Relationship of Ambient Atmosphere and Biological Aerosol Responses from a Fielded Pyrolysis-Gas Chromatography-Ion Mobility Spectrometry Bioanalytical Detector

National Research Council Canada - National Science Library

Snyder, A

2003-01-01

.... A pyrolysis-gas chromatography-ion mobility spectrometry stand-alone bioaerosol system was interfaced to an aerosol concentrator to collect ambient background aerosols and produce bioanalytical...

Recent applications of gas chromatography with high-resolution mass spectrometry.

Science.gov (United States)

Špánik, Ivan; Machyňáková, Andrea

2018-01-01

Gas chromatography coupled to high-resolution mass spectrometry is a powerful analytical method that combines excellent separation power of gas chromatography with improved identification based on an accurate mass measurement. These features designate gas chromatography with high-resolution mass spectrometry as the first choice for identification and structure elucidation of unknown volatile and semi-volatile organic compounds. Gas chromatography with high-resolution mass spectrometry quantitative analyses was previously focused on the determination of dioxins and related compounds using magnetic sector type analyzers, a standing requirement of many international standards. The introduction of a quadrupole high-resolution time-of-flight mass analyzer broadened interest in this method and novel applications were developed, especially for multi-target screening purposes. This review is focused on the development and the most interesting applications of gas chromatography coupled to high-resolution mass spectrometry towards analysis of environmental matrices, biological fluids, and food safety since 2010. The main attention is paid to various approaches and applications of gas chromatography coupled to high-resolution mass spectrometry for non-target screening to identify contaminants and to characterize the chemical composition of environmental, food, and biological samples. The most interesting quantitative applications, where a significant contribution of gas chromatography with high-resolution mass spectrometry over the currently used methods is expected, will be discussed as well. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Pyrolysis-gas chromatography-mass spectrometry for studying N-vinyl-2-pyrrolidone-co-vinyl acetate copolymers and their dissolution behaviour.

Science.gov (United States)

Chojnacka, Aleksandra; Ghaffar, Abdul; Feilden, Andrew; Treacher, Kevin; Janssen, Hans-Gerd; Schoenmakers, Peter

2011-11-14

Knowledge on the solubility behaviour and dissolution rate of speciality and commodity polymers is very important for the use of such materials in high-tech applications. We have developed methods for the quantification and characterization of dissolved copolymers of N-vinyl-2-pyrrolidone (VP) and vinyl acetate (VA) during dissolution in water. The methods are based on pyrolysis (Py) performed in a programmed-temperature vaporization injector with subsequent identification and quantification of the components in the pyrolysate using capillary gas chromatography-mass spectrometry (GC-MS). By injecting large volumes and applying cryo-focussing at the top of the column, low detection limits could be achieved. The monomer ratio was found to have the greatest effect on the dissolution rate of the PVP-co-VA copolymers. The material with the highest amount of VA (50%) dissolves significantly slower than the other grades. Size-exclusion chromatography (SEC) and Py-GC-MS were used to measure molecular weights and average chemical compositions, respectively. Combined off-line SEC//Py-GC-MS was used to determine the copolymer composition (VP/VA ratio), as a function of the molecular weight for the pure polymers. In the dissolution experiments, a constant VP/VA ratio across the dissolution curve was observed for all copolymers analysed. This suggests a random distribution of the two monomers over the molecules. Copyright © 2011 Elsevier B.V. All rights reserved.

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.

New approach to the characterization of pyrolysis coal products by gas chromatography mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Cappiello, A.; Mangani, F.; Bruner, F.; Bonfanti, L. [University of Urbino, Urbino (Italy)

1996-06-07

A method for the characterization of coal thermal behaviour, based on gas chromatographic-mass spectrometric analysis of the pyrolysate, is presented. Twelve different coal samples representative of the entire coal rank, were selected. The pyrolysis products, obtained at 800{degree}C, were first collected and then analysed in two GC-MS systems. The sampling apparatus consisted of three different traps in order to separate the products into three fractions on the basis of their volatility. The GC-MS analysis was also arranged according to this criterion. A packed column, coupled to a double-focusing magnetic mass spectrometer, was used for the volatile fractions of the pyrolysate and a capillary column, coupled to a quadruple analyser, was employed for the analysis of the condensed fraction. Sampling and analysis procedures were carried out separately, thus allowing careful optimization of the strategy for the characterization of the pyrolysate. The condensate was analysed in the selected-ion monitoring mode for the determination of different classes of compounds. Some evaluations and comparisons, extrapolated from the results obtained, are presented.

The analysis of organic constituents in leaves by pyrolysis-gas chromatography and its application to selected environmental effects on plants

Energy Technology Data Exchange (ETDEWEB)

Zhang, Hongbing

1993-09-01

The relationship between environmental stress and the concentration of certain organic compounds (carbohydrates, tannins and phenolics) in plant leaves is examined. Pyrolysis-gas chromatography-mass spectrometry (PY-GC-MS) can be a rapid and comprehensive method to profile the chemical composition of biomaterials. Enhanced structural information on biomolecules containing acid functional groups can be obtained by a modification of direct pyrolysis; simultaneous pyrolysis methylation (SPM). Initial investigation focused on the characterization of important classes of biomarkers in leaves and optimization of sample preparation and pyrolysis conditions. The pyrolytic techniques were examined as a tool to quantify the compositional changes in leaves of trees which have been subjected to different environmental stresses. Results are reported for three field applications: the effect of thinning on balsam fir trees; the effects of fertilization on kalmia plant; and the effect of ozone on white pine trees. It was found that certain pyrolysates of carbohydrates, tannins and of a dihydrochalcone were good indicators of fertilization and water stress. Two unique pyrolysate biomarkers were discovered in white pine needles as indications of ozone fumigation levels and ozone damage. 132 refs., 33 figs., 13 tabs.

Mass production of chemicals from biomass-derived oil by directly atmospheric distillation coupled with co-pyrolysis

Science.gov (United States)

Zhang, Xue-Song; Yang, Guang-Xi; Jiang, Hong; Liu, Wu-Jun; Ding, Hong-Sheng

2013-01-01

Production of renewable commodity chemicals from bio-oil derived from fast pyrolysis of biomass has received considerable interests, but hindered by the presence of innumerable components in bio-oil. In present work, we proposed and experimentally demonstrated an innovative approach combining atmospheric distillation of bio-oil with co-pyrolysis for mass production of renewable chemicals from biomass, in which no waste was produced. It was estimated that 51.86 wt.% of distillate just containing dozens of separable organic components could be recovered using this approach. Ten protogenetic and three epigenetic compounds in distillate were qualitatively identified by gas chromatography/mass spectrometry and quantified by gas chromatography. Among them, the recovery efficiencies of acetic acid, propanoic acid, and furfural were all higher than 80 wt.%. Formation pathways of the distillate components in this process were explored. This work opens up a fascinating prospect for mass production of chemical feedstock from waste biomass. PMID:23350028

Using Ramped Pyrolysis - Gas Chromatography - Mass Spectrometry to Evaluate Petroleum Hydrocarbons Following the Deepwater Horizon Oil Spill

Science.gov (United States)

Evans, M.; Rosenheim, B. E.; Bacosa, H. P.; Liu, J.; Liu, Z.

2016-02-01

In summer of 2010, the Deepwater Horizon oil spill polluted hundreds of miles of coastline along the Gulf of Mexico. A combination of human-mediated and natural weathering processes then altered the chemical composition (i.e. toxicity) of this spilled crude oil over time and space. One of the most important, yet challenging, aspects of oil spill science is to quantify these chemical changes in natural environments. In this study, we develop ramped pyrolysis - gas chromatography - mass spectrometry (Py-GC-MS) to address this challenge. In this technique, 0.1mg of freeze-dried sample is pyrolyzed over a gradual temperature ramp (50-650°C). The eluded gas is cold-trapped over different thermal ranges (a.k.a. thermal slicing) and each range is individually analyzed via GC-MS, yielding quantifiable, compound-specific results. Py-GC-MS with thermal slicing has never been used for petroleum hydrocarbon analysis, but it has many advantages - it uses minimal sample, is time efficient and does not require sample preparation (minimizing compound loss and increasing the analytical window). During development of this method, we analyzed oiled sediments and tar collected on Grand Isle, Louisiana from 2010-2012. We quantified n-alkane (C10-C38), polycyclic aromatic hydrocarbon (PAH) and hopane content and confirmed these results with traditional solvent extraction, silica gel fractionation and mass spectrometry. Overall, we found rapid depletion of n-alkanes and PAHs (>90% depletion) in all samples within one year of Deepwater Horizon. After this, n-alkanes were almost 100% depleted by 2012, while PAH degradation continued to a maximum total degradation of 99% and 98% in sediment and tar, respectively. This not only describes the fate of petroleum compounds in salt marshes and beach deposits over time, but also complements previous radiocarbon studies of the same samples showing different rates of degradation in different micro-environments. In addition, the results presented

Detailed characterization of bio-oil from pyrolysis of non-edible seed-cakes by Fourier Transform Infrared Spectroscopy (FTIR) and gas chromatography mass spectrometry (GC-MS) techniques.

Science.gov (United States)

Sugumaran, Vatsala; Prakash, Shanti; Ramu, Emmandi; Arora, Ajay Kumar; Bansal, Veena; Kagdiyal, Vivekanand; Saxena, Deepak

2017-07-15

Bio-oil obtained from pyrolysis is highly complicated mixture with valued chemicals. In order to reduce the complexity for unambiguous characterization of components present in bio-oil, solvent extractions using different solvents with increasing polarity have been adopted. The fractions have been analyzed by Fourier transform infrared (FTIR) spectroscopy for identifying the functional groups and Gas chromatography-mass spectrometry (GC-MS), for detailed characterization of components present in various fractions, thereby providing in-depth information at molecular level of various components in bio-oil. This paper reveals the potential of the analytical techniques in identification and brings out the similarities as well as differences in the components present in the bio-oil obtained from two non-edible oil seed-cakes, viz., Jatropha and Karanjia. Copyright © 2017 Elsevier B.V. All rights reserved.

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

Melanoidins-kerogen precursors and geochemical lipid sinks: a study using pyrolysis gas chromatography (PGC)

Energy Technology Data Exchange (ETDEWEB)

Larter, S R; Douglas, A G

1980-12-01

Melanoidins, acidic polymeric products of amino acid/sugar condensation reactions, are shown to be capable of reacting with and binding functionalized lipid molecules. Pyrolysis gas chromatography is used to monitor the inclusion of lipids (alcohols and acids) into, and to monitor the changes in composition caused by artificial diagenesis of, the melanoidins. Artificial diagenesis of the lipid-containing melanoidins produces a material resembling kerogen. The possible role of melanoidins in the formation of krogen is discussed as are internal transformations within kerogens during diagenesis.

Gas Chromatography-Mass Spectrometric Analysis and Insecticidal ...

African Journals Online (AJOL)

HP

Original Research Article. Gas Chromatography-Mass Spectrometric Analysis and ... into a natural fumigant/insecticide for the control of stored product insects. Keywords: Mallotus ..... stability as well as reduce cost. ACKNOWLEDGEMENT.

Pyrolysis-gas chromatography-isotope ratio mass spectrometry for monitoring natural additives in polylactic acid active food packages.

Science.gov (United States)

Llana-Ruíz-Cabello, M; Pichardo, S; Jiménez-Morillo, N T; González-Vila, F J; Guillamón, E; Bermúdez, J M; Aucejo, S; Camean, A M; González-Pérez, J A

2017-11-24

Compound-specific isotope analysis (CSIA) usually requires preparative steps (pretreatments, extraction, derivatization) to get amenable chromatographic analytes from bulk geological, biological or synthetic materials. Analytical pyrolysis (Py-GC/MS) can help to overcome such sample manipulation. This communication describe the results obtained by hyphenating analytical pyrolysis (Py-GC) with carbon isotope-ratio mass spectrometry (IRMS) for the analysis of a polylactic acid (PLA) a based bio-plastic extruded with variable quantities of a natural plant extract or oregano essential oil. The chemical structural information of pyrolysates was first determined by conventional analytical pyrolysis and the measure of δ 13 C in specific compounds was done by coupling a pyrolysis unit to a gas chromatograph connected to a continuous flow IRMS unit (Py-GC-C-IRMS). Using this Py-CSIA device it was possible to trace natural additives with depleted δ 13 C values produced by C3 photosystem vegetation (cymene: -26.7‰±2.52; terpinene: -27.1‰±0.13 and carvacrol: -27.5‰±1.80 from oregano and two unknown structures: -23.3‰±3.32 and -24.4‰±1.70 and butyl valerate: -24.1‰±3.55 from Allium spp.), within the naturally isotopically enriched bio-plastic backbone derived from corn (C4 vegetation) starch (cyclopentanones: -14.2‰±2.11; lactide enantiomers: -9.2‰±1.56 and larger polymeric units: -17.2‰±1.71). This is the first application of Py-CSIA to characterize a bio-plastic and is shown as a promising tool to study such materials, providing not only a fingerprinting, but also valuable information about the origin of the materials, allowing the traceability of additives and minimizing sample preparation. Copyright © 2017 Elsevier B.V. All rights reserved.

Gas Chromatography-Mass Spectrometric Analysis of Nematicidal ...

African Journals Online (AJOL)

Gas Chromatography-Mass Spectrometric Analysis of Nematicidal Essential Oil of Valeriana ... Tropical Journal of Pharmaceutical Research ... have a potential to be developed to natural nematicides for the control of cereal cyst nematodes.

Effluent Gas Flux Characterization During Pyrolysis of Chicken Manure

Science.gov (United States)

Clark, S. C.; Ryals, R.; Miller, D. J.; Mullen, C. A.; Pan, D.; Zondlo, M. A.; Boateng, A. A.; Hastings, M. G.

2017-12-01

Pyrolysis is a viable option for the production of agricultural resources from diverted organic waste streams and renewable bioenergy. This high temperature thermochemical process yields material with beneficial reuses, including bio-oil and biochar. Gaseous forms of carbon (C) and nitrogen (N) are also emitted during pyrolysis. The effluent mass emission rates from pyrolysis are not well characterized, thus limiting proper evaluation of the environmental benefits or costs of pyrolysis products. We present the first comprehensive suite of C and N mass emission rate measurements of a biomass pyrolysis process using chicken manure as feedstock to produce biochar and bio-oil. Two chicken manure fast pyrolysis experiments were conducted at controlled temperature ranges of 450 - 485 °C and 550 - 585 °C. Mass emission rates of N2O, NO, CO, CO2, CH4 and NH3 were measured using trace gas analyzers. Based on the system mass balance, 23-25% of the total mass of the manure feedstock was emitted as gas, while 52-55% and 23% were converted to bio-oil and biochar, respectively. CO2 and NH3 were the dominant gaseous species by mass, accounting for 58 - 65% of total C mass emitted and 99% of total reactive N mass emitted, respectively. Our gas flux measurements suggest that 1.4 to 2.7 g NH3 -N would be produced from the pyrolysis of one kg of manure. Conservatively scaling up these NH3 pyrolysis emissions in the Chesapeake Bay Watershed, where an estimated 8.64 billion kg of poultry manure is applied to agricultural soils every year, as much as 1.2 x 107 kg of NH3 could be emitted into the atmosphere annually, increasing the potential impact of atmospheric N deposition without a mechanism to capture the gas exhaust during pyrolysis. However, this is considerably less than the potential emissions from NH3 volatilization of raw chicken manure applications, which can be 20-60% of total N applied, and amount to 3.4 x 107 - 1.0 x 108 kg NH3-N yr-1. Pyrolysis has the potential to

Gas Chromatography-Mass Spectrometric Analysis and Insecticidal ...

African Journals Online (AJOL)

Tropical Journal of Pharmaceutical Research ... apelta aerial parts was analyzed by gas chromatography/mass spectrometric (GC/MS) to determine its composition. ... into a natural fumigant/insecticide for the control of stored product insects.

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.

Ultra-high performance supercritical fluid chromatography hyphenated to atmospheric pressure chemical ionization high resolution mass spectrometry for the characterization of fast pyrolysis bio-oils.

Science.gov (United States)

Crepier, Julien; Le Masle, Agnès; Charon, Nadège; Albrieux, Florian; Duchene, Pascal; Heinisch, Sabine

2018-06-01

Extensive characterization of complex mixtures requires the combination of powerful analytical techniques. A Supercritical Fluid Chromatography (SFC) method was previously developed, for the specific case of fast pyrolysis bio oils, as an alternative to gas chromatography (GC and GC × GC) or liquid chromatography (LC and LC × LC), both separation methods being generally used prior to mass spectrometry (MS) for the characterization of such complex matrices. In this study we investigated the potential of SFC hyphenated to high resolution mass spectrometry (SFC-HRMS) for this characterization using Negative ion Atmospheric Pressure Chemical ionization ((-)APCI) for the ionization source. The interface between SFC and (-)APCI/HRMS was optimized from a mix of model compounds with the objective of maximizing the signal to noise ratio. The main studied parameters included both make-up flow-rate and make-up composition. A methodology for the treatment of APCI/HRMS data is proposed. This latter allowed for the identification of molecular formulae. Both SFC-APCI/HRMS method and data processing method were applied to a mixture of 36 model compounds, first analyzed alone and then spiked in a bio-oil. In both cases, 19 compounds could be detected. Among them 9 could be detected in a fast pyrolysis bio-oil by targeted analysis. The whole procedure was applied to the characterization of a bio-oil using helpful representations such as mass-plots, van Krevelen diagrams and heteroatom class distributions. Finally the results were compared with those obtained with a Fourier Transform ion-cyclotron resonance mass spectrometer (FT-ICR/MS). Copyright © 2018 Elsevier B.V. All rights reserved.

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

Evaluation of chemical stability of polymers of XIENCE everolimus-eluting coronary stents in vivo by pyrolysis-gas chromatography/mass spectrometry.

Science.gov (United States)

Kamberi, Marika; Pinson, David; Pacetti, Stephen; Perkins, Laura E L; Hossainy, Syed; Mori, Hiroyoshi; Rapoza, Richard J; Kolodgie, Frank; Virmani, Renu

2017-09-07

The polymers poly(vinylidene fluoride-co-hexafluoropropylene) (PVDF-HFP) and poly(n-butyl methacrylate) (PBMA) are employed in manufacturing the XIENCE family of coronary stents. PBMA serves as a primer and adheres to both the stent and the drug coating. PVDF-HFP is employed in the drug matrix layer to hold the drug everolimus on the stent and control its release. Chemical stability of the polymers of XIENCE stents in the in-vivo environment was evaluated by pyrolysis-gas chromatography with mass spectrometry (Py-GC/MS) detection. For this evaluation, XIENCE stents explanted from porcine coronary arteries and from human coronary artery specimens at autopsy after 2-4 and 5-7 years of implantation, respectively, were compared to freshly manufactured XIENCE stents (controls). The comparison of pyrograms of explanted stent samples and controls showed identical fragmentation fingerprints of polymers, indicating that PVDF-HFP and PBMA maintained their chemical integrity after multiple years of XIENCE coronary stent implantation. The findings of the present study demonstrate the chemical stability of PVDF-HFP and PBMA polymers of the XIENCE family of coronary stents in the in-vivo environment, and constitute a further proof of the suitability of PVDF-HFP as a drug carrier for the drug eluting stent applications. © 2017 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 2017. © 2017 Wiley Periodicals, Inc.

Rapid and slow pyrolysis of pistachio shell: effect of pyrolysis conditions on the product yields and characterization of the liquid product

Energy Technology Data Exchange (ETDEWEB)

Putun, Ayse E [Department of Chemical Engineering, Anadolu University, Eskisehir 26470, (Turkey); Ozbay, Nurgul [Bozuyuk Vocational School, Anadolu University, Bozuyuk/Bilecik, (Turkey); Varol, Esin Apaydin; Uzun, Basak B; Ates, Fuda [Department of Chemical Engineering, Anadolu University, Eskisehir 26470, (Turkey)

2006-10-30

This study reports the experimental results for the pyrolysis of pistachio shell under different conditions in a tubular reactor under a nitrogen flow. For the different conditions of pyrolysis temperature, nitrogen flow rate and heating rate, pyrolysis temperature of 773 K gave the highest bio-oil yield with a value of 27.7% when the heating rate and carrier gas flow rate were chosen as 300 K min{sup -1} and 100 cm{sup 3} min{sup -1}, respectively. Column chromatography was applied to this bio-oil and its subfractions were characterized by elemental analysis, FT-IR and 1H-NMR. Aliphatic subfraction was conducted to gas chromatography-mass spectroscopy for further characterization. The results for the characterization show that using pistachio shell as a renewable source to produce valuable liquid products is applicable via pyrolysis. (Author)

Gas Chromatography Mass Spectrometry of Quassia undulata Seed ...

African Journals Online (AJOL)

Prof. Ogunji

The use of gas chromatography mass spectrometry (GC MS) as a sensitive and specific technique ... cold flow properties and stability of the fuel to oxidation, peroxidation and polymerization .... determinants of both the physical and chemical ...

Characterisation of uremic "Middle molecular"fractions by gas chromatography mass spectrometry, isotachophoresis, and liquid chromatography

NARCIS (Netherlands)

Schoots, A.C.; Mikkers, F.E.P.; Claessens, H.A.; Smet, de R.; Landschoot, van N.; Ringoir, S.M.G.

1982-01-01

Uremic ultrafiltrates (and normal serum, for comparison) were fractionated by means of gel filtration. The collected fractions were further investigated by combined analytical techniques: "high- performance" liquid chromatography, gas chromatography, mass spectrometry, and isotachophoresis.

Identification of Cyclopentenyl Fatty Acids by Gas Liquid Chromatography and Mass Spectrometry

DEFF Research Database (Denmark)

Shukla, V. K. S.; Abdel-Moety, E. M.; Larsen, Elfinn

1979-01-01

The straight chain fatty acids and the cyclopentenyl fatty acids present in the lipids of Hydnocarpus wightiana seeds were separated as their pyrrolidides by means of gas chromatography. A gas chromatography-mass spectrometry system confirmed the complete separation and permitted the identification...

Gas chromatography mass spectrometry : key technology in metabolomics

NARCIS (Netherlands)

Koek, Maud Marijtje

2009-01-01

Metabolomics involves the unbiased quantitative and qualitative analysis of the complete set of metabolites present in cells, body fluids and tissues. Gas chromatography coupled to mass spectrometry (GC-MS) is very suitable for metabolomics analysis, as it combines high separation power with

Comparison of gas chromatography/isotope ratio mass spectrometry and liquid chromatography/isotope ratio mass spectrometry for carbon stable-isotope analysis of carbohydrates

NARCIS (Netherlands)

Moerdijk-Poortvliet, Tanja C. W.; Schierbeek, Henk; Houtekamer, Marco; van Engeland, Tom; Derrien, Delphine; Stal, Lucas J.; Boschker, Henricus T. S.

2015-01-01

We compared gas chromatography/isotope ratio mass spectrometry (GC/IRMS) and liquid chromatography/isotope ratio mass spectrometry (LC/IRMS) for the measurement of δ(13)C values in carbohydrates. Contrary to GC/IRMS, no derivatisation is needed for LC/IRMS analysis of carbohydrates. Hence, although

Comparison of gas chromatography/isotope ratio mass spectrometry and liquid chromatography/isotope ratio mass spectrometry for carbon stable-isotope analysis of carbohydrates

NARCIS (Netherlands)

Moerdijk-Poortvliet, T.C.W.; Schierbeek, H.; Houtekamer, M.; van Engeland, T.; Derrien, D.; Stal, L.J.; Boschker, H.T.S.

2015-01-01

We compared gas chromatography/isotope ratio mass spectrometry (GC/IRMS) and liquid chromatography/isotope ratio mass spectrometry (LC/IRMS) for the measurement of d13C values in carbohydrates. Contrary to GC/IRMS, no derivatisation is needed for LC/IRMS analysis of carbohydrates. Hence, although

Comparison of gas chromatography/isotope ratio mass spectrometry and liquid chromatography/isotope ratio mass spectrometry for carbon stable-isotope analysis of carbohydrates

NARCIS (Netherlands)

Moerdijk-Poortvliet, T.C.W.; Schierbeek, H.; Houtekamer, M.; van Engeland, T.; Derrien, D.; Stal, L.J.; Boschker, H.T.S.

2015-01-01

Rationale: We compared gas chromatography/isotope ratio mass spectrometry (GC/IRMS) and liquid chromatography/isotope ratio mass spectrometry (LC/IRMS) for the measurement of δ13C values in carbohydrates. Contrary to GC/IRMS, no derivatisation is needed for LC/IRMS analysis of carbohydrates. Hence,

On the Habitability of Desert Varnish: A Combined Study by Micro-Raman Spectroscopy, X-ray Diffraction, and Methylated Pyrolysis-Gas Chromatography-Mass Spectrometry.

Science.gov (United States)

Malherbe, C; Hutchinson, I B; Ingley, R; Boom, A; Carr, A S; Edwards, H; Vertruyen, B; Gilbert, B; Eppe, G

2017-11-01

In 2020, the ESA ExoMars and NASA Mars 2020 missions will be launched to Mars to search for evidence of past and present life. In preparation for these missions, terrestrial analog samples of rock formations on Mars are studied in detail in order to optimize the scientific information that the analytical instrumentation will return. Desert varnishes are thin mineral coatings found on rocks in arid and semi-arid environments on Earth that are recognized as analog samples. During the formation of desert varnishes (which takes many hundreds of years), organic matter is incorporated, and microorganisms may also play an active role in the formation process. During this study, four complementary analytical techniques proposed for Mars missions (X-ray diffraction [XRD], Raman spectroscopy, elemental analysis, and pyrolysis-gas chromatography-mass spectrometry [Py-GC-MS]) were used to interrogate samples of desert varnish and describe their capacity to sustain life under extreme scenarios. For the first time, both the geochemistry and the organic compounds associated with desert varnish are described with the use of identical sets of samples. XRD and Raman spectroscopy measurements were used to nondestructively interrogate the mineralogy of the samples. In addition, the use of Raman spectroscopy instruments enabled the detection of β-carotene, a highly Raman-active biomarker. The content and the nature of the organic material in the samples were further investigated with elemental analysis and methylated Py-GC-MS, and a bacterial origin was determined to be likely. In the context of planetary exploration, we describe the habitable nature of desert varnish based on the biogeochemical composition of the samples. Possible interference of the geological substrate on the detectability of pyrolysis products is also suggested. Key Words: Desert varnish-Habitability-Raman spectroscopy-Py-GC-MS-XRD-ExoMars-Planetary science. Astrobiology 17, 1123-1137.

On the Habitability of Desert Varnish: A Combined Study by Micro-Raman Spectroscopy, X-ray Diffraction, and Methylated Pyrolysis-Gas Chromatography-Mass Spectrometry

Science.gov (United States)

Malherbe, C.; Hutchinson, I. B.; Ingley, R.; Boom, A.; Carr, A. S.; Edwards, H.; Vertruyen, B.; Gilbert, B.; Eppe, G.

2017-11-01

In 2020, the ESA ExoMars and NASA Mars 2020 missions will be launched to Mars to search for evidence of past and present life. In preparation for these missions, terrestrial analog samples of rock formations on Mars are studied in detail in order to optimize the scientific information that the analytical instrumentation will return. Desert varnishes are thin mineral coatings found on rocks in arid and semi-arid environments on Earth that are recognized as analog samples. During the formation of desert varnishes (which takes many hundreds of years), organic matter is incorporated, and microorganisms may also play an active role in the formation process. During this study, four complementary analytical techniques proposed for Mars missions (X-ray diffraction [XRD], Raman spectroscopy, elemental analysis, and pyrolysis-gas chromatography-mass spectrometry [Py-GC-MS]) were used to interrogate samples of desert varnish and describe their capacity to sustain life under extreme scenarios. For the first time, both the geochemistry and the organic compounds associated with desert varnish are described with the use of identical sets of samples. XRD and Raman spectroscopy measurements were used to nondestructively interrogate the mineralogy of the samples. In addition, the use of Raman spectroscopy instruments enabled the detection of β-carotene, a highly Raman-active biomarker. The content and the nature of the organic material in the samples were further investigated with elemental analysis and methylated Py-GC-MS, and a bacterial origin was determined to be likely. In the context of planetary exploration, we describe the habitable nature of desert varnish based on the biogeochemical composition of the samples. Possible interference of the geological substrate on the detectability of pyrolysis products is also suggested.

Study on condensation of biomass pyrolysis gas by spray bio-oil droplets

Energy Technology Data Exchange (ETDEWEB)

Xie, Kun; Cheng, Wen-Long [University of Science and Technology of China (China)], email: wlcheng@ustc.edu.cn; Chen, Jing [Anhui Electric Power Design Institute (China); Shi, Wen-Jing [Anhui Heli Co., Ltd (China)

2011-07-01

This is a study of bio-oil generated by fast pyrolysis; a biomass feedstock is heated to pyrolyze at a rapid rate, the gas pyrolyzed is then condensed rapidly. The interesting result is a potential alternative fuel oil. An analysis was made of the effects of the initial pyrolysis gas temperatures, the initial bio-oil droplets temperatures and diameters, and the flow ratio of the gas and the liquid droplets on the heat and mass transfer between the gas and the liquid droplets. A few criterion equations were achieved with respect to the spray condenser. This paper established the gas-liquid phase equilibrium of an aqueous multi-composition system and the spray condensation model coupling heat and mass transfer. Model calculation and analysis showed that: spray condensation can effectively cool the high-temperature pyrolysis gas quickly; with gas liquid flowing, mass transfer rate reduces; and the relationship of gas and liquid flow ratio can achieve good accuracy.

Pyrolysis process for the treatment of food waste.

Science.gov (United States)

Grycová, Barbora; Koutník, Ivan; Pryszcz, Adrian

2016-10-01

Different waste materials were pyrolysed in the laboratory pyrolysis unit to the final temperature of 800°C with a 10min delay at the final temperature. After the pyrolysis process a mass balance of the resulting products, off-line analysis of the pyrolysis gas and evaluation of solid and liquid products were carried out. The gas from the pyrolysis experiments was captured discontinuously into Tedlar gas sampling bags and the selected components were analyzed by gas chromatography (methane, ethene, ethane, propane, propene, hydrogen, carbon monoxide and carbon dioxide). The highest concentration of measured hydrogen (WaCe 61%vol.; WaPC 66%vol.) was analyzed at the temperature from 750 to 800°C. The heating values of the solid and liquid residues indicate the possibility of its further use for energy recovery. Copyright © 2016 Elsevier Ltd. All rights reserved.

Pyrolysis-gas chromatography/mass spectrometry of soil organic matter extracted from a Brazilian mangrove and Spanish salt marshes

NARCIS (Netherlands)

Perobelli Ferreira, F.; Buurman, P.; Macias, F.; Otero, X.L.; Boluda, R.

2009-01-01

The soil organic matter (SOM) extracted under different vegetation types from a Brazilian mangrove (Pai Matos Island, São Paulo State) and from three Spanish salt marshes (Betanzos Ría and Corrubedo Natural Parks, Galícia, and the Albufera Natural Park, Valencia) was investigated by pyrolysis-gas

Rapid quantification of biomarkers during kerogen microscale pyrolysis

Energy Technology Data Exchange (ETDEWEB)

Stott, A.W.; Abbott, G.D. [Fossil Fuels and Environmental Geochemistry NRG, The University, Newcastle-upon-Tyne (United Kingdom)

1995-02-01

A rapid, reproducible method incorporating closed system microscale pyrolysis and thermal desorption-gas chromatography/mass spectrometry has been developed and applied to the quantification of sterane biomarkers released during pyrolysis of the Messel oil shale kerogen under confined conditions. This method allows a substantial experimental concentration-time data set to be collected at accurately controlled temperatures, due to the low thermal inertia of the microscale borosilicate glass reaction vessels, which facilitates kinetic studies of biomarker reactions during kerogen microscale pyrolysis

ANALYSIS AND IDENTIFICATION SPIKING CHEMICAL COMPOUNDS RELATED TO CHEMICAL WEAPON CONVENTION IN UNKNOWN WATER SAMPLES USING GAS CHROMATOGRAPHY AND GAS CHROMATOGRAPHY ELECTRON IONIZATION MASS SPECTROMETRY

Directory of Open Access Journals (Sweden)

Harry Budiman

2010-06-01

Full Text Available The identification and analysis of chemical warfare agents and their degradation products is one of important component for the implementation of the convention. Nowadays, the analytical method for determination chemical warfare agent and their degradation products has been developing and improving. In order to get the sufficient analytical data as recommended by OPCW especially in Proficiency Testing, the spiking chemical compounds related to Chemical Weapon Convention in unknown water sample were determined using two different techniques such as gas chromatography and gas chromatography electron-impact ionization mass spectrometry. Neutral organic extraction, pH 11 organic extraction, cation exchanged-methylation, triethylamine/methanol-silylation were performed to extract the chemical warfare agents from the sample, before analyzing with gas chromatography. The identification of chemical warfare agents was carried out by comparing the mass spectrum of chemicals with mass spectrum reference from the OPCW Central Analytical Database (OCAD library while the retention indices calculation obtained from gas chromatography analysis was used to get the confirmation and supported data of  the chemical warfare agents. Diisopropyl methylphosphonate, 2,2-diphenyl-2-hydroacetic acid and 3-quinuclidinol were found in unknown water sample. Those chemicals were classified in schedule 2 as precursor or reactant of chemical weapons compound in schedule list of Chemical Weapon Convention.   Keywords: gas chromatography, mass spectrometry, retention indices, OCAD library, chemical warfare agents

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

African Journals Online (AJOL)

1Department of Pharmacognosy and Phytotherapy, 2Department of Pharmaceutics and Pharmaceutical Technology, University of Port Harcourt, Nigeria ... tuber-regium (synonym Pleurotus tuber regium) using gas chromatography-mass spectroscopic (GC- ... Department of Plant Science and Biotechnology,. University of ...

Comparative study of radio gas-chromatography and gas chromatography - mass spectrometry coupling in the identification of metabolites of estrogens and progesterone

International Nuclear Information System (INIS)

Adessi, G.; Nhuan, T.Q.; Jayle, M.F.

1978-01-01

Radio-gas chromatography (RGC) and gas chromatography-mass spectrometry (GC-MS) were used to identify estrogen and progesterone metabolites. The RGC enables the identification of metabolites of labelled precursors ( 3 H)-estradiol-17β and ( 14 C)-progesterone were used as precursors. The GC-MS analytical technique with mass fragmentography, offers the interest of using unlabelled precursors at physiological levels. The identification of metabolites was based on obtaining the mass spectrum or the compiled fragmentogram on the basis of the most characteristic fragment ions. More over, several metabolites can be quantified on the same fragmentogram. Results on the metabolism of estradiol-17β and progesterone by the hepatic tissue of guinea pigs are given. (Auth.)

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)

Contribution to high-temperature chromatography and high-temperature-gas-chromatography-mass spectrometry of lipids

International Nuclear Information System (INIS)

Aichholz, R.

1998-04-01

This thesis describes the use of high temperature gas chromatography for the investigation of unusual triacylglycerols, cyanolipids and bees waxes. The used glass capillary columns were pretreated and coated with tailor made synthesized high temperature stable polysiloxane phases. The selective separation properties of the individual columns were tested with a synthetic lipid mixture. Suitable derivatization procedures for the gaschromatographic analyses of neutral lipids, containing multiple bonds as well as hydroxy-, epoxy-, and carboxyl groups, were developed and optimized. Therefore conjugated olefinic-, conjugated olefinic-acetylenic-, hydroxy-, epoxy-, and conjugated olefinic keto triacylglycerols in miscellaneous plant seed oils as well as hydroxy monoesters, diesters and hydroxy diesters in bees waxes could be analysed directly with high temperature gas chromatography for the first time. In order to elucidate the structures of separated lipid compounds, high temperature gas chromatography was coupled to mass spectrometry and tandem mass spectrometry, respectively. Comparable analytical systems are hitherto not commercial available. Therefore instrumental prerequisites for a comprehensive and detailed analysis of seed oils and bees waxes were established. In GC/MS commonly two ionization methods are used, electron impact ionization and chemical ionization. For the analysis of lipids the first is of limited use only. Due to intensive fragmentation only weak molecular ions are observed. In contrast, the chemical ionization yields in better results. Dominant quasi molecular ions enable an unambiguous determination of the molecular weight. Moreover, characteristic fragment ions provide important indications of certain structural features of the examined compounds. Nevertheless, in some cases the chromatographic resolution was insufficient in order to separate all compounds present in natural lipid mixtures. Owing to the selected detection with mass spectrometry

Doping control analysis of anabolic steroids in equine urine by gas chromatography-tandem mass spectrometry.

Science.gov (United States)

Wong, April S Y; Leung, Gary N W; Leung, David K K; Wan, Terence S M

2017-09-01

Anabolic steroids are banned substances in equine sports. Gas chromatography-mass spectrometry (GC-MS) has been the traditional technique for doping control analysis of anabolic steroids in biological samples. Although liquid chromatography-mass spectrometry (LC/MS) has become an important technique in doping control, the detection of saturated hydroxysteroids by LC-MS remains a problem due to their low ionization efficiency under electrospray. The recent development in fast-scanning gas-chromatography-triple-quadrupole mass spectrometry (GC-MS/MS) has provided a better alternative with a significant reduction in chemical noise by means of selective reaction monitoring. Herein, we present a sensitive and selective method for the screening of over 50 anabolic steroids in equine urine using gas chromatography-tandem mass spectrometry (GC-MS/MS). Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Analysis of radioactive mixed hazardous waste using derivatization gas chromatography/mass spectrometry, liquid chromatography, and liquid chromatography/mass spectrometry

International Nuclear Information System (INIS)

Campbell, J.A.; Lerner, B.D.; Bean, R.M.; Grant, K.E.; Lucke, R.B.; Mong, G.M.; Clauss, S.A.

1994-08-01

Six samples of core segments from Tank 101-SY were analyzed for chelators, chelator fragments, and several carboxylic acids by derivatization gas chromatography/mass spectrometry. The major components detected were ethylenediaminetetraacetic acid, nitroso-iminodiacetic acid, nitrilotriacetic acid, citric acid, succinic acid, and ethylenediaminetriacetic acid. The chelator of highest concentration was ethylenediaminetetraacetic acid in all six samples analyzed. Liquid chromatography was used to quantitate low molecular weight acids including oxalic, formic, glycolic, and acetic acids, which are present in the waste as acid salts. From 23 to 61% of the total organic carbon in the samples analyzed was accounted for by these acids

Acid monomer analysis in waterborne polymer systems by targeted labeling of carboxylic acid functionality, followed by pyrolysis - gas chromatography.

Science.gov (United States)

Brooijmans, T; Okhuijsen, R; Oerlemans, I; Schoenmakers, P J; Peters, R

2018-05-14

Pyrolysis - gas chromatography - (PyGC) is a common method to analyse the composition of natural and synthetic resins. The analysis of acid functionality in, for example, waterborne polyacrylates and polyurethanes polymers has proven to be difficult due to solubility issues, inter- and intramolecular interaction effects, lack of detectability in chromatographic analysis, and lack of thermal stability. Conventional analytical techniques, such as PyGC, cannot be used for the direct detection and identification of acidic monomers, due to thermal rearrangements that take place during pyrolysis. To circumvent this, the carboxylic acid groups are protected prior to thermal treatment by reaction with 2-bromoacetophenone. Reaction conditions are investigated and optimised wrt. conversion measurements. The aproach is applied to waterborne polyacryalates and the results are discussed. This approach enables identification and (semi)quantitative analysis of different acid functionalities in waterborne polymers by PyGC. Copyright © 2018 Elsevier B.V. All rights reserved.

Development of a supercritical fluid chromatography method with ultraviolet and mass spectrometry detection for the characterization of biomass fast pyrolysis bio oils.

Science.gov (United States)

Crepier, Julien; Le Masle, Agnès; Charon, Nadège; Albrieux, Florian; Heinisch, Sabine

2017-08-11

The characterization of complex mixtures is a challenging issue for the development of innovative processes dedicated to biofuels and bio-products production. The huge number of compounds present in biomass fast pyrolysis oils combined with the large diversity of chemical functions represent a bottleneck as regards analytical technique development. For the extensive characterization of complex samples, supercritical fluid chromatography (SFC) can be alternative to usual separation techniques such as gas (GC) or liquid chromatography (LC). In this study, an approach is proposed to define the best conditions for the SFC separation of a fast pyrolysis bio-oil. This approach was based on SFC data obtained directly from the bio-oil itself instead of selecting model compounds as usually done. SFC conditions were optimized by using three specific, easy-to-use and quantitative criteria aiming at maximizing the separation power. Polar stationary phases (ethylpyridine bonded silica) associated to a mix of acetonitrile and water as polarity modifier provided the best results, with more than 120 peaks detected in SFC-UV. Copyright © 2017 Elsevier B.V. All rights reserved.

Fast Pyrolysis of Four Lignins from Different Isolation Processes Using Py-GC/MS

OpenAIRE

Lin, Xiaona; Sui, Shujuan; Tan, Shun; Pittman, Charles; Sun, Jianping; Zhang, Zhijun

2015-01-01

Pyrolysis is a promising approach that is being investigated to convert lignin into higher value products including biofuels and phenolic chemicals. In this study, fast pyrolysis of four types of lignin, including milled Amur linden wood lignin (MWL), enzymatic hydrolysis corn stover lignin (EHL), wheat straw alkali lignin (AL) and wheat straw sulfonate lignin (SL), were performed using pyrolysis gas-chromatography/mass spectrometry (Py-GC/MS). Thermogravimetric analysis (TGA) showed that the...

A novel methylation derivatization method for δ(18)O analysis of individual carbohydrates by gas chromatography/pyrolysis-isotope ratio mass spectrometry.

Science.gov (United States)

Lehmann, Marco M; Fischer, Maria; Blees, Jan; Zech, Michael; Siegwolf, Rolf T W; Saurer, Matthias

2016-01-15

The oxygen isotope ratio (δ(18)O) of carbohydrates derived from animals, plants, sediments, and soils provides important information about biochemical and physiological processes, past environmental conditions, and geographical origins, which are otherwise not available. Nowadays, δ(18)O analyses are often performed on carbohydrate bulk material, while compound-specific δ(18)O analyses remain challenging and methods for a wide range of individual carbohydrates are rare. To improve the δ(18)O analysis of individual carbohydrates by gas chromatography/pyrolysis-isotope ratio mass spectrometry (GC/Pyr-IRMS) we developed a new methylation derivatization method. Carbohydrates were fully methylated within 24 h in an easy-to-handle one-pot reaction in acetonitrile, using silver oxide as proton acceptor, methyl iodide as methyl group carrier, and dimethyl sulfide as catalyst. The precision of the method ranged between 0.12 and 1.09‰ for the δ(18)O values of various individual carbohydrates of different classes (mono-, di-, and trisaccharides, alditols), with an accuracy of a similar order of magnitude, despite high variation in peak areas. Based on the δ(18)O values of the main isomers, important monosaccharides such as glucose and fructose could also be precisely analyzed for the first time. We tested the method on standard mixtures, honey samples, and leaf carbohydrates extracted from Pinus sylvestris, showing that the method is also applicable to different carbohydrate mixtures. The new methylation method shows unrivalled accuracy and precision for δ(18)O analysis of various individual carbohydrates; it is fast and easy-to-handle, and may therefore find wide-spread application. Copyright © 2015 John Wiley & Sons, Ltd.

Chemical and physical characterisation of biomass-based pyrolysis oils. Literature view

Energy Technology Data Exchange (ETDEWEB)

Fagernaes, L [VTT Energy, Espoo (Finland). Energy Production Technologies

1996-12-31

Biomass-based pyrolysis oils are complex mixtures of mainly organic compounds and water. The determination of their physical and chemical properties and chemical composition is a challenge for researchers. Characterisation of biomass pyrolysis oils has been studied at many universities in North America and Europe in the 1980s and 1990s. The existing literature on the analytical methods used for these oils is reviewed in this report. For characterising the chemical composition, the bio-oils have first been mainly fractionated into different classes. Solvent extraction and adsorption chromatography are the most general methods used. In adsorption chromatography, the oils have been fractionated into different hydrocarbon and polar fractions. The fractions obtained have been analysed with various chromatographic and spectroscopic methods. Gas chromatography/mass spectrometry (GC/MS) technique is the analytical method most widely used and well adaptable for the fractions. For high-molecular-mass and highly polar compounds liquid chromatographic (LC) techniques as well as infrared (FT-IR) and nuclear magnetic resonance (1H NMR and 13C NMR) spectroscopies are more suitable due to the low volatility of pyrolysis oils. For whole pyrolysis oils, LC techniques, primarily size exclusion chromatography and FT-IR and FT-NMR spectroscopies have proved to be useful methods

Chemical and physical characterisation of biomass-based pyrolysis oils. Literature view

Energy Technology Data Exchange (ETDEWEB)

Fagernaes, L. [VTT Energy, Espoo (Finland). Energy Production Technologies

1995-12-31

Biomass-based pyrolysis oils are complex mixtures of mainly organic compounds and water. The determination of their physical and chemical properties and chemical composition is a challenge for researchers. Characterisation of biomass pyrolysis oils has been studied at many universities in North America and Europe in the 1980s and 1990s. The existing literature on the analytical methods used for these oils is reviewed in this report. For characterising the chemical composition, the bio-oils have first been mainly fractionated into different classes. Solvent extraction and adsorption chromatography are the most general methods used. In adsorption chromatography, the oils have been fractionated into different hydrocarbon and polar fractions. The fractions obtained have been analysed with various chromatographic and spectroscopic methods. Gas chromatography/mass spectrometry (GC/MS) technique is the analytical method most widely used and well adaptable for the fractions. For high-molecular-mass and highly polar compounds liquid chromatographic (LC) techniques as well as infrared (FT-IR) and nuclear magnetic resonance (1H NMR and 13C NMR) spectroscopies are more suitable due to the low volatility of pyrolysis oils. For whole pyrolysis oils, LC techniques, primarily size exclusion chromatography and FT-IR and FT-NMR spectroscopies have proved to be useful methods

High-throughput characterization of sediment organic matter by pyrolysis-gas chromatography/mass spectrometry and multivariate curve resolution: A promising analytical tool in (paleo)limnology.

Science.gov (United States)

Tolu, Julie; Gerber, Lorenz; Boily, Jean-François; Bindler, Richard

2015-06-23

Molecular-level chemical information about organic matter (OM) in sediments helps to establish the sources of OM and the prevalent degradation/diagenetic processes, both essential for understanding the cycling of carbon (C) and of the elements associated with OM (toxic trace metals and nutrients) in lake ecosystems. Ideally, analytical methods for characterizing OM should allow high sample throughput, consume small amounts of sample and yield relevant chemical information, which are essential for multidisciplinary, high-temporal resolution and/or large spatial scale investigations. We have developed a high-throughput analytical method based on pyrolysis-gas chromatography/mass spectrometry and automated data processing to characterize sedimentary OM in sediments. Our method consumes 200 μg of freeze-dried and ground sediment sample. Pyrolysis was performed at 450°C, which was found to avoid degradation of specific biomarkers (e.g., lignin compounds, fresh carbohydrates/cellulose) compared to 650°C, which is in the range of temperatures commonly applied for environmental samples. The optimization was conducted using the top ten sediment samples of an annually resolved sediment record (containing 16-18% and 1.3-1.9% of total carbon and nitrogen, respectively). Several hundred pyrolytic compound peaks were detected of which over 200 were identified, which represent different classes of organic compounds (i.e., n-alkanes, n-alkenes, 2-ketones, carboxylic acids, carbohydrates, proteins, other N compounds, (methoxy)phenols, (poly)aromatics, chlorophyll and steroids/hopanoids). Technical reproducibility measured as relative standard deviation of the identified peaks in triplicate analyses was 5.5±4.3%, with 90% of the RSD values within 10% and 98% within 15%. Finally, a multivariate calibration model was calculated between the pyrolytic degradation compounds and the sediment depth (i.e., sediment age), which is a function of degradation processes and changes in OM

The diversity of methoxyphenols released by pyrolysis-gas chromatography as predictor of soil carbon storage.

Science.gov (United States)

Jiménez-González, Marco A; Álvarez, Ana M; Carral, Pilar; González-Vila, Francisco J; Almendros, Gonzalo

2017-07-28

The variable extent to which environmental factors are involved in soil carbon storage is currently a subject of controversy. In fact, justifying why some soils accumulate more organic matter than others is not trivial. Some abiotic factors such as organo-mineral associations have classically been invoked as the main drivers for soil C stabilization. However, in this research indirect evidences based on correlations between soil C storage and compositional descriptors of the soil organic matter are presented. It is assumed that the intrinsic structure of soil organic matter should have a bearing in the soil carbon storage. This is examined here by focusing on the methoxyphenols released by direct pyrolysis from a wide variety of topsoil samples from continental Mediterranean ecosystems from Spain with different properties and carbon content. Methoxyphenols are typical signature compounds presumptively informing on the occurrence and degree of alteration of lignin in soils. The methoxyphenol assemblages (12 major guaiacyl- and syringyl-type compounds) were analyzed by pyrolysis-gas chromatography-mass spectrometry. The Shannon-Wiener diversity index was chosen to describe the complexity of this phenolic signature. A series of exploratory statistical analyses (simple regression, partial least squares regression, multidimensional scaling) were applied to analyze the relationships existing between chemical and spectroscopic characteristics and the carbon content in the soils. These treatments coincided in pointing out that significant correlations exist between the progressive molecular diversity of the methoxyphenol assemblages and the concentration of organic carbon stored in the corresponding soils. This potential of the diversity in the phenolic signature as a surrogate index of the carbon storage in soils is tentatively interpreted as the accumulation of plant macromolecules altered into microbially reworked structures not readily recognized by soil enzymes. From

Desulfurized gas production from vertical kiln pyrolysis

Science.gov (United States)

Harris, Harry A.; Jones, Jr., John B.

1978-05-30

A gas, formed as a product of a pyrolysis of oil shale, is passed through hot, retorted shale (containing at least partially decomposed calcium or magnesium carbonate) to essentially eliminate sulfur contaminants in the gas. Specifically, a single chambered pyrolysis vessel, having a pyrolysis zone and a retorted shale gas into the bottom of the retorted shale zone and cleaned product gas is withdrawn as hot product gas near the top of such zone.

On-line gas chromatography combustion/pyrolysis isotope ratio mass spectrometry (HRGC-C/P-IRMS) of pineapple (Ananas comosus L. Merr.) volatiles.

