87.03% of the total content. Then, the common peaks in leaf were extracted with orthogonal projection resolution method. Among the components determined, there were 52 components coexisting in the studied samples although the relative content of each component showed difference to some extent. The results showed a fair consistency in their GC-MS fingerprint. It was the first time to apply orthogonal projection method to compare different plant parts of Agrimonia eupatoria, and it reduced the burden of qualitative analysis as well as the subjectivity. The obtained results proved the combined approach powerful for the analysis of complex Agrimonia eupatoria samples. The developed method can be used to further study and quality control of Agrimonia eupatoria.

  5. Gas Chromatography-Mass Spectrometry Method to Quantify Benzo[a]Pyrene in Tobacco Products.

    Science.gov (United States)

    Wagner, Karl A; Huang, Chorng B; Melvin, Matt S; Ballentine, Regina; Meruva, Naren K; Flora, Jason W

    2017-08-01

    The USA Food and Drug Administration (FDA) established benzo[a]pyrene (B[a]P) as a harmful and potentially harmful constituent (HPHC) found in tobacco products. Tobacco manufacturers are required to report HPHC quantities to the FDA; however, there is currently no standardized method for determination of B[a]P in smokeless tobacco products (STPs). This work details a sensitive, selective and rapid method for the determination of B[a]P in STPs, cigarette filler and tobacco. Tobacco is extracted using methanol followed by solid-phase extraction and concentration prior to analysis by gas chromatography/mass spectrometry in the selected ion monitoring mode. Cooperation Centre for Scientific Research Relative to Tobacco reference products and 3R4F Kentucky reference cigarette filler were used for method validation. All method validation requirements were met including linearity, accuracy, precision, robustness, limit of detection (LOD) and limit of quantitation (LOQ), and stability. Calibration range of 0.5-125 ng mL-1 was achieved with the coefficient of determination (R2) greater than 0.995. The method LOQ and LOD were 0.729 and 0.216 ng/g, respectively. Using standardized methods for the measurement of HPHCs in tobacco products will reduce variability and ensure accurate data for regulatory reporting. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  6. The analysis of common metabolites of organophosphorus pesticides in urine by gas chromatography/mass spectrometry

    International Nuclear Information System (INIS)

    Park, Seong Soo; Pyo, Hee Soo; Lee, Kang Jin; Park, Song Ja; Park, Taek Kyu

    1998-01-01

    Most organophosphorus pesticides may be metabolized to yield some common phosphates in human or in animals, and these metabolites may be used as the exposure biomarkers to pesticides. In this study, we developed the extraction method of four phosphate metabolites from the spiked human urine in high recovery by the solid phase extraction with a reverse-phase cartridge (cyclohexyl silica) followed by the elution with methanol. The extracted urinary metabolites were derivatized with hexamethyldisilazane/trimethyl-chlorosilane/pyridine (2:1:10, v/v/v) and identified by gas chromatography/mass spectrometry. Calibration curve obtained from each metabolite standard using by GC/MS/SIM has shown good linearity and detection limits of metabolites were the range of 0.05-0.1 μg/ml in urine. Phenthoate, one of the organophosphorus pesticides, was orally administrated to rats. Four metabolites were detected in the rat urine. The results of this study may be applied to development of exposure biomarkers for monitoring of environmental pollutants

  7. Postmortem interval estimation: a novel approach utilizing gas chromatography/mass spectrometry-based biochemical profiling.

    Science.gov (United States)

    Kaszynski, Richard H; Nishiumi, Shin; Azuma, Takeshi; Yoshida, Masaru; Kondo, Takeshi; Takahashi, Motonori; Asano, Migiwa; Ueno, Yasuhiro

    2016-05-01

    While the molecular mechanisms underlying postmortem change have been exhaustively investigated, the establishment of an objective and reliable means for estimating postmortem interval (PMI) remains an elusive feat. In the present study, we exploit low molecular weight metabolites to estimate postmortem interval in mice. After sacrifice, serum and muscle samples were procured from C57BL/6J mice (n = 52) at seven predetermined postmortem intervals (0, 1, 3, 6, 12, 24, and 48 h). After extraction and isolation, low molecular weight metabolites were measured via gas chromatography/mass spectrometry (GC/MS) and examined via semi-quantification studies. Then, PMI prediction models were generated for each of the 175 and 163 metabolites identified in muscle and serum, respectively, using a non-linear least squares curve fitting program. A PMI estimation panel for muscle and serum was then erected which consisted of 17 (9.7%) and 14 (8.5%) of the best PMI biomarkers identified in muscle and serum profiles demonstrating statistically significant correlations between metabolite quantity and PMI. Using a single-blinded assessment, we carried out validation studies on the PMI estimation panels. Mean ± standard deviation for accuracy of muscle and serum PMI prediction panels was -0.27 ± 2.88 and -0.89 ± 2.31 h, respectively. Ultimately, these studies elucidate the utility of metabolomic profiling in PMI estimation and pave the path toward biochemical profiling studies involving human samples.

  8. Headspace Analysis of Philippine Civet Coffee Beans Using Gas Chromatography-Mass Spectrometry and Electronic Nose

    Science.gov (United States)

    Ongo, E.; Sevilla, F.; Antonelli, A.; Sberveglieri, G.; Montevecchi, G.; Sberveglieri, V.; de Paola, E. L.; Concina, I.; Falasconi, M.

    2011-11-01

    Civet coffee, the most expensive and best coffee in the world, is an economically important export product of the Philippines. With a growing threat of food adulteration and counterfeiting, a need for quality authentication is essential to protect the integrity and strong market value of Philippine civet coffee. At present, there is no internationally accepted method of verifying whether a bean is an authentic civet coffee. This study presented a practical and promising approach to identify and establish the headspace qualitative profile of Philippine civet coffee using electronic nose (E-nose) and gas chromatography-mass spectrometry (GC-MS). E-nose analysis revealed that aroma characteristic is one of the most important quality indicators of civet coffee. The findings were supported by GC-MS analysis. Principal component analysis (PCA) exhibited a clearly separated civet coffees from their control beans. The chromatographic fingerprints indicated that civet coffees differed with their control beans in terms of composition and concentration of individual volatile constituents.

  9. Exploring the Metabolomic Responses of Bacillus licheniformis to Temperature Stress by Gas Chromatography/Mass Spectrometry.

    Science.gov (United States)

    Dong, Zixing; Chen, Xiaoling; Cai, Ke; Chen, Zhixin; Wang, Hongbin; Jin, Peng; Liu, Xiaoguang; Permaul, Kugenthiren; Singh, Suren; Wang, Zhengxiang

    2018-03-28

    Owing to its high protein secretion capacity, simple nutritional requirements, and GRAS (generally regarded as safe) status, Bacillus licheniformis is widely used as a host for the industrial production of enzymes, antibiotics, and peptides. However, as compared with its close relative Bacillus subtilis , little is known about the physiology and stress responses of B. licheniformis . To explore its temperature-stress metabolome, B. licheniformis strains ATCC 14580 and B186, with respective optimal growth temperatures of 42°C and 50°C, were cultured at 42°C, 50°C, and 60°C and their corresponding metabolic profiles were determined by gas chromatography/mass spectrometry and multivariate statistical analyses. It was found that with increased growth temperatures, the two B. licheniformis strains displayed elevated cellular levels of proline, glutamate, lysine, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid, and octadecanoic acid, and decreased levels of glutamine and octadecenoic acid. Regulation of amino acid and fatty acid metabolism is likely to be associated with the evolution of protective biochemical mechanisms of B. licheniformis . Our results will help to optimize the industrial use of B. licheniformis and other important Bacillus species.

  10. Identification of floral scent in chrysanthemum cultivars and wild relatives by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Sun, Hainan; Zhang, Ting; Fan, Qingqing; Qi, Xiangyu; Zhang, Fei; Fang, Weimin; Jiang, Jiafu; Chen, Fadi; Chen, Sumei

    2015-03-25

    The objective of this study was to identify the major volatile compounds and their relative concentrations in flowers of different chrysanthemum cultivars and their wild relatives. The volatile organic components of fresh flowers were analyzed using a headspace solid-phase microextraction coupled with gas chromatography-mass spectrometry. In total, 193 volatile organic components were detected; the major scent components were monoterpenoids and oxygenated monoterpenoids, which accounted for 68.59%-99.93% of the total volatiles in all tested materials except for Chrysanthemum indicum collected from Huangshan, in which they accounted for only 37.45% of total volatiles. The major volatile compounds were camphor, α-pinene, chrysanthenone, safranal, myrcene, eucalyptol, 2,4,5,6,7,7ab-hexahydro-1H-indene, verbenone, β-phellandrene and camphene. In a hierarchical cluster analysis, 39 accessions of Chrysanthemum and its relatives formed six clusters based on their floral volatile compounds. In a principal component analysis, only spider type flowers were located closely on the score plot. The results of this study provide a basis for breeding chrysanthemum cultivars which desirable floral scents.

  11. Metabolic Profiling and Quantification of Neurotransmitters in Mouse Brain by Gas Chromatography-Mass Spectrometry.

    Science.gov (United States)

    Jäger, Christian; Hiller, Karsten; Buttini, Manuel

    2016-09-01

    Metabolites are key mediators of cellular functions, and have emerged as important modulators in a variety of diseases. Recent developments in translational biomedicine have highlighted the importance of not looking at just one disease marker or disease inducing molecule, but at populations thereof to gain a global understanding of cellular function in health and disease. The goal of metabolomics is the systematic identification and quantification of metabolite populations. One of the most pressing issues of our times is the understanding of normal and diseased nervous tissue functions. To ensure high quality data, proper sample processing is crucial. Here, we present a method for the extraction of metabolites from brain tissue, their subsequent preparation for non-targeted gas chromatography-mass spectrometry (GC-MS) measurement, as well as giving some guidelines for processing of raw data. In addition, we present a sensitive screening method for neurotransmitters based on GC-MS in selected ion monitoring mode. The precise multi-analyte detection and quantification of amino acid and monoamine neurotransmitters can be used for further studies such as metabolic modeling. Our protocol can be applied to shed light on nervous tissue function in health, as well as neurodegenerative disease mechanisms and the effect of experimental therapeutics at the metabolic level. © 2016 by John Wiley & Sons, Inc. Copyright © 2016 John Wiley & Sons, Inc.

  12. A gas chromatography-mass spectrometry method for the quantitation of clobenzorex.

    Science.gov (United States)

    Cody, J T; Valtier, S

    1999-01-01

    Drugs metabolized to amphetamine or methamphetamine are potentially significant concerns in the interpretation of amphetamine-positive urine drug-testing results. One of these compounds, clobenzorex, is an anorectic drug that is available in many countries. Clobenzorex (2-chlorobenzylamphetamine) is metabolized to amphetamine by the body and excreted in the urine. Following administration, the parent compound was detectable for a shorter time than the metabolite amphetamine, which could be detected for days. Because of the potential complication posed to the interpretation of amphetamin-positive drug tests following administration of this drug, the viability of a current amphetamine procedure using liquid-liquid extraction and conversion to the heptafluorobutyryl derivative followed by gas chromatography-mass spectrometry (GC-MS) analysis was evaluated for identification and quantitation of clobenzorex. Qualitative identification of the drug was relatively straightforward. Quantitative analysis proved to be a far more challenging process. Several compounds were evaluated for use as the internal standard in this method, including methamphetamine-d11, fenfluramine, benzphetamine, and diphenylamine. Results using these compounds proved to be less than satisfactory because of poor reproducibility of the quantitative values. Because of its similar chromatographic properties to the parent drug, the compound 3-chlorobenzylamphetamine (3-Cl-clobenzorex) was evaluated in this study as the internal standard for the quantitation of clobenzorex. Precision studies showed 3-Cl-clobenzorex to produce accurate and reliable quantitative results (within-run relative standard deviations [RSDs] clobenzorex.

  13. Analysis of fatty acid composition of Withania coagulans fruits by gas chromatography/mass spectrometry

    Directory of Open Access Journals (Sweden)

    A. Ali

    2017-10-01

    Full Text Available Background and objectives: Withania coagulans Dunal (Solanaceae fruits are recommended to treat asthma, dyspepsia, biliousness, flatulent colic, liver complaints, intestinal infections, strangury, wounds and as diuretic, emetic and sedative agent in Indian traditional system of medicine. The objective of this study was to describe the systematic fatty acid composition of the petroleum ether extract of W. coagulans fruits. Methods: Petroleum ether extract of W. coagulans fruits was prepared by maceration. Components of the W. coagulans petroleum ether extract were identified by gas chromatography-mass spectrometry and their concentrations were determined. Results: The fixed oil of W. coagulans fruits constituted of twenty nine components including unsaturated (52.36% and saturated (22.15% fatty acids, alkenes (5.65%, phytosterols (4.39%, fatty alcohols (4.14%, aromatic acid (3.56%, monoterpenes (3.22%, triterpenoids (1.83% and alkanes (2.7%. Most of the saturated and unsaturated fatty acids were identified as their methyl esters. Conclusions: Palmitoleic and 11-eicosenoic acids have been reported for the first time in petroleum ether extract of the W. coagulans fruits. The present study has illustrated the chemical nature of W. coagulans fruit and described its fatty acids composition.

  14. Prediction of Gas Chromatography-Mass Spectrometry Retention Times of Pesticide Residues by Chemometrics Methods

    Directory of Open Access Journals (Sweden)

    Elaheh Konoz

    2013-01-01

    Full Text Available A quantitative structure-retention relationships (QSRRs method is employed to predict the retention time of 300 pesticide residues in animal tissues separated by gas chromatography-mass spectroscopy (GC-MS. Firstly, a six-parameter QSRR model was developed by means of multiple linear regression. The six molecular descriptors that were considered to account for the effect of molecular structure on the retention time are number of nitrogen, Solvation connectivity index-chi 1, Balaban Y index, Moran autocorrelation-lag 2/weighted by atomic Sanderson electronegativity, total absolute charge, and radial distribution function-6.0/unweighted. A 6-7-1 back propagation artificial neural network (ANN was used to improve the accuracy of the constructed model. The standard error values of ANN model for training, test, and validation sets are 1.559, 1.517, and 1.249, respectively, which are less than those obtained reveals by multiple linear regressions model (2.402, 1.858, and 2.036, resp.. Results obtained the reliability and good predictability of nonlinear QSRR model to predict the retention time of pesticides.

  15. Gas chromatography/mass spectrometry analysis of triacetone triperoxide (TATP) degradation products.

    Science.gov (United States)

    Armitt, David; Zimmermann, Peter; Ellis-Steinborner, Simon

    2008-04-01

    Interest in the analysis and detection of triacetone triperoxide (TATP) and other organic peroxides has increased in recent years. Also of interest is the degradation and decomposition of the peroxides, not only to gain more detailed chemical information from organic peroxide samples, but also to investigate possible new procedures or mechanisms for chemical neutralisation. This report investigates the chemical degradation products of TATP after it has been treated with different acids within a sealed system over a period of 14 days. The samples were collected and analysed by solid-phase microextraction (SPME) and direct liquid injection gas chromatography/mass spectrometry (GC/MS). The results of the experiments indicate that the rate of chemical degradation of TATP and the products formed are dependent on the type of acid. The observed differences enables the type of acid used in the degradation process to be determined, provide complementary information to identify the presence of TATP, and possibly indicate new pathways that may be used to chemically neutralise TATP. (c) 2008 Commonwealth of Australia. Published by John Wiley & Sons, Ltd.

  16. Identification of Floral Scent in Chrysanthemum Cultivars and Wild Relatives by Gas Chromatography-Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Hainan Sun

    2015-03-01

    Full Text Available The objective of this study was to identify the major volatile compounds and their relative concentrations in flowers of different chrysanthemum cultivars and their wild relatives. The volatile organic components of fresh flowers were analyzed using a headspace solid-phase microextraction coupled with gas chromatography-mass spectrometry. In total, 193 volatile organic components were detected; the major scent components were monoterpenoids and oxygenated monoterpenoids, which accounted for 68.59%–99.93% of the total volatiles in all tested materials except for Chrysanthemum indicum collected from Huangshan, in which they accounted for only 37.45% of total volatiles. The major volatile compounds were camphor, α-pinene, chrysanthenone, safranal, myrcene, eucalyptol, 2,4,5,6,7,7ab-hexahydro-1H-indene, verbenone, β-phellandrene and camphene. In a hierarchical cluster analysis, 39 accessions of Chrysanthemum and its relatives formed six clusters based on their floral volatile compounds. In a principal component analysis, only spider type flowers were located closely on the score plot. The results of this study provide a basis for breeding chrysanthemum cultivars which desirable floral scents.

  17. [Determination of fenfluramine, diethylpropion and mazindol in slimming foods by gas chromatography-mass spectrometry].

    Science.gov (United States)

    Feng, Jiali; Pan, Zhenqiu; Cao, Huajuan; Wang, Chun'e

    2004-05-01

    A gas chromatography-mass spectrometry (GC/MS) analytical method for three anorectics drugs, fenfluramine, diethylpropion and mazindol, illegally adulterated in slimming foods has been developed. They can be simultaneously identified and quantified. The samples were extracted with chloroform, and then separated by GC with an HP-5MS GC capillary column. The temperature programming was started at 70 degrees C. The temperature was held at this temperature for 2 min and then increased at 10 degrees C/min to 280 degrees C. The completely separated peaks were identified by MS with a quadrupole mass filter and quantitated in selected ion monitoring mode. Compared with the NIST98 library, the matching qualities of the drugs in foods were all over 90%. The calibration curves of the drugs were excellent with correlation coefficients between 0.9991 and 0.9999, and relative standard deviations between 1.6% and 2.2%. The recoveries were between 96.0% and 102.4%. The results demonstrated that this method is suitable for the identification and quantitation of these anorectics drugs in slimming foods.

  18. Determination of pyrrolizidine alkaloids in selected feed materials with gas chromatography-mass spectrometry.

    Science.gov (United States)

    Kowalczyk, Ewelina; Kwiatek, Krzysztof

    2017-05-01

    1,2-Dehydropyrrolizidine alkaloids are known to be toxic to many animals and humans. To provide safety of feeds a method based on gas chromatography-mass spectrometry enabling the determination of a content of 1,2-unsaturated PAs in feed materials was developed. After extraction with aqueous solution of HCl and purification of the extract, 1,2-unsaturated alkaloids are reduced to their common backbone structures and subsequently derivatised with heptafluorobutyric anhydride (HFBA). The method was validated according to SANTE/11945/2015. All received parameters are consistent with the document requirements as recovery of a final compound retronecine derivative was from 81.8% to 94.4% when retrosine was used for spiking and from 72.7% to 85.5% when retrorsine N-oxide was spiked. The repeatability was calculated as relative standards deviation and ranged from 7.5% to 14.4%, for N-oxide was from 7.9% to 15.4%. The reproducibility was in the range from 14.2% to 16.3% and from 17.0% to 18.1% for free base and N-oxide respectively. The limit of quantification was determined as 10 µg kg - 1 . Good linearity of the method was obtained with coefficient of determination R 2  > 0.99. The method was applied to 35 silage and two hay samples analysis.

  19. Metabolomic study of aging in mouse plasma by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Seo, Chan; Hwang, Yun-Ho; Kim, Youngbae; Joo, Bo Sun; Yee, Sung-Tae; Kim, Cheol Min; Paik, Man-Jeong

    2016-07-01

    Metabolomic analysis of aging was performed in plasma samples of young (8 weeks) and old (72 weeks) mice as ethoxycarbonyl/methoxime/tert-butyldimethylsilyl derivatives by gas chromatography-mass spectrometry (GC-MS). As new approaches, study of altered metabolism from aging was attempted by simultaneous profiling analysis of amino acids (AAs), organic acids (OAs) and fatty acids (FAs) by GC-MS in a single run combined with pattern analysis. As a result, 27 amino acids (AAs), 17 organic acids (OAs) and 24 fatty acids (FAs) were positively screened with large variations in plasma samples. Among altered metabolites, levels of six AAs (proline, methionine, 4-hydroxyproline, pipecolic acid, glutamic acid, α-aminoadipic acid) as neurotransmetters and nutrients, five OAs (2-hydroxybutyric acid, 2-hydroxyglutaric acid, cis-aconitic acid citric acid, isocitric acid) including intermediate metabolites in the TCA cycle, and three n-3 polyunsaturated FAs (PUFAs) of α-octadecatrienoic acid, eicosapentaenoic acid and docosahexaenoic acid as potential biomarkers were significantly different between young and old groups. Their levels were normalized to the corresponding mean values of the young group and then plotted into star symbol patterns, which were clearly distinct compared with numerical data and readily distinguishable for young and old groups. Thus, the present metabolomic screening and the star pattern recognition method might be useful for understanding the complexity of biochemical events in aging. Copyright © 2016 Elsevier B.V. All rights reserved.

  20. Headspace gas chromatography-mass spectrometry of volatile compounds in murici (Byrsonima crassifolia l. Rich).

    Science.gov (United States)

    Alves, G L; Franco, M R B

    2003-01-24

    Northern and Northeastern Brazil have a natural diversity of fruits, many of which are considered exotic, presenting different flavors and aromas. The enormous diversity of fruits represents a promising area for research on aromas. There is also a great potential for the manufacture of juices, desserts or other processed products. Murici is a typical fruit from these regions presenting a different flavor, reminiscent of that of cheese. This fruit is consumed mainly as juice, ice cream or as liquor, greatly appreciated by the local population. Headspace volatile compounds of three lots of the fruit from Ceará (Fortaleza) were collected by suction on Porapak Q for 2 h and desorbed with 300 microl of acetone. The isolated volatile compounds were separated by high resolution GC. Forty-six volatile compounds were detected, of which 41 were identified by gas chromatography-mass spectrometry and Kovats indices. The most abundant compounds were ethanol (28.3%) and ethyl hexanoate (25.1%). Butanoic acid (5.1%), hexanoic acid (5.1%) and methyl butyrate (2.8%) were also detected in the headspace of the fruit and confirm its unusual cheese aroma.

  1. Analysis of ergosterol in single kernel and ground grain by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Dong, Yanhong; Steffenson, Brian J; Mirocha, Chester J

    2006-06-14

    A method for analyzing ergosterol in a single kernel and ground barley and wheat was developed using gas chromatography-mass spectrometry (GC-MS). Samples were saponified in methanolic KOH. Ergosterol was extracted by "one step" hexane extraction and subsequently silylated by N-trimethylsilylimidazole/trimethylchlorosilane (TMSI/TMCS) reagent at room temperature. The recoveries of ergosterol from ground barley were 96.6, 97.1, 97.1, 88.5, and 90.3% at the levels of 0.2, 1, 5, 10, and 20 microg/g (ppm), respectively. The recoveries from a single kernel were between 93.0 and 95.9%. The precision (coefficient of variance) of the method was in the range 0.8-12.3%. The method detection limit (MDL) and the method quantification limit (MQL) were 18.5 and 55.6 ng/g (ppb), respectively. The ergosterol analysis method developed can be used to handle 80 samples daily by one person, making it suitable for screening cereal cultivars for resistance to fungal infection. The ability for detecting low levels of ergosterol in a single kernel provides a tool to investigate early fungal invasion and to study mechanisms of resistance to fungal diseases.

  2. Identification of organic acids as potential biomarkers in the urine of autistic children using gas chromatography/mass spectrometry.

    Science.gov (United States)

    Kałużna-Czaplińska, Joanna; Żurawicz, Ewa; Struck, Wiktoria; Markuszewski, Michał

    2014-09-01

    There is a need to identify metabolic phenotypes in autism as they might each require unique approaches to prevention. Biological markers can help define autism subtypes and reveal potential therapeutic targets. The aim of the study was to identify alterations of small molecular weight compounds and to find potential biomarkers. Gas chromatography/mass spectrometry was employed to evaluate major metabolic changes in low molecular weight urine metabolites of 14 children with autism spectrum disorders vs. 10 non-autistic subjects. The results prove the usefulness of an identified set of 21 endogenous compounds (including 14 organic acids), whose levels are changed in diseased children. Gas chromatography/mass spectrometry method combined with multivariate statistical analysis techniques provide an efficient way of depicting metabolic perturbations of diseases, and may potentially be applicable as a novel strategy for the noninvasive diagnosis and treatment of autism. Copyright © 2014 Elsevier B.V. All rights reserved.

  3. Whole Microorganisms Studied by Pyrolysis-Gas Chromatography-Mass Spectrometry: Significance for Extraterrestrial Life Detection Experiments 1

    Science.gov (United States)

    Simmonds, Peter G.

    1970-01-01

    Pyrolysis-gas chromatography-mass spectrometric studies of two microorganisms, Micrococcus luteus and Bacillus subtilis var. niger, indicate that the majority of thermal fragments originate from the principal classes of bio-organic matter found in living systems such as protein and carbohydrate. Furthermore, there is a close qualitative similarity between the type of pyrolysis products found in microorganisms and the pyrolysates of other biological materials. Conversely, there is very little correlation between microbial pyrolysates and comparable pyrolysis studies of meteoritic and fossil organic matter. These observations will aid in the interpretation of a soil organic analysis experiment to be performed on the surface of Mars in 1975. The science payload of this landed mission will include a combined pyrolysis-gas chromatography-mass spectrometry instrument as well as several “direct biology experiments” which are designed to search for extraterrestrial life. PMID:16349890

  4. Quantitative assay of plasma homocysteine thiolactone by gas chromatography/mass spectrometry.

    Science.gov (United States)

    Daneshvar, Parham; Yazdanpanah, Mehrdad; Cuthbert, Carla; Cole, David E C

    2003-01-01

    Enzymatic cyclization of homocysteine forms a reactive thiolactone that may play an important role in its cardiovascular toxicity, but reliable quantitation of the free thiolactone metabolite in physiological fluids has not been reported. We have therefore used a highly selective gas chromatography/mass spectrometry (GC/MS) technique combined with the sensitivity of negative chemical ionization (NCI) to develop a quantitative method for the detection of homocysteine thiolactone (HcyTL) in plasma. To improve accuracy the deuterated isomer d(4)-HcyTL was synthesized and added to plasma as internal standard. The plasma was then treated with silica solid-phase extraction and derivatized with heptafluorobutyric anhydride. The derivative was analyzed by GC/MS in NCI mode with methane as the reagent gas and quantified by analyzing for the HcyTL ion [M(-)[bond]HF] and its d(4)-HcyTL counterpart in single-ion monitoring mode. The calibration curve showed a dynamic linear range up to 40 nmol/L. Within-day precision (n = 20, nominal concentration 5.2 nmol/L) was 0.96% and between-day precision was 3.9%, with a detection limit of 1.7 nmol/L and quantification limit of 5.2 nmol/L. Two human plasma samples had HcyTL concentrations of 18 and 25 nmol/L. This facile method for quantitation of homocysteine thiolactone opens the way for more detailed clinical studies of its potential role in homocysteine-induced arteriosclerosis and vaso-occlusive disease. Copyright 2003 John Wiley & Sons, Ltd.

  5. Phytochemical Profile of Erythrina variegata by Using High-Performance Liquid Chromatography and Gas Chromatography-Mass Spectroscopy Analyses

    OpenAIRE

    Suriyavathana Muthukrishnan; Subha Palanisamy; Senthilkumar Subramanian; Sumathi Selvaraj; Kavitha Rani Mari; Ramalingam Kuppulingam

    2016-01-01

    Natural products derived from plant sources have been utilized to treat patients with numerous diseases. The phytochemical constituents present in ethanolic leaf extract of Erythrina variegata (ELEV) were identified by using high-performance liquid chromatography (HPLC) and gas chromatography-mass spectroscopy (GC-MS) analyses. Shade dried leaves were powdered and extracted with ethanol for analyses through HPLC to identify selected flavonoids and through GC-MS to identify other molecules. Th...

  6. Serum metabolic profiling of human gastric cancer based on gas chromatography/mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Song, Hu; Peng, Jun-Sheng [Department of Gastrointestinal Surgery, the Sixth Affiliated Hospital (Gastrointestinal and Anal Hospital), Sun Yat-sen University, Guangzhou, Guangdong (China); Yao, Dong-Sheng [National Engineering Research Center of Genetic Medicine,Ji Nan University, Guangzhou, Guangdong (China); Yang, Zu-Li [Department of Gastrointestinal Surgery, the Sixth Affiliated Hospital (Gastrointestinal and Anal Hospital), Sun Yat-sen University, Guangzhou, Guangdong (China); Liu, Huan-Liang [Institute of Gastroenterology,Sun Yat-sen University, Guangzhou, Guangdong (China); Zeng, Yi-Ke [Department of Gastrointestinal Surgery, the Sixth Affiliated Hospital (Gastrointestinal and Anal Hospital), Sun Yat-sen University, Guangzhou, Guangdong (China); Shi, Xian-Ping; Lu, Bi-Yan [Institute of Gastroenterology,Sun Yat-sen University, Guangzhou, Guangdong (China)

    2011-11-25

    Research on molecular mechanisms of carcinogenesis plays an important role in diagnosing and treating gastric cancer. Metabolic profiling may offer the opportunity to understand the molecular mechanism of carcinogenesis and help to non-invasively identify the potential biomarkers for the early diagnosis of human gastric cancer. The aims of this study were to explore the underlying metabolic mechanisms of gastric cancer and to identify biomarkers associated with morbidity. Gas chromatography/mass spectrometry (GC/MS) was used to analyze the serum metabolites of 30 Chinese gastric cancer patients and 30 healthy controls. Diagnostic models for gastric cancer were constructed using orthogonal partial least squares discriminant analysis (OPLS-DA). Acquired metabolomic data were analyzed by the nonparametric Wilcoxon test to find serum metabolic biomarkers for gastric cancer. The OPLS-DA model showed adequate discrimination between cancer and non-cancer cohorts while the model failed to discriminate different pathological stages (I-IV) of gastric cancer patients. A total of 44 endogenous metabolites such as amino acids, organic acids, carbohydrates, fatty acids, and steroids were detected, of which 18 differential metabolites were identified with significant differences. A total of 13 variables were obtained for their greatest contribution in the discriminating OPLS-DA model [variable importance in the projection (VIP) value >1.0], among which 11 metabolites were identified using both VIP values (VIP >1) and the Wilcoxon test. These metabolites potentially revealed perturbations of glycolysis and of amino acid, fatty acid, cholesterol, and nucleotide metabolism of gastric cancer patients. These results suggest that gastric cancer serum metabolic profiling has great potential in detecting this disease and helping to understand its metabolic mechanisms.

  7. Extraction of pure components from overlapped signals in gas chromatography-mass spectrometry (GC-MS

    Directory of Open Access Journals (Sweden)

    Likić Vladimir A

    2009-10-01

    Full Text Available Abstract Gas chromatography-mass spectrometry (GC-MS is a widely used analytical technique for the identification and quantification of trace chemicals in complex mixtures. When complex samples are analyzed by GC-MS it is common to observe co-elution of two or more components, resulting in an overlap of signal peaks observed in the total ion chromatogram. In such situations manual signal analysis is often the most reliable means for the extraction of pure component signals; however, a systematic manual analysis over a number of samples is both tedious and prone to error. In the past 30 years a number of computational approaches were proposed to assist in the process of the extraction of pure signals from co-eluting GC-MS components. This includes empirical methods, comparison with library spectra, eigenvalue analysis, regression and others. However, to date no approach has been recognized as best, nor accepted as standard. This situation hampers general GC-MS capabilities, and in particular has implications for the development of robust, high-throughput GC-MS analytical protocols required in metabolic profiling and biomarker discovery. Here we first discuss the nature of GC-MS data, and then review some of the approaches proposed for the extraction of pure signals from co-eluting components. We summarize and classify different approaches to this problem, and examine why so many approaches proposed in the past have failed to live up to their full promise. Finally, we give some thoughts on the future developments in this field, and suggest that the progress in general computing capabilities attained in the past two decades has opened new horizons for tackling this important problem.

  8. Serum metabolic profiling of human gastric cancer based on gas chromatography/mass spectrometry

    International Nuclear Information System (INIS)

    Song, Hu; Peng, Jun-Sheng; Yao, Dong-Sheng; Yang, Zu-Li; Liu, Huan-Liang; Zeng, Yi-Ke; Shi, Xian-Ping; Lu, Bi-Yan

    2011-01-01

    Research on molecular mechanisms of carcinogenesis plays an important role in diagnosing and treating gastric cancer. Metabolic profiling may offer the opportunity to understand the molecular mechanism of carcinogenesis and help to non-invasively identify the potential biomarkers for the early diagnosis of human gastric cancer. The aims of this study were to explore the underlying metabolic mechanisms of gastric cancer and to identify biomarkers associated with morbidity. Gas chromatography/mass spectrometry (GC/MS) was used to analyze the serum metabolites of 30 Chinese gastric cancer patients and 30 healthy controls. Diagnostic models for gastric cancer were constructed using orthogonal partial least squares discriminant analysis (OPLS-DA). Acquired metabolomic data were analyzed by the nonparametric Wilcoxon test to find serum metabolic biomarkers for gastric cancer. The OPLS-DA model showed adequate discrimination between cancer and non-cancer cohorts while the model failed to discriminate different pathological stages (I-IV) of gastric cancer patients. A total of 44 endogenous metabolites such as amino acids, organic acids, carbohydrates, fatty acids, and steroids were detected, of which 18 differential metabolites were identified with significant differences. A total of 13 variables were obtained for their greatest contribution in the discriminating OPLS-DA model [variable importance in the projection (VIP) value >1.0], among which 11 metabolites were identified using both VIP values (VIP >1) and the Wilcoxon test. These metabolites potentially revealed perturbations of glycolysis and of amino acid, fatty acid, cholesterol, and nucleotide metabolism of gastric cancer patients. These results suggest that gastric cancer serum metabolic profiling has great potential in detecting this disease and helping to understand its metabolic mechanisms

  9. Triple sorbent thermal desorption/gas chromatography/mass spectrometry determination of vapor phase organic contaminants

    International Nuclear Information System (INIS)

    Ma, C.Y.; Skeen, J.T.; Dindal, A.B.; Higgins, C.E.; Jenkins, R.A.

    1994-05-01

    A thermal desorption/ps chromatography/mass spectrometry (TD/GC/MS) has been evaluated for the determination of volatile organic compounds (VOCS) in vapor phase samples using Carbosieve S-III/Carbotrap/Carotrap C triple sorbent traps (TST) similar to those available from a commercial source. The analysis was carried out with a Hewlett-Packard 5985A or 5995 GC/MS system with a modified injector to adapt an inhouse manufactured short-path desorber for transferring desorbate directly onto a cryofocusing loop for subsequent GC/MS analysis. Vapor phase standards generated from twenty six compounds were used for method validation, including alkanes, alkyl alcohols, alkyl ketones, and alkyl nitrites, a group of representative compounds that have previously been identified in a target airborne matrix. The method was validated based on the satisfactory results in terms of reproducibility, recovery rate, stability, and linearity. A relative, standard deviation of 0.55 to 24.3 % was obtained for the entire TD process (generation of gas phase standards, spiking the standards on and desorbing from TST) over a concentration range of 20 to 500 ng/trap. Linear correlation coefficients for the calibration curves as determined ranged from 0.81 to 0.99 and limits of detection ranged from 3 to 76 ng. For a majority of standards, recoveries of greater than 90% were observed. For three selected standards spiked on TSTS, minimal loss (10 to 22%) was observed after storing the spiked in, a 4 degree C refrigerator for 29 days. The only chromatographable artifact observed was a 5% conversion of isopropanol to acetone. The validated method been successfully applied, to the determination of VOCs collected from various emission sources in a diversified concentration range

  10. Surface-sampling and analysis of TATP by swabbing and gas chromatography/mass spectrometry.

    Science.gov (United States)

    Romolo, Francesco Saverio; Cassioli, Luigi; Grossi, Silvana; Cinelli, Giuseppe; Russo, Mario Vincenzo

    2013-01-10

    The method of sample recovery for trace detection and identification of explosives plays a critical role in several criminal investigations. After bombing, there can be difficulties in sending big objects to a laboratory for analysis. Traces can also be searched for on large surfaces, on hands of suspects or on surfaces where the explosive was placed during preparatory phases (e.g. places where an IED was assembled, vehicles used for transportation, etc.). In this work, triacetone triperoxide (TATP) was synthesized from commercial precursors following reported methods. Several portions of about 6mg of TATP were then spread on different surfaces (e.g. floors, tables, etc.) or used in handling tests. Three different swabbing systems were used: a commercial swab, pre-wetted with propan-2-ol (isopropanol) and water (7:3), dry paper swabs, and cotton swabs wetted with propan-2-ol. Paper and commercial swabs were also used to sample a metal plate, where a small charge of about 4g of TATP was detonated. Swabs were sealed in small glass jars with screw caps and Parafilm(®) M and sent to the laboratory for analysis. Swabs were extracted and analysed several weeks later by gas chromatography/mass spectrometry. All the three systems gave positive results, but wetted swabs collected higher amounts of TATP. The developed procedure showed its suitability for use in real cases, allowing TATP detection in several simulations, including a situation in which people wash their hands after handling the explosive. Copyright © 2012 Elsevier Ireland Ltd. All rights reserved.

  11. Triple sorbent thermal desorption/gas chromatography/mass spectrometry determination of vapor phase organic contaminants

    Energy Technology Data Exchange (ETDEWEB)

    Ma, C.Y.; Skeen, J.T.; Dindal, A.B.; Higgins, C.E.; Jenkins, R.A.