Science.gov (United States)

Preston, Christina; Richling, Elke; Elss, Sandra; Appel, Markus; Heckel, Frank; Hartlieb, Ariane; Schreier, Peter

2003-12-31

By use of extracts prepared by liquid-liquid separation of the volatiles from self-prepared juices of pineapple fruits (Ananas comosus) (n = 14) as well as commercial pineapple recovery aromas/water phases (n = 3), on-line capillary gas chromatography-isotope ratio mass spectrometry was employed in the combustion (C) and the pyrolysis (P) modes (HRGC-C/P-IRMS) to determine the delta(13)C(VPDB) and delta(2)H(VSMOW) values of selected pineapple flavor constituents. In addition to methyl 2-methylbutanoate 1, ethyl 2-methylbutanoate 2, methyl hexanoate 3, ethyl hexanoate 4, and 2,5-dimethyl-4-methoxy-3[2H]-furanone 5, each originating from the fruit, the delta(13)C(VPDB) and delta(2)H(VSMOW) data of commercial synthetic 1-5 and "natural" (biotechnologically derived) 1-4 were determined. With delta(13)C(VPDB) data of pineapple volatiles 1-4 varying from -12.8 to -24.4 per thousand, the range expected for CAM metabolism was observed. Compound 5 showed higher depletion from -20.9 to -28.6 per thousand. A similar situation was given for the delta(2)H(VSMOW) values of 3-5 from pineapple ranging from -118 to -191 per thousand, whereas 1 and 2 showed higher depleted values from -184 to -263 per thousand. In nearly all cases, analytical differentiation of 1-5 from pineapple and natural as well as synthetic origin was possible. In general, natural and synthetic 1-5 exhibited delta(13)C(VPDB) data ranging from -11.8 to -32.2 per thousand and -22.7 to -35.9 per thousand, respectively. Their delta(2)H(VSMOW) data were in the range from -242 to -323 per thousand and -49 to -163 per thousand, respectively.

Laser induced pyrolysis techniques

International Nuclear Information System (INIS)

Vanderborgh, N.E.

1976-01-01

The application of laser pyrolysis techniques to the problems of chemical analysis is discussed. The processes occurring during laser pyrolysis are first briefly reviewed. The problems encountered in laser pyrolysis gas chromatography are discussed using the analysis of phenanthrene and binary hydrocarbons. The application of this technique to the characterization of naturally occurring carbonaceous material such as oil shales and coal is illustrated

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

The Use of Gas Chromatography and Mass Spectrometry to Introduce General Chemistry Students to Percent Mass and Atomic Mass Calculations

Science.gov (United States)

Pfennig, Brian W.; Schaefer, Amy K.

2011-01-01

A general chemistry laboratory experiment is described that introduces students to instrumental analysis using gas chromatography-mass spectrometry (GC-MS), while simultaneously reinforcing the concepts of mass percent and the calculation of atomic mass. Working in small groups, students use the GC to separate and quantify the percent composition…

Rapid estimation of the organic sulphur content of kerogens, coals and asphaltenes by pyrolysis-gas chromatography

NARCIS (Netherlands)

Sinninghe Damsté, J.S.; Eglinton, T.I.; Kohnen, M.E.L.; Leeuw, J.W. de

1990-01-01

A pyrolysis-gas Chromatographic (py-g.c.) method for estimation of the Sorg/C ratio in kerogens and other forms of sedimentary macromolecular organic matter is described. The method is based upon flash pyrolysis at 610 °C for 10s and areal integration of the FID peaks attributed to

Biomass pyrolysis/gasification for product gas production: the overall investigation of parametric effects

International Nuclear Information System (INIS)

Chen, G.; Andries, J.; Luo, Z.; Spliethoff, H.

2003-01-01

The conventional biomass pyrolysis/gasification process for production of medium heating value gas for industrial or civil applications faces two disadvantages, i.e. low gas productivity and the accompanying corrosion of downstream equipment caused by the high content of tar vapour contained in the gas phase. The objective of this paper is to overcome these disadvantages, and therefore, the effects of the operating parameters on biomass pyrolysis are investigated in a laboratory setup based on the principle of keeping the heating value of the gas almost unchanged. The studied parameters include reaction temperature, residence time of volatile phase in the reactor, physico-chemical pretreatment of biomass particles, heating rate of the external heating furnace and improvement of the heat and mass transfer ability of the pyrolysis reactor. The running temperature of a separate cracking reactor and the geometrical configuration of the pyrolysis reactor are also studied. However, due to time limits, different types of catalysts are not used in this work to determine their positive influences on biomass pyrolysis behaviour. The results indicate that product gas production from biomass pyrolysis is sensitive to the operating parameters mentioned above, and the product gas heating value is high, up to 13-15 MJ/N m 3

Principles and applications of a research-oriented gas chromatography-mass spectrometry data system

International Nuclear Information System (INIS)

Campana, J.E.; Risby, T.H.; Jurs, P.C.

1979-01-01

A research-oriented gas chromatography-mass spectrometry data system for a quadrupole mass spectrometer has been developed based on a centrally located departmental computer facility. An overview of the hardware and software system is presented, emphasizing the important aspects of on-line computer data acquisition and control and the design philosophy used in the development of the system. The application of the system is demonstrated by the g.c.-m.s. analysis of a mixture of four transition metal β-diketonates (Al, Cr, Rh, and Ru tris-1,1,1-trifluoro-pentane-2,4-dionate). This anaysis involved vacuum gas chromatography with a support-coated open tubular column and detection of the eluent by chemical ionization mass spectrometry. The results demonstrate the data system capabilities and indicate the utility of the combined methodologies. (Auth.)

Analysis of small carbohydrates in several bioactive botanicals by gas chromatography with mass spectrometry and liquid chromatography with tandem mass spectrometry.

Science.gov (United States)

Moldoveanu, Serban; Scott, Wayne; Zhu, Jeff

2015-11-01

Bioactive botanicals contain natural compounds with specific biological activity, such as antibacterial, antioxidant, immune stimulating, and taste improving. A full characterization of the chemical composition of these botanicals is frequently necessary. A study of small carbohydrates from the plant materials of 18 bioactive botanicals is further described. The study presents the identification of the carbohydrate using a gas chromatographic-mass spectrometric analysis that allows detection of molecules as large as maltotetraose, after changing them into trimethylsilyl derivatives. A number of carbohydrates in the plant (fructose, glucose, mannose, sucrose, maltose, xylose, sorbitol, and myo-, chiro-, and scyllo-inositols) were quantitated using a novel liquid chromatography with tandem mass spectrometric technique. Both techniques involved new method developments. The gas chromatography with mass spectrometric analysis involved derivatization and separation on a Rxi(®)-5Sil MS column with H2 as a carrier gas. The liquid chromatographic separation was obtained using a hydrophilic interaction type column, YMC-PAC Polyamine II. The tandem mass spectrometer used an electrospray ionization source in multiple reaction monitoring positive ion mode with the detection of the adducts of the carbohydrates with Cs(+) ions. The validated quantitative procedure showed excellent precision and accuracy allowing the analysis in a wide range of concentrations of the analytes. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Evaluation of three gas chromatography and two direct mass spectrometry techniques for aroma analysis of dried red bell peppers

NARCIS (Netherlands)

Ruth, van S.M.; Boscaini, E.; Mayr, D.; Pugh, J.; Posthumus, M.A.

2003-01-01

Three gas chromatography methods and two direct mass spectrometry techniques were compared for the analysis of the aroma of rehydrated diced red bell peppers. Gas chromatography methods included systems with olfactometry detection (GC-O), flame ionisation detection (GC-FID) and mass spectrometry

The Study of Kinetic Properties and Analytical Pyrolysis of Coconut Shells

Directory of Open Access Journals (Sweden)

Mahir Said

2015-01-01

Full Text Available The kinetic properties of coconut shells during pyrolysis were studied to determine its reactivity in ground form. The kinetic parameters were determined by using thermogravimetric analyser. The activation energy was 122.780 kJ/mol. The pyrolysis products were analyzed using pyrolysis gas chromatography/mass spectrometry (Py-GC/MS. The effects of pyrolysis temperature on the distribution of the pyrolytic products were assessed in a temperature range between 673 K and 1073 K. The set time for pyrolysis was 2 s. Several compounds were observed; they were grouped into alkanes, acids, ethers and alcohols, esters, aldehydes and ketones, furans and pyrans, aromatic compounds, and nitrogen containing compounds. The product compositions varied with temperature in that range. The highest gas proportion was observed at high temperature while the acid proportion was observed to be highest in coconut shells, thus lowering the quality of bio-oil. It has been concluded that higher pyrolysis temperature increases the amount of pyrolysis products to a maximum value. It has been recommended to use coconut shell for production of gas, instead of production of bio-oil due to its high proportion of acetic acid.

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...

Identification of chemical components in Baidianling Capsule based on gas chromatography-mass spectrometry and high-performance liquid chromatography combined with Fourier transform ion cyclotron resonance mass spectrometry.

Science.gov (United States)

Wu, Wenying; Chen, Yu; Wang, Binjie; Sun, Xiaoyang; Guo, Ping; Chen, Xiaohui

2017-08-01

Baidianling Capsule, which is made from 16 Chinese herbs, has been widely used for treating vitiligo clinically. In this study, the sensitive and rapid method has been developed for the analysis of chemical components in Baidianling Capsule by gas chromatography-mass spectrometry in combination with retention indices and high-performance liquid chromatography combined with Fourier transform ion cyclotron resonance mass spectrometry. Firstly, a total of 110 potential volatile compounds obtained from different extraction procedures including alkanes, alkenes, alkynes, ketones, ethers, aldehydes, alcohols, phenols, organic acids, esters, furans, pyrrole, acid amides, heterocycles, and oxides were detected from Baidianling Capsule by gas chromatography-mass spectrometry, of which 75 were identified by mass spectrometry in combination with the retention index. Then, a total of 124 components were tentatively identified by high-performance liquid chromatography combined with Fourier transform ion cyclotron resonance mass spectrometry. Fifteen constituents from Baidianling Capsule were accurately identified by comparing the retention times with those of reference compounds, others were identified by comparing the retention times and mass spectrometry data, as well as retrieving the reference literature. This study provides a practical strategy for rapidly screening and identifying the multiple constituents of a complex traditional Chinese medicine. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

NARCIS (Netherlands)

Pacakova, V.; Leclercq, P.A.

1991-01-01

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

Catalytic Fast Pyrolysis of Alcell Lignin with Nano-NiO

Directory of Open Access Journals (Sweden)

Jiao Chen

2015-11-01

Full Text Available Catalytic fast pyrolysis of Alcell lignin with various additive ratios (5%, 10%, and 15%, mass ratio of nano-NiO was investigated using a horizontal pyrolyzer. Characterization methods, including Fourier transform infrared spectroscopy (FTIR, gas chromatography (GC, gas chromatography coupled with mass spectrometry (GC/MS, and elemental analysis, were utilized to identify the catalytic fast pyrolysis products. The results indicated that the nano-NiO catalyst had remarkable effects on the yield and quality of these products. The formation of gases, especially CO, CO2, and CH4, were greatly promoted when the additive ratio increased, while the formation of bio-char was clearly inhibited. However, when the additive ratio was 10%, the maximum yield of bio-oil (53.09 wt.% was obtained, and the corresponding maximum higher heating value (HHV was 25.33 MJ/kg. Furthermore, nano-NiO caused a large variation in the species of the compounds in bio-oil. Operating with the optimal nano-NiO additive ratio (10%, the carbon conversion rate was 65.50%, and the energy conversion rate was 74.53%.

Demonstration of conjugated dopamine in monkey CSF by gas chromatography-mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Elchisak, M A; Powers, K H; Ebert, M H

1982-09-01

A method for measuring unconjugated and conjugated dopamine in body tissues and fluids is described. Conjugated dopamine was hydrolyzed in acid to unconjugated dopamine, separated from the sample matrix by alumina chromatography, and assayed by gas chromatography-mass spectrometry. Conjugated dopamine was detected in greater concentrations than unconjugated dopamine in CSF taken from lateral ventricle or thecal sac of the Rhesus monkey. Haloperidol administration did not increase the levels of conjugated dopamine in lumbar CSF.

The lignin pyrolysis composition and pyrolysis products of palm kernel shell, wheat straw, and pine sawdust

International Nuclear Information System (INIS)

Chang, Guozhang; Huang, Yanqin; Xie, Jianjun; Yang, Huikai; Liu, Huacai; Yin, Xiuli; Wu, Chuangzhi

2016-01-01

Highlights: • The primarily pyrolysis composition of PKS lignin was p-hydroxyphenyl unit. • Higher phenol yield and lower gas energy yield were obtained from PKS pyrolysis. • PKS produced more bio-oil and biochar than WS and PS from pyrolysis at 650–850 °C. • PKS-char had poorer gasification reactivity due to higher ordering carbon degree. - Abstract: The lignin monomer composition of palm kernel shell (PKS) was characterized using pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS), and the characteristics and distributions of products obtained from PKS pyrolysis were investigated using Py-GC/MS, GC, and a specially designed pyrolysis apparatus. The gasification reactivity of PKS biochar was also characterized using thermogravimetry (TG) and Raman spectroscopy. All the results were compared with those obtained from wheat straw (WS) and pine sawdust (PS). The results showed that PKS lignin is primarily composed of p-hydroxyphenyl structural units, while WS and PS lignins are mainly made up of guaiacyl units. Both the mass and energy yields of non-condensable gases from PKS pyrolysis were lower than those obtained from WS and PS pyrolysis at 650–850 °C, owing to the lower volatile content (75.21%) and lack of methoxy groups in PKS. Compared with WS and PS, higher bio-oil productivity was observed during PKS pyrolysis. Phenols were the main component of PKS bio-oil from pyrolysis at 500 °C, and the phenol content of PKS bio-oil (13.49%) was higher than in WS bio-oil (1.62%) and PS bio-oil (0.55%). A higher yield of biochar (on an ash-free basis) was also obtained from PKS pyrolysis. Because of its greater relative degree of ordered carbon, PKS biochar exhibited lower in situ reactivity during CO_2 or H_2O gasification than WS and PS biochars. A longer residence time and addition of steam were found to be beneficial during PKS biochar gasification.

Catalytic pyrolysis of Laminaria japonica over nanoporous catalysts using Py-GC/MS

Directory of Open Access Journals (Sweden)

Jeon Jong-Ki

2011-01-01

Full Text Available Abstract The catalytic pyrolysis of Laminaria japonica was carried out over a hierarchical meso-MFI zeolite (Meso-MFI and nanoporous Al-MCM-48 using pyrolysis gas chromatography/mass spectrometry (Py-GC/MS. The effect of the catalyst type on the product distribution and chemical composition of the bio-oil was examined using Py-GC/MS. The Meso-MFI exhibited a higher activity in deoxygenation and aromatization during the catalytic pyrolysis of L. japonica. Meanwhile, the catalytic activity of Al-MCM-48 was lower than that of Meso-MFI due to its weak acidity.

Determination of 4-Chloroindole-3-Acetic Acid Methyl Ester in Lathyrus Vicia and Pisum by Gas Chromatography - Mass Spectrometry

DEFF Research Database (Denmark)

Engvild, Kjeld Christensen; Egsgaard, Helge; Larsen, Elfinn

1980-01-01

4-Chloroindole-3-acetic acid methyl ester was identified unequivocally in Lathyrus latifolius L., Vicia faba L. and Pisum sativum L. by thin layer chromatography, gas chromatography and mass spectrometry. The gas chromatographic system was able to separate underivatized chloroindole-3-acetic acid...... methyl ester isomers. The quantitative determination of 4-chloroindole-3-acetic acid methyl ester in immature seeds of these three species was performed by gas chromatography – mass spectrometry using deuterium labelled 4-chloro-indole-3-acetic acid methyl ester as an internal standard. P. sativum...

Quantitative analysis of detailed lignin monomer composition by pyrolysis-gas chromatography combined with preliminary acetylation of the samples.

Science.gov (United States)

Sonoda, T; Ona, T; Yokoi, H; Ishida, Y; Ohtani, H; Tsuge, S

2001-11-15

Detailed quantitative analysis of lignin monomer composition comprising p-coumaryl, coniferyl, and sinapyl alcohol and p-coumaraldehyde, coniferaldehyde, and sinapaldehyde in plant has not been studied from every point mainly because of artifact formation during the lignin isolation procedure, partial loss of the lignin components inherent in the chemical degradative methods, and difficulty in the explanation of the complex spectra generally observed for the lignin components. Here we propose a new method to quantify lignin monomer composition in detail by pyrolysis-gas chromatography (Py-GC) using acetylated lignin samples. The lignin acetylation procedure would contribute to prevent secondary formation of cinnamaldehydes from the corresponding alcohol forms during pyrolysis, which are otherwise unavoidable in conventional Py-GC process to some extent. On the basis of the characteristic peaks on the pyrograms of the acetylated sample, lignin monomer compositions in various dehydrogenative polymers (DHP) as lignin model compounds were determined, taking even minor components such as cinnamaldehydes into consideration. The observed compositions by Py-GC were in good agreement with the supplied lignin monomer contents on DHP synthesis. The new Py-GC method combined with sample preacetylation allowed us an accurate quantitative analysis of detailed lignin monomer composition using a microgram order of extractive-free plant samples.

Online gas chromatography combustion/pyrolysis-isotope ratio mass spectrometry (HRGC-C/P-IRMS) of (+/-)-Dihydroactinidiolide from tea ( Camellia sinensis ) and rooibos tea ( Aspalathus linearis ).

Science.gov (United States)

del Mar Caja, María; Preston, Christina; Menzel, Michael; Kempf, Michael; Schreier, Peter

2009-07-08

Online capillary gas chromatography-isotope ratio mass spectrometry in both the combustion and the pyrolysis modes (HRGC-C/P-IRMS) was employed to perform authentication studies of the flavoring agent (+/-)-dihydroactinidiolide. Thus, the delta(13)C(V-PDB) and delta(2)H(V-SMOW) values of synthetic (ex synthetic beta-ionone and natural beta-carotene) as well as enzymatically (ex synthetic and natural beta-carotene) produced references were studied in comparison with those of the natural substance isolated from black (n = 17) and green teas (n = 6) ( Camellia sinensis ) as well as Rooibos tea ( Aspalathus linearis ) (n = 7). The isotope values determined for both the synthetic and enzymatically produced samples of (+/-)-dihydroactinidiolide reflected the influence of the origin of their educts. Hence, in cases when synthetic educts were used, the delta(13)C(V-PDB) and delta(2)H(V-SMOW) values ranged from -27.0 to -28.4 per thousand and from -28 to -169 per thousand, respectively, whereas the use of natural educts led to ranges from -30.3 to -31.6 per thousand and from -154 to -228 per thousand, respectively. As to the tea samples, delta(13)C(V-PDB) and delta(2)H(V-SMOW) values ranging from -29.0 to -34.1 per thousand and from -153 to -274 per thousand, respectively, were recorded for (+/-)-dihydroactinidiolide from black and green teas, whereas that from Rooibos tea showed (2)H/(1)H ratios ranging from -189 to -210 per thousand as well as slightly enriched values in the (13)C/(12)C ratios ranging from -24.4 to -27.1 per thousand.

Pyrolysis of rice husk and corn stalk in auger reactor:Part 1. Characterization of char and gas at various temperatures

OpenAIRE

Yu, Yang; Yang, Yang; Cheng, Zhicai; Blanco, Paula H.; Liu, Ronghou; Bridgwater, A.V.; Cai, Junmeng

2016-01-01

In this study, rice husk and corn stalk have been pyrolyzed in an auger pyrolysis reactor at pyrolysis temperatures of 350, 400, 450, 500, 550, and 600 °C in order to investigate the effect of the pyrolysis temperature on the pyrolysis performance of the reactor and physicochemical properties of pyrolysis products (this paper focuses on char and gas). The results have shown that the pyrolysis temperature significantly affects the mass yields and properties of the pyrolysis products. The mass ...

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

OpenAIRE

Pacakova, V.; Leclercq, P.A.

1991-01-01

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 prod...

Identification of volatiles from pineapple (Ananas comosus L.) pulp by comprehensive two-dimensional gas chromatography and gas chromatography/mass spectrometry.

Science.gov (United States)

Pedroso, Marcio P; Ferreira, Ernesto C; Hantao, Leandro W; Bogusz, Stanislau; Augusto, Fabio

2011-07-01

Combining qualitative data from the chromatographic structure of 2-D gas chromatography with flame ionization detection (GC×GC-FID) and that from gas chromatography-mass spectrometry (GC/MS) should result in a more accurate assignment of the peak identities than the simple analysis by GC/MS, where coelution of analytes is unavoidable in highly complex samples (rendering spectra unsuitable for qualitative purposes) or for compounds in very low concentrations. Using data from GC×GC-FID combined with GC/MS can reveal coelutions that were not detected by mass spectra deconvolution software. In addition, some compounds can be identified according to the structure of the GC×GC-FID chromatogram. In this article, the volatile fractions of fresh and dehydrated pineapple pulp were evaluated. The extraction of the volatiles was performed by dynamic headspace extraction coupled to solid-phase microextraction (DHS-SPME), a technique appropriate for slurries or solid matrices. Extracted analytes were then analyzed by GC×GC-FID and GC/MS. The results obtained using both techniques were combined to improve compound identifications. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Quality improvement of pyrolysis oil from waste rubber by adding sawdust.

Science.gov (United States)

Wang, Wen-liang; Chang, Jian-min; Cai, Li-ping; Shi, Sheldon Q

2014-12-01

This work was aimed at improving the pyrolysis oil quality of waste rubber by adding larch sawdust. Using a 1 kg/h stainless pyrolysis reactor, the contents of sawdust in rubber were gradually increased from 0%, 50%, 100% and 200% (wt%) during the pyrolysis process. Using a thermo-gravimetric (TG) analyzer coupled with Fourier transform infrared (FTIR) analysis of evolving products (TG-FTIR), the weight loss characteristics of the heat under different mixtures of sawdust/rubber were observed. Using the pyrolysis-gas chromatography (GC)-mass spectrometry (Py-GC/MS), the vapors from the pyrolysis processes were collected and the compositions of the vapors were examined. During the pyrolysis process, the recovery of the pyrolysis gas and its composition were measured in-situ at a reaction temperature of 450 °C and a retaining time of 1.2s. The results indicated that the efficiency of pyrolysis was increased and the residual carbon was reduced as the percentage of sawdust increased. The adding of sawdust significantly improved the pyrolysis oil quality by reducing the polycyclic aromatic hydrocarbons (PAHs) and nitrogen and sulfur compounds contents, resulting in an improvement in the combustion efficiency of the pyrolysis oil. Copyright © 2014 Elsevier Ltd. All rights reserved.

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...

Characterization of the fermentation process by gas chromatography Lasiodiplodia theobromae and gas chromatography coupled with mass spectrometry

International Nuclear Information System (INIS)

Castillo Portela, Grolamys; Eng Sanchez, Felipe; Nogueiras Lima, Clara

2014-01-01

Lasiodiplodia theobromae is a fungus, which has been reported by some authors as a high yield producer of the phytohormone jasmonic acid (JA). An indigenous strain of this fungus has been used for producing a fermentation broth with a high JA concentration by the Cuban Research Institute for Sugar Cane Derivatives (ICIDCA), registered as BIOJAS. The broth has been applied to some agricultural crops and demonstrated its economic feasibility as plant growth regulator and biological control of various phytopathogenic microorganisms and pests. Both fermentation broth and biomass from this fungus contain some other metabolites having bioactive properties, for instance, fatty acids. This paper shows the composition and quantification of fatty acids in the biomass using Gas Chromatography (GC) and the identification of substances profile in fermentation broth by Gas Chromatography coupled to Mass Spectrometry (GC-MS). The most fatty acids in the biomass are palmitic, stearic, oleic, linoleic and linolenic acids, being oleic acid the major component. On the other hand, 2,32 % of fatty acid esters; 2,47 % of alkenes; 14,40 % of alcohols; 30,15 % of aldehydes and 21,73 % of paraffins were detected in the composition of fermentation broth

Sample collection and preparation of biofluids and extracts for gas chromatography-mass spectrometry.

Science.gov (United States)

Emwas, Abdul-Hamid M; Al-Talla, Zeyad A; Kharbatia, Najeh M

2015-01-01

To maximize the utility of gas chromatography-mass spectrometry (GC-MS) in metabonomics research, all stages of the experimental design should be standardized, including sample collection, storage, preparation, and sample separation. Moreover, the prerequisite for any GC-MS analysis is that a compound must be volatile and thermally stable if it is to be analyzed using this technique. Since many metabolites are nonvolatile and polar in nature, they are not readily amenable to analysis by GC-MS and require initial chemical derivatization of the polar functional groups in order to reduce the polarity and to increase the thermal stability and volatility of the analytes. In this chapter, an overview is presented of the optimum approach to sample collection, storage, and preparation for gas chromatography-mass spectrometry-based metabonomics with particular focus on urine samples as example of biofluids.

Characterisation of the volatile profiles of infant formulas by proton transfer reaction-mass spectrometry and gas chromatography-mass spectrometry

NARCIS (Netherlands)

Ruth, van S.M.; Floris, V.; Fayoux, S.

2006-01-01

The volatile profiles of 13 infant formulas were evaluated by proton transfer reaction-mass spectrometry (PTR-MS) and gas chromatography¿mass spectrometry (GC¿MS). The infant formulas varied in brand (Aptamil, Cow & Gate, SMA), type (for different infant target groups) and physical form

Soil organic matter chemistry changes upon secondary succession in Imperata Grasslands , Indonesia: A pyrolysis - GC/MS study

NARCIS (Netherlands)

Yassir, I.; Buurman, P.

2012-01-01

The chemical composition of soil organic matter (SOM) following secondary succession in Imperata grassland was investigated by Pyrolysis-Gas Chromatography/Mass Spectrometry (GC/MS). We studied 46 samples from different stages of succession using plots that last burned 3 and 9 years previously,

Quantitative Analysis of Bioactive Compounds from Aromatic Plants by Means of Dynamic Headspace Extraction and Multiple Headspace Extraction-Gas Chromatography-Mass Spectrometry

NARCIS (Netherlands)

Omar, Jone; Olivares, Maitane; Alonso, Ibone; Vallejo, Asier; Aizpurua-Olaizola, Oier; Etxebarria, Nestor

2016-01-01

Seven monoterpenes in 4 aromatic plants (sage, cardamom, lavender, and rosemary) were quantified in liquid extracts and directly in solid samples by means of dynamic headspace-gas chromatography-mass spectrometry (DHS-GC-MS) and multiple headspace extraction-gas chromatography-mass spectrometry

Self-activation of biochar from furfural residues by recycled pyrolysis gas.

Science.gov (United States)

Yin, Yulei; Gao, Yuan; Li, Aimin

2018-04-17

Biochar samples with controllable specific surface area and mesopore ratio were self-activated from furfural residues by recycled pyrolysis gas. The objective of this study was to develop a new cyclic utilization method for the gas produced by pyrolysis. The influences of preparation parameters on the resulting biochar were studied by varying the pyrolysis-gas flow rate, activation time and temperature. Structural characterization of the produced biochar was performed by analysis of nitrogen adsorption isotherms at 77 K and scanning electron microscope (SEM). The pyrolysis gas compositions before and after activation were determined by a gas chromatograph. The results indicated that the surface area of the biochar was increased from 167 m 2 /g to 567 m 2 /g, the total pore volume increased from 0.121 cm 3 /g to 0.380 cm 3 /g, and the ratio of the mesopore pore volume to the total pore volume increased 17-39.7%. The CO volume fraction of the pyrolysis gas changed from 34.66 to 62.29% and the CO 2 volume fraction decreased from 48.26% to 12.17% under different conditions of pyrolysis-gas flow rate, activation time and temperature. The calorific values of pyrolysis gas changed from 8.82 J/cm 3 to 14.00 J/cm 3 , which were higher than those of conventional pyrolysis gases. The slower pyrolysis-gas flow rate and higher activation time increased the efficiency of the reaction between carbon and pyrolysis gas. These results demonstrated the feasibility of treatment of the furfural residues to produce microporous and mesoporous biochar. The pyrolysis gas that results from the activation process could be used as fuel. Overall, this new self-activation method meets the development requirements of cyclic economy and cleaner production. Copyright © 2018. Published by Elsevier Ltd.

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.

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…

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.)

Evaluation of gas chromatography-combustion-isotope ratio mass spectrometry (GC-C-IRMS) for the quality assessment of citrus liqueurs.

Science.gov (United States)

Schipilliti, Luisa; Bonaccorsi, Ivana; Cotroneo, Antonella; Dugo, Paola; Mondello, Luigi

2013-02-27

Citrus liqueurs are alcoholic beverages obtained by maceration. The European Parliament protects these alcoholic beverages, forbidding the addition of nature-identical flavoring substances. However, for economical and technological reasons, producers often add natural and/or synthetic flavors to the alcoholic syrup, obtaining artificial spirit drinks. The aim of this study is to investigate the authenticity of Italian liqueurs, of lemon, bergamot, and mandarin (locally known as "limoncello", "bargamino", and "mandarinetto"), comparing the carbon isotope ratios with values determined in genuine cold-pressed peel oils. Authenticity assessment was performed using headspace-solid phase microextraction coupled to gas chromatography-combustion-isotope ratio mass spectrometry. Additional analyses were performed by direct enantioselective gas chromatography to determine the enantiomeric distribution of selected chiral volatiles and by gas chromatography-mass spectrometry for the qualitative analyses of the samples. The method allowed confirmation of genuineness. Enantioselective gas chromatography analyses confirmed the results, demonstrating the reliability of the method.

Measurement parameter selection for quantitative isotope dilution gas chromatography/mass spectrometry

International Nuclear Information System (INIS)

Colby, B.N.; Rosecrance, A.E.; Colby, M.E.

1981-01-01

By use of the two-isotope model of isotope dilution, selection criteria were developed for identifying optimum m/z's for quantitation of compounds by gas chromatography/mass spectrometry. In addition, it was possible to predict the optimum ratio of naturally abundant to labeled compound and to identify appropriate data reduction methods. The validity of these predictions was confirmed by using experimental GC/MS data for several organic compounds

Flash pyrolysis at high temperature of ligno-cellulosic biomass and its components - production of synthesis gas

International Nuclear Information System (INIS)

Couhert, C.

2007-11-01

Pyrolysis is the first stage of any thermal treatment of biomass and governs the formation of synthesis gas for the production of electricity, hydrogen or liquid fuels. The objective of this work is to establish a link between the composition of a biomass and its pyrolysis gas. We study experimental flash pyrolysis and fix the conditions in which quantities of gas are maximal, while aiming at a regime without heat and mass transfer limitations (particles about 100 μm): temperature of 950 C and residence time of about 2 s. Then we try to predict gas yields of any biomass according to its composition, applicable in this situation where thermodynamic equilibrium is not reached. We show that an additivity law does not allow correlating gas yields of a biomass with fractions of cellulose, hemi-cellulose and lignin contained in this biomass. Several explanations are suggested and examined: difference of pyrolytic behaviour of the same compound according to the biomass from which it is extracted, interactions between compounds and influence of mineral matter. With the aim of industrial application, we study pyrolysis of millimetric and centimetric size particles, and make a numerical simulation of the reactions of pyrolysis gases reforming. This simulation shows that the choice of biomass affects the quantities of synthesis gas obtained. (author)

Gas chromatography x gas chromatography-time-of-flight mass spectrometry analysis and antibacterial activity of essential oil from Amomum xanthophlebium

International Nuclear Information System (INIS)

Masila, A.; Aminah, I.; Yaakob, W.A.; Nazlina, I.

2011-01-01

Essential oils of fresh leaves, stem, rhizomes and whole aromatic plants of Amomum xanthophlebium (Zingiberaceae) were obtained by hydro distillation. Percentage yields of the leaf, stem and whole plant oils were 0.0032, 0.0074 and 0.0021 % whereas the rhizome oil obtained was very little. Chemical components of each oil and their percentages were determined by Gas Chromatography x Gas Chromatography-Time-of-Flight Mass Spectrometry (GCxGC-TOFMS). Analysis of A. xanthophlebium oils showed that they were dominated by terpenes. Main components in the leaves were allo-aromadendrene (3.41 %), (±)-globulol (2.58 %) and rosifoliol (2.55 %); stem, α-terpineol (4.25 %), rosifoliol (2.41 %) and bingpian (2.27 %); rhizomes, viridiflorol (5.72 %), (±)-globulol (5.23 %) and α-cadinol (4.81 %); whole plants, eucalyptol (4.11 %), l-α-terpineol (2.88 %) and rosifoliol (2.82 %). The stem oil of A. xanthophlebium showed antibacterial activity against Gram-negative Escherichia coli and Gram-positive methicillin-resistant Staphylococcus aureus (MRSA) at the minimum inhibitory concentration of 80 mg/ ml. (author)

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...

Formation of Methoxybenzenes from Cellulose in the Presence of Tetramethylammonium Hydroxide by Pyrolysis

International Nuclear Information System (INIS)

Choi, Sungseen; Kim, Minchul; Kim, Yunki

2013-01-01

Pyrolysis-gas chromatography/mass spectrometry (Pyrolysis-GC/MS) has been extensively used for characterizing the structural information of various macromolecules such as humic substances, woods, and synthetic polymers. Challinor improved the technique by introducing simultaneous pyrolysis and methylation with tetramethylammonium hydroxide (TMAH). As the technique offers a number of advantages over conventional pyrolysis, it has been used widely for the characterization of a wide variety of macro-organic molecules such as polysaccharides. Thermally assisted hydrolysis and methylation of carbohydrates by TMAH has been investigated. This approach has improved the separation by methylation of acidic functional group. Several researchers have demonstrated that the role of TMAH is not only the methylation of the pyrolysis products but also assisting in bond cleavage. Because TMAH possesses a strong basicity, highly basic conditions are likely to induce a variety of reactions. Pyrolysis technique using TMAH renders polar pyrolysis products volatile enough to be eluted from the GC column by subsequent online methylation

Solar coal gasification reactor with pyrolysis gas recycle

Science.gov (United States)

Aiman, William R.; Gregg, David W.

1983-01-01

Coal (or other carbonaceous matter, such as biomass) is converted into a duct gas that is substantially free from hydrocarbons. The coal is fed into a solar reactor (10), and solar energy (20) is directed into the reactor onto coal char, creating a gasification front (16) and a pyrolysis front (12). A gasification zone (32) is produced well above the coal level within the reactor. A pyrolysis zone (34) is produced immediately above the coal level. Steam (18), injected into the reactor adjacent to the gasification zone (32), reacts with char to generate product gases. Solar energy supplies the energy for the endothermic steam-char reaction. The hot product gases (38) flow from the gasification zone (32) to the pyrolysis zone (34) to generate hot char. Gases (38) are withdrawn from the pyrolysis zone (34) and reinjected into the region of the reactor adjacent the gasification zone (32). This eliminates hydrocarbons in the gas by steam reformation on the hot char. The product gas (14) is withdrawn from a region of the reactor between the gasification zone (32) and the pyrolysis zone (34). The product gas will be free of tar and other hydrocarbons, and thus be suitable for use in many processes.

Diesel characterization by high-resolution mass spectrometry - gas chromatography

International Nuclear Information System (INIS)

Baldrich, C.A

1998-01-01

High-resolution mass spectrometry-gas chromatography is combined with the HC22 method in order to obtain detailed information about the chemical composition of diesel and the distribution of different compound types in terms of its final boiling temperature from a single analysis. The total time elapsed from sample injection and signal processing to obtain final results is 90 minutes. This fact makes this methodology a new and very important tool for the decision making process concerning the most suitable final boiling temperature and the type of treatment of the product in order to obtain diesel that fulfills the international standards. The consistency and repeatability of the experimental results are demonstrated

Pyrolysis gas chromatographic study of homo polymers and copolymers of chlorotrifluoroethylene and styrene

International Nuclear Information System (INIS)

Rizvi, M.; Munir, A.

1993-01-01

Polymer degradation reactions have always been important for the development of thermally stable polymers. Among different available techniques, pyrolysis gas chromatography (PGC) has been used frequently to establish thermal stability and the plausible mechanism of degradation reactions. In the present work, homo polymers of chlorotrifluoroethylene (CTFE) and styrene and their copolymers were studied by PGC/IR for separation and identification of degraded products and to understand the degradation mechanism. Besides monomers, C/sub 2/H/sub 4/, C/sub 2/H/sub 2/, SiF/sub 4/, C/sub 6/H/sub 6/ C/sub 3/F/sub 5/Cl, C/sub 7/H sub 8/, C/sub 8/H/sub 10/ are the observed pyrolysis products. Mechanism for different degradation reactions have also been studied. (author)

Screening for estrogen residues in calf urine: Comparison of a validated yeast estrogen bioassay and gas chromatography-tandem mass spectrometry

NARCIS (Netherlands)

Nielen, M.W.F.; Bovee, T.F.H.; Heskamp, H.H.; Lasaroms, J.J.P.; Sanders, M.B.; Rhijn, van J.A.; Groot, M.J.; Hoogenboom, L.A.P.

2006-01-01

Within the European Union, the control for residues of illegal hormones in food-producing animals is based on urine analysis for a few target analytes using gas chromatography/mass spectrometry and/or liquid chromatography¿tandem mass spectrometry. Recently, we developed a robust yeast bioassay

Quality improvement of pyrolysis oil from waste rubber by adding sawdust

International Nuclear Information System (INIS)

Wang, Wen-liang; Chang, Jian-min; Cai, Li-ping; Shi, Sheldon Q.

2014-01-01

Highlights: • Rubber-pyrolysis oil is difficult to be fuel due to high proportion of PAHs. • The efficiency of pyrolysis was increased as the percentage of sawdust increased. • The adding of sawdust improved pyrolysis oil quality by reducing the PAHs content. • Adding sawdust reduced nitrogen/sulfur in oil and was easier to convert to diesel. - Abstract: This work was aimed at improving the pyrolysis oil quality of waste rubber by adding larch sawdust. Using a 1 kg/h stainless pyrolysis reactor, the contents of sawdust in rubber were gradually increased from 0%, 50%, 100% and 200% (wt%) during the pyrolysis process. Using a thermo-gravimetric (TG) analyzer coupled with Fourier transform infrared (FTIR) analysis of evolving products (TG–FTIR), the weight loss characteristics of the heat under different mixtures of sawdust/rubber were observed. Using the pyrolysis–gas chromatography (GC)–mass spectrometry (Py–GC/MS), the vapors from the pyrolysis processes were collected and the compositions of the vapors were examined. During the pyrolysis process, the recovery of the pyrolysis gas and its composition were measured in-situ at a reaction temperature of 450 °C and a retaining time of 1.2 s. The results indicated that the efficiency of pyrolysis was increased and the residual carbon was reduced as the percentage of sawdust increased. The adding of sawdust significantly improved the pyrolysis oil quality by reducing the polycyclic aromatic hydrocarbons (PAHs) and nitrogen and sulfur compounds contents, resulting in an improvement in the combustion efficiency of the pyrolysis oil

Quality improvement of pyrolysis oil from waste rubber by adding sawdust

Energy Technology Data Exchange (ETDEWEB)

Wang, Wen-liang [MOE Key Laboratory of Wooden Material Science and Application, College of Material Science and Technology, Wood Science and Technology, Beijing Forestry University, 100083 Beijing (China); Chang, Jian-min, E-mail: cjianmin@bjfu.edu.cn [MOE Key Laboratory of Wooden Material Science and Application, College of Material Science and Technology, Wood Science and Technology, Beijing Forestry University, 100083 Beijing (China); Cai, Li-ping [Mechanical and Energy Engineering Department, University of North Texas, 3940 N. Elm, Denton 72076, TX (United States); Shi, Sheldon Q., E-mail: Sheldon.Shi@unt.edu [Mechanical and Energy Engineering Department, University of North Texas, 3940 N. Elm, Denton 72076, TX (United States)

2014-12-15

Highlights: • Rubber-pyrolysis oil is difficult to be fuel due to high proportion of PAHs. • The efficiency of pyrolysis was increased as the percentage of sawdust increased. • The adding of sawdust improved pyrolysis oil quality by reducing the PAHs content. • Adding sawdust reduced nitrogen/sulfur in oil and was easier to convert to diesel. - Abstract: This work was aimed at improving the pyrolysis oil quality of waste rubber by adding larch sawdust. Using a 1 kg/h stainless pyrolysis reactor, the contents of sawdust in rubber were gradually increased from 0%, 50%, 100% and 200% (wt%) during the pyrolysis process. Using a thermo-gravimetric (TG) analyzer coupled with Fourier transform infrared (FTIR) analysis of evolving products (TG–FTIR), the weight loss characteristics of the heat under different mixtures of sawdust/rubber were observed. Using the pyrolysis–gas chromatography (GC)–mass spectrometry (Py–GC/MS), the vapors from the pyrolysis processes were collected and the compositions of the vapors were examined. During the pyrolysis process, the recovery of the pyrolysis gas and its composition were measured in-situ at a reaction temperature of 450 °C and a retaining time of 1.2 s. The results indicated that the efficiency of pyrolysis was increased and the residual carbon was reduced as the percentage of sawdust increased. The adding of sawdust significantly improved the pyrolysis oil quality by reducing the polycyclic aromatic hydrocarbons (PAHs) and nitrogen and sulfur compounds contents, resulting in an improvement in the combustion efficiency of the pyrolysis oil.

Tracking juniper berry content in oils and distillates by spectral deconvolution of gas chromatography/mass spectrometry data.

Science.gov (United States)

Robbat, Albert; Kowalsick, Amanda; Howell, Jessalin

2011-08-12

The complex nature of botanicals and essential oils makes it difficult to identify all of the constituents by gas chromatography/mass spectrometry (GC/MS) alone. In this paper, automated sequential, multidimensional gas chromatography/mass spectrometry (GC-GC/MS) was used to obtain a matrix-specific, retention time/mass spectrometry library of 190 juniper berry oil compounds. GC/MS analysis on stationary phases with different polarities confirmed the identities of each compound when spectral deconvolution software was used to analyze the oil. Also analyzed were distillates of juniper berry and its oil as well as gin from four different manufacturers. Findings showed the chemical content of juniper berry can be traced from starting material to final product and can be used to authenticate and differentiate brands. Copyright © 2011 Elsevier B.V. All rights reserved.

Pyrolysis of a waste from the grinding of scrap tyres.

Science.gov (United States)

Fernández, A M; Barriocanal, C; Alvarez, R

2012-02-15

The fibres that are used to reinforce tyres can be recovered as a waste in the process of grinding of scrap tyres. In this paper beneficiation through pyrolysis is studied since the fibres are made up of polymers with a small amount of rubber because the latter is difficult to separate. The experiments were performed at three temperatures (400, 550 and 900°C) in a horizontal oven. The three products - gas, oil and char - obtained from the pyrolysis were investigated. The composition of the gas was analyzed by means of gas chromatography. The oil was studied by gas chromatography and infrared spectroscopy. The char porous structure was determined by N(2) adsorption. In addition, the topography of the chars was studied by means of scanning electron microscopy (SEM). The products resulting from the pyrolysis of the fibres were compared with those obtained from scrap rubber. Copyright © 2011 Elsevier B.V. All rights reserved.

A fast, comprehensive screening method for doping agents in urine by gas chromatography-triple quadrupole mass spectrometry.

Science.gov (United States)

Van Eenoo, Peter; Van Gansbeke, Wim; De Brabanter, Nik; Deventer, Koen; Delbeke, Frans T

2011-05-27

The use of performance enhancing drugs in sports is prohibited. For the detection of misuse of such substances gas chromatography or liquid chromatography coupled to mass spectrometry are the most frequently used detection techniques. In this work the development and validation of a fast gas chromatography tandem mass spectrometric method for the detection of a wide range of doping agents is described. The method can determine 13 endogenous steroids (the steroid profile), 19-norandrosterone, salbutamol and 11-nor-Δ9-tetrahydrocannabinol.9carboxylic acid in the applicable ranges and to detect qualitatively over 140 substances in accordance with the minimum required performance levels of the World Anti-Doping Agency in 1ml of urine. The classes of substances included in the method are anabolic steroids, β2-agonists, stimulants, narcotics, hormone antagonists and modulators and beta-blockers. Moreover, using a short capillary column and hydrogen as a carrier gas the run time of the method is less than 8min. Copyright © 2010 Elsevier B.V. All rights reserved.

Estimation of brassylic acid by gas chromatography-mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Mohammed J. Nasrullah, Erica N. Pfarr, Pooja Thapliyal, Nicholas S. Dusek, Kristofer L. Schiele, Christy Gallagher-Lein, and James A. Bahr

2010-10-29

The main focus of this work is to estimate Brassylic Acid (BA) using gas chromatography-mass spectrometry (GC-MS). BA is a product obtained from the oxidative cleavage of Erucic Acid (EA). BA has various applications for making nylons and high performance polymers. BA is a 13 carbon compound with two carboxylic acid functional groups at the terminal end. BA has a long hydrocarbon chain that makes the molecule less sensitive to some of the characterization techniques. Although BA can be characterized by NMR, both the starting material (EA) and products BA and nonanoic acid (NA) have peaks at similar {delta}, ppm values. Hence it becomes difficult for the quick estimation of BA during its synthesis.

Differentiation of endogenous and exogenous steroids by gas chromatography-combustion-mass spectrometry isotope ratio

International Nuclear Information System (INIS)

Montes de Oca Porto, Rodny; Rosado Perez, Aristides; Correa Vidal, Margarita Teresa

2007-01-01

Urinary steroids profiles are used to control the misuse of endogenous steroids such as testosterone and dihydrotestosterone. The testosterone/epistestosterone ratio, measured by Gas Chromatography-Mass Spectrometry, is used to control testosterone administration. When T/E ratio is higher than 4, consumption of testosterone or its precursors is suspected. Recent researches have demonstrated the effectiveness of Carbon Isotope Ratio Mass Spectrometry to detect and confirm endogenous steroids administration. The ratio of the two stable carbon isotopes 1 3 C and 1 2 C allows the differentiation of natural and synthetic steroids because synthetic steroids have lower 1 3 C abundance. In fact, the carbon isotope ratios can be used to determine endogenous steroids administration even when testosterone/epistestosterone ratio is at its normal value. In the current work, some of the most important aspects related to differentiation of endogenous and exogenous steroids by means of Gas Chromatography-Combustion-Isotope Ratio Mass Spectrometry are discussed. Also, this article provides a review about the purification and sample preparation previous to the analysis, and diet effects on carbon isotope ratio of endogenous anabolics steroids is presented too

Profiling of volatile organic compounds produced by clinical Aspergillus isolates using gas chromatography-mass spectrometry

NARCIS (Netherlands)

Gerritsen, M G; Brinkman, P; Escobar Salazar, Natalia; Bos, L D; de Heer, K; Meijer, M; Janssen, H-G; de Cock, H; Wösten, H A B; Visser, C.E.; van Oers, M H J; Sterk, P J

Volatile organic compounds (VOCs) in exhaled breath may identify the presence of invasive pulmonary aspergillosis. We aimed to detect VOC profiles emitted by in vitro cultured, clinical Aspergillus isolates using gas chromatography-mass spectrometry (GC-MS). Three clinical Aspergillus isolates and a

Profiling of volatile organic compounds produced by clinical Aspergillus isolates using gas chromatography-mass spectrometry

NARCIS (Netherlands)

Gerritsen, M. G.; Brinkman, P.; Escobar, N.; Bos, L. D.; de Heer, K.; Meijer, M.; Janssen, H.-G.; de Cock, H.; Wösten, H. A. B.; Visser, C. E.; van Oers, M. H. J.; Sterk, P. J.

2018-01-01

Volatile organic compounds (VOCs) in exhaled breath may identify the presence of invasive pulmonary aspergillosis. We aimed to detect VOC profiles emitted by in vitro cultured, clinical Aspergillus isolates using gas chromatography-mass spectrometry (GC-MS). Three clinical Aspergillus isolates and a

Quantitative Analysis of Tetramethylenedisulfotetramine ("Tetramine") Spiked into Beverages by Liquid Chromatography Tandem Mass Spectrometry with Validation by Gas Chromatography Mass Spectrometry

Energy Technology Data Exchange (ETDEWEB)

Owens, J; Hok, S; Alcaraz, A; Koester, C

2008-11-13

Tetramethylenedisulfotetramine, commonly known as tetramine, is a highly neurotoxic rodenticide (human oral LD{sub 50} = 0.1 mg/kg) used in hundreds of deliberate food poisoning events in China. Here we describe a method for quantitation of tetramine spiked into beverages, including milk, juice, tea, cola, and water and cleaned up by C8 solid phase extraction and liquid-liquid extraction. Quantitation by high performance liquid chromatography tandem mass spectrometry (LC/MS/MS) was based upon fragmentation of m/z 347 to m/z 268. The method was validated by gas chromatography mass spectrometry (GC/MS) operated in SIM mode for ions m/z 212, 240, and 360. The limit of quantitation was 0.10 {micro}g/mL by LC/MS/MS versus 0.15 {micro}g/mL for GC/MS. Fortifications of the beverages at 2.5 {micro}g/mL and 0.25 {micro}g/mL were recovered ranging from 73-128% by liquid-liquid extraction for GC/MS analysis, 13-96% by SPE and 10-101% by liquid-liquid extraction for LC/MS/MS analysis.

Quantitative Analysis of Tetramethylenedisulfotetramine ('Tetramine') Spiked into Beverages by Liquid Chromatography Tandem Mass Spectrometry with Validation by Gas Chromatography Mass Spectrometry

International Nuclear Information System (INIS)

Owens, J.; Hok, S.; Alcaraz, A.; Koester, C.

2008-01-01

Tetramethylenedisulfotetramine, commonly known as tetramine, is a highly neurotoxic rodenticide (human oral LD 50 = 0.1 mg/kg) used in hundreds of deliberate food poisoning events in China. Here we describe a method for quantitation of tetramine spiked into beverages, including milk, juice, tea, cola, and water and cleaned up by C8 solid phase extraction and liquid-liquid extraction. Quantitation by high performance liquid chromatography tandem mass spectrometry (LC/MS/MS) was based upon fragmentation of m/z 347 to m/z 268. The method was validated by gas chromatography mass spectrometry (GC/MS) operated in SIM mode for ions m/z 212, 240, and 360. The limit of quantitation was 0.10 (micro)g/mL by LC/MS/MS versus 0.15 (micro)g/mL for GC/MS. Fortifications of the beverages at 2.5 (micro)g/mL and 0.25 (micro)g/mL were recovered ranging from 73-128% by liquid-liquid extraction for GC/MS analysis, 13-96% by SPE and 10-101% by liquid-liquid extraction for LC/MS/MS analysis.