    1994-05-01

    A thermal desorption/ps chromatography/mass spectrometry (TD/GC/MS) has been evaluated for the determination of volatile organic compounds (VOCS) in vapor phase samples using Carbosieve S-III/Carbotrap/Carotrap C triple sorbent traps (TST) similar to those available from a commercial source. The analysis was carried out with a Hewlett-Packard 5985A or 5995 GC/MS system with a modified injector to adapt an inhouse manufactured short-path desorber for transferring desorbate directly onto a cryofocusing loop for subsequent GC/MS analysis. Vapor phase standards generated from twenty six compounds were used for method validation, including alkanes, alkyl alcohols, alkyl ketones, and alkyl nitrites, a group of representative compounds that have previously been identified in a target airborne matrix. The method was validated based on the satisfactory results in terms of reproducibility, recovery rate, stability, and linearity. A relative, standard deviation of 0.55 to 24.3 % was obtained for the entire TD process (generation of gas phase standards, spiking the standards on and desorbing from TST) over a concentration range of 20 to 500 ng/trap. Linear correlation coefficients for the calibration curves as determined ranged from 0.81 to 0.99 and limits of detection ranged from 3 to 76 ng. For a majority of standards, recoveries of greater than 90% were observed. For three selected standards spiked on TSTS, minimal loss (10 to 22%) was observed after storing the spiked in, a 4{degree}C refrigerator for 29 days. The only chromatographable artifact observed was a 5% conversion of isopropanol to acetone. The validated method been successfully applied, to the determination of VOCs collected from various emission sources in a diversified concentration range.

  12. Simultaneous quantification of Δ9-tetrahydrocannabinol, 11-hydroxy-Δ9-tetrahydrocannabinol, and 11-nor-Δ9-tetrahydrocannabinol-9-carboxylic acid in human plasma using two-dimensional gas chromatography, cryofocusing, and electron impact-mass spectrometry

    OpenAIRE

    Lowe, Ross H.; Karschner, Erin L.; Schwilke, Eugene W.; Barnes, Allan J.; Huestis, Marilyn A.

    2007-01-01

    A two-dimensional (2D) gas chromatography/electron impact-mass spectrometry (GC/EI-MS) method for simultaneous quantification of Δ9-tetrahydrocannabinol (THC), 11-hydroxy-Δ9-tetrahydrocannabinol (11-OH-THC), and 11-nor-Δ9-tetrahydrocannabinol-9-carboxylic acid (THCCOOH) in human plasma was developed and validated. The method employs 2D capillary GC and cryofocusing for enhanced resolution and sensitivity. THC, 11-OH-THC, and THCCOOH were extracted by precipitation with acetonitrile followed b...

  13. Characterization of volatile compounds of Indian cress absolute by GC-olfactometry/VIDEO-sniff and comprehensive two-dimensional gas chromatography.

    Science.gov (United States)

    Breme, Katharina; Tournayre, Pascal; Fernandez, Xavier; Meierhenrich, Uwe J; Brevard, Hugues; Joulain, Daniel; Berdagué, Jean Louis

    2010-01-13

    Indian cress (Tropaeolum majus L.) has been consumed in salad or soup for decades, but its odor's detailed molecular composition is still unknown. Here we report on the study of the odorant profile and odor-impact compounds of Indian cress absolute by GC-olfactometry/vocabulary-intensity-duration of elementary odors by sniffing (GC-O/VIDEO-Sniff) on an eight-way multiport system, combined with GCxGC-MS analyses for the identification of odorant trace constituents. Odor impact compounds of Indian cress absolute were determined by GC-O, and the overall influence of sulfury and fruity notes stood out. Forty-four odorant compounds were identified among which 22 (50% of the identified odorant molecules) were identified by using comprehensive two-dimensional GC coupled to a time-of-flight-mass spectrometer (TOFMS). These trace compounds were not detected by 1D-qMS or could only be found with specific searches once they were detected by comprehensive 2D-GC, although they were well perceived by the judges in GC-O. This was amongst others the case for the two molecules having the highest odor impact, (E)-hex-2-enal (fruity) and diethyl trisulfide (alliaceous, sulfury, cabbage). A powerful sulfur-containing odor compound whose first identification in cress was recently reported by the authors was detected by GC-O: O,S-diethyl thiocarbonate (fruity/red fruit and sulfury odor).

  14. Effect of the nanofilm thickness on the properties of the two-dimensional electron gas at the interface between two dielectrics

    Energy Technology Data Exchange (ETDEWEB)

    Gadiev, R. M., E-mail: gadiev.radik@gmail.com; Lachinov, A. N. [M. Akmullah Baskir State Pedagogical University (Russian Federation); Karamov, D. D. [Russian Academy of Sciences, Ufa Scientific Center (Russian Federation); Kiselev, D. A. [National University of Science and Technology MISiS (Russian Federation); Kornilov, V. M. [M. Akmullah Baskir State Pedagogical University (Russian Federation)

    2016-07-15

    The mechanism of formation of the two-dimensional conductivity along the interface between two polymer dielectrics is experimentally studied. The idea of “polar catastrophe,” which was successfully used earlier to explain the electronic properties of the interface between two perovskites LaAlO{sub 3}/SrTiO{sub 3}, is chosen as a base hypothesis. Piezoelectric response microscopy is used to reveal the presence of spontaneous polarization on the surface of a polymer film, and the remanent polarization is found to decrease with increasing film thickness. As in the case of perovskites, the polymer film thickness is found to strongly affect the electrical conductivity along the interface. Substantial differences between these phenomena are detected. The change in the electrical conductivity is shown to be caused by a significant increase in the charge carrier mobility when the film thickness decreases below a certain critical value. The relation between the change in the carrier mobility and the change in the spontaneous surface polarization of the polymer film when its thickness decreases is discussed.

  15. Qualitative characteristics and comparison of volatile fraction of vodkas made from different botanical materials by comprehensive two-dimensional gas chromatography and the electronic nose based on the technology of ultra-fast gas chromatography.

    Science.gov (United States)

    Wiśniewska, Paulina; Śliwińska, Magdalena; Dymerski, Tomasz; Wardencki, Waldemar; Namieśnik, Jacek

    2017-03-01

    Vodka is a spirit-based beverage made from ethyl alcohol of agricultural origin. At present, increasingly more vodka brands have labels that specify the botanical origin of the product. Until now, the techniques for distinguishing between vodkas of different botanical origin have been costly, time-consuming and insufficient for making a distinction between vodka produced from similar raw materials. Therefore, it is of utmost importance to find a fast and relatively inexpensive technique for conducting such tests. In the present study, we employed comprehensive two-dimensional gas chromatography (GC×GC) and an electronic nose based on the technology of ultra-fast GC with chemometric methods such as partial least square discriminant analysis, discriminant function analysis and soft independent modeling of class analogy. Both techniques allow a distinction between the vodkas produced from different raw materials. In the case of GC×GC, the differences between vodkas were more noticeable than in the analysis by electronic nose; however, the electronic nose allowed the significantly faster analysis of vodkas. © 2016 Society of Chemical Industry. © 2016 Society of Chemical Industry.

  16. Biosynthetic Studies of the Male Marking Pheromone in Bumblebees by Using Labelled Fatty Acids and Two-Dimensional Gas Chromatography with Mass Detection

    Czech Academy of Sciences Publication Activity Database

    Žáček, Petr; Kindl, Jiří; Frišonsová, K.; Průchová, Markéta; Votavová, A.; Hovorka, Oldřich; Kovalczuk, T.; Valterová, Irena

    2015-01-01

    Roč. 80, č. 5 (2015), s. 839-850 ISSN 2192-6506 Institutional support: RVO:61388963 Keywords : biosynthesis * bumblebees * fatty acids * gas chromatography * pheromones Subject RIV: CC - Organic Chemistry Impact factor: 2.836, year: 2015

  17. Chemical Gated Field Effect Transistor by Hybrid Integration of One-Dimensional Silicon Nanowire and Two-Dimensional Tin Oxide Thin Film for Low Power Gas Sensor.

    Science.gov (United States)

    Han, Jin-Woo; Rim, Taiuk; Baek, Chang-Ki; Meyyappan, M

    2015-09-30

    Gas sensors based on metal-oxide-semiconductor transistor with the polysilicon gate replaced by a gas sensitive thin film have been around for over 50 years. These are not suitable for the emerging mobile and wearable sensor platforms due to operating voltages and powers far exceeding the supply capability of batteries. Here we present a novel approach to decouple the chemically sensitive region from the conducting channel for reducing the drive voltage and increasing reliability. This chemically gated field effect transistor uses silicon nanowire for the current conduction channel with a tin oxide film on top of the nanowire serving as the gas sensitive medium. The potential change induced by the molecular adsorption and desorption allows the electrically floating tin oxide film to gate the silicon channel. As the device is designed to be normally off, the power is consumed only during the gas sensing event. This feature is attractive for the battery operated sensor and wearable electronics. In addition, the decoupling of the chemical reaction and the current conduction regions allows the gas sensitive material to be free from electrical stress, thus increasing reliability. The device shows excellent gas sensitivity to the tested analytes relative to conventional metal oxide transistors and resistive sensors.

  18. Prediction of a mobile two-dimensional electron gas at the LaSc O3 /BaSn O3 (001) interface

    Science.gov (United States)

    Paudel, Tula R.; Tsymbal, Evgeny Y.

    2017-12-01

    Two-dimensional electron gases (2DEG) at oxide interfaces, such as LaAl O3 /SrTi O3 (001), have aroused significant interest due to their high carrier density (˜1014c m-2 ) and strong lateral confinement (˜1 nm). However, these 2DEGs are normally hosted by the weakly dispersive and degenerate d bands (e.g., Ti -3 d bands), which are strongly coupled to the lattice, causing mobility of such 2DEGs to be relatively low at room temperature (˜1 c m2/Vs ). Here, we propose using oxide host materials with the conduction bands formed from s electrons to increase carrier mobility and soften its temperature dependence. Using first-principles density functional theory calculations, we investigate LaSc O3 /BaSn O3 (001) heterostructure and as a model system, where the conduction band hosts the s -like carriers. We find that the polar discontinuity at this interface leads to electronic reconstruction resulting in the formation of the 2DEG at this interface. The conduction electrons reside in the highly dispersive Sn -5 s bands, which have a large band width and a low effective mass. The predicted 2DEG is expected to be highly mobile even at room temperature due to the reduced electron-phonon scattering via the inter-band scattering channel. A qualitatively similar behavior is predicted for a doped BaSn O3 , where a monolayer of BaO is replaced with LaO. We anticipate that the quantum phenomena associated with these 2DEGs to be more pronounced owing to the high mobility of the carriers.

  19. Quasi-two-dimensional holography

    International Nuclear Information System (INIS)

    Kutzner, J.; Erhard, A.; Wuestenberg, H.; Zimpfer, J.

    1980-01-01

    The acoustical holography with numerical reconstruction by area scanning is memory- and time-intensive. With the experiences by the linear holography we tried to derive a scanning for the evaluating of the two-dimensional flaw-sizes. In most practical cases it is sufficient to determine the exact depth extension of a flaw, whereas the accuracy of the length extension is less critical. For this reason the applicability of the so-called quasi-two-dimensional holography is appropriate. The used sound field given by special probes is divergent in the inclined plane and light focussed in the perpendicular plane using cylindrical lenses. (orig.) [de

  20. 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.

  1. Plasma metabolomic profiling of dairy cows affected with ketosis using gas chromatography/mass spectrometry.

    Science.gov (United States)

    Zhang, Hongyou; Wu, Ling; Xu, Chuang; Xia, Cheng; Sun, Lingwei; Shu, Shi

    2013-09-26

    Ketosis is an important problem for dairy cows` production performance. However, it is still little known about plasma metabolomics details of dairy ketosis. A gas chromatography/mass spectrometry (GC/MS) technique was used to investigate plasma metabolic differences in cows that had clinical ketosis (CK, n=22), subclinical ketosis (SK, n=32), or were clinically normal controls (NC, n=22). The endogenous plasma metabolome was measured by chemical derivatization followed by GC/MS, which led to the detection of 267 variables. A two-sample t-test of 30, 32, and 13 metabolites showed statistically significant differences between SK and NC, CK and NC, and CK and SK, respectively. Orthogonal signal correction-partial least-square discriminant analysis (OPLS-DA) revealed that the metabolic patterns of both CK and SK were mostly similar, with the exception of a few differences. The development of CK and SK involved disturbances in many metabolic pathways, mainly including fatty acid metabolism, amino acid metabolism, glycolysis, gluconeogenesis, and the pentose phosphate pathway. A diagnostic model arbitrary two groups was constructed using OPLS-DA and receiver-operator characteristic curves (ROC). Multivariate statistical diagnostics yielded the 19 potential biomarkers for SK and NC, 31 for CK and NC, and 8 for CK and SK with area under the curve (AUC) values. Our results showed the potential biomarkers from CK, SK, and NC, including carbohydrates, fatty acids, amino acids, even sitosterol and vitamin E isomers, etc. 2-piperidinecarboxylic acid and cis-9-hexadecenoic acid were closely associated with metabolic perturbations in ketosis as Glc, BHBA and NEFA for dealing with metabolic disturbances of ketosis in clinical practice. However, further research is needed to explain changes of 2,3,4-trihydroxybutyric acid, 3,4-dihydroxybutyric acid, α-aminobutyric acid, methylmalonic acid, sitosterol and α-tocopherol in CK and SK, and to reveal differences between CK and SK. Our

  2. The use of stable isotopes and gas chromatography/mass spectrometry in the identification of steroid metabolites in the equine

    International Nuclear Information System (INIS)

    Houghton, E.; Dumasia, M.C.; Teale, P.; Smith, S.J.; Cox, J.; Marshall, D.; Gower, D.B.

    1990-01-01

    Stable isotope gas chromatography/mass spectrometry has been used successfully in the elucidation of structures of urinary steroid metabolites in the horse and in the identification of metabolites isolated from in vivo perfusion and in vitro incubation studies using equine tissue preparations. Deuterium-labeled steroids, testosterone, dehydroepiandrosterone, and 5-androstene-3 beta,17 beta-diol have been synthesized by base-catalyzed isotope exchange methods and the products characterized by gas chromatography/mass spectrometry. [16,16(-2)H2]Dehydroepiandrosterone (plus radiolabeled dehydroepiandrosterone) was perfused into a testicular artery of a pony stallion and was shown to be metabolized into 2H2-labeled testosterone, 4-androstenedione, isomers of 5-androstene-3,17-diol, 19-hydroxytestosterone, and 19-hydroxy-4-androstenedione. In further studies, equine testicular minces have been incubated with 2H2-labeled and radiolabeled dehydroepiandrosterone and 5-androstene-3 beta, 17 beta-diol. The metabolites, whose identity was confirmed by stable isotope gas chromatography/mass spectrometry, proved the interconversion of the two substrates, as well as formation of testosterone and 4-androstenedione. The aromatization of dehydroepiandrosterone was also confirmed, together with the formation of an isomer of 5(10)-estrene-3,17-diol from both substrates showing 19-demethylation without concomitant aromatization. In studies of the feto-placental unit, the allantochorion was shown to aromatize [2H5]testosterone to [2H4]estradiol, the loss of one 2H from the substrate being consistent with aromatization of the A ring. The formation of 6-hydroxyestradiol was also confirmed in this study. The same technique has been valuable in determining the structure of two metabolites of nandrolone isolated from horse urine

  3. [Specific detection of urinary sympathomimetic amines for control of anti-doping by gas chromatography-mass spectroscopy].

    Science.gov (United States)

    Franceschini, A; Duthel, J M; Vallon, J J

    1991-03-22

    A specific, sensitive and reliable gas chromatography-mass spectrometry (GC-MS) technique for detection of sympathomimetic amines following urinary extraction is proposed. Amphetamine, phentermine, ephedrine, mephenorex, methylphenidate, benzphetamine, clobenzorex and internal standard (fenfluramine) are extracted from urines at pH 7.0 using elution by chloroform-isopropanol on C18 cartridges. Derivatization followed by GC-MS analysis allows identification of these drugs founded on relative retention times and mass spectra. The quantitation limit for derivatizable drugs was found to be 200 ng/ml and 500 ng/ml for underivatizable drugs.

  4. Rapid determination of polysaccharides in BianTi Soft Extract by spectrophotometry coupled with gas chromatography-mass spectrometry

    OpenAIRE

    Zheng, Minxia; Shen, Jie; Yang, Kai; Qian, Songxiang; Feng, Sujuan

    2010-01-01

    A simple approach for the rapid determination of polysaccharides in BianTi Soft Extract using spectrophotometry coupled with gas chromatography-mass spectrometry (GC-MS) was developed. The mixed standard solution composed of D-glucose, D-mannose, galactose and D-xylose in different proportions (1.00: 1.01: 0.12: 0.05) was prepared according to the monosaccharide composition analysis of the polysaccharides by GC-MS. The determination of polysaccharides by UV-Vis spectrophotometer was performed...

  5. Two dimensional plasma simulation code

    International Nuclear Information System (INIS)

    Hazak, G.; Boneh, Y.; Goshen, Sh.; Oreg, J.

    1977-03-01

    An electrostatic two-dimensional particle code for plasma simulation is described. Boundary conditions which take into account the finiteness of the system are presented. An analytic solution for the case of crossed fields plasma acceleration is derived. This solution serves as a check on a computer test run

  6. Molecular analysis of sulphur-rich brown coals by flash pyrolysis-gas chromatography-mass spectrometry: The type III-S kerogen

    NARCIS (Netherlands)

    Sinninghe Damsté, J.S.; Las Heras, F.X.C. de; Leeuw, J.W. de

    1992-01-01

    The molecular composition of five brown coals from three different basins (Maestrazgo, Mequinenza and Rubielos) in Spain was investigated by flash pyrolysis-gas chromatography and flash pyrolysis-gas chromatography-mass spectrometry. In these techniques, the macromolecular material is thermally

  7. Two-Dimensional Materials for Sensing: Graphene and Beyond

    Directory of Open Access Journals (Sweden)

    Seba Sara Varghese

    2015-09-01

    Full Text Available Two-dimensional materials have attracted great scientific attention due to their unusual and fascinating properties for use in electronics, spintronics, photovoltaics, medicine, composites, etc. Graphene, transition metal dichalcogenides such as MoS2, phosphorene, etc., which belong to the family of two-dimensional materials, have shown great promise for gas sensing applications due to their high surface-to-volume ratio, low noise and sensitivity of electronic properties to the changes in the surroundings. Two-dimensional nanostructured semiconducting metal oxide based gas sensors have also been recognized as successful gas detection devices. This review aims to provide the latest advancements in the field of gas sensors based on various two-dimensional materials with the main focus on sensor performance metrics such as sensitivity, specificity, detection limit, response time, and reversibility. Both experimental and theoretical studies on the gas sensing properties of graphene and other two-dimensional materials beyond graphene are also discussed. The article concludes with the current challenges and future prospects for two-dimensional materials in gas sensor applications.

  8. Sensitive determination of fluoride in biological samples by gas chromatography-mass spectrometry after derivatization with 2-(bromomethyl)naphthalene.

    Science.gov (United States)

    Kwon, Sun-Myung; Shin, Ho-Sang

    2014-12-10

    A gas chromatography-mass spectrometric method was developed in this study in order to determine fluoride in plasma and urine after derivatization with 2-(bromomethyl)naphthalene. 2-Fluoronaphthalene was chosen as the internal standard. The derivatization of fluoride was performed in the biological sample and the best reaction conditions (10.0 mg mL(-1) of 2-(bromomethyl)naphthalene, 1.0 mg mL(-1) of 15-crown-5-ether as a phase transfer catalyst, pH of 7.0, reaction temperature of 70°C, and heating time of 70 min) were established. The organic derivative was extracted with dichloromethane and then measured by a gas chromatography-mass spectrometry. Under the established condition, the detection limits were 11 μg L(-1) and 7 μg L(-1) by using 0.2 mL of plasma or urine, respectively. The accuracy was in a range of 100.8-107.6%, and the precision of the assay was less than 4.3% in plasma or urine. Fluoride was detected in a concentration range of 0.12-0.53 mg L(-1) in six urine samples after intake of natural mineral water containing 0.7 mg L(-1) of fluoride. Copyright © 2014 Elsevier B.V. All rights reserved.

  9. Two dimensional image correlation processor

    Science.gov (United States)

    Yao, Shi-Kai

    1992-06-01

    Two dimensional images are converted into a very long 1-dimensional data stream by means of raster scan. It is shown that the 1-dimensional correlation function of such long data streams is equivalent to the raster scan converted data of 2-dimensional correlation function of images. Real time correlation of high resolution two-dimensional images has been demonstrated using commercially available components. The advantages of this approach includes programmable electronics reference images, easy interface to objects of interest using conventional image collection optics, real time operation with high resolution images using off-the shelf components, and usefulness in the form of either black and white or full colored images. Such system would be versatile enough for robotics vision, optical inspection, and other pattern recognition and identification applications.

  10. Two-dimensional topological photonics

    Science.gov (United States)

    Khanikaev, Alexander B.; Shvets, Gennady

    2017-12-01

    Originating from the studies of two-dimensional condensed-matter states, the concept of topological order has recently been expanded to other fields of physics and engineering, particularly optics and photonics. Topological photonic structures have already overturned some of the traditional views on wave propagation and manipulation. The application of topological concepts to guided wave propagation has enabled novel photonic devices, such as reflection-free sharply bent waveguides, robust delay lines, spin-polarized switches and non-reciprocal devices. Discrete degrees of freedom, widely used in condensed-matter physics, such as spin and valley, are now entering the realm of photonics. In this Review, we summarize the latest advances in this highly dynamic field, with special emphasis on the experimental work on two-dimensional photonic topological structures.

  11. Two-dimensional critical phenomena

    International Nuclear Information System (INIS)

    Saleur, H.

    1987-09-01

    Two dimensional critical systems are studied using transformation to free fields and conformal invariance methods. The relations between the two approaches are also studied. The analytical results obtained generally depend on universality hypotheses or on renormalization group trajectories which are not established rigorously, so numerical verifications, mainly using the transfer matrix approach, are presented. The exact determination of critical exponents; the partition functions of critical models on toruses; and results as the critical point is approached are discussed [fr

  12. MetPP: a computational platform for comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry-based metabolomics.

    Science.gov (United States)

    Wei, Xiaoli; Shi, Xue; Koo, Imhoi; Kim, Seongho; Schmidt, Robin H; Arteel, Gavin E; Watson, Walter H; McClain, Craig; Zhang, Xiang

    2013-07-15

    Due to the high complexity of metabolome, the comprehensive 2D gas chromatography time-of-flight mass spectrometry (GC×GC-TOF MS) is considered as a powerful analytical platform for metabolomics study. However, the applications of GC×GC-TOF MS in metabolomics are not popular owing to the lack of bioinformatics system for data analysis. We developed a computational platform entitled metabolomics profiling pipeline (MetPP) for analysis of metabolomics data acquired on a GC×GC-TOF MS system. MetPP can process peak filtering and merging, retention index matching, peak list alignment, normalization, statistical significance tests and pattern recognition, using the peak lists deconvoluted from the instrument data as its input. The performance of MetPP software was tested with two sets of experimental data acquired in a spike-in experiment and a biomarker discovery experiment, respectively. MetPP not only correctly aligned the spiked-in metabolite standards from the experimental data, but also correctly recognized their concentration difference between sample groups. For analysis of the biomarker discovery data, 15 metabolites were recognized with significant concentration difference between the sample groups and these results agree with the literature results of histological analysis, demonstrating the effectiveness of applying MetPP software for disease biomarker discovery. The source code of MetPP is available at http://metaopen.sourceforge.net xiang.zhang@louisville.edu Supplementary data are available at Bioinformatics online.

  13. Evaluation of conditions of comprehensive two-dimensional gas chromatography that yield a near-theoretical maximum in peak capacity gain.

    Science.gov (United States)

    Klee, Matthew S; Cochran, Jack; Merrick, Mark; Blumberg, Leonid M

    2015-02-27

    The peak capacity gain (Gn) of a GC×GC system is the ratio of the system peak capacity to that of an optimized one-dimensional GC analysis lasting the same time and providing the same detection limit. A near-theoretical maximum in Gn has been experimentally demonstrated in GC×GC-TOF based on a 60m×0.25mm primary column. It was found that Gn was close to 9 compared to the theoretical maximum of about 11 for this system. A six-sigma peak capacity of 4500 was obtained during an 80min heating ramp from 50°C to 320°C. Using peak deconvolution, 2242 individual peaks were determined in a Las Vegas runoff water sample. This is the first definitive experimental demonstration known to us of an order-of-magnitude Gn. The key factors enabling this gain were: relatively sharp (about 20ms at half height) reinjection pulses into the secondary column, relatively long (60m) primary column, the same diameters in primary and secondary columns, relatively low retention factor at the end of the secondary analysis (k≅5 instead of 15, optimal for ideal conditions), optimum flow rate in both columns, and helium (rather than hydrogen) used as the carrier gas. The latter, while making the analysis 65% longer than if using H2, was a better match to the reinjection bandwidth and cycle time. Copyright © 2015 The Authors. Published by Elsevier B.V. All rights reserved.

  14. Determination of emerging contaminants in wastewater utilizing comprehensive two-dimensional gas-chromatography coupled with time-of-flight mass spectrometry.

    Science.gov (United States)

    Prebihalo, Sarah; Brockman, Adrienne; Cochran, Jack; Dorman, Frank L

    2015-11-06

    An analytical method for identification of emerging contaminants of concern, such as pesticides and organohalogens has been developed and utilized for true discovery-based analysis. In order to achieve the level of sensitivity and selectivity necessary for detecting compounds in complex samples, comprehensive gas chromatography coupled with time-of-flight mass spectrometry (GC×GC-TOFMS) was utilized to analyze wastewater samples obtained from the Pennsylvania State University wastewater treatment facility (WWTF). Determination of emerging contaminants through a process of combining samples which represent "normal background" and comparing this to new samples was developed. Results show the presence of halogenated benzotriazoles in wastewater samples as well as soil samples from Pennsylvania State University agricultural fields. The trace levels of chlorinated benzotriazoles observed in the monitoring wells present on the property indicate likely environmental degradation of the chlorinated benzotriazoles. Preliminary investigation of environmental fate of the substituted benzotriazoles indicates their likely degradation into phenol; an Environmental Protection Agency (USEPA) priority pollutant. Copyright © 2015 Elsevier B.V. All rights reserved.

  15. Exposure Assessment of Acetamide in Milk, Beef, and Coffee Using Xanthydrol Derivatization and Gas Chromatography/Mass Spectrometry.

    Science.gov (United States)

    Vismeh, Ramin; Haddad, Diane; Moore, Janette; Nielson, Chandra; Bals, Bryan; Campbell, Tim; Julian, Allen; Teymouri, Farzaneh; Jones, A Daniel; Bringi, Venkataraman

    2018-01-10

    Acetamide has been classified as a possible human carcinogen, but uncertainties exist about its levels in foods. This report presents evidence that thermal decomposition of N-acetylated sugars and amino acids in heated gas chromatograph injectors contributes to artifactual acetamide in milk and beef. An alternative gas chromatography/mass spectrometry protocol based on derivatization of acetamide with 9-xanthydrol was optimized and shown to be free of artifactual acetamide formation. The protocol was validated using a surrogate analyte approach based on d 3 -acetamide and applied to analyze 23 pasteurized whole milk, 44 raw sirloin beef, and raw milk samples from 14 different cows, and yielded levels about 10-fold lower than those obtained by direct injection without derivatization. The xanthydrol derivatization procedure detected acetamide in every food sample tested at 390 ± 60 ppb in milk, 400 ± 80 ppb in beef, and 39 000 ± 9000 ppb in roasted coffee beans.

  16. Solid-phase microcolumn extraction and gas chromatography-mass spectrometry identification of volatile organic compounds emitted by paper.

    Science.gov (United States)

    Hrivnák, Ján; Tölgyessy, Peter; Figedyová, Sona; Katuscák, Svetozár

    2009-11-15

    A rapid non-destructive sampling technique for the analysis of volatile organic compounds (VOCs) emitted by paper sheets is described. A capillary, which is connected to a microcolumn packed with Tenax TA, is inserted between two sheets at the centre of a paper stack encapsulated inside a PET/Al/PE composite foil. The other end of the microcolumn is connected to a gas-tight syringe and an appropriate volume of gaseous phase is aspirated. The microcolumn is then thermally desorbed in a modified GC inlet (modification is presented) and analysed by gas chromatography-mass spectrometry (GC-MS). In the chromatogram from the analysis of artificially aged paper sample 21 compounds were identified. Advantages of the method including the short sampling time (1 min), simplicity and economic aspect are discussed.

  17. Phonon-electron interactions in the two-dimensional electron gas in InGaAs-InAlAs modulation-doped field-effect transistor structures studied by Raman scattering

    Science.gov (United States)

    Maslar, J. E.; Dorsten, J. F.; Bohn, P. W.; Agarwala, S.; Adesida, I.; Caneau, C.; Bhat, R.

    1993-10-01

    Raman scattering by coupled longitudinal optic phonons and two-dimensional electron gas electrons in In0.53Ga0.47As-In0.52Al0.48As δ-doped heterostructures provides a powerful probe of electronic properties in these In-based structures. The two highest frequency modes, of the three coupled electron-phonon modes expected in this system, were observed, with the highest frequency mode being identified in InGaAs-based systems. The large dispersion of this mode makes it a particularly sensitive probe for changes in such properties as carrier concentration and subband energy. For structures with higher carrier concentrations coupling of the longitudinal optic phonon to multiple electron intersubband transitions is resolved. These measurements are particularly useful for heavily doped structures for which room-temperature Hall measurements cannot distinguish channel electrons from those in parallel conduction paths.

  18. Two-dimensional capillary origami

    International Nuclear Information System (INIS)

    Brubaker, N.D.; Lega, J.

    2016-01-01

    We describe a global approach to the problem of capillary origami that captures all unfolded equilibrium configurations in the two-dimensional setting where the drop is not required to fully wet the flexible plate. We provide bifurcation diagrams showing the level of encapsulation of each equilibrium configuration as a function of the volume of liquid that it contains, as well as plots representing the energy of each equilibrium branch. These diagrams indicate at what volume level the liquid drop ceases to be attached to the endpoints of the plate, which depends on the value of the contact angle. As in the case of pinned contact points, three different parameter regimes are identified, one of which predicts instantaneous encapsulation for small initial volumes of liquid. - Highlights: • Full solution set of the two-dimensional capillary origami problem. • Fluid does not necessarily wet the entire plate. • Global energy approach provides exact differential equations satisfied by minimizers. • Bifurcation diagrams highlight three different regimes. • Conditions for spontaneous encapsulation are identified.

  19. Two-dimensional capillary origami

    Energy Technology Data Exchange (ETDEWEB)

    Brubaker, N.D., E-mail: nbrubaker@math.arizona.edu; Lega, J., E-mail: lega@math.arizona.edu

    2016-01-08

    We describe a global approach to the problem of capillary origami that captures all unfolded equilibrium configurations in the two-dimensional setting where the drop is not required to fully wet the flexible plate. We provide bifurcation diagrams showing the level of encapsulation of each equilibrium configuration as a function of the volume of liquid that it contains, as well as plots representing the energy of each equilibrium branch. These diagrams indicate at what volume level the liquid drop ceases to be attached to the endpoints of the plate, which depends on the value of the contact angle. As in the case of pinned contact points, three different parameter regimes are identified, one of which predicts instantaneous encapsulation for small initial volumes of liquid. - Highlights: • Full solution set of the two-dimensional capillary origami problem. • Fluid does not necessarily wet the entire plate. • Global energy approach provides exact differential equations satisfied by minimizers. • Bifurcation diagrams highlight three different regimes. • Conditions for spontaneous encapsulation are identified.

  20. [Feasibility investigation of hydrogen instead of helium as carrier gas in the determination of five organophosphorus pesticides by gas chromatography-mass spectrometry].

    Science.gov (United States)

    Liu, Zhenxue; Zhou, Shixue

    2015-01-01

    Helium is almost the only choosable carrier gas used in gas chromatography-mass spectrometry (GC-MS). A mixed standard solution of five organophosphorus pesticides was analyzed by using GC-MS, and hydrogen or helium as carrier gas, so as to study the feasibility of hydrogen instead of helium as carrier gas for the determination of organophosphorus pesticides. Combining a mass spectrum database built by ourselves, the results were deconvolved and identified by Automated Mass Spectral Deconvolution & Identification System (AMDIS32), a software belonging to the workstation of the instrument. Then, the statistical software, IBM SPSS Statistics 19.0 was used for the clustering analysis of the data. The results indicated that when hydrogen was used as carrier gas, the peaks of the pesticides detected were slightly earlier than those when helium used as carrier gas, but the resolutions of the chromatographic peaks were lower, and the fraction good indices (Frac. Good) were lower, too. When hydrogen was used as carrier gas, the signals of the pesticides were unstable, the measuring accuracies of the pesticides were reduced too, and even more, some compounds were undetectable. Therefore, considering the measuring accuracy, the signal stability, and the safety, etc., hydrogen should be cautiously used as carrier gas in the determination of organophosphorus pesticides by GC-MS.

  1. Retrospective analysis by data processing tools for comprehensive two-dimensional gas chromatography coupled to high resolution time-of-flight mass spectrometry: a challenge for matrix-rich sediment core sample from Tokyo Bay.

    Science.gov (United States)

    Zushi, Yasuyuki; Hashimoto, Shunji; Tamada, Masafumi; Masunaga, Shigeki; Kanai, Yutaka; Tanabe, Kiyoshi

    2014-04-18

    Data processing tools for non-target analysis using comprehensive two-dimensional gas chromatography coupled with high-resolution time-of-flight mass spectrometry (GC×GC-HRTOFMS) were developed and applied to a sediment core in Tokyo Bay, focusing on chlorinated compounds in this study. The processing tools were classified in two different methods: (1) the consecutive use of mass defect filter followed by artificial neutral loss scan (MDF/artificial NLS) as a qualitative non-target screening method and (2) Entire Domain Combined Spectra Extraction and Integration Program (ComSpec) and two-dimensional peak sentinel (T-SEN) as a semi-quantitative target screening method. MDF/artificial NLS as a non-target screening approach revealed that PCBs, followed by octachlorodibenzo dioxin (OCDD), were the main chlorinated compounds present in all sediment layers. Furthermore, unknown peaks thought to be chlorinated compounds were found in increasing numbers, some in increasing amounts. T-SEN and ComSpec as a target screening approach were adapted for automatic semi-quantitative analysis showed that, in decreasing concentration order, PCBs, OCDD, and dichlorodiphenyltrichloroethane and its metabolites (DDEs, DDDs) were the main chlorinated pollutants in the sediments. The complementary use of both techniques allows us to extract significant chlorinated pollutants, including non-targeted compounds. This retrospective analysis by this approach performed well even on matrix-rich sediment samples and provided us an interesting insight of historical trends of pollution in Tokyo Bay. Copyright © 2014 Elsevier B.V. All rights reserved.

  2. 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 (Illicium and can assist with differentiating the fruits of I. verum from other species of Illicium, particularly the more toxic I. anisatum.

  3. Identification of Flavor Components in Perfumes by Headspace Solid-Phase Microextraction and Gas Chromatography-Mass Spectrometry

    Science.gov (United States)

    Knupp, Gerd; Kusch, Peter; Neugebauer, Michael

    2002-01-01

    An experiment for identification of flavor components in Original Eau de Cologne by headspace solid-phase microextraction (HS-SPME) followed by gas chromatography-mass spectrometry (GC-MS) with electron impact ionization was developed. A new SPME fiber with a dual coating of divinylbenzene and Carboxen, each suspended in polydimethylsiloxane, was used. The compounds were identified by search of the NIST 98 MS Library or by comparison with pure standards. The experiment was developed for second-year chemistry students to learn the principles of analytical instrumentation (GC-MS) and sample preparation techniques (HS-SPME). The students are able to complete this experiment in a single four-hour laboratory session.

  4. Determination of polychlorinated biphenyls in water using dynamic hollow fiber liquid-phase microextraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Li, Guanhua; Zhang, Lijun; Zhang, Zhanen

    2008-09-12

    The application of dynamic hollow fiber liquid-phase microextraction (dynamic HF-LPME) and gas chromatography-mass spectrometry (GC-MS) for the determination of trace amounts of polychlorinated biphenyls (PCBs) in water was investigated. The experimental parameters were optimized. Under the optimum conditions, the concentration enrichment factors for PCBs were from 718-fold to 840-fold. The calibration curves were linear over a range of 0.05-90 microg/L, with a correlation coefficient (r(2)) of 0.9957-0.9979. The relative standard deviation (RSD) ranged from 3.4% to 5.8% for intra-day variation and from 4.1% to 7.3% for inter-day variation. The limits of detection (LODs, S/N=3:1) were in the range of 13-41 ng/L. The recoveries for spiked water samples ranged from 85.9% to 92.0%.

  5. Analysis of tetramethylene disulfotetramine in foods using solid-phase microextraction-gas chromatography-mass spectrometry.

    Science.gov (United States)

    De Jager, Lowri S; Perfetti, Gracia A; Diachenko, Gregory W

    2008-05-23

    An automated solid-phase microextraction-gas chromatography-mass spectrometry (SPME-GC-MS) method for the determination of tetramethylene disulfotetramine in foods was developed. A comparison of direct immersion (DI) and headspace (HS) extraction techniques using a 70microm carbowax/divinylbenzene (CW/DVB) fiber is presented. The optimized DI-SPME method provided an aqueous extraction limit of detection (LOD) of 9.0ng/g while the HS-SPME LOD was 2.7ng/g. In both SPME modes, recovery was highly matrix dependent and quantification requires standard addition calibrations. Analysis of foods using DI-SPME encountered many obstacles including fiber fouling, low recovery and poor reproducibility. HS-SPME was successfully applied to food analysis with minimal interferences. Standard addition calibration curves for foods gave high linearity (R2>0.98), reproducibility (RSD<12%) and sensitivity with LODs ranging from 0.9 to 4.3ng/g.

  6. The identification of synthetic organic pigments in modern paints and modern paintings using pyrolysis-gas chromatography-mass spectrometry.

    Science.gov (United States)

    Russell, Joanna; Singer, Brian W; Perry, Justin J; Bacon, Anne

    2011-05-01

    A collection of more than 70 synthetic organic pigments were analysed using pyrolysis-gas chromatography-mass spectrometry (Py-GC-MS). We report on the analysis of diketo-pyrrolo-pyrrole, isoindolinone and perylene pigments which are classes not previously reported as being analysed by this technique. We also report on a number of azo pigments (2-naphthol, naphthol AS, arylide, diarylide, benzimidazolone and disazo condensation pigments) and phthalocyanine pigments, the Py-GC-MS analysis of which has not been previously reported. The members of each class were found to fragment in a consistent way and the pyrolysis products are reported. The technique was successfully applied to the analysis of paints used by the artist Francis Bacon (1909-1992), to simultaneously identify synthetic organic pigments and synthetic binding media in two samples of paint taken from Bacon's studio and micro-samples taken from three of his paintings and one painting attributed to him.

  7. Fatty acid composition of wild mushroom species of order Agaricales--examination by gas chromatography-mass spectrometry and chemometrics.

    Science.gov (United States)

    Marekov, Ilko; Momchilova, Svetlana; Grung, Bjørn; Nikolova-Damyanova, Boryana

    2012-12-01

    Applying gas chromatography-mass spectrometry of 4,4-dimethyloxazoline fatty acid derivatives, the fatty acid composition of 15 mushroom species belonging to 9 genera and 5 families of order Agaricales growing in Bulgaria is determined. The structure of 31 fatty acids (not all present in each species) is unambiguously elucidated, with linoleic, oleic and palmitic acids being the main components (ranging between 70.9% (Marasmius oreades) and 91.2% (Endoptychum agaricoides)). A group of three hexadecenoic positionally isomeric fatty acids, 6-, 9- and 11-16:1, appeared to be characteristic components of the examined species. By applying chemometrics it was possible to show that the fatty acid composition closely reflects the classification of the species. Copyright © 2012 Elsevier B.V. All rights reserved.

  8. Headspace solid-phase microextraction-gas chromatography-mass spectrometry applied to quality control in multilayer-packaging manufacture.

    Science.gov (United States)

    Ezquerro, Oscar; Pons, Begoña; Tena, María Teresa

    2003-08-01

    A method based on headspace solid-phase microextraction-gas chromatography-mass spectrometry is proposed for the quality control of multilayer packaging and its manufacturing process. Volatile organic compounds (VOCs) are produced in the manufacturing process of the packaging. They can cause organoleptic problems or modify the properties of the packaging depending on the nature and the amount of the VOCs formed. The quantification using packaging samples with a known VOC concentration for the calibration is proposed in order to reduce the analysis time, and the method is validated using a statistical test. Finally, the method is applied to the determination of odour-responsible compounds in multilayer packaging samples obtained under different extrusion-coating conditions, i.e. type of extruder, type of polymer and extrusion speed.

  9. Rapid determination of quetiapine in blood by gas chromatography-mass spectrometry. Application to post-mortem cases.

    Science.gov (United States)

    López-Guarnido, Olga; Tabernero, María Jesús; Hernández, Antonio F; Rodrigo, Lourdes; Bermejo, Ana M

    2014-10-01

    A simple, fast and sensitive method for the determination of quetiapine in human blood has been developed and validated. The method involved a basic liquid-liquid extraction procedure and subsequent analysis by gas chromatography-mass spectrometry, previous derivatization with bis(trimethylsilyl)-trifluoro-acetamide and chorotrimethylsilane (99 : 1). The methods of validation included linearity with a correlation coefficient > 0.99 over the range 0.02-1 µg ml(-1), intra- and interday precision (always < 12%) and accuracy (mean relative error always < 12%) to meet the bioanalytical acceptance criteria. The limit of detection was 0.005 µg ml(-1). The procedure was further applied to post mortems from the Institute of Legal Medicine, University of Santiago de Compostela. Copyright © 2013 John Wiley & Sons, Ltd.

  10. Gas chromatography-mass spectrometric study of 19-oxygenation of the aromatase inhibitor 19-methylandrostenedione with human placental microsomes.

    Science.gov (United States)

    Numazawa, Mitsuteru; Nagaoka, Masao; Handa, Wakako; Yamada, Akane

    2006-06-01

    To gain insight into the catalytic function of aromatase, we studied 19-oxygenation of 19-methyl-substituted derivative of the natural substrate androstenedione (AD), compound 1, with human placental aromatase by use of gas chromatography-mass spectrometry (GC-MS). Incubation of the 19-methyl derivative 1 with human placental microsomes in the presence of NADPH under an aerobic condition did not yield a detectable amount of [19S]19-hydroxy product 2 or its [19R]-isomer 3 when the product was analyzed as the bis-methoxime-trimethylsilyl (TMS) derivative by GC-MS; moreover, the production of estrogen was not detected as the bis-TMS derivative of estradiol (detection limit: about 3 ng and 10 pg per injection for the 19-ol and estradiol, respectively). The results reveal that the 19-methyl steroid 1 does not serve as a substrate of aromatase, although it does serve as a powerful inhibitor of the enzyme.

  11. Selective 3,4-Dihydroxyphenylalanine Analysis in Human Urine as Ethoxycarbonyltert- butyldimethylsilyl Derivatives by Gas Chromatography-Mass Spectrometry

    International Nuclear Information System (INIS)

    Paik, Man Jeong; Nguyen, Duc Toan; Cho, In Seon; Kim, Kyoung Rae; Cho, Ki Hong; Choi, Sang Dun; Lee, Gwang; Yoon, Jae Hwan; Shim, Woo Young

    2011-01-01

    A new analytical method for measurement of 3,4-dihydroxyphenylalanine (DOPA) in human urine was developed. DOPA from an aqueous solution was converted into an ethoxycarbonyl (EOC) derivative. A tertbutyldimethylsilyl (TBDMS) reaction under anhydrous conditions was then attempted for analysis by gas chromatography-mass spectrometry in selected ion monitoring mode. A new mass spectral data on DOPA as a tri-EOC/mono-TBDMS derivative was built. This method showed good linearity (r ≥ 0.999), precision (% relative standard deviation = 3.1-9.2), and accuracy (% relative error = .7.2-8.8), with a detection limit of 0.05 ng/mL. This selective and accurate method of DOPA analysis will be useful for biochemical monitoring of various neurological disorders including Parkinson's disease in biological fluids

  12. Analysis of Volatile Components of Varietal English Wines Using Stir Bar Sorptive Extraction/Gas Chromatography-Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Darren J. Caven-Quantrill

    2017-12-01

    Full Text Available Aroma is an important property of wine and it can be influenced significantly by enological practices. The aim of this work was, by use of stir bar sorptive extraction/gas chromatography-mass spectrometry (SBSE/GC-MS, to compare semi-quantitative concentrations of the volatile constituents of stainless steel tank-fermented/matured Huxelrebe, Ortega, Schönburger and Siegerrebe varietal wines from a commercial English vineyard, with corresponding wines produced by oak cask (‘barrel’ fermentation/maturation. Aroma profiles of tank and barrel wines were different, with more volatiles detected and net concentrations being higher in barrel wines. Long chain ethyl carboxylate esters were generally more abundant in barrel wines, whereas acetate esters were generally more prominent in tank wines. By conducting a short (~7 month maturation period in secondhand (third or fourth fill casks, it was possible to make wines with more complex aromas, but without obvious oak aroma.

  13. Determination of amphetamine-type stimulants in oral fluid by solid-phase microextraction and gas chromatography-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Souza, Daniele Z., E-mail: daniele.dzs@dpf.gov.br [Setor Tecnico-Cientifico, Superintendencia Regional do Departamento de Policia Federal no Rio Grande do Sul, 1365 Ipiranga Avenue, Azenha, Zip Code 90160-093 Porto Alegre, Rio Grande do Sul (Brazil); Programa de Pos-Graduacao em Ciencias Farmaceuticas, Faculdade de Farmacia, Universidade Federal do Rio Grande do Sul, 2752 Ipiranga Avenue, Santana, Zip Code 90610-000 Porto Alegre, Rio Grande do Sul (Brazil); Boehl, Paula O.; Comiran, Eloisa; Mariotti, Kristiane C. [Programa de Pos-Graduacao em Ciencias Farmaceuticas, Faculdade de Farmacia, Universidade Federal do Rio Grande do Sul, 2752 Ipiranga Avenue, Santana, Zip Code 90610-000 Porto Alegre, Rio Grande do Sul (Brazil); Pechansky, Flavio [Centro de Pesquisa em Alcool e Drogas (CPAD), Hospital de Clinicas de Porto Alegre, Universidade Federal do Rio Grande do Sul, 2350, Ramiro Barcelos Street, Zip Code 90035-903 Porto Alegre, Rio Grande do Sul (Brazil); Duarte, Paulina C.A.V. [Secretaria Nacional de Politicas sobre Drogas (SENAD), Esplanada dos Ministerios, Block ' A' , 5th floor, Zip Code 70050-907 Brasilia, Distrito Federal (Brazil); De Boni, Raquel [Centro de Pesquisa em Alcool e Drogas (CPAD), Hospital de Clinicas de Porto Alegre, Universidade Federal do Rio Grande do Sul, 2350, Ramiro Barcelos Street, Zip Code 90035-903 Porto Alegre, Rio Grande do Sul (Brazil); Froehlich, Pedro E.; Limberger, Renata P. [Programa de Pos-Graduacao em Ciencias Farmaceuticas, Faculdade de Farmacia, Universidade Federal do Rio Grande do Sul, 2752 Ipiranga Avenue, Santana, Zip Code 90610-000 Porto Alegre, Rio Grande do Sul (Brazil)

    2011-06-24

    Graphical abstract: Highlights: > Propylchloroformate derivatization of amphetamine-type stimulants in oral fluid. > Direct immersion solid-phase microextraction/gas chromatography-mass spectrometry. > Linear range 2(4)-256 ng mL{sup -1}, detection limits 0.5-2 ng mL{sup -1}. > Accuracy 98-112%, precision <15% of RSD, recovery 77-112%. > Importance of residual evaluation in checking model goodness-of-fit. - Abstract: A method for the simultaneous identification and quantification of amphetamine (AMP), methamphetamine (MET), fenproporex (FEN), diethylpropion (DIE) and methylphenidate (MPH) in oral fluid collected with Quantisal{sup TM} device has been developed and validated. Thereunto, in-matrix propylchloroformate derivatization followed by direct immersion solid-phase microextraction and gas chromatography-mass spectrometry were employed. Deuterium labeled AMP was used as internal standard for all the stimulants and analysis was performed using the selected ion monitoring mode. The detector response was linear for the studied drugs in the concentration range of 2-256 ng mL{sup -1} (neat oral fluid), except for FEN, whereas the linear range was 4-256 ng mL{sup -1}. The detection limits were 0.5 ng mL{sup -1} (MET), 1 ng mL{sup -1} (MPH) and 2 ng mL{sup -1} (DIE, AMP, FEN), respectively. Accuracy of quality control samples remained within 98.2-111.9% of the target concentrations, while precision has not exceeded 15% of the relative standard deviation. Recoveries with Quantisal{sup TM} device ranged from 77.2% to 112.1%. Also, the goodness-of-fit concerning the ordinary least squares model in the statistical inference of data has been tested through residual plotting and ANOVA. The validated method can be easily automated and then used for screening and confirmation of amphetamine-type stimulants in drivers' oral fluid.

  14. Determination of amphetamine-type stimulants in oral fluid by solid-phase microextraction and gas chromatography-mass spectrometry

    International Nuclear Information System (INIS)

    Souza, Daniele Z.; Boehl, Paula O.; Comiran, Eloisa; Mariotti, Kristiane C.; Pechansky, Flavio; Duarte, Paulina C.A.V.; De Boni, Raquel; Froehlich, Pedro E.; Limberger, Renata P.

    2011-01-01

    Graphical abstract: Highlights: → Propylchloroformate derivatization of amphetamine-type stimulants in oral fluid. → Direct immersion solid-phase microextraction/gas chromatography-mass spectrometry. → Linear range 2(4)-256 ng mL -1 , detection limits 0.5-2 ng mL -1 . → Accuracy 98-112%, precision TM device has been developed and validated. Thereunto, in-matrix propylchloroformate derivatization followed by direct immersion solid-phase microextraction and gas chromatography-mass spectrometry were employed. Deuterium labeled AMP was used as internal standard for all the stimulants and analysis was performed using the selected ion monitoring mode. The detector response was linear for the studied drugs in the concentration range of 2-256 ng mL -1 (neat oral fluid), except for FEN, whereas the linear range was 4-256 ng mL -1 . The detection limits were 0.5 ng mL -1 (MET), 1 ng mL -1 (MPH) and 2 ng mL -1 (DIE, AMP, FEN), respectively. Accuracy of quality control samples remained within 98.2-111.9% of the target concentrations, while precision has not exceeded 15% of the relative standard deviation. Recoveries with Quantisal TM device ranged from 77.2% to 112.1%. Also, the goodness-of-fit concerning the ordinary least squares model in the statistical inference of data has been tested through residual plotting and ANOVA. The validated method can be easily automated and then used for screening and confirmation of amphetamine-type stimulants in drivers' oral fluid.

  15. Application of two-dimensional gas chromatography with electron capture chemical ionization mass spectrometry to the detection of 11-nor-Delta9-tetrahydrocannabinol-9-carboxylic acid (THC-COOH) in hair.

    Science.gov (United States)

    Moore, Christine; Rana, Sumandeep; Coulter, Cynthia; Feyerherm, Fred; Prest, Harry

    2006-04-01

    The proposed federal regulations for the detection in hair of 11-nor-Delta(9)-tetrahydrocannabinol-9-carboxylic acid (THC-COOH), a metabolite of marijuana, require a confirmatory detection level of 0.05 pg/mg. At present, the only way to achieve this on a routine basis has been with the use gas chromatography with tandem mass spectrometry (GC-MS-MS) technology. Tandem MS is an expensive approach and dissuades laboratories from attempting to enter the hair-testing market. A procedure for the determination of THC-COOH in hair using two-dimensional gas chromatography (GC x GC) coupled to mass spectrometry (GC-GC-MS) is described for the first time. The method makes use of several small improvements in the extraction, GC, and MS procedures to allow the required sensitivity to be achieved. The results of this approach demonstrate detection of THC-COOH in hair at a concentration level of 0.05 pg/mg with both a target quantitation ion and a unique confirming qualifier ion, using a single-quadrupole mass selective detector. These two ions and the enhanced separation of the GC-GC provide a high degree of confidence in the determinations. The method has been successfully applied to the detection of THC-COOH in hair specimens from known marijuana users, and it reaches the levels currently proposed in the Federal Register.

  16. Optimizing loop-type cryogenic modulation in comprehensive two-dimensional gas chromatography using time-variable combination of the dual-stage jets for analysis of crude oil.

    Science.gov (United States)

    Alexandrino, Guilherme L; de Sousa, Gustavo R; de A M Reis, Francisco; Augusto, Fabio

    2018-02-09

    The enhanced chromatographic capability of the comprehensive two-dimensional gas chromatography (GC×GC) has already found several applications in analytical chemistry comprising complex samples. However, setting the appropriate chromatographic conditions that maximize sensitivity and separation efficiency in GC×GC may be more difficult than in conventional one-dimension gas chromatography, mainly due to the additional parameters strictly related to the modulation. Loop-type cryogenic modulators have been currently used for crude oil analysis using GC×GC, requiring sometimes a laborious try-and-error procedure to properly tune the dual-jets elapsed times on modulation. In this work, the advantages of choosing a time-variable combination of cold and hot jets pulses in a loop-type cryogenic modulator is presented when performing the fingerprinting analysis of crude oils using GC×GC-QMS, contrary to the conventional procedure based on a single combination for the dual-stage jets. A design of experiments approach is proposed to most effectively optimize the time-variable combination of the dual-jets elapsed times while modulating the wide hydrocarbons range along the GC×GC analysis. The most abundant classes of hydrocarbons contained in the maltenes fraction of a crude oil sample, such as paraffins, aromatics, steranes and hopanes were successfully resolved. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. Dehydration of Methylcyclohexanol Isomers in the Undergraduate Organic Laboratory and Product Analysis by Gas Chromatography-Mass Spectroscopy (GC-MS)

    Science.gov (United States)

    Clennan, Malgorzata M.; Clennan, Edward L.

    2011-01-01

    Dehydrations of "cis"- and "trans"-2-methylcyclohexanol mixtures were carried out with 60% sulfuric acid at 78-80 [degrees]C as a function of time and the products were identified by gas chromatography-mass spectroscopy (GC-MS) analysis. The compounds identified in the reaction mixtures include alkenes, 1-, 3-, and 4-methylcyclohexenes and…

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

    Science.gov (United States)

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

    2012-01-01

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

  19. Characterization of odor-active compounds of various Chrysanthemum essential oils by gas chromatography-olfactometry, gas chromatography-mass spectrometry and their correlation with sensory attributes.

    Science.gov (United States)

    Xiao, Zuobing; Fan, Binbin; Niu, Yunwei; Wu, Minling; Liu, Junhua; Ma, Shengtao

    2016-01-15

    Volatiles of five kinds of Chrysanthemum essential oils with different manufactures were characterized by descriptive sensory analysis, gas chromatography-olfactometry (GC-O), gas chromatography-mass spectrometry (GC-MS) and statistics analysis. Six sensory attributes (floral, woody, grassy, fruity, sour and minty) were selected to assess Chrysanthemum essential oils. A total of 38 volatile compounds were detected and quantified using standard substances by GC-O and GC-MS. Terpenes constituted the largest chemical group among the volatiles of the essential oils. Then partial least squares regression (PLSR) was used to elucidate the relationship between sensory attributes and aroma compounds. The result showed that α-pinene, β-thujene, α-terpinolen, β-cubebene, caryophyllene, (Z)β-farnesene, (-)-spathulenol, linalool, camphor, camphene, 4-terpineol, Z-citral and 4-isopropyltoluene were typical aroma compounds covaried with characteristic aroma of Chrysanthemum essential oils. Copyright © 2015. Published by Elsevier B.V.

  20. Method development and validation for determining 1,3-butadiene in human blood by gas chromatography-mass spectrometry and head-space gas chromatography.

    Science.gov (United States)

    Zhang, Su-Jing; Shen, Bao-Hua; Zhuo, Xian-Yi

    2013-04-01

    To develop a simple, validated method for identifying and quantifying 1,3-butadiene (BD) in human blood by gas chromatography-mass spectrometry (GC-MS) and head-space gas chromatography (HS-GC). BD was identified by GC-MS and HS-GC, and quantified by HS-GC. The method showed that BD had a good linearity from 50 to 500 microg/mL (r > 0.99). The limits of detection and quantification were 10 microg/mL and 50 microg/mL, respectively. Both the intra-day precision and inter-day precision were < 6.08%, and the accuracy was 96.98%-103.81%. The method was applied to an actual case, and the concentration of BD in the case was 242 microg/mL in human blood. This simple method is found to be useful for the routine forensic analysis of acute exposure to BD.

  1. Two-dimensional Quantum Gravity

    Science.gov (United States)

    Rolf, Juri

    1998-10-01

    This Ph.D. thesis pursues two goals: The study of the geometrical structure of two-dimensional quantum gravity and in particular its fractal nature. To address these questions we review the continuum formalism of quantum gravity with special focus on the scaling properties of the theory. We discuss several concepts of fractal dimensions which characterize the extrinsic and intrinsic geometry of quantum gravity. This work is partly based on work done in collaboration with Jan Ambjørn, Dimitrij Boulatov, Jakob L. Nielsen and Yoshiyuki Watabiki (1997). The other goal is the discussion of the discretization of quantum gravity and to address the so called quantum failure of Regge calculus. We review dynamical triangulations and show that it agrees with the continuum theory in two dimensions. Then we discuss Regge calculus and prove that a continuum limit cannot be taken in a sensible way and that it does not reproduce continuum results. This work is partly based on work done in collaboration with Jan Ambjørn, Jakob L. Nielsen and George Savvidy (1997).

  2. Simultaneous quantification of Δ9-tetrahydrocannabinol, 11-hydroxy-Δ9-tetrahydrocannabinol, and 11-nor-Δ9-tetrahydrocannabinol-9-carboxylic acid in human plasma using two-dimensional gas chromatography, cryofocusing, and electron impact-mass spectrometry

    Science.gov (United States)

    Lowe, Ross H.; Karschner, Erin L.; Schwilke, Eugene W.; Barnes, Allan J.; Huestis, Marilyn A.

    2009-01-01

    A two-dimensional (2D) gas chromatography/electron impact-mass spectrometry (GC/EI-MS) method for simultaneous quantification of Δ9-tetrahydrocannabinol (THC), 11-hydroxy-Δ9-tetrahydrocannabinol (11-OH-THC), and 11-nor-Δ9-tetrahydrocannabinol-9-carboxylic acid (THCCOOH) in human plasma was developed and validated. The method employs 2D capillary GC and cryofocusing for enhanced resolution and sensitivity. THC, 11-OH-THC, and THCCOOH were extracted by precipitation with acetonitrile followed by solid-phase extraction. GC separation of trimethylsilyl derivatives of analytes was accomplished with two capillary columns in series coupled via a pneumatic Deans switch system. Detection and quantification were accomplished with a bench-top single quadrupole mass spectrometer operated in electron impact-selected ion monitoring mode. Limits of quantification (LOQ) were 0.125, 0.25 and 0.125 ng/mL for THC, 11-OH-THC, and THCCOOH, respectively. Accuracy ranged from 86.0 to 113.0% for all analytes. Intra- and inter-assay precision, as percent relative standard deviation, was less than 14.1% for THC, 11-OH-THC, and THCCOOH. The method was successfully applied to quantification of THC and its 11-OH-THC and THCCOOH metabolites in plasma specimens following controlled administration of THC. PMID:17640656

  3. Part-per-trillion determination of pharmaceuticals, pesticides, and related organic contaminants in river water by solid-phase extraction followed by comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry.

    Science.gov (United States)

    Matamoros, Víctor; Jover, Eric; Bayona, Josep M

    2010-01-15

    An analytical procedure based on comprehensive two-dimensional gas chromatography (GC x GC) coupled with time-of-flight mass spectrometry (TOF-MS) for the simultaneous determination of 97 organic contaminants at trace concentration in river water is presented. The target analytes included 13 pharmaceuticals, 18 plasticizers, 8 personal care products, 9 acid herbicides, 8 triazines, 10 organophosphorous compounds, 5 phenylureas, 12 organochlorine biocides, 9 polycyclic aromatic hydrocarbons (PAHs), and 5 benzothiazoles and benzotriazoles. The best resolution of the target analytes in the contour plots was obtained when a nonpolar stationary phase was used in the first dimension and polar one in the second. However, in the opposite configuration, polar-nonpolar, the retention time in the second dimension exhibited a strong correlation with the log Kow (p identification criteria. The developed methodology is based on a polymeric solid-phase extraction followed by in GC-port methylation and GC x GC/TOF-MS determination. Moreover, limits of detection (LODs) and quantification (LOQs) ranged from 0.5 to 100 ng/L and from 2 to 185 ng/L, respectively. Repeatability was always lower than 20%. Finally, the developed method has been successfully applied to the determination of incurred target analytes in four river waters subjected to a different anthropogenic pressure.

  4. Simultaneous quantification of Delta9-tetrahydrocannabinol, 11-hydroxy-Delta9-tetrahydrocannabinol, and 11-nor-Delta9-tetrahydrocannabinol-9-carboxylic acid in human plasma using two-dimensional gas chromatography, cryofocusing, and electron impact-mass spectrometry.

    Science.gov (United States)

    Lowe, Ross H; Karschner, Erin L; Schwilke, Eugene W; Barnes, Allan J; Huestis, Marilyn A

    2007-09-07

    A two-dimensional (2D) gas chromatography/electron impact-mass spectrometry (GC/EI-MS) method for simultaneous quantification of Delta(9)-tetrahydrocannabinol (THC), 11-hydroxy-Delta(9)-tetrahydrocannabinol (11-OH-THC), and 11-nor-Delta(9)-tetrahydrocannabinol-9-carboxylic acid (THCCOOH) in human plasma was developed and validated. The method employs 2D capillary GC and cryofocusing for enhanced resolution and sensitivity. THC, 11-OH-THC, and THCCOOH were extracted by precipitation with acetonitrile followed by solid-phase extraction. GC separation of trimethylsilyl derivatives of analytes was accomplished with two capillary columns in series coupled via a pneumatic Deans switch system. Detection and quantification were accomplished with a bench-top single quadrupole mass spectrometer operated in electron impact-selected ion monitoring mode. Limits of quantification (LOQ) were 0.125, 0.25 and 0.125 ng/mL for THC, 11-OH-THC, and THCCOOH, respectively. Accuracy ranged from 86.0 to 113.0% for all analytes. Intra- and inter-assay precision, as percent relative standard deviation, was less than 14.1% for THC, 11-OH-THC, and THCCOOH. The method was successfully applied to quantification of THC and its 11-OH-THC and THCCOOH metabolites in plasma specimens following controlled administration of THC.

  5. Comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry combined with solid phase microextraction as a powerful tool for quantification of ethyl carbamate in fortified wines. The case study of Madeira wine.

    Science.gov (United States)

    Perestrelo, Rosa; Petronilho, Sílvia; Câmara, José S; Rocha, Sílvia M

    2010-05-14

    An analytical methodology based on headspace solid phase microextraction (HS-SPME) combined with comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry (GC x GC-ToFMS) was developed for the identification and quantification of the toxic contaminant ethyl carbamate (EC) directly in fortified wines. The method performance was assessed for dry/medium dry and sweet/medium sweet model wines, and for quantification purposes, calibration plots were performed for both matrices using the ion extraction chromatography (IEC) mode (m/z 62). Good linearity was obtained with a regression coefficient (r(2)) higher than 0.981. A good precision was attained (R.S.D. wines. The quantification limits (LOQ) and recovery for dry wines were 14.38 microg/L and 88.6%, whereas for sweet wines were 9.16 microg/L and 99.4%, respectively. The higher performance was attained with sweet model wine, as increasing of glucose content improves the volatile compound in headspace, and a better linearity, recovery and precision were achieved. The analytical methodology was applied to analyse 20 fortified Madeira wines including different types of wine (dry, medium dry, sweet, and medium sweet) obtained from several harvests in Madeira Island (Portugal). The EC levels ranged from 54.1 microg/L (medium dry) to 162.5 microg/L (medium sweet). 2010 Elsevier B.V. All rights reserved.

  6. Enhancement of two dimensional electron gas concentrations due to Si3N4 passivation on Al0.3Ga0.7N/GaN heterostructure: strain and interface capacitance analysis

    Directory of Open Access Journals (Sweden)

    Syed Mukulika Dinara

    2015-04-01

    Full Text Available Enhancement of two dimensional electron gas (2DEG concentrations at Al0.3Ga0.7N/GaN hetero interface after a-Si3N4 (SiN passivation has been investigated from non-destructive High Resolution X-ray Diffraction (HRXRD analysis, depletion depth and capacitance-voltage (C-V profile measurement. The crystalline quality and strained in-plane lattice parameters of Al0.3Ga0.7N and GaN were evaluated from double axis (002 symmetric (ω-2θ diffraction scan and double axis (105 asymmetric reciprocal space mapping (DA RSM which revealed that the tensile strain of the Al0.3Ga0.7N layer increased by 15.6% after SiN passivation. In accordance with the predictions from theoretical solution of Schrödinger-Poisson’s equations, both electrochemical capacitance voltage (ECV depletion depth profile and C-V characteristics analyses were performed which implied effective 9.5% increase in 2DEG carrier density after passivation. The enhancement of polarization charges results from increased tensile strain in the Al0.3Ga0.7N layer and also due to the decreased surface states at the interface of SiN/Al0.3Ga0.7N layer, effectively improving the carrier confinement at the interface.

  7. Enhanced two dimensional electron gas transport characteristics in Al2O3/AlInN/GaN metal-oxide-semiconductor high-electron-mobility transistors on Si substrate

    Science.gov (United States)

    Freedsman, J. J.; Watanabe, A.; Urayama, Y.; Egawa, T.

    2015-09-01

    The authors report on Al2O3/Al0.85In0.15N/GaN Metal-Oxide-Semiconductor High-Electron-Mobility Transistor (MOS-HEMT) on Si fabricated by using atomic layer deposited Al2O3 as gate insulator and passivation layer. The MOS-HEMT with the gate length of 2 μm exhibits excellent direct-current (dc) characteristics with a drain current maximum of 1270 mA/mm at a gate bias of 3 V and an off-state breakdown voltage of 180 V for a gate-drain spacing of 4 μm. Also, the 1 μm-gate MOS-HEMT shows good radio-frequency (rf) response such as current gain and maximum oscillation cut-off frequencies of 10 and 34 GHz, respectively. The capacitance-voltage characteristics at 1 MHz revealed significant increase in two-dimensional electron gas (2DEG) density for the MOS-HEMT compared to conventional Schottky barrier HEMTs. Analyses using drain-source conductivity measurements showed improvements in 2DEG transport characteristics for the MOS-HEMT. The enhancements in dc and rf performances of the Al2O3/Al0.85In0.15N/GaN MOS-HEMT are attributed to the improvements in 2DEG characteristics.

  8. Enhanced two dimensional electron gas transport characteristics in Al2O3/AlInN/GaN metal-oxide-semiconductor high-electron-mobility transistors on Si substrate

    International Nuclear Information System (INIS)

    Freedsman, J. J.; Watanabe, A.; Urayama, Y.; Egawa, T.

    2015-01-01

    The authors report on Al 2 O 3 /Al 0.85 In 0.15 N/GaN Metal-Oxide-Semiconductor High-Electron-Mobility Transistor (MOS-HEMT) on Si fabricated by using atomic layer deposited Al 2 O 3 as gate insulator and passivation layer. The MOS-HEMT with the gate length of 2 μm exhibits excellent direct-current (dc) characteristics with a drain current maximum of 1270 mA/mm at a gate bias of 3 V and an off-state breakdown voltage of 180 V for a gate-drain spacing of 4 μm. Also, the 1 μm-gate MOS-HEMT shows good radio-frequency (rf) response such as current gain and maximum oscillation cut-off frequencies of 10 and 34 GHz, respectively. The capacitance-voltage characteristics at 1 MHz revealed significant increase in two-dimensional electron gas (2DEG) density for the MOS-HEMT compared to conventional Schottky barrier HEMTs. Analyses using drain-source conductivity measurements showed improvements in 2DEG transport characteristics for the MOS-HEMT. The enhancements in dc and rf performances of the Al 2 O 3 /Al 0.85 In 0.15 N/GaN MOS-HEMT are attributed to the improvements in 2DEG characteristics

  9. Field-effect mobility of a two dimensional electron gas in an n-channel of Si-SiO2 MOS structure with due consideration of some practical features

    Science.gov (United States)

    Basu, A.; Middya, T. R.; Bhattacharya, D. P.

    2017-09-01

    The field-effect mobility characteristics of a non-degenerate ensemble of a two dimensional electron gas for interaction with acoustic mode lattice vibrations in the Si-SiO2 MOS structure at the high surface electric fields are calculated here for the low and high temperature cases. The calculation takes due account of some features which are usually neglected. These include the effects of (i) the transverse component of the phonon wave vector, (ii) the realistic model of the infinite triangular potential well along the transverse direction, while applying the momentum conservation approximation, and (iii) the full form of the phonon distribution function at low temperatures. The results seem to be interesting in that they are significantly different from what follows from other theories that neglect the effects of the above features. Moreover, the agreement between the results which are obtained here with the experimental data seems to be significantly better. The scope for further refinement of the present theory has been discussed.

  10. Analysis of organic compounds of water-in-crude oil emulsions separated by microwave heating using comprehensive two-dimensional gas chromatography and time-of-flight mass spectrometry.

    Science.gov (United States)

    Freitas, Lisiane S; Von Mühlen, Carin; Bortoluzzi, Janaína H; Zini, Claudia A; Fortuny, Montserrat; Dariva, Claudio; Coutinho, Raquel C C; Santos, Alexandre F; Caramão, Elina B

    2009-04-03

    In this work the higher peak capacity and resolution of comprehensive two-dimensional gas chromatography (GCxGC) has been successfully applied, for the first time, to tentatively identify several polar organic compounds of organic extracts of aqueous phases resulting from microwave demulsification process of water-in-crude oil emulsions. Results have shown that higher temperatures and longer exposure time to microwave irradiation produced water phases with a wider variety of polar organic compounds. The microwave process showed to be suitable for the extraction of several polar compounds classes of petroleum. The proposed microwave extraction method and GCxGC identification of polar compounds of petroleum samples are of practical interest for the petrochemical industry due to corrosion and related problems associated with these polar compounds in refinery equipments. The GCxGC/time-of-flight MS technique shows to be very important in the total separation of different classes of compounds and allows the identification of many compounds in these classes.

  11. Determination of benzene, toluene, ethylbenzene and xylenes in air by solid phase micro-extraction/gas chromatography/mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Tumbiolo, Simonetta; Gal, Jean-Francois; Maria, Pierre-Charles [Universite de Nice-Sophia Antipolis, Laboratoire de Radiochimie, Sciences Analytiques et Environnement, Faculte des Sciences, Nice Cedex 2 (France); Zerbinati, Orfeo [Universita del Piemonte Orientale ' ' Amedeo Avogadro' ' , Dipartimento di Scienze e Tecnologie Avanzate, Alessandria (Italy)

    2004-11-01

    The aim of the study was to analyse BTEX compounds (benzene, toluene, ethylbenzene, xylenes) in air by solid phase micro-extraction/gas chromatography/mass spectrometry (SPME/GC/MS), and this article presents the features of the calibration method proposed. Examples of real-world air analysis are given. Standard gaseous mixtures of BTEX in air were generated by dynamic dilution. SPME sampling was carried out under non-equilibrium conditions using a Carboxen/PDMS fibre exposed for 30 min to standard gas mixtures or to ambient air. The behaviour of the analytical response was studied from 0 to 65 {mu}g/m{sup 3} by adding increasing amounts of BTEX to the air matrix. Detection limits range from 0.05 to 0.1 {mu}g/m{sup 3} for benzene, depending on the fibre. Inter-fibre relative standard deviations (reproducibility) are larger than 18%, although the repeatability for an individual fibre is better than 10%. Therefore, each fibre should be considered to be a particular sampling device, and characterised individually depending on the required accuracy. Sampling indoor and outdoor air by SPME appears to be a suitable short-delay diagnostic method for volatile organic compounds, taking advantage of short sampling time and simplicity. (orig.)

  12. Determination of Levetiracetam in Human Plasma by Dispersive Liquid-Liquid Microextraction Followed by Gas Chromatography-Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Greyce Kelly Steinhorst Alcantara

    2016-01-01

    Full Text Available Levetiracetam (LEV is an antiepileptic drug that is clinically effective in generalized and partial epilepsy syndromes. The use of this drug has been increasing in clinical practice and intra- or -interindividual variability has been exhibited for special population. For this reason, bioanalytical methods are required for drug monitoring in biological matrices. So this work presents a dispersive liquid-liquid microextraction method followed by gas chromatography-mass spectrometry (DLLME-GC-MS for LEV quantification in human plasma. However, due to the matrix complexity a previous purification step is required. Unlike other pretreatment techniques presented in the literature, for the first time, a procedure employing ultrafiltration tubes Amicon® (10 kDa porous size without organic solvent consumption was developed. GC-MS analyses were carried out using a linear temperature program, capillary fused silica column, and helium as the carrier gas. DLLME optimized parameters were type and volume of extraction and dispersing solvents, salt addition, and vortex agitation time. Under chosen parameters (extraction solvent: chloroform, 130 μL; dispersing solvent: isopropyl alcohol, 400 μL; no salt addition and no vortex agitation time, the method was completely validated and all parameters were in agreement with the literature recommendations. LEV was quantified in patient’s plasma sample using less than 550 μL of organic solvent.

  13. Fragmentation Pathways of Trifluoroacetyl Derivatives of Methamphetamine, Amphetamine, and Methylenedioxyphenyl alkylamine Designer Drugs by Gas Chromatography/Mass Spectrometry

    International Nuclear Information System (INIS)

    Kumazawa, T.; Xiao-Pen, L.; Sato, K.

    2011-01-01

    Methamphetamine (MA), amphetamine (AM), and the methylenedioxyphenyl alkylamine designer drugs, such as 3,4-methylenedioxymethamphetamine (MDMA), 3,4-methylenedioxy ethylamphetamine (MDEA), N-methyl-1-(3,4-methylenedioxyphenyl)-2-butanamine (MBDB), 3,4-methylenedioxyamphetamine (MDA), and 3,4-(methylenedioxyphenyl)-2-butanamine (BDB), are widely abused as psychedelics. In this paper, these compounds were derivatized with trifluoroacetic (TFA) anhydride and analyzed by gas chromatography/mass spectrometry using electron ionization in positive mode. Gas chromatographic separation for TFA derivatives of all compounds was successfully resolved using an Equity-5 fused silica capillary column with a poly (5% diphenyl-95% dimethylsiloxane) stationary phase. Base peaks or prominent peaks of MA, AM, MDMA, MDEA, MBDB, MDA, and BDB appeared at m/z 154, 140, 154, 168, 168, 135, and 135, respectively. These occurred due to a-cleavage from the amide nitrogen, splitting into the TFA imine species and benzyl or methylenedioxybenzyl cations. Further prominent fragment ions at m/z 118 for MA and AM, m/z 162 for MDMA, MDEA, and MDA, and m/z 176 for MBDB and BDB were produced by cleavage of the phenylpropane or methylenedioxy propane hydrocarbon radical cation via a hydrogen rearrangement. These fragmentation pathways for the TFA derivatives of all the compounds are summarized and illustrated in this paper.