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

Metabolomics by Gas Chromatography-Mass Spectrometry: the combination of targeted and untargeted profiling

Science.gov (United States)

Fiehn, Oliver

2016-01-01

Gas chromatography-mass spectrometry (GC-MS)-based metabolomics is ideal for identifying and quantitating small molecular metabolites (metabolomics easily allows integrating targeted assays for absolute quantification of specific metabolites with untargeted metabolomics to discover novel compounds. Complemented by database annotations using large spectral libraries and validated, standardized standard operating procedures, GC-MS can identify and semi-quantify over 200 compounds per study in human body fluids (e.g., plasma, urine or stool) samples. Deconvolution software enables detection of more than 300 additional unidentified signals that can be annotated through accurate mass instruments with appropriate data processing workflows, similar to liquid chromatography-MS untargeted profiling (LC-MS). Hence, GC-MS is a mature technology that not only uses classic detectors (‘quadrupole’) but also target mass spectrometers (‘triple quadrupole’) and accurate mass instruments (‘quadrupole-time of flight’). This unit covers the following aspects of GC-MS-based metabolomics: (i) sample preparation from mammalian samples, (ii) acquisition of data, (iii) quality control, and (iv) data processing. PMID:27038389

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.

Stable carbon isotopic composition of gasolines determined by isotope ratio monitoring gas chromatography mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Smallwood, B.J.; Philp, R.P.; Allen, J.D. [University of Oklahoma, Norman, OK (United States). School of Geology and Geophysics

2002-07-01

A large number of underground gasoline storage facilities in the United States continuously leak gasoline into the subsurface, which makes gasoline a major groundwater contaminant. Gas chromatography (GC) and gas chromatography-mass spectrometry (GC-MS) are used currently to characterize contaminated groundwater and soils. Correlations of contaminants with suspected source(s) are extremely difficult by these techniques because many gasolines have similar hydrocarbon distributions. The present study applied the technique of isotope ratio monitoring gas chromatography-mass spectrometry (irmGC-MS) to 19 gasoline samples from different areas of the USA. This allows a much better correlation of gasoline contaminants to source. Data obtained indicate a wide range of {sup {delta}}{sup 13}C values for 16 ubiquitous compounds in the gasolines. The majority of samples could be distinguished from each other on the basis of {sup {delta}}{sup 13}C hydrocarbon composition. The oxygenated additive methyl tertiary butyl ether (MTBE) was present in ten of the gasolines analyzed, and had a relatively narrow range of {sup {delta}}{sup 13}C values (-30.4 to -28.3 per mille). Preliminary investigations were also made to determine the extent of carbon isotopic fractionation after simple water washing and evaporation experiments. Results indicate that the majority of compounds did not undergo significant carbon isotopic fractionation as a result of these processes. (author)

Detection of Stimulants and Narcotics by Liquid Chromatography-Tandem Mass Spectrometry and Gas Chromatography-Mass Spectrometry for Sports Doping Control.

Science.gov (United States)

Ahrens, Brian D; Kucherova, Yulia; Butch, Anthony W

2016-01-01

Sports drug testing laboratories are required to detect several classes of compounds that are prohibited at all times, which include anabolic agents, peptide hormones, growth factors, beta-2 agonists, hormones and metabolic modulators, and diuretics/masking agents. Other classes of compounds such as stimulants, narcotics, cannabinoids, and glucocorticoids are also prohibited, but only when an athlete is in competition. A single class of compounds can contain a large number of prohibited substances and all of the compounds should be detected by the testing procedure. Since there are almost 70 stimulants on the prohibited list it can be a challenge to develop a single screening method that will optimally detect all the compounds. We describe a combined liquid chromatography-tandem mass spectrometry (LC-MS/MS) and gas chromatography-mass spectrometry (GC-MS) testing method for detection of all the stimulants and narcotics on the World Anti-Doping Agency prohibited list. Urine for LC-MS/MS testing does not require sample pretreatment and is a direct dilute and shoot method. Urine samples for the GC-MS method require a liquid-liquid extraction followed by derivatization with trifluoroacetic anhydride.

Influence of reaction parameters on brown coal-polyolefinic plastic co-pyrolysis behavior

Energy Technology Data Exchange (ETDEWEB)

Sharypov, V.I.; Beregovtsova, N.G.; Kuznetsov, B.N. [Institute of Chemistry and Chemical Technology SB RAS, K.Marx Str. 42, 660049 Krasnoyarsk (Russian Federation); Cebolla, V.L. [Instituto de Carboquimica, CSIC, Miguel Luesma, 4, 50015 Zaragoza (Spain); Collura, S.; Finqueneisel, G.; Zimny, T.; Weber, J.V. [Laboratoire de Chimie et Applications, Universite de Metz, rue V.Demange, 57500 Saint-Avold (France)

2007-03-15

Co-processing of polyolefinic polymers with Kansk-Achinsk (Russia) brown coal was investigated by thermogravimetry (TG) and autoclave pyrolysis under argon and hydrogen pressure in catalytic conditions (or not). Gas chromatography-mass spectrometry (GC-MS) and high performance thin layer chromatography (HPTLC) were used to analyze the distillate products. Some synergistic effects indicate chemical interaction between the products of thermal decomposition of coal and plastic. In co-pyrolysis under H{sub 2} a significant increasing of coal conversion degree as a function of polymer amount in feedstock was found. Simultaneously the coal promoted formation of distillate products from polymers. Some alkyl aromatic and O-containing substances were detected in co-pyrolysis fraction boiling in the range 180-350 C, indicating interactions between coal and plastic. Iron containing ore materials, modified by mechanochemical treatment, demonstrated a catalytic activity in hydropyrolysis process. In catalytic conditions, increases of the mixtures conversion degree by 9-13 wt.%, of distillate fraction yields by 1.2-1.6 times and a decrease of olefins and polycyclic components were observed. (author)

Gas Chromatography-Mass Spectrometric Analysis of Nematicidal ...

African Journals Online (AJOL)

Purpose: To investigate the chemical composition and nematicidal activity of the essential oil of. Valeriana amurensis ... Methods: The essential oil of V. amurensis roots was obtained by hydrodistillation and analyzed by gas chromatography (GC) ..... Aβ1-40 and Caspase-3 in Alzheimer's disease model rat's brain. J Chin ...

Application of time-of-flight mass spectrometry with laser-based photoionization methods for analytical pyrolysis of PVC

Energy Technology Data Exchange (ETDEWEB)

Streibel, T.; Muehlberger, F. [GSF - Forschungszentrum fuer Umwelt und Gesundheit GmbH, Neuherberg (Germany); Adam, T.; Zimmermann, R. [Augsburg Univ. (Germany); Cao, L. [National Center for Iron and Steel, Beijing, BJ (China)

2004-09-15

Chlorinated benzenes and phenols generated from PVC pyrolysis are known to be precursors of PCDD/F formation. Therefore, selective and sensitive monitoring of these substances during PVC pyrolysis processes on an on-line, real-time basis could be very useful for the understanding of PCDD/F formation pathways. In this study, we investigated the pyrolysis gas from PVC samples derived from steel recycling by means of simultaneous single photon ionization/resonance-enhanced multiphoton ionization time-of-flight mass spectrometry (SPI/REMPI-TOFMS). The application of these soft photo-ionization techniques in mass spectrometry enables a fast and comprehensive analysis of this complex matrix without generating fragment ions, which would interfere with molecule ions making interpretation of the obtained mass spectra very difficult.

Unique distributions of hydrocarbons and sulphur compounds released by flash pyrolysis from the fossilised alga Gloeocapsomorpha prisca, a major constituent in one of four Ordovician kerogens

NARCIS (Netherlands)

Sinninghe Damsté, J.S.; Douglas, A.G.; Fowler, M.G.; Eglinton, T.I.

1991-01-01

Kerogens isolated from four rocks of Ordovician age from North America have been analysed by combined pyrolysis-gas chromatography-mass spectrometry to compare and contrast the type and distribution of sulphur-containing compounds and aromatic and aliphatic hydrocarbons present in the

Gas chromatography at the Tritium Laboratory Karlsruhe

International Nuclear Information System (INIS)

Laesser, R.; Gruenhagen, S.

2003-08-01

Among the analytical techniques (mass spectrometry, laser Raman spectroscopy, gas chromatography, use of ionisation chambers) employed at the Tritium Laboratory Karlsruhe (TLK), gas chromatography plays a prominent role. The main reasons for that are the simplicity of the gas chromatographic separation process, the small space required for the equipment, the low investment costs in comparison to other methods, the robustness of the equipment, the simple and straightforward analysis and the fact that all gas species of interest (with the exception of water) can easily be detected by gas chromatographic means. The conventional gas chromatographs GC1 and GC2 used in the Tritium Measurement Techniques (TMT) System of the TLK and the gas chromatograph GC3 of the experiment CAPER are presented in detail, by discussing their flow diagrams, their major components, the chromatograms measured by means of various detectors, shortcomings and possible improvements. One of the main disadvantages of the conventional gas chromatography is the long retention times required for the analysis of hydrogen gas mixtures. To overcome this disadvantage, micro gas chromatography for hydrogen analysis was developed. Reduction of the retention times by one order of magnitude was achieved. (orig.)

Authenticity assessment of gamma- and delta-decalactone from prunus fruits by gas chromatography combustion/pyrolysis isotope ratio mass spectrometry (GC-C/P-IRMS).

Science.gov (United States)

Tamura, Hirotoshi; Appel, Markus; Richling, Elke; Schreier, Peter

2005-06-29

Authenticity assessment of gamma-decalactone (1) and delta-decalactone (2) from peach (Prunus persica var. persica), apricot (Prunus armeniaca), and nectarine (Prunus persica var. nectarina) was performed using gas chromatography-isotope ratio mass spectrometry (GC-IRMS) in the combustion (C) and pyrolysis (P) mode. In addition, commercially available synthetic (nature-identical) 1 and 2 as well as biotechnologically produced samples (declared to be "natural") were characterized by their delta(2)H(V)(-)(SMOW) and delta(13)C(V)(-)(PDB) values. For the Prunus fruits under study, rather narrow ranges of delta(13)C(V)(-)(PDB) and delta(2)H(V)(-)(SMOW) data of 1, varying from - 34.6 per thousand to - 38.4 per thousand and -160 per thousand to -206 per thousand, respectively, were obtained. Synthetic references of 1 showed delta(13)C(V)(-)(PDB) and delta(2)H(V)(-)(SMOW) data ranging from -27.4 per thousand to -28.3 per thousand and -151 per thousand to -184 per thousand, respectively. Samples of 1 declared to be "natural" exhibited ranges from -28.1 per thousand to -29.2 per thousand and -192 per thousand to -286 per thousand for delta(13)C(V)(-)(PDB) and delta(2)H(V)(-)(SMOW), respectively. For 2 from peach, apricot, and nectarine, delta(13)C(V)(-)(PDB) values ranging from -34.0 per thousand to -37.9 per thousand were determined; the delta(2)H(V)(-)(SMOW) values ranged from -171 per thousand to -228 per thousand. The delta(13)C(V)(-)(PDB) and delta(2)H(V)(-)(SMOW) data for synthetic 2 were -28.2 per thousand and -171 per thousand, respectively, that is, similar to those of 2 from "natural" origin, ranging from -27.7 per thousand to -30.1 per thousand and -185 per thousand to -230 per thousand for delta(13)C(V)(-)(PDB) and delta(2)H(V)(-)(SMOW), respectively. GC-C/P-IRMS allowed clear-cut analytical differentiation of the synthetic and "ex-plant" origin of 1 and 2, whereas narrow ranges of delta(13)C(V)(-)(PDB) and delta(2)H(V)(-)(SMOW) data were found for samples of

Coal pyrolysis under synthesis gas, hydrogen and nitrogen

Energy Technology Data Exchange (ETDEWEB)

Ariunaa, A.; Li Bao-Qing; Li Wen; Purevsuren, B. (and others) [Chinese Academy of Sciences, Taiyuan (China)

2007-02-15

Chinese Xundian, Mongolian Shiveeovoo lignites and Khoot oil shale are pyrolyzed under synthesis gas (SG) at temperature range from 400 to 800{sup o}C for lignite and from 300 to 600{sup o}C for oil shale with heating rate of 10{sup o}C/min in a fixed bed reactor. The results were compared with those obtained by pyrolysis under hydrogen and nitrogen. The results showed that unlike pyrolysis at high pressure, there are only slight different in the yields of char and tar among pyrolyses under various gases at room pressure for lignite, while higher liquid yield with lower yields of char and gas was obtained in pyrolysis of oil shale under SG and H{sub 2} than under N{sub 2}. It is found that the pyrite S can be easily removed to partially convert to organic S under various gaseous atmosphere and the total sulfur removal for oil shale is much less than lignite, which might be related to its high ash content. The higher total sulfur removal and less organic S content in the presence of SG in comparison with those under N{sub 2} and even under H{sub 2} in pyrolysis of Xundian lignite might result from the action of CO in SG. However, CO does not show its function in pyrolysis of Khoot oil shale, which might also be related to the high ash content. The results reported show the possibility of using synthesis gas instead of pure hydrogen as the reactive gas for coal hydropyrolysis. 11 refs., 4 figs., 6 tabs.

Validation of a confirmatory method for the determination of melamine in egg by gas chromatography-mass spectrometry and ultra-performance liquid chromatography-tandem mass spectrometry

International Nuclear Information System (INIS)

Xia Xi; Ding Shuangyang; Li Xiaowei; Gong Xiao; Zhang Suxia; Jiang Haiyang; Li Jiancheng; Shen Jianzhong

2009-01-01

A sensitive and reliable method was developed and validated for detection and confirmation of melamine in egg based on gas chromatography-mass spectrometry (GC-MS) and ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Trichloroacetic acid solution was used for sample extraction and precipitation of proteins. The aqueous extracts were subjected to solid-phase extraction by mixed-mode reversed-phase/strong cation-exchange cartridges. Using ultra-performance liquid chromatography and electrospray ionization in the positive ion mode, melamine was determined by LC-MS/MS, which was completed in 5 min for each injection. For the GC-MS analysis, extracted melamine was derivatized with N,O-bis(trimethylsilyl)trifluoracetamide prior to selected ion monitoring detection in electron impact mode. The average recovery of melamine from fortified samples ranged from 85.2% to 103.2%, with coefficients of variation lower than 12%. The limit of detection obtained by GC-MS and UPLC-MS/MS was 10 and 5 μg kg -1 , respectively. This validated method was successfully applied to the determination of melamine in real samples from market.

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.

Phytochemical analyses of Ziziphus jujuba Mill. var. spinosa seed by ultrahigh performance liquid chromatography-tandem mass spectrometry and gas chromatography-mass spectrometry.

Science.gov (United States)

Yang, Bao; Yang, Hongshun; Chen, Feng; Hua, Yanglin; Jiang, Yueming

2013-11-21

Ziziphus jujuba Mill. var. spinosa (Z. jujuba) seeds have attracted much attention within the field of medicine due to their significant effects against disturbances of the central nervous system. Secondary metabolites composition is key to the influence of the pharmaceutical and commercial qualities of this plant. In this work, the phytochemical profile of Z. jujuba seeds was analysed by ultrahigh performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) and gas chromatography-mass spectrometry (GC-MS). The UPLC-MS/MS information identified the main secondary metabolites in Z. jujuba seeds, including flavonoid C-glycosides, triterpene acids and unsaturated fatty acids. The leading chemical identified by UPLC-MS/MS was betulinic acid, and oleic acid was the leading volatile from the GC-MS results. All the samples tested showed similar phytochemical profiles, but levels of the chemical compounds varied. Principal component analysis revealed the principal secondary metabolites that could define the differences in quality. It was confirmed that the combination of UPLC-MS/MS and GC-MS was an effective technique to demonstrate the pharmaceutical quality of Z. jujuba seeds.

Thermodynamic analyses of hydrogen production from sub-quality natural gas. Part I: Pyrolysis and autothermal pyrolysis

Science.gov (United States)

Huang, Cunping; T-Raissi, Ali

Sub-quality natural gas (SQNG) is defined as natural gas whose composition exceeds pipeline specifications of nitrogen, carbon dioxide (CO 2) and/or hydrogen sulfide (H 2S). Approximately one-third of the U.S. natural gas resource is sub-quality gas [1]. Due to the high cost of removing H 2S from hydrocarbons using current processing technologies, SQNG wells are often capped and the gas remains in the ground. We propose and analyze a two-step hydrogen production scheme using SQNG as feedstock. The first step of the process involves hydrocarbon processing (via steam-methane reformation, autothermal steam-methane reformation, pyrolysis and autothermal pyrolysis) in the presence of H 2S. Our analyses reveal that H 2S existing in SQNG is stable and can be considered as an inert gas. No sulfur dioxide (SO 2) and/or sulfur trioxide (SO 3) is formed from the introduction of oxygen to SQNG. In the second step, after the separation of hydrogen from the main stream, un-reacted H 2S is used to reform the remaining methane, generating more hydrogen and carbon disulfide (CS 2). Thermodynamic analyses on SQNG feedstock containing up to 10% (v/v) H 2S have shown that no H 2S separation is required in this process. The Part I of this paper includes only thermodynamic analyses for SQNG pyrolysis and autothermal pyrolysis.

Characterization of some sedimentary sequences from Cambay basin, India, by pyrolysis-GC

Science.gov (United States)

Philp, R. P.; Garg, A. K.

Pyrolysis-gas chromatography of sedimentary sequences from a key exploratory well of the southern Cambay Basin, India, has been performed to characterize the nature of the source material and its maturity. In samples from the Eocene-Paleocene section (2960-3407 m), the pyrolysate is dominated by hydrocarbons in the lower molecular weight region indicating a significant input algal source material. The presence of various xylenes and phenols in the pyrograms is indicative of a significant input from higher plant material. The organic material in this section is interpreted to have been derived from marine-terrestrial source inputs deposited under swampy to marine and reducing environments. Good mature source rocks with type III kerogens which are wet gas/gas condensate-prone have been identified in this region. This paper intends to discuss the characterization of source rocks using the pyrolysis-gas chromatography approach and the significance of the distribution of the pyrolysis product.

Study of radiolysis products of natural organic materials by means of gas chromatography

International Nuclear Information System (INIS)

Pogocki, D.

1994-01-01

Analytical methods based on gas chromatography for identification determination of products arising during food irradiation have been presented. Behind the classics version of the methods one has shown also combined methods being the on-line connection of gas chromatography with mass spectroscopy as well as gas chromatography with liquid chromatography and mass spectroscopy. The applicability as well as weakness and advantages of each version have been discussed on the context of food irradiation. 11 refs, 7 figs

Non-polar lipids characterization of Quinoa (Chenopodium quinoa) seed by comprehensive two-dimensional gas chromatography with flame ionization/mass spectrometry detection and non-aqueous reversed-phase liquid chromatography with atmospheric pressure chemical ionization mass spectrometry detection.

Science.gov (United States)

Fanali, Chiara; Beccaria, Marco; Salivo, Simona; Tranchida, Peter; Tripodo, Giusy; Farnetti, Sara; Dugo, Laura; Dugo, Paola; Mondello, Luigi

2015-07-08

A chemical characterization of major lipid components, namely, triacylglycerols, fatty acids and the unsaponifiable fraction, in a Quinoa seed lipids sample is reported. To tackle such a task, non-aqueous reversed-phase high-performance liquid chromatography with mass spectrometry detection was employed. The latter was interfaced with atmospheric pressure chemical ionization for the analysis of triacylglycerols. The main triacylglycerols (>10%) were represented by OLP, OOL and OLL (P = palmitoyl, O = oleoyl, L = linoleoyl); the latter was present in the oil sample at the highest percentage (18.1%). Furthermore, fatty acid methyl esters were evaluated by gas chromatography with flame ionization detection. 89% of the total fatty acids was represented by unsaturated fatty acid methyl esters with the greatest percentage represented by linoleic and oleic acids accounting for approximately 48 and 28%, respectively. An extensive characterization of the unsaponifiable fraction of Quinoa seed lipids was performed for the first time, by using comprehensive two-dimensional gas chromatography with dual mass spectrometry/flame ionization detection. Overall, 66 compounds of the unsaponifiable fraction were tentatively identified, many constituents of which (particularly sterols) were confirmed by using gas chromatography with high-resolution time-of-flight mass spectrometry. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Characterization of bio-oil from induction-heating pyrolysis of food-processing sewage sludges using chromatographic analysis.

Science.gov (United States)

Tsai, Wen-Tien; Lee, Mei-Kuei; Chang, Jeng-Hung; Su, Ting-Yi; Chang, Yuan-Ming

2009-05-01

In this study, gas chromatography-mass spectrometry (GC-MS) was used to analyze the pyrolytic bio-oils and gas fractions derived from the pyrolysis of industrial sewage sludges using induction-heating technique. The liquid products were obtained from the cryogenic condensation of the devolatilization fraction in a nitrogen atmosphere using a heating rate of 300 degrees C/min ranging from 25 to 500 degrees C. The analytical results showed that the pyrolysis bio-oils were very complex mixtures of organic compounds and contained a lot of nitrogenated and/or oxygenated compounds such as aliphatic hydrocarbons, phenols, pyridines, pyrroles, amines, ketones, and so on. These organic hydrocarbons containing nitrogen and/or oxygen should originate from the protein and nucleic acid textures of the microbial organisms present in the sewage sludge. The non-condensable devolatilization fractions were also composed of nitrogenated and oxygenated compounds, but contained small fractions of phenols, 1H-indoles, and fatty carboxylic acids. On the other hand, the compositions in the non-condensable gas products were principally carbon dioxide, carbon monoxide and methane analyzed by gas chromatography-thermal conductivity detector (GC-TCD).

ANALYSIS OF ARTEMISININ AND RELATED SESQUITERPENOIDS FROM ARTEMISIA-ANNUA L BY COMBINED GAS-CHROMATOGRAPHY MASS-SPECTROMETRY

NARCIS (Netherlands)

WOERDENBAG, HJ; PRAS, N; BOS, R; VISSER, JF; HENDRIKS, H; MALINGRE, TM

1991-01-01

The sesquiterpenoid artemisinin (3) and its biosynthetic precursors arteannuic acid (1), arteannuin B (2) and artemisitene (4) can be separated and identified by combined gas chromatography/mass spectrometry both as a mixture of reference standards as well as in extracts of Artemisia annua L. From

Thermogravimetric and Pyrolysis-Capillary Gas Chromatography-Mass Spectrometric Analysis of Pinus Halepensis Mill. Wood

International Nuclear Information System (INIS)

Hafsi, S.; Benbouzid, M.; Zimny, T.

2005-01-01

The analytical methods TG and Py-capillary-GC-MS were used to study the thermal degradation of Pinus Halepensis Mill. wood. The TG analysis in air and in nitrogen showed that the percentage content of char and ash were, 23.1% and 7.7% respectively. TG and DTG analysis proved that the evolution of organic degradation products occurs mainly between 215C and 380C and has its maximum evolution rate at 360C in nitrogen and 347C in air. Py-capillary-GC-MS analysis of the pyrolysis at 400C identified the presence of valuable chemicals such aliphatic and aromatic hydrocarbons, phenols, aldehydes, esters and saturated and unsaturated long chain fatty acids. (author)

Gas chromatography with simultaneous detection: Ultraviolet spectroscopy, flame ionization, and mass spectrometry.

Science.gov (United States)

Gras, Ronda; Luong, Jim; Haddad, Paul R; Shellie, Robert A

2018-05-08

An effective analytical strategy was developed and implemented to exploit the synergy derived from three different detector classes for gas chromatography, namely ultraviolet spectroscopy, flame ionization, and mass spectrometry for volatile compound analysis. This strategy was achieved by successfully hyphenating a user-selectable multi-wavelength diode array detector featuring a positive temperature coefficient thermistor as an isothermal heater to a gas chromatograph. By exploiting the non-destructive nature of the diode array detector, the effluent from the detector was split to two parallel detectors; namely a quadrupole mass spectrometer and a flame ionization detector. This multi-hyphenated configuration with the use of three detectors is a powerful approach not only for selective detection enhancement but also for improvement in structural elucidation of volatile compounds where fewer fragments can be obtained or for isomeric compound analysis. With the diode array detector capable of generating high resolution gas phase spectra, the information collected provides useful confirmatory information without a total dependence on the chromatographic separation process which is based on retention time. This information-rich approach to chromatography is achieved without incurring extra analytical time, resulting in improvements in compound identification accuracy, analytical productivity, and cost. Chromatographic performance obtained from model compounds was found to be acceptable with a relative standard deviation of the retention times of less than 0.01% RSD, and a repeatability at two levels of concentration of 100 and 1000 ppm (v/v) of less than 5% (n = 10). With this configuration, correlation of data between the three detectors was simplified by having near identical retention times for the analytes studied. Copyright © 2018 Elsevier B.V. All rights reserved.

Fast Pyrolysis of Four Lignins from Different Isolation Processes Using Py-GC/MS

Directory of Open Access Journals (Sweden)

Xiaona Lin

2015-06-01

Full Text Available Pyrolysis is a promising approach that is being investigated to convert lignin into higher value products including biofuels and phenolic chemicals. In this study, fast pyrolysis of four types of lignin, including milled Amur linden wood lignin (MWL, enzymatic hydrolysis corn stover lignin (EHL, wheat straw alkali lignin (AL and wheat straw sulfonate lignin (SL, were performed using pyrolysis gas-chromatography/mass spectrometry (Py-GC/MS. Thermogravimetric analysis (TGA showed that the four lignins exhibited widely different thermolysis behaviors. The four lignins had similar functional groups according to the FTIR analysis. Syringyl, guaiacyl and p-hydroxyphenylpropane structural units were broken down during pyrolysis. Fast pyrolysis product distributions from the four lignins depended strongly on the lignin origin and isolation process. Phenols were the most abundant pyrolysis products from MWL, EHL and AL. However, SL produced a large number of furan compounds and sulfur compounds originating from kraft pulping. The effects of pyrolysis temperature and time on the product distributions from corn stover EHL were also studied. At 350 °C, EHL pyrolysis mainly produced acids and alcohols, while phenols became the main products at higher temperature. No obvious influence of pyrolysis time was observed on EHL pyrolysis product distributions.

Evaluation of co-pyrolysis petrochemical wastewater sludge with lignite in a thermogravimetric analyzer and a packed-bed reactor: Pyrolysis characteristics, kinetics, and products analysis.

Science.gov (United States)

Mu, Lin; Chen, Jianbiao; Yao, Pikai; Zhou, Dapeng; Zhao, Liang; Yin, Hongchao

2016-12-01

Co-pyrolysis characteristics of petrochemical wastewater sludge and Huolinhe lignite were investigated using thermogravimetric analyzer and packed-bed reactor coupled with Fourier transform infrared spectrometer and gas chromatography. The pyrolysis characteristics of the blends at various sludge blending ratios were compared with those of the individual materials. Thermogravimetric experiments showed that the interactions between the blends were beneficial to generate more residues. In packed-bed reactor, synergetic effects promoted the release of gas products and left less liquid and solid products than those calculated by additive manner. Fourier transform infrared spectrometer analysis showed that main functional groups in chars gradually disappeared with pyrolysis temperatures increasing, and H 2 O, CH 4 , CO, and CO 2 appeared in volatiles during pyrolysis. Gas compositions analysis indicated that, the yields of H 2 and CO clearly increased as the pyrolysis temperature and sludge blending ratio increasing, while the changes of CH 4 and CO 2 yields were relatively complex. Copyright © 2016 Elsevier Ltd. All rights reserved.

Analysis of human plasma lipids by using comprehensive two-dimensional gas chromatography with dual detection and with the support of high-resolution time-of-flight mass spectrometry for structural elucidation.

Science.gov (United States)

Salivo, Simona; Beccaria, Marco; Sullini, Giuseppe; Tranchida, Peter Q; Dugo, Paola; Mondello, Luigi

2015-01-01

The main focus of the present research is the analysis of the unsaponifiable lipid fraction of human plasma by using data derived from comprehensive two-dimensional gas chromatography with dual quadrupole mass spectrometry and flame ionization detection. This approach enabled us to attain both mass spectral information and analyte percentage data. Furthermore, gas chromatography coupled with high-resolution time-of-flight mass spectrometry was used to increase the reliability of identification of several unsaponifiable lipid constituents. The synergism between both the high-resolution gas chromatography and mass spectrometry processes enabled us to attain a more in-depth knowledge of the unsaponifiable fraction of human plasma. Additionally, information was attained on the fatty acid and triacylglycerol composition of the plasma samples, subjected to investigation by using comprehensive two-dimensional gas chromatography with dual quadrupole mass spectrometry and flame ionization detection and high-performance liquid chromatography with atmospheric pressure chemical ionization quadrupole mass spectrometry, respectively. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

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

Determination of ifosfamide, 2-and 3-dechloroethyifosfamide using gas chromatography with nitrogen-phosphorus or mass spectrometry detection

NARCIS (Netherlands)

Kerbusch, T; Jeuken, MJ; Derraz, J; van Putten, JWG; Huitema, ADR; Beijnen, JH

2000-01-01

A comparison was made between methods for determining ifosfamide (IF), 2- (2DCE) and 3-dechloroethylifosfamide (3DCE) using gas chromatography with nitrogen-phosphorus detection (GC-NPD) versus positive ion electron-impact ion-trap mass spectrometry (GC-MS'). Sample pretreatment involved

Simultaneous Determination of Cocaine, Cocaethylene, and Their Possible Pentafluoropropylated Metabolites and Pyrolysis Products by Gas Chromatography/Mass Spectrometry

National Research Council Canada - National Science Library

Cardona, Patrick

2003-01-01

.... Therefore, it is important to determine concentrations of COC and its metabolites ethanol analogs, and pyrolysis products for establishing the degree of toxicity that possible ingestion of ethanol...

Study on aroma components of osmanthus by absorption wire gas chromatography/mass spectrometry

International Nuclear Information System (INIS)

Feng Janyue; Zhao Jing; Huang Qiaoqiao; Feng Lianmei

2001-01-01

The aroma components of fresh osmanthus are captured by absorption wires. The fragrant components absorbed in the wires are desorbed immediately at 358 degree C in Curie-point pyrolyzed, and then led into GC/MS to analyze. As a result, 41 aroma compounds such as β-linalool, linalooloxide, β-ocimene etc. in osmanthus are detected qualitatively by gas chromatography/mass spectrometry. This method can be used to analyze the change of aroma compounds of fresh flowers while blossoming

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

The production of hydrogen-rich gas by wet sludge pyrolysis using waste heat from blast-furnace slag

International Nuclear Information System (INIS)

Luo, Siyi; Feng, Yu

2016-01-01

Blast furnace (BF) slag, a byproduct of steelmaking industry, contains a large amount of sensible heat and is composed of some metal oxides, which exhibits preferable catalytic performance in improving tar cracking and C_nH_m reforming. This paper presents a heat recovery system from the heat of BF slag, which generates hydrogen-rich gas via the endothermic reactions of sludge pyrolysis. The effects of various parameters including the slag temperature, the mass ratio of slag to sludge (B/S), particle size and feed moisture on product yields and gas characteristics were evaluated separately. It was found that the pyrolysis products distribution was significantly influenced by the BF slag temperature. The differences resulting from varying B/S practically disappear as higher temperature heat carrier is approached. The optimum feed moisture was in favour of sludge pyrolysis by getting char and tar participate in gasification reactions, improving gas yield and quality. BF slag as catalyst can greatly increase H_2 and CO contents of gas by improving tar degradation and reforming of biogas (CO_2 and CH_4). Decreasing the slag particles size was helpful to sludge primary pyrolysis to produce more light gases, less char and condensate, while its effects on gas compositions was not evident. - Highlights: • The sensible heat of molten slag was recovered and converted into combustible gas. • A novel rotary pyrolysis reactor using BF slag as heat carrier was presented. • The moisture in sludge was used as the gasification medium and hydrogen source.

Comparison of gas chromatography/isotope ratio mass spectrometry and liquid chromatography/isotope ratio mass spectrometry for carbon stable-isotope analysis of carbohydrates.

Science.gov (United States)

Moerdijk-Poortvliet, Tanja C W; Schierbeek, Henk; Houtekamer, Marco; van Engeland, Tom; Derrien, Delphine; Stal, Lucas J; Boschker, Henricus T S

2015-07-15

We compared gas chromatography/isotope ratio mass spectrometry (GC/IRMS) and liquid chromatography/isotope ratio mass spectrometry (LC/IRMS) for the measurement of δ(13)C values in carbohydrates. Contrary to GC/IRMS, no derivatisation is needed for LC/IRMS analysis of carbohydrates. Hence, although LC/IRMS is expected to be more accurate and precise, no direct comparison has been reported. GC/IRMS with the aldonitrile penta-acetate (ANPA) derivatisation method was compared with LC/IRMS without derivatisation. A large number of glucose standards and a variety of natural samples were analysed for five neutral carbohydrates at natural abundance as well as at (13)C-enriched levels. Gas chromatography/chemical ionisation mass spectrometry (GC/CIMS) was applied to check for incomplete derivatisation of the carbohydrate, which would impair the accuracy of the GC/IRMS method. The LC/IRMS technique provided excellent precision (±0.08‰ and ±3.1‰ at natural abundance and enrichment levels, respectively) for the glucose standards and this technique proved to be superior to GC/IRMS (±0.62‰ and ±19.8‰ at natural abundance and enrichment levels, respectively). For GC/IRMS measurements the derivatisation correction and the conversion of carbohydrates into CO2 had a considerable effect on the measured δ(13)C values. However, we did not find any significant differences in the accuracy of the two techniques over the full range of natural δ(13)C abundances and (13)C-labelled glucose. The difference in the performance of GC/IRMS and LC/IRMS diminished when the δ(13)C values were measured in natural samples, because the chromatographic performance and background correction became critical factors, particularly for LC/IRMS. The derivatisation of carbohydrates for the GC/IRMS method was complete. Although both LC/IRMS and GC/IRMS are reliable techniques for compound-specific stable carbon isotope analysis of carbohydrates (provided that derivatisation is complete and the

Gas Chromatography-Mass Spectrometry for Metabolite Profiling of Japanese Black Cattle Naturally Contaminated with Zearalenone and Sterigmatocystin

NARCIS (Netherlands)

Toda, Katsuki; Kokushi, Emiko; Uno, Seiichi; Shiiba, Ayaka; Hasunuma, Hiroshi; Fushimi, Yasuo; Wijayagunawardane, Missaka P B; Zhang, Chunhua; Yamato, Osamu; Taniguchi, Masayasu; Fink-Gremmels, Johanna; Takagi, Mitsuhiro

2017-01-01

The objective of this study was to evaluate the metabolic profile of cattle fed with or without zearalenone (ZEN) and sterigmatocystin (STC)-contaminated diets using a gas chromatography-mass spectrometry metabolomics approach. Urinary samples were collected from individual animals (n = 6 per herd)

Chlorococcalean microalgae Ankistrodesmus convolutes biodiesel characterization with Fourier transform-infrared spectroscopy and gas chromatography mass spectroscopy techniques

Directory of Open Access Journals (Sweden)

Swati SONAWANE

2015-12-01

Full Text Available The Chlorococcalean microalgae Ankistrodesmus convolutes was found in fresh water Godawari reservoir, Ahmednagar district of Maharashtra State, India. Microalgae are modern biomass for the production of liquid biofuel due to its high solar cultivation efficiency. The collection, harvesting and drying processes were play vital role in converting algal biomass into energy liquid fuel. The oil extraction was the important step for the biodiesel synthesis. The fatty acid methyl ester (FAME synthesis was carried through base catalyzed transesterification method. The product was analyzed by using the hyphened techniques like Fourier Transform-Infrared spectroscopy (FT-IR and Gas Chromatography Mass Spectroscopy (GCMS. FT-IR Spectroscopy was results the ester as functional group of obtained product while the Gas Chromatography Mass Spectroscopy was results the six type of fatty acid methyl ester with different concentration. Ankistrodesmus convolutes biodiesel consist of 46.5% saturated and 49.14% unsaturated FAME.

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

Determination of cholesterol and four phytosterols in foods without derivatization by gas chromatography-tandem mass spectrometry

Directory of Open Access Journals (Sweden)

Yan-Zong Chen

2015-12-01

Full Text Available In this study, a method for determination of cholesterol and four phytosterols by gas chromatography coupled with electron impact ionization mode–tandem mass spectrometry without derivatization in general food was developed. The sample was saponified with 7.5% KOH in methanol. After heating on hot plate and reflux for 60 minutes, the saponified portion was extracted with n-hexane/petroleum ether (50:50, v/v. The extracts were evaporated with rotary evaporator and then redissolved with tetrahydrofuran. The tetrahydrofuran layer was transferred into an injection vial and analyzed by gas chromatography on a 30 m VF-5 column. Limit of quantification was 2 mg/kg. Recoveries of cholesterol and four phytosterols from general food were between 91% and 100%.

Comparison of radioimmunoassay and gas chromatographic mass spectrometric assay for d-amphetamine

International Nuclear Information System (INIS)

Powers, K.H.; Ebert, M.H.

1979-01-01

Quantification of low levels of psychotropic drugs (10 -7 to 10 -9 g ml -1 ) in small volumes of plasma requires sensitive and accurate methods. Validation of these methods is best achieved by comparing results obtained using several techniques. In this study, amphetamine levels in plasma were measured using gas chromatography mass spectrometry and radioimmunoassay. Correlation of the results obtained by the two methods was found to be positive and high (R = 0.9822). The average coefficient of variation between assays for gas chromatography mass spectrometry was 5.8% and for radioimmunoassay was 12.3%, while the average coefficient of variation within assays for gas chromatography mass spectrometry was 4.9% and for radioimmunoassay 6.9%. Although gas chromatography mass spectrometry was 1.9 times more sensitive than radioimmunoassay, for most purposes, the convenience of the radioimmunoassay method outweighs the technical superiority of gas chromatography mass spectrometry. (author)

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.

Comparison of Gas Chromatography-Mass Spectrometry and Gas Chromatography-Tandem Mass Spectrometry with Electron Ionization and Negative-Ion Chemical Ionization for Analyses of Pesticides at Trace Levels in Atmospheric Samples

Directory of Open Access Journals (Sweden)

Renata Raina

2008-01-01

Full Text Available A comparison of detection limits of gas chromatography-mass spectrometry (GC-MS in selected ion monitoring (SIM with gas chromatography-tandem mass spectrometry (GC-MS/MS in selected reaction monitoring (SRM mode with both electron ionization (EI and negative-ion chemical ionization (NCI are presented for over 50 pesticides ranging from organochlorines (OCs, organophosphorus pesticides (OPs and pre-emergent herbicides used in the Canadian prairies (triallate, trifluralin, ethalfluralin. The developed GC-EI/SIM, GC-NCI/SIM, and GC-NCI/SRM are suitable for the determination of pesticides in air sample extracts at concentrations <100 pg µL -1 (< 100 pg m -3 in air. No one method could be used to analyze the range of pre-emergent herbicides, OPs, and OCs investigated. In general GC-NCI/SIM provided the lowest method detection limits (MDLs commonly 2.5-10 pg µL -1 along with best confirmation (<25% RSD of ion ratio, while GC-NCI/SRM is recommended for use where added selectivity or confirmation is required (such as parathion-ethyl, tokuthion, carbofenothion. GC-EI/SRM at concentration < 100 pg µL -1 was not suitable for most pesticides. GC-EI/SIM was more prone to interference issues than NCI methods, but gave good sensitivity (MDLs 1-10 pg µL -1 for pesticides with poor NCI response (OPs: sulfotep, phorate, aspon, ethion, and OCs: alachlor, aldrin, perthane, and DDE, DDD, DDT.

Thermodynamic Model for Updraft Gasifier with External Recirculation of Pyrolysis Gas

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Fajri Vidian

2016-01-01

Full Text Available Most of the thermodynamic modeling of gasification for updraft gasifier uses one process of decomposition (decomposition of fuel. In the present study, a thermodynamic model which uses two processes of decomposition (decomposition of fuel and char is used. The model is implemented in modification of updraft gasifier with external recirculation of pyrolysis gas to the combustion zone and the gas flowing out from the side stream (reduction zone in the updraft gasifier. The goal of the model obtains the influences of amount of recirculation pyrolysis gas fraction to combustion zone on combustible gas and tar. The significant results of modification updraft are that the increases amount of recirculation of pyrolysis gas will increase the composition of H2 and reduce the composition of tar; then the composition of CO and CH4 is dependent on equivalence ratio. The results of the model for combustible gas composition are compared with previous study.

A comparison of fast and reactive pyrolysis with insitu derivatisation of fructose, inulin and Jerusalem artichoke (Helianthus tuberosus).

Science.gov (United States)

Mattonai, Marco; Ribechini, Erika

2018-08-09

Reactive pyrolysis is a technique that provides mechanistic information by performing pyrolysis of the substrate in a sealed glass capsule at elevated temperature and pressure for relatively long time. This technique has already shown great potential for the analysis of biomass, favouring the formation of only the most thermostable compounds. In this work, both fast and reactive pyrolysis with on-line gas chromatography-mass spectrometry analysis (Py-GC/MS) are used to study fructose, inulin and Jerusalem artichoke tubers (Heliantus tuberosus). Interesting differences were found between the two systems, and became even more evident as the reaction time was increased. The most striking result was the formation of di-fructose dianhydrides (DFAs), a class of compounds with interesting biological activities. DFAs were obtained in high yields from reactive pyrolysis, but not from fast pyrolysis. Hypotheses on the pyrolysis mechanisms were made based upon the composition of the pyrolysates. This work describes for the first time the behaviour of fructans under reactive pyrolysis. Copyright © 2018 Elsevier B.V. All rights reserved.

Advantages of Atmospheric Pressure Chemical Ionization in Gas Chromatography Tandem Mass Spectrometry: Pyrethroid Insecticides as a Case Study

NARCIS (Netherlands)

Portolés, T.; Mol, J.G.J.; Sancho, J.V.; Hernández, F.

2012-01-01

Gas chromatography coupled to mass spectrometry (GC/MS) has been extensively applied for determination of volatile, nonpolar, compounds in many applied fields like food safety, environment, or toxicology. The wide majority of methods reported use electron ionization (EI), which may result in

Mass spectrometric studies of fast pyrolysis of cellulose

Energy Technology Data Exchange (ETDEWEB)

Degenstein, John; Hurt, Matt; Murria, Priya; Easton, McKay; Choudhari, Harshavardhan; Yang, Linan; Riedeman, James; Carlsen, Mark; Nash, John; Agrawal, Rakesh; Delgass, W.; Ribeiro, Fabio; Kenttämaa, Hilkka

2015-01-01

A fast pyrolysis probe/linear quadrupole ion trap mass spectrometer combination was used to study the primary fast pyrolysis products (those that first leave the hot pyrolysis surface) of cellulose, cellobiose, cellotriose, cellotetraose, cellopentaose, and cellohexaose, as well as of cellobiosan, cellotriosan, and cellopentosan, at 600°C. Similar products with different branching ratios were found for the oligosaccharides and cellulose, as reported previously. However, identical products (with the exception of two) with similar branching ratios were measured for cellotriosan (and cellopentosan) and cellulose. This result demonstrates that cellotriosan is an excellent small-molecule surrogate for studies of the fast pyrolysis of cellulose and also that most fast pyrolysis products of cellulose do not originate from the reducing end. Based on several observations, the fast pyrolysis of cellulose is suggested to initiate predominantly via two competing processes: the formation of anhydro-oligosaccharides, such as cellobiosan, cellotriosan, and cellopentosan (major route), and the elimination of glycolaldehyde (or isomeric) units from the reducing end of oligosaccharides formed from cellulose during fast pyrolysis.

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.

Simultaneous analysis of fourteen tertiary amine stimulants in human urine for doping control purposes by liquid chromatography-tandem mass spectrometry and gas chromatography-mass spectrometry

International Nuclear Information System (INIS)

Lu Jianghai; Wang San; Dong Ying; Wang Xiaobing; Yang Shuming; Zhang Jianli; Deng Jing; Qin Yang; Xu Youxuan; Wu Moutian; Ouyang Gangfeng

2010-01-01

A method for the simultaneous screening and confirmation of the presence of fourteen tertiary amine stimulants in human urine by gas chromatography-mass spectrometry (GC-MS) in combination with liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been developed and validated. Solid phase extraction (SPE) and liquid-liquid extraction (LLE) approaches were utilized for the pre-treatment of the urine samples. The study indicated that the capillary temperature played a significant role in the signal abundances of the protonated molecules of cropropamide and crotethamide under positive ion electrospray ionization (ESI) conditions. In addition, comparison studies of two different pre-treatment approaches as well as the two ionization modes were conducted. The LODs of the developed method for all the analytes were lower than the minimum required performance limit (MRPL) as set forth in the World Anti-Doping Agency (WADA) technical document for laboratories. The human urine sample obtained after oral administration of prolintane.HCl was successfully analyzed by the developed method, which demonstrated the applicability and reliability of the method for routine doping control analysis.

Application of gas chromatography-surface ionization organic mass spectrometry to forensic toxicology.

Science.gov (United States)

Ishii, Akira; Watanabe-Suzuki, Kanako; Seno, Hiroshi; Suzuki, Osamu; Katsumata, Yoshinao

2002-08-25

Surface ionization (SI), which consists in the formation of positive and negative ions along the course of thermal desorption of particles from a solid surface, was first applied as a detector for gas chromatography (GC), GC-surface ionization detection (SID); we developed many new sensitive methods for the determination of abused and other drugs by GC-SID. Recently, Fujii has devised a combination of SI and a quadrupole mass spectrometer and named this system a surface ionization organic mass spectrometer (SIOMS), which is highly selective and sensitive for organic compounds containing tertiary amino groups. We have tried to apply this mass spectrometer to forensic toxicological study; so far we have succeeded in determining important drugs-of-abuse and toxic compounds, such as phencyclidine (PCP), pethidine, pentazocine, MPTP and its derivatives from human body fluids with high sensitivity and selectivity. In this review, we describe our recent studies on the application of GC-SIOMS to forensic toxicology. Copyright 2002 Elsevier Science B.V.

PYROLYSIS OF ISOCHRYSIS MICROALGAE WITH METAL OXIDE CATALYSTS FOR BIO-OIL PRODUCTION

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TEVFİK AYSU

2016-12-01

Full Text Available Pyrolysis of Isochrysis microalgae was carried out in a fixed-bed reactor without and with metal oxide catalysts (CeO2, TiO2, Al2O3 at the temperatures of 450, 500 and 550 oC with a constant heating rate of 40 oC/min. The pyrolysis conditions including catalyst and temperature were studied in terms of their effects on the yields of pyrolysis products and quality. The amount of bio-char, bio-oil and gas products was calculated. The composition of the produced bio-oils was determined by Elemental analysis (EA, Fourier transform infrared spectroscopy (FT-IR, proton nuclear magnetic resonance (1H NMR and Gas chromatography/mass spectrometry (GC–MS techniques. As a result of the pyrolysis experiments, it is shown that there have been significant effects of both catalyst and temperature on the conversion of Isochrysis microalgae into solid, liquid (bio-oil and gas products. The highest bio-oil yield (24.30 % including aqueous phase was obtained in the presence of TiO2 (50% as catalyst at 500 °C. 98 different compounds were identified by GC-MS in bio-oils obtained at 500 oC. According to 1H NMR analysis, bio-oils contained ∼60-64 % aliphatic and ∼17-19 % aromatic structural units. EA showed that the bio-oils contained ∼66-69 % C and having 31-34 MJ/kg higher heating values.

Simultaneous determination of creatinine and creatine in human serum by double-spike isotope dilution liquid chromatography-tandem mass spectrometry (LC-MS/MS) and gas chromatography-mass spectrometry (GC-MS).

Science.gov (United States)

Fernández-Fernández, Mario; Rodríguez-González, Pablo; Añón Álvarez, M Elena; Rodríguez, Felix; Menéndez, Francisco V Álvarez; García Alonso, J Ignacio

2015-04-07

This work describes the first multiple spiking isotope dilution procedure for organic compounds using (13)C labeling. A double-spiking isotope dilution method capable of correcting and quantifying the creatine-creatinine interconversion occurring during the analytical determination of both compounds in human serum is presented. The determination of serum creatinine may be affected by the interconversion between creatine and creatinine during sample preparation or by inefficient chemical separation of those compounds by solid phase extraction (SPE). The methodology is based on the use differently labeled (13)C analogues ((13)C1-creatinine and (13)C2-creatine), the measurement of the isotopic distribution of creatine and creatinine by liquid chromatography-tandem mass spectrometry (LC-MS/MS) and the application of multiple linear regression. Five different lyophilized serum-based controls and two certified human serum reference materials (ERM-DA252a and ERM-DA253a) were analyzed to evaluate the accuracy and precision of the proposed double-spike LC-MS/MS method. The methodology was applied to study the creatine-creatinine interconversion during LC-MS/MS and gas chromatography-mass spectrometry (GC-MS) analyses and the separation efficiency of the SPE step required in the traditional gas chromatography-isotope dilution mass spectrometry (GC-IDMS) reference methods employed for the determination of serum creatinine. The analysis of real serum samples by GC-MS showed that creatine-creatinine separation by SPE can be a nonquantitative step that may induce creatinine overestimations up to 28% in samples containing high amounts of creatine. Also, a detectable conversion of creatine into creatinine was observed during sample preparation for LC-MS/MS. The developed double-spike LC-MS/MS improves the current state of the art for the determination of creatinine in human serum by isotope dilution mass spectrometry (IDMS), because corrections are made for all the possible errors

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.

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.

[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.

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

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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.

Discrimination of bacteria using pyrolysis-gas chromatography-differential mobility spectrometry (Py-GC-DMS) and chemometrics.

Science.gov (United States)

Cheung, William; Xu, Yu; Thomas, C L Paul; Goodacre, Royston

2009-03-01

Discrimination of bacteria was investigated using pyrolysis-gas chromatography-differential mobility spectrometry (Py-GC-DMS). Three strains belonging to the genus Bacillus were investigated and these included two strains of Bacillus subtilis and a single Bacillus megaterium. These were chosen so as to evaluate the possibility of bacterial strain discrimination using Py-GC-DMS. The instrument was constructed in-house and the long-term reproducibility of the instrument was evaluated over a period of 60 days using a Scotch whisky quality control. To assess the reproducibility further each bacterium was cultured six times and each culture was analysed in replicate to give three analytical replicates. The DMS data were generated in both positive and negative modes, and the data in each mode were analysed independently of each other. The Py-GC-DMS data were pre-processed via correlation optimised warping (COW) and asymmetric least square (ALS) to align the DMS chromatograms and to remove any unavoidable baseline shifts, prior to normalisation. Processed chromatograms were analysed using principal component analysis (PCA) followed by supervised learning methodology using partial least squares for discriminant analysis (PLS-DA). It was found that the separations between B. subtilis and B. megaterium can be readily observed by PCA; however, strain discrimination within the two B. subtilis was only possible using supervised learning. As multiple biological replicates were analysed an exhaustive splitting of the training and test sets was undertaken and this allowed correct classification rates (CCRs) to be assessed for the 3375 test sets. It was found that with PLS-DA the negative ion mode DMS data were more discriminatory than the positive mode data.

Data correlation in on-line solid-phase extraction-gas chromatography-atomic emission/mass spectrometric detection of unknown microcontaminants

NARCIS (Netherlands)

Hankemeier, Th.; Rozenbrand, J.; Abhadur, M.; Vreuls, J.J.; Brinkman, U.A.Th.

1998-01-01

A procedure is described for the (non-target) screening of hetero-atom-containing compounds in tap and waste water by correlating data obtained by gas chromatography (GC) using atomic emission (AED) and mass selective (MS) detection. Solid-phase extraction (SPE) was coupled on-line to both GC

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

Comparative Analysis of Mass Spectral Similarity Measures on Peak Alignment for Comprehensive Two-Dimensional Gas Chromatography Mass Spectrometry

Science.gov (United States)

2013-01-01

Peak alignment is a critical procedure in mass spectrometry-based biomarker discovery in metabolomics. One of peak alignment approaches to comprehensive two-dimensional gas chromatography mass spectrometry (GC×GC-MS) data is peak matching-based alignment. A key to the peak matching-based alignment is the calculation of mass spectral similarity scores. Various mass spectral similarity measures have been developed mainly for compound identification, but the effect of these spectral similarity measures on the performance of peak matching-based alignment still remains unknown. Therefore, we selected five mass spectral similarity measures, cosine correlation, Pearson's correlation, Spearman's correlation, partial correlation, and part correlation, and examined their effects on peak alignment using two sets of experimental GC×GC-MS data. The results show that the spectral similarity measure does not affect the alignment accuracy significantly in analysis of data from less complex samples, while the partial correlation performs much better than other spectral similarity measures when analyzing experimental data acquired from complex biological samples. PMID:24151524

Identification of di(ethylhexyl) phthalate as impurity in the analysis by using chromatography gas tandem mass spectrometry

Science.gov (United States)

Pusfitasari, Eka Dian; Hendarsyah, Hendris; Salahuddin, Ariani, Novita

2017-01-01

Di(ethylhexyl) phthalate (DEHP) is a plasticizer commonly used in plastics. Physically DEHP has a low vapor pressure. DEHP can seep into the liquid in direct contact with the plastic wrapping materials, and typically can occur rapidly if extractable into food or non-polar solvents, such as oil, once the food is packaged in PVC packaging materials. DEHP has been analyzed by using gas chromatography which has a high sensitivity level. If the equipment used for the analysis is made from plastic containing DEHP, then it may be possible that DEHP can be extracted and appear on the outcome of the injection. It can interfere with the process of analysis, especially for the analysis of food samples. This study has identified the present of DEHP in the blank injection performed by Gas Chromatography tandem Mass Spectrometry with Selected Ion Monitoring mode (SIM). Researchers are required to verify whether the gas chromatographic system used is ready for the analysis process. In addition, the comparison and calculation of the intensity of the ion fragmentation spectra generated by mass spectrometry detector can be used for the qualitative determination to ensure the presence of the target compound. In this study is also discussed the differences between the high-intensity fragmentation of DEHP and dioctyl phthalate (DOP).

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…

Comparison of photoacoustic radiometry to gas chromatography/mass spectrometry methods for monitoring chlorinated hydrocarbons

International Nuclear Information System (INIS)

Sollid, J.E.; Trujillo, V.L.; Limback, S.P.; Woloshun, K.A.

1996-01-01

A comparison of two methods of gas chromatography mass spectrometry (GCMS) and a nondispersive infrared technique, photoacoustic radiometry (PAR), is presented in the context of field monitoring a disposal site. First is presented an historical account describing the site and early monitoring to provide an overview. The intent and nature of the monitoring program changed when it was proposed to expand the Radiological Waste Site close to the Hazardous Waste Site. Both the sampling methods and analysis techniques were refined in the course of this exercise

[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.

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.

Gas chromatography-mass spectrometry and high-performance liquid chromatography-diode array detection for dating of paper ink.

Science.gov (United States)

Díaz-Santana, Oscar; Vega-Moreno, Daura; Conde-Hardisson, Francisco

2017-09-15

An extraction and determination method is shown for the analysis of dyes and solvents present in two types of ballpoint pen inks that are deposited onto paper. Ink extracts are analysed using a combination of gas chromatography with mass spectrometry (GC-MS), and high-pressure liquid chromatography with photodiode array detection (HPLC-DAD), within a single sample extraction procedure. Seventeen solvents and thirteen dyes contained in two Montblanc ® inks (black and blue) were monitored for 45 months at monthly intervals, in order to determine variations in the concentrations of the compounds over time. We also studied the relative variations between different compounds and the generation of degradation products such as phenol. The concentration data obtained from these compounds during their exposure have been analysed and a multiple regression model is developed for each ink type that allows an estimate of the exposure time of the ink on paper with a maximum error of between 4 and 7 months. Copyright © 2017 Elsevier B.V. All rights reserved.

Synthesis of carbon nanotubes and porous carbons from printed circuit board waste pyrolysis oil

International Nuclear Information System (INIS)

Quan Cui; Li Aimin; Gao Ningbo

2010-01-01

The possibility and feasibility of using pyrolysis oil from printed circuit board (PCB) waste as a precursor for advanced carbonaceous materials is presented. The PCB waste was first pyrolyzed in a laboratory scale fixed bed reactor at 600 deg. C to prepare pyrolysis oil. The analysis of pyrolysis oil by gas chromatography-mass spectroscopy indicated that it contained a very high proportion of phenol and phenol derivatives. It was then polymerized in formaldehyde solution to synthesize pyrolysis oil-based resin which was used as a precursor to prepare carbon nanotubes (CNTs) and porous carbons. Scanning electron microscopy and transmission microscopy investigation showed that the resulting CNTs had hollow cores with outer diameter of ∼338 nm and wall thickness of ∼86 nm and most of them were filled with metal nanoparticles or nanorods. X-ray diffraction reveals that CNTs have an amorphous structure. Nitrogen adsorption isotherm analysis indicated the prepared porous carbons had a Brunauer-Emmett-Teller surface area of 1214 m 2 /g. The mechanism of the formation of the CNTs and porous carbons was discussed.

High-throughput differentiation of heparin from other glycosaminoglycans by pyrolysis mass spectrometry.

Science.gov (United States)

Nemes, Peter; Hoover, William J; Keire, David A

2013-08-06

Sensors with high chemical specificity and enhanced sample throughput are vital to screening food products and medical devices for chemical or biochemical contaminants that may pose a threat to public health. For example, the rapid detection of oversulfated chondroitin sulfate (OSCS) in heparin could prevent reoccurrence of heparin adulteration that caused hundreds of severe adverse events including deaths worldwide in 2007-2008. Here, rapid pyrolysis is integrated with direct analysis in real time (DART) mass spectrometry to rapidly screen major glycosaminoglycans, including heparin, chondroitin sulfate A, dermatan sulfate, and OSCS. The results demonstrate that, compared to traditional liquid chromatography-based analyses, pyrolysis mass spectrometry achieved at least 250-fold higher sample throughput and was compatible with samples volume-limited to about 300 nL. Pyrolysis yielded an abundance of fragment ions (e.g., 150 different m/z species), many of which were specific to the parent compound. Using multivariate and statistical data analysis models, these data enabled facile differentiation of the glycosaminoglycans with high throughput. After method development was completed, authentically contaminated samples obtained during the heparin crisis by the FDA were analyzed in a blinded manner for OSCS contamination. The lower limit of differentiation and detection were 0.1% (w/w) OSCS in heparin and 100 ng/μL (20 ng) OSCS in water, respectively. For quantitative purposes the linear dynamic range spanned approximately 3 orders of magnitude. Moreover, this chemical readout was successfully employed to find clues in the manufacturing history of the heparin samples that can be used for surveillance purposes. The presented technology and data analysis protocols are anticipated to be readily adaptable to other chemical and biochemical agents and volume-limited samples.

Understanding the fast pyrolysis of lignin.

Science.gov (United States)

Patwardhan, Pushkaraj R; Brown, Robert C; Shanks, Brent H

2011-11-18

In the present study, pyrolysis of corn stover lignin was investigated by using a micro-pyrolyzer coupled with a GC-MS/FID (FID=flame ionization detector). The system has pyrolysis-vapor residence times of 15-20 ms, thus providing a regime of minimal secondary reactions. The primary pyrolysis product distribution obtained from lignin is reported. Over 84 % mass balance and almost complete closure on carbon balance is achieved. In another set of experiments, the pyrolysis vapors emerging from the micro-pyrolyzer are condensed to obtain lignin-derived bio-oil. The chemical composition of the bio-oil is analyzed by using GC-MS and gel permeation chromatography techniques. The comparison between results of two sets of experiments indicates that monomeric compounds are the primary pyrolysis products of lignin, which recombine after primary pyrolysis to produce oligomeric compounds. Further, the effect of minerals (NaCl, KCl, MgCl(2), and CaCl(2)) and temperature on the primary pyrolysis product distribution is investigated. The study provides insights into the fundamental mechanisms of lignin pyrolysis and a basis for developing more descriptive models of biomass pyrolysis. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Collaborative trial validation study of two methods, one based on high performance liquid chromatography-tandem mass spectrometry and on gas chromatography-mass spectrometry for the determination of acrylamide in bakery and potato products.

Science.gov (United States)

Wenzl, Thomas; Karasek, Lubomir; Rosen, Johan; Hellenaes, Karl-Erik; Crews, Colin; Castle, Laurence; Anklam, Elke

2006-11-03

A European inter-laboratory study was conducted to validate two analytical procedures for the determination of acrylamide in bakery ware (crispbreads, biscuits) and potato products (chips), within a concentration range from about 20 microg/kg to about 9000 microgg/kg. The methods are based on gas chromatography-mass spectrometry (GC-MS) of the derivatised analyte and on high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) of native acrylamide. Isotope dilution with isotopically labelled acrylamide was an integral part of both methods. The study was evaluated according to internationally accepted guidelines. The performance of the HPLC-MS/MS method was found to be superior to that of the GC-MS method and to be fit-for-the-purpose.

Derivatisation/solid-phase microextraction followed by gas chromatography-mass spectrometry for the analysis of phenoxy acid herbicides in aqueous samples

DEFF Research Database (Denmark)

Nilsson, Torben; Baglio, Daniela; Galdo-Miguez, Isabel

1998-01-01

Different combinations of derivatisation and solid-phase microextraction followed by gas chromatography-mass spectrometry were optimised and evaluated for the analysis of phenoxy acid herbicides in water. The most successful derivatisation approach was aqueous-phase derivatisation with benzyl...

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.

Analysis of acylcarnitines as their N-demethylated ester derivatives by gas chromatography-chemical ionization mass spectrometry.

Science.gov (United States)

Huang, Z H; Gage, D A; Bieber, L L; Sweeley, C C

1991-11-15

A novel approach to the analysis of acylcarnitines has been developed. It involves a direct esterification using propyl chloroformate in aqueous propanol followed by ion-pair extraction with potassium iodide into chloroform and subsequent on-column N-demethylation of the resulting acylcarnitine propyl ester iodides. The products, acyl N-demethylcarnitine propyl esters, are volatile and are easily analyzed by gas chromatography-chemical ionization mass spectrometry. For medium-chain-length (C4-C12) acylcarnitine standards, detection limits are demonstrated to be well below 1 ng starting material using selected ion monitoring. Well-separated gas chromatographic peaks and structure-specific mass spectra are obtained with samples of synthetic and biological origin. Seven acylcarnitines have been characterized in the urine of a patient suffering from medium-chain acyl-CoA dehydrogenase deficiency.

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

Liquid oil and residual characteristics of printed circuit board recycle by pyrolysis

Energy Technology Data Exchange (ETDEWEB)

Lin, Kuo-Hsiung [Department of Environmental Engineering and Science, Fooyin University, Kaohsiung, Taiwan (China); Chiang, Hung-Lung, E-mail: hlchiang@mail.cmu.edu.tw [Department of Health Risk Management, China Medical University, Taichung, Taiwan (China)

2014-04-01

Highlights: • Pyrolysis is a technology for recycling of the non-metal fraction of PCBs. • Liquid product constituents were analyzed for PCB pyrolysis. • Water-soluble ionic species were determined for PCB pyrolysis exhaust. - Abstract: Non-metal fractions of waste printed circuit boards (PCBs) were thermally treated (200–500 °C) under nitrogen atmosphere. Carbon, hydrogen, and nitrogen were determined by elemental analyzer, bromine by instrumental neutron activation analysis (INAA), phosphorus by energy dispersive X-ray spectrometer (EDX), and 29 trace elements by inductively coupled plasma atomic emission spectrometer (ICP-AES) and mass spectrometry (ICP-MS) for raw material and pyrolysis residues. Organic compositions of liquid oil were identified by GC (gas chromatography)–MS, trace element composition by ICP system, and 12 water-soluble ions by IC (ionic chromatography). Elemental content of carbon was >450 mg/g, oxygen 300 mg/g, bromine and hydrogen 60 mg/g, nitrogen 30 mg/g, and phosphorus 28 mg/g. Sulfur was trace in PCBs. Copper content was 25–28 mg/g, iron 1.3–1.7 mg/g, tin 0.8–1.0 mg/g and magnesium 0.4–1.0 mg/g; those were the main metals in the raw materials and pyrolytic residues. In the liquid products, carbon content was 68–73%, hydrogen was 10–14%, nitrogen was 4–5%, and sulfur was less than 0.05% at pyrolysis temperatures from 300 to 500 °C. Phenol, 3-bromophenol, 2-methylphenol and 4-propan-2-ylphenol were major species in liquid products, accounting for >50% of analyzed organic species. Bromides, ammonium and phosphate were the main species in water sorption samples for PCB pyrolysis exhaust.

Quantitative analysis of abused drugs in physiological fluids by gas chromatography/chemical ionization mass spectrometry

International Nuclear Information System (INIS)

Foltz, R.L.

1978-01-01

Methods have been developed for quantitative analysis of commonly abused drugs in physiological fluids using gas chromatography/chemical ionization mass spectrometry. The methods are being evaluated in volunteer analytical and toxicological laboratories, and analytical manuals describing the methods are being prepared. The specific drug and metabolites included in this program are: Δ 9 -tetrahydrocannabinol, methadone, phencyclidine, methaqualone, morphine, amphetamine, methamphetamine, mescaline, 2,5-dimethoxy-4-methyl amphetamine, cocaine, benzoylecgonine, diazepam, and N-desmethyldiazepam. The current analytical methods utilize relatively conventional instrumentation and procedures, and are capable of measuring drug concentrations as low as 1 ng/ml. Various newer techniques such as sample clean-up by high performance liquid chromatography, separation by glass capillary chromatography, and ionization by negative ion chemical ionization are being investigated with respect to their potential for achieving higher sensitivity and specificity, as well as their ability to facilitate simultaneous analysis of more than one drug and metabolite. (Auth.)

Formation of nitrogen-containing compounds during microwave pyrolysis of microalgae: Product distribution and reaction pathways.

Science.gov (United States)

Huang, Feng; Tahmasebi, Arash; Maliutina, Kristina; Yu, Jianglong

2017-12-01

The formation of nitrogen-containing compounds in bio-oil during microwave pyrolysis of Chlorella and Spirulina microalgae has been investigated in this study. Activated carbon (AC) and magnetite (Fe 3 O 4 ) were used as microwave receptors during microwave pyrolysis experiments. It has been found that the use of Fe 3 O 4 increased the total yield of bio-oil. The use of different microwave receptors did not seem to have affected the total yield of nitrogen-containing compounds in the bio-oil. However, Fe 3 O 4 promoted the formation of nitrogen-containing aliphatics, thereby reducing the formation of nitrogen-containing aromatics. The use of AC promoted the dehydration reactions during amino acid decomposition, thereby enhancing the formation of nitrogen-containing aromatics during pyrolysis. From the gas chromatography-mass spectrometry (GC-MS) analysis results, the major high-value nitrogen-containing compounds in the pyrolysis bio-oil of Chlorella and Spirulina were identified as indole and dodecamide. The formation mechanisms of nitrogen-containing compounds were proposed and discussed. Copyright © 2017 Elsevier Ltd. All rights reserved.

Insights into pyrolysis and co-pyrolysis of biomass and polystyrene: Thermochemical behaviors, kinetics and evolved gas analysis

International Nuclear Information System (INIS)

Özsin, Gamzenur; Pütün, Ayşe Eren

2017-01-01

Highlights: • TGA/MS/FT-IR was used to explore effect of polystyrene on pyrolytic decomposition of biomass. • The model-free iso-conversional methods were used for kinetic analysis. • Interactions occurred depending on the characteristics of the biomass. • TGA/MS and TGA/FT-IR coupling were used for gas analysis of co-pyrolysis for the first time. - Abstract: The purpose of this study was to investigate the effect on polystyrene (PS) during co-pyrolysis with biomass through thermal decomposition. The model-free iso-conversional methods (Kissinger, Friedman, Flynn-Wall-Ozawa, Kissinger-Akahira-Sunose, Starink and Vyazovkin) were adopted to calculate activation energy of the pyrolysis and co-pyrolysis process of two biomass samples (walnut shell: WS and peach stones: PST) with PS. It is found that biomass blending to PS decreased activation energy values and resulted in multi-step reaction mechanisms. Furthermore, changes in the evolution profiles of methyl, water, methoxy, carbon dioxide, benzene and styrene was monitored through evolved gas analysis via TGA/FT-IR and TGA/MS. Detection of temperature dependent release of volatiles indicated the differences occur as a result of compositional differences of biomass.

Analysis of [U-13C6]glucose in human plasma using liquid chromatography/isotope ratio mass spectrometry compared with two other mass spectrometry techniques

NARCIS (Netherlands)

Schierbeek, H.; Moerdijk-Poortvliet, T.C.W.; van den Akker, C.H.P.; te Braake, F.W.J.; Boschker, H.T.S.; van Goudoever, J.B.

2009-01-01

The use of stable isotope labelled glucose provides insight into glucose metabolism. The 13C-isotopic enrichment of glucose is usually measured by gas chromatography/mass spectrometry (GC/MS) or gas chromatography/combustion/isotope ratio mass spectrometry (GC/C/IRMS). However, in both techniques

Isotope ratio mass spectrometry coupled to liquid and gas chromatography for wine ethanol characterization.

Science.gov (United States)

Cabañero, Ana I; Recio, Jose L; Rupérez, Mercedes

2008-10-01

Two new procedures for wine ethanol 13C/12C isotope ratio determination, using high-performance liquid chromatography and gas chromatography isotope ratio mass spectrometry (HPLC/IRMS and GC/IRMS), have been developed to improve isotopic methods dedicated to the study of wine authenticity. Parameters influencing separation of ethanol from wine matrix such as column, temperature, mobile phase, flow rates and injection mode were investigated. Twenty-three wine samples from various origins were analyzed for validation of the procedures. The analytical precision was better than 0.15 per thousand, and no significant isotopic fractionation was observed employing both separative techniques coupled to IRMS. No significant differences and a very strong correlation (r = 0.99) were observed between the 13C/12C ratios obtained by the official method (elemental analyzer/isotope ratio mass spectrometry) and the proposed new methodology. The potential advantages of the developed methods over the traditional one are speed (reducing time required from hours to minutes) and simplicity. In addition, these are the first isotopic methods that allow 13C/12C determination directly from a liquid sample with no previous ethanol isolation, overcoming technical difficulties associated with sample treatment.

The potential of Isotope Ratio Mass Spectrometry (IRMS) and gas chromatography-IRMS analysis of triacetone triperoxide in forensic explosives investigations

NARCIS (Netherlands)

Bezemer, K.D.B.; Koeberg, M.; Heijden, A.E.D.M. van der; Driel, C.A. va; Blaga, C.; Bruinsma, J.; Asten, A.C. van

2016-01-01

Studying links between triacetone triperoxide (TATP) samples from crime scenes and suspects can assist in criminal investigations. Isotope ratio mass spectrometry (IRMS) and gas chromatography (GC)-IRMS were used to measure the isotopic compositions of TATP and its precursors acetone and hydrogen

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

Classical electron ionization mass spectra in gas chromatography/mass spectrometry with supersonic molecular beams.

Science.gov (United States)

Gordin, Alexander; Fialkov, Alexander B; Amirav, Aviv

2008-09-01

A major benefit of gas chromatography/mass spectrometry (GC/MS) with a supersonic molecular beam (SMB) interface and its fly-through ion source is the ability to obtain electron ionization of vibrationally cold molecules (cold EI), which show enhanced molecular ions. However, GC/MS with an SMB also has the flexibility to perform 'classical EI' mode of operation which provides mass spectra to mimic those in commercial 70 eV electron ionization MS libraries. Classical EI in SMB is obtained through simple reduction of the helium make-up gas flow rate, which reduces the SMB cooling efficiency; hence the vibrational temperatures of the molecules are similar to those in traditional EI ion sources. In classical EI-SMB mode, the relative abundance of the molecular ion can be tuned and, as a result, excellent identification probabilities and very good matching factors to the NIST MS library are obtained. Classical EI-SMB with the fly-through dual cage ion source has analyte sensitivity similar to that of the standard EI ion source of a basic GC/MS system. The fly-through EI ion source in combination with the SMB interface can serve for cold EI, classical EI-SMB, and cluster chemical ionization (CCI) modes of operation, all easily exchangeable through a simple and quick change (not involving hardware). Furthermore, the fly-through ion source eliminates sample scattering from the walls of the ion source, and thus it offers full sample inertness, tailing-free operation, and no ion-molecule reaction interferences. It is also robust and enables increased column flow rate capability without affecting the sensitivity.

Pyrolysis of Rubber in a Screw Reactor

Science.gov (United States)

Lozhechnik, A. V.; Savchin, V. V.

2016-11-01

On the basis of an analysis of thermal methods described in the literature and from the results of experimental investigations of steam conversion, the authors have developed and created a facility for thermal processing of rubber waste. Rubber crumb was used as the raw material; the temperature in the reactor was 500°C; nitrogen, steam, and a mixture of light hydrocarbons (noncondensable part of pyrolysis products) represented the working medium. The pyrolysis yielded 36-38% of a solid fraction, 54-56% of a liquid hydrocarbon fraction, and 6-9% of noncondensable gases. Changes in the composition of the gas mixture have been determined at different stages of processing. Gas chromatography of pyrolysis gases has shown that the basic gases produced by pyrolysis are H2 and hydrocarbons C2H4, C3H6, C3H8, C4H8, C2H6, C3H6O2, and C4H10, and a small amount of H2S, CO, and CO2. Noncondensable gases will be used as a fuel to heat the reactor and to implement the process.

Co-pyrolysis of waste tire/coal mixtures for smokeless fuel, maltenes and hydrogen-rich gas production

International Nuclear Information System (INIS)

Bičáková, Olga; Straka, Pavel

2016-01-01

Highlights: • Co-pyrolysis of waste tires/coal mixtures yields mainly smokeless fuel (55–74 wt%). • Alternatively, the smokeless fuel can serve as carbonaceous sorbent. • The obtained tar contained maltenes (80–85 wt%) and asphaltenes (6–8 wt%). • Tar from co-pyrolysis can serve as heating oil or a source of maltenes for repairing of asphalt surfaces. • The hydrogen-rich gas was obtained (61–65 vol% H_2, 24–25 vol% CH_4, 1.4–2 vol% CO_2). - Abstract: The processing of waste tires with two different types of bituminous coal was studied through the slow co-pyrolysis of 1 kg of waste tire/coal mixtures with 15, 30 and 60 wt% waste tires on a laboratory scale. The waste tire/coal mixtures were pyrolysed using a quartz reactor in a stationary bed. The mixtures were heated at a rate 5 °C/min up to the final temperature of 900 °C with a soaking time of 30 min at the required temperature. The mass balance of the process and the properties of the coke and tar obtained were evaluated, further, the influence of the admixture in the charge on the amount and composition of the obtained coke and tar was determined. It was found that the smokeless fuel/carbonaceous sorbent and a high yield of tar for further use can be obtained through the slow co-pyrolysis. The obtained tars contained mostly maltenes (80–85 wt%). FTIR analysis showed that the maltenes from the co-pyrolysis of coal/waste tires exhibited significantly lower aromaticity as compared with that from coal alone. The gas obtained from pyrolysis or co-pyrolysis of waste tire/coal mixtures contained a high amount of hydrogen (above 60 vol%) and methane (above 20 vol%).

Hyphenated and comprehensive liquid chromatography × gas chromatography-mass spectrometry for the identification of Mycobacterium tuberculosis.

Science.gov (United States)

Mourão, Marta P B; Denekamp, Ilse; Kuijper, Sjoukje; Kolk, Arend H J; Janssen, Hans-Gerd

2016-03-25

Tuberculosis is one of the world's most emerging public health problems, particularly in developing countries. Chromatography based methods have been used to tackle this epidemic by focusing on biomarker detection. Unfortunately, interferences from lipids in the sputum matrix, particularly cholesterol, adversely affect the identification and detection of the marker compounds. The present contribution describes the serial combination of normal phase liquid chromatography (NPLC) with thermally assisted hydrolysis and methylation followed by gas chromatography-mass spectrometry (THM-GC-MS) to overcome the difficulties of biomarker evaluation. The in-series combination consists of an LC analysis where fractions are collected and then transferred to the THM-GC-MS system. This was either done with comprehensive coupling, transferring all the fractions, or with hyphenated interfacing, i.e. off-line multi heart-cutting, transferring only selected fractions. Owing to the high sensitivity and selectivity of LC as a sample pre-treatment method, and to the high specificity of the MS as a detector, this analytical approach, NPLC × THM-GC-MS, is extremely sensitive. The results obtained indicate that this analytical set-up is able to detect down to 1 × 10(3) mycobacteria/mL of Mycobacterium tuberculosis strain 124, spiked in blank sputum samples. It is a powerful analytical tool and also has great potential for full automation. If further studies demonstrate its usefulness when applied blind in real sputum specimens, this technique could compete with the current smear microscopy in the early diagnosis of tuberculosis. Copyright © 2015 Elsevier B.V. All rights reserved.

Chemical/structural characterization of carbon nanoparticles produced by laser pyrolysis and used for nanotube growth

International Nuclear Information System (INIS)

Orlanducci, S.; Valentini, F.; Piccirillo, S.; Terranova, M.L.; Botti, S.; Ciardi, R.; Rossi, M.; Palleschi, G.

2004-01-01

Carbon nanoparticles produced by CO 2 laser pyrolysis have been investigated using morphological and structural probes such as high-resolution scanning electron microscopy, transmission electron microscopy, Raman spectroscopy and electron diffraction, as well as chemical probes, such as gas chromatography-mass spectrometry and fast atom bombardment-mass spectrometry. The produced particles resulted to have a spherical shape and a diameter of about 50 nm with graphitic domains of the order of 80 A. They contain appreciable fractions of polycyclic aromatic hydrocarbons, which can be extracted with toluene, as well as fullerene units. The implications of these results for the use of carbon nanopowders in the carbon nanotube synthesis are also discussed

Pyrolysis and oxidative pyrolysis experiments with organization exchange resin

International Nuclear Information System (INIS)

Chun, Ung Kyung

1997-01-01

Pyrolysis may be an important pretreatment step before vitrification in a cold crucible melter (CCM). During vitrification of organic resin the carbon or other remaining residues may harm the performance of the cold crucible melter of the eventual stability of the final glass product. Hence, it is important to reduce or prevent such harmful waste from entry into the cold crucible melter. Pretreatment with pyrolysis will generally provide volume reduction resulting in less amount of solid waste that needs to be handled by the CCM; in addition, the pyrolytic processes may breakdown much of the complex organics causing release through volatilization resulting in less carbon and other harmful substances. Hence, KEPRI has undertaken studies on the pyrolysis and oxidative pyrolysis of organic ion exchange resin. Pyrolysis and oxidative pyrolysis were examined with TGA and a tube furnace. TGA results for pyrolysis with the flow of nitrogen indicate that even after pyrolyzing from room temperature to about 900 deg C, a significant mass fraction of the original cationic resin remains, approximately 46 %. The anionic resin when pyrolytically heated in a flow of nitrogen only, from room temperature to about 900 deg C, produced a final residue mass fraction of about 8 percent. Oxidation at a ratio of air to nitrogen, 1:2, reduced the cationic resin to 5.3% when heated at 5 C/min. Oxidation of anionic resin at the same ratio and same heating rate left almost no solid residue. Pyrolysis (e.g. nitrogen-only environment) in the tube furnace of larger samples relative to the TGA produced very similar results to the TGA. The differences may be attributed to the scale effects such as surface area exposure to the gas stream, temperature distributions throughout the resin, etc. (author) 7 refs., 7 figs

Pyrolysis and oxidative pyrolysis experiments with organization exchange resin

Energy Technology Data Exchange (ETDEWEB)

Chun, Ung Kyung [Korea Electric Power Research Insititute, Taejon (Korea, Republic of)

1997-12-31

Pyrolysis may be an important pretreatment step before vitrification in a cold crucible melter (CCM). During vitrification of organic resin the carbon or other remaining residues may harm the performance of the cold crucible melter of the eventual stability of the final glass product. Hence, it is important to reduce or prevent such harmful waste from entry into the cold crucible melter. Pretreatment with pyrolysis will generally provide volume reduction resulting in less amount of solid waste that needs to be handled by the CCM; in addition, the pyrolytic processes may breakdown much of the complex organics causing release through volatilization resulting in less carbon and other harmful substances. Hence, KEPRI has undertaken studies on the pyrolysis and oxidative pyrolysis of organic ion exchange resin. Pyrolysis and oxidative pyrolysis were examined with TGA and a tube furnace. TGA results for pyrolysis with the flow of nitrogen indicate that even after pyrolyzing from room temperature to about 900 deg C, a significant mass fraction of the original cationic resin remains, approximately 46 %. The anionic resin when pyrolytically heated in a flow of nitrogen only, from room temperature to about 900 deg C, produced a final residue mass fraction of about 8 percent. Oxidation at a ratio of air to nitrogen, 1:2, reduced the cationic resin to 5.3% when heated at 5 C/min. Oxidation of anionic resin at the same ratio and same heating rate left almost no solid residue. Pyrolysis (e.g. nitrogen-only environment) in the tube furnace of larger samples relative to the TGA produced very similar results to the TGA. The differences may be attributed to the scale effects such as surface area exposure to the gas stream, temperature distributions throughout the resin, etc. (author) 7 refs., 7 figs.

Polycyclic aromatic hydrocarbons (PAHs) and volatile organic compounds (VOCs) mitigation in the pyrolysis process of waste tires using CO₂ as a reaction medium.

Science.gov (United States)

Kwon, Eilhann E; Oh, Jeong-Ik; Kim, Ki-Hyun

2015-09-01

Our work reported the CO2-assisted mitigation of PAHs and VOCs in the thermo-chemical process (i.e., pyrolysis). To investigate the pyrolysis of used tires to recover energy and chemical products, the experiments were conducted using a laboratory-scale batch-type reactor. In particular, to examine the influence of the CO2 in pyrolysis of a tire, the pyrolytic products including C1-5-hydrocarbons (HCs), volatile organic carbons (VOCs), and polycyclic aromatic hydrocarbons (PAHs) were evaluated qualitatively by gas chromatography (GC) with mass spectroscopy (MS) as well as with a thermal conductivity detector (TCD). The mass balance of the pyrolytic products under various pyrolytic conditions was established on the basis of their weight fractions of the pyrolytic products. Our experimental work experimentally validated that the amount of gaseous pyrolytic products increased when using CO2 as a pyrolysis medium, while substantially altering the production of pyrolytic oil in absolute content (7.3-17.2%) and in relative composition (including PAHs and VOCs). Thus, the co-feeding of CO2 in the pyrolysis process can be considered an environmentally benign and energy efficient process. Copyright © 2015 Elsevier Ltd. All rights reserved.

Measurement of Muscle Protein Fractional Synthetic Rate by Capillary Gas Chromatography/Combustion Isotope Ratio Mass Spectrometry

OpenAIRE

Yarasheski, Kevin E.; Smith, Kenneth; Rennie, Michael J.; Bier, Dennis M.

1992-01-01

The measurement of skeletal muscle protein fractional synthetic rate using an infusion of (1-13C)leucine and measuring the isotopic abundance of the tracer in skeletal muscle protein by preparative gas chromatography (GC)/ninhydrin isotope ratio mass spectrometry (IRMS) is laborious and subject to errors owing to contamination by 12C. The purpose of this study was to compare muscle (13C)leucine enrichment measured with the conventional preparative GC/ninhydrin IRMS approach to a new, continuo...

Characterisation and discrimination of various types of lac resin using gas chromatography mass spectrometry techniques with quaternary ammonium reagents.

Science.gov (United States)

Sutherland, K; del Río, J C

2014-04-18

A variety of lac resin samples obtained from artists' suppliers, industrial manufacturers, and museum collections were analysed using gas chromatography mass spectrometry (GCMS) and reactive pyrolysis GCMS with quaternary ammonium reagents. These techniques allowed a detailed chemical characterisation of microgram-sized samples, based on the detection and identification of derivatives of the hydroxy aliphatic and cyclic (sesquiterpene) acids that compose the resin. Differences in composition could be related to the nature of the resin, e.g. wax-containing (unrefined), bleached, or aged samples. Furthermore, differences in the relative abundances of aliphatic hydroxyacids appear to be associated with the biological source of the resin. The diagnostic value of newly characterised lac components, including 8-hydroxyacids, is discussed here for the first time. Identification of derivatised components was aided by AMDIS deconvolution software, and discrimination of samples was enhanced by statistical evaluation of data using principal component analysis. The robustness of the analyses, together with the minimal sample size required, make these very powerful approaches for the characterisation of lac resin in museum objects. The value of such analyses for enhancing the understanding of museum collections is illustrated by two case studies of objects in the collection of the Philadelphia Museum of Art: a restorer's varnish on a painting by Luca Signorelli, and a pictorial inlay in an early nineteenth-century High Chest by George Dyer. Copyright © 2014 Elsevier B.V. All rights reserved.

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…

Qualitative and Quantitative Analysis of Volatile Components of Zhengtian Pills Using Gas Chromatography Mass Spectrometry and Ultra-High Performance Liquid Chromatography.

Science.gov (United States)

Liu, Cui-Ting; Zhang, Min; Yan, Ping; Liu, Hai-Chan; Liu, Xing-Yun; Zhan, Ruo-Ting

2016-01-01

Zhengtian pills (ZTPs) are traditional Chinese medicine (TCM) which have been commonly used to treat headaches. Volatile components of ZTPs extracted by ethyl acetate with an ultrasonic method were analyzed by gas chromatography mass spectrometry (GC-MS). Twenty-two components were identified, accounting for 78.884% of the total components of volatile oil. The three main volatile components including protocatechuic acid, ferulic acid, and ligustilide were simultaneously determined using ultra-high performance liquid chromatography coupled with diode array detection (UHPLC-DAD). Baseline separation was achieved on an XB-C18 column with linear gradient elution of methanol-0.2% acetic acid aqueous solution. The UHPLC-DAD method provided good linearity (R (2) ≥ 0.9992), precision (RSD components, protocatechuic acid, ferulic acid, and ligustilide, in 13 batches of ZTPs, which is suitable for discrimination and quality assessment of ZTPs.

Direct Growth of Bacteria in Headspace Vials Allows for Screening of Volatiles by Gas Chromatography Mass Spectrometry

OpenAIRE

Collin M. Timm; Evan P. Lloyd; Amanda Egan; Ray Mariner; David Karig

2018-01-01

Bacterially produced volatile organic compounds (VOCs) can modify growth patterns of eukaryotic hosts and competing/cohabiting microbes. These compounds have been implicated in skin disorders and attraction of biting pests. Current methods to detect and characterize VOCs from microbial cultures can be laborious and low-throughput, making it difficult to understand the behavior of microbial populations. In this work we present an efficient method employing gas chromatography/mass spectrometry ...

Ink dating using thermal desorption and gas chromatography / mass spectrometry: comparison of results obtained in two laboratories

OpenAIRE

Koenig, A.; Bügler, J.; Kirsch, D.; Köhler, F.; Weyermann, C.

2015-01-01

Recent ink dating methods focused mainly on changes in solvent amounts occurring over time. A promising method was developed at the Landeskriminalamt of Munich using thermal desorption (TD) followed by gas chromatography / mass spectrometry (GC/MS) analysis. Sequential extractions of the phenoxyethanol present in ballpoint pen ink entries were carried out at two different temperatures. This method is applied in forensic practice and is currently implemented in several laboratories participati...

Gas chromatography-mass spectrometry with supersonic molecular beams.

Science.gov (United States)

Amirav, Aviv; Gordin, Alexander; Poliak, Marina; Fialkov, Alexander B

2008-02-01

Gas chromatography-mass spectrometry (GC-MS) with supersonic molecular beams (SMBs) (also named Supersonic GC-MS) is based on GC and MS interface with SMBs and on the electron ionization (EI) of vibrationally cold analytes in the SMBs (cold EI) in a fly-through ion source. This ion source is inherently inert and further characterized by fast response and vacuum background filtration capability. The same ion source offers three modes of ionization including cold EI, classical EI and cluster chemical ionization (CI). Cold EI, as a main mode, provides enhanced molecular ions combined with an effective library sample identification, which is supplemented and complemented by a powerful isotope abundance analysis method and software. The range of low-volatility and thermally labile compounds amenable for analysis is significantly increased owing to the use of the contact-free, fly-through ion source and the ability to lower sample elution temperatures through the use of high column carrier gas flow rates. Effective, fast GC-MS is enabled particularly owing to the possible use of high column flow rates and improved system selectivity in view of the enhancement of the molecular ion. This fast GC-MS with SMB can be further improved via the added selectivity of MS-MS, which by itself benefits from the enhancement of the molecular ion, the most suitable parent ion for MS-MS. Supersonic GC-MS is characterized by low limits of detection (LOD), and its sensitivity is superior to that of standard GC-MS, particularly for samples that are hard for analysis. The GC separation of the Supersonic GC-MS can be improved with pulsed flow modulation (PFM) GC x GC-MS. Electron ionization LC-MS with SMB can also be combined with the Supersonic GC-MS, with fast and easy switching between these two modes of operation. (c) 2008 John Wiley & Sons, Ltd.

Extending the molecular application range of gas chromatography

NARCIS (Netherlands)

Kaal, E.; Janssen, H.-G.

2008-01-01

Gas chromatography is an important analytical technique for qualitative and quantitative analysis in a wide range of application areas. It is fast, provides a high peak capacity, is sensitive and allows combination with a wide range of selective detection methods including mass spectrometry.

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.

The Application of Resonance-Enhanced Multiphoton Ionization Technique in Gas Chromatography Mass Spectrometry

Directory of Open Access Journals (Sweden)

Adan Li

2014-01-01

Full Text Available Gas chromatography resonance-enhanced multiphoton ionization time-of-flight mass spectrometry (GC/REMPI-TOFMS using a nanosecond laser has been applied to analyze the 16 polycyclic aromatic hydrocarbons (PAHs. The excited-state lifetime, absorption characters, and energy of electronic states of the 16 PAHs were investigated to optimize the ionization yield. A river water sample pretreated by means of solid phase extraction was analyzed to evaluate the performance of the analytical instrument. The results suggested that REMPI is superior to electron impact ionization method for soft ionization and suppresses the background signal due to aliphatic hydrocarbons. Thus, GC/REMPI-TOFMS is a more reliable method for the determination of PAHs present in the environment.

An appraisal on the degradation of paracetamol by TiO2/UV system in aqueous medium: product identification by gas chromatography-mass spectrometry (GC-MS)

OpenAIRE

Dalmázio,Ilza; Alves,Tânia M. A.; Augusti,Rodinei

2008-01-01

The advanced oxidation of paracetamol (1) promoted by TiO2/UV system in aqueous medium was investigated. Continuous monitoring by several techniques, such as UV-Vis spectroscopy, HPLC (high performance liquid chromatography), TOC (total organic carbon), and ESI-MS (electrospray ionization mass spectrometry), revealed that whereas the removal of paracetamol was highly efficient under these conditions, its mineralization was not likewise accomplished. GC-MS (gas chromatography-mass spectrometry...

Analysis of the chemical composition of the essential oils extracted from Lippia lacunosa Mart. and Schauer and Lippia rotundifolia Cham. (Verbenaceae) by gas chromatography and gas chromatography-mass spectrometry

International Nuclear Information System (INIS)

Leitao, Suzana G.; Barbosa, Ymira Galico; Viccini, Lyderson F.; Salimena, Fatima R.G.; Peixoto, Paulo H.P.

2008-01-01

Lippia lacunosa and L. rotundifolia (Verbenaceae) are two Brazilian species of complex taxonomic delimitation. The composition of the essential oils from leaves and flowers of these plants was investigated by gas chromatography (GC) and gas chromatography coupled with mass spectrometry (GC-MS) analysis. The major components of the essential oils of flowers and leaves of L. lacunosa were: myrcene (14.7% and 11.9%), myrcenone (45.2% and 64.2%), Z-ocimenone (5.7% and 5.2%), and E-ocimenone (14.7% and 4.1%), respectively; whereas in L. rotundifolia (flowers and leaves) were ..-pinene (8.7% and 1.8%), myrcene (5.1% and 3.6%), limonene (26.0% and 7.9 %), cis-pinocamphone (4.5% and 3.1%) and myrtenal (22.3% and 16.7%), respectively. The essential oils from L. lacunosa exhibited a strong and pleasant mango aroma, which was related to the presence of myrcene and myrcenone. The marked differences in the chemical composition of their essential oils may represent a powerful tool for the botanical classification. (author)

Analysis of the chemical composition of the essential oils extracted from Lippia lacunosa Mart. and Schauer and Lippia rotundifolia Cham. (Verbenaceae) by gas chromatography and gas chromatography-mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Leitao, Suzana G.; Barbosa, Ymira Galico [Universidade Federal do Rio de Janeiro (UFRJ), Rio de Janeiro, RJ (Brazil). Fac. de Farmacia; Oliveira, Danilo R. de; Leitao, Gilda G. [Universidade Federal do Rio de Janeiro (UFRJ), Rio de Janeiro, RJ (Brazil). Nucleo de Pesquisas de Produtos Naturais]. E-mail: sgleitao@pharma.ufrj.br; Suelsen, Valeria; Martino, Virginia [Universidad de Buenos Aires (Argentina). Facultad de Farmacia y Bioquimica; Bizzo, Humberto R.; Lopes, Daise [EMBRAPA Agroindustria de Alimentos, Rio de Janeiro, RJ (Brazil); Viccini, Lyderson F.; Salimena, Fatima R.G.; Peixoto, Paulo H.P. [Universidade Federal de Juiz de Fora (UFJF), Juiz de Fora, MG (Brazil). Inst. de Ciencias Biolgicas

2008-07-01

Lippia lacunosa and L. rotundifolia (Verbenaceae) are two Brazilian species of complex taxonomic delimitation. The composition of the essential oils from leaves and flowers of these plants was investigated by gas chromatography (GC) and gas chromatography coupled with mass spectrometry (GC-MS) analysis. The major components of the essential oils of flowers and leaves of L. lacunosa were: myrcene (14.7% and 11.9%), myrcenone (45.2% and 64.2%), Z-ocimenone (5.7% and 5.2%), and E-ocimenone (14.7% and 4.1%), respectively; whereas in L. rotundifolia (flowers and leaves) were ..-pinene (8.7% and 1.8%), myrcene (5.1% and 3.6%), limonene (26.0% and 7.9 %), cis-pinocamphone (4.5% and 3.1%) and myrtenal (22.3% and 16.7%), respectively. The essential oils from L. lacunosa exhibited a strong and pleasant mango aroma, which was related to the presence of myrcene and myrcenone. The marked differences in the chemical composition of their essential oils may represent a powerful tool for the botanical classification. (author)

Catalytic fast co-pyrolysis of biomass and food waste to produce aromatics: Analytical Py-GC/MS study.

Science.gov (United States)

Zhang, Bo; Zhong, Zhaoping; Min, Min; Ding, Kuan; Xie, Qinglong; Ruan, Roger

2015-01-01

In this study, catalytic fast co-pyrolysis (co-CFP) of corn stalk and food waste (FW) was carried out to produce aromatics using quantitative pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS), and ZSM-5 zeolite in the hydrogen form was employed as the catalyst. Co-CFP temperature and a parameter called hydrogen to carbon effective ratio (H/C(eff) ratio) were examined for their effects on the relative content of aromatics. Experimental results showed that co-CFP temperature of 600 °C was optimal for the formation of aromatics and other organic pyrolysis products. Besides, H/C(eff) ratio had an important influence on product distribution. The yield of total organic pyrolysis products and relative content of aromatics increased non-linearly with increasing H/C(eff) ratio. There was an apparent synergistic effect between corn stalk and FW during co-CFP process, which promoted the production of aromatics significantly. Co-CFP of biomass and FW was an effective method to produce aromatics and other petrochemicals. Copyright © 2015. Published by Elsevier Ltd.

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…

Development of conjugate methods with gas chromatography for inorganic compounds analysis

International Nuclear Information System (INIS)

Baccan, N.

1975-01-01

The application of gas chromatography combined with mass spectrometry or with nuclear methods for the analysis of inorganic compounds is studied. The advantages of the use of a gas chromatograph coupled with a quadrupole mass spectrometer or with a high resolution radiation detector, are discussed. We also studied the formation and solvent extraction of metal chelates; an aliquot of the organic phase was directly injected into the gas chromatograph and the eluted compounds were detected by mass spectrometry or, when radioactive, by nuclear methods. (author)

MEASUREMENT OF PYRETHROID RESIDUES IN ENVIRONMENTAL AND FOOD SAMPLES BY ENHANCED SOLVENT EXTRACTION/SUPERCRITICAL FLUID EXTRACTION COUPLED WITH GAS CHROMATOGRAPHY-TANDEM MASS SPECTROMETRY

Science.gov (United States)

The abstract summarizes pyrethorid methods development research. It provides a summary of sample preparation and analytical techniques such as supercritical fluid extraction, enhance solvent extraction, gas chromatography and tandem mass spectrometry.

Demonstration of the waste tire pyrolysis process on pilot scale in a continuous auger reactor

International Nuclear Information System (INIS)

Martínez, Juan Daniel; Murillo, Ramón; García, Tomás; Veses, Alberto

2013-01-01

Highlights: • The continuous pyrolysis of waste tire has been demonstrated at pilot scale in an auger reactor. • More than 500 kg of waste tires were processed in 100 operational hours. • The yields and characteristics of the pyrolysis products remained constant. • Mass and energy balances for an industrial scale plant are provided. • The reaction enthalpy necessary to perform the waste tire pyrolysis was determined. -- Abstract: This work shows the technical feasibility for valorizing waste tires by pyrolysis using a pilot scale facility with a nominal capacity of 150 kW th . A continuous auger reactor was operated to perform thirteen independent experiments that conducted to the processing of more than 500 kg of shredded waste tires in 100 h of operation. The reaction temperature was 550 °C and the pressure was 1 bar in all the runs. Under these conditions, yields to solid, liquid and gas were 40.5 ± 0.3, 42.6 ± 0.1 and 16.9 ± 0.3 wt.% respectively. Ultimate and proximate analyses as well as heating value analysis were conducted for both the solid and liquid fraction. pH, water content, total acid number (TAN), viscosity and density were also assessed for the liquid and compared to the specifications of marine fuels (standard ISO 8217). Gas chromatography was used to calculate the composition of the gaseous fraction. It was observed that all these properties remained practically invariable along the experiments without any significant technical problem. In addition, the reaction enthalpy necessary to perform the waste tire pyrolysis process (907.1 ± 40.0 kJ/kg) was determined from the combustion and formation enthalpies of waste tire and conversion products. Finally, a mass balance closure was performed showing an excellent reliability of the data obtained from the experimental campaign

Demonstration of the waste tire pyrolysis process on pilot scale in a continuous auger reactor

Energy Technology Data Exchange (ETDEWEB)

Martínez, Juan Daniel, E-mail: juand.martinez@upb.edu.co [Instituto de Carboquímica, ICB-CSIC, Miguel Luesma Castán 4, 50018, Zaragoza (Spain); Grupo de Investigaciones Ambientales, Instituto de Energía, Materiales y Medio Ambiente, Universidad Pontificia Bolivariana, Circular 1 N°70-01, Bloque 11, piso 2, Medellín (Colombia); Murillo, Ramón; García, Tomás; Veses, Alberto [Instituto de Carboquímica, ICB-CSIC, Miguel Luesma Castán 4, 50018, Zaragoza (Spain)

2013-10-15

Highlights: • The continuous pyrolysis of waste tire has been demonstrated at pilot scale in an auger reactor. • More than 500 kg of waste tires were processed in 100 operational hours. • The yields and characteristics of the pyrolysis products remained constant. • Mass and energy balances for an industrial scale plant are provided. • The reaction enthalpy necessary to perform the waste tire pyrolysis was determined. -- Abstract: This work shows the technical feasibility for valorizing waste tires by pyrolysis using a pilot scale facility with a nominal capacity of 150 kW{sub th}. A continuous auger reactor was operated to perform thirteen independent experiments that conducted to the processing of more than 500 kg of shredded waste tires in 100 h of operation. The reaction temperature was 550 °C and the pressure was 1 bar in all the runs. Under these conditions, yields to solid, liquid and gas were 40.5 ± 0.3, 42.6 ± 0.1 and 16.9 ± 0.3 wt.% respectively. Ultimate and proximate analyses as well as heating value analysis were conducted for both the solid and liquid fraction. pH, water content, total acid number (TAN), viscosity and density were also assessed for the liquid and compared to the specifications of marine fuels (standard ISO 8217). Gas chromatography was used to calculate the composition of the gaseous fraction. It was observed that all these properties remained practically invariable along the experiments without any significant technical problem. In addition, the reaction enthalpy necessary to perform the waste tire pyrolysis process (907.1 ± 40.0 kJ/kg) was determined from the combustion and formation enthalpies of waste tire and conversion products. Finally, a mass balance closure was performed showing an excellent reliability of the data obtained from the experimental campaign.