  14. Correlation of rocket propulsion fuel properties with chemical composition using comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry followed by partial least squares regression analysis.

    Science.gov (United States)

    Kehimkar, Benjamin; Hoggard, Jamin C; Marney, Luke C; Billingsley, Matthew C; Fraga, Carlos G; Bruno, Thomas J; Synovec, Robert E

    2014-01-31

    There is an increased need to more fully assess and control the composition of kerosene-based rocket propulsion fuels such as RP-1. In particular, it is critical to make better quantitative connections among the following three attributes: fuel performance (thermal stability, sooting propensity, engine specific impulse, etc.), fuel properties (such as flash point, density, kinematic viscosity, net heat of combustion, and hydrogen content), and the chemical composition of a given fuel, i.e., amounts of specific chemical compounds and compound classes present in a fuel as a result of feedstock blending and/or processing. Recent efforts in predicting fuel chemical and physical behavior through modeling put greater emphasis on attaining detailed and accurate fuel properties and fuel composition information. Often, one-dimensional gas chromatography (GC) combined with mass spectrometry (MS) is employed to provide chemical composition information. Building on approaches that used GC-MS, but to glean substantially more chemical information from these complex fuels, we recently studied the use of comprehensive two dimensional (2D) gas chromatography combined with time-of-flight mass spectrometry (GC×GC-TOFMS) using a "reversed column" format: RTX-wax column for the first dimension, and a RTX-1 column for the second dimension. In this report, by applying chemometric data analysis, specifically partial least-squares (PLS) regression analysis, we are able to readily model (and correlate) the chemical compositional information provided by use of GC×GC-TOFMS to RP-1 fuel property information such as density, kinematic viscosity, net heat of combustion, and so on. Furthermore, we readily identified compounds that contribute significantly to measured differences in fuel properties based on results from the PLS models. We anticipate this new chemical analysis strategy will have broad implications for the development of high fidelity composition-property models, leading to an

  15. Measurement of selected polybrominated diphenyl ethers, polybrominated and polychlorinated biphenyls, and organochlorine pesticides in human serum and milk using comprehensive two-dimensional gas chromatography isotope dilution time-of-flight mass spectrometry.

    Science.gov (United States)

    Focant, Jean-François; Sjödin, Andreas; Turner, Wayman E; Patterson, Donald G

    2004-11-01

    A new method using comprehensive two-dimensional gas chromatography and isotope dilution time-of-flight mass spectrometry (GCxGC-IDTOFMS) for the simultaneous measurement of selected polychlorinated biphenyls (PCBs), organochlorine pesticides (OCPs), and brominated flame retardants is presented. In contrast to the reference methods based on classical GC/MS, a single injection of the extract containing all compounds of interest results in accurate identification and quantification. Using GCxGC ensures the chromatographic separation of most compounds, and TOFMS allows mass spectral deconvolution of coeluting compounds as well as the use of (13)C-labeled internal standards for quantification. Isotope ratio measurements of the most intense ions for both native and labels ensure the required specificity. The use of this new method with an automated sample preparation procedure developed at the Centers for Disease Control and Prevention (CDC) for the analysis of human serum and milk compared favorably to conventional isotope-dilution one-dimensional gas chromatography-high-resolution mass spectrometry (GC-IDHRMS) for the different human serum and milk pools tested. The instrumental detection limits ranged between 0.5 pg/microL and 10 pg/microL and the method detection limits ranged between 1 and 15 pg/microL (N = 59 analytes). The reproducibility of the method was almost as good as with GC-IDHRMS, the relative standard deviations ranging between 1 and 11% for OCPs measured in human serum. OCP, PBDE, and PCB levels measured using the two methods were highly correlated, and the deviations between the two methods were below 20% for most analytes with concentrations above 1 ng/g milk lipids.

  16. [Structure determination of alkyd resins by simultaneous pyrolysis methylation gas chromatography-mass spectometry].

    Science.gov (United States)

    Cao, J Y; Fu, D H; Zhang, F; Liang, D

    2000-09-01

    Several types of alkyd resins have been analyzed by simultaneous pyrolysis methylation gas chromatography mass spectrometry (SPM-GC-MS). The samples were mixed with tetramethylammonium hydroxide, and the process included simultaneous pyrolysis derivatization and mass spectrometry determination. SPM-GC-MS conditions: a vertical microfurnace-type pyrolyzer was directly attached to a gas chromatograph-mass spectrometer. About 20 ug of the mixed alkyd resin sample was introduced into the center of the pyrolyzer at 450 degrees C under the flow of helium carrier gas. The inlet mode was split with an injection interval of 10 s and the inlet pressure was 82.7 kPa. The gas chromatograph was fitted with a fused-silica capillary column ( SE-54 30 m x0.25 mm i.d. x 0.25 um). Temperature program settings were: initial temperature, 40 degrees C, hold 2 min; increase at 6 degrees C min 1 to 220 degrees C, hold 14 min; increase at 10 degrees C min 1 to 280 degrees C, hold 8 min. All pyrolysis products referred to were identified by mass spectrometry. The temperature of the ion source was 210 degrees C and that of the transfer line was 250 degrees C. The technique could give additional information about the composition of the dibasic acids, polyols, six types of drying oils, and modified alkyd resins. The method is sensitive, accurate, convenient, and involves minimal sample manipulation.

  17. The theory of critical phenomena in two-dimensional systems

    International Nuclear Information System (INIS)

    Olvera de la C, M.

    1981-01-01

    An exposition of the theory of critical phenomena in two-dimensional physical systems is presented. The first six chapters deal with the mean field theory of critical phenomena, scale invariance of the thermodynamic functions, Kadanoff's spin block construction, Wilson's renormalization group treatment of critical phenomena in configuration space, and the two-dimensional Ising model on a triangular lattice. The second part of this work is made of four chapters devoted to the application of the ideas expounded in the first part to the discussion of critical phenomena in superfluid films, two-dimensional crystals and the two-dimensional XY model of magnetic systems. Chapters seven to ten are devoted to the following subjects: analysis of long range order in one, two, and three-dimensional physical systems. Topological defects in the XY model, in superfluid films and in two-dimensional crystals. The Thouless-Kosterlitz iterated mean field theory of the dipole gas. The renormalization group treatment of the XY model, superfluid films and two-dimensional crystal. (author)

  18. Chemotaxonomic Characterization of Microorganisms by Capillary Gas Chromatography-Mass Spectrometry

    Science.gov (United States)

    1988-06-01

    indirectly detecting differences in carbohydrate composition ( Lancefield grouping ). The group B-specific polysaccharide consists of a backbcne of...carbohydrate pyrolysis product generated from the glucitol moiety. We have further used pattern recognition to differentiate several Lancefield groups of... Group A and Group B Streptococci by Pyrolysis Gas Chromatography- Mass Spectrometry," A- alytical Chemistry, 59, 1410-1413 (1987). S. L. Morgan, M. D

  19. Carbohydrate analysis of hemicelluloses by gas chromatography-mass spectrometry of acteylated methyl glycosides

    DEFF Research Database (Denmark)

    Sárossy, Zsuzsa; Plackett, David; Egsgaard, Helge

    2012-01-01

    A method based on gas chromatography–mass spectrometry analysis of acetylated methyl glycosides was developed in order to analyze monosaccharides obtained from various hemicelluloses. The derivatives of monosaccharide standards, arabinose, glucose, and xylose were studied in detail and 13C-labele......-labeled analogues were used for identification and quantitative analysis. Excellent chromatographic separation of the monosaccharide derivatives was found and identification of the anomeric configuration was feasible through a prepared and identified pure methyl 2,3,4,6-tetra...

  20. Identification of bound alcohols in soil humic acids by gas chromatography-mass spectrometry

    OpenAIRE

    Berthier , Gersende; Dou , Sen; Peakman , Torren; Lichtfouse , Eric

    2000-01-01

    International audience; Humic acids are complex, partly macromolecular, yellow-brownish substances occurring in soils, waters and sediments. In order to shed some light on their molecular structure, crop humic acids were cleaved by alkaline hydrolysis (KOH). The products were fractionated by thin layer chromatography to give mono-alcohols which were analysed as acetate derivatives by gas chromatography coupled to mass spectrometry. Linear alcohols, sterols, stanols and plant-derived triterpen...

  1. Quasi-two-dimensional electron gas at the interface of γ-Al{sub 2}O{sub 3}/SrTiO{sub 3} heterostructures grown by atomic layer deposition

    Energy Technology Data Exchange (ETDEWEB)

    Ngo, Thong Q.; McDaniel, Martin D.; Ekerdt, John G., E-mail: ekerdt@che.utexas.edu [Department of Chemical Engineering, University of Texas at Austin, Austin, Texas 78712 (United States); Goble, Nicholas J.; Gao, Xuan P. A. [Department of Physics, Case Western Reserve University, Cleveland, Ohio 44106 (United States); Posadas, Agham; Kormondy, Kristy J.; Demkov, Alexander A. [Department of Physics, University of Texas at Austin, Austin, Texas 78712 (United States); Lu, Sirong [School of Engineering for Matter, Transport and Engineering, Arizona State University, Tempe, Arizona 85287 (United States); Jordan-Sweet, Jean [IBM T.J. Watson Research Center, Yorktown Heights, New York 10598 (United States); Smith, David J. [Department of Physics, Arizona State University, Tempe, Arizona 85287 (United States)

    2015-09-21

    We report the formation of a quasi-two-dimensional electron gas (2-DEG) at the interface of γ-Al{sub 2}O{sub 3}/TiO{sub 2}-terminated SrTiO{sub 3} (STO) grown by atomic layer deposition (ALD). The ALD growth of Al{sub 2}O{sub 3} on STO(001) single crystal substrates was performed at temperatures in the range of 200–345 °C. Trimethylaluminum and water were used as co-reactants. In situ reflection high energy electron diffraction, ex situ x-ray diffraction, and ex situ cross-sectional transmission electron microscopy were used to determine the crystallinity of the Al{sub 2}O{sub 3} films. As-deposited Al{sub 2}O{sub 3} films grown above 300 °C were crystalline with the γ-Al{sub 2}O{sub 3} phase. In situ x-ray photoelectron spectroscopy was used to characterize the Al{sub 2}O{sub 3}/STO interface, indicating that a Ti{sup 3+} feature in the Ti 2p spectrum of STO was formed after 2–3 ALD cycles of Al{sub 2}O{sub 3} at 345 °C and even after the exposure to trimethylaluminum alone at 300 and 345 °C. The interface quasi-2-DEG is metallic and exhibits mobility values of ∼4 and 3000 cm{sup 2} V{sup −1} s{sup −1} at room temperature and 15 K, respectively. The interfacial conductivity depended on the thickness of the Al{sub 2}O{sub 3} layer. The Ti{sup 3+} signal originated from the near-interfacial region and vanished after annealing in an oxygen environment.

  2. Tile-based Fisher ratio analysis of comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC × GC-TOFMS) data using a null distribution approach.

    Science.gov (United States)

    Parsons, Brendon A; Marney, Luke C; Siegler, W Christopher; Hoggard, Jamin C; Wright, Bob W; Synovec, Robert E

    2015-04-07

    Comprehensive two-dimensional (2D) gas chromatography coupled with time-of-flight mass spectrometry (GC × GC-TOFMS) is a versatile instrumental platform capable of collecting highly informative, yet highly complex, chemical data for a variety of samples. Fisher-ratio (F-ratio) analysis applied to the supervised comparison of sample classes algorithmically reduces complex GC × GC-TOFMS data sets to find class distinguishing chemical features. F-ratio analysis, using a tile-based algorithm, significantly reduces the adverse effects of chromatographic misalignment and spurious covariance of the detected signal, enhancing the discovery of true positives while simultaneously reducing the likelihood of detecting false positives. Herein, we report a study using tile-based F-ratio analysis whereby four non-native analytes were spiked into diesel fuel at several concentrations ranging from 0 to 100 ppm. Spike level comparisons were performed in two regimes: comparing the spiked samples to the nonspiked fuel matrix and to each other at relative concentration factors of two. Redundant hits were algorithmically removed by refocusing the tiled results onto the original high resolution pixel level data. To objectively limit the tile-based F-ratio results to only features which are statistically likely to be true positives, we developed a combinatorial technique using null class comparisons, called null distribution analysis, by which we determined a statistically defensible F-ratio cutoff for the analysis of the hit list. After applying null distribution analysis, spiked analytes were reliably discovered at ∼1 to ∼10 ppm (∼5 to ∼50 pg using a 200:1 split), depending upon the degree of mass spectral selectivity and 2D chromatographic resolution, with minimal occurrence of false positives. To place the relevance of this work among other methods in this field, results are compared to those for pixel and peak table-based approaches.

  3. Enhanced two dimensional electron gas transport characteristics in Al{sub 2}O{sub 3}/AlInN/GaN metal-oxide-semiconductor high-electron-mobility transistors on Si substrate

    Energy Technology Data Exchange (ETDEWEB)

    Freedsman, J. J., E-mail: freedy54@gmail.com; Watanabe, A.; Urayama, Y. [Research Center for Nano-Devices and Advanced Materials, Nagoya Institute of Technology, Gokiso-cho, Showa-ku, Nagoya 466 8555 (Japan); Egawa, T., E-mail: egawa.takashi@nitech.ac.jp [Research Center for Nano-Devices and Advanced Materials, Nagoya Institute of Technology, Gokiso-cho, Showa-ku, Nagoya 466 8555 (Japan); Innovation Center for Multi-Business of Nitride Semiconductors, Nagoya Institute of Technology, Gokiso-cho, Showa-ku, Nagoya 466 8555 (Japan)

    2015-09-07

    The authors report on Al{sub 2}O{sub 3}/Al{sub 0.85}In{sub 0.15}N/GaN Metal-Oxide-Semiconductor High-Electron-Mobility Transistor (MOS-HEMT) on Si fabricated by using atomic layer deposited Al{sub 2}O{sub 3} as gate insulator and passivation layer. The MOS-HEMT with the gate length of 2 μm exhibits excellent direct-current (dc) characteristics with a drain current maximum of 1270 mA/mm at a gate bias of 3 V and an off-state breakdown voltage of 180 V for a gate-drain spacing of 4 μm. Also, the 1 μm-gate MOS-HEMT shows good radio-frequency (rf) response such as current gain and maximum oscillation cut-off frequencies of 10 and 34 GHz, respectively. The capacitance-voltage characteristics at 1 MHz revealed significant increase in two-dimensional electron gas (2DEG) density for the MOS-HEMT compared to conventional Schottky barrier HEMTs. Analyses using drain-source conductivity measurements showed improvements in 2DEG transport characteristics for the MOS-HEMT. The enhancements in dc and rf performances of the Al{sub 2}O{sub 3}/Al{sub 0.85}In{sub 0.15}N/GaN MOS-HEMT are attributed to the improvements in 2DEG characteristics.

  4. On the use of ionic liquid capillary columns for analysis of aromatic hydrocarbons in low-boiling petrochemical products by one-dimensional and comprehensive two-dimensional gas chromatography.

    Science.gov (United States)

    Krupčík, Ján; Gorovenko, Roman; Špánik, Ivan; Bočková, Ingrid; Sandra, Pat; Armstrong, Daniel W

    2013-08-02

    One-dimensional and comprehensive two-dimensional flow modulated gas chromatography with simultaneous flame ionization and mass spectrometric detection were applied for the identification and quantification of benzene, toluene, ethyl benzene and xylenes (BTEX) as well as of all C9-C11 aromatic hydrocarbons in the low-boiling petroleum products gasoline, reformate and fluid catalytic cracking (FCC) samples. GC×GC experiments were performed on two reversed phase polarity column sets namely SLB-IL100 (25m×250μm i.d.×0.2μm df)+HP-5MS (5m×250μm i.d.×0.25μm df) and SLB-IL111 (30m×250μm i.d.×0.2μm df)+HP-5MS (5m×250μm i.d.×0.25μm df). The one-dimensional GC experiments were carried out on the same ionic liquid columns. The most powerful method is GC×GC on the SLB-111+HP-5MS column combination. Quantitative analysis of individual aromatic hydrocarbons (C6-C11) present in gasoline, reformate and fluid catalytic cracking (FCC) samples was performed by GC×GC-FID using the internal normalization method. Mass spectra obtained by GC×GC-qMSD were used for identification of the aromatic hydrocarbons in these samples. Copyright © 2013 Elsevier B.V. All rights reserved.

  5. Identification of fentanyl metabolites in rat urine by gas chromatography-mass spectrometry with stable-isotope tracers

    Energy Technology Data Exchange (ETDEWEB)

    Goromaru, T.; Matsuura, H.; Furuta, T.; Baba, S.; Yoshimura, N.; Miyawaki, T.; Sameshima, T.

    The metabolites of fentanyl (l), which has been widely used as a neuroleptic analgesic agent, were identified in urine of rats by gas chromatography-mass spectrometry combined with a stable-isotope tracer technique. After the oral administration of an equimolar mixture of l and deuterium-labeled l (l/l-d5), the urinary metabolites were extracted with chloroform at pH 9.0. Extracts were derivatized and analyzed by GC/MS. Metabolites were identified by the presence of doublet ion peaks separated by 5 amu, and chemical structures were established from analyses of fragmentation pathways. The metabolites were identified as 4-N-(N-propionylanilino)-piperidine, 4-N-(N-hydroxypropionylanilino)piperidine, 4-N-(N-propionylanilino) hydroxypiperidine, 1-(2-phenethyl)-4-N-(N-hydroxypropionylanilino)piperidine and 1-(2-phenethyl)-4-N-(N-propionylanilino)hydroxypiperidine. These metabolites, together with unchanged l, were also detected in urine of rats receiving l/l-d5 intravenously, by selected-ion monitoring of the specific cluster ions.

  6. Gas chromatography-mass spectrometry analysis of different organic crude extracts from the local medicinal plant of Thymus vulgaris L.

    Science.gov (United States)

    Hashmi, Laila Salim Al; Hossain, Mohammad Amzad; Weli, Afaf Mohammed; Al-Riyami, Qasim; Al-Sabahi, Jamal Nasser

    2013-01-01

    To isolate and analyze the chemical composition in different crude extracts of from the leaves of locally grown of Thymus vulgaris L (T. vulgaris) by gas chromatography-mass spectrometry (GC-MS). The shade dried leaves powder was extracted with methanol by using Soxhlet extractor. Methanol crude extracts of T. vulgaris and the derived fractions of hexane, chloroform, ethyl acetate and butanol were obtained. Qualitative analyses of various organic crude extracts of T. vulgaris by using GC-MS showed that there were different types of high and low molecular weight compounds. Most of the isolated and identified compounds by GC-MS in the crude extracts are basically biologically important. Further, the T. vulgaris leaf possessed certain characteristics that can be ascribed to cultivation on a domestic plantation. The crude extracts were prepared from the powder leaves of T. vulgaris for respective compounds can be chosen on the basis of above GC-MS analysis. All the major compounds were identified and characterized by spectroscopic method in different organic crude extracts of T. vulgaris are biologically active molecules. Thus the identification of a good number of compounds in various crude extracts of T. vulgaris might have some ecological role.

  7. Characterization of volatile compounds in fermented milk using solid-phase microextraction methods coupled with gas chromatography-mass spectrometry.

    Science.gov (United States)

    Dan, T; Wang, D; Jin, R L; Zhang, H P; Zhou, T T; Sun, T S

    2017-04-01

    Lactic acid bacteria (LAB) are industrially important bacteria that are widely used in the fermented food industry, especially in the manufacture of yogurt. Characteristic flavors are produced by LAB during fermentation and storage that affect the quality and acceptability of fermented milk products. In this study, the volatile compounds in milk fermented by Streptococcus thermophilus IMAU80842 alone, Lactobacillus delbrueckii ssp. bulgaricus IMAU20401 alone, or both species together were identified using solid-phase microextraction methods coupled with gas chromatography-mass spectrometry. A total of 53, 43, and 32 volatile compounds were identified in milk fermented by S. thermophilus alone, L. delbrueckii ssp. bulgaricus alone, or both species together, respectively. The presence of some important flavor compounds was confirmed: acetic acid, acetaldehyde, acetoin, 2,3-butanedione, ethanol, and 1-heptanol. Our results demonstrate that the composition of the volatile compounds in fermented milk depends on the species of LAB used and whether they are used alone or in combination. This is important for the selection of appropriate starter cultures for the production of different types of fermented milk product with particular flavors. Copyright © 2017 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

  8. Implementation of an Environmental Focus in an Undergraduate Chemistry Curriculum by the Addition of Gas Chromatography-Mass Spectrometry

    Science.gov (United States)

    Atterholt, Cynthia; Butcher, David J.; Bacon, J. Roger; Kwochka, William R.; Woosley, Royce

    2000-12-01

    The Department Chemistry and Physics at Western Carolina University has added an environmental focus to its curriculum, and gas chromatography-mass spectrometry (GC-MS) was identified as an essential tool in environmental analysis. GC-MS is used in undergraduate chemistry courses in: (i) the identification of synthesized compounds and natural products, (ii) monitoring compounds and their degradation in the environment, and (iii) analytical method development. In Organic Chemistry, the GC-MS is used to characterize natural products and the products of an environmentally benign chemical synthesis. In Environmental Chemistry, the GC-MS is used to identify compounds of environmental interest, such as pesticides in soil samples, polycyclic aromatic hydrocarbons in water, and hydrocarbons in gasoline samples. In Instrumental Analysis I, students characterize numerous compounds in cigarette smoke using GC-MS. In Instrumental Analysis II, students are presented with an analytical chemistry problem for which they research protocols, collect samples, and perform the analyses. The GC-MS has been used to identify volatile compounds in a number of complex mixtures. Also, research in chemistry is a significant part of our curriculum, and numerous undergraduate students have used the GC-MS in their research. The addition of GC-MS has enhanced many of our undergraduate laboratory courses and student-led research projects.

  9. Characterization of commercial synthetic resins by pyrolysis-gas chromatography/mass spectrometry: application to modern art and conservation.

    Science.gov (United States)

    Peris-Vicente, J; Baumer, U; Stege, H; Lutzenberger, K; Gimeno Adelantado, J V

    2009-04-15

    To characterize a set of synthetic resins, a methodology by pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) has been developed. The studied reference materials were commercial versions of a wide range of synthetic resins. For each polymer, the pyrolytic and chromatographic conditions were optimized to adequately resolve the fragment mixture in a short time. The proposed analytical method does not require previous treatment of the sample, and due to its high sensitivity, only a small sample quantity in the microgram range can be used. The pyrolysis temperature was found to have little effect on the obtained pyrograms. The summarized data set for the individual polymer materials, especially the characteristic fragments with a structure close to the monomeric unit, was useful to identify commercial synthetic resins. These materials were used in the art and conservation field, as binding media, paint additives, painting varnishes, coatings, or consolidants. Two case studies are introduced where direct Py-GC/MS and thermally assisted hydrolysis and methylation GC/MS were applied on art objects: first, a modern gluing material of a medieval reverse glass painting, and the second example, the binding medium of a painting by Georg Baselitz ("Senta", 1992/1993) from the Sammlung Moderne Kunst at the Pinakothek der Moderne, Munich.

  10. Rapid detection of five anesthetics in tilapias by in vivo solid phase microextraction coupling with gas chromatography-mass spectrometry.

    Science.gov (United States)

    Huang, Shuyao; Xu, Jianqiao; Wu, Jiayi; Hong, Haojia; Chen, Guosheng; Jiang, Ruifen; Zhu, Fang; Liu, Yuan; Ouyang, Gangfeng

    2017-06-01

    The concentration of five rapidly metabolized anesthetics in living tilapias was determined in this study, by the presented method coupling in vivo solid phase microextraction (SPME) to gas chromatography-mass spectrometry (GC-MS), which was the first time that in vivo sampling method was adapted in detecting the anesthetic residue in the living aquatic product. The analytical performance of the developed method was evaluated in homogenized tilapia dorsal muscle, and the results demonstrated that the present method possessed low detection limits 1.7-9.4ngg -1 ), wide linear ranges (10 or 30-5000ngg -1 ), and satisfactory reproducibility (relative standard deviations no more than 8.1% and 10.8% for inter-fiber and intra-fiber assays, respectively). Standard curves were established in homogenized tilapia dorsal muscle for calibrating in vivo SPME in living tilapias. And the concentrations determined by in vivo SPME were close to those determined by the liquid extraction. By using the present method, one anesthetic residue was detected above the detection limit in tilapias from the local markets. Comparing to traditional methods, the present one exhibited superior time-efficiency and cost performance, as the extraction time was only ten minutes, which was short to successfully avoid the possible loss of analytes caused by elimination and sample storage. In addition, owing to the time-efficiency of the present method, the elimination of the anesthetics in tilapias was traced successfully in the laboratory. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Phytochemical Profile of Erythrina variegata by Using High-Performance Liquid Chromatography and Gas Chromatography-Mass Spectroscopy Analyses.

    Science.gov (United States)

    Muthukrishnan, Suriyavathana; Palanisamy, Subha; Subramanian, Senthilkumar; Selvaraj, Sumathi; Mari, Kavitha Rani; Kuppulingam, Ramalingam

    2016-08-01

    Natural products derived from plant sources have been utilized to treat patients with numerous diseases. The phytochemical constituents present in ethanolic leaf extract of Erythrina variegata (ELEV) were identified by using high-performance liquid chromatography (HPLC) and gas chromatography-mass spectroscopy (GC-MS) analyses. Shade dried leaves were powdered and extracted with ethanol for analyses through HPLC to identify selected flavonoids and through GC-MS to identify other molecules. The HPLC analysis of ELEV showed the presence of gallic and caffeic acids as the major components at concentrations of 2.0 ppm and 0.1 ppm, respectively, as well as other components. GC-MS analysis revealed the presence of 3-eicosyne; 3,7,11,15-tetramethyl-2-hexadecen-1-ol; butanoic acid, 3-methyl-3,7-dimethyl-6-octenyl ester; phytol; 1,2-benzenedicarboxylic acid, diundecyl ester; 1-octanol, 2-butyl-; squalene; and 2H-pyran, 2-(7-heptadecynyloxy) tetrahydro-derivative. Because pharmacopuncture is a new evolving natural mode that uses herbal extracts for treating patients with various ailments with minimum pain and maximum effect, the results of this study are particularly important and show that ELEV possesses a wide range of phytochemical constituents, as indicated above, as effective active principle molecules that can be used individually or in combination to treat patients with various diseases. Copyright © 2016. Published by Elsevier B.V.

  12. [Determination of five synthetic musks in perfume by headspace solid-phase microextraction and gas chromatography-mass spectrometry].

    Science.gov (United States)

    Wang, Guannan; Tang, Hua; Chen, Dazhou; Feng, Jie; Li, Lei

    2012-02-01

    A method for headspace solid-phase microextraction (HS-SPME), followed by gas chromatography-mass spectrometry (GC-MS) analysis was established for the determination of five commonly used synthetic musks in perfume. Two polycyclic musks (celestolide and tonalide) and three nitro musks (musk ambrette, musk xylene and musk ketone) were used as analytes in the optimization of the analytical method. Six parameters, such as the extraction temperature, equilibrium time, extraction time, desorption time, injector temperature and solution of salting out, were optimized by exposing the 65 microm polydimethylsiloxane-divinyl-benzene (PDMS-DVB) fiber to the headspace of magnetically stirred (600 r/min) sample. According to the results of the optimization experiments, the following conclusion can be drawn: The water-diluted sample in a 10 mL headspace-vial was efficiently extracted for 20 min after the system was equilibrated for 3 min at 60 degrees C. After extraction, the fiber was immediately inserted into the GC injector and desorbed at 250 degrees C for 3 min. The spiked recoveries were in the range of 82.0% - 103.3% and the relative standard deviations (RSDs) were between 1.8% and 9.4%. Meanwhile, the limits of detection (LODs) ranged from 0.6 ng/g to 2.1 ng/g. This method is characterized by rapidity, high sensitivity, good linearity and repeatability for all the target compounds. It is applicable to the analysis of synthetic musks in perfumes.

  13. The determination of polycyclic aromatic hydrocarbons in human urine by high-resolution gas chromatography-mass spectrometry.

    Science.gov (United States)

    Cho, Sung-Hee; Lee, Sun-Kyung; Kim, Chong Hyeak

    2017-12-12

    Polycyclic aromatic hydrocarbons (PAHs), organic compounds formed by at least two condensed aromatic rings, are ubiquitous environmental pollutants that are produced by incomplete combustion of organic materials. PAHs have been classified as carcinogenIC to humans by the International Agency for Research on Cancer, because they can bind to DNA, causing mutations. Therefore, the levels of PAHs in human urine can be used as an indicator for potential carcinogenesis and cell mutation. An analytical method was developed for the accurate measurement of PAHs in urine using high-resolution gas chromatography-mass spectrometry. Urine samples were extracted by an Oasis HLB extraction cartridge after enzymatic hydrolysis with a β-glucuronidase/arylsulfatase cocktail. The 18 PAHs were separated using an Agilent DB-5 MS capillary column (30 m × 0.25 mm, 0.25 μm) and monitored by time-of-flight mass spectrometry. Under the optimized method, the linearity of calibration curves was >0.994. The limits of detection at a signal-to-noise ratio of 3 were 10-100 ng/L. The coefficients of variation were in the range of 0.4-9.0%. The present method was highly accurate for simultaneous determination of 18 PAHs in human urine and could be applied to monitoring and biomedical investigations to check exposure of PAHs. Copyright © 2017 John Wiley & Sons, Ltd.

  14. Application of a Gas Chromatography/Mass Spectrometric Method for the Determination of Butyltin Compounds in Sediment

    International Nuclear Information System (INIS)

    Chung, Min Young; Kim, Byung Joo; Yim, Yong Heon; So, Hun Young; Won, Yong Il; Jung, Pyong Gil; Kim, Yong Seong

    2004-01-01

    A gas chromatography/mass spectrometric (GC/MS) method has been developed for the determination of trace mono-n-butyltin (MBT), di-n-butyltin (DBT), and tri-n-butyltin (TBT) compounds in sediments. Samples were extracted by 10% acetic acid in methanol containing 0.03% tropolone and were then derivatized for GC/MS analysis. Ethylation by sodium tetraethylborate and phenylation by sodium tetraphenylborate were evaluated as a derivatization reaction of the organotins in sample extract. n-Hexane was added into reaction media in the beginning of the reaction for the continuous extraction of derivatized organotins. Ethylation requires less than 2 hours to get proper derivatization yields for MBT, DBT, and TBT altogether and produces relatively low amounts of side reaction products. Compared to ethylation, phenylation requires much longer time but provides relatively lower yield and produces considerable amounts of side reaction products. Therefore, the ethylation reaction was applied for the analysis of organotin compounds in sediment. An isotope dilution mass spectrometric (IDMS) method based on GC/MS has been applied to the accurate determination of DBT compounds in the sediments. The IDMS results from the analyses of sediment samples showed a reasonable repeatability and a good agreement with the values obtained by IDMS based on liquid chromatography/induced coupled plasma/mass spectrometry

  15. Characterization of the volatile profiles of beer using headspace solid-phase microextraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Rossi, Serena; Sileoni, Valeria; Perretti, Giuseppe; Marconi, Ombretta

    2014-03-30

    The objective of this study was a multivariate characterization of the volatile profile of beers. Such a characterization is timely considering the increasing worldwide consumption of beer, the continuous growth of microbreweries and the importance of volatile compounds to beer flavour. A method employing solid-phase microextraction and gas chromatography-mass spectrometry (SPME-GC-MS) was optimized and then applied to a sample set of 36 industrial and craft beers of various styles and fermentation types. The volatile profiles of different beer styles is described, with particular attention paid to the volatile compounds characteristic of a spontaneously fermented lambic raspberry framboise beer. Furthermore, it was also possible to identify which specific volatile compounds are principally responsible for the differences in the volatile profiles of top- and bottom-fermented beers. Moreover, a volatile fingerprint of the craft top-fermented Italian beers was defined, as they show a very similar volatile profile. Finally, the volatile compounds that are characteristic of the bock-style beers are described. The SPME-GC-MS analytical method optimized in this study is suitable for characterizing the volatile fingerprint of different beers, especially on the basis of the kind of fermentation (top, bottom or spontaneous), the method of production and the style of the beer. © 2013 Society of Chemical Industry.

  16. Quantification of Stable Isotope Traces Close to Natural Enrichment in Human Plasma Metabolites Using Gas Chromatography-Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Lisa Krämer

    2018-02-01

    Full Text Available Currently, changes in metabolic fluxes following consumption of stable isotope-enriched foods are usually limited to the analysis of postprandial kinetics of glucose. Kinetic information on a larger diversity of metabolites is often lacking, mainly due to the marginal percentage of fully isotopically enriched plant material in the administered food product, and hence, an even weaker 13C enrichment in downstream plasma metabolites. Therefore, we developed an analytical workflow to determine weak 13C enrichments of diverse plasma metabolites with conventional gas chromatography-mass spectrometry (GC-MS. The limit of quantification was increased by optimizing (1 the metabolite extraction from plasma, (2 the GC-MS measurement, and (3 most importantly, the computational data processing. We applied our workflow to study the catabolic dynamics of 13C-enriched wheat bread in three human subjects. For that purpose, we collected time-resolved human plasma samples at 16 timepoints after the consumption of 13C-labeled bread and quantified 13C enrichment of 12 metabolites (glucose, lactate, alanine, glycine, serine, citrate, glutamate, glutamine, valine, isoleucine, tyrosine, and threonine. Based on isotopomer specific analysis, we were able to distinguish catabolic profiles of starch and protein hydrolysis. More generally, our study highlights that conventional GC-MS equipment is sufficient to detect isotope traces below 1% if an appropriate data processing is integrated.

  17. Determination of breath isoprene and acetone concentration with a needle-type extraction device in gas chromatography-mass spectrometry.

    Science.gov (United States)

    Ueta, Ikuo; Mizuguchi, Ayako; Okamoto, Mitsuyoshi; Sakamaki, Hiroyuki; Hosoe, Masahiko; Ishiguro, Motoyuki; Saito, Yoshihiro

    2014-03-20

    Isoprene in human breath is said to be related to cholesterol metabolism, and the possibility of the correlations with some clinical parameters has been studied. However, at this stage, no clear benefit of breath isoprene has been reported for clinical diagnosis. In this work, isoprene and acetone concentrations were measured in the breath of healthy and obese subjects using a needle-type extraction device for subsequent analysis in gas chromatography-mass spectrometry (GC-MS) to investigate the possibility of these compounds as an indicator of possible diseases. After measuring intraday and interday variations of isoprene and acetone concentrations in breath samples of healthy subjects, their concentrations were also determined in 80 healthy and 17 obese subjects. In addition, correlation between these breath concentrations and the blood tests result was studied for these healthy and obese subjects. The results indicated successful determination of breath isoprene and acetone in this work, however, no clear correlation was observed between these measured values and the blood test results. Breath isoprene concentration may not be a useful indicator for obesity or hypercholesterolemia. Copyright © 2014 Elsevier B.V. All rights reserved.

  18. Determination of carbon number distributions of complex phthalates by gas chromatography-mass spectrometry with ammonia chemical ionization.

    Science.gov (United States)

    Di Sanzo, Frank P; Lim, Peniel J; Han, Wenning W

    2015-01-01

    An assay method for phthalate esters with a complex mixture of isomer of varying carbon numbers, such as di-isononyl phthalate (DINP) and di-isodecyl phthalate (DIDP), using gas chromatography-mass spectrometry (GC-MS) positive chemical ionization (PCI) with 5% ammonia in methane is described. GC-MS-PCI-NH3, unlike GC-MS electron ionization (EI) (GC-MS-EI) that produces generally m/z 149 ion as the main base peak and low intensity M(+) peaks, produces higher intensity (M + 1) ions that allow the determination of total (R + R') carbon number distributions based on the various R and R' alkyl groups of the di-esters moiety. The technique allows distinguishing among the various commercial DINP and DIDP plasticizers. The carbon number distributions are determined in the acceptable range of 85 mole percent (m/m). Several examples of analysis made on commercial DINP and DIDP are presented. The use of only 5% instead of 100% ammonia simplifies use of GC-MS-PCI-NH3 but still produces sufficient M + 1 ion intensities that are appropriate for the assay. In addition, use of low concentrations of ammonia mitigates potential safety aspects related to use of ammonia and provides less corrosion for the instrument hardware. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  19. Liquid-phase microextraction combined with hollow fiber as a sample preparation technique prior to gas chromatography/mass spectrometry.