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.

Co-pyrolysis of coal with hydrogen-rich gases. 1. Coal pyrolysis under coke-oven gas and synthesis gas

Energy Technology Data Exchange (ETDEWEB)

Liao, H.; Li, B.; Zhang, B. [Chinese Academy of Sciences, Taiyuan (China). State Key Lab. of Coal Conversion

1998-06-01

To improve the economics of the hydropyrolysis process, it has been suggested that cheaper hydrogen-rich gases (such as coke oven gas, synthesis gas) could be used instead of pure hydrogen. Pyrolysis of Chinese Xianfeng lignite was carried out with coke oven gas (COG) and synthesis gas (SG) as reactive gases at 0.1-5 MPa and at a final temperature up to 650{degree}C with a heating rate of 5-25{degree}C min{sup -1} in a 10 g fixed-bed reactor. The results indicate that it is possible to use COG and SG instead of pure hydrogen in hydropyrolysis, but that the experimental conditions must be adjusted to optimize the yields of the valuable chemicals. 14 refs., 3 figs., 6 tabs.

Determination of clebopride in plasma by capillary gas chromatography-negative-ion chemical ionization mass spectrometry.

Science.gov (United States)

Robinson, P R; Jones, M D; Maddock, J

1988-11-18

A procedure for the analysis of clebopride in plasma using capillary gas chromatography-negative-ion chemical ionization mass spectrometry has been developed. Employing an ethoxy analogue as internal standard, the two compounds were extracted from basified plasma using dichloromethane. Subsequent reaction with heptafluorobutyryl imidazole produced volatile monoheptafluorobutyryl derivatives whose ammonia negative-ion mass spectra proved ideal for selected-ion monitoring. The recovery of clebopride from plasma at 0.536 nmol/l was found to be 85.5 +/- 0.9% (n = 3) whilst measurement down to 0.268 nmol/l was possible with a coefficient of variation of 7.9%. Plasma levels of the compound are reported in two volunteers following ingestion of 1 mg of clebopride as the malate salt.

Serum/plasma methylmercury determination by isotope dilution gas chromatography-inductively coupled plasma mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Baxter, Douglas C., E-mail: douglas.baxter@alsglobal.com [ALS Scandinavia AB, Aurorum 10, 977 75 Lulea (Sweden); Faarinen, Mikko [ALS Scandinavia AB, Aurorum 10, 977 75 Lulea (Sweden); Osterlund, Helene; Rodushkin, Ilia [ALS Scandinavia AB, Aurorum 10, 977 75 Lulea (Sweden); Division of Geosciences, Lulea University of Technology, 977 87 Lulea (Sweden); Christensen, Morten [ALS Scandinavia AB, Maskinvaegen 2, 183 53 Taeby (Sweden)

2011-09-09

Highlights: {center_dot} We determine methylmercury in serum and plasma using isotope dilution calibration. {center_dot} Separation by gas chromatography and detection by inductively coupled plasma mass spectrometry. {center_dot} Data for 50 specimens provides first reference range for methylmercury in serum. {center_dot} Serum samples shown to be stable for 11 months in refrigerator. - Abstract: A method for the determination of methylmercury in plasma and serum samples was developed. The method uses isotope dilution with {sup 198}Hg-labeled methylmercury, extraction into dichloromethane, back-extraction into water, aqueous-phase ethylation, purge and trap collection, thermal desorption, separation by gas chromatography, and mercury isotope specific detection by inductively coupled plasma mass spectrometry. By spiking 2 mL sample with 1.2 ng tracer, measurements in a concentration interval of (0.007-2.9) {mu}g L{sup -1} could be performed with uncertainty amplification factors <2. A limit of quantification of 0.03 {mu}g L{sup -1} was estimated at 10 times the standard deviation of concentrations measured in preparation blanks. Within- and between-run relative standard deviations were <10% at added concentration levels of 0.14 {mu}g L{sup -1}, 0.35 {mu}g L{sup -1} and 2.8 {mu}g L{sup -1}, with recoveries in the range 82-110%. Application of the method to 50 plasma/serum samples yielded a median (mean; range) concentration of methylmercury of 0.081 (0.091; <0.03-0.19) {mu}g L{sup -1}. This is the first time methylmercury has been directly measured in this kind of specimen, and is therefore the first estimate of a reference range.

Bio-oil production from dry sewage sludge by fast pyrolysis in an electrically-heated fluidized bed reactor

Directory of Open Access Journals (Sweden)

Renato O. Arazo

2017-01-01

Full Text Available The optimization of bio-oil produced from sewage sludge using fast pyrolysis in a fluidized bed reactor was investigated. Effects of temperature, sludge particle size and vapor residence time on bio-oil properties, such as yield, high heating value (HHV and moisture content were evaluated through experimental and statistical analyses. Characterization of the pyrolysis products (bio-oil and biogas was also done. Optimum conditions produced a bio-oil product with an HHV that is nearly twice as much as lignocellulosic-derived bio-oil, and with properties comparable to heavy fuel oil. Contrary to generally acidic bio-oil, the sludge-derived bio-oil has almost neutral pH which could minimize the pipeline and engine corrosions. The Fourier Transform Infrared and gas-chromatography and mass spectrometry analyses of bio-oil showed a dominant presence of gasoline-like compounds. These results demonstrate that fast pyrolysis of sewage sludge from domestic wastewater treatment plant is a favorable technology to produce biofuels for various applications.

Catalytic Upgrading of Biomass Fast Pyrolysis Vapors with Nano Metal Oxides: An Analytical Py-GC/MS Study

Energy Technology Data Exchange (ETDEWEB)

Qiang Lu [National Engineering Laboratory for Biomass Power Generation Equipment, North China Electric Power University, Beijing (China); Zhi-Fei Zhang [National Engineering Laboratory for Biomass Power Generation Equipment, North China Electric Power University, Beijing (China); Chang-Qing Dong [National Engineering Laboratory for Biomass Power Generation Equipment, North China Electric Power University, Beijing (China); Xi-Feng Zhu [Key Laboratory for Biomass Clean Energy of Anhui Province, University of Science and Technology of China, Hefei (China)

2010-10-15

Fast pyrolysis of poplar wood followed with catalytic cracking of the pyrolysis vapors was performed using analytical pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS). The catalysts applied in this study were nano MgO, CaO, TiO2, Fe2O3, NiO and ZnO. These catalysts displayed different catalytic capabilities towards the pyrolytic products. The catalysis by CaO significantly reduced the levels of phenols and anhydrosugars, and eliminated the acids, while it increased the formation of cyclopentanones, hydrocarbons and several light compounds. ZnO was a mild catalyst, as it only slightly altered the pyrolytic products. The other four catalysts all decreased the linear aldehydes dramatically, while the increased the ketones and cyclopentanones. They also reduced the anhydrosugars, except for NiO. Moreover, the catalysis by Fe2O3 resulted in the formation of various hydrocarbons. However, none of these catalysts except CaO were able to greatly reduce the acids.

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.

Multiresidue analysis of pesticides in olive oil by gel permeation chromatography followed by gas chromatography-tandem mass-spectrometric determination

International Nuclear Information System (INIS)

Sanchez, Andres Garcia; Martos, Natividad Ramos; Ballesteros, Evaristo

2006-01-01

A method for the multiresidue analysis of olive oil samples for 26 pesticides is proposed. Residual pesticides are extracted from oil using an n-hexane/acetonitrile mixture, extracts being cleaned-up by gel permeation chromatography (GPC) for analysis by gas chromatography-tandem mass spectrometry (GC-MS/MS). Electron ionization and chemical ionization are employed in a single analysis for the determination of pesticides. Pesticide recoveries from virgin and refined olive oil spiked with 10, 100 and 250 μg/kg concentrations of the pesticides ranged from 83.8 to 110.3%. The proposed method features good sensitivity: its limits of quantification are low enough to allow pesticide residues to be determined at concentrations below the maximum residue levels legally accepted. The precision, expressed as relative standard deviation, ranges from 4.93 to 8.11%. Applicability was tested on 40 olive oil samples. Several pesticides were detected in most of the virgin olive oil samples. By contrast, refined olive samples contained few pesticides, and only endosulfan sulphate was detected in all

Energy and resource utilization of deinking sludge pyrolysis

International Nuclear Information System (INIS)

Lou, Rui; Wu, Shubin; Lv, Gaojin; Yang, Qing

2012-01-01

The thermochemical conversion technique was applied in deinking sludge from the pulp and papermaking industrial to indagate the utilization of sludge biomass to energy, and the pyrolysis characteristics and pyrolytic products of deinking sludge were studied with thermogravimetric analysis (TGA) and pyrolysis coupled with gas chromatograph–mass spectrometer (Py-GC/MS). The static tubular furnace as an applied industrial research was used to study deinking sludge pyrolysis. The solid, gas and liquid of products was characterized by electron probe microanalysis (EPMA), gas chromatograph (GC) and gas chromatograph–mass (GC/MS), respectively. The results revealed that the weight-loss process of deinking sludge was a non-isothermal reaction and composed of four stages, i.e. dewater stage, volatile releasing stage, carbon burnout stage and some calcium carbonate decomposition. Pyrolytic products from deinking sludge in the static tubular furnace were comprised of the gaseous (29.78%), condensed liquid (bio-oil, 24.41%) and solid residues (45.81%). The volatiles from deinking sludge pyrolyzing were almost aromatic hydrocarbons, i.e. styrene, toluene and benzene and few acids and the solid was calcium carbonate (CaCO 3 ) that can be reused as paper filler. Deinking sludge was converted into high-grade fuel and chemicals by means of thermochemical conversion techniques, hence, pyrolysis of paper deinking sludge had a promising development on the comprehensive utilization.

Analyse quantitative des effluents de pyrolyse en milieu ouvert et fermé Quantitative Analysis of Pyrolysis Effluents in an Open and Closed System

Directory of Open Access Journals (Sweden)

Behar F.

2006-11-01

Full Text Available Dans la première partie de l'article, nous décrivons une technique de pyrolyse en milieu ouvert qui permet de caractériser les matières organiques complexes comme le kérogène, le charbon, les asphaltènes de roche et d'huiles, les substances humiques et fulviques etc. Les effluents de pyrolyse sont récupérés et fractionnés quantitativement puis analysés par des techniques spécifiques comme la chromatographie en phase gazeuse et le couplage chromatographie/spectrométrie de masse. Dans la deuxième partie, est présentée une technique de pyrolyse en milieu fermé pour simuler au laboratoire l'évolution thermique des kérogènes, asphaltènes ou huiles. Nous nous sommes surtout attachés à dresser des bilans massiques et des bilans de l'hydrogène sur l'ensemble des produits de pyrolyse. Pour cela, nous avons distingué cinq classes de poids moléculaire croissant : C1, C2-C5, C6-C13, C14+ et coke. La récupération quantitative et la séparation de chacune des cinq fractions permet une analyse moléculaire détaillée de chacune d'elles. The first part of this article describes an open pyrolysis system in order to characterize complex organic matter such as kerogen, coal, rock and oil asphaltenes and humic substances, etc. Pyrolysis effluents are recovered, fractionated quantitatively by liquid chromatography, and then they are analyzed by specific techniques such as gas chromatography and chromatography/mass-spectrometry coupling. The second part describes a pyrolysis technique in a closed system, used for the laboratory simulation of the thermal evolution of kerogens, asphaltenes or oils. A special effort has been made to give the mass and hydrogen balances for all pyrolysis products. For this, five classes have been distinguised with increasing molecular weight: C1, C2-C5, C6-C13, C14+ and coke. The quantitative recovery and the separation of each of the five fractions is used to make a detailed molecular analysis of each of

Co-pyrolysis of waste propylene and gas oil from Campos Basin: a case study; Tecnologia de co-pirolise de polipropileno pos-consumo com gasoleo da Bacia de Campos: um estudo de caso

Energy Technology Data Exchange (ETDEWEB)

Assumpcao, Luiz Carlos F.N. de; Aguiar, Monica Regina M.P. de [Universidade do Estado do Rio de Janeiro (UERJ), RJ (Brazil); Carbonell, Montserrat Motas [PETROBRAS, Rio de Janeiro, RJ (Brazil)

2008-07-01

In this study the process of co-pyrolysis of plastic polypropylene residues with gas-oil was evaluated, varying the temperature and the amount of polypropylene. The co-pyrolysis is a promising route to minimize the environmental impact caused by the inadequate plastic disposal, preventing its accumulation and giving a better use of the not renewable raw material (oil). The polypropylene samples and gas-oil were submitted to the thermal co-pyrolysis in inert atmosphere, varying the temperature from 400 deg C to 500 deg C and the amount of PP from 0,1 to 1,0 g. The influence of gas-oil was evaluated carrying the co-pyrolysis in the absence of PP. The pyrolyzed liquids produced by this thermal treatment had been characterized by modified gaseous chromatography objectifying the evaluation of the diesel fractions generation. As a result, the increase of PP amount lead to a reduction in the income of the pyrolytic liquid and to increase of the amount of solid generated. The effect of the increase of temperature showed an inverse result. The addition of PP in the reactor showed little interference in diesel range of distillation in the co-pyrolysis. On the other hand, an increase in temperature favors the increase of products in this range of distillation. The results show that plastic residue co-pyrolysis is a potential method of chemical recycling. (author)

Capillary gas-solid chromatography

International Nuclear Information System (INIS)

Berezkin, V.G.

1996-01-01

Modern state of gas adsorption chromatography in open capillary columns has been analyzed. The history of the method development and its role in gas chromatography, ways to construct open adsorptional capillary columns, foundations of the theory of retention and washing of chromatographic regions in gas adsorption capillary columns have been considered. The fields is extensively and for analyzing volatile compounds of different isotopic composition, inorganic and organic gases, volatile organic polar compounds, aqueous solutions of organic compounds. Separation of nuclear-spin isomers and isotopes of hydrogen is the first illustrative example of practical application of the adsorption capillary chromatography. It is shown that duration of protium and deuterium nuclear isomers may be reduced if the column temperature is brought to 47 K

Numerical modeling of pyrolysis of sawdust in a packed bed

Energy Technology Data Exchange (ETDEWEB)

Meng, Qingmin; Chen, Xiaoping [Southeast Univ., Nanjing (China). School of Energy and Environment

2013-07-01

An unsteady, one-dimensional mathematical model has been developed to describe the pyrolysis of sawdust in a packed bed. The sawdust bed was pyrolyzed using the hot gas and an electric heater outside the bed as the source of energy. The developed model includes mass, momentum and energy conservations of gas and solid within the bed. The gas flow in the bed is modeled using Darcy's law for fluid through a porous medium. The heat transfer model includes heat conduction inside the bed and convection between the bed and the hot gas. The kinetic model consists of primary pyrolysis reaction. A finite volume fully implicit scheme is employed for solving the heat and mass transfer model equations. A Runge-Kutta fourth order method is used for the chemical kinetics model equations. The model predictions of mass loss history and temperature were validated with published experimental results, showing a good agreement. The effects of inlet temperature on the pyrolysis process have been analyzed with model simulation. A sensitivity analysis using the model suggests that the predictions could be improved by considering the second reaction which could generate volatile flowing in the void.

A moving-bed gasifier with internal recycle of pyrolysis gas

NARCIS (Netherlands)

Susanto, H.; Beenackers, A.A C M

A co-current moving bed gasifier with internal recycle and separate combustion of pyrolysis gas has been developed with the aim of producing a design suitable for scaling-up downdraft gasifiers while maintaining a low tar content in the producer gas. Using wood chips with a moisture content of 7-9

Factors That Contribute to Assay Variation in Quantitative Analysis of Sex Steroid Hormones Using Liquid and Gas Chromatography-Mass Spectrometry

Science.gov (United States)

Xu, Xia; Veenstra, Timothy D.

2012-01-01

The list of physiological events in which sex steroids play a role continues to increase. To decipher the roles that sex steroids play in any condition requires high quality cohorts of samples and assays that provide highly accurate quantitative measures. Liquid and gas chromatography coupled with mass spectrometry (LC-MS and GC-MS) have…

Multiple inert gas elimination technique by micropore membrane inlet mass spectrometry--a comparison with reference gas chromatography.

Science.gov (United States)

Kretzschmar, Moritz; Schilling, Thomas; Vogt, Andreas; Rothen, Hans Ulrich; Borges, João Batista; Hachenberg, Thomas; Larsson, Anders; Baumgardner, James E; Hedenstierna, Göran

2013-10-15

The mismatching of alveolar ventilation and perfusion (VA/Q) is the major determinant of impaired gas exchange. The gold standard for measuring VA/Q distributions is based on measurements of the elimination and retention of infused inert gases. Conventional multiple inert gas elimination technique (MIGET) uses gas chromatography (GC) to measure the inert gas partial pressures, which requires tonometry of blood samples with a gas that can then be injected into the chromatograph. The method is laborious and requires meticulous care. A new technique based on micropore membrane inlet mass spectrometry (MMIMS) facilitates the handling of blood and gas samples and provides nearly real-time analysis. In this study we compared MIGET by GC and MMIMS in 10 piglets: 1) 3 with healthy lungs; 2) 4 with oleic acid injury; and 3) 3 with isolated left lower lobe ventilation. The different protocols ensured a large range of normal and abnormal VA/Q distributions. Eight inert gases (SF6, krypton, ethane, cyclopropane, desflurane, enflurane, diethyl ether, and acetone) were infused; six of these gases were measured with MMIMS, and six were measured with GC. We found close agreement of retention and excretion of the gases and the constructed VA/Q distributions between GC and MMIMS, and predicted PaO2 from both methods compared well with measured PaO2. VA/Q by GC produced more widely dispersed modes than MMIMS, explained in part by differences in the algorithms used to calculate VA/Q distributions. In conclusion, MMIMS enables faster measurement of VA/Q, is less demanding than GC, and produces comparable results.

Gas Chromatography and Mass Spectrometry Measurements and Protocols for Database and Library Development Relating to Organic Species in Support of the Mars Science Laboratory

Science.gov (United States)

Misra, P.; Garcia, R.; Mahaffy, P. R.

2010-04-01

An organic contaminant database and library has been developed for use with the Sample Analysis at Mars (SAM) instrumentation utilizing laboratory-based Gas Chromatography-Mass Spectrometry measurements of pyrolyzed and baked material samples.

Pyrolysis of polystyrene waste in the presence of activated carbon in conventional and microwave heating using modified thermocouple.

Science.gov (United States)

Prathiba, R; Shruthi, M; Miranda, Lima Rose

2018-06-01

Pyrolysis process was experimented using two types of heating source, namely conventional and microwave. Polystyrene (PS) plastic waste was used as feedstock in a batch reactor for both the conventional (slow pyrolysis) and microwave pyrolysis. The effect of activated carbon to polystyrene ratio on (i) yield of oil, gas and residues (ii) reaction temperature (iii) reaction time were studied. Quality of oil from pyrolysis of polystyrene were assessed for the possible applicability in fuel production. Microwave power of 450 W and polymer to activated carbon ratio of 10:1, resulted in the highest oil yield of 93.04 wt.% with a higher heating value of 45 MJ kg -1 and a kinematic viscosity of 2.7 cSt. Microwave heating when compared to conventional heating method, exhibits a reaction temperature and time of 330 °C in 5.5 min, whereas in conventional heating system it was 418 °C in 60 min. The gas chromatography-mass spectrometry analysis of liquid oil from microwave pyrolysis predominantly yields alkenes of 8.44 wt.%, α-methyl styrene 0.96 wt.%, condensed ring aromatics 23.21 wt.% and benzene derivatives 26.77 wt.% when the polystyrene to activated carbon ratio was 10:1. Significant factor of using microwave heating is the amount of energy converted (kWh) is lesser than conventional heating. Copyright © 2018 Elsevier Ltd. All rights reserved.

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…

Analysis of quinocide in unprocessed primaquine diphosphate and primaquine diphosphate tablets using gas chromatography-mass spectrometry with supersonic molecular beams.

Science.gov (United States)

Brondz, Ilia; Fialkov, Alexander B; Amirav, Aviv

2009-01-30

Malaria is one of the most widespread and deadly diseases on the planet. Every year, about 500 million new cases are diagnosed, and the annual death toll is about 3 million. Primaquine has strong antiparasitic effects against gametocytes and can therefore prevent the spread of the parasite from treated patients to mosquitoes. It is also used in radical cures and prevents relapse. Consequently, primaquine is an often-used drug. In this study the separation of unprocessed primaquine from the contaminant quinocide based on gas chromatography-mass spectrometry with supersonic molecular beam (SMB) is presented and 7.5 mg primaquine diphosphate tablets were analyzed. We present a novel method for fast determination of quinocide which is an isomer of primaquine as the main contaminant in unprocessed primaquine and in its medical form as tablets by gas chromatography-mass spectrometry with SMB (also named supersonic GC-MS). Supersonic GC-MS provides enhanced molecular ion without any ion source related peak tailing plus extended range of compounds amenable for GC-MS analysis. In addition, major isomer mass spectral effects were revealed in the mass spectra of primaquine and quinocide which facilitated the unambiguous identification of quinocide in primaquine tablets. Fast GC-MS analysis is demonstrated with less then 2 min elution time of the drug and its main contaminants.

Determination of radiochemical purity using gas chromatography

International Nuclear Information System (INIS)

1975-01-01

The concepts of chromatography, gas chromatography, activity, radiochemical impurity are defined; the procedure of the application of gas chromatography for detecting radiochemical purity of substances is standardized. (E.F.)

The leaf volatile constituents of Isatis tinctoria by Solid-Phase Microextraction and Gas chromatography/Mass Spectrometry.

Science.gov (United States)

Condurso, Cettina; Verzera, Antonella; Romeo, Vincenza; Ziino, Marisa; Trozzi, Alessandra; Ragusa, Salvatore

2006-08-01

The leaf volatile constituents of Isatis tinctoria L. (Brassicaceae) have been studied by Solid-Phase Microextraction and Gas chromatography/Mass Spectrometry (SPME/GC-MS). Seventy components were fully characterized by mass spectra, linear retention indices, and injection of standards; the average composition (ppm) as single components and classes of substances is reported. Aliphatic hydrocarbons, acids, alcohols, aldehydes and esters, aromatic aldehydes, esters and ethers, furans, isothiocyanates and thiocyanates, sulfurated compounds, nitriles, terpenes and sesquiterpenes were identified. Leaf volatiles in Isatis tinctoria L. were characterized by a high amount of isothiocyanates which accounted for about 40 % of the total volatile fraction. Isothiocyanates are important and characteristic flavour compounds in Brassica vegetables and the cancer chemo-protective attributes are recently responsible for their growing interest.

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.

Investigation of solid organic waste processing by oxidative pyrolysis

Science.gov (United States)

Kolibaba, O. B.; Sokolsky, A. I.; Gabitov, R. N.

2017-11-01

A thermal analysis of a mixture of municipal solid waste (MSW) of the average morphological composition and its individual components was carried out in order to develop ways to improve the efficiency of its utilization for energy production in thermal reactors. Experimental studies were performed on a synchronous thermal analyzer NETZSCH STA 449 F3 Jupiter combined with a quadrupole mass spectrometer QMC 403. Based on the results of the experiments, the temperature ranges of the pyrolysis process were determined as well as the rate of decrease of the mass of the sample of solid waste during the drying and oxidative pyrolysis processes, the thermal effects accompanying these processes, as well as the composition and volumes of gases produced during oxidative pyrolysis of solid waste and its components in an atmosphere with oxygen content of 1%, 5%, and 10%. On the basis of experimental data the dependences of the yield of gas on the moisture content of MSW were obtained under different pyrolysis conditions under which a gas of various calorific values was produced.

Gas chromatography/mass spectrometry analysis of very long chain fatty acids, docosahexaenoic acid, phytanic acid and plasmalogen for the screening of peroxisomal disorders

NARCIS (Netherlands)

Takemoto, Yasuhiko; Suzuki, Yasuyuki; Horibe, Ryoko; Shimozawa, Nobuyuki; Wanders, Ronald J. A.; Kondo, Naomi

2003-01-01

Very long chain fatty acids (VLCFAs) and docosahexaenoic acid (DHA), phytanic acid, and plasmalogens are usually measured individually. A novel method for the screening of peroxisomal disorders, using gas chromatography/mass spectrometry (GC/MS), was developed. Saturated and unsaturated fatty acids,

Method for manufacturing raw mass for gas concrete

Energy Technology Data Exchange (ETDEWEB)

Hellestam, C J.S.

1949-06-30

A method is described for processing a raw mass of oil shale and limestone directly useable for the production of gas concrete, characterized in that the processing is divided into three partial processes, of which the first comprises a pyrolysis with extraction of oil, shale gas, hydrogen sulfide and shale coke; the second, burning of the shale coke while preventing the fusing temperature from being exceeded; and the third partial process is a continued burning at higher temperature in the range of 1100/sup 0/C after the addition of limestone and, if required, extra fuel.

Thermogravimetric-Mass Spectrometric Study of the Pyrolysis Behavior of PVC

Institute of Scientific and Technical Information of China (English)

SUN Qing-lei; SHI Xin-gang; LIN Yun-liang; ZHU He; WANG Xiao; CHENG Chuan-ge; LIU Jian-hua

2007-01-01

The pyrolysis characteristics of PVC were systematically investigated using a Netzschne TG thermo-balance coupled to a quadrupole mass spectrometer. The pyrolysis conditions were 0.1 MPa of Ar, a heating rate of 10 ℃/min and a final temperature of 1000 ℃. Both the thermogravimetric properties and the simultaneous evolution of gaseous products during pyrolysis were studied. The TG/DTG results showed that as the pyrolysis temperature increases the weight loss and weight loss rate of PVC increases. Near 412 ℃ the weight loss rate attained its peak value. At higher temperatures the rate of loss gradually decreases. The gases evolved during thermogravimetric analysis were analyzed by a mass spectrometer, monitoring the relative intensity of HCl, C6H6, light hydrocarbon and chlorine-containing gases. The evolution curves showed that HCl, C6H6, light hydrocarbon and chlorine-containing gases all peak at about 416 ℃. This is consistent with the fact that the weight loss curves also peak at about 412 ℃. The extensive HCl evolution is consistent with the high chlorine content of PVC. The formation of these gases can be explained by considering these reactions: dehydrochlorination, intramolecular cyclization and the addition of HCl to unsaturated hydrocarbons.

Gas chromatography in space

Science.gov (United States)

Akapo, S. O.; Dimandja, J. M.; Kojiro, D. R.; Valentin, J. R.; Carle, G. C.

1999-01-01

Gas chromatography has proven to be a very useful analytical technique for in situ analysis of extraterrestrial environments as demonstrated by its successful operation on spacecraft missions to Mars and Venus. The technique is also one of the six scientific instruments aboard the Huygens probe to explore Titan's atmosphere and surface. A review of gas chromatography in previous space missions and some recent developments in the current environment of fiscal constraints and payload size limitations are presented.

Magnetic micro-solid-phase extraction based on magnetite-MCM-41 with gas chromatography-mass spectrometry for the determination of antidepressant drugs in biological fluids.

Science.gov (United States)

Kamaruzaman, Sazlinda; Sanagi, Mohd Marsin; Yahaya, Noorfatimah; Wan Ibrahim, Wan Aini; Endud, Salasiah; Wan Ibrahim, Wan Nazihah

2017-11-01

A new facile magnetic micro-solid-phase extraction coupled to gas chromatography and mass spectrometry detection was developed for the extraction and determination of selected antidepressant drugs in biological fluids using magnetite-MCM-41 as adsorbent. The synthesized sorbent was characterized by several spectroscopic techniques. The maximum extraction efficiency for extraction of 500 μg/L antidepressant drugs from aqueous solution was obtained with 15 mg of magnetite-MCM-41 at pH 12. The analyte was desorbed using 100 μL of acetonitrile prior to gas chromatography determination. This method was rapid in which the adsorption procedure was completed in 60 s. Under the optimized conditions using 15 mL of antidepressant drugs sample, the calibration curve showed good linearity in the range of 0.05-500 μg/L (r 2  = 0.996-0.999). Good limits of detection (0.008-0.010 μg/L) were obtained for the analytes with good relative standard deviations of solid-phase extraction with gas chromatography and mass spectrometry is a convenient, fast, and economical method for the extraction and determination of amitriptyline and chlorpromazine in biological samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Analysis of 62 synthetic cannabinoids by gas chromatography-mass spectrometry with photoionization.

Science.gov (United States)

Akutsu, Mamoru; Sugie, Ken-Ichi; Saito, Koichi

2017-01-01

Gas chromatography-mass spectrometry (GC-MS) in electron ionization (EI) mode is one of the most commonly used techniques for analysis of synthetic cannabinoids, because the GC-EI-MS spectra contain characteristic fragment ions for identification of a compound; however, the information on its molecular ions is frequently lacking. To obtain such molecular ion information, GC-MS in chemical ionization (CI) mode is frequently used. However, GC-CI-MS requires a relatively tedious process using reagent gas such as methane or isobutane. In this study, we show that GC-MS in photoionization (PI) mode provided molecular ions in all spectra of 62 synthetic cannabinoids, and 35 of the 62 compounds showed only the molecular radical cations. Except for the 35 compounds, the PI spectra showed very simple patterns with the molecular peak plus only a few fragment peak(s). An advantage is that the ion source for GC-PI-MS can easily be used for GC-EI-MS as well. Therefore, GC-EI/PI-MS will be a useful tool for the identification of synthetic cannabinoids contained in a dubious product. To the best of our knowledge, this is the first report to use GC-PI-MS for analysis of synthetic cannabinoids.

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.

[Determination of acetanilide herbicide residues in tea by gas chromatography-mass spectrometry with two different ionization techniques].

Science.gov (United States)

Shen, Weijian; Xu, Jinzhong; Yang, Wenquan; Shen, Chongyu; Zhao, Zengyun; Ding, Tao; Wu, Bin

2007-09-01

An analytical method of solid phase extraction-gas chromatography-mass spectrometry with two different ionization techniques was established for simultaneous determination of 12 acetanilide herbicide residues in tea-leaves. Herbicides were extracted from tea-leaf samples with ethyl acetate. The extract was cleaned-up on an active carbon SPE column connected to a Florisil SPE column. Analytical screening was determined by the technique of gas chromatography (GC)-mass spectrometry (MS) in the selected ion monitoring (SIM) mode with either electron impact ionization (EI) or negative chemical ionization (NCI). It is reliable and stable that the recoveries of all herbicides were in the range from 50% to 110% at three spiked levels, 10 microg/kg, 20 microg/kg and 40 microg/kg, and the relative standard deviations (RSDs) were no more than 10.9%. The two different ionization techniques are complementary as more ion fragmentation information can be obtained from the EI mode while more molecular ion information from the NCI mode. By comparison of the two techniques, the selectivity of NCI-SIM was much better than that of EI-SIM method. The sensitivities of the both techniques were high, the limit of quantitative (LOQ) for each herbicide was no more than 2.0 microg/kg, and the limit of detection (LOD) with NCI-SIM technique was much lower than that of EI-SIM when analyzing herbicides with several halogen atoms in the molecule.

Calibration and Data Processing in Gas Chromatography Combustion Isotope Ratio Mass Spectrometry

Science.gov (United States)

Zhang, Ying; Tobias, Herbert J.; Sacks, Gavin L.; Brenna, J. Thomas

2013-01-01

Compound-specific isotope analysis (CSIA) by gas chromatography combustion isotope ratio mass spectrometry (GCC-IRMS) is a powerful technique for the sourcing of substances, such as determination of the geographic or chemical origin of drugs and food adulteration, and it is especially invaluable as a confirmatory tool for detection of the use of synthetic steroids in competitive sport. We review here principles and practices for data processing and calibration of GCC-IRMS data with consideration to anti-doping analyses, with a focus on carbon isotopic analysis (13C/12C). After a brief review of peak definition, the isotopologue signal reduction methods of summation, curve-fitting, and linear regression are described and reviewed. Principles for isotopic calibration are considered in the context of the Δ13C = δ13CM – δ13CE difference measurements required for establishing adverse analytical findings for metabolites relative to endogenous reference compounds. Considerations for the anti-doping analyst are reviewed. PMID:22362612

Odor and odorous chemical emissions from dairy and swine facilities: Part 5-Simultaneous chemical and sensory analysis with Gas Chromatography - Mass Spectrometry - Olfactometry

Science.gov (United States)

Simultaneous chemical and sensory analyses using gas chromatography-mass spectrometry-olfactometry (GC-MS-O) for air samples collected at barn exhaust fans were used for quantification and ranking of odor impact of target odorous gases. Fifteen target odorous VOCs (odorants) were selected. Air sampl...

Fast co-pyrolysis of waste newspaper with high-density polyethylene for high yields of alcohols and hydrocarbons.

Science.gov (United States)

Chen, Weimin; Shi, Shukai; Chen, Minzhi; Zhou, Xiaoyan

2017-09-01

Waste newspaper (WP) was first co-pyrolyzed with high-density polyethylene (HDPE) using pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) to enhance the yields of alcohols and hydrocarbons. The effects of WP: HDPE feed ratio (100:0, 75:25, 50:50, 25:75, 0:100) and temperature (500-800°C) on products distribution were investigated and the interaction mechanism during co-pyrolysis was also proposed. Maximum yields of alcohols and hydrocarbons reached 85.88% (feed ratio 50:50wt.%, 600°C). Hydrogen supplements and deoxidation by HDPE and subsequently fragments recombination result in the conversion of aldehydes and ketones into branched hydrocarbons. Radicals from WP degradation favor the secondary crack for HDPE products resulting in the formation of linear hydrocarbons with low carbon number. Hydrocarbons with activated radical site from HDPE degradation were interacted with hydroxyl from WP degradation promoting the formation of linear long chain alcohols. Moreover, co-pyrolysis significantly enhanced condensable oil qualities, which were close to commercial diesel No. 0. Copyright © 2017 Elsevier Ltd. All rights reserved.

Development of a Method for Rapid Determination of Morpholine in Juices and Drugs by Gas Chromatography-Mass Spectrometry

Directory of Open Access Journals (Sweden)

Mengsi Cao

2018-01-01

Full Text Available A reliable derivatization method has been developed to detect and quantify morpholine in apple juices and ibuprofen with gas chromatography-mass spectrometry. Morpholine can react with sodium nitrite under acidic condition to produce stable and volatile N-nitrosomorpholine derivative. In this experiment, various factors affecting the derivatization and extraction process were optimized, including volume and concentration of hydrochloric acid, quantity of sodium nitrite, derivatization temperature, derivatization time, extraction reagents, and extraction time. The derivative was extracted with dichloromethane and determined by gas chromatography-mass spectrometry. The linearity range of morpholine was 10–500 μg·L−1 with good correlation, and limits of detection (LOD and limits of quantification (LOQ were 7.3 μg·L−1 and 24.4 μg·L−1, respectively. Low, medium, and high concentrations of morpholine were added in apple juices and ibuprofen samples to evaluate standard recovery rate and relative standard deviation. The spiked recovery rate ranged from 94.3% to 109.0%, and the intraday repeatability and interday reproducibility were 2.0%–4.4% and 3.3%–7.0%, respectively. The developed method has good accuracy and precision. This quantitative method for morpholine is simple, sensitive, rapid, and low cost and can successfully be applied to analyze the residual morpholine in apple juices and drug samples.

Analysis of particulate polycyclic aromatic hydrocarbons by on-line coupled supercritical fluid extraction-liquid chromatography-gas chromatography-mass spectrometry

Science.gov (United States)

Shimmo, Masahiko; Adler, Heidi; Hyötyläinen, Tuulia; Hartonen, Kari; Kulmala, Markku; Riekkola, Marja-Liisa

An on-line supercritical fluid extraction-liquid chromatography-gas chromatography-mass spectrometry (SFE-LC-GC-MS) method was developed for the analysis of the particulate polycyclic aromatic hydrocarbons (PAHs). The limits of detection of the system for the quantification standards were in the range of 0.25-0.57 ng, while the limits of determinations for filter samples varied from 0.02 to 0.04 ng m -3 (24 h sampling). The linearity was excellent from 5 to 300 ng ( R2>0.967). The analysis could be carried out in a closed system without tedious manual sample pretreatment and with no risk of errors by contamination or loss of the analytes. The results of the SFE-LC-GC-MS method were comparable with those for Soxhlet and shake-flask extractions with GC-MS. The new method was applied to the analysis of PAHs collected by high-volume filter in the Helsinki area to study the seasonal trend of the concentrations. The individual PAH concentrations varied from 0.015 to more than 1 ng m -3, while total PAH concentrations varied from 0.81 to 5.68 ng m -3. The concentrations were generally higher in winter than in summer. The mass percentage of the total PAHs in total suspended particulates ranged from 2.85×10 -3% in July to 15.0×10 -3% in December. Increased emissions in winter, meteorological conditions, and more serious artefacts during the sampling in summer season may explain the concentration profiles.

Characterization of the designer drug deschloroketamine (2-methylamino-2-phenylcyclohexanone) by gas chromatography/mass spectrometry, liquid chromatography/high-resolution mass spectrometry, multistage mass spectrometry, and nuclear magnetic resonance.

Science.gov (United States)

Frison, Giampietro; Zamengo, Luca; Zancanaro, Flavio; Tisato, Francesco; Traldi, Pietro

2016-01-15

Clinical and forensic toxicology laboratories are challenged every day by the analytical aspects of the new psychoactive substances phenomenon. In this study we describe the analytical characterization of a new ketamine derivative, deschloroketamine (2-methylamino-2-phenylcyclohexanone), contained in seized powders. The analytical techniques employed include gas chromatography/mass spectrometry (GC/MS), liquid chromatography/electrospray ionization coupled with Orbitrap high-resolution/MS (LC/ESI-HRMS), multistage MS (ESI-MS(n)), and NMR. The LC/ESI-HRMS analyses consisted of accurate mass measurements of MH(+) ions in full-scan mode; comparison of experimental and calculated MH(+) isotopic patterns; and examination of the isotopic fine structure (IFS) of the M + 1, M + 2, M + 3 isotopic peaks relative to the monoisotopic M + 0 peak. The collision-induced product ions of the MH(+) ions were studied by both HRMS and MS(n). (1)H and (13)C NMR measurements were carried out to confirm the chemical structure of the analyte. The EI mass spectra obtained by GC/MS analysis showed the presence of molecular ions at m/z 203, and main fragment ions at m/z 175, 174, 160, 147, 146, and 132. The application of LC/ESI-HRMS allowed us to obtain: the accurate mass of deschloroketamine MH(+) ions with a mass accuracy of 1.47 ppm; fully superimposable experimental and calculated MH(+) isotopic patterns, with a relative isotopic abundance value of 3.69 %; and the IFS of the M + 1, M + 2, M + 3 isotopic peaks completely in accordance with theoretical values. Examination of the product ions of MH(+), as well as the study of both (1)H and (13)C NMR spectra, enabled the full characterization of the molecular structure of deschloroketamine. The combination of the employed analytical techniques allowed the characterization of the seized psychoactive substance, in spite of the lack of a reference standard. Deschloroketamine is a ketamine analogue considered to be

Effect of catalyst contact mode and gas atmosphere during catalytic pyrolysis of waste plastics

International Nuclear Information System (INIS)

Xue, Yuan; Johnston, Patrick; Bai, Xianglan

2017-01-01

Highlights: • PE, PP, PS and PET were catalytically pyrolyzed in a tandem micro-pyrolyzer. • Product distribution and composition were varied at in-situ and ex-situ pyrolysis. • Hydrogen carrier gas suppressed coke formation and reduced polyaromatic content. • Positive synergies between PE and PS, or PE and PET were found. - Abstract: In the present study, polyethylene (PE), polypropylene (PP), polystyrene (PS) and polyethylene terephthalate (PET) were pyrolyzed using HZSM-5 zeolite in a tandem micro-pyrolyzer to investigate the effects of plastic type, catalyst and feedstock contact mode, as well as the type of carrier gas on product distribution. Among the four plastics, PS produced highest aromatic yields up to 85% whereas PE and PP mainly produced aliphatic hydrocarbons. In comparison to ex-situ pyrolysis, in-situ pyrolysis of the plastics produced more solid residue but also promoted the formation of aromatic hydrocarbons, except PS. For PS, ex-situ pyrolysis produced a higher yield of aromatics than in-situ pyrolysis, mostly contributed by high styrene yield. During in-situ pyrolysis, the catalyst reduced the decomposition temperatures of the plastics in the order of PE, PP, PS and PET from high to low. Hydrogen carrier gas reduced solid residue and also increased the selectivity of single ring aromatics in comparison to inert pyrolysis. Hydrogen was more beneficial to PS and PET than PE and PP in terms of reducing coke yield and increasing hydrocarbon yield. The present study also showed that catalytically co-pyrolyzing PS and PE, or PET and PE increases the yield of aromatics and reduces the yield of solid residue due to hydrogen transfer from PE to PS or PET and alkylation reactions among the plastic-derivatives.

Genetic and Quantitative Trait Locus Analysis for Bio-Oil Compounds after Fast Pyrolysis in Maize Cobs.

Directory of Open Access Journals (Sweden)

Brandon Jeffrey

Full Text Available Fast pyrolysis has been identified as one of the biorenewable conversion platforms that could be a part of an alternative energy future, but it has not yet received the same attention as cellulosic ethanol in the analysis of genetic inheritance within potential feedstocks such as maize. Ten bio-oil compounds were measured via pyrolysis/gas chromatography-mass spectrometry (Py/GC-MS in maize cobs. 184 recombinant inbred lines (RILs of the intermated B73 x Mo17 (IBM Syn4 population were analyzed in two environments, using 1339 markers, for quantitative trait locus (QTL mapping. QTL mapping was performed using composite interval mapping with significance thresholds established by 1000 permutations at α = 0.05. 50 QTL were found in total across those ten traits with R2 values ranging from 1.7 to 5.8%, indicating a complex quantitative inheritance of these traits.

Upgrading pine sawdust pyrolysis oil to green biofuels by HDO over zinc-assisted Pd/C catalyst

International Nuclear Information System (INIS)

Huang, Yinbin; Wei, Lin; Zhao, Xianhui; Cheng, Shouyun; Julson, James; Cao, Yuhe; Gu, Zhengrong

2016-01-01

Highlights: • The Pd/Zn synergistic catalysis was employed. • The true pyrolysis oil as substrate was used in HDO. • The products (gas and liquid) were analyzed. • The optimal reaction conditions were obtained. - Abstract: Upgrading pyrolysis oil by hydrodeoxygenation (HDO) is a promising route for the production of advanced biofuels. The proper reaction conditions and catalysts are important for the success of this process. Previously our research group investigated the ratio of Zn and Pd on the synergistic effect for HDO bio-oil upgrading. This present research focuses on determining the optimal reaction conditions for HDO conversion of pyrolysis oil produced from pine sawdust. Temperatures of 150, 200 and 250 °C and hydrogen pressures of 1.38, 2.76 and 4.14 MPa were evaluated. Syngas, liquids and coke were the primary products evaluated. Syngas was characterized using a Gas chromatography (GC). The liquids were characterized using a Gas chromatography–mass spectrometry (GC–MS). Increasing reaction temperature resulted in increased coke yields. Treatment at 250 °C and 1.38 MPa resulted in the highest hydrocarbon content (6.06%). The treatment at 200 °C and 1.38 MPa produced the largest amounts of hydrocarbons in C_6–C_1_2 range (5.07%). The physicochemical characterizations further support the GCMS results. Syngas analysis revealed that higher hydrogen pressure leads to increased hydrogen consumption and results in more oxy-compounds conversion to hydrocarbons. The syngas analysis also supports the liquid analysis result.

Radiogas chromatography mass spectrometry in the selected ion monitoring mode

International Nuclear Information System (INIS)

Doerfler, D.L.; Rosenblum, E.R.; Malloy, J.M.; Naworal, J.D.; McManus, I.R.; Campbell, I.M.

1980-01-01

The value of selected ion monitoring in analyzing biological radio isotope incorporation experiments by radiogas chromatography mass spectrometry is illustrated with reference to the biosynthesis of the mycotoxin mycophenolic acid in Penicillium brevicompactum and the mode of action of the anticholesterolemic drug 20,25-diazacholesterol. Both examples used 1-[ 14 C]acetate precursors. It is shown that the increased sensitivity and specificity of the selected ion monitoring mode detector permits straightforward detection and identification of the relatively small cellular pools associated with metabolic intermediates. The computer program RADSIM is described. Problems that still exist in using radiogas gas chromatography mass spectrometry technology to analyse isotope incorporation experiments are discussed. (author)

Quantification of short- and medium-chain chlorinated paraffins in environmental samples by gas chromatography quadrupole time-of-flight mass spectrometry.

Science.gov (United States)

Gao, Wei; Wu, Jing; Wang, Yawei; Jiang, Guibin

2016-06-24

Chlorinated paraffins (CPs) are technical products produced and used in bulk for a number of purposes. However, the analysis of CPs is challenging, as they are complex mixtures of compounds and isomers. We herein report the development of an analytical method for the analysis of short-chain CPs (SCCPs) and medium-chain CPs (MCCPs) using quadrupole time-of-flight high-resolution mass spectrometry (GC-NCI-qTOF-HRMS). This method employs gas chromatography with a chemical ionization source working in negative mode. The linear relationship between chlorination and the CP total response factors was applied to quantify the CP content and the congener group distribution patterns. In a single injection, 24 SCCP formula groups and 24 MCCP formula groups were quantified. Extraction of accurate masses using qTOF-HRMS allowed the SCCPs and MCCPs to be distinguished, with interference from other chemicals (e.g., PCBs) being largely avoided. The SCCP and MCCP detection limits were 24-81ng/mL and 27-170ng/mL, respectively. Comparison of the obtained results with analytical results from gas chromatography coupled with electron capture negative ionization low-resolution mass spectrometry (GC-ECNI-LRMS) indicate that the developed technique is a more accurate and convenient method for the analysis of CPs in samples from a range of matrices. Copyright © 2016 Elsevier B.V. All rights reserved.

Isotope-dilution gas chromatography-mass spectrometry method for the analysis of hydroxyurea.

Science.gov (United States)

Garg, Uttam; Scott, David; Frazee, Clint; Kearns, Gregory; Neville, Kathleen

2015-06-01

Hydroxyurea is used in the treatment of various malignancies and sickle cell disease. There are limited studies on the pharmacokinetics of hydroxyurea, particularly in pediatric patients. An accurate, precise, and sensitive method is needed to support such studies and to monitor therapeutic adherence. We describe a novel gas chromatography-mass spectrometry (GC-MS) method for the determination of hydroxyurea concentration in plasma using stable labeled hydroxyurea C N2 as an internal standard. The method involved an organic extraction followed by the preparation of trimethylsilyl (TMS) derivatives of hydroxyurea for GC-MS selected ion-monitoring analysis. The following mass-to-charge (m/z) ratio ions for silated hydroxyurea and hydroxyurea C N2 were monitored: hydroxyurea-quantitative ion 277, qualifier ions 292 and 249; hydroxyurea C N2-quantitative ion 280, qualifier ion 295. This method was evaluated for reportable range, accuracy, within-run and between-run imprecisions, and limits of quantification. The reportable range for the method was 0.1-100 mcg/mL. All results were accurate within an allowable error of 15%. Within-run and between-run imprecisions were hydroxyurea described here is accurate, sensitive, precise, and robust. Its characteristics make the method suitable for supporting pharmacokinetic studies and/or clinical therapeutic monitoring.

Liquid and gas chromatography coupled to isotope ratio mass spectrometry for the determination of 13C-valine isotopic ratios in complex biological samples

NARCIS (Netherlands)

Godin, Jean-Philippe; Breuillé, Denis; Obled, Christiane; Papet, Isabelle; Schierbeek, Henk; Hopfgartner, Gérard; Fay, Laurent-Bernard

2008-01-01

On-line gas chromatography-combustion-isotope ratio mass spectrometry (GC-C-IRMS) is commonly used to measure isotopic ratios at natural abundance as well as for tracer studies in nutritional and medical research. However, high-precision (13)C isotopic enrichment can also be measured by liquid

Quantification of plasma myo-inositol using gas chromatography-mass spectrometry.

Science.gov (United States)

Guo, Jin; Shi, Yingfei; Xu, Chengbao; Zhong, Rugang; Zhang, Feng; Zhang, Ting; Niu, Bo; Wang, Jianhua

2016-09-01

Myo-inositol (MI) deficiency is associated with an increased risk for neural tube defects (NTDs), mental disorders and metabolic diseases. We developed a gas chromatography-mass spectrometry (GC-MS) method to detect MI in human plasma, which was accurate, relatively efficient and convenient for clinical application. An external standard method was used for determination of plasma MI. Samples were analyzed by GC-MS after derivatization. The stable-isotope labeled internal standard approach was used to validate the method's accuracy. Alpha fetal protein (AFP) was detected by chemiluminescence immunoassay. The method was validated by determining the linearity, sensitivity and recovery rate. There was a good agreement between the internal standard approach and the present method. The NTD-affected pregnancies showed lower plasma MI (P=0.024) and higher AFP levels (P=0.001) than control. Maternal MI level showed a better discrimination in spina bifida subgroup, while AFP level showed a better discrimination in anencephaly subgroup after stratification analysis. We developed a sensitive and reliable method for the detection of clinical plasma MI, which might be a marker for NTDs screening, and established fundamental knowledge for clinical diagnosis and prevention for the diseases related to disturbed MI metabolism. Copyright © 2016 Elsevier B.V. All rights reserved.

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

[Determination of naphthenic acids in distillates of crude oil by gas chromatography/chemical ionization-mass spectrometry].

Science.gov (United States)

Lü, Zhenbo; Tian, Songbai; Zhai, Yuchun; Sun, Yanwei; Zhuang, Lihong

2004-05-01

The petroleum carboxylic acids in 200-420 degrees C distillate of crude oil were separated by the extraction with column chromatography on an anion exchange resin. The effect of the composition and structure of naphthenic acids on separation were studied by the infra-red (IR) spectroscopic techniques. Naphthenic acids and iso-butane reagent gas were introduced into the ion source for chemical ionization, in which the ions represented by [M + C4H9]+ were used to calculate the relative molecular mass for each acid. Based on the mass spectra of pure fatty and naphthenic acids, in combination with the z-series formula CnH(2n + z)O2, the naphthenic acids can be classified into fatty, mono-, bi- ... hexa-cyclic types. The results indicated that the relative molecular mass range of naphthenic acids in this distillates was 170-510, and the carbon number range was C10-C35. The contents of bi-cyclic and tri-cyclic naphthenic acids were higher than others.

DETERMINATION OF A BOUND MUSK XYLENE METABOLITE IN CARP HEMOGLOBIN AS A BIOMARKER OF EXPOSURE BY GAS CHROMATOGRAPHY MASS SPECTROMETRY USING SELECTED ION MONITORING

Science.gov (United States)

Musk xylene (MX) is widely used as a fragrance ingredient in commercial toiletries. Identification and quantification of a bound 4-amino-MX (AMX) metabolite was carried out by gas chromatography-mass spectrometry (GC/MS), with selected ion monitoring (SIM). Detection of AMX occur...

Application of gas chromatography in hydrogen isotope separation

International Nuclear Information System (INIS)

Ye Xiaoqiu; Sang Ge; Peng Lixia; Xue Yan; Cao Wei

2008-01-01

The principle of gas chromatographic separation of hydrogen isotopes was briefly introduced. The main technology and their development of separating hydrogen isotopes, including elution chromatography, hydrogen-displacement chromatography, self-displacement chromatography and frontal chromatography were discussed in detail. The prospect of hydrogen isotope separation by gas chromatography was presented. (authors)

The effect of pyrolysis temperature of palm oil shell on quantity and quality of liquid smoke

International Nuclear Information System (INIS)

Ratnawati; Singgih Hartanto

2010-01-01

Palm oil shell can be processed into carbon and liquid smoke through pyrolysis reaction where liquid smoke was obtained by condensation of smoke produced. In this research, liquid smoke was produced by pyrolysis of 5 kg palm oil shell at temperature of 200 °C, 300 °C, and 400 °C for 4 hours and the composition of liquid smoke was analyzed with Gas Chromatography -Mass Spectrometry (GC-MS). The pyrolysis processes at 200°C, 300 °C, and 400 °C produced 460 mL, 510 mL, and 550 mL of liquid smoke and 3.98, 3.24 and 1.49 kg of carbon respectively. The result of liquid smoke with pyrolysis process at 200 °C were 30.73 %(w/w) of antioxidant and food flavor component (guaiacol, 2,3 - butanedione, furfural and 2-methyl-2-cyclopentanone), and 34.31 %(w/w) of harmful components (phenol , 2-propanone, 2-butanone and cyclopentanone). At 400 °C, 27.39 %(w/w) of components can be used in food products and 26.51 %(w/w) of components was harmful for health. Liquid smoke produced from this experiment cannot yet be used as food preservative because it still contains harmful components which are dangerous for health, therefore it needs further separation. (author)

Pyrolysis of propane under vacuum carburizing conditions. An experimental and modeling study

Energy Technology Data Exchange (ETDEWEB)

Khan, R.U.; Bajohr, S.; Buchholz, D.; Reimert, R. [Engler-Bunte-Institut, Bereich Gas, Erdoel und Kohle, Engler Bunte Ring 1, Universitaet Karlsruhe, 76131 Karlsruhe (Germany); Minh, H.D.; Norinaga, K.; Janardhanan, V.M.; Tischer, S.; Deutschmann, O. [Institute of Chemical Technology, University of Karlsruhe, 76128 Karlsruhe (Germany)

2008-03-15

Propane has been pyrolyzed in a flow reactor system at different temperatures ranging from 640 C to 1010 C and at 8 mbar of partial pressure which are typical vacuum carburizing conditions for steel. Nitrogen was used as a carrier gas. The products of pyrolysis were collected and analyzed by gas chromatography. The reactor was numerically simulated by 1D and 2D flow models coupled to a detailed gas phase reaction mechanism. The gas atmosphere composition has been predicted under the conditions of vacuum carburizing of steel. (author)

Comprehensive two-dimensional gas chromatography/time-of-flight mass spectrometry peak sorting algorithm.

Science.gov (United States)

Oh, Cheolhwan; Huang, Xiaodong; Regnier, Fred E; Buck, Charles; Zhang, Xiang

2008-02-01

We report a novel peak sorting method for the two-dimensional gas chromatography/time-of-flight mass spectrometry (GC x GC/TOF-MS) system. The objective of peak sorting is to recognize peaks from the same metabolite occurring in different samples from thousands of peaks detected in the analytical procedure. The developed algorithm is based on the fact that the chromatographic peaks for a given analyte have similar retention times in all of the chromatograms. Raw instrument data are first processed by ChromaTOF (Leco) software to provide the peak tables. Our algorithm achieves peak sorting by utilizing the first- and second-dimension retention times in the peak tables and the mass spectra generated during the process of electron impact ionization. The algorithm searches the peak tables for the peaks generated by the same type of metabolite using several search criteria. Our software also includes options to eliminate non-target peaks from the sorting results, e.g., peaks of contaminants. The developed software package has been tested using a mixture of standard metabolites and another mixture of standard metabolites spiked into human serum. Manual validation demonstrates high accuracy of peak sorting with this algorithm.

Evaluating the effect of potassium on cellulose pyrolysis reaction kinetics

International Nuclear Information System (INIS)

Trendewicz, Anna; Evans, Robert; Dutta, Abhijit; Sykes, Robert; Carpenter, Daniel; Braun, Robert

2015-01-01

This paper proposes modifications to an existing cellulose pyrolysis mechanism in order to include the effect of potassium on product yields and composition. The changes in activation energies and pre-exponential factors due to potassium were evaluated based on the experimental data collected from pyrolysis of cellulose samples treated with different levels of potassium (0–1% mass fraction). The experiments were performed in a pyrolysis reactor coupled to a molecular beam mass spectrometer (MBMS). Principal component analysis (PCA) performed on the collected data revealed that cellulose pyrolysis products could be divided into two groups: anhydrosugars and other fragmentation products (hydroxyacetaldehyde, 5-hydroxymethylfurfural, acetyl compounds). Multivariate curve resolution (MCR) was used to extract the time resolved concentration score profiles of principal components. Kinetic tests revealed that potassium apparently inhibits the formation of anhydrosugars and catalyzes char formation. Therefore, the oil yield predicted at 500 ° C decreased from 87.9% from cellulose to 54.0% from cellulose with 0.5% mass fraction potassium treatment. The decrease in oil yield was accompanied by increased yield of char and gases produced via a catalyzed dehydration reaction. The predicted char and gas yield from cellulose were 3.7% and 8.4%, respectively. Introducing 0.5% mass fraction potassium treatment resulted in an increase of char yield to 12.1% and gas yield to 33.9%. The validation of the cellulose pyrolysis mechanism with experimental data from a fluidized-bed reactor, after this correction for potassium, showed good agreement with our results, with differences in product yields of up to 5%

Extractive alkylation of 6-mercaptopurine and determination in plasma by gas chromatography-mass spectrometry.

Science.gov (United States)

Floberg, S; Hartvig, P; Lindström, B; Lönner-Holm, G; Odlind, B

1981-09-11

An analytical procedure was developed for the determination of 6-mercaptopurine in plasma. Owing to the polar character and low plasma concentration of the compound, extraction and derivatization was carried out directly from the plasma sample by extractive alkylation. Determination was made using gas chromatography-mass spectrometry with multiple-ion detection. Conditions with respect to the rate of formation and the stability of the derivative formed in the extractive alkylation step were evaluated. The selectively of the method to azathioprine and to metabolites was thoroughly investigated. No 6-mercaptopurine was formed from azathioprine added to water or plasma and run through the method. The method enables the detection of 2 ng of 6 mercaptopurine in a 1.0-ml plasma sample. Quantitative determinations were done down to 10 ng/ml 6 mercaptopurine in plasma.

Chromatography mass spectrometry and its use in identification in the radiolysis products of polycyclic aromatic hydrocarbons and organic compounds

International Nuclear Information System (INIS)

Ibadov, N.A.; Suleymanov, B.A.

2010-01-01

Full text : Increased attention to the environment is the result of dramatically increased human activity, which in turn is caused by the rapid growth of population of the planet. Extremely powerful tool for control of pollution of different environmental objects - Chromatographic methods to analyze complex mixtures of components. This work is devoted to methods of gas chromatography - mass - spectroscopy and its use in identifying the pollutants of natural environments. Devices that allow obtaining the mass spectra are called mass spectrometers. Sensitivity of gas chromatography-mass spectrometry (typically 10-6-10-9 g) determined by the sensitivity of the mass spectrometer detector. Its essence lies in the fact that the recording of chromatograms is not the full ion current and the most characteristic ions of the substance. With varying degrees of probability in the water identified over 100 individual organic compounds, including PHs. The method of gas chromatography-mass spectrometry identified compounds in natural waters, soils, soil and sediments.

Mass Spectrometry Parameters Optimization for the 46 Multiclass Pesticides Determination in Strawberries with Gas Chromatography Ion-Trap Tandem Mass Spectrometry

Science.gov (United States)

Fernandes, Virgínia C.; Vera, Jose L.; Domingues, Valentina F.; Silva, Luís M. S.; Mateus, Nuno; Delerue-Matos, Cristina

2012-12-01

Multiclass analysis method was optimized in order to analyze pesticides traces by gas chromatography with ion-trap and tandem mass spectrometry (GC-MS/MS). The influence of some analytical parameters on pesticide signal response was explored. Five ion trap mass spectrometry (IT-MS) operating parameters, including isolation time (IT), excitation voltage (EV), excitation time (ET), maximum excitation energy or " q" value (q), and isolation mass window (IMW) were numerically tested in order to maximize the instrument analytical signal response. For this, multiple linear regression was used in data analysis to evaluate the influence of the five parameters on the analytical response in the ion trap mass spectrometer and to predict its response. The assessment of the five parameters based on the regression equations substantially increased the sensitivity of IT-MS/MS in the MS/MS mode. The results obtained show that for most of the pesticides, these parameters have a strong influence on both signal response and detection limit. Using the optimized method, a multiclass pesticide analysis was performed for 46 pesticides in a strawberry matrix. Levels higher than the limit established for strawberries by the European Union were found in some samples.

Trends in the analysis of natural gas by capillary gas chromatography

NARCIS (Netherlands)

Cramers, C.A.M.G.; Rossum, van G.J.

1986-01-01

The importance of correct determination of physical and chemical properties of natural gas is evident. The calculation of calorific value or hydrocarbon dew point requires detailed analysis as can be provided by gas chromatography. Analysis by gas chromatography is a necessary complement to direct

Effect of pyrolysis temperature on the composition of the oils obtained from sewage sludge

International Nuclear Information System (INIS)

Sanchez, M.E.; Menendez, J.A.; Dominguez, A.; Pis, J.J.; Martinez, O.; Calvo, L.F.; Bernad, P.L.

2009-01-01

Sewage sludge was pyrolysed in a quartz reactor at 350, 450, 550 and 950 o C. The pyrolysis oils from the sewage sludge were characterized in detail by means of gas chromatography-mass spectrometry (GC-MS). Changes in the composition of the oils related to the process conditions were assessed by normalizing the areas of the peaks. It was demonstrated that, as the temperature of pyrolysis increased from 350 to 950 o C, the concentration of mono-aromatic hydrocarbons in the oils also increased. Conversely, phenol and its alkyl derivatives showed a strong decrease in their concentration as temperature rose. Polycyclic aromatic hydrocarbons (PAHs) with two to three rings passed through a maximum at a pyrolysis temperature of 450 o C. PAHs with 4-5 rings also presented a major increase as temperature increased up to 450 o C, the concentration at 950 o C being slightly higher than that at 450 o C. Quantification of the main compounds showed that sewage sludge pyrolysis oils contain significant quantities of potentially high-value hydrocarbons such as mono-aromatic hydrocarbons and phenolic compounds. The oils also contain substantial concentrations of PAHs, even at the lowest temperature of 350 o C. The pathway to PAH formation is believed to be via the Diels-Alder reaction and also via secondary reactions of oxygenated compounds such as phenols.

Gas chromatography--inductively coupled plasma--time-of-flight mass spectrometry for the speciation analysis of organolead compounds in environmental water samples.

Science.gov (United States)

Heisterkamp, M; Adams, F C

2001-07-01

The application of inductively coupled plasma--time-of-flight mass spectrometry for the speciation analysis of organolead compounds in environmental waters is described. Construction of the transfer line was achieved by means of a relatively simple and rapid coupling procedure. Derivatization of the ionic lead species was achieved by in-situ propylation with sodium tetrapropylborate; simultaneous extraction of the derivatized compounds in hexane was followed by separation and detection by capillary gas chromatography hyphenated to inductively coupled plasma-time-of-flight mass spectrometry. Detection limits for the different organolead species ranged from 10 to 15 fg (as Pb), corresponding to procedural detection limits between 50 and 75 ng L(-1), on the basis of a 50 mL snow sample, extraction with 200 microL hexane, and subsequent injection of 1 microL of the organic extract on to the column. The accuracy of the system was confirmed by additional analysis of the water samples by capillary gas chromatography coupled with microwave-induced plasma-atomic-emission spectrometry and the analysis of a standard reference material CRM 605 (road dust) with a certified content of trimethyllead.

Aliphatic Hydrocarbons from Lignocellulose by Pyrolysis over Cesium-Modified Amorphous Silica Alumina Catalysts

NARCIS (Netherlands)

Zabeti, M.; Sai Sankar Gupta, Karthick Babu; Raman, G.; Lefferts, Leon; Schallmoser, Stefan; Lercher, Johannes A.; Seshan, K.

2015-01-01

Cesium-modified amorphous silica alumina (Cs/ASA) is a promising catalyst for the production of hydrocarbons through pyrolysis of biomass. Catalytic pyrolysis of pinewood over Cs/ASA in a pyrolyzer system in conjunction with a gas chromatograph and mass spectrometer resulted in a 22% yield of

Pyrolysis responses of kevlar/epoxy composite materials on laser irradiating

Science.gov (United States)

Liu, Wei-ping; Wei, Cheng-hua; Zhou, Meng-lian; Ma, Zhi-liang; Song, Ming-ying; Wu, Li-xiong

2017-05-01

The pyrolysis responses of kevlar/epoxy composite materials are valuable to study in a case of high temperature rising rate for its widely application. Distinguishing from the Thermal Gravimetric Analysis method, an apparatus is built to research the pyrolysis responses of kevlar/epoxy composite materials irradiated by laser in order to offer a high temperature rising rate of the sample. By deploying the apparatus, a near real-time gas pressure response can be obtained. The sample mass is weighted before laser irradiating and after an experiment finished. Then, the gas products molecular weight and the sample mass loss evolution are derived. It is found that the pressure and mass of the gas products increase with the laser power if it is less than 240W, while the molecular weight varies inversely. The variation tendency is confusing while the laser power is bigger than 240W. It needs more deeper investigations to bring it to light.

Simultaneous determination of zearalenone and its derivatives in edible vegetable oil by gel permeation chromatography and gas chromatography-triple quadrupole mass spectrometry.

Science.gov (United States)

Qian, Mingrong; Zhang, Hu; Wu, Liqin; Jin, Nuo; Wang, Jianmei; Jiang, Kezhi

2015-01-01

A sensitive gas chromatographic-triple quadrupole mass spectrometric (GC-QqQ MS) analytical method, for the determination of zearalenone and its five derivatives in edible vegetable oil, was developed. After the vegetable oil samples were prepared using gel permeation chromatography, the eluent was collected, evaporated and dried with nitrogen gas. The residue was silylated with N,O-bis-trimethylsilyltrifluoroacetamide, containing 1% trimethylchlorosilane. GC-QqQ MS was performed in the reaction-monitoring mode to confirm and quantify mycotoxins in vegetable oil. The limits of quantitation were 0.03-0.2 μg kg(-1) for the six mycotoxins. The average recoveries, measured at 2, 20 and 200 μg kg(-1), were in the range 80.3-96.5%. Zearalenone was detected in the range 5.2-184.6 μg kg(-1) in nine maize oils and at 40.7 μg kg(-1) in a rapeseed oil from the local market. Copyright © 2014 Elsevier Ltd. All rights reserved.

Reinforcement of the bio-gas conversion from pyrolysis of wheat straw by hot caustic pre-extraction.

Science.gov (United States)

Zhang, Lilong; Chen, Keli; He, Liang; Peng, Lincai

2018-01-01

Pyrolysis has attracted growing interest as a versatile means to convert biomass into valuable products. Wheat straw has been considered to be a promising biomass resource due to its low price and easy availability. However, most of the products obtained from wheat straw pyrolysis are usually of low quality. Hot soda extraction has the advantage of selective dissolution of lignin whilst retaining the carbohydrates. This can selectively convert biomass into high-quality desired products and suppress the formation of undesirable products. The aim of this study was to investigate the pyrolysis properties of wheat straw under different hot caustic pretreatment conditions. Compared with the untreated straw, a greater amount of gas was released and fewer residues were retained in the extracted wheat straw, which was caused by an increase in porosity. When the NaOH loading was 14%, the average pore size of the extracted straw increased by 12% and the cumulative pore volume increased by 157% compared with the untreated straw. The extracted straw obtained from the 14% NaOH extraction was clearly selective for pyrolysis products. On one hand, many lignin pyrolysis products disappeared, and only four main lignin-unit-pyrolysis products were retained. On the other hand, polysaccharide pyrolysis products were enriched. Both propanone and furfural have outstanding peak intensities that could account for approximately 30% of the total pyrolysis products. However, with the excessive addition of NaOH (i.e. > 22% w/w) during pretreatment, the conversion of bio-gas products decreased. Thermogravimetric and low-temperature nitrogen-adsorption analysis showed that the pore structure had been seriously destroyed, leading to the closing of the release paths of the bio-gas and thus increasing the re-polymerisation of small bio-gas molecules. After suitable extraction (14% NaOH loading extraction), a considerable amount (25%) of the soluble components dissolved out of the straw. This

Diagnosis of propionic acidemia by gas chromatography coupled to mass spectrometry in a case analysis

International Nuclear Information System (INIS)

Camayd Viera, Ivette; Robaina Jimenez, Zoe; Contreras Roura, Jiovanna

2011-01-01

Propionic acidemia is an inherited metabolic disease caused by a deficiency in the propionyl-CoA carboxilase, a biotin-dependent mitochondrial enzyme. The disorder is a clinically heterogeneous disease and one of the most frequently occurring organic acidurias. We report the first Cuban case with a severe form of propionic acidemia followed by acidosis and death. The diagnosis was carried out by gas chromatography coupled to mass spectrometry. Our aim is to highlight the importance of organic acids urine analysis as part of the first laboratory tests in undiagnosed seriously ill children. The definitive diagnosis is important as it serves as a clear guideline to establish a suitable treatment and allows geneticists to provide patients with a proper genetic counseling

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.

Green tide to green fuels: TG–FTIR analysis and kinetic study of Ulva prolifera pyrolysis

International Nuclear Information System (INIS)

Ceylan, Selim; Goldfarb, Jillian L.

2015-01-01

Highlights: • Distributed Activation Energy Model applied to Ulva prolifera pyrolysis. • Model and experimental data in good agreement to predict activation energy. • Ulva prolifera shows relatively low activation energy compared to other macroalgae. • Evolved gas analysis shows CO 2 emission decreasing with temperature. • Methane evolution increases with temperature, peaks at 800 °C. - Abstract: The world grapples with identifying renewable replacements for fossil fuels. Ulva prolifera, a macroalgae species that has caused green tides in China and Europe, represents a possible source of renewable energy. Given its low lipid content, thermochemical conversion techniques such as pyrolysis may be more suitable than biochemical techniques. We apply the Distributed Activation Energy Model to determine the activation energy of pyrolysis of U. prolifera from thermogravimetric data with combined evolved gas analysis via FTIR. Correlation coefficients for the DAEM were greater than 0.98 at each conversion; the apparent activation energy ranged from 130 to 152 kJ/mol, in good accord with the literature. Three stages of decomposition were noted over the entire temperature range; below 110 °C mass loss due to moisture removal. The largest stage of pyrolysis occurred between 190 and 400 °C with peak mass loss conversion rates up to 8.1 wt% per minute at 20 °C/min. The concentration of CO 2 in the evolved gas peaked along with mass loss rate at 242.7 °C. Stage III of pyrolysis saw a slow mass loss rate and a significant amount of methane from the macroalgae. Given its low energy, nutrient, land and maintenance requirements to grow, tolerance to a variety of environmental conditions, and low pyrolysis activation energies (as compared to other macroalgae), thermochemical conversion via pyrolysis is a viable way to extract energy from this seaweed species

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.

Tissue-specific metabolite profiling of Cyperus rotundus L. rhizomes and (+)-nootkatone quantitation by laser microdissection, ultra-high-performance liquid chromatography-quadrupole time-of-flight mass spectrometry, and gas chromatography-mass spectrometry techniques.

Science.gov (United States)

Jaiswal, Yogini; Liang, Zhitao; Guo, Ping; Ho, Hing-Man; Chen, Hubiao; Zhao, Zhongzhen

2014-07-23

Cyperus rotundus L. is a plant species commonly found in both India and China. The caused destruction of this plant is of critical concern for agricultural produce. Nevertheless, it can serve as a potential source of the commercially important sesquiterpenoid (+)-nootkatone. The present work describes comparative metabolite profiling and (+)-nootkatone content determination in rhizome samples collected from these two countries. Laser dissected tissues, namely, the cortex, hypodermal fiber bundles, endodermis, amphivasal vascular bundles, and whole rhizomes were analyzed by ultra-high-performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UHPLC-QTOF MS). Gas chromatography-mass spectrometry (GC-MS) analysis was used for profiling of essential oil constituents and quantitation of (+)-nootkatone. The content of (+)-nootkatone was found to be higher in samples from India (30.47 μg/10 g) compared to samples from China (21.72 μg/10 g). The method was validated as per International Conference on Harmonisation (ICH) guidelines (Q2 R1). The results from this study can be applied for quality control and efficient utilization of this terpenoid-rich plant for several applications in food-based industries.

Pyrolysis of biomass briquettes, modelling and experimental verification

NARCIS (Netherlands)

van der Aa, B; Lammers, G; Beenackers, AACM; Kopetz, H; Weber, T; Palz, W; Chartier, P; Ferrero, GL

1998-01-01

Carbonisation of biomass briquettes was studied using a dedicated single briquette carbonisation reactor. The reactor enabled continuous measurement of the briquette mass and continuous measurement of the radial temperature profile in the briquette. Furthermore pyrolysis gas production and

Analysis of pollutants in air and water using gas chromatography and headspace gas chromatography

Energy Technology Data Exchange (ETDEWEB)

Stenner, H.

1980-01-01

The combination 'personal sampling' with headspace gas chromatography to determine traces of formaldehyde, phenol and benzene in air is investigated in this work, with the aim of developing maximum workplace concentration values (MWL values). Further possible applications of gas chromatography in trace analysis in the environmentally protected area. The analysis of chromium in waste waters (Cr III as acetyl acetonate complex) is investigated as further possible application, whereby optimum conditions are obtained. A modified flame ionization detector was used to increase the detection sensitivity.

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

Gas chromatography-mass spectrometry evidence for several endogenous auxins in pea seedling organs.

Science.gov (United States)

Schneider, E A; Kazakoff, C W; Wightman, F

1985-08-01

Qualitative analysis by gas chromatography-mass spectrometry (GC-MS) of the auxins present in the root, cotyledons and epicotyl of 3-dold etiolated pea (Pisum sativum L., cv. Alaska) seedlings has shown that all three organs contain phenylacetic acid (PAA), 3-indoleacetic acid (IAA) and 4-chloro-3-indoleacetic acid (4Cl-IAA). In addition, 3-indolepropionic acid (IPA) was present in the root and 3-indolebutyric acid (IBA) was detected in both root and epicotyl. Phenylacetic acid, IAA and IPA were measured quantitatively in the three organs by GC-MS-single ion monitoring, using deuterated internal standards. Levels of IAA were found to range from 13 to 115 pmol g(-1) FW, while amounts of PAA were considerably higher (347-451 pmol g(-1) FW) and the level of IPA was quite low (5 pmol g(-1) FW). On a molar basis the PAA:IAA ratio in the whole seedling was approx. 15:1.

Effects of Non-Equilibrium Chemistry and Darcy-Forchheimer Flow of Pyrolysis Gas for a Charring Ablator

Science.gov (United States)

Chen, Yih-Kanq; Milos, Frank S.

2011-01-01

The Fully Implicit Ablation and Thermal Response code, FIAT, simulates pyrolysis and ablation of thermal protection materials and systems. The governing equations, which include energy conservation, a three-component decomposition model, and a surface energy balance, are solved with a moving grid. This work describes new modeling capabilities that are added to a special version of FIAT. These capabilities include a time-dependent pyrolysis gas flow momentum equation with Darcy-Forchheimer terms and pyrolysis gas species conservation equations with finite-rate homogeneous chemical reactions. The total energy conservation equation is also enhanced for consistency with these new additions. Parametric studies are performed using this enhanced version of FIAT. Two groups of analyses of Phenolic Impregnated Carbon Ablator (PICA) are presented. In the first group, an Orion flight environment for a proposed Lunar-return trajectory is considered. In the second group, various test conditions for arcjet models are examined. The central focus of these parametric studies is to understand the effect of pyrolysis gas momentum transfer on PICA material in-depth thermal responses with finite-rate, equilibrium, or frozen homogeneous gas chemistry. Results are presented, discussed, and compared with those predicted by the baseline PICA/FIAT ablation and thermal response model developed by the Orion Thermal Protection System Advanced Development Project.

Automated mini-column solid-phase extraction cleanup for high-throughput analysis of chemical contaminants in foods by low-pressure gas chromatography – tandem mass spectrometry

Science.gov (United States)

This study demonstrated the application of an automated high-throughput mini-cartridge solid-phase extraction (mini-SPE) cleanup for the rapid low-pressure gas chromatography – tandem mass spectrometry (LPGC-MS/MS) analysis of pesticides and environmental contaminants in QuEChERS extracts of foods. ...

Variability of matrix effects in liquid and gas chromatography - mass spectrometry analysis of pesticide residues after QuEChERS sample preparation of different food crops

Science.gov (United States)

Gas and liquid chromatography (GC and LC) coupled to sophisticated mass spectrometry (MS) instruments are among the most powerful analytical tools currently available to monitor pesticide residues in food, among other applications. However, both GC-MS and LC-MS are susceptible to matrix effects whi...

Thermal-maturity limit for primary thermogenic-gas generation from humic coals as determined by hydrous pyrolysis

Science.gov (United States)

Lewan, Michael; Kotarba, M.J.

2014-01-01

Hydrous-pyrolysis experiments at 360°C (680°F) for 72 h were conducted on 53 humic coals representing ranks from lignite through anthracite to determine the upper maturity limit for hydrocarbon-gas generation from their kerogen and associated bitumen (i.e., primary gas generation). These experimental conditions are below those needed for oil cracking to ensure that generated gas was not derived from the decomposition of expelled oil generated from some of the coals (i.e., secondary gas generation). Experimental results showed that generation of hydrocarbon gas ends before a vitrinite reflectance of 2.0%. This reflectance is equivalent to Rock-Eval maximum-yield temperature and hydrogen indices (HIs) of 555°C (1031°F) and 35 mg/g total organic carbon (TOC), respectively. At these maturity levels, essentially no soluble bitumen is present in the coals before or after hydrous pyrolysis. The equivalent kerogen atomic H/C ratio is 0.50 at the primary gas-generation limit and indicates that no alkyl moieties are remaining to source hydrocarbon gases. The convergence of atomic H/C ratios of type-II and -I kerogen to this same value at a reflectance of indicates that the primary gas-generation limits for humic coal and type-III kerogen also apply to oil-prone kerogen. Although gas generation from source rocks does not exceed vitrinite reflectance values greater than , trapped hydrocarbon gases can remain stable at higher reflectance values. Distinguishing trapped gas from generated gas in hydrous-pyrolysis experiments is readily determined by of the hydrocarbon gases when a -depleted water is used in the experiments. Water serves as a source of hydrogen in hydrous pyrolysis and, as a result, the use of -depleted water is reflected in the generated gases but not pre-existing trapped gases.

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).

New Methodologies for Qualitative and Semi-Quantitative Determination of Carbon-Centered Free Radicals in Cigarette Smoke Using Liquid ChromatographyTandem Mass Spectrometry and Gas Chromatography-Mass Selective Detection

Directory of Open Access Journals (Sweden)

Gerardi AR

2014-12-01

Full Text Available Several approaches were explored to develop a high throughput procedure for relative determination of 14 different carbon-centered free radicals, both acyl and alkylaminocarbonyl type, in cigarette smoke. Two trapping procedures using 3-cyano-2,2,5,5-tetramethyl-1-pyrrolidinyloxy, or 3-cyanoproxyl radical (3-CNP were designed for this study: a trapping in solution and b trapping on a solid support which was a Cambridge filter pad. Fresh whole smoke and vapor phase smoke from mainstream cigarette smoke from Kentucky Reference Cigarettes 2R4F, as partitioned via an unadulterated Cambridge filter pad, were transferred into each trapping system in separate experiments. The 3-CNP coated Cambridge filter pad approach was shown to be superior to the impinger procedure as described in this study. Gas chromatography coupled with mass selective detection (GC-MS was employed for the first time as an alternate means of detecting several relatively highly concentrated radical adducts. Liquid chromatography tandem mass spectrometry (LC-MS/MS with precursor ion monitoring and selected ion monitoring (SIM was used for detecting the large array of radicals, including several not previously reported: formyl, crotonyl, acrolein, aminocarbonyl, and anilinocarbonyl radicals. Relative quantitation was achieved using as external calibration standards of 4-(1-pyrrolidinobenzaldehyde and nicotine. It was determined that the yield of carbon-centered free radicals by reference cigarette 2R4F was approximately 265 nmoles/cigarette at 35 mL puff/60 sec interval/2 sec duration smoking conditions.

Determination of vitamins D2 and D3 in selected food matrices by online high-performance liquid chromatography-gas chromatography-mass spectrometry (HPLC-GC-MS).

Science.gov (United States)

Nestola, Marco; Thellmann, Andrea

2015-01-01

An online normal-phase liquid chromatography-gas chromatography-mass spectrometry (HPLC-GC-MS) method was developed for the determination of vitamins D2 and D3 in selected food matrices. Transfer of the sample from HPLC to GC was realized by large volume on-column injection; detection was performed with a time-of-flight mass spectrometer (TOF-MS). Typical GC problems in the determination of vitamin D such as sample degradation or sensitivity issues, previously reported in the literature, were not observed. Determination of total vitamin D content was done by quantitation of its pyro isomer based on an isotopically labelled internal standard (ISTD). Extracted ion traces of analyte and ISTD showed cross-contribution, but non-linearity of the calibration curve was not determined inside the chosen calibration range by selection of appropriate quantifier ions. Absolute limits of detection (LOD) and quantitation (LOQ) for vitamins D2 and D3 were calculated as approximately 50 and 150 pg, respectively. Repeatability with internal standard correction was below 2 %. Good agreement between quantitative results of an established high-performance liquid chromatography with UV detection (HPLC-UV) method and HPLC-GC-MS was found. Sterol-enriched margarine was subjected to HPLC-GC-MS and HPLC-MS/MS for comparison, because HPLC-UV showed strong matrix interferences. HPLC-GC-MS produced comparable results with less manual sample cleanup. In summary, online hyphenation of HPLC and GC allowed a minimization in manual sample preparation with an increase of sample throughput.

Flash pyrolysis at high temperature of ligno-cellulosic biomass and its components - production of synthesis gas; Pyrolyse flash a haute temperature de la biomasse ligno-cellulosique et de ses composes - production de gaz de synthese

Energy Technology Data Exchange (ETDEWEB)

Couhert, C

2007-11-15

Pyrolysis is the first stage of any thermal treatment of biomass and governs the formation of synthesis gas for the production of electricity, hydrogen or liquid fuels. The objective of this work is to establish a link between the composition of a biomass and its pyrolysis gas. We study experimental flash pyrolysis and fix the conditions in which quantities of gas are maximal, while aiming at a regime without heat and mass transfer limitations (particles about 100 {mu}m): temperature of 950 C and residence time of about 2 s. Then we try to predict gas yields of any biomass according to its composition, applicable in this situation where thermodynamic equilibrium is not reached. We show that an additivity law does not allow correlating gas yields of a biomass with fractions of cellulose, hemi-cellulose and lignin contained in this biomass. Several explanations are suggested and examined: difference of pyrolytic behaviour of the same compound according to the biomass from which it is extracted, interactions between compounds and influence of mineral matter. With the aim of industrial application, we study pyrolysis of millimetric and centimetric size particles, and make a numerical simulation of the reactions of pyrolysis gases reforming. This simulation shows that the choice of biomass affects the quantities of synthesis gas obtained. (author)

Pyrolysis gas chromatographic atomic emission detection for sediments, coals and other petrochemical precursors

Energy Technology Data Exchange (ETDEWEB)

Seeley, J.A.; Zeng, Y.D.; Uden, P.C.; Eglinton, T.I.; Ericson, I. (Massachusetts University, Amherst, MA (USA). Dept. of Chemistry)

1992-09-01

On-line flash pyrolysis coupled to a capillary gas chromatograph for the characterization of marine sediments, coals and other heterogeneous solid samples is described. A helium microwave-induced plasma is used for chromatographic detection by atomic emission spectrometry. Simultaneous multi-element detection is achieved with a photodiode array detector. The optical path of the gas chromatographic atomic emission detector is purged with helium, allowing simultaneous, sensitive detection of atomic emission from sulfur 181 nm, phosphorous 186 nm, arsenic 189 nm, selenium 196 nm and carbon 193 nm. Several sediment and coal samples have been analysed for their carbon, nitrogen, sulfur, oxygen, phosphorous, arsenic and selenium content. Qualitative information indicating the occurrence and distribution of these elements in the samples can be used to gauge the relative stage of diagenetic evolution of the samples and provide information on their depositional environment. In some instances the chromatographic behaviour of the compounds produced upon pyrolysis is improved through on-line alkylation. This on-line derivatization is achieved by adding liquid reagents to the pyrolysis probe or by adding liquid reagents to the pyrolysis probe or by adding solid reagents either to the solid sample or by packing the reagent in the injection port of the chromatograph.

Comparative determination of phenytoin by spectrophotometry, gas chromatography, liquid chromatography, enzyme immunoassay, and radioimmunoassay

International Nuclear Information System (INIS)

Castro, A.; Ibanez, J.; DiCesare, J.L.; Adams, R.F.; Malkus, H.

1978-01-01

Sera from patients being treated with phenytoin were analyzed for the drug by spectrophotometry, gas chromatography, radioimmunoasay, enzyme immunoassay, and liquid chromatography. The assay values obtained were intercompared statistically. Enzyme immunoassay and liquid chromatography appear to be attractive alternatives to the more traditional methods of spectrophotometry and gas chromatography. Our radioimmunoassay data correlated poorly with results by the four other methods

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

NARCIS (Netherlands)

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

2008-01-01

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

A STUDY ON CARBON ISOTOPE OF CO2 AND CH4 IN WESTERN DIENG PLATEU BY GAS CHROMATOGRAPHY- ISOTOPE RATIO MASS SPECTROMETER (GC-IRMS

Directory of Open Access Journals (Sweden)

Hanik Humaida

2010-06-01

Full Text Available The carbon isotope can be used to evaluate volcanism phenomenon of volcano. The study of carbon isotope of CO2 and CH4 was carried out in western Dieng Plateau by mass-spectrometer. Before analysis, sampel was separated by gas chromatography using a Porapak-Q column and a FID (Flame Ionization Detector detector. The gas was oxidized by copper oxide at 850oC before being ionized in mass-spectrometer for isotope analysis. The CO2 content in Candradimuka crater (-4.10 O/OO, indicated that the gas may be as volcanic gas. The other CO2 from Sumber and western Gua Jimat, had isotope value  of -10.05 and -12.07 O/OO, respectively, indicating contamination from crustal and subduction material. The carbon isotope of CH4 gas from Pancasan village was -63.42 O/OO, that may be categorized as biogenic gas.   Keywords: isotope, CO2, CH4, Dieng.

Organic sulphur in macromolecular sedimentary organic matter. II. Analysis of distributions of sulphur-containing pyrolysis products using multivariate techniques

NARCIS (Netherlands)

Sinninghe Damsté, J.S.; Eglinton, T.I.; Pool, W.; Leeuw, J.W. de; Eijkel, G.; Boon, J.J.

1992-01-01

This study describes the analysis of sulphur-containing products from Curie-point pyrolysis (Py) of eighty-five samples (kerogens, bitumen, and petroleum asphaltenes and coals) using gas chromatography (GC) in combination with sulphur-selective detection. Peak areas of approximately forty individual

Methods in endogenous steroid profiling - A comparison of gas chromatography mass spectrometry (GC-MS) with supercritical fluid chromatography tandem mass spectrometry (SFC-MS/MS).

Science.gov (United States)

Teubel, Juliane; Wüst, Bernhard; Schipke, Carola G; Peters, Oliver; Parr, Maria Kristina

2018-06-15

In various fields of endocrinology, the determination of steroid hormones synthesised by the human body plays an important role. Research on central neurosteroids has been intensified within the last years, as they are discussed as biomarkers for various cognitive disorders. Their concentrations in cerebrospinal fluid (CSF) are considered to be regulated independently from peripheral fluids. For that reason, the challenging matrix CSF becomes a very interesting specimen for analysis. Concentrations are expected to be very low and available amount of CSF is limited. Thus, a comprehensive method for very sensitive quantification of a set of analytes as large as possible in one analytical aliquot is desired. However, high structural similarities of the selected panel of 51 steroids and steroid sulfates, including numerous isomers, challenges achievement of chromatographic selectivity. Since decades the analysis of endogenous steroids in various body fluids is mainly performed by gas chromatography (GC) coupled to (tandem) mass spectrometry (MS(/MS)). Due to the structure of the steroids of interest, derivatisation is performed to meet the analytical requirements for GC-MS(/MS). Most of the laboratories use a two-step derivatisation in multi-analyte assays that was already published in the 1980s. However, for some steroids this elaborate procedure yields multiple isomeric derivatives. Thus, some laboratories utilize (ultra) high performance liquid chromatography ((U)HPLC)-MS/MS as alternative but, even UHPLC is not able to separate some of the isomeric pairs. Supercritical fluid chromatography (SFC) as an orthogonal separation technique to GC and (U)HPLC may help to overcome these issues. Within this project the two most promising methods for endogenous steroid profiling were investigated and compared: the "gold standard" GC-MS and the orthogonal separation technique SFC-MS/MS. Different derivatisation procedures for gas chromatographic detection were explored and the

Identification and discrimination of oral asaccharolytic Eubacterium spp. by pyrolysis mass spectrometry and artificial neural networks.

Science.gov (United States)

Goodacre, R; Hiom, S J; Cheeseman, S L; Murdoch, D; Weightman, A J; Wade, W G

1996-02-01

Curie-point pyrolysis mass spectra were obtained from 29 oral asaccharolytic Eubacterium strains and 6 abscess isolates previously identified as Peptostreptococcus heliotrinreducens. Pyrolysis mass spectrometry (PyMS) with cluster analysis was able to clarify the taxonomic position of this group of organisms. Artificial neural networks (ANNS) were then trained by supervised learning (with the back-propagation algorithm) to recognize the strains from their pyrolysis mass spectra; all Eubacterium strains were correctly identified, and the abscess isolates were identified as un-named Eubacterium taxon C2 and were distinct from the type strain of P. heliotrinreducens. These results demonstrate that the combination of PyMS and ANNs provides a rapid and accurate identification technique.

Improving quantitative gas chromatography-electron ionization mass spectrometry results using a modified ion source: demonstration for a pharmaceutical application.

Science.gov (United States)

D'Autry, Ward; Wolfs, Kris; Hoogmartens, Jos; Adams, Erwin; Van Schepdael, Ann

2011-07-01

Gas chromatography-mass spectrometry is a well established analytical technique. However, mass spectrometers with electron ionization sources may suffer from signal drifts, hereby negatively influencing quantitative performance. To demonstrate this phenomenon for a real application, a static headspace-gas chromatography method in combination with electron ionization-quadrupole mass spectrometry was optimized for the determination of residual dichloromethane in coronary stent coatings. Validating the method, the quantitative performance of an original stainless steel ion source was compared to that of a modified ion source. Ion source modification included the application of a gold coating on the repeller and exit plate. Several validation aspects such as limit of detection, limit of quantification, linearity and precision were evaluated using both ion sources. It was found that, as expected, the stainless steel ion source suffered from signal drift. As a consequence, non-linearity and high RSD values for repeated analyses were obtained. An additional experiment was performed to check whether an internal standard compound would lead to better results. It was found that the signal drift patterns of the analyte and internal standard were different, consequently leading to high RSD values for the response factor. With the modified ion source however, a more stable signal was observed resulting in acceptable linearity and precision. Moreover, it was also found that sensitivity improved compared to the stainless steel ion source. Finally, the optimized method with the modified ion source was applied to determine residual dichloromethane in the coating of coronary stents. The solvent was detected but found to be below the limit of quantification. Copyright © 2011 Elsevier B.V. All rights reserved.

Pyrolysis kinetics of spent lark mushroom substrate and characterization of bio-oil obtained from the substrate

International Nuclear Information System (INIS)

Jiang, Haifeng; Cheng, Zhiqiang; Zhao, Tianqi; Liu, Mengzhu; Zhang, Mingyue; Li, Jianing; Hu, Meijuan; Zhang, Li; Li, Junfeng

2014-01-01

Highlights: • Pyrolysis behavior of spent lark mushroom substrate is investigated. • Significant pyrolysis stage occurs at the range of 232–382 °C. • Kinetics reveals the influence of heating rate on pyrolysis process. • The maximum bio-oil yield is found at 470 °C. • The characterization shows obtained oil can be utilized as a potential resource. - Abstract: In our work, thermal behavior and kinetic characteristics of spent lark mushroom substrate were evaluated to elaborate the thermal decomposition mechanisms and explore the influence of heating rate by using thermogravimetric analyzer and Coats–Redfern method. The study of pyrolysis temperature of raw material was also operated at the range of 410–530 °C, under the feeding rate 0.36 g/min, and the nitrogen flow 16 L/h. The results showed that the maximum bio-oil yield was obtained at 470 °C with the yield of 14.4 wt.%. The analysis of Fourier transform infrared spectrometer and gas chromatography coupled with mass selective detector indicated that the target liquid production was consisted of phenols, hydrocarbons and other components. Simultaneously, the low oxygen and high hydrogen content in bio-oil was also determined by elemental analysis. Based on the above-mentioned results, we demonstrated that the bio-oil obtained from the substrate had high utilization value as a potential energy resource

Online study on the co-pyrolysis of coal and corn with vacuum ultraviolet photoionization mass spectrometry.

Science.gov (United States)

Weng, Jun-Jie; Liu, Yue-Xi; Zhu, Ya-Nan; Pan, Yang; Tian, Zhen-Yu

2017-11-01

With the aim to support the experimental tests in a circulating fluidized bed pilot plant, the pyrolysis processes of coal, corn, and coal-corn blend have been studied with an online pyrolysis photoionization time-of-flight mass spectrometry (Py-PI-TOFMS). The mass spectra at different temperatures (300-800°C) as well as time-evolved profiles of selected species were measured. The pyrolysis products such as alkanes, alkenes, phenols, aromatics, as well as nitrogen- and sulfur-containing species were detected. As temperature rises, the relative ion intensities of high molecular weight products tend to decrease, while those of aromatics increase significantly. During the co-pyrolysis, coal can promote the reaction temperature of cellulose in corn. Time-evolved profiles demonstrate that coal can affect pyrolysis rate of cellulose, hemicellulose, and lignin of corn in blend. This work shows that Py-PI-TOFMS is a powerful approach to permit a better understanding of the mechanisms underlying the co-pyrolysis of coal and biomass. Copyright © 2017 Elsevier Ltd. All rights reserved.

Characterization of the Key Aroma Compounds in Chinese Syrah Wine by Gas Chromatography-Olfactometry-Mass Spectrometry and Aroma Reconstitution Studies.

Science.gov (United States)

Zhao, Pengtao; Gao, Jinxin; Qian, Michael; Li, Hua

2017-06-24

The key aroma compounds and the organoleptic quality of two Chinese Syrah wines from the Yunnan Shangri-La region and Ningxia Helan mountain region were characterized. The most important eighty aroma-active compounds were identified by Gas Chromatography-Olfactometry. In both Syrah samples, ethyl 2-methylpropanoate, ethyl 3-methylbutanoate, 3-methylbutyl acetate, 2- and 3-methyl-1-butanol, ethyl hexanoate, ethyl octanoate, 2-phenethyl acetate, methional, 3-methylbutanoic acid, hexanoic acid, octanoic acid, β -damascenone, guaiacol, 2-phenylethanol, trans -whiskylactone, 4-ethylguaiacol, eugenol, 4-ethylphenol, and sotolon were detected to have the highest odor intensities. In the chemical analysis, 72 compounds were quantitated by Stir Bar Sorptive Extraction combined with Gas Chromatography Mass Spectrometry. Based on the Odor Activity Value (OAV), the aromas were reconstituted by combining aroma compounds in the synthetic wine, and sensory descriptive analysis was used to verify the chemical data. Fatty acid ethyl esters, acetate esters, and β -damascenone were found with higher OAVs in the more fruity-smelling sample of Helan Mountain rather than Shangri-La.

Auto shredder residue recycling: Mechanical separation and pyrolysis

International Nuclear Information System (INIS)

Santini, Alessandro; Passarini, Fabrizio; Vassura, Ivano; Serrano, David; Dufour, Javier; Morselli, Luciano

2012-01-01

Highlights: ► In this work, we exploited mechanical separation and pyrolysis to recycle ASR. ► Pyrolysis of the floating organic fraction is promising in reaching ELV Directive targets. ► Zeolite catalyst improve pyrolysis oil and gas yield. - Abstract: sets a goal of 85% material recycling from end-of-life vehicles (ELVs) by the end of 2015. The current ELV recycling rate is around 80%, while the remaining waste is called automotive shredder residue (ASR), or car fluff. In Europe, this is mainly landfilled because it is extremely heterogeneous and often polluted with car fluids. Despite technical difficulties, in the coming years it will be necessary to recover materials from car fluff in order to meet the ELV Directive requirement. This study deals with ASR pretreatment and pyrolysis, and aims to determine whether the ELV material recycling target may be achieved by car fluff mechanical separation followed by pyrolysis with a bench scale reactor. Results show that flotation followed by pyrolysis of the light, organic fraction may be a suitable ASR recycling technique if the oil can be further refined and used as a chemical. Moreover, metals are liberated during thermal cracking and can be easily separated from the pyrolysis char, amounting to roughly 5% in mass. Lastly, pyrolysis can be a good starting point from a “waste-to-chemicals” perspective, but further research should be done with a focus on oil and gas refining, in order both to make products suitable for the chemical industry and to render the whole recycling process economically feasible.

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 ...

XII All-Russian conference on gas chromatography. Program. Summary of reports

International Nuclear Information System (INIS)

2002-01-01

Program and summary of reports of the XII All-Russian conference on gas chromatography are performed. The conference took place in Samara, 10-14 June, 2002. Reports on physicochemical regularities of gas chromatography, application of chromatographic methods in atomic energetics are included in the program of the conference. Part of the reports are deleted to the analytical application of the gas chromatography. Adsorbents for the gas chromatography, complex methods, mathematic methods in chromatography, ecological aspects of the gas chromatography [ru

Ionic liquid stationary phases for gas chromatography.

Science.gov (United States)

Poole, Colin F; Poole, Salwa K

2011-04-01

This article provides a summary of the development of ionic liquids as stationary phases for gas chromatography beginning with early work on packed columns that established details of the retention mechanism and established working methods to characterize selectivity differences compared with molecular stationary phases through the modern development of multi-centered cation and cross-linked ionic liquids for high-temperature applications in capillary gas chromatography. Since there are many reviews on ionic liquids dealing with all aspects of their chemical and physical properties, the emphasis in this article is placed on the role of gas chromatography played in the design of ionic liquids of low melting point, high thermal stability, high viscosity, and variable selectivity for separations. Ionic liquids provide unprecedented opportunities for extending the selectivity range and temperature-operating range of columns for gas chromatography, an area of separation science that has otherwise been almost stagnant for over a decade. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Recycling of Zinc- and Lead-Bearing Residues with Pyrolysis Gas

Science.gov (United States)

Pichler, C.; Antrekowitsch, J.

2015-09-01

Efforts in the metallurgical industry for an approximation to the zero waste concept has led to many different investigations. Together with the greenhouse effect, CO2 emissions have caused additional costs for different process steps in the industry. For this reason, alternative carbon carriers have been sought, and charcoal was found to be an ideal substitute, due to its CO2 neutrality. In order to use it in the metallurgical industry, an optimization of the charcoal production through a carbonization process must be carried out. Beside the charcoal, pyrolysis gas also occurs during the heating of wood or agricultural wastes under the exclusion of air. Because of combustible compounds in this gas, it is possible to use it as a reduction agent instead of fossil carbon carriers. Together with the idea of preventing landfilling of metallurgical by-products, an investigation was carried out to treat zinc- and lead-containing materials. For this issue a special process concept was designed and developed. The main aspect was to recycle the zinc- and lead-containing Waelz slag, which results from the processing of steel mill dusts, in a vertical retort. Two different sizes of facilities were constructed to perform the reaction system of the solid Waelz slag with the gaseous reduction agent of pyrolysis gas.

Detection of lysergic acid diethylamide (LSD) in urine by gas chromatography-ion trap tandem mass spectrometry.

Science.gov (United States)

Sklerov, J H; Kalasinsky, K S; Ehorn, C A

1999-10-01

A confirmatory method for the detection and quantitation of lysergic acid diethylamide (LSD) is presented. The method employs gas chromatography-tandem mass spectrometry (GC-MS-MS) using an internal ionization ion trap detector for sensitive MS-MS-in-time measurements of LSD extracted from urine. Following a single-step solid-phase extraction of 5 mL of urine, underivatized LSD can be measured with limits of quantitation and detection of 80 and 20 pg/mL, respectively. Temperature-programmed on-column injections of urine extracts were linear over the concentration range 20-2000 pg/mL (r2 = 0.999). Intraday and interday coefficients of variation were LSD-positive samples in this laboratory. Comparisons with alternate GC-MS methods and extraction procedures are discussed.