    Science.gov (United States)

    Zhao, Limian; Lee, Hian Kee

    2002-06-01

    Two modes of liquid-phase microextraction (LPME) combined with hollow fiber (HF) were developed for gas chromatography/mass spectrometry (GC/MS). Both methodologies, that is, static LPME with HF and dynamic LPME with HF, involved the use of a small volume of organic solvent impregnated in the hollow fiber, which was held by the needle of a conventional GC syringe. In static LPME/HF, the hollow fiber impregnated with solvent was immersed in the aqueous sample, and the extraction processed under stirring; in dynamic LPME/HF, the solvent was repeatedly withdrawn into and discharged from the hollow fiber by a syringe pump. This is believed to be the first reported instance of a semiautomated liquid microextraction procedure. The performance of the two techniques was demonstrated in the analysis of two PAH compounds in an aqueous sample. Static LPME/HF provided approximately 35-fold enrichment in 10 min and good reproducibility (approximately 4%). Dynamic LPME/HF could provide higher enrichment (approximately 75-fold) in 10 min and even better reproducibility (approximately 3%). Both methods allow the direct transfer of extracted analytes to a GC/MS system for analysis.

  20. [Development of a gas chromatography-mass spectrometry method for the metabolomic study of rice (Oryza sativa L.) grain].

    Science.gov (United States)

    Zhou, Jia; Wang, Shuangyuan; Chang, Yuwei; Zhao, Yanni; Lu, Xin; Zhao, Chunxia; Xu, Guowang

    2012-10-01

    An analytical strategy for the metabolic profiling of rice grain was developed based on gas chromatography-mass spectrometry (GC-MS). For the purpose of obtaining abundant metabolite information, sample preparation step prior to instrumental analysis is necessary to be optimized. D-optimal experimental design was applied to optimize the extraction solvent. Four solvents, including water, methanol, isopropanol and acetonitrile, and their combinations were evaluated for the extraction efficiency using multivariate statistical analysis (partial least square regression). The count of resolved peaks and the sum of peak areas were taken as the evaluation indexes. Methanol/water (80:20, v/v) mixture was highly efficient for rice metabolites and was selected as the suitable solvent formulation. Then, the analytical characteristics of the method were measured. More than 90% of the metabolites had satisfactory precisions, reproducibilities and stabilities (relative standard deviations (RSDs) < 30%). Most of the detected metabolites (about 88.0% of total peak area) showed good linear responses. With the optimized analytical protocol, 315 metabolites were detected in rice and 86 of which were structurally identified by searching in the NIST 08/Wiley standard mass spectral library, covering carbohydrates, amino acids, organic acids, steroids and so on which showed a broad coverage of metabolite data. The established method is expected to be useful for the metabolomic studies of rice.

  1. Application of gas chromatography-mass spectrometry in analyzing pharmacokinetics and distribution of deltamethrin in miniature pig tissues.

    Science.gov (United States)

    Zhu, Pan; Fan, Sai; Zou, Jian Hong; Miao, Hong; Li, Jing Guang; Zhang, Guo Wen; Wu, Yong Ning

    2014-06-01

    To characterize the pharmacokinetics and distribution profiles of deltamethrin in miniature pig tissues by gas chromatography-mass spectrometry (GC-MS). Pharmacokinetics and distribution of deltamethrin in blood and tissues of 30 miniature pigs were studied by GC-MS after oral administration of deltamethrin (5 mg/kg bw). Data were processed by 3P97 software. The serum deltamethrin level was significantly lower in tissues than in blood of miniature pigs. The AUC0-72 h, Cmax, of deltamethrin were 555.330 ± 316.987 ng h/mL and 17.861 ± 11.129 ng/mL, respectively. The Tmax, of deltamethrin was 6.004 ± 3.131 h. The metabolism of deltamethrin in miniature pigs is fit for a one-compartment model with a weighting function of 1/C2. Deltamethrin is rapidly hydrolyzed and accumulated in miniature pig tissues. Copyright © 2014 The Editorial Board of Biomedical and Environmental Sciences. Published by China CDC. All rights reserved.

  2. Rapid Determination of Clenbuterol in Pork by Direct Immersion Solid-Phase Microextraction Coupled with Gas Chromatography-Mass Spectrometry.

    Science.gov (United States)

    Ye, Diru; Wu, Susu; Xu, Jianqiao; Jiang, Ruifen; Zhu, Fang; Ouyang, Gangfeng

    2016-02-01

    Direct immersion solid-phase microextraction (DI-SPME) coupled with gas chromatography-mass spectrometry (GC-MS) was developed for rapid analysis of clenbuterol in pork for the first time. In this work, a low-cost homemade 44 µm polydimethylsiloxane (PDMS) SPME fiber was employed to extract clenbuterol in pork. After extraction, derivatization was performed by suspending the fiber in the headspace of the 2 mL sample vial saturated with a vapor of 100 µL hexamethyldisilazane. Lastly, the fiber was directly introduced to GC-MS for analysis. All parameters that influenced absorption (extraction time), derivatization (derivatization reagent, time and temperature) and desorption (desorption time) were optimized. Under optimized conditions, the method offered a wide linear range (10-1000 ng g(-1)) and a low detection limit (3.6 ng g(-1)). Finally, the method was successfully applied in the analysis of pork from the market, and recoveries of the method for spiked pork were 97.4-105.7%. Compared with the traditional solvent extraction method, the proposed method was much cheaper and fast. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  3. Quantification of Stable Isotope Traces Close to Natural Enrichment in Human Plasma Metabolites Using Gas Chromatography-Mass Spectrometry.

    Science.gov (United States)

    Krämer, Lisa; Jäger, Christian; Trezzi, Jean-Pierre; Jacobs, Doris M; Hiller, Karsten

    2018-02-14

    Currently, changes in metabolic fluxes following consumption of stable isotope-enriched foods are usually limited to the analysis of postprandial kinetics of glucose. Kinetic information on a larger diversity of metabolites is often lacking, mainly due to the marginal percentage of fully isotopically enriched plant material in the administered food product, and hence, an even weaker 13 C enrichment in downstream plasma metabolites. Therefore, we developed an analytical workflow to determine weak 13 C enrichments of diverse plasma metabolites with conventional gas chromatography-mass spectrometry (GC-MS). The limit of quantification was increased by optimizing (1) the metabolite extraction from plasma, (2) the GC-MS measurement, and (3) most importantly, the computational data processing. We applied our workflow to study the catabolic dynamics of 13 C-enriched wheat bread in three human subjects. For that purpose, we collected time-resolved human plasma samples at 16 timepoints after the consumption of 13 C-labeled bread and quantified 13 C enrichment of 12 metabolites (glucose, lactate, alanine, glycine, serine, citrate, glutamate, glutamine, valine, isoleucine, tyrosine, and threonine). Based on isotopomer specific analysis, we were able to distinguish catabolic profiles of starch and protein hydrolysis. More generally, our study highlights that conventional GC-MS equipment is sufficient to detect isotope traces below 1% if an appropriate data processing is integrated.

  4. Determination of Panthenol, Cholecalciferol and Tocopherol in Cosmetic Products by Gas Chromatography-Mass Spectrometry in SIM Mode.

    Science.gov (United States)

    Jeong, H J; Lee, M H; Ro, K W; Hur, C W; Kim, J W

    1999-02-01

    A novel simple method to detect vitamins in cosmetic products by gas chromatography-mass spectrometry (GC-MS) has been developed. Three vitamins (panthenol, cholecalciferol and tocopherol) were used for this study. Vitamins were prepared by dissolving in tetrahydrofuran (ThF), and silylated with bis-trimethylsilyltri-fluoroacetamide- trichloromethylsilane (BSTFA). Silylated vitamins were separated on a fused-silica capillary column coated with DB-5. The identification of each vitamin was accomplished by retention time and mass spectrum library search with a computer, and the quantitation was made in the selected-ion monitoring (SIM) mode of GC-MS. SIM mode had given sensitivity to determine 50 pg of panthenol, 285 pg of cholecalciferol and 130 pg of tocopherol. Linearity was maintained over the range 0.005-0.20% for each vitamin. Each cosmetic product (i.e. hair tonic and lotion) was found to contain amounts of the vitamins. This method was sensitive and gave 77.5-99.9% recovery of each vitamin from these cosmetic products. From these results, we concluded that silylation with BSTFA followed by GC-MS analysis allows the simple, convenient and exact determination of panthenol, cholecalciferol and tocopherol.

  5. DETERMINATION AND CLASSIFICATION OF VOLATILE COMPOUNDS OF PASTIRMA USING SOLID PHASE MICROEXTRACTION/GAS CHROMATOGRAPHY/MASS SPECTROMETRY

    Directory of Open Access Journals (Sweden)

    Eda Demirok

    2013-10-01

    Full Text Available Pastırma, a traditional dry cured Turkish meat product, has a great number of specific aroma compounds, which occur as a result of lipid oxidation, protein degradation and formulation of çemen paste. These compounds give characteristic flavor to pastırma and the main objective of this study was to determine the nature of these compounds. Fifty-eight volatile compounds, grouped into nine chemical classes were identified using solid phase microextraction technique (SPME coupled to gas chromatography/mass spectrometry (GC-MS. Aldehydes, mostly lipid oxidation products, were determined as the major chemical group, representing 17.54-78.02% of total volatile compounds. The major volatile aldehyde was hexanal (2.36-55.41%, followed by 2-methyl-2-butenal (0.97-14.69% and then heptanal (0.29-4.77%. Sulfur compounds possibly derived from spices or formed by proteolysis of sulfur-containing amino acids, were the second most abundant group, with concentrations ranging between 6.04 and 50.60%. Other important volatile compounds of pastırma were aliphatic hydrocarbons, aromatic ketones, hydrocarbons, esters, alcohols, acids, terpenes, and furans.

  6. Determining the Levels of Volatile Organic Pollutants in Urban Air Using a Gas Chromatography-Mass Spectrometry Method

    Directory of Open Access Journals (Sweden)

    Simona Nicoara

    2009-01-01

    Full Text Available The paper presents the application of a method based on coupled gas chromatography-mass spectrometry, using an isotopically labelled internal standard for the quantitative analysis of benzene (B, toluene (T, ethyl benzene (E, and o-, m-, p-xylenes (X. Their atmospheric concentrations were determined based on short-term sampling, in different sites of Cluj-Napoca, a highly populated urban centre in N-W Romania, with numerous and diversified road vehicles with internal combustion engines. The method is relatively inexpensive and simple and shows good precision and linearity in the ranges of 7–60 μg/m3 (B, 13–90 μg/m3 (T, 7–50 μg/m3 (E, 10–70 μg/m3 (X-m,p, and 20–130 μg/m3 (X-o. The limits of quantitation/detection of the method LOQ/LOD are of 10/5 μg/m3 (Xo, 5/3 μg/m3 (B, E, X-m,p, and of 3/1 μg/m3 (T, respectively.

  7. Comparison of gas chromatography/mass spectrometry and immunoassay techniques on concentrations of atrazine in storm runoff

    Science.gov (United States)

    Lydy, Michael J.; Carter, D.S.; Crawford, Charles G.

    1996-01-01

    Gas chromatography/mass spectrometry (GC/MS) and enzyme-linked immunosorbent assay (ELISA) techniques were used to measure concentrations of dissolved atrazine in 149 surface-water samples. Samples were collected during May 1992–September 1993 near the mouth of the White River (Indiana) and in two small tributaries of the river. GC/MS was performed on a Hewlett-Packard 5971 A, with electron impact ionization and selected ion monitoring of filtered water samples extracted by C-18 solid phase extraction; ELISA was performed with a magnetic-particle-based assay with photometric analysis. ELISA results compared reasonably well to GC/MS measurements at concentrations below the Maximum Contaminant Level for drinking water set by the U.S. Environmental Protection Agency (3.0 μg/L), but a systematic negative bias was observed at higher concentrations. When higher concentration samples were diluted into the linear range of calibration, the relation improved. A slight positive bias was seen in all of the ELISA data compared to the GC/MS results, and the bias could be partially explained by correcting the ELISA data for cross reactivity with other triazine herbicides. The highest concentrations of atrazine were found during the first major runoff event after the atrazine was applied. Concentrations decreased throughout the rest of the sampling period even though large runoff events occurred during this time, indicating that most atrazine loading to surface waters in the study area occurs within a few weeks after application.

  8. Improvements on enzymatic hydrolysis of human hair for illicit drug determination by gas chromatography/mass spectrometry.

    Science.gov (United States)

    Míguez-Framil, Martha; Moreda-Piñeiro, Antonio; Bermejo-Barrera, Pilar; López, Patricia; Tabernero, María Jesús; Bermejo, Ana María

    2007-11-15

    The use of ultrasound energy for accelerating the pronase E enzymatic hydrolysis of human hair for extracting illicit drugs has been novelty tested. The enzymatic extracts obtained after 30 min of sonication in an ultrasonic water bath were subjected to an optimized solid-phase extraction process, which involved a solution of 2.0% (v/v) acetic acid in methanol as eluting solution and concentration by N2 stream evaporation. A gas chromatography/mass spectrometry method was used to separate and determine cocaine, benzoylecgonine, codeine, morphine, and 6-monoacethylmorphine in 20 min. Variables affecting ultrasound-assisted pronase E hydrolysis such as hydrolysis temperature, hydrolysis time, enzyme concentration, catalyzer (1,4-dithiothreitol) concentration, ionic strength, pH, and ultrasound frequency were simultaneously evaluated by a Plackett-Burman design 2(8) PBD of resolution III. The most statistically significant variables were ionic strength and pH, which means that analyte extraction is mainly attributed to pronase E activity. The optimization or evaluation of all the factors has led to an accelerated pronase E hydrolysis of human hair, which can be completed in 30 min. Results have been found to be statistically similar to those obtained with conventional pronase E hydrolysis. The accelerated method was finally applied to several human hair samples from multidrug abusers.

  9. Quantitative determination of methamphetamine in oral fluid by liquid-liquid extraction and gas chromatography/mass spectrometry.

    Science.gov (United States)

    Bahmanabadi, L; Akhgari, M; Jokar, F; Sadeghi, H B

    2017-02-01

    Methamphetamine abuse is one of the most medical and social problems many countries face. In spite of the ban on the use of methamphetamine, it is widely available in Iran's drug black market. There are many analytical methods for the detection of methamphetamine in biological specimen. Oral fluid has become a popular specimen to test for the presence of methamphetamine. The purpose of the present study was to develop a method for the extraction and detection of methamphetamine in oral fluid samples using liquid-liquid extraction (LLE) and gas chromatography/mass spectrometry (GC/MS) methods. An analytical study was designed in that blank and 50 authentic oral fluid samples were collected to be first extracted by LLE and subsequently analysed by GC/MS. The method was fully validated and showed an excellent intra- and inter-assay precision (reflex sympathetic dystrophy ˂ 10%) for external quality control samples. Recovery with LLE methods was 96%. Limit of detection and limit of quantitation were 5 and 15 ng/mL, respectively. The method showed high selectivity, no additional peak due to interfering substances in samples was observed. The introduced method was sensitive, accurate and precise enough for the extraction of methamphetamine from oral fluid samples in forensic toxicology laboratories.

  10. Determination of polycyclic aromatic hydrocarbons in soil by miniaturized ultrasonic extraction and gas chromatography-mass selective detection

    Energy Technology Data Exchange (ETDEWEB)

    Ozcan, Senar; Tor, Ali; Aydin, Mehmet Emin [Selcuk University, Department of Environmental Engineering, Konya (Turkey)

    2009-10-15

    A miniaturized ultrasonic extraction procedure was developed for the determination of polycyclic aromatic hydrocarbons (PAHs) in soil by gas chromatography-mass spectrometry. After determination of the most suitable extraction solvent with 5 min sonication time, several other parameters (sample amount, solvent volume and number of extraction times) were optimized using a 2{sup 3}factorial experimental design. Recoveries of PAHs from spiked soil samples were over 90% for three different fortification levels between 50 and 300 {mu}g/kg, and relative standard deviations of the recoveries were in the range of < 1-15%. The limits of detection ranged from 0.002 to 1.87 {mu}g/kg. The performance of the developed procedure was also compared with other traditional Soxhlet, shake flask and large scale ultrasonic extraction procedures on real soil samples, and extraction methods showed comparable efficiencies. The proposed procedure required small volumes of solvent and sample. It was practicable, rapid and easy to use for analysis of PAHs in soils. (Abstract Copyright [2009], Wiley Periodicals, Inc.)

  11. Phytochemical Profile of Erythrina variegata by Using High-Performance Liquid Chromatography and Gas Chromatography-Mass Spectroscopy Analyses

    Directory of Open Access Journals (Sweden)

    Suriyavathana Muthukrishnan

    2016-08-01

    Full Text Available Natural products derived from plant sources have been utilized to treat patients with numerous diseases. The phytochemical constituents present in ethanolic leaf extract of Erythrina variegata (ELEV were identified by using high-performance liquid chromatography (HPLC and gas chromatography-mass spectroscopy (GC-MS analyses. Shade dried leaves were powdered and extracted with ethanol for analyses through HPLC to identify selected flavonoids and through GC-MS to identify other molecules. The HPLC analysis of ELEV showed the presence of gallic and caffeic acids as the major components at concentrations of 2.0 ppm and 0.1 ppm, respectively, as well as other components. GC-MS analysis revealed the presence of 3-eicosyne; 3,7,11,15-tetramethyl-2-hexadecen-1-ol; butanoic acid, 3-methyl-3,7-dimethyl-6-octenyl ester; phytol; 1,2-benzenedicarboxylic acid, diundecyl ester; 1-octanol, 2-butyl-; squalene; and 2H-pyran, 2-(7-heptadecynyloxy tetrahydro-derivative. Because pharmacopuncture is a new evolving natural mode that uses herbal extracts for treating patients with various ailments with minimum pain and maximum effect, the results of this study are particularly important and show that ELEV possesses a wide range of phytochemical constituents, as indicated above, as effective active principle molecules that can be used individually or in combination to treat patients with various diseases.

  12. Trace determination of the flame retardant tetrabromobisphenol A in the atmosphere by gas chromatography-mass spectrometry

    International Nuclear Information System (INIS)

    Xie Zhiyong; Ebinghaus, Ralf; Lohmann, Rainer; Heemken, Olaf; Caba, Armando; Puettmann, Wilhelm

    2007-01-01

    A simple and effective method has been developed for analysis of the flame retardant tetrabromobisphenol A (TBBPA) in environmental samples by using modified soxhlet extraction in combination with silica gel clean-up, derivatization with silylation reagent and gas chromatography-mass spectrometry (GC-MS) in selected ion monitoring mode (SIM). Satisfactory recoveries were achieved for the large volume sampling, soxhlet extraction and silica gel clean-up. The overall recovery is 79 ± 1%. The derivatization procedure is simple and fast, and produces stable TBBPA derivative. GC-MS with electronic impact (EI) ionization mode shows better detection power than using negative chemical ionization (NCI) mode. EI gives a method detection limit of 0.04 pg m -3 and enables to determine trace TBBPA in ambient air in remote area. The method was successfully applied to the determination of TBBPA in atmospheric samples collected over land and coastal regions. The concentrations of TBBPA ranged from below the method detection limit (0.04 pg m -3 ) to 0.85 pg m -3 . A declining trend with increasing latitude was present from the Wadden Sea to the Arctic. The atmospheric occurrence of TBBPA in the Arctic is significant and might imply that TBBPA has long-range transport potential

  13. Measurement of rimantadine in plasma by capillary gas chromatography/mass spectrometry with a deuterium-labeled internal standard

    International Nuclear Information System (INIS)

    Herold, D.A.; Anonick, P.K.; Kinter, M.; Hayden, F.G.

    1988-01-01

    Rimantadine is a synthetic antiviral agent used in prophylaxis and in treating the early stages of uncomplicated influenza A illness. We describe a stable isotope-dilution assay involving capillary gas chromatography/mass spectrometry. We used 200 ng of d3-rimantadine, added to 1 mL of plasma, as the internal standard. The rimantadine was extracted from the plasma with a Bond-Elut CN column, the column was washed with water, and the rimantadine was eluted with methanol, dried, and treated to form the t-butyldimethylsilyl derivative. The mass spectrometer was operated in the selected ion monitoring mode. Ions at m/z 236 and m/z 239 were monitored, corresponding to the loss of C4H9 from the rimantadine derivative and d3-rimantadine, respectively. Within-run precision (CVs) ranged from 8.9% at 29 micrograms/L to 3.2% at 1666 micrograms/L. Corresponding data for between-run precision were 5.4% and 1.7%. Treated volunteers (n = 86) provided plasma samples with a concentration range of 153 to 1127 micrograms/L. This simplified method allows rapid, precise assay of rimantadine in plasma

  14. Gas chromatography-mass spectrometry and Raman imaging measurement of squalene content and distribution in human hair.

    Science.gov (United States)

    Wu, Yan; Chen, Guoqiang; Ji, Chengdong; Hoptroff, Michael; Jones, Andrew; Collins, Luisa Z; Janssen, Hans-Gerd

    2016-03-01

    A sensitive and specific gas chromatography-mass spectrometry (GC-MS) method was developed and validated for the measurement of the squalene content from root to tip, in both Chinese black virgin and bleached hair. Deuterated squalene was used as the internal standard. For quantification, selective ion monitoring (SIM) at m/z 410.0 and 347.0 were monitored for squalene and deuterated squalene, respectively. Different methods for the extraction of squalene from ex vivo human hair were compared including organic solvent extraction and acid/alkali hydrolysis. The best extraction efficiency was obtained by using a mixed solvent consisting of chloroform:methanol = 2:1 (v:v). The linear range of squalene ran from 1.0 to 50.0 μg mL(-1). The limit of detection (LOD) was 0.10 μg mL(-1) (corresponding to 0.005 mg g(-1) in human hair), which enabled quantification of squalene in human hair at very low level. The recovery of squalene was 96.4 ± 1.46% (n = 3). Using the above-mentioned mixed solvent extraction, squalene content in human hair was successfully quantified from root to tip. Meanwhile, a Raman imaging method was developed to visualize the squalene distribution in Chinese white virgin hair from cuticle to medulla.

  15. Urinary Metabolomic Study of Chlorogenic Acid in a Rat Model of Chronic Sleep Deprivation Using Gas Chromatography-Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Wei-ni Ma

    2018-01-01

    Full Text Available The urinary metabolomic study based on gas chromatography-mass spectrometry (GC-MS had been developed to investigate the possible antidepressant mechanism of chlorogenic acid (CGA in a rat model of sleep deprivation (SD. According to pattern recognition analysis, there was a clear separation among big platform group (BP, sleep deprivation group (SD, and the CGA (model + CGA, and CGA group was much closer to the BP group by showing a tendency of recovering towards BP group. Thirty-six significantly changed metabolites related to antidepressant by CGA were identified and used to explore the potential mechanism. Combined with the result of the classic behavioral tests and biochemical indices, CGA has significant antidepressant effects in a rat model of SD, suggesting that the mechanism of action of CGA might be involved in regulating the abnormal pathway of nicotinate and nicotinamide metabolism; glyoxylate and dicarboxylate metabolism; glycine, serine, and threonine metabolism; and arginine and proline metabolism. Our results also show that metabolomics analysis based on GC-MS is a useful tool for exploring biomarkers involved in depression and elucidating the potential therapeutic mechanisms of Chinese medicine.

  16. Determination of amphetamine-type stimulants in oral fluid by solid-phase microextraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Souza, Daniele Z; Boehl, Paula O; Comiran, Eloisa; Mariotti, Kristiane C; Pechansky, Flavio; Duarte, Paulina C A V; De Boni, Raquel; Froehlich, Pedro E; Limberger, Renata P

    2011-06-24

    A method for the simultaneous identification and quantification of amphetamine (AMP), methamphetamine (MET), fenproporex (FEN), diethylpropion (DIE) and methylphenidate (MPH) in oral fluid collected with Quantisal™ device has been developed and validated. Thereunto, in-matrix propylchloroformate derivatization followed by direct immersion solid-phase microextraction and gas chromatography-mass spectrometry were employed. Deuterium labeled AMP was used as internal standard for all the stimulants and analysis was performed using the selected ion monitoring mode. The detector response was linear for the studied drugs in the concentration range of 2-256 ng mL(-1) (neat oral fluid), except for FEN, whereas the linear range was 4-256 ng mL(-1). The detection limits were 0.5 ng mL(-1) (MET), 1 ng mL(-1) (MPH) and 2 ng mL(-1) (DIE, AMP, FEN), respectively. Accuracy of quality control samples remained within 98.2-111.9% of the target concentrations, while precision has not exceeded 15% of the relative standard deviation. Recoveries with Quantisal™ device ranged from 77.2% to 112.1%. Also, the goodness-of-fit concerning the ordinary least squares model in the statistical inference of data has been tested through residual plotting and ANOVA. The validated method can be easily automated and then used for screening and confirmation of amphetamine-type stimulants in drivers' oral fluid. Copyright © 2011 Elsevier B.V. All rights reserved.

  17. Determination of alkylphenolic residues in fresh fruits and vegetables by extractive steam distillation and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Yang, Deng-Kai; Ding, Wang-Hsien

    2005-09-23

    This study describes a simple and sensitive method for determining the alkylphenolic compounds, 4-tert-octylphenol (4-t-OP), 4-nonylphenol isomers (4-NPs), and their monoethoxylates (4-t-OP1EO and 4-NP1EOs), in fresh fruits and vegetables. The method involves extracting a sample by a modified Nielson-Kryger steam distillation extraction using n-hexane for 1 h. The alkylphenolic compounds were identified and quantitated by gas chromatography-mass spectrometry (GC-MS) in selected ion monitoring (SIM) mode. Various pH values and amounts of NaCl added to the sample solution were evaluated as extraction conditions. The quantitation limit of this method was less than 0.2 ng/g in 10 g (fresh weight) of sample. Recovery of alkylphenolic compounds in spiked samples exceeded 64% while R.S.D. ranged from 1.0 to 9.8%. Alkylphenolic residues were detected in fresh fruits and vegetables at concentrations of 4-NPs and 4-t-OP from n.d. to 16 ng/g and from n.d. to 4.8 ng/g (fresh weight), respectively. NP1EO and OP1EO were always below the quantitation limit.

  18. Determination of alkylphenol residues in baby-food purees by steam distillation extraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Li, Chia-Tien; Cheng, Chin-Yuan; Ding, Wang-Hsien

    2008-02-01

    This paper describes a simple and sensitive method for determining alkylphenols namely 4-tert-octylphenol (4-t-OP) and the isomers of 4-nonylphenol (4-NPs) present in various types of baby-food purees. The method involves extracting a sample with n-hexane for 1h using a modified Nielson-Kryger steam distillation extraction system and then identifying and quantitating the alkylphenols using a gas chromatography-mass spectrometry (GC-MS) operated in the selected ion monitoring (SIM) mode. The extraction conditions were evaluated at various values of pH of the sample solution. The limits of quantitation for this method were 0.2 ng/g from 1.0 g (wet weight) samples of 4-t-OP and the 4-NPs. The intra- and interbatch precisions and accuracies were also determined. The precision, in terms of the relative standard deviation (RSD), were less than 8%. Most of the recoveries of the alkylphenols from various spiked samples exceeded 60%, while the values of RSD ranged from 1% to 10%. Alkylphenol residues were detected in baby-food purees at concentrations of up to 19 ng/g (wet weight) for 4-t-OP and up to 21 ng/g (wet weight) for the 4-NPs.

  19. Development and Applications of Portable Gas Chromatography-Mass Spectrometry for Emergency Responders, the Military, and Law-Enforcement Organizations.

    Science.gov (United States)

    Leary, Pauline E; Dobson, Gareth S; Reffner, John A

    2016-05-01

    Portable gas chromatography-mass spectrometry (GC-MS) systems are being deployed for field use, and are designed with this goal in mind. Performance characteristics of instruments that are successful in the field are different from those of equivalent technologies that are successful in a laboratory setting. These field-portable systems are extending the capabilities of the field user, providing investigative leads and confirmatory identifications in real time. Many different types of users benefit from the availability of this technology including emergency responders, the military, and law-enforcement organizations. This manuscript describes performance characteristics that are important for field-portable instruments, especially field-portable GC-MS systems, and demonstrates the value of this equipment to the disciplines of explosives investigations, fire investigations, and counterfeit-drug detection. This paper describes the current state of portable GC-MS technology, including a review of the development of portable GC-MS, as well as a demonstration of the value of this capability using different examples. © The Author(s) 2016.

  20. Headspace Hanging Drop Liquid Phase Microextraction and Gas Chromatography-Mass Spectrometry for the Analysis of Flavors from Clove Buds

    Energy Technology Data Exchange (ETDEWEB)

    Jung, Mi Jin; Shin, Yeon Jae; Oh, Se Yeon; Kim, Nam Sun; Kim, Kun; Lee, Dong Sun [Seoul Women' s University, Seoul (Korea, Republic of)

    2006-02-15

    A novel sample pretreatment technique, headspace hanging drop liquid phase microextraction (HS-LPME) was studied and applied to the determination of flavors from solid clove buds by gas chromatography-mass spectrometry (GC-MS). Several parameters affecting on HS-LPME such as organic solvent drop volume, extraction time, extraction temperature and phase ratio were investigated. 1-Octanol was selected as the extracting solvent, drop size was fixed to 0.6 μL. 60 min extraction time at 25 .deg. C was chosen. HS-LPME has the good efficiency demonstrated by the higher partition equilibrium constant (K{sub lh}) values and concentration factor (CF) values. The limits of detection (LOD) were 1.5-3.2 ng. The amounts of eugenol, β-caryophyllene and eugenol acetate from the clove bud sample were 1.90 mg/g, 1.47 mg/g and 7.0 mg/g, respectively. This hanging drop based method is a simple, fast and easy sample enrichment technique using minimal solvent. HSLPME is an alternative sample preparation method for the analysis of volatile aroma compounds by GC-MS.

  1. Validation of biomarkers for distinguishing Mycobacterium tuberculosis from non-tuberculous mycobacteria using gas chromatography-mass spectrometry and chemometrics.

    Directory of Open Access Journals (Sweden)

    Ngoc A Dang

    Full Text Available Tuberculosis (TB remains a major international health problem. Rapid differentiation of Mycobacterium tuberculosis complex (MTB from non-tuberculous mycobacteria (NTM is critical for decisions regarding patient management and choice of therapeutic regimen. Recently we developed a 20-compound model to distinguish between MTB and NTM. It is based on thermally assisted hydrolysis and methylation gas chromatography-mass spectrometry and partial least square discriminant analysis. Here we report the validation of this model with two independent sample sets, one consisting of 39 MTB and 17 NTM isolates from the Netherlands, the other comprising 103 isolates (91 MTB and 12 NTM from Stellenbosch, Cape Town, South Africa. All the MTB strains in the 56 Dutch samples were correctly identified and the model had a sensitivity of 100% and a specificity of 94%. For the South African samples the model had a sensitivity of 88% and specificity of 100%. Based on our model, we have developed a new decision-tree that allows the differentiation of MTB from NTM with 100% accuracy. Encouraged by these findings we will proceed with the development of a simple, rapid, affordable, high-throughput test to identify MTB directly in sputum.

  2. Development of a gas chromatography-mass spectrometry technique to diagnose white snakeroot (Ageratina altissima) poisoning in a cow.

    Science.gov (United States)

    Meyerholtz, Kimberly A; Burcham, Grant N; Miller, Margaret A; Wilson, Christina R; Hooser, Stephen B; Lee, Stephen T

    2011-07-01

    An 8-year-old, crossbred beef cow was referred to the Indiana Animal Disease Diagnostic Laboratory at Purdue University for a complete necropsy in October 2009. The cow was the sixth to die in a 7-day period. Affected cows were reportedly stumbling and became weak, excitable, and recumbent. Histologically, myonecrosis was severe in the skeletal muscles and mild in the heart and tongue. According to the submitter, exposure to a poisonous plant was suspected, and a plant specimen received from this case was identified as white snakeroot (Ageratina altissima). Using the white snakeroot specimen, a gas chromatography-mass spectrometry analytical method for the detection of tremetone and dehydrotremetone (2 components of white snakeroot) was developed. Both tremetone and dehydrotremetone were detected in the plant specimen. Dehydrotremetone was recovered from the liver, while neither component was recovered in the rumen content. In the past, because of the lack of standard reference material, the diagnosis of white snakeroot poisoning was based mainly on history of exposure and the presence of the plant in the rumen. The analytical method described herein can be used to document exposure to tremetone or dehydrotremetone in cases of suspected white snakeroot poisoning when coupled with the appropriate clinical signs and lesions.

  3. Recent trends in application of multivariate curve resolution approaches for improving gas chromatography-mass spectrometry analysis of essential oils.

    Science.gov (United States)

    Jalali-Heravi, Mehdi; Parastar, Hadi

    2011-08-15

    Essential oils (EOs) are valuable natural products that are popular nowadays in the world due to their effects on the health conditions of human beings and their role in preventing and curing diseases. In addition, EOs have a broad range of applications in foods, perfumes, cosmetics and human nutrition. Among different techniques for analysis of EOs, gas chromatography-mass spectrometry (GC-MS) is the most important one in recent years. However, there are some fundamental problems in GC-MS analysis including baseline drift, spectral background, noise, low S/N (signal to noise) ratio, changes in the peak shapes and co-elution. Multivariate curve resolution (MCR) approaches cope with ongoing challenges and are able to handle these problems. This review focuses on the application of MCR techniques for improving GC-MS analysis of EOs published between January 2000 and December 2010. In the first part, the importance of EOs in human life and their relevance in analytical chemistry is discussed. In the second part, an insight into some basics needed to understand prospects and limitations of the MCR techniques are given. In the third part, the significance of the combination of the MCR approaches with GC-MS analysis of EOs is highlighted. Furthermore, the commonly used algorithms for preprocessing, chemical rank determination, local rank analysis and multivariate resolution in the field of EOs analysis are reviewed. Copyright © 2011 Elsevier B.V. All rights reserved.

  4. Metabolomic investigation of porcine muscle and fatty tissue after Clenbuterol treatment using gas chromatography/mass spectrometry.

    Science.gov (United States)

    Li, Guanglei; Fu, Yuhua; Han, Xiaosong; Li, Xinyun; Li, Changchun

    2016-07-22

    Clenbuterol is a β-adrenergic agonist used as additive to increase the muscle mass of meat-producing animals. Previous studies were limited to evaluations of animal growth performance and determination of the residues. Several studies have focused on urine samples. Little information about the underlying molecular mechanisms that can explain Clenbuterol metabolism and promote energy repartition in animal muscle and fatty tissue is available. Therefore, this research aims to detect the metabolite variations in muscle and fatty tissue acquired from Chinese pigs fed with Clenbuterol using gas chromatography/mass spectrometry (GC/MS). Ten two-month old Enshi black pigs were fed under the same condition; five of which were fed with basic ration containing Clenbuterol for one month, whereas the other five pigs were fed only with basic ration. Muscle and fatty tissue were subjected to metabolomics analysis using GC/MS. Differences in metabolomic profiles between the two groups were characterized by multivariate statistical analysis. The muscle samples showed that 15 metabolites were significantly different in the Clenbuterol-treated group compared with the control group; 13 potential biomarkers were found in the fatty tissue. Most of the metabolites were associated with fatty acid metabolism and amino acid metabolism. Glycerol, phenylalanine, and leucine were the common metabolites between the muscle and fatty tissue. These metabolites may provide a new clue that contributes to the understanding of the energy reassignment induced by Clenbuterol. Copyright © 2016 Elsevier B.V. All rights reserved.

  5. Gas Chromatography-Mass Spectrometry Analysis of Ulva fasciata (Green Seaweed Extract and Evaluation of Its Cytoprotective and Antigenotoxic Effects

    Directory of Open Access Journals (Sweden)

    Idania Rodeiro

    2015-01-01

    Full Text Available The chemical composition and biological properties of Ulva fasciata aqueous-ethanolic extract were examined. Five components were identified in one fraction prepared from the extract by gas chromatography-mass spectrometry, and palmitic acid and its ethyl ester accounted for 76% of the total identified components. Furthermore, we assessed the extract’s antioxidant properties by using the DPPH, ABTS, and lipid peroxidation assays and found that the extract had a moderate scavenging effect. In an experiment involving preexposition and coexposition of the extract (1–500 µg/mL and benzo[a]pyrene (BP, the extract was found to be nontoxic to C9 cells in culture and to inhibit the cytotoxicity induced by BP. As BP is biotransformed by CYP1A and CYP2B subfamilies, we explored the possible interaction of the extract with these enzymes. The extract (25–50 µg/mL inhibited CYP1A1 activity in rat liver microsomes. Analysis of the inhibition kinetics revealed a mixed-type inhibitory effect on CYP1A1 supersome. The effects of the extract on BP-induced DNA damage and hepatic CYP activity in mice were also investigated. Micronuclei induction by BP and liver CYP1A1/2 activities significantly decreased in animals treated with the extract. The results suggest that Ulva fasciata aqueous-ethanolic extract inhibits BP bioactivation and it may be a potential chemopreventive agent.

  6. Headspace-trap gas chromatography-mass spectrometry for determination of sulphur mustard and related compounds in soil.

    Science.gov (United States)

    Røen, Bent T; Unneberg, Erik; Tørnes, John Aa; Lundanes, Elsa

    2010-04-02

    Methods for trace determination of sulphur mustard (HD) and some related cyclic sulphur compounds in soil samples have been developed using headspace-trap in combination with gas chromatography-mass spectrometry (GC-MS). Two quite different types of soil were employed in the method optimisation (sandy loam and silty clay loam). Prior to analysis, water saturated with sodium chloride was added to the samples, at a water to soil ratio of 1:1. A detection limit of 3 ng/g was achieved for HD, while the cyclic sulphur compounds 1,4-thioxane, 1,3-dithiolane and 1,4-dithiane could be detected at 0.2-0.7 ng/g. The methods were validated in the concentration range from the limit of quantification (LOQ) to hundred times LOQ. The within assay precision at fifty times LOQ was 6.9-7.3% relative standard deviation (RSD) for determination of the cyclic sulphur compounds, and 15% RSD for determination of HD. Recoveries were in the range of 43-60% from the two soil types. As the technique requires very little sample preparation, the total time for sample handling and analysis was less than 1h. The technique was successfully employed for the determination of cyclic sulphur compounds in a sediment sample from an old dumping site for chemical munitions, known to contain HD degradation products. Copyright (c) 2010 Elsevier B.V. All rights reserved.

  7. Method development for fingerprinting of biodiesel blends by solid-phase extraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Yang, Zeyu; Hollebone, Bruce P; Wang, Zhendi; Yang, Chun; Landriault, Mike

    2011-11-01

    A method based on the combination of solid-phase extraction (SPE) with gas chromatography-mass spectrometry (GC/MS) for detailed chemical fingerprinting of biodiesel/petrodiesel blends was developed in the present study. Forensic identification, commonly referred to as chemical fingerprinting, is based on the relative distributions of individual aliphatic hydrocarbons, aromatic hydrocarbons, fatty acid alkyl esters, and free sterols. Fractionation of fuel samples is optimized for the separation of fatty acid esters and free sterols from petroleum hydrocarbons into four fractions: aliphatic, aromatic, fatty acid ester, and polar components. The final recoveries of aliphatic and aromatic hydrocarbons were determined to be in the range of 65-103%, 73-105% for FAMEs, and 78-103% for free sterols in the polar fraction. Excellent separation with negligible crossover of components with different polarities between fractions was observed. Quantitative analysis of blend levels and individual chemical distribution were achieved. The method has great potential for the identification of biodiesel in diesel fuel blends and could form the basis of a method for characterization of biodiesel-contaminated environmental samples. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Gas Chromatography-Mass Spectrometry Analysis of Ulva fasciata (Green Seaweed) Extract and Evaluation of Its Cytoprotective and Antigenotoxic Effects.

    Science.gov (United States)

    Rodeiro, Idania; Olguín, Sitlali; Santes, Rebeca; Herrera, José A; Pérez, Carlos L; Mangas, Raisa; Hernández, Yasnay; Fernández, Gisselle; Hernández, Ivones; Hernández-Ojeda, Sandra; Camacho-Carranza, Rafael; Valencia-Olvera, Ana; Espinosa-Aguirre, Jesús Javier

    2015-01-01

    The chemical composition and biological properties of Ulva fasciata aqueous-ethanolic extract were examined. Five components were identified in one fraction prepared from the extract by gas chromatography-mass spectrometry, and palmitic acid and its ethyl ester accounted for 76% of the total identified components. Furthermore, we assessed the extract's antioxidant properties by using the DPPH, ABTS, and lipid peroxidation assays and found that the extract had a moderate scavenging effect. In an experiment involving preexposition and coexposition of the extract (1-500 µg/mL) and benzo[a]pyrene (BP), the extract was found to be nontoxic to C9 cells in culture and to inhibit the cytotoxicity induced by BP. As BP is biotransformed by CYP1A and CYP2B subfamilies, we explored the possible interaction of the extract with these enzymes. The extract (25-50 µg/mL) inhibited CYP1A1 activity in rat liver microsomes. Analysis of the inhibition kinetics revealed a mixed-type inhibitory effect on CYP1A1 supersome. The effects of the extract on BP-induced DNA damage and hepatic CYP activity in mice were also investigated. Micronuclei induction by BP and liver CYP1A1/2 activities significantly decreased in animals treated with the extract. The results suggest that Ulva fasciata aqueous-ethanolic extract inhibits BP bioactivation and it may be a potential chemopreventive agent.

  9. Fermi liquid of two-dimensional polar molecules

    NARCIS (Netherlands)

    Lu, Z.K; Shlyapnikov, G.V.

    2012-01-01

    We study Fermi-liquid properties of a weakly interacting two-dimensional gas of single-component fermionic polar molecules with dipole moments d oriented perpendicularly to the plane of their translational motion. This geometry allows the minimization of inelastic losses due to chemical reactions

  10. Full evaporation dynamic headspace and gas chromatography-mass spectrometry for uniform enrichment of odor compounds in aqueous samples.

    Science.gov (United States)

    Ochiai, Nobuo; Sasamoto, Kikuo; Hoffmann, Andreas; Okanoya, Kazunori

    2012-06-01

    A method for analysis of a wide range of odor compounds in aqueous samples at sub-ng mL⁻¹ to μg mL⁻¹ levels was developed by full evaporation dynamic headspace (FEDHS) and gas chromatography-mass spectrometry (GC-MS). Compared to conventional DHS and headspace solid phase microextraction (HS-SPME), FEDHS provides more uniform enrichment over the entire polarity range for odor compounds in aqueous samples. FEDHS at 80°C using 3 L of purge gas allows complete vaporization of 100 μL of an aqueous sample, and trapping and drying it in an adsorbent packed tube, while providing high recoveries (85-103%) of the 18 model odor compounds (water solubility at 25°C: log0.54-5.65 mg L⁻¹, vapor pressure at 25°C: 0.011-3.2 mm Hg) and leaving most of the low volatile matrix behind. The FEDHS-GC-MS method showed good linearity (r²>0.9909) and high sensitivity (limit of detection: 0.21-5.2 ng mL⁻¹) for the model compounds even with the scan mode in the conventional MS. The feasibility and benefit of the method was demonstrated with analyses of key odor compounds including hydrophilic and less volatile characteristics in beverages (whiskey and green tea). In a single malt whiskey sample, phenolic compounds including vanillin could be determined in the range of 0.92-5.1 μg mL⁻¹ (RSDfuraneol, indole, maltol, and pyrazine congeners) were determined in the range of 0.21-110 ng mL⁻¹ (RSD<10%, n=6). Copyright © 2012 Elsevier B.V. All rights reserved.

  11. The simultaneous identification of metoprolol and its major acidic and basic metabolites in human urine by gas chromatography-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Li, Feng; Cooper, S.F. [Universite du Quebec, Pointe-Claire (Canada)

    1996-12-31

    A novel gas chromatography-mass spectrometric (GC-MS) method was developed to confirm and identify metoprolol and its metabolites by double derivatization with S-(-)menthyl chloroformate [(-)-MCF] and N-methyl(trimethylsilyl-trifluoroacetamide) (MSTFA). This is the first report, which describes the simultaneous identification of metoprolol, its one major acidc and other basic metabolites in human urine based on solid-phase extraction with C{sub 18} reversed-phase cartridges. 12 refs., 4 figs.

  12. Determination of amphetamine-type stimulants (ATSs) and synthetic cathinones in urine using solid phase micro-extraction fibre tips and gas chromatography-mass spectrometry

    OpenAIRE

    Alsenedi, Khalid A.; Morrison, Calum

    2018-01-01

    In recent years, an increasing number of stimulant drugs and new psychoactive substances (NPSs) have caused concern in scientific communities and therefore innovative methods to extract compounds from complex biological samples are required. This work is aimed at developing and validating a clean, convenient and straightforward extraction procedure with microliter amounts of organic solvent using Solid Phase Micro-Extraction tips (SPME tips) and analysis using Gas Chromatography-Mass Spectrom...

  13. Study on the biodeterioration of alkyd ah resin used as a binding medium for modern paintings by pyrolysis-gas chromatography-mass spectrometry and ftir spectroscopy

    OpenAIRE

    Domenech Carbo, Mª Teresa; BITOSSI, GIOVANNA; De La Cruz Cañizares, Juana; BOLIVAR GALIANO, FERNANDO; López Miras, Mª del Mar; Romero Noguera, Julio; MARTIN SANCHEZ, INES; GIMENO ADELANTADO, JOSE VICENTE; DOMENECH CARBO, ANTONIO

    2008-01-01

    Evaluation of the alteration produced by microbiological attack on alkyd resins has been carried out by FTIR spectroscopy and Pyrolysis-Gas Chromatography/Mass Spectrometry (Py-GC/MS). The latter included the online derivatisation of alkyd resins using hexamethyldisilazane during pyrolysis. Specimens consisting of thin films of resins formed on glass slides were used. Analyses performed on the specimens in which different genera of bacteria and fungi were inoculated and allowed to grow, indic...

  14. Introduction to the study on the biodeterioration of the poly(vinyl) acetate resin mowilith 50 using ftir spectroscopy and pyrolysis-gas chromatography-mass spectrometry

    OpenAIRE

    Domenech Carbo, Mª Teresa; BITOSSI, GIOVANNA; Osete Cortina, Laura; Yusa Marco, Dolores Julia; BOLIVAR GALIANO, FERNANDO; López Miras, Mª del Mar; Fernández Vivas, María Antonia; Martín Sánchez, Inés

    2007-01-01

    Evaluation of the alteration produced by microbiological attack on the poly(vinyl) acetate (PVA) resin Mowilith 50 has been carried out using FTIR spectroscopy and Pyrolysis-Gas Chromatography/Mass Spectrometry (Py-GC/MS). The latter proposed method includes the on-line derivatization of vinyl resins using hexamethyldisilazane during pyrolysis. Specimens consisting of thin films formed on glass slides from drying of an acetone solution of this PVA resin have been used. Analyses performed on t...

  15. Methods of analysis-Determination of pesticides in sediment using gas chromatography/mass spectrometry

    Science.gov (United States)

    Hladik, Michelle; McWayne, Megan M.

    2012-01-01

    A method for the determination of 119 pesticides in environmental sediment samples is described. The method was developed by the U.S. Geological Survey (USGS) in support of the National Water Quality Assessment (NAWQA) Program. The pesticides included in this method were chosen through prior prioritization. Herbicides, insecticides, and fungicides along with degradates are included in this method and span a variety of chemical classes including, but not limited to, chloroacetanilides, organochlorines, organophosphates, pyrethroids, triazines, and triazoles. Sediment samples are extracted by using an accelerated solvent extraction system (ASE®, and the compounds of interest are separated from co-extracted matrix interferences (including sulfur) by passing the extracts through high performance liquid chromatography (HPLC) with gel-permeation chromatography (GPC) along with the use of either stacked graphitized carbon and alumina solid-phase extraction (SPE) cartridges or packed Florisil®. Chromatographic separation, detection, and quantification of the pesticides from the sediment-sample extracts are done by using gas chromatography with mass spectrometry (GC/MS). Recoveries in test sediment samples fortified at 10 micrograms per kilogram (μg/kg) dry weight ranged from 75 to 102 percent; relative standard deviations ranged from 3 to 13 percent. Method detection limits (MDLs), calculated by using U.S. Environmental Protection Agency procedures (40 CFR 136, Appendix B), ranged from 0.6 to 3.4 μg/kg dry weight.

  16. Determination of Selected Phthalates by Gas Chromatography-Mass Spectrometry in Personal Perfumes.

    Science.gov (United States)

    Orecchio, Santino; Indelicato, Roberta; Barreca, Salvatore

    2015-01-01

    A simple and fast method is proposed to analyze commercial personal perfumes. Our method includes measurement of phthalates, known to be major sources of endocrine disruptor chemicals (EDC), which originate from the less volatile fraction of perfumes. The quantification of phthalates were carried out directly with no sample preparation required on 30 samples of commercial products using gas chromatography and mass spectrometry (GC-MS) as a detector. The total concentrations of 15 investigated compounds ranged from 17 to 9650 mg/L with an average of 2643 mg/L. The highest total concentration was found in cologne. Diethyl phthalate (DEP), diisobutyl phthalate (DiBP), di(2-ethylhexyl) phthalate (DEHP), and di-n-butyl phthalate (DBP) were detected in appreciable concentrations. Further, it was found that the composition of counterfeit samples varied widely from that of authentic products. The composition of old products was different from that of recent perfumes, which contain less harmful chemicals, attributed to the ban on some phthalates in Europe due their toxicity. It should be noted that older and contaminated products are not equivalent to authentic products when considering quality, safety, and probably effectiveness. Older and nonapproved perfumes contain chemicals that are not allowed for commercial use and may contain toxic impurities.

  17. Measuring deuterium enrichment of glucose hydrogen atoms by gas chromatography/mass spectrometry.

    Science.gov (United States)

    Antoniewicz, Maciek R; Kelleher, Joanne K; Stephanopoulos, Gregory

    2011-04-15

    We developed a simple and accurate method for determining deuterium enrichment of glucose hydrogen atoms by electron impact gas chromatography mass spectrometry (GC/MS). First, we prepared 18 derivatives of glucose and screened over 200 glucose fragments to evaluate the accuracy and precision of mass isotopomer data for each fragment. We identified three glucose derivatives that gave six analytically useful ions: (1) glucose aldonitrile pentapropionate (m/z 173 derived from C4-C5 bond cleavage; m/z 259 from C3-C4 cleavage; m/z 284 from C4-C5 cleavage; and m/z 370 from C5-C6 cleavage); (2) glucose 1,2,5,6-di-isopropylidene propionate (m/z 301, no cleavage of glucose carbon atoms); and (3) glucose methyloxime pentapropionate (m/z 145 from C2-C3 cleavage). Deuterium enrichment at each carbon position of glucose was determined by least-squares regression of mass isotopomer distributions. The validity of the approach was tested using labeled glucose standards and carefully prepared mixtures of standards. Our method determines deuterium enrichment of glucose hydrogen atoms with an accuracy of 0.3 mol %, or better, without the use of any calibration curves or correction factors. The analysis requires only 20 μL of plasma, which makes the method applicable for studying gluconeogenesis using deuterated water in cell culture and animal experiments. © 2011 American Chemical Society

  18. Characterisation of varnishes used in violins by pyrolysis-gas chromatography/mass spectrometry.

    Science.gov (United States)

    Chiavari, Giuseppe; Montalbani, Simona; Otero, Vanessa

    2008-12-01

    The correct characterisation and a detailed knowledge of the materials originally used in violin varnishes, like natural resins, is crucial for the conservation in museums and for a suitable restoration technique. The study presented here reports on the potential of pyrolysis (Py) coupled with gas chromatography (GC) and mass spectrometry (MS) for the identification of chemical markers of each resin; this technique is very sensitive and selective, it needs a small quantity of sample and does not require chemical treatments. To improve the chromatographic behaviour of polar compounds the derivatising agent tetramethylammonium hydroxide (TMAH) in combination with pyrolysis has been used, in the so-called TMAH thermochemolysis or thermally assisted hydrolysis and methylation (THM), or more simply pyrolysis-methylation. The natural resins studied were colophony, sandarac, manila copal, elemi, amber and benzoin, mainly composed of terpenic compounds, with the exception of the latter, composed of aromatic compounds. Many compounds were identified; in particular, methyl esters of resinous acids that, individually or in a group, can be used as chemical markers. However, through this technique it was not possible to distinguish between the sandarac and manila copal resins because their chromatographic behaviour is very similar. Finally, the procedure applied has been employed in the characterisation of original varnish samples.

  19. [Simultaneous determination of ten organotin compounds in polyvinyl chloride plastics using gas chromatography-mass spectrometry].

    Science.gov (United States)

    Li, Ying; Li, Bin; Liu, Li; Zhang, Chen; Wu, Jingwu; Liu, Zhihong; Li, Xintian

    2009-01-01

    A rapid and effective gas chromatography coupled with mass spectrometry method has been developed systematically and studied for the simultaneous determination of 10 organotin compounds, dibutyltin-dichloride (DBT), n-butyltin-trichloride (MBT), triethyltinchloride (TET), fentin-chloride (TPhT), chlorotributylstannane (TBT), tri-n-propyltinchloride (TPrT), diphenyltin-dichloride (DPhT), tetrabutyltin (TeBT), di-n-octyltin-dichloride (DOT), phenyltin trichloride (MPhT)), in polyvinyl chloride (PVC) plastics. The PVC sample was dissolved with tetrahydrofuran and the polymer in the sample was precipitated with methanol, and then the target compounds were derivatized with sodium tetraethylborate and extracted with hexane under ultrasonication. The qualitative and quantitative analysis were carried out by GC-MS and the total ion chromatogram and selected ion chromatogram were obtained. The derivatization and extraction conditions, such as the derivatization time, derivatization pH value, dosages of derivatization reagent and precipitation reagent were optimized. The good linearities, recoveries and precisions were obtained. The linearity ranges were 0.5 - 50 mg/L. The linearity correlation coefficients of 10 organotin compounds were between 0.997 8 and 0.999 7. The average recoveries were 84.23% - 109.1% with relative standard deviations of 4.24% - 10.75%. The established method has been successfully applied to the determination of organotin compounds in PVC plastics.

  20. Structural investigations of neuromelanin by pyrolysis-gas chromatography/mass spectrometry

    International Nuclear Information System (INIS)

    Dzierzega-Lecznar, A.; Kurkiewicz, S.; Stepien, K.; Chodurek, E.; Riederer, P.; Gerlach, M.

    2006-01-01

    Pyrolysis combined with gas chromatography and mass spectrometry (Py-GC/MS) was applied for structural investigations of the human substantia nigra neuromelanin. Using synthetic neuromelanins, we have demonstrated that Py-GC/MS is suitable for identification and differentiation of both eumelanin (dopamine-derived) and pheomelanin (cysteinyldopamine-derived) component of the pigment. Structural information on melanin monomers was inferred from their pyrolytic markers. When the human neuromelanin was subjected to pyrolysis, none of the heterocyclic, sulfur-containing markers of pheomelanin component was detected among the thermal degradation products. We have concluded that nigral pigment isolated from normal brain tissue does not contain benzothiazine-type monomers, and that cysteinyldopamine-originated units may be incorporated into the polymer in uncyclized form. The most abundant pyrolysis product was identified as limonene, which indicates that nigral pigment is tightly associated with an isoprenoid-type compound. Pyrolysis in the presence of the methylating reagent allowed identification of high levels of saturated and monounsaturated straight-chain C14-C18 fatty acid species chemically bound to the pigment macromolecule. (author)

  1. Characterization by Gas Chromatography-Mass Spectrometry of Commercially Available Thinner in the City of Cartagena

    Directory of Open Access Journals (Sweden)

    Jesus Olivero

    2013-09-01

    Full Text Available Thinner is a widely used product in the industry of paints, lubricants and adhesives. Its composition varies according to its use and quality. However, its chronic exposure is a concern, because it can affect major organs such as lungs, liver, kidney and the adrenal glands. This study characterizes the composition of several thinner samples commercially available in the city of Cartagena. Twelve samples were collected in different stores, these were then analyzed through gas chromatography coupled to mass spectrometry (GC/MS. The results showed that not only the composition but also the relative distribution of the components present in the samples are variable. Thirty two compounds were detected: toluene, o-xylene, p-xylene and ethylbenzene —among others— with occurrence frequencies of 91.7, 66.7, 75, and 66.7 %, respectively. The lack of knowledge regarding the risk of poisoning, produced when handling this type of mixtures, may be the cause of many health problems in people exposed to thinner, both in workplace and domestic activities. A data mining showed the potential association between thinner components and clinical manifestations, which include kidney and liver damage, hair loss, haematological disorders, dermatitis, anxiety and balance problems, among others. In conclusion, thinner has large variability, both in terms of components and of their relative composition. The adverse health effects of direct or indirect exposure to these components have been widely described in the literature.

  2. Analysis of galanthamine-type alkaloids by capillary gas chromatography-mass spectrometry in plants.

    Science.gov (United States)

    Berkov, Strahil; Bastida, Jaume; Viladomat, Francesc; Codina, Carles

    2008-01-01

    Galanthamine, an acetylcholinesterase inhibitor used for the treatment of Alzheimer's disease, and galanthamine-type alkaloids are synthesised in different plants of the family Amaryllidaceae. A capillary gas chromatographic-mass spectroscopic (CGC-MS) method for the separation of 7 galanthamine type alkaloids, including galanthamine and epigalanthamine, is described in the present paper. A simple method for the routine quantification of galanthamine in plants was developed using pre-packed columns with diatomaceous earth (Isolute HM-N), allowing simultaneous preparation of a large number of samples. Galanthamine showed excellent linearity in the range from 50 to 1000 microg/mL and the limit of quantification was 5 microg/mL in total ion current mode and 1.6 ng/mL in selected ion monitoring mode. The recovery of galanthamine was more than 90%. Interday reproducibility (RSD) of the extraction was 2.74%. A method to find and to microextract Amaryllidaceae alkaloids in low-mass plant samples is also described.

  3. Topology optimization of two-dimensional waveguides

    DEFF Research Database (Denmark)

    Jensen, Jakob Søndergaard; Sigmund, Ole

    2003-01-01

    In this work we use the method of topology optimization to design two-dimensional waveguides with low transmission loss.......In this work we use the method of topology optimization to design two-dimensional waveguides with low transmission loss....

  4. Identification of key aromatic compounds in Congou black tea by PLSR with variable importance of projection scores and gas chromatography-mass spectrometry/gas chromatography-olfactometry.

    Science.gov (United States)

    Mao, Shihong; Lu, Changqi; Li, Meifeng; Ye, Yulong; Wei, Xu; Tong, Huarong

    2018-04-13

    Gas chromatography-olfactometry (GC-O) is the most frequently used method to estimate the sensory contribution of single odorant, but disregards the interactions between volatiles. In order to select the key volatiles responsible for the aroma attributes of Congou black tea (Camellia sinensis), instrumental, sensory and multivariate statistical approaches were applied. By sensory analysis, nine panelists developed 8 descriptors, namely, floral, sweet, fruity, green, roasted, oil, spicy, and off-odor. Linalool, (E)-furan linalool oxide, (Z)-pyran linalool oxide, methyl salicylate, β-myrcene, phenylethyl alcohol which identified from the most representative samples by GC-O procedure, were the essential aroma-active compounds in the formation of basic Congou black tea aroma. In addition, 136 volatiles were identified by gas chromatography-mass spectrometry (GC-MS), among which 55 compounds were determined as the key factors for the six sensory attributes by partial least-square regression (PLSR) with variable importance of projection (VIP) scores. Our results demonstrated that HS-SPME/GC-MS/GC-O was a fast approach for isolation and quantification aroma-active compounds. PLSR method was also considered to be a useful tool in selecting important variables for sensory attributes. These two strategies allowed us to comprehensively evaluate the sensorial contribution of single volatile from different perspectives, can be applied to related products for comprehensive quality control. This article is protected by copyright. All rights reserved.

  5. Odour-active compounds of Citrus deliciosa Tenore var. Caí essential oils detected by gas chromatography-mass spectrometry and gas chromatography-olfactometry

    Directory of Open Access Journals (Sweden)

    Manuel A. Minteguiaga

    2017-11-01

    Full Text Available Context: Mandarins are a complex taxonomic group including different species, cultivars and hybrids growing around the world being fruits greatly appreciated by the consumers. Citrus deliciosa Tenore var. Caí originates from Rio Grande do Sul State (Brazil and the fruit is characterised by its pleasant properties, especially its aroma. Aims: To evaluate the C. deliciosa cold-pressed essential oils, classified as “green”, “yellow” and “red” according to fruit maturity, and the one produced by distillation by gas chromatography-mass spectrometry (GC-MS and gas chromatography-olfactometry (GC-O. Methods: The essential oils aromatic quality was evaluated by GC-O through a panel of trained judges. The identification of the volatile compounds was performed by GC-MS and their quantification by GC-FID. Results: The chemical composition of the three types of cold-pressed essential oils was very similar. However, the distilled oil presented a higher concentration of oxygenated monoterpenes (mainly α-terpineol, 4-terpineol and sabinene hydrates. Herbaceous and floral aromatic notes were able to describe the “green” oil, while for the distilled oil wood and unpleasant notes were perceived. Conclusions: The cold-pressed oils did not show nor chemical, or aromatic differences, by the fruit maturity. The distilled oil was characterized by aromatic nuances making the oil less appreciated (inferior quality than the cold-pressed oil. Probably as consequence of artifacts formation during the distillation process.

  6. Comparison of aroma volatiles in commercial Merlot and Cabernet Sauvignon wines using gas chromatography-olfactometry and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Gürbüz, Ozan; Rouseff, June M; Rouseff, Russell L

    2006-05-31

    Seventy-four aroma active compounds were observed in Merlot and Cabernet Sauvignon wines produced in California and Australia. Volatiles were sampled using solid phase microextraction and analyzed using time-intensity gas chromatography-olfactometry and gas chromatography-mass spectrometry (GC-MS). The most intense odorants were 3-methyl-1-butanol, 3-hydroxy-2-butanone, octanal, ethyl hexanoate, ethyl 2-methylbutanoate, beta-damascenone, 2-methoxyphenol, 4-ethenyl-2-methoxy-phenol, ethyl 3-methylbutanoate, acetic acid, and 2-phenylethanol. Aroma compounds were classified according to their aroma descriptor similarity and summed into nine distinct categories consisting of fruity, sulfury, caramel/cooked, spicy/peppery, floral, earthy, pungent/chemical, woody, and green/vegetative/fatty. Both Merlot and Cabernet Sauvignon wines were characterized by high fruity, caramel, green, and earthy aroma totals. Although there were distinct quantitative differences between Merlot and Cabernet wines, the relative aroma category profiles of the four wines were similar. Of the 66 volatiles identified by GC-MS, 28 were esters and 19 were minor alcohols. Between 81 and 88% of the total MS total ion chromatogram peak areas from each wine type were produced from only eight compounds: ethanol, ethyl octanoate, ethyl decanoate, ethyl acetate, 3-methyl-1-butanol, ethyl hexanoate, diethyl succinate, and 2-phenylethanol. Merlot wines from both Australia and California contained 4-5 times more ethyl octanoate than Cabernet Sauvignon wines from the same sources.

  7. Hydrogen sulfide measurement by headspace-gas chromatography-mass spectrometry (HS-GC-MS): application to gaseous samples and gas dissolved in muscle.

    Science.gov (United States)

    Varlet, Vincent; Giuliani, Nicole; Palmiere, Cristian; Maujean, Géraldine; Augsburger, Marc

    2015-01-01

    The aim of our study was to present a new headspace-gas chromatography-mass spectrometry (HS-GC-MS) method applicable to the routine determination of hydrogen sulfide (H(2)S) concentrations in biological and gaseous samples. The primary analytical drawback of the GC/MS methods for H(2)S measurement discussed in the literature was the absence of a specific H(2)S internal standard required to perform quantification. Although a deuterated hydrogen sulfide (D(2)S) standard is currently available, this standard is not often used because this standard is expensive and is only available in the gas phase. As an alternative approach, D(2)S can be generated in situ by reacting deuterated chloride with sodium sulfide; however, this technique can lead to low recovery yield and potential isotopic fractionation. Therefore, N(2)O was chosen for use as an internal standard. This method allows precise measurements of H(2)S concentrations in biological and gaseous samples. Therefore, a full validation using accuracy profile based on the β-expectation tolerance interval is presented. Finally, this method was applied to quantify H(2)S in an actual case of H(2)S fatal intoxication. © The Author 2014. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  8. Determining the Probability of Achieving a Successful Quantitative Analysis for Gas Chromatography-Mass Spectrometry.

    Science.gov (United States)

    Pinkerton, David K; Reaser, Brooke C; Berrier, Kelsey L; Synovec, Robert E

    2017-09-19

    A new approach is presented to determine the probability of achieving a successful quantitative analysis for gas chromatography coupled with mass spectrometry (GC-MS). The proposed theory is based upon a probabilistic description of peak overlap in GC-MS separations to determine the probability of obtaining a successful quantitative analysis, which has its lower limit of chromatographic resolution R s at some minimum chemometric resolution, R s *; that is to say, successful quantitative analysis can be achieved when R s ≥ R s *. The value of R s * must be experimentally determined and is dependent on the chemometric method to be applied. The approach presented makes use of the assumption that analyte peaks are independent and randomly distributed across the separation space or are at least locally random, namely, that each analyte represents an independent Bernoulli random variable, which is then used to predict the binomial probability of successful quantitative analysis. The theoretical framework is based on the chromatographic-saturation factor and chemometric-enhanced peak capacity. For a given separation, the probability of quantitative success can be improved via two pathways, a chromatographic-efficiency pathway that reduces the saturation of the sample and a chemometric pathway that reduces R s * and improves the chemometric-enhanced peak capacity. This theory is demonstrated through a simulation-based study to approximate the resolution limit, R s *, of multivariate curve resolution-alternating least-squares (MCR-ALS). For this study, R s * was determined to be ∼0.3, and depending on the analytical expectations for the quantitative bias and the obtained mass-spectral match value, a lower value of R s * ∼ 0.2 may be achievable.

  9. Onsite well screening with a transportable gas chromatography/mass spectrometer system

    International Nuclear Information System (INIS)

    Rossabi, J.; Eckenrode, B.A.; Owens, B.

    1992-01-01

    The number of hazardous waste site operations continue to multiply. The requirements for efficient chemical assessment and monitoring of these sites become more stringent daily. As more samples are required, the time required for cleanup operations also increases and may make analytical costs prohibitive. Thus improvements in operation efficiency and reduction of cost in evaluating specific sites to minimize or eliminate their toxic effects on the surrounding environment are critical. For many years a formal policy did not exist for the disposal of waste solvents and other chemicals, thus many of these compounds were disposed of ensite. So long as these materials were contained onsite they were not considered to pose a threat to the surrounding environment. We have since determined that many of these compounds found their way into the groundwater. Contaminants such as trichloroethylene and perchloroethylene, which were heavily used for cleaning and degreasing purposes, must be monitored. Groundwater wells can be used to define the location and extent of the migration of any contaminant plume and aid in the determination of required cleanup. The major problem is that monitoring of hundreds of wells may be necessary, requiring several hundred samples on a quarterly basis to characterize the degree and extent of any contamination. Onsite analysis of monitoring wells for this characterization of waste operations could provide time savings and significant cost reduction. Field analyses can provide the required analytical results quickly and at a reduced cost without compromising either sample integrity or data quality. By using onsite analytical instrumentation, such as a field-transportable gas chromatograph/mass spectrometer (GC/MS), screening analyses can be performed to eliminate retturning to the laboratory with meaningless samples. Onsite GC/MS will provide qualitative or semi-quantitative information that can significantly simplify subsequent laboratory analyses

  10. Technical advance: simultaneous analysis of metabolites in potato tuber by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Roessner, U; Wagner, C; Kopka, J; Trethewey, R N; Willmitzer, L

    2000-07-01

    A new method is presented in which gas chromatography coupled to mass spectrometry (GC-MS) allows the quantitative and qualitative detection of more than 150 compounds within a potato tuber, in a highly sensitive and specific manner. In contrast to other methods developed for metabolite analysis in plant systems, this method represents an unbiased and open approach that allows the detection of unexpected changes in metabolite levels. Although the method represents a compromise for a wide range of metabolites in terms of extraction, chemical modification and GC-MS analysis, for 25 metabolites analysed in detail the recoveries were found to be within the generally accepted range of 70-140%. Further, the reproducibility of the method was high: the error occurring in the analysis procedures was found to be less than 6% for 30 out of 33 compounds tested. Biological variability exceeded the systematic error of the analysis by a factor of up to 10. The method is also suited for upscaling, potentially allowing the simultaneous analysis of a large number of samples. As a first example this method has been applied to soil- and in vitro-grown tubers. Due to the simultaneous analysis of a wide range of metabolites it was immediately apparent that these systems differ significantly in their metabolism. Furthermore, the parallel insight into many pathways allows some conclusions to be drawn about the underlying physiological differences between both tuber systems. As a second example, transgenic lines modified in sucrose catabolism or starch synthesis were analysed. This example illustrates the power of an unbiased approach to detecting unexpected changes in transgenic lines.

  11. The use of comprehensive two-dimensional gas chromatography and structure-activity modeling for screening and preliminary risk assessment of organic contaminants in soil, sediment, and surface water

    Energy Technology Data Exchange (ETDEWEB)

    Moreira Bastos, Patricia; Haglund, Peter [Umeaa Univ. (Sweden). Dept. of Chemistry

    2012-08-15

    Purpose: This article aims to investigate the use and benefits of using comprehensive two-dimensional gas chromatography (GC x GC) and structure-activity relationship modeling for screening and prioritization of organic contaminants in complex matrices. The benefit of applying comprehensive screening techniques to samples with high organic contaminant content is primarily that compounds with diverse physicochemical properties can be analyzed simultaneously. Here, a heavily contaminated industrial area was surveyed for organic pollutants by analyzing soil, sediment, and surface water samples. The hazard of the pollutants were ranked using SARs. Material and methods: The water samples were liquid-liquid extracted using dichloromethane and directly analyzed by GC x GC-time-of-flight mass spectrometry (GC x GC-TofMS). Soil and sediment samples were extracted with dichloromethane in an ultrasonic bath and subjected to gel permeation chromatography to eliminate lipids and humic matter. The low molecular weight fraction was then analyzed with GC x GC-TofMS. Results and discussion: More than 10,000 components were found in each sample, of which ca. 300 individual compounds were unambiguously identified using the National Institute of Standards and Technology mass spectra library and authentic reference standards. Alkanes, polycyclic aromatic hydrocarbons, and phthalates were generally the most abundant and were found in all matrices. In contrast, chlorinated compounds such as chlorophenols, biphenyls, and chlorinated pesticides were only detected in samples from a few hotspot regions. The toxicities of the most frequently detected compounds and of the compounds detected at the highest concentrations in samples from hotspot regions were estimated by ecological structure-activity relationships. The ratio of the measured concentration to the predicted toxicity level was then calculated for each compound and used for an initial risk assessment in order to prioritize compounds

  12. Chemical characterization of the acid alteration of diesel fuel: Non-targeted analysis by two-dimensional gas chromatography coupled with time-of-flight mass spectrometry with tile-based Fisher ratio and combinatorial threshold determination.

    Science.gov (United States)

    Parsons, Brendon A; Pinkerton, David K; Wright, Bob W; Synovec, Robert E

    2016-04-01

    The illicit chemical alteration of petroleum fuels is of keen interest, particularly to regulatory agencies that set fuel specifications, or taxes/credits based on those specifications. One type of alteration is the reaction of diesel fuel with concentrated sulfuric acid. Such reactions are known to subtly alter the chemical composition of the fuel, particularly the aromatic species native to the fuel. Comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry (GC×GC-TOFMS) is well suited for the analysis of diesel fuel, but may provide the analyst with an overwhelming amount of data, particularly in sample-class comparison experiments comprised of many samples. Tile-based Fisher-ratio (F-ratio) analysis reduces the abundance of data in a GC×GC-TOFMS experiment to only the peaks which significantly distinguish the unaltered and acid altered sample classes. Three samples of diesel fuel from differently branded filling stations were each altered to discover chemical features, i.e., analyte peaks, which were consistently changed by the acid reaction. Using different fuels prioritizes the discovery of features likely to be robust to the variation present between fuel samples and may consequently be useful in determining whether an unknown sample has been acid altered. The subsequent analysis confirmed that aromatic species are removed by the acid alteration, with the degree of removal consistent with predicted reactivity toward electrophilic aromatic sulfonation. Additionally, we observed that alkenes and alkynes were also removed from the fuel, and that sulfur dioxide or compounds that degrade to sulfur dioxide are generated by the acid alteration. In addition to applying the previously reported tile-based F-ratio method, this report also expands null distribution analysis to algorithmically determine an F-ratio threshold to confidently select only the features which are sufficiently class-distinguishing. When applied to the acid

  13. Chemical characterization of the acid alteration of diesel fuel: Non-targeted analysis by two-dimensional gas chromatography coupled with time-of-flight mass spectrometry with tile-based Fisher ratio and combinatorial threshold determination

    Energy Technology Data Exchange (ETDEWEB)

    Parsons, Brendon A.; Pinkerton, David K.; Wright, Bob W.; Synovec, Robert E.

    2016-04-01

    The illicit chemical alteration of petroleum fuels is of scientific interest, particularly to regulatory agencies which set fuel specifications, or excises based on those specifications. One type of alteration is the reaction of diesel fuel with concentrated sulfuric acid. Such reactions are known to subtly alter the chemical composition of the fuel, particularly the aromatic species native to the fuel. Comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry (GC × GC–TOFMS) is ideally suited for the analysis of diesel fuel, but may provide the analyst with an overwhelming amount of data, particularly in sample-class comparison experiments comprised of many samples. The tile-based Fisher-ratio (F-ratio) method reduces the abundance of data in a GC × GC–TOFMS experiment to only the peaks which significantly distinguish the unaltered and acid altered sample classes. Three samples of diesel fuel from different filling stations were each altered to discover chemical features, i.e., analyte peaks, which were consistently changed by the acid reaction. Using different fuels prioritizes the discovery of features which are likely to be robust to the variation present between fuel samples and which will consequently be useful in determining whether an unknown sample has been acid altered. The subsequent analysis confirmed that aromatic species are removed by the acid alteration, with the degree of removal consistent with predicted reactivity toward electrophilic aromatic sulfonation. Additionally, we observed that alkenes and alkynes were also removed from the fuel, and that sulfur dioxide or compounds that degrade to sulfur dioxide are generated by the acid alteration. In addition to applying the previously reported tile-based F-ratio method, this report also expands null distribution analysis to algorithmically determine an F-ratio threshold to confidently select only the features which are sufficiently class-distinguishing. When

  14. Fuzzy C-means clustering for chromatographic fingerprints analysis: A gas chromatography-mass spectrometry case study.