Liquid Chromatography-Tandem Mass Spectrometry: An Emerging Technology in the Toxicology Laboratory.

Science.gov (United States)

Zhang, Yan Victoria; Wei, Bin; Zhu, Yu; Zhang, Yanhua; Bluth, Martin H

2016-12-01

In the last decade, liquid chromatography-tandem mass spectrometry (LC-MS/MS) has seen enormous growth in routine toxicology laboratories. LC-MS/MS offers significant advantages over other traditional testing, such as immunoassay and gas chromatography-mass spectrometry methodologies. Major strengths of LC-MS/MS include improvement in specificity, flexibility, and sample throughput when compared with other technologies. Here, the basic principles of LC-MS/MS technology are reviewed, followed by advantages and disadvantages of this technology compared with other traditional techniques. In addition, toxicology applications of LC-MS/MS for simultaneous detection of large panels of analytes are presented. Copyright © 2016 Elsevier Inc. All rights reserved.

Gas chromatography-mass spectrometry study of the essential oils of Schinus longifolia (Lindl.) speg., Schinus fasciculata (Griseb.) I. M. Johnst., and Schinus areira L.

Science.gov (United States)

Murray, Ana P; Frontera, María A; Tomas, María A; Mulet, María C

2005-01-01

The essential oil composition from the aerial parts of three Anacardiaceae growing in Bahía Blanca, Argentina was studied by gas chromatography and gas chromatography-mass spectrometry. The essential oils of S. longifolia and S. fasciculata have been studied for the first time. The major constituents were alpha-pinene (46.5%), beta-pinene (15.1%) and alpha-phellandrene (10.1%) for S. longifolia and limonene (10.9%), beta-phellandrene (6.16%) and alpha-phellandrene (5.6%) for S. fasciculata. The major components of the essential oil of S. areira were limonene (28.6%), alpha-phellandrene (10.1%), sabinene (9.2%) and camphene (9.2%) differing from the literature data. The essential oils from S. areira and S. longifolia exhibited a high biotoxicity in a brine shrimp assay with Artemia persimilis.

The pyrolysis of gas condensate at the Shatlyk field

Energy Technology Data Exchange (ETDEWEB)

Magaril, R.Z.; Khankuliyev, K.; Kul' zhayev, B.A.; Sergiyenko, S.R.

1984-01-01

The continuing growth in industrial demand for lower olefins for the manufacture of polymer materials has necessitated an expansion in the manufacture of ethylene. Gas condensate may serve as a source of ethylene manufacturing. The influence of the contact temperature and time in the pyrolysis of unseparated condensate from the Shatlyk field on the yield of lower olefins was investigated. It was discovered that the total yield of lower olefins (C2-C4) increases with an increase in the pyrolysis temperature, reaching a maximum of 63 to 67 percent by weight at a temperature of 1098 degrees Kelvin and contact time of .5 to .7 seconds, and at 1123 degrees Kelvin and .3 seconds, the maximum ethylene yield (40 percent) was obtained at 1123 degrees Kelvin, and at all previously noted temperatures with a contact time of .9 seconds.

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.

Comprehensive two-dimensional gas chromatography for the analysis of organohalogenated micro-contaminants

NARCIS (Netherlands)

Korytar, P.; Haglund, P.; Boer, de J.; Brinkman, U.A.Th.

2006-01-01

We explain the principles of comprehensive two-dimensional gas chromatography (GC × GC), and discuss key instrumental aspects - with emphasis on column combinations and mass spectrometric detection. As the main item of interest, we review the potential of GC × GC for the analysis of

A comparative study of three tissue-cultured Dendrobium species and their wild correspondences by headspace gas chromatography-mass spectrometry combined with chemometric methods.

Science.gov (United States)

Chen, Nai-Dong; You, Tao; Li, Jun; Bai, Li-Tao; Hao, Jing-Wen; Xu, Xiao-Yuan

2016-10-01

Plant tissue culture technique is widely used in the conservation and utilization of rare and endangered medicinal plants and it is crucial for tissue culture stocks to obtain the ability to produce similar bioactive components as their wild correspondences. In this paper, a headspace gas chromatography-mass spectrometry method combined with chemometric methods was applied to analyze and evaluate the volatile compounds in tissue-cultured and wild Dendrobium huoshanense Cheng and Tang, Dendrobium officinale Kimura et Migo and Dendrobium moniliforme (Linn.) Sw. In total, 63 volatile compounds were separated, with 53 being identified from the three Dendrobium spp. Different provenances of Dendrobiums had characteristic chemicals and showed remarkable quantity discrepancy of common compositions. The similarity evaluation disclosed that the accumulation of volatile compounds in Dendrobium samples might be affected by their provenance. Principal component analysis showed that the first three components explained 85.9% of data variance, demonstrating a good discrimination between samples. Gas chromatography-mass spectrometry techniques, combined with chemometrics, might be an effective strategy for identifying the species and their provenance, especially in the assessment of tissue-cultured Dendrobium quality for use in raw herbal medicines. Copyright © 2016. Published by Elsevier B.V.

Characterisation of Tertiary Catalan lacustrine oil shales: Discovery of extremely organic sulphur-rich type I kerogens

NARCIS (Netherlands)

Sinninghe Damsté, J.S.; Las Heras, F.X.C. de; Bergen, P.F. van; Leeuw, J.W. de

1993-01-01

The kerogens of three Tertiary Catalan lacustrine oil shales were analyzed by light microscopy, flash pyrolysis-gas chromatography-mass spectrometry, and bulk composition methods (elemental analysis, Rock Eval pyrolysis). Two of the three kerogens (Ribesalbes and Campins) are extremely rich in

Improved fatty acid detection in micro-algae and aquatic meiofauna species using a direct thermal desorption interface combined with comprehensive gas chromatography-time-of-flight mass spectrometry

NARCIS (Netherlands)

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

2008-01-01

Comprehensive two-dimensional gas chromatography (GC × GC) with time-of-flight mass spectrometry detection is used to profile the fatty acid composition of whole/intact aquatic microorganisms such as the common fresh water green algae Scenedesmus acutus and the filamentous cyanobacterium Limnothrix

Improved fatty acid detection in micro-algae and aquatic meiofauna species using a direct thermal desorption interface combined with comprehensive gas chromatography-time-of-flight mass spectrometry

NARCIS (Netherlands)

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

2008-01-01

Comprehensive two-dimensional gas chromatography (GC x GC) with time-of-flight mass spectrometry detection is used to profile the fatty acid composition of whole/intact aquatic microorganisms such as the common fresh water green algae Scenedesmus acutus and the filamentous cyanobacterium Limnothrix

Well-to-wheels analysis of fast pyrolysis pathways with the GREET model.

Energy Technology Data Exchange (ETDEWEB)

Han, J.; Elgowainy, A.; Palou-Rivera, I.; Dunn, J.B.; Wang, M.Q. (Energy Systems)

2011-12-01

The pyrolysis of biomass can help produce liquid transportation fuels with properties similar to those of petroleum gasoline and diesel fuel. Argonne National Laboratory conducted a life-cycle (i.e., well-to-wheels [WTW]) analysis of various pyrolysis pathways by expanding and employing the Greenhouse Gases, Regulated Emissions, and Energy Use in Transportation (GREET) model. The WTW energy use and greenhouse gas (GHG) emissions from the pyrolysis pathways were compared with those from the baseline petroleum gasoline and diesel pathways. Various pyrolysis pathway scenarios with a wide variety of possible hydrogen sources, liquid fuel yields, and co-product application and treatment methods were considered. At one extreme, when hydrogen is produced from natural gas and when bio-char is used for process energy needs, the pyrolysis-based liquid fuel yield is high (32% of the dry mass of biomass input). The reductions in WTW fossil energy use and GHG emissions relative to those that occur when baseline petroleum fuels are used, however, is modest, at 50% and 51%, respectively, on a per unit of fuel energy basis. At the other extreme, when hydrogen is produced internally via reforming of pyrolysis oil and when bio-char is sequestered in soil applications, the pyrolysis-based liquid fuel yield is low (15% of the dry mass of biomass input), but the reductions in WTW fossil energy use and GHG emissions are large, at 79% and 96%, respectively, relative to those that occur when baseline petroleum fuels are used. The petroleum energy use in all scenarios was restricted to biomass collection and transportation activities, which resulted in a reduction in WTW petroleum energy use of 92-95% relative to that found when baseline petroleum fuels are used. Internal hydrogen production (i.e., via reforming of pyrolysis oil) significantly reduces fossil fuel use and GHG emissions because the hydrogen from fuel gas or pyrolysis oil (renewable sources) displaces that from fossil fuel

Thermo-Catalytic Pyrolysis of Waste Plastics from End of Life Vehicle

Directory of Open Access Journals (Sweden)

Miskolczi Norbert

2016-01-01

Full Text Available Pyrolysis of waste plastics is widely used recycling method. Owing to the end-of-life vehicles regulations, 95% of passenger cars and vehicles must reused/recovered after the dismantling. Pyrolysis of waste polyethylene and polypropylene obtained from end-of-life vehicles was investigated in a continuously stirred batch reactor using 500 and 600°C temperatures. To ensure the pyrolysis reactions the tested catalysts (5% of ZSM-5, HZSM-5, Ni-ZSM-5 and Fe-ZSM-5 were added directly to the mixtures of raw materials. Products of pyrolysis were separated into gases, pyrolysis oil and heavy oil, which was further analyzed by gas-chromatography, Fourier transformed infrared spectroscopy and other standardized methods. Based on the results it was concluded, that the catalysts significantly increase the yields of volatile products, and modify their composition. Especially the alkane/alkene ratio, the methane concentration and the concentration of branched hydrocarbon could be affected by the applied catalysts. Ni-ZSM-5 catalyst had the highest activity in methane production, while HZSM-5 catalyst proved effective in isomerization reactions. Using H-ZSM-5, Ni-ZSM-5, and Fe-ZSM-5 catalyst notably decreased average molecular weight of pyrolysis oils and significantly higher aromatic content was observed.

A study of paint sludge deactivation by pyrolysis reactions

Directory of Open Access Journals (Sweden)

Muniz L.A.R.

2003-01-01

Full Text Available The production of large quantities of paint sludge is a serious environmental problem. This work evaluates the use of pyrolysis reaction as a process for deactivating paint sludge that generates a combustible gas phase, a solvent liquid phase and an inert solid phase. These wastes were classified into three types: water-based solvent (latex resin and solvents based on their resins (alkyd and polyurethane. An electrically heated stainless steel batch reactor with a capacity of 579 mL and a maximum pressure of 30 atm was used. Following the reactor, a flash separator, which was operated at atmospheric pressure, partially condensed and separated liquid and gas products. Pressure and temperature were monitored on-line by a control and data acquisition system, which adjusted the heating power supplied to the pyrolysis reactor. Reactions followed an experimental design with two factors (reaction time and temperature and three levels (10, 50 and 90 minutes; 450, 550 and 650degreesC. The response variables were liquid and solid masses and net heat of combustion. The optimal operational range for the pyrolysis process was obtained for each response variable. A significant reduction in total mass of solid waste was obtained.

Liquid chromatography - mass spectrometry analysis of pharmaceuticals

International Nuclear Information System (INIS)

Macasek, F.

2003-01-01

The drugs represent mostly non-volatile and thermally labile solutes, often available only in small amounts like it is in case of radiopharmaceuticals. Therefor, the favourable separation techniques for such compounds are HPLC, capillary electrophoresis and also TLC 1. Liquid chromatography with mass spectrometric detector (LC/MS) is especially powerful for their microanalysis. Mass spectrometry separating the ions in high vacuum was presumably used as detector for gas chromatography effluent but the on-line coupling with liquid eluant flow 0.1-1 mL/min is far more challenging. New types of ion sources were constructed for simultaneous removal of solvent and ionisation of solutes at atmospheric pressure (API). At present, a relatively wide choice of successfully designed commercial equipment is available either for small organic molecules and larger biomolecules (Perkin-Elmer, Agilent, Jeol, Bruker Daltonics, ThermoQuest, Shimadzu). The features of the LC/MS systems are presented. LC/MS as a new quality control tool for [F-18]fluorodeoxyglucose (FDG) radiopharmaceutical, which has became the most spread radiopharmaceutical for positron emission tomography (PET), was proposed. Other applications of the LC/MS are reviewed. (author)

Determination of tetrahydrozoline in urine and blood using gas chromatography-mass spectrometry (GC-MS).

Science.gov (United States)

Peat, Judy; Garg, Uttam

2010-01-01

Tetrahydrozoline, a derivative of imidazoline, is widely used for the symptomatic relief of conjunctival and nasal congestion; however, intentional or unintentional high doses can result in toxicity manifested by hypotension, tachycardia, and CNS depression. The detection of the drug in blood and urine is helpful in the diagnosis and management of a toxic patient. For the analysis, plasma, serum, or urine is added to a tube containing alkaline buffer and organic extraction solvents, and tetrahydrozoline from the sample is extracted into the organic phase by gentle mixing. After centrifugation, the upper organic solvent layer containing the drug is removed and dried under stream of nitrogen at 40 degrees C. The residue is reconstituted in a hexane-ethanol mixture and analyzed using gas-chromatography-mass spectrometry. Quantitation of the drug is done by comparing responses of unknown sample to the responses of the calibrators using selected ion monitoring. Naphazoline is used as an internal standard.

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.

Direct sample introduction-gas chromatography-mass spectrometry for the determination of haloanisole compounds in cork stoppers.

Science.gov (United States)

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

2016-12-02

A solventless analytical method is proposed for analyzing the compounds responsible for cork taint in cork stoppers. Direct sample introduction (DSI) is evaluated as a sample introduction system for the gas chromatography-mass spectrometry (GC-MS) determination of four haloanisoles (HAs) in cork samples. Several parameters affecting the DSI step, including desorption temperature and time, gas flow rate and other focusing parameters, were optimized using univariate and multivariate approaches. The proposed method shows high sensitivity and minimises sample handling, with detection limits of 1.6-2.6ngg -1 , depending on the compound. The suitability of the optimized procedure as a screening method was evaluated by obtaining decision limits (CCα) and detection capabilities (CCβ) for each analyte, which were found to be in 6.9-11.8 and 8.7-14.8ngg -1 , respectively, depending on the compound. Twenty-four cork samples were analysed, and 2,4,6-trichloroanisole was found in four of them at levels between 12.6 and 53ngg -1 . Copyright © 2016 Elsevier B.V. All rights reserved.

Electric plants to gas, influence of both Mineral Matter and Air Oxidation in coal pyrolysis

International Nuclear Information System (INIS)

Mondragon, F.; Jaramillo, A.; Quintero, G.

1995-01-01

In this work some coal samples from different Colombia's deposits are analyzed. In first stage, material matter is removed from coal by acid treatment with HF/HCl, and aerial oxidation of coal is made with air in oven to 150 Centigrade degree temperature. In second stage, pyrolysis is carried out in two different techniques: 1. Thermogravimetric Analysis (TGA) and 2. Programmed Temperature Pyrolysis (PTP) in a pyrolyzer equipped with a quadrupole mass spectrometer. In both techniques, the coal samples are heated in different rates to 650 Centigrade degree. During PTP trials the evolution of CH4, H2S, hydrocarbons (m/z=42), CO2, benzene and toluene are monitored. Studied coal samples showed: 1). A gas conversion range between 48.8% to 21.8%; 2). A decrease in the gas conversion between 2% to 4%, when oxidation it is applied; 3). The temperature at the one which is presented the maximum evolution of CH4 is similar for all coal samples; 4). The maximum evolution of H2S depends on mineral matter composition, occurs between 480 to 550 Centigrade degrees and is presented due to pyrite decomposition. 5). The evolution of CO2 occurs between 100 to 650 Centigrade degree, its production is generated in different stage of the mentioned temperature range, and in some coal samples is presented due to inorganic origin

Identification of organic sulfur compounds in coal bitumen obtained by different extraction techniques using comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometric detection

Energy Technology Data Exchange (ETDEWEB)

Machado, Maria Elisabete; Cappelli Fontanive, Fernando; Bastos Caramao, Elina; Alcaraz Zini, Claudia [Universidade Federal do Rio Grande do Sul, Instituto de Quimica, Porto Alegre, RS (Brazil); Oliveira, Jose Vladimir de [URI, Universidade Regional Integrada do Alto Uruguai e das Missoes, Erechim, RS (Brazil)

2011-11-15

The determination of organic sulfur compounds (OSC) in coal is of great interest. Technically and operationally these compounds are not easily removed and promote corrosion of equipment. Environmentally, the burning of sulfur compounds leads to the emission of SO{sub x} gases, which are major contributors to acid rain. Health-wise, it is well known that these compounds have mutagenic and carcinogenic properties. Bitumen can be extracted from coal by different techniques, and use of gas chromatography coupled to mass spectrometric detection enables identification of compounds present in coal extracts. The OSC from three different bitumens were tentatively identified by use of three different extraction techniques: accelerated solvent extraction (ASE), ultrasonic extraction (UE), and supercritical-fluid extraction (SFE). Results obtained from one-dimensional gas chromatography (1D GC) coupled to quadrupole mass spectrometric detection (GC-qMS) and from two-dimensional gas chromatography with time-of-flight mass spectrometric detection (GC x GC-TOFMS) were compared. By use of 2D GC, a greater number of OSC were found in ASE bitumen than in SFE and UE bitumens. No OSC were identified with 1D GC-qMS, although some benzothiophenes and dibenzothiophenes were detected by use of EIM and SIM modes. GC x GC-TOFMS applied to investigation of OSC in bitumens resulted in analytical improvement, as more OSC classes and compounds were identified (thiols, sulfides, thiophenes, naphthothiophenes, benzothiophenes, and benzonaphthothiophenes). The roof-tile effect was observed for OSC and PAH in all bitumens. Several co-elutions among analytes and with matrix interferents were solved by use of GC x GC. (orig.)

Kinetics of ethylcyclohexane pyrolysis and oxidation: An experimental and detailed kinetic modeling study

KAUST Repository

Wang, Zhandong

2015-07-01

Ethylcyclohexane (ECH) is a model compound for cycloalkanes with long alkyl side-chains. A preliminary investigation on ECH (Wang et al., Proc. Combust. Inst., 35, 2015, 367-375) revealed that an accurate ECH kinetic model with detailed fuel consumption mechanism and aromatic growth pathways, as well as additional ECH pyrolysis and oxidation data with detailed species concentration covering a wide pressure and temperature range are required to understand the ECH combustion kinetics. In this work, the flow reactor pyrolysis of ECH at various pressures (30, 150 and 760Torr) was studied using synchrotron vacuum ultraviolet (VUV) photoionization mass spectrometry (PIMS) and gas chromatography (GC). The mole fraction profiles of numerous major and minor species were evaluated, and good agreement was observed between the PIMS and GC data sets. Furthermore, a fuel-rich burner-stabilized laminar premixed ECH/O2/Ar flame at 30Torr was studied using synchrotron VUV PIMS. A detailed kinetic model for ECH high temperature pyrolysis and oxidation was developed and validated against the pyrolysis and flame data performed in this work. Further validation of the kinetic model is presented against literature data including species concentrations in jet-stirred reactor oxidation, ignition delay times in a shock tube, and laminar flame speeds at various pressures and equivalence ratios. The model well predicts the consumption of ECH, the growth of aromatics, and the global combustion properties. Reaction flux and sensitivity analysis were utilized to elucidate chemical kinetic features of ECH combustion under various reaction conditions. © 2015 The Combustion Institute.

Gas Chromatographic-Mass Spectrometric Analysis of Essential Oil ...

African Journals Online (AJOL)

Purpose: To analyze the essential oil composition of the flower of Jasminum officinale L. var. grandifloroum L. (Jasminum grandiflorum) by gas chromatography-mass spectrometry (GC-MS). Methods: The optimum GC-MS conditions used for the analysis were 250 oC inlet temperature, 150 oC MSD detector temperature, ...

Analysis of volatile organic compounds in pleural effusions by headspace solid-phase microextraction coupled with cryotrap gas chromatography and mass spectrometry.

Science.gov (United States)

Huang, Zhongping; Zhang, Jie; Zhang, Peipei; Wang, Hong; Pan, Zaifa; Wang, Lili

2016-07-01

Headspace solid-phase microextraction coupled with cryotrap gas chromatography and mass spectrometry was applied to the analysis of volatile organic compounds in pleural effusions. The highly volatile organic compounds were separated successfully with high sensitivity by the employment of a cryotrap device, with the construction of a cold column head by freezing a segment of metal capillary with liquid nitrogen. A total of 76 volatile organic compounds were identified in 50 pleural effusion samples (20 malignant effusions and 30 benign effusions). Among them, 34 more volatile organic compounds were detected with the retention time less than 8 min, by comparing with the normal headspace solid-phase microextraction coupled with gas chromatography and mass spectrometry method. Furthermore, 24 volatile organic compounds with high occurrence frequency in pleural effusion samples, 18 of which with the retention time less than 8 min, were selected for the comparative analysis. The results of average peak area comparison and box-plot analysis showed that except for cyclohexanone, 2-ethyl-1-hexanol, and tetramethylbenzene, which have been reported as potential cancer biomarkers, cyclohexanol, dichloromethane, ethyl acetate, n-heptane, ethylbenzene, and xylene also had differential expression between malignant and benign effusions. Therefore, the proposed approach was valuable for the comprehensive characterization of volatile organic compounds in pleural effusions. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Analysis of isothiazolinones in environmental waters by gas chromatography-mass spectrometry.

Science.gov (United States)

Rafoth, Astrid; Gabriel, Sabine; Sacher, Frank; Brauch, Heinz-Jürgen

2007-09-14

This paper describes an analytical method for the determination of five biocides of isothiazolinone type (2-methyl-3-isothiazolinone (MI), 5-chloro-2-methyl-3-isothiazolinone (CMI), 1,2-benzisothiazolinone (BIT), 2-octyl-3-isothiazolinone (OI), 4,5-dichloro-2-octyl-3-isothiazolinone (DCOI)) in environmental waters. The method is based on pre-concentration of the analytes by solid-phase extraction onto a mixture of a polymeric material and RP-C18 material and subsequent determination by gas chromatography-mass spectrometry (GC-MS). One of the target compounds (BIT) is derivatised with diazomethane after pre-concentration to improve its chromatographic performance. The method was optimised with respect to pre-concentration conditions (liquid-liquid extraction versus solid-phase extraction, solid-phase material, elution solvent and volume) and extensively validated. Applying the method to surface waters, groundwaters, and drinking waters, limits of detection between 0.01 and 0.1 microg/l could be achieved and the repeatability was below 10% for all compounds except for MI. Additional investigations showed that the stability of the isothiazolinones in environmental waters is limited and sample storage at 4 degrees C is mandatory to preserve the target biocides. First investigations of influents and effluents of a wastewater treatment plant showed that conventional wastewater treatment exhibits a high efficiency for removal of the isothiazolinones. In river waters, the target isothiazolinones could not be detected.

Analysis of Frankincense in Archaeological Samples by Gas Chromatography-Mass Spectrometry

International Nuclear Information System (INIS)

Mathe, C.; Archier, P.; Vieillescazes, C.; Connan, J.; Mouton, M.

2007-01-01

Four archaeological samples, unearthed from Qana in Yemen were analysed by analytical technique, currently applied in the field of petroleum geochemistry, and by gas chromatography coupled with a mass spectrometer (GC-MS). Sample no 1286 comes from a burned warehouse and samples no 964, 963 and 962 from the central sanctuary. These specimens were probably exposed to a heating source. In each case olibanum resin was identified according to the presence of their chemical markers corresponding to α-, β-boswellic and lupeolic acids (3α-hydroxy-olean-12-en-24-oic, 3α-hydroxy-urs-12-en-24-oic and 3α-hydroxy-lup-20(29)en-24-oic acids) and their respective O-acetyled derivatives (3α- O-acetyl -olean-12-en-24-oic, 3α-O-acetyl-urs-12-en-24-oic and 3α-O-acetyl-lup-20(29)-en-24-oic acids). Concerning the thermal degradation state of samples, the GC-MS results are in agreement with the geochemical ones. Sample no 1286 and 964 correspond to ageing incense which has not undergone any heating action and are consequently relatively well preserved. Lastly, samples no 963 and 962 are thermally degraded resins and their gross composition data permits to conclude that sample no 963 is only partially burnt while sample no 962 has been much more degraded

Identification and differentiation of methcathinone analogs by gas chromatography-mass spectrometry.

Science.gov (United States)

Tsujikawa, Kenji; Mikuma, Toshiyasu; Kuwayama, Kenji; Miyaguchi, Hajime; Kanamori, Tatsuyuki; Iwata, Yuko T; Inoue, Hiroyuki

2013-08-01

To overcome a number of challenges involved in analyzing methcathinone (MC) analogues, we performed gas chromatography-mass spectrometry (GC-MS) analysis, including sample preparation, of nine MC analogues - 4-methylmethcathinone, three positional isomers of fluoromethcathinones, 4-methoxymethcathinone, N-ethylcathinone, N,N-dimethylcathinone, buphedrone, and pentedrone. The MC analogues underwent dehydrogenation when the free bases were analyzed using splitless injection. Most of this thermal degradation was prevented using split injection. This indicated that a shorter residence time in the hot injector prevented decomposition. Uniquely, 2-fluoromethcathinone degraded to another product in a process that could not be prevented by the split injection. Replacing the liner with a new, clean one was also effective in preventing thermal degradation. Most of the analytes showed a substantial loss (>30%) when the free base solution in ethyl acetate was evaporated under a nitrogen stream. Adding a small amount of dimethylformamide as a solvent keeper had a noticeable effect, but it did not completely prevent the loss. Three positional isomers of fluoromethcathinones were separated with baseline resolution by heptafluorobutyrylation with a slow column heating rate (8 °C/min) using a non-polar DB-5 ms capillary column. These results will be useful for the forensic analysis of MC analogues in confiscated materials. Copyright © 2012 John Wiley & Sons, Ltd.

Catalytic Pyrolysis of Chilean Oak: Influence of Brønsted Acid Sites of Chilean Natural Zeolite

Directory of Open Access Journals (Sweden)

Serguei Alejandro Martín

2017-11-01

Full Text Available This paper proposes the Chilean natural zeolite as catalyst on bio-oil upgrade processes. The aim of this study was to analyze chemical composition of bio-oil samples obtained from catalytic pyrolysis of Chilean native oak in order to increase bio-oil stability during storage. In order to identify chemical compounds before and after storage, biomass pyrolysis was carried out in a fixed bed reactor at 623 K and bio-oil samples were characterized by gas chromatography/mass spectrophotometry (GC/MS. A bio-oil fractionation method was successfully applied here. Results indicate that bio-oil viscosity decreases due to active sites on the zeolite framework. Active acids sites were associated with an increment of alcohols, aldehydes, and hydrocarbon content during storage. Higher composition on aldehydes and alcohols after storage could be attributed to the occurrence of carbonyl reduction reactions that promotes them. These reactions are influenced by zeolite surface characteristics and could be achieved via the direct contribution of Brønsted acid sites to Chilean natural zeolite.

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.

Identification of volatile organic compounds (VOCs) in different colour carrot (Daucus carota L.) cultivars using static headspace/gas chromatography/mass spectrometry

OpenAIRE

Zehra Güler; Fatih Karaca; Halit Yetisir

2015-01-01

Volatile organic compounds (VOCs) as well as sugar and acid contents affect carrot flavour. This study compared VOCs in 11 carrot cultivars. Gas chromatography/mass spectrometry using static headspace technique was applied to analyse the VOCs. The number of VOCs per sample ranged from 17 to 31. The primarily VOCs identified in raw carrots with the exception of “Yellow Stone” were terpenes, ranging from 65 to 95%. The monoterpenes with values ranging from 31 to 89% were higher than those (from...

Characterisation of capillary ionic liquid columns for gas chromatography-mass spectrometry analysis of fatty acid methyl esters.

Science.gov (United States)

Zeng, Annie Xu; Chin, Sung-Tong; Nolvachai, Yada; Kulsing, Chadin; Sidisky, Leonard M; Marriott, Philip J

2013-11-25

Due to their distinct chemical properties, the application of ionic liquid (IL) compounds as gas chromatography (GC) stationary phases offer unique GC separation especially in the analysis of geometric and positional fatty acid methyl ester (FAME) isomers. Elution behaviour of FAME on several commercialised IL capillary columns including phosphonium based SLB-IL59, SLB-IL60, SLB-IL61 and SLB-IL76 and imidazolium based SLB-IL82, SLB-IL100, and SLB-IL111 as well as a general purpose column SLB-5ms, were evaluated in gas chromatography-mass spectrometry (GC-MS) analysis. The phases were further characterised by using a linear solvation energy relationship (LSER) approach according to the equivalent chain length (ECL) index of FAME. Among all tested IL columns, elution temperatures of saturated FAME increased as their McReynolds' polarity value decreased, except for IL60. ECL values increased markedly as the stationary phase polarity increased, particularly for the polyunsaturated FAME. The LSER study indicated a lowest l/e value at 0.864 for IL111, displaying phase selectivity towards unsaturated FAME, with higher peak capacity within a carbon number isomer group. s and e descriptors calculated from LSER were validated by excellent correlation with dipole moments and lowest unoccupied molecular orbital (LUMO) energies, with R(2) values of 0.99 and 0.92 respectively, calculated using GAUSSIAN. Copyright © 2013 Elsevier B.V. All rights reserved.

Screening of environmental contaminants in honey bee wax comb using gas chromatography-high-resolution time-of-flight mass spectrometry.

Science.gov (United States)

Gómez-Ramos, M M; García-Valcárcel, A I; Tadeo, J L; Fernández-Alba, A R; Hernando, M D

2016-03-01

This study reports an analytical approach intended to be used for investigation of non-targeted environmental contaminants and to characterize the organic pollution pattern of bee wax comb samples. The method comprises a generic extraction followed by detection with gas chromatography coupled to high-resolution time-of-flight mass spectrometry (GC-TOF-MS), operated in electron impact ionization (EI) mode. The screening approach for the investigation of non-targeted contaminants consisted of initial peak detection by deconvolution and matching the first-stage mass spectra EI-MS(1) with a nominal mass spectral library. To gain further confidence in the structural characterization of the contaminants under investigation, the molecular formula of representative ions (molecular ion when present in the EI spectrum) and, for at least other two fragment ions, was provided for those with an accurate mass scoring (mass error contaminants in 50 samples of bee wax comb. This approach has allowed the tentative identification of some GC-amenable contaminants belonging to different chemical groups, among them, phthalates and polycyclic aromatic hydrocarbons (PAHs), along with residues of veterinary treatments used in apiculture.

Compound-Specific Chlorine Isotope Analysis of Tetrachloromethane and Trichloromethane by Gas Chromatography-Isotope Ratio Mass Spectrometry vs Gas Chromatography-Quadrupole Mass Spectrometry: Method Development and Evaluation of Precision and Trueness.

Science.gov (United States)

Heckel, Benjamin; Rodríguez-Fernández, Diana; Torrentó, Clara; Meyer, Armin; Palau, Jordi; Domènech, Cristina; Rosell, Mònica; Soler, Albert; Hunkeler, Daniel; Elsner, Martin

2017-03-21

Compound-specific chlorine isotope analysis of tetrachloromethane (CCl 4 ) and trichloromethane (CHCl 3 ) was explored by both, gas chromatography-isotope ratio mass spectrometry (GC-IRMS) and GC-quadrupole MS (GC-qMS), where GC-qMS was validated in an interlaboratory comparison between Munich and Neuchâtel with the same type of commercial GC-qMS instrument. GC-IRMS measurements analyzed CCl isotopologue ions, whereas GC-qMS analyzed the isotopologue ions CCl 3 , CCl 2 , CCl (of CCl 4 ) and CHCl 3 , CHCl 2 , CHCl (of CHCl 3 ), respectively. Lowest amount dependence (good linearity) was obtained (i) in H-containing fragment ions where interference of 35 Cl- to 37 Cl-containing ions was avoided; (ii) with tuning parameters favoring one predominant rather than multiple fragment ions in the mass spectra. Optimized GC-qMS parameters (dwell time 70 ms, 2 most abundant ions) resulted in standard deviations of 0.2‰ (CHCl 3 ) and 0.4‰ (CCl 4 ), which are only about twice as large as 0.1‰ and 0.2‰ for GC-IRMS. To compare also the trueness of both methods and laboratories, samples from CCl 4 and CHCl 3 degradation experiments were analyzed and calibrated against isotopically different reference standards for both CCl 4 and CHCl 3 (two of each). Excellent agreement confirms that true results can be obtained by both methods provided that a consistent set of isotopically characterized reference materials is used.

Comprehensive gas chromatography coupled to mass spectrometry for the separation of pesticides in a very complex matrix.

Science.gov (United States)

Mondello, Luigi; Casilli, Alessandro; Tranchida, Peter Quinto; Lo Presti, Maria; Dugo, Paola; Dugo, Giovanni

2007-11-01

The present research is focused on the development of a comprehensive two-dimensional gas chromatography-rapid scanning quadrupole mass spectrometric (GC x GC-qMS) methodology for the analysis of trace-amount pesticides contained in a complex real-world sample. Reliable peak assignment was carried out by using a recently developed, dedicated pesticide MS library (for comprehensive GC analysis), characterized by a twin-filter search procedure, the first based on a minimum degree of spectral similarity and the second on the interactive use of linear retention indices (LRI). The library was constructed by subjecting mixtures of commonly used pesticides to GC x GC-qMS analysis and then deriving their pure mass spectra and LRI values. In order to verify the effectiveness of the approach, a pesticide-contaminated red grapefruit extract was analysed. The certainty of peak assignment was attained by exploiting both the enhanced separation power of dual-oven GC x GC and the highly effective search procedure.

Identification of volatile organic compounds (VOCs in plastic products using gas chromatography and mass spectrometry (GC/MS

Directory of Open Access Journals (Sweden)

Nerlis Pajaro-Castro

2014-10-01

Full Text Available Plastic materials are widely used in daily life. They contain a wide range of compounds with low molecular mass, including monomeric and oligomeric residues of polymerization, solvent-related chemicals residues, and various additives. Plastic products made of expanded polystyrene (EPS are currently employed as food containers. This study therefore sought to identify volatile organic compounds released by EPS from food packages and utensils used in Cartagena, Colombia. EPS-based plates, food and soup containers were subjected to various temperatures and released chemicals captured by solid phase microextraction, followed by on-column thermal desorption and gas chromatography/mass spectrometry analysis. The results revealed the presence of at least 30 different compounds in the EPS-based products examined; the most frequently found were benzaldehyde, styrene, ethylbenzene and tetradecane. The release of these molecules was temperature-dependent. It is therefore advisable to regulate the use of EPS products which may be subjected to heating in order to protect human health by decreasing the exposure to these chemicals.

Analysis of Polycyclic Aromatic Hydrocarbons in Ambient Aerosols by Using One-Dimensional and Comprehensive Two-Dimensional Gas Chromatography Combined with Mass Spectrometric Method: A Comparative Study

Directory of Open Access Journals (Sweden)

Yun Gyong Ahn

2018-01-01

Full Text Available Advanced separation technology paired with mass spectrometry is an ideal method for the analysis of atmospheric samples having complex chemical compositions. Due to the huge variety of both natural and anthropogenic sources of organic compounds, simultaneous quantification and identification of organic compounds in aerosol samples represents a demanding analytical challenge. In this regard, comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry (GC×GC-TOFMS has become an effective analytical method. However, verification and validation approaches to quantify these analytes have not been critically evaluated. We compared the performance of gas chromatography with quadrupole mass spectrometry (GC-qMS and GC×GC-TOFMS for quantitative analysis of eighteen target polycyclic aromatic hydrocarbons (PAHs. The quantitative obtained results such as limits of detection (LODs, limits of quantification (LOQs, and recoveries of target PAHs were approximately equivalent based on both analytical methods. Furthermore, a larger number of analytes were consistently identified from the aerosol samples by GC×GC-TOFMS compared to GC-qMS. Our findings suggest that GC×GC-TOFMS would be widely applicable to the atmospheric and related sciences with simultaneous target and nontarget analysis in a single run.

A high-throughput method for liquid chromatography-tandem mass spectrometry determination of plasma alkylresorcinols, biomarkers of whole grain wheat and rye intake

DEFF Research Database (Denmark)

Ross, Alastair B; Svelander, Cecilia; Savolainen, Otto I

2016-01-01

supported extraction methods for extracting alkylresorcinols from plasma and improved a normal-phase liquid chromatography coupled to a tandem mass spectrometer method to reduce sample analysis time. The method was validated and compared with gas chromatography-mass spectrometry analysis. Sample preparation...

Analysis of Essential Oil in Jerusalem Artichoke (Helianthus tuberosus L.) Leaves and Tubers by Gas Chromatography-Mass Spectrometry.

Science.gov (United States)

Helmi, Zead; Al Azzam, Khaldun Mohammad; Tsymbalista, Yuliya; Ghazleh, Refat Abo; Shaibah, Hassan; Aboul-Enein, Hassan

2014-12-01

To investigate, for the first time, the chemical composition of essential oil of the tubers and leaves of Jerusalem artichoke (Helianthus tuberosus L.), a species of sunflower native to eastern North America, growing in Ukraine. A hydrodistillation apparatus was used for the extraction of volatile components and then it was analysed by gas chromatography equipped with a split-splitless injector (split ratio, 1:50) and flame ionization detector (FID). The oil was analyzed under linear temperature programming applied at 4°C/min from 50°C - 340°C. Temperatures of the injector and FID detector were maintained at 280°C and 300°C, respectively. The chemical analysis of the oil was carried out using gas chromatography coupled to mass spectrometry (GC-MS), to determine the chemical composition of the volatile fraction. The essential oils content ranged from 0.00019 to 0.03486 and 0.00011 to 0.00205 (g/100g), in leaves and tubers, respectively. The qualitative and quantitative analysis led to the identification of 17 components in both species samples. The major component found in leaves and tubers was (-)-β-bisabolene with 70.7% and 63.1%, respectively. Essential oil profile of Jerusalem artichoke species showed significant differences between leaves and tubers species. Additionally, the leaves of Jerusalem artichoke are a promising source of natural β-bisabolene.

Kinetics of pyrolysis and combustion of spherical wood particles in a fluidized bed

International Nuclear Information System (INIS)

Mazziotti di Celso, Giuseppe; Rapagnà, Sergio; Prisciandaro, Marina; Zanoelo, Everton Fernando

2014-01-01

Highlights: • H 2 , CO 2 , CO and CH 4 released during wood pyrolysis were experimentally monitored. • CO 2 formed by burning the residual tar/char mixture was experimentally determined. • The kinetics of species production was reproduced with two simplified models. • The increase of the bed reactor temperature statistically enhanced the gas yield. • The pyrolysis time is statistically reduced by decreasing the particle size. - Abstract: The kinetics of wood pyrolysis and combustion of residual fuel at different particle diameters and temperatures was investigated. A known mass of wooden spheres was fed at the top of a fluidized bed reactor filled with olivine particles and fluidized with nitrogen. The concentration of H 2 , CO 2 , CO and CH 4 was on-line monitored with gas analyzers. An irreversible first order reaction was applied to describe the biomass pyrolysis. The rate constant was dependent on the average temperature of wood particle, obtained by solving the transient one-dimensional problem of heat conduction in a sphere. The rate for an irreversible second order reaction between the residual fuel and oxygen at the fluid–solid interface, which takes a finite resistance to mass transfer into account, was adopted to describe the combustion. The semi-empirical kinetic models for pyrolysis and combustion were able to describe, with certain limitations inherent to model simplifications, the experimental transient results of molar flow rates of major released species. A statistical model based on the results of the factorial design of experiments (3 2 ) confirmed a statistical significant effect of temperature and wood particle diameter on the gas yield and time of pyrolysis, respectively

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.

Quantitative analysis of arbutin and hydroquinone in strawberry tree (Arbutus unedo L., Ericaceae) leaves by gas chromatography-mass spectrometry.

Science.gov (United States)

Jurica, Karlo; Karačonji, Irena Brčić; Šegan, Sandra; Opsenica, Dušanka Milojković; Kremer, Dario

2015-09-01

The phenolic glycoside arbutin and its metabolite with uroantiseptic activity hydroquinone occur naturally in the leaves of various medicinal plants and spices. In this study, an extraction procedure coupled with gas chromatography-mass spectrometry (GC-MS) was developed to determine arbutin and hydroquinone content in strawberry tree (Arbutus unedo L., Ericaceae) leaves. The method showed good linearity (R2>0.9987) in the tested concentration range (0.5-200 μg mL(-1)), as well as good precision (RSD<5%), analytical recovery (96.2-98.0%), and sensitivity (limit of detection=0.009 and 0.004 μg mL(-1) for arbutin and hydroquinone, respectively). The results obtained by the validated GC-MS method corresponded well to those obtained by high performance liquid chromatography (HPLC) method. The proposed method was then applied for determining arbutin and hydroquinone content in methanolic leaf extracts. The amount of arbutin in the leaves collected on the island of Koločep (6.82 mg g(-1) dry weight) was found to be higher (tpaired=43.57, tc=2.92) in comparison to the amount of arbutin in the leaves collected on the island of Mali Lošinj (2.75 mg g(-1) dry weight). Hydroquinone was not detected in any of the samples. The analytical features of the proposed GC-MS method demonstrated that arbutin and hydroquinone could be determined alternatively by gas chromatography. Due to its wide concentration range, the method could also be suitable for arbutin and hydroquinone analysis in leaves of other plant families (Rosaceae, Lamiaceae, etc.).

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...

Bioaccumulation study of acrylate monomers in algae (Chlorella Kessleri) by PY-GC and PY-GC/MS

International Nuclear Information System (INIS)

Halas, L.; Orinak, A.; Adamova, M.; Ladomersky, J.

2004-01-01

Acrylate monomers methylmethacrylate (MMA) and cyclohexylmethacrylate (CHMA) bioaccumulation has been determined in aquatic organism, algae (Chlorella kessleri). Algae were collected in amount of 0.4 mg and directly injected to the paralytic cell. In algae bodies accumulated monomers were analysed by pyrolysis gas chromatography (Py-GC) and pyrolysis gas chromatography coupled with mass spectrometry (Py-GC/MS). Traces of the accumulated monomers in algae body can be determined after 1-, 2 -, 3-weeks of incubation. Maximum content of MMA was determined after 3-week of experiment, contrariwise in the case of CHMA after 2-week exposition. Relationship with pyrolysis temperature has also been studied. (authors)

Fast methods for screening of trichothecenes in fungal cultures using gas chromatography-tandem mass spectrometry

DEFF Research Database (Denmark)

Nielsen, Kristian Fog; Thrane, Ulf

2001-01-01

The paper presents a fast method for trichothecene profiling and chemotaxonomic studies in species of Fusarium, Stachybotrys, Trichoderma and Memnoniella. Micro scale extracted crude Fusarium extracts were derivatised using pentafluoropropionic anhydride and analysed by gas chromatography...

In line wood plastic composite pyrolyses and HZSM-5 conversion of the pyrolysis vapors

International Nuclear Information System (INIS)

Lin, Xiaona; Zhang, Zhijun; Tan, Shun; Wang, Fengqiang; Song, Yongming; Wang, Qingwen; Pittman, Charles U.

2017-01-01

Graphical abstract: HZSM-5 can be used to catalytic convert Wood Fiber-Polypropylene or Wood Fiber-Polypropylene pyrolysis vapors into aromatic compounds in reasonable selectivities. This provides a recycling utilization WPCs wastes method. - Highlights: • Converting wood/plastic composites (WPC) wastes into aromatics. • Recycling WPC by fast pyrolysis coupled with vapor catalytic cracking. • Selective production of aromatics from WPCs and their components over HZSM-5. • Acid site concentration inside zeolite was critical for maximizing aromatic yield. • Synergistic effects between wood and plastics enhanced aromatics production. - Abstract: Wood powder-high density polyethylene (WPE) and wood powder-polypropylene (WPP) composites were pyrolyzed at 550 °C in the presence of HZSM-5 catalysts using analytical pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS). Immediately passing the pyrolysis vapors through the HZSM-5 changed the product distribution by producing aromatic hydrocarbons and eliminating tar formation. Zeolite HZSM-5 was employed with three different silica-to-alumina ratios (25, 50, 260). The influence of catalysts on the yields of aliphatic and aromatic hydrocarbons, furan derivatives, lignin-derived compounds and acetic acid was studied. High yields of aliphatic hydrocarbons formed in WPE or WPP pyrolysis alone. The highest yields of aromatic hydrocarbons from WPE or WPP pyrolysis vapors over HZSM-5 occurred with a zeolite framework Si/Al ratio of 25 (more acid sites), suggesting that the concentration of acid sites inside the zeolite was critical for maximizing aromatic yield. Exposing vapors to HZSM-5 increased the hydrocarbon yields and reduced the amount of acetic acid produced, resulting in increased calorific value. The yields of typical aromatics from catalytic pyrolysis of WPP mixture and composites were higher than those of the calculated values of poplar wood and PP catalytic pyrolysis individually, indicating that a

Validation Results for Core-Scale Oil Shale Pyrolysis

Energy Technology Data Exchange (ETDEWEB)

Staten, Josh; Tiwari, Pankaj

2015-03-01

This report summarizes a study of oil shale pyrolysis at various scales and the subsequent development a model for in situ production of oil from oil shale. Oil shale from the Mahogany zone of the Green River formation was used in all experiments. Pyrolysis experiments were conducted at four scales, powdered samples (100 mesh) and core samples of 0.75”, 1” and 2.5” diameters. The batch, semibatch and continuous flow pyrolysis experiments were designed to study the effect of temperature (300°C to 500°C), heating rate (1°C/min to 10°C/min), pressure (ambient and 500 psig) and size of the sample on product formation. Comprehensive analyses were performed on reactants and products - liquid, gas and spent shale. These experimental studies were designed to understand the relevant coupled phenomena (reaction kinetics, heat transfer, mass transfer, thermodynamics) at multiple scales. A model for oil shale pyrolysis was developed in the COMSOL multiphysics platform. A general kinetic model was integrated with important physical and chemical phenomena that occur during pyrolysis. The secondary reactions of coking and cracking in the product phase were addressed. The multiscale experimental data generated and the models developed provide an understanding of the simultaneous effects of chemical kinetics, and heat and mass transfer on oil quality and yield. The comprehensive data collected in this study will help advance the move to large-scale in situ oil production from the pyrolysis of oil shale.

Synergetic effect of sewage sludge and biomass co-pyrolysis: A combined study in thermogravimetric analyzer and a fixed bed reactor

International Nuclear Information System (INIS)

Wang, Xuebin; Deng, Shuanghui; Tan, Houzhang; Adeosun, Adewale; Vujanović, Milan; Yang, Fuxin; Duić, Neven

2016-01-01

Highlights: • The synergetic effect of sewage sludge and wheat straw co-pyrolysis was studied. • The mass balance measurement of gas, tar, and char was performed. • The synergetic effect shows strongest under a certain biomass addition ratio around 60%. • The required heat of co-pyrolysis is significantly reduced. - Abstract: Much attention has been given to the valuable products from the pyrolysis of sewage sludge. In this study, the pyrolysis of sewage sludge, biomass (wheat straw) and their mixtures in different proportions were carried out in a thermogravimetric analyzer (TGA) and fixed-bed reactor. The effects of pyrolysis temperature and percentage of wheat straw in wheat straw–sewage sludge mixtures on product distributions in terms of gas, liquid and char and the gas composition were investigated. Results indicate that there is a significantly synergetic effect during the co-pyrolysis processes of sewage sludge and wheat straw, accelerating the pyrolysis reactions. The synergetic effect resulted in an increase in gas and liquid yields but a decrease in char yield. The gas composition and the synergetic effect degree are strongly affected by the wheat straw proportions, and the strongest synergetic effect of sewage sludge and wheat straw co-pyrolysis appears at the biomass proportion of 60 wt.%. With an increase of temperature, the gas yield from the pyrolysis of sewage sludge increased but the liquid and char yields decreased. Moreover, the required heat of co-pyrolysis is significantly reduced compared with the pyrolysis of sewage sludge and wheat straw pyrolysis alone, because of the exothermic reactions between the ash components in two fuel samples.

Ionizing radiation effects in Acai oil analysed by gas chromatography coupled to mass spectrometry technique

International Nuclear Information System (INIS)

Valli, Felipe; Fernandes, Carlos Eduardo; Moura, Sergio; Machado, Ana Carolina; Furasawa, Helio Akira; Pires, Maria Aparecida Faustino; Bustillos, Oscar Vega

2007-01-01

The Acai fruit is a well know Brazilian seed plant used in large scale as a source of feed stock, specially in the Brazilian North-east region. The Acai oil is use in many purposes from fuel sources to medicine. The scope of this paper is to analyzed the chemical structures modification of the acai oil after the ionizing radiation. The radiation were set in the range of 10 to 25 kGy in the extracted Acai oil. The analyses were made by gas chromatography coupled to mass spectrometry techniques. A GC/MS Shimatzu QP-5000 equipped with 30 meters DB-5 capillary column with internal diameter of 0.25 mm and 0.25 μm film thickness was used. Helium was used as carried gas and gave a column head pressure of 12 p.s.i. (1 p.s.i. = 6894.76 Pa) and an average flux of 1 ml/min. The temperature program for the GC column consisted of a 4-minutes hold at 75 deg C, a 15 deg C /min ramp to 200 deg C, 8 minutes isothermal. 20 deg C/min ramp to 250 deg C, 2 minutes isothermal. The extraction of the fatty acids was based on liquid-liquid method using chloroform as solvent. The chromatograms resulted shows the presences of the oleic acid and others fatty acids identify by the mass spectra library (NIST-92). The ionization radiation deplete the fatty acids presents in the Acai oil. Details on the chemical qualitative analytical is present as well in this work. (author)

Flash pyrolysis of linseed (Linum usitatissimum L.) for production of liquid fuels

Energy Technology Data Exchange (ETDEWEB)

Acikgoz, C. [Department of Chemical Technology, Bilecik Higher Vocational School, GueluembeCampus, Anadolu University, 11030 Bilecik (Turkey); Kockar, O.M. [Department of Chemical Engineering, Faculty of Engineering and Architecture, iki Eyluel Campus, Anadolu University, 26470 Eskisehir (Turkey)

2007-03-15

Flash pyrolysis experiments of linseed (Linum usitatissimum L.) were performed in a tubular transport reactor at atmospheric pressure under nitrogen atmosphere. The effects of pyrolysis temperature and particle size on the yields of products were investigated with the sweep gas flow rate of 100 cm{sup 3} min{sup -1}. The temperature of pyrolysis and particle size were varied in the ranges 400-700 C and 0.6 mm < D{sub p} < 1.25 mm, 1.25 mm < D{sub p} < 1.8 mm, D{sub p} > 1.8 mm, respectively. The maximum oil yield of 68.8% was obtained at a pyrolysis temperature of 550 C, and the particle size of D{sub p} > 1.8 mm. The char and liquid product were analyzed to determine their elemental composition and calorific value. In particular, the chemical composition of the oil was investigated using chromatographic and spectroscopic techniques ({sup 1}H NMR, IR, column chromatography and GC). The chemical characterization has shown that the oil obtained from linseed can be used as a renewable fuel and chemical feedstock. (author)

Extending the range of compounds amenable for gas chromatography-mass spectrometric analysis.