    Science.gov (United States)

    Parastar, Hadi; Bazrafshan, Alisina

    2016-03-18

    Fuzzy C-means clustering (FCM) is proposed as a promising method for the clustering of chromatographic fingerprints of complex samples, such as essential oils. As an example, secondary metabolites of 14 citrus leaves samples are extracted and analyzed by gas chromatography-mass spectrometry (GC-MS). The obtained chromatographic fingerprints are divided to desired number of chromatographic regions. Owing to the fact that chromatographic problems, such as elution time shift and peak overlap can significantly affect the clustering results, therefore, each chromatographic region is analyzed using multivariate curve resolution-alternating least squares (MCR-ALS) to address these problems. Then, the resolved elution profiles are used to make a new data matrix based on peak areas of pure components to cluster by FCM. The FCM clustering parameters (i.e., fuzziness coefficient and number of cluster) are optimized by two different methods of partial least squares (PLS) as a conventional method and minimization of FCM objective function as our new idea. The results showed that minimization of FCM objective function is an easier and better way to optimize FCM clustering parameters. Then, the optimized FCM clustering algorithm is used to cluster samples and variables to figure out the similarities and dissimilarities among samples and to find discriminant secondary metabolites in each cluster (chemotype). Finally, the FCM clustering results are compared with those of principal component analysis (PCA), hierarchical cluster analysis (HCA) and Kohonon maps. The results confirmed the outperformance of FCM over the frequently used clustering algorithms. Copyright © 2016 Elsevier B.V. All rights reserved.

  15. Cerumen of Australian stingless bees ( Tetragonula carbonaria): gas chromatography-mass spectrometry fingerprints and potential anti-inflammatory properties

    Science.gov (United States)

    Massaro, Flavia Carmelina; Brooks, Peter Richard; Wallace, Helen Margaret; Russell, Fraser Donald

    2011-04-01

    Cerumen, or propolis, is a mixture of plant resins enriched with bee secretions. In Australia, stingless bees are important pollinators that use cerumen for nest construction and possibly for colony's health. While extensive research attests to the therapeutic properties of honeybee ( Apis mellifera) propolis, the biological and medicinal properties of Australian stingless bee cerumen are largely unknown. In this study, the chemical and biological properties of polar extracts of cerumen from Tetragonula carbonaria in South East Queensland, Australia were investigated using gas chromatography-mass spectrometry (GC-MS) analyses and in vitro 5-lipoxygenase (5-LOX) cell-free assays. Extracts were tested against comparative (commercial tincture of A. mellifera propolis) and positive controls (Trolox and gallic acid). Distinct GC-MS fingerprints of a mixed diterpenic profile typical of native bee cerumen were obtained with pimaric acid (6.31 ± 0.97%, w/w), isopimaric acid (12.23 ± 3.03%, w/w), and gallic acid (5.79 ± 0.81%, w/w) tentatively identified as useful chemical markers. Characteristic flavonoids and prenylated phenolics found in honeybee propolis were absent. Cerumen extracts from T. carbonaria inhibited activity of 5-LOX, an enzyme known to catalyse production of proinflammatory mediators (IC50 19.97 ± 2.67 μg/ml, mean ± SEM, n = 4). Extracts had similar potency to Trolox (IC50 12.78 ± 1.82 μg/ml), but were less potent than honeybee propolis (IC50 5.90 ± 0.62 μg/ml) or gallic acid (IC50 5.62 ± 0.35 μg/ml, P beekeeping industry.

  16. Determination of nitrogen mustard hydrolysis products, ethanolamines by gas chromatography-mass spectrometry after tert-butyldimethylsilyl derivatization.

    Science.gov (United States)

    Ohsawa, Isaac; Seto, Yasuo

    2006-07-28

    A method for determining N-ethyldiethanolamine (EDEA), N-methyldiethanolamine (MDEA) and triethanolamine (TEA), hydrolysis products of nitrogen mustards, in water, urine and blood samples using gas chromatography-mass spectrometry (GC-MS) after derivatization by tert-butyldimethylsilylation (TBDMS) is described. The sample solution was evaporated to dryness, and reacted with N-methyl-N-(tert-butyldimethylsilyl)trifluoroacetamide (MTBSTFA) at 60 degrees C for 1h. The TBDMS derivatives were separated on a DB-5 column and detected by electron-ionization MS. The quantitation of EDEA, MDEA and TEA was performed by measuring the respective peak areas on the extracted ion chromatograms of m/z 216, m/z 202 and m/z 346, respectively, using nonadecane (C19), the peak area of which was measured at m/z 268, as an internal standard. When the water sample was initially analyzed, considerable loss of EDEA, MDEA and TEA occurred by evaporation. The addition of hydrochloric acid (HCl) to the water sample (final 1 mM), however, permitted quantitative recoveries to be achieved (88%, 88% and 79% for EDEA-(TBDMS)2, MDEA-(TBDMS)2 and TEA-(TBDMS)3, respectively). The limits of detections (LODs, scan mode, S/N = 3) were 2.5, 2.5 and 10 ng/ml for EDEA, MDEA and TEA, respectively. Ethanolamines could be also determined in urine samples (volume 0.1 ml), with reasonable recoveries of 72-100% by the addition of HCl (final 1 mM). For the analysis of serum samples, the sample was precipitated by the addition of perchloric acid (final 3.2%), and the resulting supernatant was neutralized with potassium carbonate, and then acidified by the addition of HCl. The recovery of TBDMS derivatives of ethanolamines was found to rather low (7-31%).

  17. Estimation of D-Arabinose by Gas Chromatography/Mass Spectrometry as Surrogate for Mycobacterial Lipoarabinomannan in Human Urine.

    Directory of Open Access Journals (Sweden)

    Prithwiraj De

    Full Text Available Globally, tuberculosis is slowly declining each year and it is estimated that 37 million lives were saved between 2000 and 2013 through effective diagnosis and treatment. Currently, diagnosis relies on demonstration of the bacteria, Mycobacterium tuberculosis (Mtb, in clinical specimens by serial sputum microscopy, culture and molecular testing. Commercial immunoassay lateral flow kits developed to detect Mtb lipoglycan lipoarabinomannan (LAM in urine as a marker of active TB exhibit poor sensitivity, especially in immunocompetent individuals, perhaps due to low abundance of the analyte. Our present study was designed to develop methods to validate the presence of LAM in a quantitative fashion in human urine samples obtained from culture-confirmed TB patients. Herein we describe, a consolidated approach for isolating LAM from the urine and quantifying D-arabinose as a proxy for LAM, using Gas Chromatography/Mass Spectrometry. 298 urine samples obtained from a repository were rigorously analyzed and shown to contain varying amounts of LAM-equivalent ranging between ~10-40 ng/mL. To further substantiate that D-arabinose detected in the samples originated from LAM, tuberculostearic acid, the unique 10-methyloctadecanoic acid present at the phosphatidylinositol end of LAM was also analyzed in a set of samples and found to be present confirming that the D-arabinose was indeed derived from LAM. Among the 144 samples from culture-negative TB suspects, 30 showed presence of D-arabinose suggesting another source of the analyte, such as disseminated TB or from non-tuberculosis mycobacterium. Our work validates that LAM is present in the urine samples of culture-positive patients in small but readily detectable amounts. The study further substantiates LAM in urine as a powerful biomarker for active tuberculosis.

  18. Molecular analysis of intact preen waxes of Calidris canutus (Aves: Scolopacidae) by gas chromatography/mass spectrometry.

    Science.gov (United States)

    Dekker, M H; Piersma, T; Damsté, J S

    2000-05-01

    The intact preen wax esters of the red knot Calidris canutus were studied with gas chromatography/mass spectrometry (GC/MS) and GC/MS/MS. In this latter technique, transitions from the molecular ion to fragment ions representing the fatty acid moiety of the wax esters were measured, providing additional resolution to the analysis of wax esters. The C21-C32 wax esters are composed of complex mixtures of hundreds of individual isomers. The odd carbon-numbered wax esters are predominantly composed of even carbon-numbered n-alcohols (C14, C16, and C18) esterified predominantly with odd carbon-numbered 2-methyl fatty acids (C7, C9, C11, and C13), resulting in relatively simple distributions. The even carbon-numbered wax esters show a far more complex distribution due to a number of factors: (i) Their n-alcohol moieties are not dominated by even carbon-numbered n-alcohols esterified with odd carbon-numbered 2-methyl fatty acids, but odd and even carbon-numbered n-alcohols participate in approximately equal amounts; (ii) odd carbon-numbered methyl-branched alcohols participate abundantly in these wax ester clusters; and (iii) with increasing molecular weight, various isomers of the 2,6-, 2,8-, and 2,10-dimethyl branched fatty acids also participate in the even carbon-numbered wax esters. The data demonstrate that there is a clear biosynthetic control on the wax ester composition although the reasons for the complex chemistry of the waxes are not yet understood.

  19. Development and validation of a gas chromatography-mass spectrometry assay for opiates and cocaine in human teeth.

    Science.gov (United States)

    Pellegrini, Manuela; Casá, Adriana; Marchei, Emilia; Pacifici, Roberta; Mayné, Ruth; Barbero, Vanessa; Garcia-Algar, Oscar; Pichini, Simona

    2006-02-24

    A procedure based on gas chromatography-mass spectrometry (GC-MS) is described for determination of opiates (6-monoacetylmorphine, morphine and codeine) and cocaine and metabolites (cocaine, benzoylecgonine and cocaethylene) in human teeth. After addition of nalorphine as internal standard, pulverized samples were incubated in HCl at 37 degrees C for 18 h. Then, after pH adjustment to 6, and the analytes were extracted with two volumes of 3 ml of chloroform/isopropanol (9:1). Chromatography was performed on a fused silica capillary column and analytes were determined in the selected-ion-monitoring (SIM) mode. The assay was validated in the range 7.5 (6.0 in case of codeine) to 500 ng/g with mean absolute recoveries ranged between 74.1 and 92.1% for the different analytes and precision and accuracy always better than 15%. The method was applied to the analysis of teeth from drug-addicts to assess past chronic consumption and verify self-reported declarations. In case of opiates, concentration range was 36.5-570.0 ng/g for 6-monoacetylmorphine, 8.7-154.8 ng/g for morphine and 7.9-127.9 ng/g for codeine. Cocaine concentration ranged between 5.6 and 57.2 ng/g with its principal metabolite benzoylecgonine varying from 12.6 to 81.7 ng/g and cocaethylene present in only one sample at 10 ng/g value. Teeth can be a promising non-invasive biological matrix in biomedical analysis for both clinical and forensic purposes.

  20. Multi-Residue Analysis of Pesticides in Pistachio Using Gas Chromatography-Mass Spectrometry (GC/MS

    Directory of Open Access Journals (Sweden)

    Azadeh Emami

    2014-12-01

    Full Text Available Background: Analysis of pesticide residues in food and other environmental commodities have become an essential requirement for consumers, producers, food inspectors and authorities. This study is focused on validation of an accurate, rapid and reliable method for multi-residual analysis of pesticides in pistachio as a strategic crop for export and one of the main nuts in Iranian food basket. Methods: We developed a "Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS method based on spiking blank samples and used the data for drawing calibration curves instead of standard solutions. Sample preparations were developed for determination of 12 pesticide residues in pistachio by gas chromatography-mass spectrometry (GC/MS. Results: Recovery of pesticides at 5 concentration levels (n=3 was in the range of 81.40% - 93.08 %. The method proved to be repeatable in the majority of samples with relative standard deviation (RSD of lower than 20%. The limits of detection and quantification for all pesticides were 2 ppb and 10 ppb, respectively. Conclusion: The calibration curves of pesticides were linear in the range of 10-500 (ng/g and correlation coefficient of entire pesticides was higher than 0.994. The recovery of pesticides at 5 concentration levels (n=3 was in range of 81.41- 91.80 %. The method was proved to be repeatable with the majority of RSDs being lower than 20%. The limits of detection and quantification for all pesticides were 2 and 10 ppb, respectively. The recoveries and repeatabilities were in accordance with the criteria set by SANCO Guideline (Commission of the European Communities, 2006.

  1. Analysis of nitroaromatic compounds in urine by gas chromatography-mass spectrometry for the biological monitoring of explosives.

    Science.gov (United States)

    Bader, M; Göen, T; Müller, J; Angerer, J

    1998-06-12

    Organic nitrocompounds are the most frequently used constituents of explosives and some of them have been evaluated to be highly toxic or even carcinogenic. Human contact with explosives may originate from a variety of sources, including occupational exposure during the production of ammunition as well as environmental exposure due to the contamination of soil and ground water reservoirs on former military production sites and training areas. This paper describes two gas chromatography-mass spectrometry-selected ion monitoring methods for the determination of twelve nitroaromatic compounds in urine (nitrobenzene, 1,2-dinitrobenzene, 1,3-dinitrobenzene, 1,3,5-trinitrobenzene, 2-nitrotoluene, 3-nitrotoluene, 4-nitrotoluene, 2,4-dinitrotoluene, 2,6-dinitrotoluene, 2,4,6-trinitrotoluene, 2-amino-4,6-dinitrotoluene, 4-amino-2,6-dinitrotoluene). The analytes are detectable in the lowest microg/l range, with imprecisions of 3-22% within series and 5-29% between series, depending on the compound of interest. Both procedures are rapid and relatively easy to perform and, therefore, are advantageous for the screening of occupationally or environmentally exposed persons. We analysed urine samples obtained from nine workers from an ammunition dismantling workshop and from twelve control persons. 2,4,6-Trinitrotoluene was detected in six samples at concentrations between 4 and 43 microg/l. The main metabolites of 2,4,6-trinitrotoluene, 4-amino-2,6-dinitrotoluene and 2-amino-4,6-dinitrotoluene, were found in a concentration range from 143 to 16,832 microg/l and from 24 to 5787 microg/l, respectively. Nonconjugated aminodinitrotoluenes were present as varying percentages of the total amount. 2,4-Dinitrotoluene and 2,6-dinitrotoluene were found in two samples (2-9 microg/l). Nitroaromatics were not detectable in urine specimens from control persons.

  2. Simultaneous analysis of urinary phthalate metabolites of residents in Korea using isotope dilution gas chromatography-mass spectrometry.

    Science.gov (United States)

    Kim, Miok; Song, Na Rae; Choi, Jong-Ho; Lee, Jeongae; Pyo, Heesoo

    2014-02-01

    Phthalates are used in industry products, household items, and medical tools as plasticizers. Human exposure to phthalates has raised concern about its toxicity. In the present study, optimization was conducted for the simultaneous analysis of eight kinds of phthalate metabolites using gas chromatography-mass spectrometry (GC-MS): MEP, MiBP, MnBP, MBzP, MiNP, MEHP, MEOHP, and MEHHP. In order to minimize the matrix effect and to do quantitative analysis, isotope dilution and LLE-GC-MS methods were performed. Urine samples were enzymatically hydrolyzed, extracted with a mixture of n-hexane and ethyl ether (8:2; v:v), and subsequently derivatized with trimethylsilylation. All eight kinds of analytes showed clear resolution and high reproducibility in GC-MS results. The method detection limit ranged from 0.05 ng/mL to 0.2 ng/mL. Calibration curves were found to be linear from 0.2 to 100 ng/mL with -(2)>0.992. The relative standard deviation of the intraday precision using water and urine ranged from 2.1% to 16.3%. The analysis was performed with urine samples that were collected from adults residing in the Republic of Korea. The analyzed concentration results were compared according to gender and region. As a result, DEHP metabolites showed the highest detected concentration (75.92 μg/g creatinine, 100%), and MiNP, a metabolite of DiNP, showed the lowest detected concentration (0.42 μg/g creatinine, 22.5%). On average, female urine (200.76 μg/g creatinine) had a higher detected concentration of ∑8 phthalate metabolites than male urine. Samples from rural regions (211.96 μg/g creatinine) had higher levels than samples from urban regions. © 2013.

  3. Differentiation of South American crack and domestic (US) crack cocaine via headspace-gas chromatography/mass spectrometry.

    Science.gov (United States)

    Colley, Valerie L; Casale, John F

    2015-03-01

    South American 'crack' cocaine, produced directly from coca leaf, can be distinguished from US domestically produced crack on the basis of occluded solvent profiles. In addition, analysis of domestically produced crack indicates the solvents that were used for cocaine hydrochloride (HCl) processing in South America. Samples of cocaine base (N=3) from South America and cocaine from the USA (N=157 base, N=88 HCl) were analyzed by headspace-gas chromatography-mass spectrometry (HS-GC-MS) to determine their solvent profiles. Each cocaine HCl sample was then converted to crack cocaine using the traditional crack production method and re-examined by HS-GC-MS. The resulting occluded solvent profiles were then compared to their original HCl solvent profiles. Analysis of the corresponding crack samples confirmed the same primary processing solvents found in the original HCl samples, but at reduced levels. Domestically seized crack samples also contained reduced levels of base-to-HCl conversion solvents. In contrast, analysis of South American crack samples confirmed the presence of low to high boiling hydrocarbons and no base-to-HCl conversion solvents. The presented study showed analysis of crack cocaine samples provides data on which processing solvents were originally utilized in the production of cocaine HCl in South America, prior to conversion to crack cocaine. Determination of processing solvents provides valuable information to the counter-drug intelligence community and assists the law enforcement community in determining cocaine distribution and trafficking routes throughout the world. Published 2014. This article is a U.S. Government work and is in the public domain in the USA.

  4. Gas chromatography/mass spectrometry-based urine metabolome study in children for inborn errors of metabolism: An Indian experience.

    Science.gov (United States)

    Hampe, Mahesh H; Panaskar, Shrimant N; Yadav, Ashwini A; Ingale, Pramod W

    2017-02-01

    The present study highlights the feasibility of gas chromatography/mass spectrometry (GC/MS)-based analysis for simultaneous detection of >200 marker metabolites in urine found in characteristic pattern in inborn errors of metabolism (IEM) in India. During this retrospective study conducted from July 2013 to January 2016, we collected urine specimens on filter papers from Indian children across the country along with relevant demographic and clinical data. The laboratory technique involved urease pretreatment followed by deproteinization, derivatization, and subsequent computer-aided analysis of organic acids, amino acids, fatty acids, and sugars by GC/MS, which enable chemical diagnosis of IEM. Totally 23,140 patients were investigated for IEM with an estimated frequency of about 1.40%, that is, 323 positive cases. Most frequent disorders observed were of primary lactic acidemia (27.2%) and organic acidemia (methylmalonic aciduria, glutaric acidemia type I, propionic aciduria, etc.) followed by aminoacidopathies (maple syrup urine disease, phenylketonuria, tyrosinemia, etc.). Furthermore, alkaptonuria, canavan disease, and 4-hydroxybutyric aciduria were also diagnosed. Prompt treatment following diagnosis led to a better outcome in a considerable number of patients. GC/MS with one-step metabolomics enables quick detection, accurate identification, and precise quantification of a wide range of urinary markers that may not be discovered using existing newborn screening programs. The technique is effective as a second-tier test to other established screening technologies, as well as one-step primary screening tool for a wide spectrum of IEM. Copyright © 2016 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights reserved.

  5. Graphitized carbon in gas-liquid-solid chromatography and gas chromatography/mass spectrometric analysis of high boiling hydrocarbon mixtures

    International Nuclear Information System (INIS)

    Ciccioli, P.; Hayes, J.M.; Rinaldi, G.; Denson, K.B.; Meinschein, W.G.

    1979-01-01

    Gas--liquid--solid chromatography (GLSC) employing a poly(phenyl ether) (PPE 20) liquid phase on graphitized carbon black (GCB) is applicable to the analyses of crude oils and distillates of sedimentary rocks. The elution of C 4 to C 40 hydrocarbons which consist of n-alkanes, isoprenoid-type alkanes, steranes, olefins, and aromatic hydrocarbons can be handled in a single GC run. A GLSC column in tandem with a mass spectrometer provides an excellent means for the identification of geochemically significant organic compounds in complex natural mixtures. 8 figures, 4 tables

  6. Comprehensive lipidomic analysis of human plasma using multidimensional liquid- and gas-phase separations: Two-dimensional liquid chromatography-mass spectrometry vs. liquid chromatography-trapped-ion-mobility-mass spectrometry

    NARCIS (Netherlands)

    Baglai, A.; Gargano, A.F.G.; Jordens, J.; Mengerink, Y.; Honing, M.; van der Wal, S.; Schoenmakers, P.J.

    2017-01-01

    Recent advancements in separation science have resulted in the commercialization of multidimensional separation systems that provide higher peak capacities and, hence, enable a more-detailed characterization of complex mixtures. In particular, two powerful analytical tools are increasingly used by

  7. Development of Two-Dimensional NMR

    Indian Academy of Sciences (India)

    Home; Journals; Resonance – Journal of Science Education; Volume 20; Issue 11. Development of Two-Dimensional NMR: Strucure Determination of Biomolecules in Solution. Anil Kumar. General Article Volume 20 Issue 11 November 2015 pp 995-1002 ...

  8. Conoscopic holography: two-dimensional numerical reconstructions.

    Science.gov (United States)

    Mugnier, L M; Sirat, G Y; Charlot, D

    1993-01-01

    Conoscopic holography is an incoherent light holographic technique based on the properties of crystal optics. We present experimental results of the numerical reconstruction of a two-dimensional object from its conoscopic hologram.

  9. H₂ sensing properties of two-dimensional zinc oxide nanostructures.

    Science.gov (United States)

    Tonezzer, Matteo; Iannotta, Salvatore

    2014-05-01

    In this work we have grown particular zinc oxide two-dimensional nanostructures which are essentially a series of hexagonal very thin sheets. The hexagonal wurtzite crystal structure gives them their peculiar shape, whose dimensions are few microns wide, with a thickness in the order of 25 nm. Such kind of nanostructure, grown by thermal oxidation of evaporated metallic zinc on a silica substrate, has been used to fabricate conductometric gas sensors, investigated then for hydrogen gas detection. The "depletion layer sensing mechanism" is clarified, explaining how the geometrical factors of one- and two-dimensional nanostructures affect their sensing parameters. The comparison with one-dimensional ZnO nanowires based structures shows that two-dimensional nanostructures are ideal for gas sensing, due to their tiny thickness, which is comparable to the depletion-layer thickness, and their large cross-section, which increases the base current, thus lowering the limit of detection. The response to H₂ has been found good even to sub-ppm concentrations, with response and recovery times shorter than 18s in the whole range of H₂ concentrations investigated (500 ppb-10 ppm). The limit of detection has been found around 200 ppb for H₂ gas even at relatively low working temperature (175 °C). Copyright © 2014 Elsevier B.V. All rights reserved.

  10. Simultaneous determination of lincomycin and spectinomycin residues in animal tissues by gas chromatography-nitrogen phosphorus detection and gas chromatography-mass spectrometry with accelerated solvent extraction.

    Science.gov (United States)

    Tao, Y; Chen, D; Yu, G; Yu, H; Pan, Y; Wang, Y; Huang, L; Yuan, Z

    2011-02-01

    A new multi-dimensional analytical method using gas chromatography-nitrogen phosphorus detection (GC-NPD) and gas chromatography-mass spectrometry (GC-MS) was developed for qualitative and quantitative measurement of lincomycin and spectinomycin residues in food animal tissues. This method is based on a new extraction procedure using accelerated solvent extraction (ASE). The analytes were extracted by phosphate buffer with trichloroacetic acid deproteinization and clean-up by C₁₈ solid-phase extraction (SPE) adding dodecanesulfonic acid sodium salt as an ion-pair reagent. The eluted fraction was evaporated and derivatised with N,O-bis(trimethylsilyl) trifluoroacetamide (BSTFA) for GC-NPD analysis and GC-MS confirmation. Parameters for extraction pressure, temperature and cycle of ASE, clean-up, derivatisation and analysis procedure were optimised. The method was validated in muscle, kidney and liver of swine, bovine with a low concentration (limit of quantification) of 16.4 and 21.4 µg kg⁻¹ for these two analytes using GC-NPD. For GC-MS, the limits of quantification were 4.1 and 5.6 µg kg⁻¹, respectively. Spiked recoveries from levels of 20 to 200 µg kg⁻¹ were found to be between 73% and 99% with a relative standard deviation (RSD) of less than 17% in GC-NPD. For GC-MS, levels from 5 to 20 µg kg⁻¹ had between 70% and 93% with an RSD of less than 21%. This rapid and reliable method can be used for the characterisation and quantification of residues of lincomycin and spectinomycin in animal tissues.

  11. Monitoring the ripening process of Cheddar cheese based on hydrophilic component profiling using gas chromatography-mass spectrometry.

    Science.gov (United States)

    Ochi, H; Sakai, Y; Koishihara, H; Abe, F; Bamba, T; Fukusaki, E

    2013-01-01

    We proposed an application methodology that combines metabolic profiling with multiple appropriate multivariate analyses and verified it on the industrial scale of the ripening process of Cheddar cheese to make practical use of hydrophilic low-molecular-weight compound profiling using gas chromatography-mass spectrometry to design optimal conditions and quality monitoring of the cheese ripening process. Principal components analysis provided an overview of the effect of sodium chloride content and kind of lactic acid bacteria starter on the metabolic profile in the ripening process of Cheddar cheese and orthogonal partial least squares-discriminant analysis unveiled the difference in characteristic metabolites. When the sodium chloride contents were different (1.6 and 0.2%) but the same lactic acid bacteria starter was used, the 2 cheeses were classified by orthogonal partial least squares-discriminant analysis from their metabolic profiles, but were not given perfect discrimination. Not much difference existed in the metabolic profile between the 2 cheeses. Compounds including lactose, galactose, lactic acid, 4-aminobutyric acid, and phosphate were identified as contents that differed between the 2 cheeses. On the other hand, in the case of the same salt content of 1.6%, but different kinds of lactic acid bacteria starter, an excellent distinctive discrimination model was obtained, which showed that the difference of lactic acid bacteria starter caused an obvious difference in metabolic profiles. Compounds including lactic acid, lactose, urea, 4-aminobutyric acid, galactose, phosphate, proline, isoleucine, glycine, alanine, lysine, leucine, valine, and pyroglutamic acid were identified as contents that differed between the 2 cheeses. Then, a good sensory prediction model for "rich flavor," which was defined as "thick and rich, including umami taste and soy sauce-like flavor," was constructed based on the metabolic profile during ripening using partial least

  12. Analysis of polysulfides in drinking water distribution systems using headspace solid-phase microextraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Kristiana, Ina; Heitz, Anna; Joll, Cynthia; Sathasivan, Arumugam

    2010-09-17

    Sulfide and polysulfides are strong nucleophiles and reducing agents that participate in many environmentally significant processes such as the formation of sulfide minerals and volatile organic sulfur compounds. Their presence in drinking water distribution systems are of particular concern and need to be assessed, since these species consume disinfectants and dissolved oxygen, react with metal ions to produce insoluble metal sulfides, and cause taste and odour problems. The analysis of sulfide and polysulfides in drinking water distribution systems is challenging due to their low concentrations, thermal instability and their susceptibility to undergo oxidation and disproportionation reactions. This paper reports on the development and optimisation of a rapid, simple, and sensitive method for the determination of sulfide and polysulfides in drinking water distribution systems. The method uses methyl iodide to derivatize sulfide and polysulfides into their corresponding dimethyl(poly)sulfides, which are then extracted using solid-phase microextraction in the headspace mode and analysed by gas chromatography-mass spectrometry. Good sensitivity was achieved for the analysis of dimethyl(poly)sulfides, with detection limits ranging from 50 to 240 ng L(-1). The method also demonstrated good precision (repeatability: 3-7%) and good linearity over two orders of magnitude. Matrix effects from raw drinking water containing organic carbon (3.8 mg L(-1)) and from sediment material from a drinking water distribution system were shown to have no interferences in the analysis of dimethyl(poly)sulfides. The method provides a rapid, robust, and reliable mean to analyse trace levels of sulfides and polysulfides in aqueous systems. The new method described here is more accessible and user-friendly than methods based on closed-loop stripping analysis, which have been traditionally used for the analysis of these compounds. The optimised method was used to analyse samples collected

  13. Pressurized liquid extraction-gas chromatography-mass spectrometry analysis of fragrance allergens, musks, phthalates and preservatives in baby wipes.

    Science.gov (United States)

    Celeiro, Maria; Lamas, J Pablo; Garcia-Jares, Carmen; Llompart, Maria

    2015-03-06

    Baby wipes and wet toilet paper are specific hygiene care daily products used on newborn and children skin. These products may contain complexes mixtures of harmful chemicals. A method based on pressurized liquid extraction (PLE) followed by gas chromatography-mass spectrometry (GC-MS) has been developed for the simultaneous determination of sixty-five chemical compounds (fragrance allergens, preservatives, musks, and phthalates) in wipes and wet toilet paper for children. These compounds are legislated in Europe according Regulation EC No 1223/2009, being twelve of them banned for their use in cosmetics, and one of them, 3-iodo-2-propynyl butylcarbamate (IPBC), is banned in products intended for children under 3 years. Also, propyl-, and butylparaben will be prohibited in leave-on cosmetic products designed for application on the nappy area of children under 3 years from April 2015. PLE is a fast, simple, easily automated technique, which permits to integrate a clean-up step during the extraction process reducing analysis time and stages. The proposed PLE-based procedure was optimized on real non-spiked baby wipe samples by means of experimental design to study the influence on extraction of parameters such as extraction solvent, temperature, extraction time, and sorbent type. Under the selected conditions, the method was validated showing satisfactory linearity, and intra-day, and inter-day precision. Recoveries were between 80-115% for most of the compounds with relative standard deviations (RSD) lower than 15%. Finally, twenty real samples were analyzed. Thirty-six of the target analytes were detected, highlighting the presence of phenoxyethanol in all analyzed samples at high concentration levels (up to 0.8%, 800μgg(-1)). Methyl paraben (MeP), and ethyl paraben (EtP) were found in 40-50% of the samples, and the recently banned isobutyl paraben (iBuP) and isopropyl paraben (iPrP), were detected in one and seven samples, respectively, at concentrations between

  14. Determination of "new psychoactive substances" in postmortem matrices using microwave derivatization and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Margalho, Cláudia; Castanheira, Alice; Real, Francisco Corte; Gallardo, Eugenia; López-Rivadulla, Manuel

    2016-05-01

    Despite worldwide efforts aiming to ban the marketing and subsequent abuse of psychoactive substances such as synthetic cathinones and phenethylamines, there has been an alarming growth of both in recent years. Different compounds similar to those already existing are continuously appearing in the market in order to circumvent the legislation. An analytical methodology has been validated for qualitative and quantitative determinations of D-cathine (D-norpseudoehedrine), ephedrine, methcathinone, 1-(4-methoxyphenyl)-propan-2-amine (PMA), mephedrone, methedrone, 2,5-dimethoxy-4-methylamphetamine (DOM), 4-bromo-2,5-dimethoxyamphetamine (DOB), 2,5-dimethoxyphenethylamine (2C-H), 4-bromo-2,5-dimethoxyphenethylamine (2C-B), 4-iodo-2,5-dimethoxyphenethylamine (2C-I), 2-[2,5-dimethoxy-4-(ethylthio)phenyl]ethanamine (2C-T-2), 2,5-dimethoxy-4-isopropylthiophenethylamine (2C-T-4) and 2-[2,5-dimethoxy-4-(propylthio)phenyl]ethanamine (2C-T-7), in low volumes of vitreous humor (100 μL), pericardial fluid (250 μL) and whole blood (250 μL), using deutered amphetamine, ephedrine and mephedrone as internal standards. The validation parameters included selectivity, linearity and limits of detection and quantification, intra- and interday precision and trueness, recovery and stability. The method included mixed-mode solid phase extraction, followed by microwave fast derivatization and analysis by gas chromatography-mass spectrometry operated in selected ion monitoring mode. The procedure was linear between 5 and 600 ng/mL, with determination coefficients higher than 0.99 for all analytes. Intra- and interday precision ranged from 0.1 to 13.6%, while accuracy variability was within 80-120% interval from the nominal concentration at all studied levels. The extraction efficiencies ranged from 76.6 to 112.8%. Stability was considered acceptable for all compounds in the studied matrices. The developed assay was applied to authentic samples of the Laboratory of Chemistry and Forensic

  15. Unsupervised classification of petroleum Certified Reference Materials and other fuels by chemometric analysis of gas chromatography-mass spectrometry data.

    Science.gov (United States)

    de Carvalho Rocha, Werickson Fortunato; Schantz, Michele M; Sheen, David A; Chu, Pamela M; Lippa, Katrice A

    2017-06-01

    As feedstocks transition from conventional oil to unconventional petroleum sources and biomass, it will be necessary to determine whether a particular fuel or fuel blend is suitable for use in engines. Certifying a fuel as safe for use is time-consuming and expensive and must be performed for each new fuel. In principle, suitability of a fuel should be completely determined by its chemical composition. This composition can be probed through use of detailed analytical techniques such as gas chromatography-mass spectroscopy (GC-MS). In traditional analysis, chromatograms would be used to determine the details of the composition. In the approach taken in this paper, the chromatogram is assumed to be entirely representative of the composition of a fuel, and is used directly as the input to an algorithm in order to develop a model that is predictive of a fuel's suitability. When a new fuel is proposed for service, its suitability for any application could then be ascertained by using this model to compare its chromatogram with those of the fuels already known to be suitable for that application. In this paper, we lay the mathematical and informatics groundwork for a predictive model of hydrocarbon properties. The objective of this work was to develop a reliable model for unsupervised classification of the hydrocarbons as a prelude to developing a predictive model of their engine-relevant physical and chemical properties. A set of hydrocarbons including biodiesel fuels, gasoline, highway and marine diesel fuels, and crude oils was collected and GC-MS profiles obtained. These profiles were then analyzed using multi-way principal components analysis (MPCA), principal factors analysis (PARAFAC), and a self-organizing map (SOM), which is a kind of artificial neural network. It was found that, while MPCA and PARAFAC were able to recover descriptive models of the fuels, their linear nature obscured some of the finer physical details due to the widely varying composition of the

  16. A dynamic programming approach for the alignment of signal peaks in multiple gas chromatography-mass spectrometry experiments

    Directory of Open Access Journals (Sweden)

    McConville Malcolm J

    2007-10-01

    Full Text Available Abstract Background Gas chromatography-mass spectrometry (GC-MS is a robust platform for the profiling of certain classes of small molecules in biological samples. When multiple samples are profiled, including replicates of the same sample and/or different sample states, one needs to account for retention time drifts between experiments. This can be achieved either by the alignment of chromatographic profiles prior to peak detection, or by matching signal peaks after they have been extracted from chromatogram data matrices. Automated retention time correction is particularly important in non-targeted profiling studies. Results A new approach for matching signal peaks based on dynamic programming is presented. The proposed approach relies on both peak retention times and mass spectra. The alignment of more than two peak lists involves three steps: (1 all possible pairs of peak lists are aligned, and similarity of each pair of peak lists is estimated; (2 the guide tree is built based on the similarity between the peak lists; (3 peak lists are progressively aligned starting with the two most similar peak lists, following the guide tree until all peak lists are exhausted. When two or more experiments are performed on different sample states and each consisting of multiple replicates, peak lists within each set of replicate experiments are aligned first (within-state alignment, and subsequently the resulting alignments are aligned themselves (between-state alignment. When more than two sets of replicate experiments are present, the between-state alignment also employs the guide tree. We demonstrate the usefulness of this approach on GC-MS metabolic profiling experiments acquired on wild-type and mutant Leishmania mexicana parasites. Conclusion We propose a progressive method to match signal peaks across multiple GC-MS experiments based on dynamic programming. A sensitive peak similarity function is proposed to balance peak retention time and peak

  17. Determination of chlorobenzenes in textiles by pressurized hot water extraction followed by vortex-assisted liquid-liquid microextraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Lu, Yang; Zhu, Yan

    2013-12-06

    A method for quantitative determination of chlorobenzenes in textiles is developed, using pressurized hot water extraction (PHWE), vortex-assisted liquid-liquid microextraction (VALLME) and gas chromatography-mass spectrometry (GC-MS). VALLME serves as a trapping step after PHWE. The extraction conditions are investigated, as well as the quantitative features such as linearity, limits of detection (LODs), limits of quantification (LOQs), repeatabilities and reproducibilities between days. LOQs of 0.018-0.032mg/kg were achieved. The present method provides good repeatabilities (RSDtextiles. Copyright © 2013 Elsevier B.V. All rights reserved.

  18. Different Analytical Procedures for the Study of Organic Residues in Archeological Ceramic Samples with the Use of Gas Chromatography-mass Spectrometry.

    Science.gov (United States)

    Kałużna-Czaplińska, Joanna; Rosiak, Angelina; Kwapińska, Marzena; Kwapiński, Witold

    2016-01-01

    The analysis of the composition of organic residues present in pottery is an important source of information for historians and archeologists. Chemical characterization of the materials provides information on diets, habits, technologies, and original use of the vessels. This review presents the problem of analytical studies of archeological materials with a special emphasis on organic residues. Current methods used in the determination of different organic compounds in archeological ceramics are presented. Particular attention is paid to the procedures of analysis of archeological ceramic samples used before gas chromatography-mass spectrometry. Advantages and disadvantages of different extraction methods and application of proper quality assurance/quality control procedures are discussed.

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

    OpenAIRE

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

    2016-01-01

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

  20. Dynamic solid phase microextraction for sampling of airborne sarin with gas chromatography-mass spectrometry for rapid field detection and quantification.

    Science.gov (United States)

    Hook, Gary L; Jackson Lepage, Carmela; Miller, Stephen I; Smith, Philip A

    2004-08-01

    A portable dynamic air sampler and solid phase microextraction were used to simultaneously detect, identify, and quantify airborne sarin with immediate analysis of samples using a field portable gas chromatography-mass spectrometry system. A mathematical model was used with knowledge of the mass of sarin trapped, linear air velocity past the exposed sampling fiber, and sample duration allowing calculation of concentration estimates. For organizations with suitable field portable instrumentation, these methods are potentially useful for rapid onsite detection and quantification of high concern analytes, either through direct environmental sampling or through sampling of air collected in bags.