Science.gov (United States)

Fialkov, Alexander B; Gordin, Alexander; Amirav, Aviv

2003-04-04

Gas chromatography-mass spectrometry (GC-MS) suffers from a major limitation in that an expanding number of thermally labile or low volatility compounds of interest are not amenable for analysis. We found that the elution temperatures of compounds from GC can be significantly lowered by reducing the column length, increasing the carrier gas flow rate, reducing the capillary column film thickness and lowering the temperature programming rate. Pyrene is eluted at 287 degrees C in standard GC-MS with a 30 m x 0.25 mm I.D. column with 1-microm DB5ms film and 1-ml/min He column flow rate. In contrast, pyrene is eluted at 79 degrees C in our "Supersonic GC-MS" system using a 1 m x 0.25 mm I.D. column with 0.1-microm DB5ms film and 100-ml/min He column flow rate. A simple model has been invoked to explain the significantly (up to 208 degrees C) lower elution temperatures observed. According to this model, every halving of the temperature programming rate, or number of separation plates (either through increased flow rate or due to reduced column length), results in approximately 20 degrees C lower elution temperature. These considerably lower elution temperatures enable the analysis of an extended range of thermally labile and low volatility compounds, that otherwise could not be analyzed by standard GC-MS. We demonstrate the analysis of large polycyclic aromatic hydrocarbons (PAHs) such as decacyclene with ten fused rings, well above the current GC limit of PAHs with six rings. Even a metalloporphirin such as magnesiumoctaethylporphin was easily analyzed with elution temperatures below 300 degrees C. Furthermore, a range of thermally labile compounds were analyzed including carbamates such as methomyl, aldicarb, aldicarbsulfone and oxamyl, explosives such as pentaerythritol tetranitrate, Tetryl and HMX, and drugs such as reserpine (608 a.m.u.). Supersonic GC-MS was used, based on the coupling of a supersonic molecular beam (SMB) inlet and ion sources with a bench

Normalization of natural gas composition data measured by gas chromatography

International Nuclear Information System (INIS)

Milton, Martin J T; Harris, Peter M; Brown, Andrew S; Cowper, Chris J

2009-01-01

The composition of natural gas determined by gas chromatography is routinely used as the basis for calculating physico-chemical properties of the gas. Since the data measured by gas chromatography have particular statistical properties, the methods used to determine the composition can make use of a priori assumptions about the statistical model for the data. We discuss a generalized approach to determining the composition, and show that there are particular statistical models for the data for which the generalized approach reduces to the widely used method of post-normalization. We also show that the post-normalization approach provides reasonable estimates of the composition for cases where it cannot be shown to arise rigorously from the statistical structure of the data

Modelling solid-convective flash pyrolysis of straw and wood in the Pyrolysis Centrifuge Reactor

DEFF Research Database (Denmark)

Bech, Niels; Larsen, Morten Boberg; Jensen, Peter Arendt

2009-01-01

in the Pyrolysis Centrifuge Reactor, a novel solid-convective flash pyrolysis reactor. The model relies on the original concept for ablative pyrolysis of particles being pyrolysed through the formation of an intermediate liquid compound which is further degraded to form liquid organics, char, and gas. To describe...

delta 13C analyses of vegetable oil fatty acid components, determined by gas chromatography--combustion--isotope ratio mass spectrometry, after saponification or regiospecific hydrolysis.

Science.gov (United States)

Woodbury, S E; Evershed, R P; Rossell, J B

1998-05-01

The delta 13C values of the major fatty acids of several different commercially important vegetable oils were measured by gas chromatography--combustion--isotope ratio mass spectrometry. The delta 13C values obtained were found to fall into two distinct groups, representing the C3 and C4 plants classes from which the oils were derived. The delta 13C values of the oils were measured by continuous flow elemental isotope ratio mass spectrometry and were found to be similar to their fatty acids, with slight differences between individual fatty acids. Investigations were then made into the influence on the delta 13C values of fatty acids of the position occupied on the glycerol backbone. Pancreatic lipase was employed to selectively hydrolyse fatty acids from the 1- and 3-positions with the progress of the reaction being followed by high-temperature gas chromatography in order to determine the optimum incubation time. The 2-monoacylglycerols were then isolated by thin-layer chromatography and fatty acid methyl esters prepared. The delta 13C values obtained indicate that fatty acids from any position on the glycerol backbone are isotopically identical. Thus, whilst quantification of fatty acid composition at the 2-position and measurement of delta 13C values of oils and their major fatty acids are useful criteria in edible oil purity assessment, measurement of delta 13C values of fatty acids from the 2-position does not assist with oil purity assignments.

Use of electron ionization and atmospheric pressure chemical ionization in gas chromatography coupled to time-of-flight mass spetrometry for screening and identification of organic pollutants in waters

NARCIS (Netherlands)

Portoles, T.; Mol, J.G.J.; Sancho, J.V.; Hernandez, F.

2014-01-01

A new approach has been developed for multiclass screening of organic contaminants in water based on the use of gas chromatography coupled to hybrid quadrupole high-resolution time-of-flight mass spectrometry with atmospheric pressure chemical ionization (GC–(APCI)QTOF MS). The soft ionization

Precipitation and valorisation of lignin obtained from South African Kraft mill black liquor

CSIR Research Space (South Africa)

Namane, Mpho

2016-04-01

Full Text Available (NMR), size exclusion chromatography (SEC), and pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS). SEC data revealed a narrow molecular weight distribution with a small polydispersity index in the lignin sample – all desirable features...

CFD analysis of combustion of natural gas and syngas from biomass pyrolysis in the combustion chamber of a micro gas turbine

Energy Technology Data Exchange (ETDEWEB)

Fantozzi, Francesco; Laranci, Paolo; D' Alessandro, Bruno [University of Perugia (DII/UNIPG) (Italy). Dept. of Industrial Engineering], Emails: fanto@unipg.it, paolo.laranci@unipg.it, dalessandro@bio-net.it

2009-07-01

Micro gas turbines (MGT) can be profitably used for the production of distributed energy (DE), with the possibility to use gaseous fuels with low BTU derived from biomass or waste through the pyrolysis or gasification processes. These synthesis gases (SG) show significant differences with respect to natural gas (NG), in terms of composition, calorific value, content of hydrogen, tar and particulate matter content; such differences can be turn into problems of ignition, instability burning, difficulties in controlling the emissions and fouling. CFD analysis of the combustion process is an essential tool for identifying the main critical arising in using these gases, in order to modify existing geometries and to develop new generation of combustor for use with low BTU gases. This paper describes the activities of experimental and numerical analysis carried out to study the combustion process occurring inside an existing annular Rich-Quench-Lean (RQL) Combustion Chamber (CC) of a 80 kW MGT. In the paper some results of a CFD study of the combustion process performed with an original developed chemical models are reported in terms of temperature and velocity distributions inside the CC and in terms of compositions of turbine inlet gas and of its thermodynamic parameters (mass flow, temperature, pressure). An evaluation of pollutant emissions of CO, CO{sub 2} and NOx and a comparison with the available experimental data relating to the case of combustion of NG is also provided in the paper. Moreover, the carried out investigation concerns the case of operation with a SG fuel derived from biomass in an Integrated Pyrolysis Regenerated Plant (IPRP). (author)

Potential pyrolysis pathway assessment for microalgae-based aviation fuel based on energy conversion efficiency and life cycle

International Nuclear Information System (INIS)

Guo, Fang; Wang, Xin; Yang, Xiaoyi

2017-01-01

Highlights: • High lipid content in microalgae increases energy conversion efficiency. • Indirect pathway has the highest mass ratio, energy ratio and energy efficiency. • The Isochrysis indirect pathway produces most kerosene component precursor. • The Isochrysis indirect pyrolysis pathway shows the best performance in LCA. - Abstract: Although the research of microalgae pyrolysis has been conducted for many years, there is a lack of investigations on energy efficiency and life cycle assessment. In this study, we investigated the biocrude yield and energy efficiency of direct pyrolysis, microalgae residue pyrolysis after lipid extraction (indirect pyrolysis), and different microalgae co-pyrolysis. This research also investigated the life cycle assessment of the three different pyrolysis pathways. A system boundary of Well-to-Wake (WTWa) was defined and included sub-process models, such as feedstock production, fuel production and pump-to-wheels (PTW) stages. The pathway of Isochrysis indirect pyrolysis shows the best performance in the mass ratio and energy ratio, produces the most kerosene component precursor, has the lowest WTWa total energy input, fossil fuel consumption and greenhouse gas emissions, and resultes in the best energy efficiency. All the evidence indicates that Isochrysis R2 pathway is a potential and optimal pyrolysis pathway to liquid biofuels. The mass ratio of pyrolysis biocrude is shown to be the decisive factor for different microalgae species. The sensitivity analysis results also indicates that the life cycle indicators are particularly sensitive to the mass ratio of pyrolysis biocrude for microalgae-based hydrotreated pyrolysis aviation fuel.

[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.

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.

Use of [18O4] phosphoric acid in the quantitation of phosphate by gas-liquid chromatography-mass spectrometry analysis

International Nuclear Information System (INIS)

Graff, G.; Krick, T.P.; Walseth, T.F.; Goldberg, N.D.

1980-01-01

A procedure is described to quantitate inorganic phosphate in the form of the tris(trimethylsilyl) (TMS) phosphate by gas-liquid chromatography-mass spectrometry (glc-ms) that increases the previously reported detection limit from the microgram to the nanogram range. The sensitivity for detecting TMS-phosphate by glc-ms analysis was shown to be limited by an increasing fractional loss with decreasing concentrations of TMS-phosphate analyzed due to its adsorption on different types of glc column supports. The method developed employs [ 18 O 4 ] phosphoric acid which serves as both an internal standard to permit quantitation and as a carrier to minimize sample adsorption on the glc column support

Kinetic study and syngas production from pyrolysis of forestry waste

International Nuclear Information System (INIS)

Hu, Mian; Wang, Xun; Chen, Jian; Yang, Ping; Liu, Cuixia; Xiao, Bo; Guo, Dabin

2017-01-01

Highlights: • Pyrolysis process can be divided into three stages using differential DTG method. • A modified discrete DAEM model fitted experimental data well. • Fe/biochar catalyst showed a good performance on catalytic reforming process. - Abstract: Kinetic study and syngas production from pyrolysis of forestry waste (pine sawdust (PS)) were investigated using a thermogravimetric analyzer (TGA) and a fixed-bed reactor, respectively. In TGA, it was found that the pyrolysis of PS could be divided into three stages and stage II was the major mass reduction stage with mass loss of 73–74%. The discrete distributed activation energy model (DAEM) with discrete 200 first-order reactions was introduced to study the pyrolysis kinetic. The results indicated that the DAEM with 200 first-order reactions could approximate the pyrolysis process with an excellent fit between experimental and calculated data. The apparent activation energies of PS ranged from 147.86 kJ·mol −1 to 395.76 kJ·mol −1 , with corresponding pre-exponential factors of 8.30 × 10 13 s −1 to 3.11 × 10 25 s −1 . In the fixed-bed reactor, char supported iron catalyst was prepared for tar cracking. Compared with no catalyst which the gas yield and tar yield were 0.58 N m 3 /kg biomass and 201.23 g/kg biomass, the gas yield was markedly increased to 1.02 N m 3 /kg biomass and the tar yield was decreased to only 26.37 g/kg biomass in the presence of char supported iron catalyst. These results indicated that char supported iron catalyst could potentially be used to catalytically decompose tar molecules in syngas generated via biomass pyrolysis.

Vinegar Metabolomics: An Explorative Study of Commercial Balsamic Vinegars Using Gas Chromatography-Mass Spectrometry

Directory of Open Access Journals (Sweden)

Farhana R. Pinu

2016-07-01

Full Text Available Balsamic vinegar is a popular food condiment produced from cooked grape must by two successive fermentation (anaerobic and aerobic processes. Although many studies have been performed to determine the composition of major metabolites, including sugars and aroma compounds, no study has been undertaken yet to characterize the comprehensive metabolite composition of balsamic vinegars. Here, we present the first metabolomics study of commercial balsamic vinegars by gas chromatography coupled to mass spectrometry (GC-MS. The combination of three GC-MS methods allowed us to detect >1500 features in vinegar samples, of which 123 metabolites were accurately identified, including 25 amino acids, 26 carboxylic acids, 13 sugars and sugar alcohols, four fatty acids, one vitamin, one tripeptide and over 47 aroma compounds. Moreover, we identified for the first time in vinegar five volatile metabolites: acetin, 2-methylpyrazine, 2-acetyl-1-pyroline, 4-anisidine and 1,3-diacetoxypropane. Therefore, we demonstrated the capability of metabolomics for detecting and identifying large number of metabolites and some of them could be used to distinguish vinegar samples based on their origin and potentially quality.

Optimization of focused ultrasonic extraction of propellant components determined by gas chromatography/mass spectrometry.

Science.gov (United States)

Fryš, Ondřej; Česla, Petr; Bajerová, Petra; Adam, Martin; Ventura, Karel

2012-09-15

A method for focused ultrasonic extraction of nitroglycerin, triphenyl amine and acetyl tributyl citrate presented in double-base propellant samples following by the gas chromatography/mass spectrometry analysis was developed. A face-centered central composite design of the experiments and response surface modeling was used for optimization of the time, amplitude and sample amount. The dichloromethane was used as the extractant solvent. The optimal extraction conditions with respect to the maximum yield of the lowest abundant compound triphenyl amine were found at the 20 min extraction time, 35% amplitude of ultrasonic waves and 2.5 g of the propellant sample. The results obtained under optimal conditions were compared with the results achieved with validated Soxhlet extraction method, which is typically used for isolation and pre-concentration of compounds from the samples of explosives. The extraction yields for acetyl tributyl citrate using both extraction methods were comparable; however, the yield of ultrasonic extraction of nitroglycerin and triphenyl amine was lower than using Soxhlet extraction. The possible sources of different extraction yields are estimated and discussed. Copyright © 2012 Elsevier B.V. All rights reserved.

Simultaneous Determination of Alkoxyalcohols in Wet Wipes Using Static Headspace Gas Chromatography and Mass Spectrometry

Energy Technology Data Exchange (ETDEWEB)

Lee, So Jin; Pyo, Hee Soo; Chung, Bong Chul; Lee, Jeon Gae [KIST, Seoul (Korea, Republic of); Kim, Hai Dong [Kyung Hee University, Seoul (Korea, Republic of)

2014-09-15

Alkoxyalcohols are used as solvents or preservatives in various consumer products such as wet wipes. The metabolites of alkoxyalcohols are known to be chronically toxic and carcinogenic to animals. Thus, an analytical method is needed to monitor alkoxyalcohols in wet wipes. The aim of this study was to develop a simultaneous analytical method for 14 alkoxyalcohols using headspace gas chromatography coupled with mass spectrometry to analyze the wet wipes. This method was developed by comparing with various headspace extraction parameters. The linear calibration curves were obtained for the method (r2 > 0.995). The limit of detection of alkoxyalcohols ranged from 2 to 200 ng mL-1. The precision of the determinative method was less than 18.20% coefficient of variation both intra and inter days. The accuracy of the method ranged from 82.86% to 119.83%. (2-Methoxymethylethoxy)propanol, 2-phenoxyethanol, and 1-phenoxy-2-propanol were mainly detected in wet wipes.

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

Determination of long-chain fatty acids in serum by gas chromatography coupled to mass spectrometry

International Nuclear Information System (INIS)

Nuevas Paz, Lauro; Camayd Viera, Ivette

2014-01-01

The quantification of long-chain fatty acids is fundamental for the diagnosis of several peroxisome disorders, particularly those in which the β-oxidation peroxisome of fatty acids is affected. In this work the implementation of an analytical method for the determination of these markers in serum by gas chromatography coupled to mass spectrometry is described. Besides, samples from patients with a diagnostic impression of adrenoleukodystrophy linked to the X chromosome were analyzed. The necessary experimental conditions were achieved for the separation and quantification of C22:0, C24:0 and C26:0 fatty acids in serum, which are biochemical markers of various peroxisome diseases. The application of this method allowed confirming the diagnosis of three patients with a diagnostic impression of adrenoleukodystrophy linked to the X chromosome. The application of the method in daily practice will allow the Cuban medical system to count on a new laboratory parameter for the diagnosis of peroxisome disorders

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.

Monitoring the behaviour of 4-ketocyclophosphamide versus cyclophosphamide during capillary gas chromatography by mass spectrometry

NARCIS (Netherlands)

Bruijn, de E.A.; Oosterom, van A.T.; Leclercq, P.A.; Haan, de J.W.; Ven, van de L.J.M.; Tjaden, U.R.

1987-01-01

Capillary Gas Chromatography (CGC) is capable of determining underivatized cyclophosphamide (CPA) using SCOT OV 275 columns. Then CPA is subjected to in situ degradation resulting in formation of a cyclization product which can be determined selectively in biological fluids. In routine bioanalysis

[Target and non-target screening of volatile organic compounds in industrial exhaust gas using thermal desorption-gas chromatography-mass spectrometry].

Science.gov (United States)

Ma, Huilian; Jin, Jing; Li, Yun; Chen, Jiping

2017-10-08

A method of comprehensive screening of the target and non-target volatile organic compounds (VOCs) in industrial exhaust gas using thermal desorption-gas chromatography-mass spectrometry (TD-GC-MS) has been developed. In this paper, two types of solid phase adsorption column were compared, and the Tenex SS TD Tube was selected. The analytes were enriched into the adsorption tube by constant flow sampling, and detected by TD-GC-MS in full scan mode. Target compounds were quantified by internal standard method, and the quantities of non-target compounds were calculated by response coefficient of toluene. The method detection limits (MDLs) for the 24 VOCs were 1.06 to 5.44 ng, and MDLs could also be expressed as 0.004 to 0.018 mg/m 3 assuming that the sampling volume was 300 mL. The average recoveries were in the range of 78.4% to 89.4% with the relative standard deviations (RSDs) of 3.9% to 14.4% ( n =7). The established analytical method was applied for the comprehensive screening of VOCs in a waste incineration power plant in Dalian city. Twenty-nine VOCs were identified. In these compounds, only five VOCs were the target compounds set in advance, which accounted for 26.7% of the total VOCs identified. Therefore, this study further proved the importance of screening non-target compounds in the analysis of VOCs in industrial exhaust gas, and has certain reference significance for the complete determination of VOCs distribution.

Detection of radiation-induced hydrocarbons in Camembert irradiated before and after the maturing process-comparison of florisil column chromatography and on-line coupled liquid chromatography-gas chromatography

International Nuclear Information System (INIS)

Schulzki, G.; Spiegelberg, A.; Bögl, K.W.; Schreiber, G.A.

1995-01-01

The influence of the maturing process on the detection of radiation-induced volatile hydrocarbons in the fat of Camembert has been investigated. Two analytical methods for separation of the hydrocarbon fraction from the lipid were applied: Florisil column chromatography with subsequent gas chromatographic-mass spectrometric (GC-MS) determination as well as on-line coupled liquid chromatography-GC-MS. The maturing process had no influence on the detection of radiation-induced volatiles. Comparable results were achieved with both analytical methods. However, preference is given to the more effective on-line coupled LC-GC method

ENVIRONMENTAL ANALYSIS BY AB INITIO QUANTUM MECHANICAL COMPUTATION AND GAS CHROMATOGRAPHY/FOURIER TRANSFORM INFRARED SPECTROMETRY.

Science.gov (United States)

Computational chemistry, in conjunction with gas chromatography/mass spectrometry/Fourier transform infrared spectrometry (GC/MS/FT-IR), was used to tentatively identify seven tetrachlorobutadiene (TCBD) isomers detected in an environmental sample. Computation of the TCBD infrare...

Microwave pyrolysis using self-generated pyrolysis gas as activating agent: An innovative single-step approach to convert waste palm shell into activated carbon

Science.gov (United States)

Yek, Peter Nai Yuh; Keey Liew, Rock; Shahril Osman, Mohammad; Chung Wong, Chee; Lam, Su Shiung

2017-11-01

Waste palm shell (WPS) is a biomass residue largely available from palm oil industries. An innovative microwave pyrolysis method was developed to produce biochar from WPS while the pyrolysis gas generated as another product is simultaneously used as activating agent to transform the biochar into waste palm shell activated carbon (WPSAC), thus allowing carbonization and activation to be performed simultaneously in a single-step approach. The pyrolysis method was investigated over a range of process temperature and feedstock amount with emphasis on the yield and composition of the WPSAC obtained. The WPSAC was tested as dye adsorbent in removing methylene blue. This pyrolysis approach provided a fast heating rate (37.5°/min) and short process time (20 min) in transforming WPS into WPSAC, recording a product yield of 40 wt%. The WPSAC was detected with high BET surface area (≥ 1200 m2/g), low ash content (< 5 wt%), and high pore volume (≥ 0.54 cm3/g), thus recording high adsorption efficiency of 440 mg of dye/g. The desirable process features (fast heating rate, short process time) and the recovery of WPSAC suggest the exceptional promise of the single-step microwave pyrolysis approach to produce high-grade WPSAC from WPS.

Bio-oil production through pyrolysis of blue-green algae blooms (BGAB): Product distribution and bio-oil characterization

International Nuclear Information System (INIS)

Hu, Zhiquan; Zheng, Yang; Yan, Feng; Xiao, Bo; Liu, Shiming

2013-01-01

Pyrolysis experiments of blue-green algae blooms (BGAB) were carried out in a fixed-bed reactor to determine the effects of pyrolysis temperature, particle size and sweep gas flow rate on pyrolysis product yields and bio-oil properties. The pyrolysis temperature, particle size and sweep gas flow rate were varied in the ranges of 300–700 °C, below 0.25–2.5 mm and 50–400 mL min −1 , respectively. The maximum oil yield of 54.97% was obtained at a pyrolysis temperature of 500 °C, particle size below 0.25 mm and sweep gas flow rate of 100 mL min −1 . The elemental analysis and calorific value of the oil were determined, and the chemical composition of the oil was investigated using gas chromatography–mass spectroscopy (GC–MS) technique. The analysis of bio-oil composition showed that bio-oil from BGAB could be a potential source of renewable fuel with a heating value of 31.9 MJ kg −1 . - Highlights: ► Bio-oil production from pyrolysis of blue-green algae blooms in fixed bed reactor. ► Effects of pyrolysis conditions on product distribution were investigated. ► The maximum bio-oil yield reached 54.97 wt %. ► The bio-oil has high heating value and may be suitable as renewable fuel. ► Pyrolysis of algal biomass beneficial for energy recovery, eutrophication control

Analysis and comparison of biomass pyrolysis/gasification condensates: Final report

Energy Technology Data Exchange (ETDEWEB)

Elliott, D.C.

1986-06-01

This report provides results of chemical and physical analysis of condensates from eleven biomass gasification and pyrolysis systems. The samples were representative of the various reactor configurations being researched within the Department of Energy, Biomass Thermochemical Conversion program. The condensates included tar phases and aqueous phases. The analyses included gross compositional analysis (elemental analysis, ash, moisture), physical characterization (pour point, viscosity, density, heat of combustion, distillation), specific chemical analysis (gas chromatography/mass spectrometry, infrared spectrophotometry, proton and carbon-13 nuclear magnetic resonance spectrometry) and biological activity (Ames assay and mouse skin tumorigenicity tests). These results are the first step of a longer term program to determine the properties, handling requirements, and utility of the condensates recovered from biomass gasification and pyrolysis. The analytical data demonstrates the wide range of chemical composition of the organics recovered in the condensates and suggests a direct relationship between operating temperature and chemical composition of the condensates. A continuous pathway of thermal degradation of the tar components as a function of temperature is proposed. Variations in the chemical composition of the organic components in the tars are reflected in the physical properties of tars and phase stability in relation to water in the condensate. The biological activity appears to be limited to the tars produced at high temperatures. 56 refs., 25 figs., 21 tabs.

Direct chemical-analysis of uv laser-ablation products of organic polymers by using selective ion monitoring mode in gas-chromatography mass-spectrometry

Science.gov (United States)

Cho, Yirang; Lee, H.W.; Fountain, S.T.; Lubman, D.M.

1994-01-01

Trace quantities of laser ablated organic polymers were analyzed by using commercial capillary column gas chromatography/mass spectrometry; the instrument was modified so that the laser ablation products could be introduced into the capillary column directly and the constituents of each peak in the chromatogram were identified by using a mass spectrometer. The present study takes advantage of the selective ion monitoring mode for significantly improving the sensitivity of the mass spectrometer as a detector, which is critical in analyzing the trace quantities and confirming the presence or absence of the species of interest in laser ablated polymers. The initial composition of the laser ablated polymers was obtained by using an electron impact reflectron time-of-flight mass spectrometer and the possible structure of the fragments observed in the spectra was proposed based on the structure of the polymers.

Comparison of ultra high performance supercritical fluid chromatography, ultra high performance liquid chromatography, and gas chromatography for the separation of synthetic cathinones.

Science.gov (United States)

Carnes, Stephanie; O'Brien, Stacey; Szewczak, Angelica; Tremeau-Cayel, Lauriane; Rowe, Walter F; McCord, Bruce; Lurie, Ira S

2017-09-01

A comparison of ultra high performance supercritical fluid chromatography, ultra high performance liquid chromatography, and gas chromatography for the separation of synthetic cathinones has been conducted. Nine different mixtures of bath salts were analyzed in this study. The three different chromatographic techniques were examined using a general set of controlled synthetic cathinones as well as a variety of other synthetic cathinones that exist as positional isomers. Overall 35 different synthetic cathinones were analyzed. A variety of column types and chromatographic modes were examined for developing each separation. For the ultra high performance supercritical fluid chromatography separations, analyses were performed using a series of Torus and Trefoil columns with either ammonium formate or ammonium hydroxide as additives, and methanol, ethanol or isopropanol organic solvents as modifiers. Ultra high performance liquid chromatographic separations were performed in both reversed phase and hydrophilic interaction chromatographic modes using SPP C18 and SPP HILIC columns. Gas chromatography separations were performed using an Elite-5MS capillary column. The orthogonality of ultra high performance supercritical fluid chromatography, ultra high performance liquid chromatography, and gas chromatography was examined using principal component analysis. For the best overall separation of synthetic cathinones, the use of ultra high performance supercritical fluid chromatography in combination with gas chromatography is recommended. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of some volatile compounds in alcoholic beverage by headspace solid-phase microextraction gas chromatography - mass spectrometry

Science.gov (United States)

Schmutzer, G.; Avram, V.; Feher, I.; David, L.; Moldovan, Z.

2012-02-01

The volatile composition of alcoholic beverage was studied by headspace solid-phase microextraction (HSSPME) method and gas chromatography - mass spectrometry (GC-MS). Some volatile compounds, such as alcohols, esters, terpenes and other are mainly responsible for the flavor of fortified wines and their amounts specify the quality of the alcoholic beverages. From this perspective it is interesting to develop a rapid, selective and sensitive analytical method suitable for simultaneous quantification of the main molecules being responsible for the organoleptic characteristic of alcoholic beverages. Vermouth fortified drink was analyzed in order to characterize the volatile profile. Using the HS-SPME/GC-MS a number of twenty-six volatile compounds from a commercial market alcoholic beverage were identified. The most abundant compounds were m-thymol, o-thymol and eugenol, alongside of the ethyl ester compounds.

Coupling of gas chromatography and electrospray ionization high resolution mass spectrometry for the analysis of anabolic steroids as trimethylsilyl derivatives in human urine.

Science.gov (United States)

Cha, Eunju; Jeong, Eun Sook; Cha, Sangwon; Lee, Jaeick

2017-04-29

In this study, gas chromatography (GC) was interfaced with high resolution mass spectrometry (HRMS) with electrospray ionization source (ESI) and the relevant parameters were investigated to enhance the ionization efficiency. In GC-ESI, the distances (x-, y- and z) and angle between the ESI needle, GC capillary column and MS orifice were set to 7 (x-distance), 4 (y-distance), and 1 mm (z-distance). The ESI spray solvent, acid modifier and nebulizer gas flow were methanol, 0.1% formic acid and 5 arbitrary units, respectively. Based on these results, analytical conditions for GC-ESI/HRMS were established. In particular, the results of spray solvent flow indicated a concentration-dependent mechanism (peak dilution effect), and other parameters also greatly influenced the ionization performance. The developed GC-ESI/HRMS was then applied to the analysis of anabolic steroids as trimethylsilyl (TMS) derivatives in human urine to demonstrate its application. The ionization profiles of TMS-derivatized steroids were investigated and compared with those of underivatized steroids obtained from gas chromatography-electrospray ionization/mass spectrometry (GC-ESI/MS) and liquid chromatography-electrospray ionization/mass spectrometry (LC-ESI/MS). The steroids exhibited ionization profiles based on their structural characteristics, regardless of the analyte phase or derivatization. Groups I and II with conjugated or unconjugated keto functional groups at C3 generated the [M+H] + and [M+H-TMS] + ions, respectively. On the other hand, Groups III and IV gave rise to the characteristic fragment ions [M+H-TMS-H 2 O] + and [M+H-2TMS-H 2 O] + , corresponding to loss of a neutral TMS·H 2 O moiety from the protonated molecular ion by in-source dissociation. To the best of our knowledge, this is the first study to successfully ionize and analyze steroids as TMS derivatives using ESI coupled with GC. The present system has enabled the ionization of TMS derivatives under ESI conditions

Data on acetic acid–methanol–methyl acetate–water mixture analysised by dual packed column Gas Chromatography

Directory of Open Access Journals (Sweden)

Mallaiah Mekala

2018-06-01

Full Text Available The composition of multicomponent determination by colorimetric titration is difficult. This complexity is easily overcome by using Gas Chromatography technique instead of wet method for multi-component mixture analysis. In Gas Chromatography, first the standard chart is prepared by using the known amount sample concentration as the reference. Once calibration chart is prepared the unknown sample concentration easily measured by using the standard chart. In the present study a standard calibration chart developed for the four component system of acetic acid–methanol–methyl acetate–water. The samples were taken at various concentrations of all components and different chromatograms obtained under various concentrations respectively. The method of optimization was first carried out to get the sharp peaks of individual components and binary pairs also. By using those conditions, the multi components concentrations were estimated. From the present results, the area under gas chromatogram is linearly varying with mole% of the components compared to mass%. Keywords: Gas Chromatography, Esterification, Calibration, Retention time, Optimization

[Determination of iodine and its species in plant samples using ion chromatography-inductively coupled plasma mass spectrometry].

Science.gov (United States)

Lin, Li; Chen, Guang; Chen, Yuhong

2011-07-01

A method was established for the determination of iodine and its species in plant samples using ion chromatography-inductively coupled plasma mass spectrometry (IC-ICP/ MS). Alkaline extraction and IC-ICP/MS were applied as the sample pre-treatment method and the detection technique respectively, for iodate and iodide determination. Moreover, high-temperature pyrolysis absorption was adopted as the pre-treatment method for total iodine analysis, which finally converted all the iodine species into iodide and measured the iodide by IC-ICP/MS. The recoveries of iodine for alkaline extraction and high-temperature pyrolysis absorption were 89.6%-97.5% and 95.2%-111.2%, respectively. The results were satisfactory. The detection limit of iodine was 0.010 mg/kg. The iodine and its speciation contents in several kinds of plant samples such as seaweeds, kelp, cabbage, tea leaf and spinach were investigated. It was shown that the iodine in seaweeds mainly existed as organic iodine; while the ones in kelp, cabbage, tea leaf and spinach mainly existed as inorganic iodine.

A low thermal mass fast gas chromatograph and its implementation in fast gas chromatography mass spectrometry with supersonic molecular beams.

Science.gov (United States)

Fialkov, Alexander B; Moragn, Mati; Amirav, Aviv

2011-12-30

A new type of low thermal mass (LTM) fast gas chromatograph (GC) was designed and operated in combination with gas chromatography mass spectrometry (GC-MS) with supersonic molecular beams (SMB), including GC-MS-MS with SMB, thereby providing a novel combination with unique capabilities. The LTM fast GC is based on a short capillary column inserted inside a stainless steel tube that is resistively heated. It is located and mounted outside the standard GC oven on its available top detector port, while the capillary column is connected as usual to the standard GC injector and supersonic molecular beam interface transfer line. This new type of fast GC-MS with SMB enables less than 1 min full range temperature programming and cooling down analysis cycle time. The operation of the fast GC-MS with SMB was explored and 1 min full analysis cycle time of a mixture of 16 hydrocarbons in the C(10)H(22) up to C(44)H(90) range was achieved. The use of 35 mL/min high column flow rate enabled the elution of C(44)H(90) in less than 45 s while the SMB interface enabled splitless acceptance of this high flow rate and the provision of dominant molecular ions. A novel compound 9-benzylazidanthracene was analyzed for its purity and a synthetic chemistry process was monitored for the optimization of the chemical reaction yield. Biodiesel was analyzed in jet fuel (by both GC-MS and GC-MS-MS) in under 1 min as 5 ppm fatty acid methyl esters. Authentic iprodion and cypermethrin pesticides were analyzed in grapes extract in both full scan mode and fast GC-MS-MS mode in under 1 min cycle time and explosive mixture including TATP, TNT and RDX was analyzed in under 1 min combined with exhibiting dominant molecular ion for TATP. Fast GC-MS with SMB is based on trading GC separation for speed of analysis while enhancing the separation power of the MS via the enhancement of the molecular ion in the electron ionization of cold molecules in the SMB. This paper further discusses several features of

Modelling and experimental investigation of waste tyre pyrolysis process in a laboratory reactor

Directory of Open Access Journals (Sweden)

Rudniak Leszek

2017-09-01

Full Text Available A mathematical model of waste tyre pyrolysis process is developed in this work. Tyre material decomposition based on a simplified reaction mechanism leads to main product lumps: noncondensable (gas, condensable (pyrolytic oil and solid (char. The model takes into account kinetics of heat and mass transfer in the grain of the shredded rubber material as well as surrounding gas phase. The main reaction routes were modelled as the pseudo-first order reactions with a rate constant calculated from the Arrhenius type equation using literature values of activation energy determined for main tyre constituents based on TG/DTG measurements and tuned pre-exponential parameter values obtained by fitting theoretical predictions to the experimental results obtained in our laboratory reactor. The model was implemented within the CFD software (ANSYS Fluent. The results of numerical simulation of the pyrolysis process revealed non-uniformity of sample’s porosity and temperature. The simulation predictions were in satisfactory agreement with the experimentally measured mass loss of the tyre sample during pyrolysis process investigated in a laboratory reactor.

Gas chromatography/multiphoton ionization/time-of-flight mass spectrometry of polychlorinated biphenyls

International Nuclear Information System (INIS)

Matsui, Taiki; Uchimura, Tomohiro; Imasaka, Totaro

2011-01-01

A sample mixture of polychlorinated biphenyls (PCBs) was measured by gas chromatography/multiphoton ionization/time-of-flight mass spectrometry (GC/MPI/TOF-MS) using four types of laser sources. When a fourth harmonic emission (266 nm) of a picosecond Nd:YAG laser (1064 nm) was utilized, highly chlorinated PCBs larger than hepta-CBs were not observed. A fifth harmonic emission (213 nm) of the picosecond Nd:YAG laser allowed the measurement of PCBs from di-CBs to octa-CBs, and the limit of detection (LOD) was several pg for each component of PCBs. The LOD for the total amount of PCBs, which was calculated using the protocol provided by the Ministry of the Environment, Japan, was 1000 pg. The signal intensity of the congeners with chlorine atoms at the ortho positions (non-coplanar PCBs) was enhanced by using the fifth harmonic emission. When the fourth harmonic emission remaining after fifth harmonic generation was simultaneously used, the LOD for total PCBs was improved to 667 pg. The PCB sample was also measured using a third harmonic emission (267 nm) of a femtosecond Ti:sapphire laser (800 nm), providing an LOD of 677 pg. Thus, the two-color beam (266/213 nm) of a picosecond Nd:YAG laser had a comparable, or even slightly superior, performance to the more expensive femtosecond Ti:sapphire laser.

Environmental application of elemental speciation analysis based on liquid or gas chromatography hyphenated to inductively coupled plasma mass spectrometry-A review

International Nuclear Information System (INIS)

Popp, Maximilian; Hann, Stephan; Koellensperger, Gunda

2010-01-01

In recent years the number of environmental applications of elemental speciation analysis using inductively coupled plasma mass spectrometry (ICP-MS) as detector has increased significantly. The analytical characteristics, such as extremely low detection limits (LOD) for almost all elements, the wide linear range, the possibility for multi-elemental analysis and the possibility to apply isotope dilution mass spectrometry (IDMS) make ICP-MS an attractive tool for elemental speciation analysis. Two methodological approaches, i.e. the combination of ICP-MS with high performance liquid chromatography (HPLC) and gas chromatography (GC), dominate the field. Besides the investigation of metals and metalloids and their species (e.g. Sn, Hg, As), representing 'classic' elements in environmental science, more recently other elements (e.g. P, S, Br, I) amenable to ICP-MS determination were addressed. In addition, the introduction of isotope dilution analysis and the development of isotopically labeled species-specific standards have contributed to the success of ICP-MS in the field. The aim of this review is to summarize these developments and to highlight recent trends in the environmental application of ICP-MS coupled to GC and HPLC.

Gas chromatography

International Nuclear Information System (INIS)

Cram, S.P.; Risby, T.H.; Field, L.R.; Yu, W.L.

1980-01-01

In addition to the published literature for the years 1978 - 79, this review of developments in the field of gas chromatography includes earlier articles of particular significance appearing in foreign journals and the patent literature which was not available at the time of the previous review. The articles cited were selected as presenting the most fundamental developments in theory, methodology, and instrumentation. Some applications are cited if they reflect an advance in the state-of-the-art or have particular relevance to new developments. 1149 references are cited

Terpenoid composition and botanical affinity of Cretaceous resins from India and Myanmar

Energy Technology Data Exchange (ETDEWEB)

Dutta, Suryendu; Mallick, Monalisa [Department of Earth Sciences, Indian Institute of Technology-Bombay (India); Kumar, Kishor [Wadia Institute of Himalayan Geology, Uttarakhand (India); Mann, Ulrich [Forschungzentrum Juelich (Germany). Institut fuer Chemie und Dynamik der Geosphaere; Greenwood, Paul F. [John De Laeter Mass Spectrometry and WA Biogeochemistry Centres (M090), University of Western Australia, Crawley (Australia)

2011-01-01

Fossil resins from the Cretaceous sediments of Meghalaya, India and Kachin, Myanmar (Burma) were analysed using Curie point pyrolysis-gas chromatography-mass spectrometry and thermochemolysis gas chromatography-mass spectrometry to help elucidate their botanical source. The major pyrolysis products and methyl-esterified thermochemolysis products of both the resins were abietane and labdane type diterpenoids with minor amount of sesquiterpenoids. The thermochemolysis products also included methyl-16,17-dinor callitrisate, methyl-16,17-dinor dehydroabietate and methyl-8-pimaren-18-oate - the latter two from just the Myanmarese resin. The exclusive presence of both labdane and abietane diterpenoids and the lack of phenolic terpenoids may suggest that the studied Cretaceous resins were derived from Pinaceae (pine family) conifers. (author)

Investigation of zinc recovery by hydrogen reduction assisted pyrolysis of alkaline and zinc-carbon battery waste.

Science.gov (United States)

Ebin, Burçak; Petranikova, Martina; Steenari, Britt-Marie; Ekberg, Christian

2017-10-01

Zinc (Zn) recovery from alkaline and zinc-carbon (Zn-C) battery waste were studied by a laboratory scale pyrolysis process at a reaction temperature of 950°C for 15-60min residence time using 5%H 2(g) -N 2(g) mixture at 1.0L/min gas flow rate. The effect of different cooling rates on the properties of pyrolysis residue, manganese oxide particles, were also investigated. Morphological and structural characterization of the produced Zn particles were performed. The battery black mass was characterized with respect to the properties and chemical composition of the waste battery particles. The thermodynamics of the pyrolysis process was studied using the HSC Chemistry 5.11 software. A hydrogen reduction reaction of the battery black mass (washed with Milli-Q water) takes place at the chosen temperature and makes it possible to produce fine Zn particles by rapid condensation following the evaporation of Zn from the pyrolysis batch. The amount of Zn that can be separated from the black mass increases by extending the residence time. Recovery of 99.8% of the Zn was achieved at 950°C for 60min residence time using 1.0L/min gas flow rate. The pyrolysis residue contains MnO and Mn 2 O 3 compounds, and the oxidation state of manganese can be controlled by cooling rate and atmosphere. The Zn particles exhibit spherical and hexagonal particle morphology with a particle size varying between 200nm and 3µm. However the particles were formed by aggregation of nanoparticles which are primarily nucleated from the gas phase. Copyright © 2017 Elsevier Ltd. All rights reserved.

Cortisol production rates measured by liquid chromatography/mass spectrometry

International Nuclear Information System (INIS)

Esteban, N.V.; Yergey, A.L.

1990-01-01

Cortisol production rates (FPRs) in physiologic and pathologic states in humans have been investigated over the past 30 years. However, there has been conflicting evidence concerning the validity of the currently accepted value of FPRs in humans (12 to 15 mg/m2/d) as determined by radiotracer methodology. The present study reviews previous methods proposed for the measurement of FPRs in humans and discusses the applications of the first method for the direct determination of 24-hour plasma FPRs during continuous administration of a stable isotope, using a thermospray high-pressure liquid chromatography-mass spectrometry technique. The technique is fast, sensitive, and, unlike gas chromatography-mass spectrometry methods, does not require derivatization, allowing on-line detection and quantification of plasma cortisol after a simple extraction procedure. The results of determination of plasma FPRs by stable tracer/mass spectrometry are directly in units of mass/time and, unlike radiotracer methods, are independent of any determination of volume of distribution or cortisol concentration. Our methodology offers distinct advantages over radiotracer techniques in simplicity and reliability since only single measurements of isotope ratios are required. The technique was validated in adrenalectomized patients. Circadian variations in daily FRPs were observed in normal volunteers, and, to date, results suggest a lower FRP in normal children and adults than previously believed. 88 references

21 CFR 862.2250 - Gas liquid chromatography system for clinical use.

Science.gov (United States)

2010-04-01

... 21 Food and Drugs 8 2010-04-01 2010-04-01 false Gas liquid chromatography system for clinical use... Instruments § 862.2250 Gas liquid chromatography system for clinical use. (a) Identification. A gas liquid chromatography system for clinical use is a device intended to separate one or more drugs or compounds from a...

Co-processing of agricultural plastic waste and switchgrass via tail gas reactive pyrolysis

Science.gov (United States)

Mixtures of agricultural plastic waste in the form of polyethylene hay bale covers (PE) (4-37%) and switchgrass were investigated using the US Department of Agriculture’s tail gas reactive pyrolysis (TGRP) at different temperatures (400-570 deg C). TGRP of switchgrass and plastic mixtures significan...

State-of-the art of selective detection and identification of I-, Br-, Cl-, and F-containing compounds in gas chromatography and liquid chromatography.

Science.gov (United States)

Brede, Cato; Pedersen-Bjergaard, Stig

2004-09-24

This review article presents an overview of halogen-specific detection in gas chromatography (GC) and liquid chromatography (LC). Attention is primarily focused on the use of plasma emission spectroscopy and plasma mass spectrometry as detectors, but other halogen-selective detection principles are also mentioned. Different instrumental configurations are discussed both with respect to technical set-up and performance, the principal reasons for halogen-selective detection are highlighted, and recent applications are reviewed from areas such as environmental chemistry, petroleum characterization, and drug analysis.

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

Combined thin layer chromatography and gas chromatography with mass spectrometric analysis of lipid classes and fatty acids in malnourished polar bears (Ursus maritimus) which swam to Iceland.

Science.gov (United States)

Eibler, Dorothee; Krüger, Sabine; Skírnisson, Karl; Vetter, Walter

2017-03-01

Between 2008 and 2011, four polar bears (Ursus maritimus) from the Greenland population swam and/or drifted on ice to Iceland where they arrived in very poor body condition. Body fat resources in these animals were only between 0% and 10% of the body weight (usually 25%). Here we studied the lipid composition in different tissues (adipose tissue if available, liver, kidney and muscle). Lipid classes were determined by thin layer chromatography (TLC) and on-column gas chromatography with mass spectrometry (GC/MS). The fatty acid pattern of total lipids and free fatty acids was analyzed by GC/MS in selected ion monitoring (SIM) mode. Additionally, cholesteryl esters and native fatty acid methyl esters, initially detected as zones in thin layer chromatograms, were enriched by solid phase extraction and quantified by GC/MS. The ratio of free fatty acids to native fatty acid methyl esters could be correlated with the remained body lipids in the polar bears and thus may also serve as a marker for other starving animals or even for humans. Copyright © 2017 Elsevier B.V. All rights reserved.

Microextraction with polyethersulfone for bisphenol-A, alkylphenols and hormones determination in water samples by means of gas chromatography-mass spectrometry and liquid chromatography-tandem mass spectrometry analysis.

Science.gov (United States)

Ros, O; Vallejo, A; Blanco-Zubiaguirre, L; Olivares, M; Delgado, A; Etxebarria, N; Prieto, A

2015-03-01

In the present work, the suitability of polyethersulfone (PES) tube was assessed for the simultaneous sorptive microextraction of commonly found endocrine disrupting compounds in natural waters such as bisphenol-A (BPA), nonylphenol technical mixture (NP mix), 4-tert-octylphenol (4tOP), 4-n-octylphenol (4-nOP), 17β-estradiol (E2) and 17α-ethynilestradiol (EE2). After the concentration of target compounds in the PES polymer, the analytes were recovered soaking the polymer with a suitable solvent (ethyl acetate or methanol), derivatized using N,O-bis(trimethylsilyl)trifluoroacetamide with 1% of trimethylchlorosilane (BSTFA+1% TMCS) and determined by gas chromatography-mass spectrometry (GC-MS). The analysis was also performed without derivatization step by means of liquid chromatography-tandem mass spectrometry (LC-MS/MS). Extraction parameters (addition of MeOH, ionic strength, extraction speed and time and desorption time) were evaluated and the optimum conditions were fixed as follows: 150 mL water samples containing a 10% (w/v) of sodium chloride and using 5 tubular PES sorbent fibers (1.5 cm length×0.7 mm o.d.). Equilibrium conditions were achieved after 9 h, with absolute extraction efficiencies ranging from 27 to 56%. On the whole, good apparent recoveries were achieved (68-103% and 81-122% for GC-MS and LC-MS/MS, respectively) using deuterated analogues as surrogates. Achieved quantification limits (LOQs) varied between 2-154 ng/L and 2-63 ng/L for all the compounds using GC-MS and LC-MS/MS, respectively. The effect of organic matter was evaluated previous to apply the final method to the analysis of estuarine and wastewater real samples. The comparison of both methods showed that overall, PES-LC-MS/MS provided shorter sample preparation time and better LODs, but PES-silylation-GC-MS allowed the simultaneous determination of all the studied compounds with adequate repeatability and accuracy. Copyright © 2014 Elsevier B.V. All rights reserved.

Fuels and chemicals from equine-waste-derived tail gas reactive pyrolysis oil: technoeconomic analysis, environmental and exergetic life cycle assessment

Science.gov (United States)

Horse manure, whose improper disposal imposes considerable environmental costs, constitutes an apt feedstock for conversion to renewable fuels and chemicals when tail gas reactive pyrolysis (TGRP) is employed. TGRP is a modification of fast pyrolysis that recycles its non-condensable gases and produ...

[Determination of short chain chlorinated paraffins in polyvinyl chloride plastics by gas chromatography-negative chemical ion/mass spectrometry].

Science.gov (United States)

Xing, Yuanna; Lin, Zhihui; Feng, Anhong; Wang, Xin; Gong, Yemeng; Chen, Zeyong

2015-02-01

A novel method was established to determine short chain chlorinated paraffins (SC-CPs) in polyvinyl chloride (PVC) plastics by gas chromatography-negative chemical ion/mass spectrometry (GC-NCI/MS). Ultrasonic extraction was used to extract SCCPs from PVC plastics. The optimal extraction time was 1.5 h, and concentrated sulfuric acid was adopted to purify the extracted solution. Finally, SCCPs in a sample were detected by GC-NCI/MS at 160 C and with methane reagent gas at 1. 5 mL/min. This method was not influenced by medium chain chlorinated paraffins (MCCPs) in the sample, and accurate quantitation was made for SCCPs. Twelve batches of samples were analyzed and SCCPs were detected in each batch with the contents from 0. 3 x 10(2)mg/kg to 3. 5 x 10(4)mg/kg. With respect to European limitation of SC-CPs (1%), four batches of samples did not comply with the European regulation, and they accounted for 33. 3%. Obviously, high SCCPs risk was presented in PVC plastics.

[Determination of acetochlor and oxyfluorfen by capillary gas chromatography].

Science.gov (United States)

Xiang, Wen-Sheng; Wang, Xiang-Jing; Wang, Jing; Wang, Qing

2002-09-01

A method is described for the determination of acetochlor and oxyfluorfen by capillary gas chromatography with FID and an SE-30 capillary column (60 m x 0.53 mm i. d., 1.5 microm), using dibutyl phthalate as the internal standard. The standard deviations for acetochlor and oxyfluorfen concentration(mass fraction) were 0.44% and 0.47% respectively. The relative standard deviations for acetochlor and oxyfluorfen were 0.79% and 0.88% and the average recoveries for acetochlor and oxyfluorfen were 99.3% and 101.1% respectively. The method is simple, rapid and accurate.

Hydrogen sulfide measurement by headspace-gas chromatography-mass spectrometry (HS-GC-MS): application to gaseous samples and gas dissolved in muscle.