  1. [Combined use of tandem mass spectrometry with urine gas chromatography/mass spectrometry is useful for diagnosis of inborn errors of metabolism in children].

    Science.gov (United States)

    Xie, Li-Juan; Zhu, Jian-Xing; Zhu, Xiao-Dong; Li, Hua-Jun; Han, Lian-Shu; Gu, Xue-Fan

    2008-02-01

    Many inborn errors of metabolism have similar presenting clinical manifestations, making early diagnosis difficult. We report our experience with tandem mass spectrometry combined with urine gas chromatography/mass spectrometry as a means of definitively diagnosing inborn errors of metabolism. One hundred and thirty-two children with suspected inborn errors of metabolism but without specific clinical manifestations, admitted to the Xinhua Hospital Affiliated to Shanghai Jiaotong University School of Medicine between June 1, 2003 and September 30, 2006, were studied. Children received routine biochemical examinations, as well as mass spectrometry and gas chromatography-mass spectrometry. Fifteen cases (11.5%) were confirmed as having inborn errors of metabolism, including 6 cases of methylmalonic acidemia, 2 of propionic academia, 2 of Type II citrullinemia, 1 of biotinidase deficiency, 1 of tyrosinemia, 1 of maple syrup urine disease, 1 of omithine transcarbamylase deficiency and 1 of very long chain Acyl CoA dehydrogenase deficiency. The combined use of tandem mass spectrometry with urine gas chromatography mass spectrometry is useful for early diagnosis of inborn errors of metabolism in children with suspected inborn errors of metabolism but without specific clinical manifestations.

  2. Analysis of pharmaceutical and other organic wastewater compounds in filtered and unfiltered water samples by gas chromatography/mass spectrometry

    Science.gov (United States)

    Zaugg, Steven D.; Phillips, Patrick J.; Smith, Steven G.

    2014-01-01

    Research on the effects of exposure of stream biota to complex mixtures of pharmaceuticals and other organic compounds associated with wastewater requires the development of additional analytical capabilities for these compounds in water samples. Two gas chromatography/mass spectrometry (GC/MS) analytical methods used at the U.S. Geological Survey National Water Quality Laboratory (NWQL) to analyze organic compounds associated with wastewater were adapted to include additional pharmaceutical and other organic compounds beginning in 2009. This report includes a description of method performance for 42 additional compounds for the filtered-water method (hereafter referred to as the filtered method) and 46 additional compounds for the unfiltered-water method (hereafter referred to as the unfiltered method). The method performance for the filtered method described in this report has been published for seven of these compounds; however, the addition of several other compounds to the filtered method and the addition of the compounds to the unfiltered method resulted in the need to document method performance for both of the modified methods. Most of these added compounds are pharmaceuticals or pharmaceutical degradates, although two nonpharmaceutical compounds are included in each method. The main pharmaceutical compound classes added to the two modified methods include muscle relaxants, opiates, analgesics, and sedatives. These types of compounds were added to the original filtered and unfiltered methods largely in response to the tentative identification of a wide range of pharmaceutical and other organic compounds in samples collected from wastewater-treatment plants. Filtered water samples are extracted by vacuum through disposable solid-phase cartridges that contain modified polystyrene-divinylbenzene resin. Unfiltered samples are extracted by using continuous liquid-liquid extraction with dichloromethane. The compounds of interest for filtered and unfiltered sample

  3. Determination of heat purgeable and ambient purgeable volatile organic compounds in water by gas chromatography/mass spectrometry

    Science.gov (United States)

    Rose, Donna L.; Sandstrom, Mark W.; Murtagh, Lucinda K.

    2016-09-08

    Two new analytical methods have been developed by the U.S. Geological Survey (USGS) National Water Quality Laboratory (NWQL) that allow the determination of 37 heat purgeable volatile organic compounds (VOCs) (USGS Method O-4437-16 [NWQL Laboratory Schedule (LS) 4437]) and 49 ambient purgeable VOCs (USGS Method O-4436-16 [NWQL LS 4436]) in unfiltered water. This report documents the procedures and initial performance of both methods. The compounds chosen for inclusion in the methods were determined as having high priority by the USGS National Water-Quality Assessment (NAWQA) Program. Both methods use a purge-and-trap technique with gas chromatography/mass spectrometry. The compounds are extracted from the sample by bubbling helium through a 25-milliliter sample. For the polar and less volatile compounds, the sample is heated at 60 degrees Celsius, whereas the less polar and more volatile compounds are purged using a separate analytical procedure at ambient temperature. The compounds are trapped on a sorbent trap, desorbed into a gas chromatograph/mass spectrometer for separation, and then identified and quantified. Sample preservation is recommended for both methods by adding a 1:1 solution of hydrochloric acid (HCl [1:1]) to water samples to adjust the pH to 2. Analysis within 14 days from sampling is recommended.The heat purgeable method (USGS Method O-4437-16) operates with the mass spectrometer in the simultaneous full scan/selected ion monitoring mode. This method supersedes USGS Method O-4024-03 (NWQL LS 4024). Method detection limits (MDLs) for fumigant compounds 1,2-dibromoethane, 1,2-dichloropropane, 1,2,3-trichloropropane, chloropicrin, and 1,2-dibromo-3-chloropropane range from 0.002 to 0.010 microgram per liter (µg/L). The MDLs for all remaining heat purgeable VOCs range from 0.006 µg/L for tert-butyl methyl ether to 3 µg/L for alpha-terpineol. Calculated holding times indicate that 36 of the 37 heat purgeable VOCs are stable for a minimum of 14 days

  4. Chapter 3. Determination of semivolatile organic compounds and polycyclic aromatic hydrocarbons in solids by gas chromatography/mass spectrometry

    Science.gov (United States)

    Zaugg, Steven D.; Burkhardt, Mark R.; Burbank, Teresa L.; Olson, Mary C.; Iverson, Jana L.; Schroeder, Michael P.

    2006-01-01

    A method for the determination of 38 polycyclic aromatic hydrocarbons (PAHs) and semivolatile organic compounds in solid samples is described. Samples are extracted using a pressurized solvent extraction system. The compounds of interest are extracted from the solid sample twice at 13,800 kilopascals; first at 120 degrees Celsius using a water/isopropyl alcohol mixture (50:50, volume-to-volume ratio), and then the sample is extracted at 200 degrees Celsius using a water/isopropyl alcohol mixture (80:20, volume-to-volume ratio). The compounds are isolated using disposable solid-phase extraction (SPE) cartridges containing divinylbenzene-vinylpyrrolidone copolymer resin. The cartridges are dried with nitrogen gas, and then sorbed compounds are eluted from the SPE material using a dichloromethane/diethyl ether mixture (80:20, volume-to-volume ratio) and passed through a sodium sulfate/Florisil SPE cartridge to remove residual water and to further clean up the extract. The concentrated extract is solvent exchanged into ethyl acetate and the solvent volume reduced to 0.5 milliliter. Internal standard compounds are added prior to analysis by capillary-column gas chromatography/mass spectrometry. Comparisons of PAH data for 28 sediment samples extracted by Soxhlet and the accelerated solvent extraction (ASE) method described in this report produced similar results. Extraction of PAH compounds from standard reference material using this method also compared favorably with Soxhlet extraction. The recoveries of PAHs less than molecular weight 202 (pyrene or fluoranthene) are higher by up to 20 percent using this ASE method, whereas the recoveries of PAHs greater than or equal to molecular weight 202 are equivalent. This ASE method of sample extraction of solids has advantages over conventional Soxhlet extraction by increasing automation of the extraction process, reducing extraction time, and using less solvent. Extract cleanup also is greatly simplified because SPE replaces

  5. Giant tunability of the two-dimensional electron gas at the interface of γ-Al2O3/SrTiO3

    DEFF Research Database (Denmark)

    Niu, Wei; Zhang, Yu; Gan, Yulin

    2017-01-01

    a dielectric solid insulator, i.e. in the configuration of conventional field-effect transistors. To surpass this long-standing limit, we used ionic liquids as the dielectric layer for electrostatic gating of oxide interfaces in an electric double layer transistor (EDLT) configuration. Herein, we reported......Two-dimensional electron gases (2DEGs) formed at the interface between two oxide insulators provide a rich platform for the next generation of electronic devices. However, their high carrier density makes it rather challenging to control the interface properties under a low electric field through...

  6. TWO-DIMENSIONAL TOPOLOGY OF COSMOLOGICAL REIONIZATION

    International Nuclear Information System (INIS)

    Wang, Yougang; Xu, Yidong; Chen, Xuelei; Park, Changbom; Kim, Juhan

    2015-01-01

    We study the two-dimensional topology of the 21-cm differential brightness temperature for two hydrodynamic radiative transfer simulations and two semi-numerical models. In each model, we calculate the two-dimensional genus curve for the early, middle, and late epochs of reionization. It is found that the genus curve depends strongly on the ionized fraction of hydrogen in each model. The genus curves are significantly different for different reionization scenarios even when the ionized faction is the same. We find that the two-dimensional topology analysis method is a useful tool to constrain the reionization models. Our method can be applied to the future observations such as those of the Square Kilometre Array

  7. Dirac cones in two-dimensional borane

    Science.gov (United States)

    Martinez-Canales, Miguel; Galeev, Timur R.; Boldyrev, Alexander I.; Pickard, Chris J.

    2017-11-01

    We introduce two-dimensional borane, a single-layered material of BH stoichiometry, with promising electronic properties. We show that, according to density functional theory calculations, two-dimensional borane is semimetallic, with two symmetry-related Dirac cones meeting right at the Fermi energy Ef. The curvature of the cones is lower than in graphene, thus closer to the ideal linear dispersion. Its structure, formed by a puckered trigonal boron network with hydrogen atoms connected to each boron atom, can be understood as distorted, hydrogenated borophene [Mannix et al., Science 350, 1513 (2015), 10.1126/science.aad1080]. Chemical bonding analysis reveals the boron layer in the network being bound by delocalized four-center two-electron σ bonds. Finally, we suggest high pressure could be a feasible route to synthesize two-dimensional borane.

  8. Two-dimensional x-ray diffraction

    CERN Document Server

    He, Bob B

    2009-01-01

    Written by one of the pioneers of 2D X-Ray Diffraction, this useful guide covers the fundamentals, experimental methods and applications of two-dimensional x-ray diffraction, including geometry convention, x-ray source and optics, two-dimensional detectors, diffraction data interpretation, and configurations for various applications, such as phase identification, texture, stress, microstructure analysis, crystallinity, thin film analysis and combinatorial screening. Experimental examples in materials research, pharmaceuticals, and forensics are also given. This presents a key resource to resea

  9. Analysis of Mixed Aryl/Alkyl Esters by Pyrolysis Gas Chromatography-Mass Spectrometry in the Presence of Perchlorate

    Science.gov (United States)

    Burton, A. S.; Locke, D. R.; Lewis, E. K.

    2017-01-01

    Mars is an important target for Astrobiology. A key goal of the MSL mission was to determine whether Mars was habitable in the past, a que-tion that has now been definitely determined to be yes. Another key goal for Mars exploration is to understand the origin and distribution of organic material on Mars; this question is being addressed by the SAM instrument on MSL, and will also be informed by two upcoming Mars exploration missions, ExoMars and Mars 2020. These latter two missions have instrumentation capable of detecting and characterize organic molecules. Over the next decade, these missions will analyze organics in surface, near-surface and sub-surface samples. Each mission has the capability to analyze organics by different methods (pyrolysis gas chromatography-mass spectrometry [py-GC-MS]; laser desorption and thermal volatilization GC-MS; and Raman spectroscopy). Plausibly extraterrestrial organics were recently discovered by the Mars Science Laboratory (MSL), providing an important first step towards understanding the organic inventory on Mars [1]. The compounds detected were chlorobenzenes and chloroalkanes, but it was argued that chlorination of these compounds occurred during pyrolysis of samples containing unchlorinated organics in the presence of perchlorate. A recent report analyzed a suite of aromatic (benzene, toluene, benzoic acid, phthalic acid, and mellitic acid) and aliphatic (acetic acid, propane, propanol, and hexane) by pyrolysis under SAM-like conditions in the presence of perchlorate to attempt to constrain possible precursor molecules for the organic molecules detected on Mars. For aromatic compounds, the aromatic acids all readily produced SAM-relevant chlorobenzes, whereas benzene and toluene did not. This observation suggests that the chlorobenzene detected on Mars could have derived from compounds like mellitic acid, consistent with the previous hypothesis by Benner et al. [3]. Among the aliphatic molecules, it was shown that

  10. Dipolar vortices in two-dimensional flows

    DEFF Research Database (Denmark)

    Juul Rasmussen, J.; Hesthaven, J.S.; Lynov, Jens-Peter

    1996-01-01

    The dynamics of dipolar vortex solutions to the two-dimensional Euler equations is studied. A new type of nonlinear dipole is found and its dynamics in a slightly viscous system is compared with the dynamics of the Lamb dipole. The evolution of dipolar structures from an initial turbulent patch...

  11. Analytical simulation of two dimensional advection dispersion ...

    African Journals Online (AJOL)

    The study was designed to investigate the analytical simulation of two dimensional advection dispersion equation of contaminant transport. The steady state flow condition of the contaminant transport where inorganic contaminants in aqueous waste solutions are disposed of at the land surface where it would migrate ...

  12. Analytical Simulation of Two Dimensional Advection Dispersion ...

    African Journals Online (AJOL)

    ADOWIE PERE

    ABSTRACT: The study was designed to investigate the analytical simulation of two dimensional advection dispersion equation of contaminant transport. The steady state flow condition of the contaminant transport where inorganic contaminants in aqueous waste solutions are disposed of at the land surface where it would ...

  13. Two-dimensional position sensitive neutron detector

    Indian Academy of Sciences (India)

    A two-dimensional position sensitive neutron detector has been developed. The detector is a 3He + Kr filled multiwire proportional counter with charge division position readout and has a sensitive area of 345 mm × 345 mm, pixel size 5 mm × 5 mm, active depth 25 mm and is designed for efficiency of 70% for 4 Å neutrons.

  14. Stability of two-dimensional vorticity filaments

    International Nuclear Information System (INIS)

    Elhmaidi, D.; Provenzale, A.; Lili, T.; Babiano, A.

    2004-01-01

    We discuss the results of a numerical study on the stability of two-dimensional vorticity filaments around a circular vortex. We illustrate how the stability of the filaments depends on the balance between the strain associated with the far field of the vortex and the local vorticity of the filament, and we discuss an empirical criterion for filament stability

  15. Two-dimensional membranes in motion

    NARCIS (Netherlands)

    Davidovikj, D.

    2018-01-01

    This thesis revolves around nanomechanical membranes made of suspended two - dimensional materials. Chapters 1-3 give an introduction to the field of 2D-based nanomechanical devices together with an overview of the underlying physics and the measurementtools used in subsequent chapters. The research

  16. Piezoelectricity in Two-Dimensional Materials

    KAUST Repository

    Wu, Tao

    2015-02-25

    Powering up 2D materials: Recent experimental studies confirmed the existence of piezoelectricity - the conversion of mechanical stress into electricity - in two-dimensional single-layer MoS2 nanosheets. The results represent a milestone towards embedding low-dimensional materials into future disruptive technologies. © 2015 Wiley-VCH Verlag GmbH & Co. KGaA.

  17. Sums of two-dimensional spectral triples

    DEFF Research Database (Denmark)

    Christensen, Erik; Ivan, Cristina

    2007-01-01

    We study countable sums of two dimensional modules for the continuous complex functions on a compact metric space and show that it is possible to construct a spectral triple which gives the original metric back. This spectral triple will be finitely summable for any positive parameter. We also co...

  18. A novel two dimensional particle velocity sensor

    NARCIS (Netherlands)

    Pjetri, O.; Wiegerink, Remco J.; Lammerink, Theodorus S.J.; Krijnen, Gijsbertus J.M.

    2013-01-01

    In this paper we present a two wire, two-dimensional particle velocity sensor. The miniature sensor of size 1.0x2.5x0.525 mm, consisting of only two crossed wires, shows excellent directional sensitivity in both directions, thus requiring no directivity calibration, and is relatively easy to

  19. Transient two-dimensional fuel-concentration measurement technique

    Science.gov (United States)

    Konishi, Tadashi; Naka, Syuji; Ito, Akihiko; Saito, Kozo

    1997-11-01

    We propose a nonintrusive experimental technique, the transient fuel-concentration measurement technique (TFMT), that is capable of being used to measure two-dimensional profiles of transient fuel concentrations over an open liquid fuel surface. The TFMT is based on single-wavelength holographic interferometry; its response time is less than 1 s and spatial resolution is 0.1 mol. % /0.1 mm. It was applied to measure both methanol vapor and n-propanol vapor concentrations. To assess the accuracy of the technique, our results were compared with steady-state methanol and n-propanol fuel-vapor concentrations measured by other researchers with a microsampling technique combined with gas chromatography. We found the TFMT to be accurate for on-line monitoring of two-dimensional profiles of fuel-vapor concentrations.

  20. A salting out-acetonitrile homogeneous extraction coupled with gas chromatography-mass spectrometry method for the simultaneous determination of thirteen N-nitrosamines in skin care cosmetics.

    Science.gov (United States)

    Dong, Hao; Guo, Xindong; Xian, Yanping; Luo, Haiying; Wang, Bin; Wu, Yuluan

    2015-11-27

    A sensitive gas chromatography-mass spectrometry method was established for the simultaneous determination of thirteen N-nitrosamines (NAs) in skin care cosmetics. The cosmetics samples were firstly dispersed by water and subsequently extracted and purified using salting out-acetonitrile homogeneous extraction method. Finally, the extracting solution was concentrated by slow nitrogen gas blowing. All of the samples were separated by INNOWAX capillary chromatographic column, and detected by selected ion monitoring (SIM) mode of gas chromatography-mass spectrometry (GC-MS) and quantified by isotope internal standard method. The method was validated for linearity and range, accuracy, precision and sensitivity. Under the optimized condition, the calibration curves were linear over the selected concentration ranges of 2-500μg/L for all the thirteen analytes, with calculated coefficients of determination (R(2)) of greater than 0.996. The limits of detection (LODs) and the limits of quantitation (LOQs) of the method were 3-15μg/kg and 10-50μg/kg, respectively. Recoveries were calculated at three levels of concentration spiked in two kinds of cosmetics (skin care cream and water). The values were found between 93.8% and 121.0% with relative standard deviation (RSD) values of 2.5-7.2% for intra-day precision (n=6) and 3.3-6.7% for inter-day precision (n=5). The method was successfully applied to analyze twenty-two cosmetics samples and N-nitrosodimethylamine (NDMA) was detected in one sample with the concentration of 207μg/kg. Copyright © 2015 Elsevier B.V. All rights reserved.

  1. Two-dimensional sensitivity calculation code: SENSETWO

    International Nuclear Information System (INIS)

    Yamauchi, Michinori; Nakayama, Mitsuo; Minami, Kazuyoshi; Seki, Yasushi; Iida, Hiromasa.

    1979-05-01

    A SENSETWO code for the calculation of cross section sensitivities with a two-dimensional model has been developed, on the basis of first order perturbation theory. It uses forward neutron and/or gamma-ray fluxes and adjoint fluxes obtained by two-dimensional discrete ordinates code TWOTRAN-II. The data and informations of cross sections, geometry, nuclide density, response functions, etc. are transmitted to SENSETWO by the dump magnetic tape made in TWOTRAN calculations. The required input for SENSETWO calculations is thus very simple. The SENSETWO yields as printed output the cross section sensitivities for each coarse mesh zone and for each energy group, as well as the plotted output of sensitivity profiles specified by the input. A special feature of the code is that it also calculates the reaction rate with the response function used as the adjoint source in TWOTRAN adjoint calculation and the calculated forward flux from the TWOTRAN forward calculation. (author)

  2. Two-dimensional ranking of Wikipedia articles

    Science.gov (United States)

    Zhirov, A. O.; Zhirov, O. V.; Shepelyansky, D. L.

    2010-10-01

    The Library of Babel, described by Jorge Luis Borges, stores an enormous amount of information. The Library exists ab aeterno. Wikipedia, a free online encyclopaedia, becomes a modern analogue of such a Library. Information retrieval and ranking of Wikipedia articles become the challenge of modern society. While PageRank highlights very well known nodes with many ingoing links, CheiRank highlights very communicative nodes with many outgoing links. In this way the ranking becomes two-dimensional. Using CheiRank and PageRank we analyze the properties of two-dimensional ranking of all Wikipedia English articles and show that it gives their reliable classification with rich and nontrivial features. Detailed studies are done for countries, universities, personalities, physicists, chess players, Dow-Jones companies and other categories.

  3. Two-dimensional confinement of heavy fermions

    International Nuclear Information System (INIS)

    Shishido, Hiroaki; Shibauchi, Takasada; Matsuda, Yuji; Terashima, Takahito

    2010-01-01

    Metallic systems with the strongest electron correlations are realized in certain rare-earth and actinide compounds whose physics are dominated by f-electrons. These materials are known as heavy fermions, so called because the effective mass of the conduction electrons is enhanced via correlation effects up to as much as several hundreds times the free electron mass. To date the electronic structure of all heavy-fermion compounds is essentially three-dimensional. Here we report on the first realization of a two-dimensional heavy-fermion system, where the dimensionality is adjusted in a controllable fashion by fabricating heterostructures using molecular beam epitaxy. The two-dimensional heavy fermion system displays striking deviations from the standard Fermi liquid low-temperature electronic properties. (author)

  4. Toward two-dimensional search engines

    International Nuclear Information System (INIS)

    Ermann, L; Shepelyansky, D L; Chepelianskii, A D

    2012-01-01

    We study the statistical properties of various directed networks using ranking of their nodes based on the dominant vectors of the Google matrix known as PageRank and CheiRank. On average PageRank orders nodes proportionally to a number of ingoing links, while CheiRank orders nodes proportionally to a number of outgoing links. In this way, the ranking of nodes becomes two dimensional which paves the way for the development of two-dimensional search engines of a new type. Statistical properties of information flow on the PageRank–CheiRank plane are analyzed for networks of British, French and Italian universities, Wikipedia, Linux Kernel, gene regulation and other networks. A special emphasis is done for British universities networks using the large database publicly available in the UK. Methods of spam links control are also analyzed. (paper)

  5. Plasmonics with two-dimensional conductors

    Science.gov (United States)

    Yoon, Hosang; Yeung, Kitty Y. M.; Kim, Philip; Ham, Donhee

    2014-01-01

    A wealth of effort in photonics has been dedicated to the study and engineering of surface plasmonic waves in the skin of three-dimensional bulk metals, owing largely to their trait of subwavelength confinement. Plasmonic waves in two-dimensional conductors, such as semiconductor heterojunction and graphene, contrast the surface plasmonic waves on bulk metals, as the former emerge at gigahertz to terahertz and infrared frequencies well below the photonics regime and can exhibit far stronger subwavelength confinement. This review elucidates the machinery behind the unique behaviours of the two-dimensional plasmonic waves and discusses how they can be engineered to create ultra-subwavelength plasmonic circuits and metamaterials for infrared and gigahertz to terahertz integrated electronics. PMID:24567472

  6. Optimization for Decocting Later of Menthae Herba in Eungyo-San, a Herbal Formula, Using Response Surface Methodology with Gas Chromatography/Mass Spectrometry.

    Science.gov (United States)

    Ha, Woo-Ram; Park, Jin-Hyung; Kim, Jung-Hoon

    2018-01-01

    "Decocting later" is important procedure for the extraction of herbal medicines containing volatile compounds. This study was performed to investigate optimal conditions for "Decocting later" of Menthae herba in Eungyo-san (EGS) and correlation between extraction variables and the yields of d/l-menthol, a marker compound of Menthae herba. The decocting temperature, total decocting time, and decocting later time were chosen as individual variables, and the yield of d/l-menthol was set as the response value which were calculated by using a Box-Behnken design (BBD). The amount of d/l-menthol was quantified using gas chromatography/mass spectrometry. Response surface methodology (RSM) was used to predict optimal conditions for decocting later of Menthae herba into the formula. Optimal conditions for "Decocting later" from RSM were as follows: 100.63°C of decocting temperature; 82.95 min of total decocting time; 19.11 min of decocting later time. Both decocting temperature and total decocting time showed significant correlation with the yield of d/l-menthol. These results suggest that the decocting temperature and total decocting time were influential factors, and RSM can be applied for optimizing the conditions of "Decocting later" of Menthae herba in EGS. Gas chromatography/mass spectrometry method developed was applied to quantify the d/l-menthol, a volatile compound in Menthae Herba, in Eungyo-san decoction (EGS)d/l-Menthol was extracted in the chloroform layer of the partition between EGS decoction and chloroformA Box-Behnken design produced the predicted response values (yield of d/l-menthol in EGS) from the actual response values with individual variables including decocting temperature, total decocting time, and decocting later timeOptimal conditions for "Decocting later" of Menthae Herba in EGS obtained from the response surface methodology were 100.63°C of decocting temperature, 82.95 min of total decocting time, and 19.11 min of decocting later time

  7. Two-dimensional Kagome photonic bandgap waveguide

    DEFF Research Database (Denmark)

    Nielsen, Jens Bo; Søndergaard, Thomas; Libori, Stig E. Barkou

    2000-01-01

    The transverse-magnetic photonic-bandgap-guidance properties are investigated for a planar two-dimensional (2-D) Kagome waveguide configuration using a full-vectorial plane-wave-expansion method. Single-moded well-localized low-index guided modes are found. The localization of the optical modes...... is investigated with respect to the width of the 2-D Kagome waveguide, and the number of modes existing for specific frequencies and waveguide widths is mapped out....

  8. Superintegrability on the two dimensional hyperboloid

    International Nuclear Information System (INIS)

    Akopyan, E.; Pogosyan, G.S.; Kalnins, E.G.; Miller, W. Jr

    1998-01-01

    This work is devoted to the investigation of the quantum mechanical systems on the two dimensional hyperboloid which admit separation of variables in at least two coordinate systems. Here we consider two potentials introduced in a paper of C.P.Boyer, E.G.Kalnins and P.Winternitz, which haven't been studied yet. An example of an interbasis expansion is given and the structure of the quadratic algebra generated by the integrals of motion is carried out

  9. Antiferromagnetism of two-dimensional electronic gas on light-irradiated SrTiO3 and at LaAlO3/SrTiO3 interfaces

    Science.gov (United States)

    Gor'kov, L. P.

    2015-06-01

    To gain an insight into the origin of tunable two-dimensional (2D) electronic liquid at the interfaces of transition-metal oxides, we address properties of a conducting layer on the light-irradiated surfaces of SrTiO3; the energy spectrum of the latter is known and consists of the titanium dxz/dyz and dxy bands. Recently, Santander-Syro et al (2014 Nature Mater. 13 1085) revealed that the dxy bands actually comprise two chiral branches with the Kramers degeneracy at the zone center lifted in the absence of a magnetic moment. We suggest that interacting electrons on the irradiated SrTiO3 go over into a magnetic phase as the result of one of the instabilities of the 2D Fermi liquid with exchange interactions, and point out the concrete antiferromagnetic order parameter. Large energy scales of the order of Fermi energy ∼0.1 eV inherent in this mechanism warrant stability of the magnetic ground state against ever-present effects of disorder. Arguments are given that electrons at the irradiated SrTiO3 surface and at the LaAlO3/SrTiO3 interfaces undergo a kind of first-order transformation into one and the same phase of the 2D electronic Fermi liquid with reduced magnetic symmetry.

  10. Two-Dimensional Electron System in Electromagnetic Radiation Field

    Science.gov (United States)

    Lungu, Radu Paul; Manolescu, Andrei

    We consider a two-dimensional electron gas in the presence of a monochromatic linear polarized electromagnetic field, within the Floquet formalism. The Floquet states have a simple relation with the energy eigenstates in the absence of the field. Therefore the single-particle and the two-particle Green functions of the many-body system with Coulomb interactions, in the radiation field, can be formally calculated by the standard diagrammatic techniques, as for the conservative system. We derive the elementary excitations of quasi-particle type, the plasma dispersion relation, and the ground state quasi-energy, and we relate them to the corresponding results for the conservative system.

  11. Quantum wells physics and electronics of two-dimensional systems

    CERN Document Server

    Shik, A

    1998-01-01

    This invaluable book is devoted to the physics, technology and device applications of semiconductor structures with ultrathin layers where the electronic properties are governed by the quantum-mechanical laws. Such structures called quantum wells or structures with the two-dimensional electron gas, have become one of the most actively investigated objects in modern solid state physics. Electronic properties of quantum wells differ dramatically from those of bulk semiconductors, which allows one to observe new types of physical phenomena, such as the quantum Hall effect and many other so-far-un

  12. Two-dimensional Bose and Fermi gases beyond weak coupling

    Science.gov (United States)

    França, Guilherme; LeClair, André; Squires, Joshua

    2017-07-01

    Using a formalism based on the two-body S-matrix we study two-dimensional Bose and Fermi gases with both attractive and repulsive interactions. Approximate analytic expressions, valid at weak coupling and beyond, are developed and applied to the Berezinskii-Kosterlitz-Thouless (BKT) transition. We successfully recover the correct logarithmic functional form of the critical chemical potential and density for the Bose gas. For fermions, the BKT critical temperature is calculated in BCS and BEC regimes through consideration of Tan’s contact.

  13. Anisotropic mass density by two-dimensional acoustic metamaterials

    Energy Technology Data Exchange (ETDEWEB)

    Torrent, Daniel; Sanchez-Dehesa, Jose [Wave Phenomena Group, Department of Electronic Engineering, Polytechnic University of Valencia, C/Camino de Vera s/n, E-46022 Valencia (Spain)], E-mail: jsdehesa@upvnet.upv.es

    2008-02-15

    We show that specially designed two-dimensional arrangements of full elastic cylinders embedded in a nonviscous fluid or gas define (in the homogenization limit) a new class of acoustic metamaterials characterized by a dynamical effective mass density that is anisotropic. Here, analytic expressions for the dynamical mass density and the effective sound velocity tensors are derived in the long wavelength limit. Both show an explicit dependence on the lattice filling fraction, the elastic properties of cylinders relative to the background, their positions in the unit cell, and their multiple scattering interactions. Several examples of these metamaterials are reported and discussed.

  14. Magnetism and pairing of two-dimensional trapped fermions.

    Science.gov (United States)

    Chiesa, Simone; Varney, Christopher N; Rigol, Marcos; Scalettar, Richard T

    2011-01-21

    The emergence of local phases in a trapped two-component Fermi gas in an optical lattice is studied using quantum Monte Carlo simulations. We treat temperatures that are comparable to or lower than those presently achievable in experiments and large enough systems that both magnetic and paired phases can be detected by inspection of the behavior of suitable short-range correlations. We use the latter to suggest the interaction strength and temperature range at which experimental observation of incipient magnetism and d-wave pairing are more likely and evaluate the relation between entropy and temperature in two-dimensional confined fermionic systems.

  15. Stopping power of two-dimensional spin quantum electron gases

    Science.gov (United States)

    Zhang, Ya; Jiang, Wei; Yi, Lin

    2015-04-01

    Quantum effects can contribute significantly to the electronic stopping powers in the interactions between the fast moving beams and the degenerate electron gases. From the Pauli equation, the spin quantum hydrodynamic (SQHD) model is derived and used to calculate the stopping power and the induced electron density for protons moving above a two-dimensional (2D) electron gas with considering spin effect under an external in-plane magnetic field. In our calculation, the stopping power is not only modulated by the spin direction, but also varied with the strength of the spin effect. It is demonstrated that the spin effect can obviously enhance or reduce the stopping power of a 2D electron gas within a laboratory magnetic field condition (several tens of Tesla), thus a negative stopping power appears at some specific proton velocity, which implies the protons drain energy from the Pauli gas, showing another significant example of the low-dimensional physics.

  16. Determination of seven pyrethroids biocides and their synergist in indoor air by thermal-desorption gas chromatography/mass spectrometry after sampling on Tenax TA ® passive tubes.

    Science.gov (United States)

    Raeppel, Caroline; Appenzeller, Brice M; Millet, Maurice

    2015-01-01

    A method coupling thermal desorption and gas chromatography/mass spectrometry (GC/MS) was developed for the simultaneous determination of 7 pyrethroids (allethrin, bifenthrin, cyphenothrin, imiprothrin, permethrin, prallethrin and tetramethrin) and piperonyl butoxide adsorbed on Tenax TA(®) passive samplers after exposure in indoor air. Thermal desorption was selected as it permits efficient and rapid extraction without solvent used together with a good sensitivity. Detection (S/N>3) and quantification (S/N>10) limits varied between 0.001 ng and 2.5 ng and between 0.005 and 10 ng respectively with a reproducibility varied between 14% (bifenthrin) and 39% (permethrin). The method was used for the comparison indoor air contamination after low-pressure spraying and fumigation application in a rubbish chute situated in the basement of a building. Copyright © 2014 Elsevier B.V. All rights reserved.

  17. Metabolite profiling of Camellia sinensis by automated sequential, multidimensional gas chromatography/mass spectrometry reveals strong monsoon effects on tea constituents.

    Science.gov (United States)

    Kowalsick, Amanda; Kfoury, Nicole; Robbat, Albert; Ahmed, Selena; Orians, Colin; Griffin, Timothy; Cash, Sean B; Stepp, John Richard

    2014-11-28

    Seasonal variation in tea (Camellia sinensis (L.) Kuntze; Theaceae) chemistry was investigated using automated sequential, multidimensional gas chromatography/mass spectrometry (GC-GC/MS). Metabolite libraries were produced for teas harvested from the Bulang Mountains in Yunnan, China before and after the onset of the East Asian Monsoon. A total of 201 spring and 196 monsoon metabolites were identified, with 169 common and 59 seasonally unique compounds. An additional 163 metabolites were detected but their identity could not be confirmed. Spectral deconvolution of GC/MS data was used to measure the relative concentrations in the teas. Within each family individual metabolite concentrations increased, decreased and stayed the same. The major constituents in both teas were linalool (28%), geraniol (13%), α-terpineol (10%), hotrienol (4%) and nerol (3%). This work provides the foundation to monitor seasonal variations of tea chemistry. Copyright © 2014 Elsevier B.V. All rights reserved.

  18. Gas Chromatography-Mass Spectrometry-Olfactometry To Control the Aroma Fingerprint of Extra Virgin Olive Oil from Three Tunisian Cultivars at Three Harvest Times.

    Science.gov (United States)

    Ben Brahim, Samia; Amanpour, Asghar; Chtourou, Fatma; Kelebek, Hasim; Selli, Serkan; Bouaziz, Mohamed

    2018-03-21

    Gas chromatography-mass spectrometry-olfactometry was used for the analysis of volatile compounds and key odorants of three less studied Tunisian olive oil cultivars for the first time. A total of 42 aroma compounds were identified and quantified in extra virgin olive oils. The present study revealed that the most dominant volatiles in olive oil samples qualitatively and quantitatively were aldehydes and alcohols, followed by terpenes and esters. Indeed, chemometric analysis has shown a correlation between chemical compounds and sensory properties. The determination of aroma-active compounds of olive oil samples was carried out using aroma extract dilution analysis. A total of 15 aroma-active compounds were detected in the aromatic extract of extra virgin olive oil, of which 14 were identified. On the basis of the flavor dilution (FD) factor, the most potent aromatic active compound was hexanal (FD = 512) in Fakhari olive oil, (FD = 256) in Touffehi oils, and (FD = 128) in Jemri olive oil.

  19. Gas chromatography-mass spectrometry determination of the pentafluorobenzoyl derivative of methylhydrazine in false morel (Gyromitra esculenta) as a monitor for the content of the toxin gyromitrin.

    Science.gov (United States)

    Arshadi, Mehrdad; Nilsson, Calle; Magnusson, Bengt

    2006-09-01

    The main toxic compound found in false morel (Gyromitra esculenta) is acetaldehyde-N-methyl-N-formylhydrazone (gyromitrin). This paper describes a method of determining the total hydrazones content based on acid hydrolysis of gyromitrin and other related hydrazones in air-dried false morel followed by derivatisation of methylhydrazine with pentafluorobenzoyl chloride. The derivative, tris-pentafluorobenzoyl methylhydrazine (tris-PFB-MH) is analyzed by gas chromatography-mass spectrometry. The overall precision of the method is better than 10% (relative standard deviation) for 0.5 ng/microl methylhydrazine in solution. The minimum detectable concentration of methylhydrazine (tris-PFB-MH) by this method is estimated to be approximately 12 pg/microl, which is equal to 0.3 microg/g dry matter (DM) of false morel.

  20. Miniaturized hollow fiber assisted liquid-phase microextraction and gas chromatography-mass spectrometry for the measurement of progesterone in human serum.

    Science.gov (United States)

    Kawaguchi, Migaku; Takatsu, Akiko

    2009-01-15

    Miniaturized hollow fiber assisted liquid-phase microextraction (HF-LPME) and gas chromatography-mass spectrometry (GC-MS) for the determination of progesterone in human serum sample is described. The detection limit and the quantification limit of progesterone in human serum sample are 0.5 and 2 ng mL(-1) (ppb), respectively. The calibration curve for progesterone is linear with a correlation coefficient of >0.999 in the range of 2-500 ng mL(-1). The average recoveries of progesterone in human serum samples spiked with 5, 50 and 200 ng mL(-1) progesterone are 97.4% (R.S.D.: 9.3%), 100.3% (R.S.D.: 4.7%) and 99.8% (R.S.D.: 3.4%), respectively. This simple, accurate, sensitive and selective analytical method can be applicable for the determination of progesterone in human serum samples.